TW568965B - A polyester fiber and fabric made thereof - Google Patents
A polyester fiber and fabric made thereof Download PDFInfo
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568965 五、發明説明(1 ) 本發明係有關一種聚三甲撐對苯二甲酸酯系纖維,特 別是有關於常壓下可利用陽離子染料,分散染料中任何一 種或雙方染料進行深色染色之,聚三甲撐對苯二甲酸酯系 纖維及使用其之布料。 聚三甲撐對苯二甲酸酯纖維爲,具有來自低彈性率的 柔軟觸感,優良彈性回復性與類似尼龍纖維之性質及兼具 免燙性,尺寸安定性,耐變黃性等類似聚乙撐對苯二甲酸 酯纖維之性質的劃時代纖維,因此,可將其特徵應用於衣 料,地毯等。 但,聚三甲撐對苯二甲酸酯纖維有染色方面之問題存 在。即,.已知之聚三甲撐對苯二甲酸酯纖維所使用的染料 需限定爲分散染料,且需於1 1 0〜1 2 0°C之高壓下方 能進行深色染色,因此,在染色.上存在著非常大的問題。 纖維所使用之染料限定爲分散染料的情形下,會降低 所得染色物之鮮明性及使乾洗堅牢性,濕摩擦堅牢性,昇 華堅牢性等變差。 另外,要進行深色染色時,其染色溫度爲1 1 0〜 好潆部中史桴冷杓Κ.Τ-消f'合:^社印¾ ----------m 1 * i yN ---^---0— T 、-u (^'1間-«釕而之注&窬項.;€::項8木1二 1 2 0 °C,結果這類高溫會造成熱分解而無法使混用的其 他纖維之布料進行染色。其例如,混用聚三甲撐對苯二甲 酸酯纖維及聚尿烷彈性絲,羊毛,絲綢,乙酸鹽等其他纖 維時,雖能得到具有目前所沒有之柔軟觸感的混用布料, 但,當染色階段超過1 1 0 °C時,這些其他纖維令明顯降 低強度及白化而失去透明性,因此有明顯損害商品性之問 題。 本纸張尺度適用中國國家彳?專(CNS ) Λ川L仏(210〆 ?〜'·、/:· ) _4· 568965 五、發明説明(2 ) 目前尙未出現一種能於常壓下利用陽離子染料,分散 染料中任何一種或雙方染料進行深色染色之能解決上述問 題的聚三甲撐對苯二甲酸酯纖維。 而且,於已知之技術範圍內仍無可利用分散染料以外 之染料,例如陽離子染料進行染色的技術。 ' 雖然尙無有關對聚三甲撐對苯二甲酸酯纖維的具體應 用之記載,但,已知的對提高以聚乙撐對苯二甲酸酯纖維 爲中心之聚酯纖維對陽離子染料之染色性的方法有,於聚 縮合反應結束前將具有磺酸金屬鹼或磺酸4級辚鹼之間苯 二酸加入聚酯中,使其共聚合之方法(特公昭3 4 — 10497號公報,特公昭47 — 22334號公報,特 開平5 — 2 3 0 7 1 3號公報)。但,所得之纖維於常壓 下不具陽離子染料之可染性,又,因其彈性率較高,故只 能得到堅硬的布料。另外,已知的於常壓下可賦予陽離子 可染性之方法有,於聚乙撐對苯二甲酸酯中以具有磺酸金 屬鹼之間苯二酸與己二酸,間苯二酸般二羧酸或其烷基酯 作爲共聚合成分之方法(例如,特開昭5 7 — 6 6 1 1 9 號公報)。但,所得之纖維會提高彈牲率,故只能得到硬 梆梆的布料。 對分散染料具有良好染色性及可降低彈性率之具有優 良彈性回復性的纖維例子如,特開昭5 2 — 5 3 2 0號公 報所揭示的聚三甲撐對苯二甲酸酯纖維,又,特表平9 -5 0 9 2 2 5號公報中則揭示,可於常壓下利用分散染料 對聚三甲撐對苯二甲酸酯纖維進行染色之方法。但,這些 : .II · I _ * - 1 ml -:-! I -- 1 - - -, f J'·、1 I—-I ........ -1 - —In V J 、-口 (对1間 而之本刃) 本紙张尺度適用中國國專(CNS ) A川:仏() . c . 568965568965 V. Description of the invention (1) The present invention relates to a polytrimethylene terephthalate fiber, and in particular, to the use of cationic dyes, disperse dyes, or both dyes for dark dyeing under normal pressure. , Polytrimethylene terephthalate fiber and cloth using it. Polytrimethylene terephthalate fiber is a soft polymer with low elasticity, excellent elastic recovery and similar properties to nylon fibers, and has both iron-free properties, dimensional stability, and yellowing resistance. Ethylene terephthalate fiber is an epoch-making fiber. Therefore, its characteristics can be applied to clothing, carpets, etc. However, polytrimethylene terephthalate fibers have problems with dyeing. That is, the known dyes used in polytrimethylene terephthalate fibers must be limited to disperse dyes, and they must be capable of dark-color dyeing under a high pressure of 110 to 120 ° C. Therefore, There are very big problems. When the dye used in the fiber is limited to a disperse dye, the sharpness of the obtained dyed matter is reduced, and the fastness to dry cleaning, the fastness to wet rubbing, and the fastness to sublimation are deteriorated. In addition, when dark-colored dyeing is to be performed, the dyeing temperature is 1 1 0 to 桴. 桴. 桴 -.f ′ 合: ^ 社 印 ¾ ---------- m 1 * i yN --- ^ --- 0— T 、 -u (^ '1 room- «ruthenium note & 窬 item .; € :: item 8 wood 1 2 1 2 0 ° C High temperature will cause thermal decomposition and cannot be used to dye other mixed fabrics. For example, when using polytrimethylene terephthalate fibers and polyurethane elastic silk, wool, silk, acetate and other fibers, It is possible to obtain a mixed-use cloth with a soft touch that is not presently available. However, when the dyeing stage exceeds 110 ° C, these other fibers significantly reduce strength and whitening, and lose transparency, so there is a problem that the commerciality is significantly impaired. This paper size is applicable to the Chinese National Institute of Technology (CNS) Λ 川 L 仏 (210〆? ~ '·, /: ·) _4 · 568965 V. Description of the invention (2) At present, there is no one that can be used under normal pressure. Polytrimethylene terephthalate fibers that can solve the above problems by dyeing dark colors of any one or both of cationic dyes and disperse dyes. Also, it is known In the technical scope, there is still no technology that can use dyes other than disperse dyes, such as cationic dyes. 'Although there is no record about the specific application of polytrimethylene terephthalate fibers, it is known that The method for improving the dyeability of cationic dyes of polyester fibers centered on polyethylene terephthalate fibers is to have a sulfonic acid metal base or a sulfonic acid class 4 sulfonium base before the polycondensation reaction is completed. Method for adding diacid to polyester and copolymerizing it (Japanese Patent Publication No. 3 4-10497, Japanese Patent Publication No. 47-22334, Japanese Patent Publication No. 5-2 3 0 7 13). However, the obtained fiber There is no dyeability of cationic dyes under normal pressure, and because of its high elasticity, only hard cloths can be obtained. In addition, known methods that can impart cationic dyeability under normal pressure are: A method for using ethylene terephthalate to copolymerize phthalic acid, adipic acid, isophthalic acid-like dicarboxylic acid or an alkyl ester thereof with a metal sulfonic acid base (for example, JP-A-2004 5 7 — 6 6 1 1 9). However, the income Fibers can increase the rate of elasticity, so only rigid fabrics can be obtained. Examples of fibers with good dyeability to disperse dyes and excellent elastic recovery properties that can reduce the elasticity rate are shown in JP 5 2 — 5 3 2 0 The polytrimethylene terephthalate fiber disclosed in the gazette, and the special publication No. 9 -5 0 9 2 2 5 discloses that the polytrimethylene terephthalate can be used for disperse dyes under normal pressure. Method for dyeing formate fiber. But these: .II · I _ *-1 ml-:-! I-1---, f J '·, 1 I—-I ...... .. -1-—In VJ 、 -mouth (to the edge of 1) This paper size is applicable to China National Academy of Sciences (CNS) A Chuan: 仏 (). C. 568965
A 五、發明説·明(3 ) ' 纖維均無法於常壓下利用陽離子染料進行染色。另外,經 本發明者們詳細檢討後發現,對分散染料而言,在已知文 獻所揭示之技術中,於常壓下僅能進行染料濃度極薄之染 色。例如,特表平9 — 5 0 9 2 2 5號公報之實施例中所 使用的染料濃度僅爲0 .5 % 〇 w f (此% 〇 w f單位係 指,染液中經染料濃度染色之纖維的重量% )。但,在衣 料領域裏除了淡色,中色布料外,仍需要深色布料。而這 類深色布料之染料濃度需爲4 % 〇 w f以上,又,視場合 此濃度需爲1 0%owf以上,但,聚三甲撐對苯二甲酸 酯纖維於常壓下無法充分抽空染料,因此無法染成深色。 故本發明之目的爲,提供一種於常壓下可利用陽離子 染料,分散染料中任何一種或雙方染料進行深色染色之聚 三甲撐對苯二甲酸酯系纖維。 本發明之另一目的爲,提供一種能使混用聚尿烷彈性 纖維,羊毛,絲綢,乙酸鹽等之複合纖維製品於不損及其 較低之耐熱牲的纖維物性下,進行染色之聚三甲撑對苯二 甲酸酯系纖維。 經嫡部中次样冷ΛΜ.Τ.消f'合竹社印氣 本發明之另一目的爲,提供一種由常壓下能牢固染色 之聚三甲撐對苯二甲酸酯系纖維與其他纖維材料交織,混 紡,交編而成之布料。 又,本發明亦包含一具體目的,其爲,提供一種可利 用常用之常壓染色設備,以簡單·方法進行牢固染色之聚尿 烷彈性纖維與聚三甲撐對苯二甲酸酯系纖維的混用布料。 經本發明者們專心硏究後發明,以利用特定之共聚合 木紙张尺度適用中國國家«枣(CNS ) Λ川:仏(Τι0x7^/:' /; a 568965 五、發明説明(4 ) 比率使特定的第成分共聚合之聚三甲撐對苯二甲酸酯作 爲聚合物,而調製成的具有一定損耗正接之峰溫度,彈性 率,彈性回復率等範圍的聚酯纖維可解決上述問題,而完 成了本發明。 -即,本發明的第一項發明係特徵爲,於聚三甲撐對苯 二甲酸酯中使第3成分共聚合而成之聚酯所形成的纖維中 ,第3成分爲,共聚合比率0 · 5〜5克分子%之酯形成 性磺酸鹽化合物,又,此纖維之損耗正接的峰溫度爲8 5 〜1 1 5 °C,纖維之彈性率Q ( g / d )與彈性回復率R (% )之關係符合下列式(1 )之聚酯纖維及使用其的布 料。 . 、 〇 · 1 8 S Q / R $ 0 · 4 5 .........式(1 ) 本發明之第二項發明係特徵爲,於聚三甲撐對苯二甲 酸酯中使第3成分共聚合而成之聚酯所形成的纖維中,第 3成分爲,選自小共聚合比率1·5〜12重量%之碳數 4〜1 2的脂肪族或脂環式乙二醇,(2 )共聚合比率3 〜9重量%之碳數2〜1 4的脂肪族或脂環式二殘酸,或 者間苯一酸’ (3)共聚合比率3〜10重量%的聚院撐 二醇中的至少一種之化合物,又,此纖維之損耗正接的峰 溫度爲8 5〜1 0 2 °C,此纖維之彈性率q ( g / 與 彈性回復率R ( % )之關係符合下列式(1 )的聚酯纖維 及使用其之布料。 本纸张尺度適用中國國家ft卑(CNS ) j: / ----------------- 568965 五、發明説明(5 ) 0 · 1 8 S Q / R $ 0 · 4 5 .........式(1 ) ---------^—— (計1間遠背而之注項^項寫本S } 構成本發明之聚酯纖維的聚合物爲,於聚三甲撐對苯 二甲酸酯中使特定量之第3成分共聚合的聚酯,又广此聚 三甲撐對苯二甲酸酯係指1以對苯二酸爲酸成分且以三甲 二醇(1,3 -丙二醇)爲二醇成分的聚酯。. 因以特定量之酯形成性磺酸鹽化合物作爲共聚合的第 3成分,故可得到常壓下陽離子染·料可染性纖維。又,因 係與特定量之(1 )碳數4〜1 2之脂肪族或脂環式乙二 -醇’ (2)碳數2〜14之脂肪族或脂環式二羧酸,或者 間苯二酸,(3 )聚烷撐二醇中所選出至少一種之化合物 共聚合,故可得到常壓下分散染料可染性纖維。 本發明所使用之酯形成性磺酸鹽化合物例子如,下列 一般式所示之合磺酸鹽基化合物。A V. Invention Statement · Ming (3) 'No fiber can be dyed with cationic dyes under normal pressure. In addition, after a detailed review by the inventors, it was found that, for the disperse dyes, in the technology disclosed in the known literature, only dyeing with extremely low dye concentrations can be performed under normal pressure. For example, the dye concentration used in the examples of Japanese Patent Publication No. 9-5 0 9 2 2 5 is only 0.5% 〇wf (this% 〇wf unit refers to the fiber dyed in the dyeing solution with dye concentration the weight of% ). However, in the field of clothing, in addition to light-colored, medium-colored fabrics, dark fabrics are still required. The dye concentration of such dark fabrics must be above 4% 0wf, and depending on the occasion, this concentration must be above 10% owf. However, polytrimethylene terephthalate fibers cannot be fully evacuated under normal pressure. Dyes cannot be dyed dark. It is therefore an object of the present invention to provide a polytrimethylene terephthalate fiber which can be dyed in a dark color using any one or both of cationic dyes and disperse dyes under normal pressure. Another object of the present invention is to provide a polytrimethylene which can be used for mixing composite fiber products such as polyurethane elastic fibers, wool, silk, acetate, etc., without damaging the physical properties of fibers with low heat resistance. Terephthalate fiber. Middle-order sample cold ΛΜ.Τ. 消 f ′ 合 竹 社 印 气 in the warp section Another object of the present invention is to provide a polytrimethylene terephthalate fiber and other fibers which can be dyed firmly under normal pressure. Interwoven, blended, and interwoven fabrics of fiber materials. In addition, the present invention also includes a specific object, which is to provide a polyurethane fiber and a polytrimethylene terephthalate fiber which can be firmly dyed in a simple and simple manner by using ordinary atmospheric dyeing equipment. Mix fabric. The present inventors invented after intensive research to use the specific copolymerized wood paper size to apply the Chinese country «Jujube (CNS) Λ 川: 仏 (Τι0x7 ^ /: '/; a 568965 V. Description of the invention (4) ratio Polytrimethylene terephthalate copolymerized with a specific first component as a polymer, and a polyester fiber prepared with a certain range of peak temperature, elastic modulus, elastic recovery rate, etc., can solve the above problems. The present invention has been completed.-That is, the first invention of the present invention is characterized in that, in the fiber formed from a polyester obtained by copolymerizing the third component in polytrimethylene terephthalate, the third The composition is an ester-forming sulfonate compound having a copolymerization ratio of 0.5 to 5 mol%, and the peak temperature at which the loss of this fiber is directly connected is 8 5 to 1 15 ° C, and the elastic modulus of the fiber Q (g / d) and the elastic recovery rate R (%) The polyester fiber and the cloth using it are in accordance with the following formula (1).. 〇 · 18 SQ / R $ 0 · 4 5 ....... .. Formula (1) The second invention of the present invention is characterized in that the third component is co-existed in polytrimethylene terephthalate. In the fiber formed from the polymerized polyester, the third component is an aliphatic or alicyclic ethylene glycol selected from a carbon number of 4 to 12 with a small copolymerization ratio of 1.5 to 12% by weight, (2 ) Copolymerization ratio of 3 to 9% by weight of aliphatic or alicyclic di-residual acid with carbon number of 2 to 14 or isophthalic acid '(3) Polyaerythylene glycol with copolymerization ratio of 3 to 10% by weight The compound has at least one of the following compounds, and the peak temperature of the loss of the fiber is 8 5 ~ 10 2 ° C, and the relationship between the elastic modulus q (g / and the elastic recovery rate R (%) of the fiber conforms to the following formula ( 1) Polyester fiber and the cloth used in it. The paper size is applicable to the Chinese national ft (CNS) j: / ----------------- 568965 V. Description of the invention (5 ) 0 · 1 8 SQ / R $ 0 · 4 5 ......... Equation (1) --------- ^ —— (including 1 far-reaching note ^ item Script S} The polymer constituting the polyester fiber of the present invention is a polyester in which a specific amount of the third component is copolymerized in polytrimethylene terephthalate, and this polytrimethylene terephthalate is widely used. Ester means 1 with terephthalic acid as the acid component and trimethyl glycol (1,3-propanediol) Polyester with a diol component. Since a specific amount of an ester-forming sulfonate compound is used as the third component for copolymerization, cationic dyes and dyeable fibers can be obtained under normal pressure. (1) aliphatic or alicyclic ethylene glycol with 4 to 12 carbons' (2) aliphatic or alicyclic dicarboxylic acid with 2 to 14 carbons, or isophthalic acid, (3) At least one selected compound of the polyalkylene glycol is copolymerized, so disperse dyeable fibers can be obtained under normal pressure. Examples of the ester-forming sulfonate compound used in the present invention are sulfonate-based compounds represented by the following general formulas.
RR
2 Μ R 3 I ο Z —— S 爲 2 R f τχ R 中 式 Η 〇 〇2 Μ R 3 I ο Z ——S is 2 R f τχ R Chinese formula Η 〇 〇 〇
R 〇 〇 C R 〇 c 〇 Η Η 〇 Η c Η Η c /IV 〇 〇 c 基 烷 之 m 爲R 〇 〇 C R 〇 c 〇 Η 〇 〇 Η c Η Η c / IV 〇 〇 c m
基 之 異 相 或 同 相 爲 可 2 R Η中整 ρΟ其之屬 ](^ ^ 以爲Μ Η 〇 R 數 ,、 碳又式 爲,或 4 R ) 或,數 Η ΝThe heterogeneous or homogeneous phase of the base is the integer ρΟ 2R 其 in which it belongs] (^ ^ thought as M Η 〇 R number, and the carbon formula is, or 4 R) or, the number Η Ν
IX 與 適 I度 尺 紙IX and moderate I degree rule paper
Ts C 一準 568965 Λ 7 n? 一 -1 - _____ι _ _ 五、發明説明(6 ) — PR3R4R5R6所示之鐵基(其中,R3,R4,R5, R6爲選自氫原端子b,烷基,芳基及羥基烷基中相同或相 異之基,又以碳數1〜10之烷基爲佳)。若Μ爲金屬時 ,又以鹼金屬,鹼土類金屬爲佳。Ζ爲3價之有機基,又 以3價之芳基族基爲佳。 這類使酯形成性磺酸鹽化合物共聚合之情形下,可得 到常壓下能以陽離子染料染成深色的纖維。另外,比起聚 三甲撐對苯二甲酸酯均聚物纖維,其對分散染料今成爲易 染性。至於本發明之常壓下可染色一事係指,9 0 °C下對 纖維的抽空率可達7 0%以上。 另外,此陽離子可染絲具有適度的鹼減量特性,因此 ,可利用鹼減量而得到更柔軟之觸感。此鹼減量待指,於 鹼性水溶液中對布料進行加熱時,可溶解纖維表面之部分 聚合物。又,適度的鹼減量係指,可利用工業方式控制鹼 減量之量及速度。另一項驚人特徵爲,例如,實質上陽離 子可染之聚乙撐對苯二甲酸酯纖維的鹼減量速度太快,無 法利用工業方式加以控制,但,本發明之聚酯纖維之鹼減 量速度可同陽離子不可染之一般的聚乙撐對苯二甲酸酯纖 維,利用已知之方法進行鹼減量。因此,經鹼減量之本發 明的聚酯纖維除了可更柔軟外,還具有因纖維表面存在數 // m程度之微細孔,而具有乾爽感及可使染色更顯明等特 徵。 較佳之酯形成性磺酸鹽化合物的具體例子如,5 -鈉 磺基間苯二酸,5 —鉀磺基間苯二酸,4 一鈉磺基一 2 , 木紙张尺度適用中國國家Ϊ?皁(CNS ) Λ川:,¾ ( 21(Γχ Π ι . Q ~ ' 568965 A 7 _________ )\1 • ’一一一’ *·一 丨_丨 _ —- ·- 一, 一_ . » »_—»〆·_ - « «*-,—·,丨丨丨— __ 五、發明説明(7 ) 6 -萘二羧酸,2 —鈉磺基—4 —羥基安息香酸,3,5 一二羧酸苯磺酸四甲基鳞鹽,3 ,5 一二羧酸苯磺酸四丁 基鱗鹽,3 ,5 -二羧酸苯磺酸三丁基甲基鱗鹽,2,6 —二羧酸萘—4 一磺酸四丁基鳞鹽,2,6 —二羧酸萘、— 4 一磺酸四甲基鱗鹽,3,5 -二羧酸苯磺酸銨鹽等‘,或 這些化合物之甲酯,二甲基酯等酯衍生物。其中又以其甲 酯,二甲基酯等酯衍生物因具有優良之聚合物白度,聚合 速度而特別佳。 此酯形成性磺酸鹽化合物對聚三甲撐對苯二甲酸酯之 共聚合比率需爲,對構成聚酯之全部酸成分的總克分子數 爲0 · 5〜5克分子%。荐此酯形成性磺酸鹽化合物之共 聚合比率低於0 . 5克分子%時,常壓下將無法利用陽離 子染料進行染色。又,酯野成性磺酸鹽化合物之比率超過 5克分子%時,除了會使聚合物之耐熱性變差及使聚合性 ,紡絲性變得非常差外,還會使纖維變黃。就對陽離子染 料能充分維持染色性及兼具聚合性,紡絲性觀點,又以1 〜3克分子%爲佳,特佳爲1·2〜25克分子%。 本發明所使用之碳數4〜1 2的脂肪族乙二醇,’脂環 式乙二醇之具體例子如,1 ,2 —丁二醇,1 ,3 一丁二 醇,1 ,4 — 丁二醇,新戊二醇,1 ,5 —戊撐二醇,1 ,6 -己撐二醇,庚撐二醇,辛撐二醇,癸撐二醇,十二 撐二醇,1 ,4 一環己二醇,1 ,3 —環己二醇,1 ,2 一環己二醇,1 ,4 一環己烷二甲醇,1 ,3 —環己烷二 甲醇,1 ,2 —環己烷二甲醇等。因這些乙二醇與聚三甲 本纸张尺度適用中國國家牦隼(CNS ) Λ‘1β仏(2】0χ _ 568965 五、發明説明(8 ) 撐對苯二甲酸酯共聚合,故常壓下可利用分散染料染成深 色。就具有優良之聚合物的白度,熱分解性,耐光性觀點 ,這些脂肪族或脂環式·乙二醇中夂以1 ,4 — 丁二醇,1 ,6 —己撐二醇,新戊二醇,環己烷二甲醇爲佳。另外, 就具有優良之聚合速度,乾洗堅牢性觀點又以1 ,4 -丁 二醇特別佳。 丨聚- 這些乙二醇對聚三甲撐對苯二甲酸酯之共聚合比率需 爲,對聚合物重量爲1·5〜12重量%。若共聚合比率 低於1 · 5重量%時,常壓下將無法利用分散染料染成深 、-口 色。另外,乙二醇之共聚合比率與彈性,彈性回復率,熔 點,玻璃化點,染色性等具有非常大的相關性。因此,當 共聚合比率超出1 2重量%時,今有明顯地降低熔點或玻 璃化點,使熱/固定性之後加工或整燙等一般使用階段下的 觸感變硬及,降低染色後布料的乾洗堅牢性等缺點。其中 又以2〜1 0重量%爲佳,更佳爲3〜7重量%。 •本發明所使用的碳數2〜1 4之脂肪族或脂環式二羧 酸的具體例子如,草酸,丙二酸,琥珀酸,戊二酸,己二 酸,庚二酸,辛二酸,癸二酸,月桂二酸,2 一甲基戊二 酸,2 —甲基己二酸,富馬酸,馬來酸,衣康酸,1 , 4 一環己烷二羧酸,1 ,3 —環己烷二羧酸,;l , 2 一環己 烷二羧酸等。因這些二羧酸與聚三甲撐對苯二甲酸酯共聚 合,故常壓下可利用分散染料染成深色。 就共聚合時具有優良之聚合速度及具有優良耐光性觀 點,這些脂肪族或脂環式二羧酸或者間苯二酸中又以癸二 木紙張尺度適用中國國家(Ι準(CNS ) Λ川:H 210m" T:•一一 --------------------------- 568965 五、發明説明(9 ) • 一 酸,月桂一酸,1 ,4 一環己烷二羧酸,間苯二酸爲佳。 另外,就聚合物具有優良之乾洗堅牢度觀點,又以間苯二 酸特別佳。 - I: I («先問-«^1:而之;τ&1ν 項巧^、:·^本 rc:: 這些脂肪族或脂環式二羧酸或者間苯二酸對聚三甲撐 對苯二甲酸酯之共聚合比率需爲,對聚合物重量爲3〜9 重量%。若共聚合比率低於3重量%時,常壓下將無法染 成深色。又,共聚合比率超過9重量%時,會明顯地降低 熔點或玻璃化點,因此,會有使熱固定性之後加工或整湯 等一般使用階段下的觸感變硬及,降低染色後布料的乾洗 堅牢性等缺點。其中又以3〜8重量%爲佳,更佳爲3〜 7重量%。 經滅部中吹行消贽合0社印¥ 本發明亦可使用聚烷撐二醇作爲共聚合成分。若以共 聚合乙二醇或酸者作爲第3成分時,會降低熔點而使紡絲 性變差及,對所得纖維進行後加工時,會因熱,熱源而產 生熔著或明顯收縮等,故會使處理性變差。但,以聚烷撐 二醇作爲第3成分時,不會降低熔點,因此不會有前述之 問題。其因爲,其分子量較大,因此會使聚合物中的聚烷 撐二醇局在化。又,所使用之聚烷撐二醇可爲聚乙二醇, 聚三甲二醇,聚四甲二醇或其共聚合物中任何一種,但, 就熱安定觀點,又以聚乙二醇最佳。 , 另外,聚烷撐二醇之平均分子量較佳爲3 0 0〜 20000。若平均分子量低於300時,會因含有較佳 分子量之聚烷撐二醇,而於高真空下聚合時減壓餾去’結 果所得聚合物中所含之聚烷撐二醇量將無一定性。因此 本紙張尺度適用中國國家柯專(CNS )八‘川:仏(210,χ 丨 -12 - 568965 Λ 7 * IP ___ 五、發明説明(10 ) 將使原絲之強伸度物性,染色性,熱特性等不均勻’故製 品之特性將不齊。 I - .......I -------- 1· - I i I I - : Λ -1 m , \―Ψ 、-口 (^lwM^:而之、項^¾ 本.rczc ) 又,平均分子量超過2 0 0 0 0時,會因聚合物中存 在差多量的未共聚合之高分子量聚烷撐二醇,而降低染色 性,乾洗堅牢性,耐光堅牢性。聚烷撐二醇之平均分子量 又以400〜10000爲佳,更佳爲500〜5000 0 \ 聚烷撐二醇對聚三甲撐對苯二甲酸酯之共聚合比率需 爲,對聚合物重量爲3〜1 0重量%。若聚烷撐二醇之比 率低於3重量%時,常壓下無法利用分散染料染成深、色。 又,聚烷撐二醇之比率超過1 〇重量%時,會降低聚合物 之耐熱性及使聚合性,紡絲性變得非常差。另外,亦會產 生玻璃化點過低,而使熱固定性之後加工或整燙等一般使 用階段下的觸感變硬及,大幅降低染色後布料之乾洗堅牢 性,耐光堅牢性等缺點。其中又以4〜8重量%爲佳。 於不阻害本發明之目的的範圍下,構成本發明之聚酯 纖維的聚合物可與第4成分共聚合或摻合。又,既使使用 適類第4成分,亦需遵守上述之共聚合比率範圍,方能不 阻害本發明之目的。這些組合中,特別是酯形成性磺酸鹽 化合物與(1 )藤數4〜1 2之脂也族或脂環式乙二醇, (2 )碳數2〜1 4之脂肪族或脂環式二羧酸,或間苯二 酸,(3 )聚烷撐二醇中所選出至少一種之化合物共聚合 後,可得到常壓下能利用陽離子染料,分散染料雙方進行 染色之聚酯維。又,其共,聚合比率較佳爲,酯形成性磺 本紙張尺度適用中國國家代卑(CNS ) 仏(210, /_允、 -Ή - 568965 五、發明説明(11 ) 、酸鹽化合物1 : 2〜2· 5克分子%,前述(1)〜(3 )中所選出的至少一種之化合物3〜7重量%。 n n ------I ---u— n IP (邙^閲球^::而之:/Τ&φ^ϊ'-Γίτ^ϊί?本.rcc 另外,必要時本發明之聚酯纖維可與各種添加劑,例! 如,平光劑,熱安定劑,消泡劑,整色劑,難燃劑,防氧 化劑,紫外線吸收劑,紅外線吸收劑,結晶核劑,螢光@ 白劑等共聚合或混合。 本發明所使用之聚酯可利用極限黏度規定其分子量, 又,極限黏度〔7?〕較佳爲0 . 3〜2 · 0,更佳爲 0 · 3 5〜1 · 5,特別佳爲0 . 4〜1 · 2,此黏度下 可得到具有優良之強度,紡絲性的聚酯纖維。若極限黏度 低於0 . 3時,會因聚合物之聚合度過低而使紡絲性不安 定。另外,所得之纖維的強度亦不足。相反地,若極限黏 度超過2 · 0時,會因熔融黏度過高而無法平順地利用齒 輪唧筒進行計量及,會因吐出不良等降低紡絲性。 基本上,製造構成本發明之聚酯纖維的聚合物之方法 可爲,利用已知之方法進行聚合。即,於一般的聚三甲撐 對苯二甲酸酯的製造過程中,可於對苯二甲酸或對苯二酸 二甲酯等對苯二酸低級酯與三甲二醇進行酯交換反應及接 下來的聚縮合反應之任何階段添加第3成分。若此時之反 應物爲酯形成.性磺酸鹽化合物與脂肪族或脂環式二羧酸, 或間苯二酸時,因需促進其與三甲二醇之反應,故最好於 酯交換前添加,又,若爲聚烷撐二醇時,爲了防止聚合物 變黃及減壓時的突沸,最好係於酯交換反應結束後添加。 另外,爲了兼具反應速度,聚合物之白度,熱安定性’最 本紙張尺度適用中國國家牦讀·( CNS )八川:ίΓ( 210x2 V 7 :Ή· \λαΖ 568965 五、發明説明(12 ) 好使用金屬乙酸鹽,鈦烷氧化合物等酯交換觸媒〇 · 〇 1 〜0 . 1重量%。至於反應溫度則爲200〜240 °c° 又,可使用銻氧化物,鈦烷氧基等聚縮合觸媒,特別是使 用鈦烷氧基時,可兼具酯交換觸媒功用。就反應速度,聚 合物之白度觀點,對全部羧酸量之觸媒量較佳爲0 · 〇 1 〜0 . 1重量%。至於其反應溫度則爲240〜180° ,真空度則爲0 . 001〜1 t 〇 r r。另外,上述的各 種添加劑可於聚合過程之任意階段下添加,但,爲了將反 應阻害抑制至最低,較好於酯交換反應結束後之任何階段 下添加。 M消部中史桴沙為nc_T消f'合竹社印來 又,利用上述方法製得之構成本發明的聚酯纖維之聚 合物亦可利用於氮,氬等不活性氣體中,或常壓下進行固 相聚合而提高分子量。若適用這類方法時,除了可抑制聚 合物變.黃及減少造成斷絲或起毛之原因的低聚物外,還可 提高強度。固相聚合方法例如可爲,直接適用的使用聚乙 撐對苯二甲酸酯之已知的方法,但,爲了提高白度,固相 聚合前之預聚物的極限黏度較佳爲0 · 4〜0 · 8,固相 聚合溫度較佳爲1 7 0〜2 3 0 °C,時間可依所希望之黏 度而不同,一般爲3〜3 6小時。 又,成本煢明之聚酯纖維的聚合物可由,摻合2種可 得到目的之共聚合組成的聚合物而製得。例如,共聚合5 · 重量%之1 ,4 一丁二醇的聚三甲撐對苯二甲酸酯可由, 混合聚三甲撐對苯二甲酸酯9 5重量%,聚三甲撐對苯二 甲酸酯5重量%而製得。又,混合方式可爲,利用聚合爸 木紙張尺度適用中國國家;(:f牟(CNS ) Λ川:,½ ( 210x ; ί;、 _ H —·· 568965 . A? • ΙΠ 一 —-__* I I· . 1 - . M ,賴輪· · - •一一 •一 I - · ^ . . . * ,- t •㈣〜· --— 五、發明説明(13 ) : —ϋ —m I -is: -- = I-- - n I^人。—m -------- ------ -—— (^lwric:而之注項本) 混合以使其充分進行酯交換而得到,或更簡便的以片狀摻 合狀態於擠押機中進行反應。這類方法因能得到充分快速 之酯交換速度,故可得到均質聚合物。 對構成本發明之聚酯纖維的聚合物之製造方法而言, 重要的是能維持聚合物之白度。而聚三甲撐對苯二甲酸酯 與第3成分共聚合時,易於聚合過程或紡絲過程中進行著 色。因此提高白度之方法除了適用上述之較佳的觸媒量, 反應溫度外,較佳爲同時使用熱安定劑或著色抑制劑。此 熱安定劑較佳爲,5價或3價之磷化合物,例如三甲基磷 酸鹽-,三乙基磷酸鹽,三苯基磷酸鹽,三甲基亞磷酸鹽, 三乙基亞磷酸鹽,三苯基亞磷酸鹽,磷酸,亞磷酸等。其 對聚合物之添加量較佳爲0·01〜0.07重量%。另 外,著色抑制之例子如,乙酸鈷,甲酸鈷等,其對聚合物 之添加量較佳爲0·01〜0·07重量%。又,對預聚 物固相聚合時能提高白度而言,將極限黏度提高至0 · 9 以上爲極有效之方法。而所得之聚合物既使成爲纖維亦能 保有優良之白度。此白度之後述b値較佳爲一 2〜1 0, 又以一1〜6更堆。 另外,使用酯形成性磺酸鹽化合物時需特別注意,聚 合過程中於紡口組件處易生成易凝聚之物及易生成三甲撐 乙二醇二聚物(構造式: OCH2CH2CH2〇CH2CH2CH2〇H)。若凝聚 之量過多時,會增加紡口組件內的壓力上升,而易造成絲 斷裂及,爲了防止而增加紡口組件之交換頻率,因此會降 1、紙张尺度適用中國國家;枣(CNS ) Λ川:i ( 210, :、、€ ·> -16 - 568965 五、發明説明(14 ) · I m m In nn —^ϋ !!ί 1 ^ i 低生產生等問題存在。另外,若三甲撐乙二醇二聚物量過 多時,會有降低熔融時之熱安定性及耐光性等問.題。爲了 防止這類問題較好能於聚合時之任意階段中添加某種添力口 劑。此類添加劑例子如,乙酸鋰,碳酸鋰,甲酸鋰,乙酸 鈉,碳酸鈉,甲酸鈉,氫氧化鈉,氫氧化鈣,氫氧化鉀與 鹼性金屬鹽。又,其對酯形成性磺酸鹽化合物之添加量較 佳爲2 0〜4 0 0克分子%,又以7 0〜2 0 0克分子% 爲佳。Ts C quasi 568965 Λ 7 n? -1-_____ ι _ _ V. Description of the invention (6)-iron group shown in PR3R4R5R6 (wherein R3, R4, R5, R6 are selected from hydrogen terminal b, alkyl , The same or different groups in the aryl group and the hydroxyalkyl group, and the alkyl group having 1 to 10 carbon atoms is preferable). If M is a metal, alkali metals and alkaline earth metals are preferred. Z is a trivalent organic group, and a trivalent aryl group is preferred. When such an ester-forming sulfonate compound is copolymerized, fibers which can be dyed to a dark color with a cationic dye under normal pressure can be obtained. In addition, compared to polytrimethylene terephthalate homopolymer fibers, it is now more susceptible to disperse dyes. As for the dyeability under normal pressure of the present invention, it means that the evacuation rate of the fiber at 90 ° C can reach more than 70%. In addition, this cationic dyeable yarn has a moderate alkali-reducing characteristic. Therefore, the alkali-reducing can be used to obtain a softer feel. This alkali weight reduction means that when the cloth is heated in an alkaline aqueous solution, a part of the polymer on the surface of the fiber can be dissolved. In addition, a moderate alkali reduction means that the amount and rate of alkali reduction can be controlled industrially. Another amazing feature is that, for example, the alkali reduction rate of substantially cationic dyeable polyethylene terephthalate fibers is too fast to be controlled industrially, but the alkali reduction of the polyester fibers of the present invention The speed can be the same as that of ordinary polyethylene terephthalate fibers which are not dyed by cations, and alkali reduction can be performed by known methods. Therefore, in addition to the alkali-reduced polyester fiber of the present invention, in addition to being softer, it has characteristics such as fine pores on the surface of the fiber of several // m, which has a dry feel and makes dyeing more visible. Specific examples of preferred ester-forming sulfonate compounds are, for example, 5-sodium sulfoisophthalic acid, 5-potassium sulfoisophthalic acid, 4-sodium sulfo-2, and wood paper scales applicable to China. Ϊ Soap (CNS) Λ 川:, ¾ (21 (Γχ Π ι. Q ~ '568965 A 7 _________) \ 1 •' 一一 一 '* · 一 丨 _ 丨 _ —- ·-, one_. » »_—» 〆 · _-«« *-, — ·, 丨 丨 丨 — __ V. Description of the Invention (7) 6-naphthalenedicarboxylic acid, 2-sodium sulfo-4—hydroxybenzoic acid, 3, 5 Tetramethylscale salt of benzenesulfonic acid monocarboxylic acid, 3,5 Tetrabutylscale salt of benzenesulfonic acid dicarboxylic acid, Tributylmethyl scale salt of 3,5-dicarboxylic acid benzenesulfonic acid, 2,6-di Carboxylic acid naphthalene-4 tetrabutylsulfonic acid scale salt, 2,6-dicarboxylic naphthalene, tetramethyltetramethylsulfonic acid scale salt, 3,5-dicarboxylic acid ammonium benzenesulfonic acid salt, etc., or Ester derivatives such as methyl esters and dimethyl esters of these compounds. Among them, ester derivatives such as methyl esters and dimethyl esters are particularly excellent because of their excellent polymer whiteness and polymerization speed. This ester-forming sulfonic acid Copolymerization ratio of acid salt compound to polytrimethylene terephthalate It is necessary that the total number of moles of all acid components constituting the polyester is 0.5 to 5 mole%. It is recommended that when the copolymerization ratio of the ester-forming sulfonate compound is less than 0.5 mole%, often It cannot be dyed with a cationic dye under pressure. In addition, when the ratio of the ester field-generating sulfonate compound exceeds 5 mol%, in addition to the deterioration of the polymer's heat resistance and polymerizability, the spinnability becomes very high. In addition, it can also cause the fiber to turn yellow. From the viewpoint of fully maintaining the dyeability and the polymerizability and spinnability of cationic dyes, it is preferably 1 to 3 mol%, particularly preferably 1.2 to 25 g. Molecular%. The aliphatic ethylene glycol having 4 to 12 carbon atoms used in the present invention, and specific examples of the "alicyclic ethylene glycol" are, for example, 1,2-butanediol, 1,3 butanediol, 1 , 4-butanediol, neopentyl glycol, 1,5-pentanediol, 1,6-hexylene glycol, heptanediol, octylene glycol, decylene glycol, dodecyl glycol , 1, 4-cyclohexanediol, 1, 3-cyclohexanediol, 1, 2-cyclohexanediol, 1, 4-cyclohexanedimethanol, 1, 3-cyclohexanedimethanol, 1 , 2-Cyclohexanedimethanol, etc. Because these ethylene glycol and polytrimethylene paper standards are applicable to the Chinese national standard (CNS) Λ'1β 仏 (2) 0χ _ 568965 V. Description of the invention (8) p-xylene Formate copolymerization, so it can be dyed dark with disperse dyes under normal pressure. From the viewpoint of excellent polymer whiteness, thermal decomposition, and light resistance, these aliphatic or alicyclic ethylene glycol 1,4-butanediol, 1,6-hexamethylene glycol, neopentyl glycol, and cyclohexanedimethanol are preferred. In addition, it has excellent polymerization speed and 1, 4-in terms of fastness to dry cleaning. Butylene glycol is particularly preferred. Poly-The copolymerization ratio of these ethylene glycol to polytrimethylene terephthalate is required to be 1.5 to 12% by weight based on the weight of the polymer. If the copolymerization ratio is less than 1.5% by weight, it is impossible to use a disperse dye to make a deep,-mouth color under normal pressure. In addition, the copolymerization ratio of ethylene glycol has a great correlation with elasticity, elastic recovery rate, melting point, glass transition point, and dyeability. Therefore, when the copolymerization ratio exceeds 12% by weight, the melting point or the glass transition point is significantly reduced, and the tactile sensation in the general use stage such as processing or ironing after heat / fixation is hardened and the cloth after dyeing is reduced. Dry cleaning fastness and other disadvantages. Among these, 2 to 10% by weight is more preferable, and 3 to 7% by weight is more preferable. • Specific examples of aliphatic or alicyclic dicarboxylic acids having a carbon number of 2 to 14 such as oxalic acid, malonic acid, succinic acid, glutaric acid, adipic acid, pimelic acid, suberic acid Acid, sebacic acid, lauric acid, 2-methylglutaric acid, 2-methyl adipic acid, fumaric acid, maleic acid, itaconic acid, 1, 4-cyclohexanedicarboxylic acid, 1, 3-cyclohexanedicarboxylic acid; 1, 2, cyclohexanedicarboxylic acid, etc. Since these dicarboxylic acids are copolymerized with polytrimethylene terephthalate, they can be dyed dark with disperse dyes under normal pressure. From the standpoint of excellent polymerization speed and light resistance during copolymerization, these aliphatic or alicyclic dicarboxylic acids or isophthalic acid are suitable for the Chinese national standard (Secondary Standard (CNS)) : H 210m " T: • One one --------------------------- 568965 V. Description of the invention (9) • One acid, one laurel Acid, 1, 4-cyclohexanedicarboxylic acid, isophthalic acid is preferred. In addition, from the viewpoint of excellent dry fastness of polymers, isophthalic acid is particularly preferred.-I: I («Ask first- «^ 1: And; τ & 1ν terms ^,: · ^ this rc :: copolymerization ratio of these aliphatic or alicyclic dicarboxylic acids or isophthalic acid to polytrimethylene terephthalate It is required that the weight of the polymer is 3 to 9% by weight. If the copolymerization ratio is less than 3% by weight, it cannot be dyed dark under normal pressure. When the copolymerization ratio exceeds 9% by weight, it will be significantly reduced. Because of its melting point or glass transition point, it has the disadvantages of hardening the touch during general use, such as post-heat-set processing or whole soup, and reducing the dry-cleaning fastness of dyed fabrics. 3 to 8% by weight is more preferable, and 3 to 7% by weight is more preferable. The present invention can also use polyalkylene glycol as a copolymerization component. If the copolymerization of ethylene When a diol or an acid is used as the third component, the melting point is lowered, and the spinnability is deteriorated. When the obtained fiber is post-processed, heat or a heat source may cause fusion or significant shrinkage, which may result in handleability. It becomes worse. However, when polyalkylene glycol is used as the third component, the melting point is not lowered, so there is no problem described above. Because of its large molecular weight, it causes polyalkylene glycol in the polymer. It is localized. In addition, the polyalkylene glycol used may be any one of polyethylene glycol, polytrimethylene glycol, polytetramethylene glycol, or a copolymer thereof. Ethylene glycol is the best. In addition, the average molecular weight of the polyalkylene glycol is preferably 300 to 20000. If the average molecular weight is less than 300, the polyalkylene glycol may have a higher molecular weight than the polyalkylene glycol. When polymerizing under vacuum, it is distilled off under reduced pressure. As a result, the amount of polyalkylene glycol contained in the polymer obtained will not be certain. Therefore, this paper standard is applicable to the Chinese National Academy of Sciences (CNS) Ya'kawa: 仏 (210, χ 丨 -12-568965 Λ 7 * IP ___) 5. Description of the invention (10) will make the raw silk strong elongation physical properties and dyeability The thermal characteristics are not uniform, so the characteristics of the product will be different. I-....... I -------- 1 ·-I i II-: Λ -1 m, \ ―Ψ, -Mouth (^ lwM ^: and, item ^ ¾ 本 .rczc), and if the average molecular weight exceeds 20000, there will be a large amount of uncopolymerized high molecular weight polyalkylene glycol in the polymer, And reduce dyeing, dry cleaning fastness, light fastness. The average molecular weight of polyalkylene glycol is preferably 400 ~ 10000, more preferably 500 ~ 5000 0 \ The copolymerization ratio of polyalkylene glycol to polytrimethylene terephthalate needs to be It is 3 to 10% by weight. When the ratio of the polyalkylene glycol is less than 3% by weight, it is impossible to use a disperse dye to produce a deep, deep color under normal pressure. When the ratio of the polyalkylene glycol exceeds 10% by weight, the heat resistance of the polymer is lowered, the polymerizability is deteriorated, and the spinnability is extremely deteriorated. In addition, the glass transition point is too low, which makes the touch feel harder during general use such as processing or ironing after heat setting, and greatly reduces the dry-cleaning fastness and light fastness of dyed fabrics. Among them, 4 to 8% by weight is preferable. The polymer constituting the polyester fiber of the present invention may be copolymerized or blended with the fourth component so long as the object of the present invention is not hindered. In addition, even if a suitable fourth component is used, the above-mentioned copolymerization ratio range must be observed so as not to hinder the object of the present invention. Among these combinations, especially the ester-forming sulfonate compound and (1) an aliphatic or alicyclic ethylene glycol having a number of 4 to 12 and (2) an aliphatic or alicyclic carbon having a number of 2 to 1 4 After copolymerizing at least one selected compound of formula dicarboxylic acid, isophthalic acid, and (3) polyalkylene glycol, a polyester dimension can be obtained which can be dyed by both cationic dyes and disperse dyes under normal pressure. In addition, its co-polymerization ratio is preferably such that the ester-forming sulfonated paper scale is applicable to the Chinese National Substitution (CNS) 仏 (210, / _ 允, -Ή-568965) 5. Description of the Invention (11), Acid Compound 1 : 2 to 2.5 mol%, 3 to 7% by weight of at least one compound selected from the above (1) to (3). Nn ------ I --- u- n IP (邙 ^ Reading ball ^ :: And: / Τ & φ ^ ϊ'-Γίτ ^ ϊί? 本 .rcc In addition, the polyester fiber of the present invention can be used with various additives, if necessary! For example, flattening agent, heat stabilizer, consumer Foaming agent, color stabilizer, flame retardant, antioxidant, ultraviolet absorber, infrared absorber, crystal nucleating agent, fluorescent @ white agent, etc. are copolymerized or mixed. The polyester used in the present invention can be defined by its limiting viscosity. Molecular weight, and the limiting viscosity [7?] Is preferably 0.3 ~ 2 · 0, more preferably 0 · 3 5 ~ 1 · 5, particularly preferably 0.4 ~ 1 · 2, and can be obtained at this viscosity. Excellent strength and spinnable polyester fiber. If the limiting viscosity is lower than 0.3, the spinnability will be unstable due to the low polymerization degree of the polymer. In addition, the strength of the obtained fiber will be strong. On the contrary, if the limiting viscosity exceeds 2.0, the melt viscosity will be too high to smoothly measure with a gear drum, and the spinnability will be lowered due to poor ejection. Basically, the composition of the present invention constitutes The polymer of polyester fiber may be polymerized by a known method. That is, in the general manufacturing process of polytrimethylene terephthalate, it can be used in terephthalic acid or dimethyl terephthalate. The tertiary terephthalate, such as an ester, is subjected to a transesterification reaction with trimethylol and the subsequent polycondensation reaction is added at any stage. If the reactant at this time is an ester, the sulfonate compound and the aliphatic or In the case of alicyclic dicarboxylic acid or isophthalic acid, it is best to add it before transesterification because it needs to promote the reaction with trimethylol. In the case of polyalkylene glycol, in order to prevent the polymer from changing. Yellow and bumping under reduced pressure are best added after the transesterification reaction is completed. In addition, in order to have the reaction speed, the whiteness of the polymer, and the thermal stability, the paper size is applicable to Chinese national readings (CNS) Hachikawa: ίΓ (210x2 V 7: Ή · \ λαZ 568965 V. Description of the invention (12) It is good to use transesterification catalysts such as metal acetates, titanyl oxy compounds, etc. 〇1 ~ 0.1% by weight. For the reaction temperature is 200 ~ 240 ° c ° Polycondensation catalysts such as antimony oxide and titanyloxy can be used. Especially when titanyloxy is used, it can also serve as a transesterification catalyst. From the viewpoint of reaction speed and whiteness of polymers, The catalyst amount of the total carboxylic acid amount is preferably 0. 〇1 to 0.1% by weight. As for the reaction temperature, it is 240 to 180 °, and the degree of vacuum is 0.001 to 1 t 〇rr. In addition, the various additives mentioned above can be added at any stage of the polymerization process. However, in order to minimize reaction resistance, it is preferable to add at any stage after the transesterification reaction is completed. Shi Shao in M Department is printed by nc_T elimination f 'Hezhusha, and the polymer constituting the polyester fiber of the present invention prepared by the above method can also be used in inert gas such as nitrogen, argon, or often Solid phase polymerization is performed under pressure to increase the molecular weight. If this method is applied, in addition to inhibiting polymer yellowing and reducing oligomers that cause breaks or fluff, it can also increase strength. The solid-phase polymerization method may be, for example, a known method using polyethylene terephthalate as a direct applicable method. However, in order to increase the whiteness, the limiting viscosity of the prepolymer before the solid-phase polymerization is preferably 0. 4 ~ 0 · 8, the solid-state polymerization temperature is preferably 170 ~ 230 ° C, and the time can be different depending on the desired viscosity, generally 3 ~ 36 hours. In addition, a polymer of polyester fiber having a low cost can be obtained by blending two kinds of polymers to obtain a desired copolymer composition. For example, polytrimethylene terephthalate copolymerized with 5.4% by weight of 1,4-monobutylene glycol may be mixed with polytrimethylene terephthalate at 95% by weight and polytrimethylene terephthalate. 5% by weight of the acid ester. In addition, the mixing method may be that the paper size of the aggregated paper is applicable to the Chinese country; (: f 牟 (CNS) Λ 川:, ½ (210x; ί ;, _ H — ·· 568965. A? • ΙΠ 一 —-__ * II ·. 1-. M, Lailun · ·-• one one • one I-· ^... *,-T • ㈣ ~ · --- V. Description of the invention (13): —ϋ —m I -is:-= I---n I ^ 人. —m -------- ------ -—— (^ lwric: And the note item) Mix to make it fully It can be obtained by transesterification, or more conveniently, it can be reacted in the extruder in the state of tablet blending. This type of method can obtain a sufficiently fast transesterification speed, so that a homogeneous polymer can be obtained. For the polyester constituting the present invention It is important for the production method of the polymer of the fiber to maintain the whiteness of the polymer. When polytrimethylene terephthalate is copolymerized with the third component, it is easy to be colored during polymerization or spinning. Therefore, in addition to the above-mentioned preferred catalyst amount and reaction temperature, the method of improving whiteness is preferably using a thermal stabilizer or a coloring inhibitor. The thermal stabilizer is preferably a 5-valent or 3-valent phosphorus compound. , Such as trimethyl phosphate-, triethyl phosphate, triphenyl phosphate, trimethyl phosphite, triethyl phosphite, triphenyl phosphite, phosphoric acid, phosphorous acid, etc. The addition amount of the polymer is preferably from 0.01 to 0.07% by weight. In addition, examples of the coloration suppression are, for example, cobalt acetate, cobalt formate, etc., and the addition amount of the polymer to the polymer is preferably from 0.01 to 0.07% by weight. In addition, in order to increase the whiteness of the prepolymer during solid-phase polymerization, it is extremely effective to increase the limiting viscosity to above 0.99. The obtained polymer can maintain excellent whiteness even when it becomes a fiber. After this whiteness, b 値 is preferably 2 to 10, and more to 1 to 6. In addition, when using an ester-forming sulfonate compound, special attention should be paid to it. It is easy to form at the spinneret component during the polymerization process. Easily agglomerates and trimethylethylene glycol dimer (structure formula: OCH2CH2CH2〇CH2CH2CH2〇H). If the amount of agglomerates is too large, the pressure in the spinneret component will increase, which will easily cause silk breakage and, In order to prevent this, the exchange frequency of the spun assembly is increased, so it will be reduced by 1. The scale is applicable to the Chinese country; Jujube (CNS) Λchuan: i (210,: ,, € · > -16-568965 V. Description of the invention (14) · I mm In nn — ^ ϋ !! ί 1 ^ i Low production There are problems such as health problems. In addition, if the amount of triethylene glycol dimer is too large, there will be problems such as reducing the thermal stability and light resistance during melting. To prevent such problems, it is better to be at any stage during polymerization. Add some kind of mouthfeel. Examples of such additives are lithium acetate, lithium carbonate, lithium formate, sodium acetate, sodium carbonate, sodium formate, sodium hydroxide, calcium hydroxide, potassium hydroxide and alkaline metal salts. The addition amount of the ester-forming sulfonate compound is preferably from 20 to 400 mol%, and more preferably from 70 to 200 mol%.
、1T 本發明之聚酯纖維的形態可爲長纖維或短纖維,若爲 長纖維時可爲複合絲或單纖絲。其總旦並無特別限制,可 爲5〜lOOOd,若作爲衣料用時又以5〜200d特 別佳。又,單纖絲亦無特別限制,較佳爲〇 · 〇 〇 〇 1〜 1 0 d。另外,剖面形狀可爲圓型,三角型,扁平型,星 型’ W型等’並無特限制,又,可爲中實型或中空型。 經漪部中次徉蜱>«.Jn〈.T.消费合竹社印於 當第3成分爲酯形成性磺酸鹽化合物時,本發明之聚 酯纖維中由動式黏彈性測定求得的損耗正接之峰溫度(以 下略稱爲「Tmax」)爲85〜115。(:,又,第3成 分係選自(1)共聚合比率1 · 5.〜12重量%之碳數4 〜12的脂肪族或脂環式乙二醇,(2)共聚合比率3〜 9重量%之碳數2〜1 4的脂肪族或脂環式二羧酸,或間 苯二酸’ (3)共聚合比率3〜10重量%之聚烷撐二醇 等至少1種時,此峰溫度爲8 5〜1 〇 2°C。其因爲,此 範圍下本發明可確保利用陽離子染料或/及分散染料之常 壓可染性及高堅牢性。又,T m a X能影響非晶部分之分 1、紙張尺度適用中國國家ϋ ( cns Dm叱---------------- 568965 五、發明説明(15 ) 子密度,即,丁 m a X値愈小非晶部分之分子密度愈小, 因此,能增加染料進入之空隙部分而易吸入染料,故可提 高抽空率。但,使用任何一種第3成分且T m a X低於 8 5 °C時,因低溫下分子易移動,故於熱固定性之一般的 後加工或整烫等一般使用階段下會過度增加收縮,而使觸 感變差’或降低染色後布料之乾洗堅牢性。另外,當第3 成分爲酯形成性磺酸鹽化合物且T m a X超過1 1 5 °C時 ,會降低本發明之目的的染色性及,吸入染料之空隙過小 而使常壓下陽離子染料無污染成深色。又,第3成分係選 自(1)共聚合比率1 · 5〜12重量%之碳數4〜12 的脂肪族或脂環式乙二醇,(2 )共聚合比率3〜9重量 %之碳數2〜1 4的脂肪族或脂環式二羧酸,或間苯二酸 ,(3)共聚合比率3〜10重量%的聚烷撐二醇等群中 的至少1種且T m a X超過1 〇 2 °C時,會使吸入染料之 空隙部分過少,而常壓下無法利用分散染料染成深色。 經消部中史栉泠趵巧丁,消资合竹社印製 因此,Tm a X爲纖維之構造因數,故既使擁有相同 之共聚合組成的聚合物,亦會因觸紡絲溫度,防絲速度, 延伸倍率,熱處理溫度,洗淨條件,鹼減量條件,染色條 件等紡絲條件及後加工條件而具有不同値。特別是熱固定 溫度會對此値產生很大變化,因此,重要的是利用熱固定 溫度的變化’使T m a X値位於上述範圍內。至於設定熱 固定的方式有所差異,例如,本發明所規定之聚酯纖維的 情形下,若熱固定溫度爲室溫至1 5 0。(:時T m a X會緩 緩上升,又,超過1 6 0 °C時會明顯下降。因其變化比率 本紙張尺度適用中國國r牦卑(CNS ) Λ( 2丨0,? :Λ \ . Q一 ; 568965 五、發明説明(16 ) 會因共聚合比率而異,故需調查及檢討熱固定溫度與 Tm a X之關係。就本發明而言,若越過1 1 5°C時會減 少染色性改善效果而無常壓可染性。但,過低亦不佳,會 因非晶部分過粗,而有易吸入染料的同時易溢出之缺點。 即,,特別是會降低乾洗堅牢性,濕摩擦堅牢性及洗濯堅牢 性等。另外,會因熱固定時的硬化而有觸感變差及降低尺 寸安定性等問題。較佳之Τ πΓ a X範圍雖會因第3成分之 種類而不同,但,认酯形成性磺酸鹽化合物爲第3成分時 較佳爲9 7〜1 1 2 °C,又,以(1 )共聚合比率1 . 5 〜1 2重量%之碳數4〜1 2的脂肪族或脂環式乙二醇, (2)共聚合比率3〜9重量%之碳數2〜14的脂肪族 或脂環式二羧酸,(3)共聚合比率3〜10重量%之烷 撐二酸中至少1種爲第,3成分時,較佳爲8 5〜1 0 2 °C ,又以9 0〜9 8 °C特別佳。 又,本發明之聚酯纖維的彈性率Q ( g / d )及經 2 0 %伸長後,放置1分鐘的彈性回復率R ( % )需符合 下列式(1 )。其因爲,符合式(1 )時,由本發明之聚 酯纖維而得到的布料會不同於目前之聚酯纖維所得到的布 料,可得到比尼龍更佳之柔軟觸感。 0 · 1 8$Q/R$0 · 4 5 .........式(1 ) 若Q / R > 0 · 4 5時,會因彈性率過高而無法得到 本發明之目的的與尼龍相同之柔軟觸感,或會因彈性回復 木紙張尺度適用中國國家彳·?唪(CNS ) Λ川:仏、(2\0^μ)Ί :、、} ) _ 19- —~ -I II : ......... ....... —1 ϋϋν ϋ li I j人。------ _ *对1間Mu而之注厶爹項ft本h 訂 麵淖部中史枒續而nc Vi消费合社印來 568965 五、發明説明(17 ) *· I i-Ξ- - 111 —II -1 - - - 1 - !1- I I JJy - I- ---- : ------ 1---1--- (^?1間讀$而之^4-^項^功-^本1二 性不足而使一時增加的應力而變形且無法回復原有纖維, 故只能得到形態安定性較差之布料。實質上並不存在Q / R < 0 · 1 8之領域,(因此本發明以0 · 1 8爲Q / R之 下限。另外,式(1 )範圍下的具體彈性率一般爲2 5〜 4 0 g/d‘,彈性回復率爲7 0〜9 9%。 至於由共聚合比率1 . 2^2 · 5克分子%之酯形成 性磺酸鹽化合物與共聚合比率3〜7重量%之(1)碳數 4〜1 2的脂肪族或脂環式乙二醇,(2 )碳數4〜1 2 之脂肪族或脂環式二羧酸,或間苯二酸,(3 )聚烷撐二1T The shape of the polyester fiber of the present invention may be long fiber or short fiber, and if it is a long fiber, it may be a composite fiber or a single fiber. The denier is not particularly limited, but may be 5 to 1,000 d, and particularly preferably 5 to 200 d when used as clothing. The monofilament is not particularly limited, but is preferably 〇 〇 〇 〇 1 to 10 d. In addition, the cross-sectional shape may be round, triangular, flat, star-shaped, 'W-shaped, etc.' and is not particularly limited, and may be a solid or hollow type. The secondary tick in the Jingyi Department> «.Jn <.T. Consumption by Hezhu Co., Ltd. When the third component is an ester-forming sulfonate compound, the polyester fiber of the present invention is determined by dynamic viscoelasticity measurement. The peak temperature of the loss loss (hereinafter referred to as "Tmax") is 85 to 115. (: And the third component is selected from (1) an aliphatic or alicyclic ethylene glycol having a copolymerization ratio of 1 · 5 to 12% by weight and a carbon number of 4 to 12, and (2) a copolymerization ratio of 3 to 9% by weight of aliphatic or alicyclic dicarboxylic acids having 2 to 14 carbon atoms, or isophthalic acid '(3) at least one type of polyalkylene glycol having a copolymerization ratio of 3 to 10% by weight, This peak temperature is 8 5 ~ 10 ° C. Because the present invention can ensure the normal pressure dyeability and high fastness of cationic dyes and / or disperse dyes in this range. In addition, T ma X can affect non- Crystal fractions 1. The paper size is applicable to the Chinese national standard (cns Dm 叱 ---------------- 568965 V. Description of the invention (15) Sub-density, that is, Ding Ma X 値 越The smaller the molecular density of the small amorphous part, therefore, it can increase the void portion where the dye enters and easily inhale the dye, so the evacuation rate can be increased. However, when using any of the third components and T ma X is lower than 8 5 ° C Because the molecules are easy to move at low temperature, it will increase the shrinkage excessively during the general use process such as general post-processing or ironing, which will make the touch worse, or reduce the fabric after dyeing. The dry-cleaning fastness. In addition, when the third component is an ester-forming sulfonate compound and T ma X exceeds 1 15 ° C, the dyeability of the object of the present invention will be reduced, and the void of the inhaled dye will be too small to make the The cationic dye is darkened without contamination. The third component is selected from (1) an aliphatic or alicyclic ethylene glycol having a carbon number of 4 to 12 with a copolymerization ratio of 1.5 to 12% by weight, (2 ) A copolymerization ratio of 3 to 9% by weight of an aliphatic or alicyclic dicarboxylic acid having a carbon number of 2 to 14 or an isophthalic acid, (3) a copolymerization ratio of 3 to 10% by weight of a polyalkylene glycol When at least one of the isogroups and T ma X exceeds 102 ° C, the void portion of the inhaled dye will be too small, and the disperse dye cannot be used to dye dark colors at normal pressure. D, printed by Xiaozi Hezhu Co., Ltd. Therefore, Tm a X is the structural factor of the fiber, so even if the polymer has the same copolymer composition, it will also be affected by the spinning temperature, anti-filament speed, elongation ratio, heat treatment temperature , Washing conditions, alkali reduction conditions, dyeing conditions and other spinning conditions and post-processing conditions have different characteristics. Especially heat The fixed temperature will cause a large change in this temperature. Therefore, it is important to use the change of the thermal fixation temperature to make T ma X 値 fall within the above range. As for the method of setting the thermal fixation, there are differences, for example, according to the present invention. In the case of polyester fibers, if the heat-fixing temperature is from room temperature to 150 °. (: T ma X will slowly rise, and it will drop significantly when it exceeds 160 ° C. Because of the change ratio of this paper scale Applicable to China's national standard (CNS) Λ (2 丨 0 ,?: Λ \. Q 一; 568965 V. Description of invention (16) will vary depending on the copolymerization ratio, so it is necessary to investigate and review the heat-fixing temperature and Tm a The relationship of X. In the present invention, when the temperature is over 115 ° C, the dyeing improvement effect is reduced without the normal-pressure dyeability. However, if it is too low, it is not good. Because the amorphous part is too thick, it has the disadvantages that it is easy to inhale the dye and easy to overflow. That is, in particular, the fastness to dry cleaning, the fastness to wet rubbing, and the fastness to washing are reduced. In addition, there are problems such as deterioration in touch feeling and reduction in size stability due to hardening during heat fixing. Although the preferred range of τ πΓ a X varies depending on the type of the third component, it is preferably 9 7 to 1 1 2 ° C when the ester-forming sulfonate compound is recognized as the third component, and (1 ) Copolymerization ratio 1.5 to 12 2% by weight of aliphatic or alicyclic ethylene glycol with 2 to 4 carbon atoms, (2) Copolymerization ratio 3 to 9% by weight of 2 to 14 aliphatic carbons with carbon number Or alicyclic dicarboxylic acid, (3) at least one of the alkylene diacids having a copolymerization ratio of 3 to 10% by weight is the first, and when the third component is, preferably 8 5 to 10 2 ° C, and 9 0 ~ 9 8 ° C is particularly good. In addition, the elastic modulus Q (g / d) of the polyester fiber of the present invention and the elastic recovery rate R (%) after being left to stand for one minute after 20% elongation need to conform to the following formula (1). This is because, when the formula (1) is satisfied, the cloth obtained from the polyester fiber of the present invention is different from the cloth obtained from the current polyester fiber, and a softer touch than nylon can be obtained. 0 · 1 8 $ Q / R $ 0 · 4 5 ......... Formula (1) If Q / R > 0 · 4 5, the object of the present invention cannot be obtained because the elasticity is too high. It has the same soft touch as nylon, or it may apply to the Chinese country due to the elastic recovery of wood paper. 尺度 ·? 唪 (CNS) Λ 川: 仏, (2 \ 0 ^ μ) Ί: ,,}) _ 19- — ~ -I II: ......... ....... —1 ϋϋν ϋ li I j people. ------ _ * Note to 1 Mu 厶 项 ft ft 本 淖 淖 h 桠 桠 桠 桠 桠 桠 桠 桠 桠 桠 桠 and nc Vi Consumer Co., Ltd. printed 568965 V. Description of the invention (17) * · I i- Ξ--111 —II -1---1-! 1- II JJy-I- ----: ------ 1 --- 1 --- (^? Read $ while 1 ^ 4- ^ Term ^ Work- ^ The lack of duality causes the temporary increase in stress and deformation and cannot restore the original fiber, so only fabrics with poor morphological stability can be obtained. In essence, there is no Q / R < 0 · In the field of 18, (so the present invention takes 0 · 18 as the lower limit of Q / R. In addition, the specific elastic modulus in the range of formula (1) is generally 2 5 ~ 40 g / d ', and the elastic recovery rate is 70 to 9 9%. As for the copolymerization ratio of 1.2 ^ 2 · 5 mol% of the ester-forming sulfonate compound and the copolymerization ratio of 3 to 7% by weight (1) the number of carbons is 4 to 12 Aliphatic or alicyclic ethylene glycol, (2) aliphatic or alicyclic dicarboxylic acid having 4 to 12 carbon atoms, or isophthalic acid, (3) polyalkylene diene
S 醇中所選出的至少一種共聚合而成之聚三甲撐對苯二甲酸 酯纖維,其纖維之T m a X亦需爲8 5〜1 1 5 °C,且其 彈性率Q ( g / d )及彈性回復率R ( % )之關係亦需符 合式1,其理由同上述之Tmax與式(1)。 本發明之聚酯纖維可利用下列方法而製得。 即,本發明之聚酯纖維可由,利用擠押機等使乾燥至 水分量至少爲1 0 0 p pm以下,又以5 0 P pm以下爲 任;^聚合物熔融後「由紡口擠押出熔融之聚合物並捲取, 其次進行延伸而得到。又,此捲取後的延伸係指,紡絲後 以捲絲管等捲取,再利用其他裝置對此絲進行延伸,即, 可利用一般方法,或使擠出於紡口之聚合物完全冷卻固化 後,以具有一定回轉速度之第一滾軸分數次捲取,於滾軸 前後完全沒有張力之情形下,利用第一滾軸與設置於第一 滾軸後方的第二滾軸間進行延伸之紡絲與延伸過程直接結 合的直延法。 木紙張尺度適用中國國I#導(CNS )· Λ找ΊΜ 210 ) . _ 2〇7 … 568965 五、發明説明(μ ) 下面將舉例說明一般方法。 本發明之使聚合物熔融紡絲時的紡絲溫度爲2 4 0〜 320 °c,又以240〜300 °C爲佳,更佳爲240〜 2 8 〇 °C。若紡絲溫度低於2 4 0 t時,會因溫度過低而 難有安定的熔融狀態,而會增大所得纖維之斑,或無法得 到合適的強度及延伸度。又,紡絲溫度超過3 2 0 °C時, 會使熱分解變得激烈,而使所得絲著色,或無法得到合適 的強度及延伸度。 絲的捲取速度並無特別限制,但一般爲3 5 0 〇 m / mi η,又以2500m/mi η以下爲佳,更佳爲 2 0 〇 〇 m、/ m i η。若捲取速度超過3 5 0 0m/ m i η時,會使捲取前過度結晶化而無法提升延伸過程之 延伸倍率,因此無法使分子定向而無法得到充分的強度或 彈性回復率及,因捲得太緊而無法由捲絲管等捲取機取下 。又,延伸時之延伸倍率爲2〜4倍,又以2 . 2〜 經滅部中史桴冷而负.τ-消费合竹社印¥ >- I— ml — ? ..... I..... -- I . Jv、1--1 -- =-- 1-- ---, -.1 : 爿刁 、-0 3 · 7倍爲佳’更佳爲2 · 5〜3 · 5倍。若延伸倍率低 於2倍時,利用延伸方式將無法使聚合物充分定向,而降 低所得絲之彈性回復率,故無法符合式(1 )。又,超過 4倍時,會產生激烈的斷絲情形,故無法安定地延伸。 延伸時的溫度就延伸層而言爲3 0〜8 0 °C,又以 3 5〜7 0 t:爲佳,更佳爲4 0〜6 5 °C。若延伸層之溫 度低於3 0 °C時,延伸時易產生斷絲,而無法連續得到纖 維。又,超過8 0 °C時會因延伸滾軸等加熱層而使纖維之 滑動性變差,故易發生單絲斷裂而成爲起絨毛的絲。另外 本紙张尺度適用中^國家ί’?率(CNS ) Λ從ί 568965 五、發明説明(19 ) ,會因聚合物流失而無法充分定向,故會降低彈性回復率 0 又,爲了避免纖維構造的經時變化’延伸後需進行熱 處理。此熱處理溫度爲9 0〜2 (To °c,又以1 0 0〜The polytrimethylene terephthalate fiber obtained by copolymerizing at least one selected from S alcohol, the T ma X of the fiber also needs to be 8 5 ~ 1 1 5 ° C, and the elastic modulus Q (g / The relationship between d) and the elastic recovery rate R (%) must also conform to Formula 1, for the same reason as the above Tmax and Formula (1). The polyester fiber of the present invention can be produced by the following method. That is, the polyester fiber of the present invention can be dried by using an extruder or the like to a moisture content of at least 100 p pm or less, and 50 p pm or less; ^ After the polymer is melted, "extrude from the spinning mouth The melted polymer is taken up and taken up, followed by drawing. In addition, the taken-out drawing refers to taking up a take-up tube or the like after spinning, and then using another device to draw the filament, that is, it can be used. The general method, or after the polymer extruded on the spinning mouth is completely cooled and solidified, it is wound up in several times on a first roller with a certain rotation speed. In the case where there is no tension at the front and back of the roller, the first roller and the A direct drawing method in which the spinning and extension processes are directly combined between the second rollers located behind the first rollers. The wood and paper standards are applicable to China's I # guide (CNS) · ΛFindΊΜ 210). _ 2〇 7… 568965 V. Description of the invention (μ) The general method will be described below by way of example. In the present invention, the spinning temperature of the polymer when it is melt-spun is 2 0 0 to 320 ° C, and preferably 240 to 300 ° C. More preferably, it is 240 to 280 ° C. If the spinning temperature is lower than 240 tons, Because the temperature is too low, it is difficult to have a stable molten state, which will increase the plaque of the obtained fiber, or fail to obtain appropriate strength and elongation. When the spinning temperature exceeds 3 2 0 ° C, it will cause thermal decomposition. It is intense, and the obtained silk is colored, or appropriate strength and elongation cannot be obtained. The winding speed of the silk is not particularly limited, but it is generally 3 500 m / mi η, and preferably 2500 m / mi η or less. More preferably, it is 2000 m, / mi η. If the winding speed exceeds 3 500 m / mi η, it will cause excessive crystallization before coiling and cannot increase the stretching ratio of the stretching process, so the molecules cannot be oriented and Unable to obtain sufficient strength or elastic recovery rate, and because it is too tight to be taken off by a reel such as a coiler. Also, the stretching ratio during stretching is 2 to 4 times, and 2.2 to 2 The history of the ministry is cold and negative. Τ-Consumer Hezhusha Seal ¥ >-I— ml —? ..... I .....-I. Jv, 1--1-=- 1-- ---, -.1: Diao Diao, -0 3 · 7 times is better, more preferably 2 · 5 ~ 3 · 5 times. If the extension ratio is less than 2 times, the extension method cannot be used. Fully oriented polymer , And reduce the elastic recovery rate of the obtained yarn, so it can not meet the formula (1). Moreover, when it exceeds 4 times, a fierce broken wire situation will occur, so it cannot be stretched stably. The temperature during stretching is 3 for the stretched layer. 0 ~ 8 0 ° C, and then 3 5 ~ 7 0 t: better, more preferably 40 ~ 6 5 ° C. If the temperature of the extension layer is lower than 30 ° C, wire breakage is easy to occur during extension, It is impossible to continuously obtain fibers. When the temperature exceeds 80 ° C, the sliding properties of the fibers are deteriorated due to the stretching of the heating layer such as a roller. Therefore, the filaments are easily broken and become fluffed filaments. In addition, this paper is applicable to the national country's rate (CNS) Λ ί 568965 V. Description of the invention (19), it will not be fully oriented due to polymer loss, so it will reduce the elastic recovery rate. Also, in order to avoid fiber structure The change over time requires heat treatment after elongation. The heat treatment temperature is 9 0 ~ 2 (To ° c, and then 1 0 0 ~
I 1 9 0 °C爲佳,更佳爲1 1 0〜1 1 8 °C。若熱處理溫度 低於9 0 °C時,纖維將無法充分的結晶化,而使彈性回復 性變差。若溫度高於2 0 0 °C時’會因切斷熱處理層而無 法延伸。 - 訂 經滅部中次標贽合竹社印來 下面將奉例說明直延法。即,利用通過設於紡口下方 之環境溫度保持爲3 0〜2 0〇°C之長2〜8 0 cm的保 溫領域,抑制由紡口擠出之熔融複合絲產生激烈冷卻後’ 使此熔融複合絲急冷以變成固體複合絲,再以加熱至4 0 〜70°C之回轉速度3 0 0〜3 0 0 Om/m i η的第一 滾軸捲附,並利用第一滾軸與速度比第一滾軸更快之第二 滾軸間進行1 · 5〜3倍延伸,其後以速度比第二滾軸慢 之捲取機捲取。又,必要時可於紡絲過程進行混染處理。 另外,亦可先以3 0 0〜.3 0 〇 〇 m / m i η的紡絲速度 學取未延伸後,再通過前述之第一滾軸·,第二滾軸而捲取 〇 . 同一般方法又以進行聚合物之熔融擠出後’不可直接 於紡口使擠出之熔融複合絲急冷,而需使其通過設置於紡 口下方之環境溫度保持爲3 0〜2 0 0°C的長2〜 8 0 c m之保溫領域,以抑制激烈冷卻後’再將此熔融複 合絲經急冷後所得固體複合絲供應給延伸步·驟爲佳。通過 ------ __ - - - „ I, I , · - - ----- -- •…一 II. 一一 一-一,- 本紙張尺度適用中國國家代率(CNS ) Λ川:½ ( 210〆?W、- 22 - 568965 五、發明説明(2〇 ) 此保溫領域之目的爲,抑制因急冷而使聚合物生成微細結 晶或極度定向之非晶部分,而易於延伸步驟製得延伸之非 晶構造,故本發明可完成必要的纖維物性’。因聚三甲撐對 苯二甲酸酯具有比,例如聚乙撐對苯二甲酸酯與聚酯更快 速的結晶化速度,故對抑制微細結晶或極度定同之非晶部 分的生成而言,此類的緩慢冷卻不失爲極有效之方法。若 低於3 0°C時,會因急冷而不易提升延伸倍率。又’高於 2 0 0 °C時易造成斷絲。此保溫領域之溫度又以4 0〜 2 0 0 °C爲佳·,更佳爲5 0〜1 5 0 °C。另外,保溫領域 之長度又以5〜3 0 c m爲佳。對絲之紡絲速度而言’第 一滾軸之捲附速度爲300〜3000m/mi η。若紡 絲速度低於3 0 0 m / m i η時,雖具有優良之紡絲安定 性,但,今明顯降低生產性。又,超過3 0 0 0 m / m i η時,會增加捲取前的非晶部之定向或部分結晶化, 而無法使延伸步驟提升延伸倍率,因此,分子無法定向而 不易得到充分的絲強度。此速度又以1 5 0 0〜2 7 0 0 m / m i η爲佳。 因需使纖維之非晶部分進行緩和定向,故捲取機之速 度比第一滾軸低,因此,可減少聚甲撐對苯二甲酸酯纖維 進行大收縮,又,因非晶部分鬆弛而成爲易吸收染料之構 造,故可提升染色性。另外無張力比(捲取速度/第二滾 軸速度)爲0 · 95〜0 . 99,又以0 · 95〜 0 . 9 8爲佳。 依據延伸倍率而決定的第二滾軸之速度一般爲6 0 0 本紙张尺度適用中國國家朽卑(CNS ) Λ4丨丨:仏(2K)x2V·?:、,# )' ~ ο^Γ — …— 568965 五、發明説明(21 ) · 6 0 Q 〇 m /m i η。又,第一滾軸與第二滾軸間的延 伸倍率爲1 · 3〜3倍又以2〜2 · 7倍爲佳。若延伸倍 率低於1 · 3倍時,將無法利用延伸而使聚合物充分定向 ’因此’會降低所得纖維之強度或彈性回復率。又,超過 3倍時,會快速起毛,而無法安定地進行延伸。第一滾軸 之溫度爲4 0〜7 0 °C,其因爲,此溫度範圍下易於延伸 。其中又以5 0〜6 0°C爲佳。第二滾軸之目的爲進行熱 固疋’因此將溫度設定爲1 2 0〜1 6 0。(:。若溫度低於 1 2 0 °c時,會缺乏熱固定性而易成爲熱變形,經時變化 之纖維及降低顯色性。又,超過1 6 0 °C時,會造成起毛 或斷絲情形,因此無法安定地進行紡絲。其中又以1 2 〇 〜1 5 0 °C爲佳。 爲了使所得纖維具有充分的均質性及品質,最重要的 係適用上述一般法及直延法所示的較佳條件。又,評估此 適用較佳之紡絲條件而得到的纖維品質之參數,例如可爲 u %。U %爲,表示纖維剖面之均質性的參數,而適用上 述較佳條件下所得之U %可爲2 · 5 %以下,又,依場合 可達1.5%以下。 單獨使用上述所得聚酯纖維’或以其爲布料之部分材 料時,可得到具有優良之柔軟性,伸縮性及顯色性的布料 。又,作爲布料之部材時,所使用的其他纖維並無特別限 制,但特別是混用,聚尿烷彈性纖維所代表之伸縮纖維, 纖維素纖維,羊毛,絲綢,乙酸鹽時,可得到使用尼龍纖 維或聚乙撐對苯二甲酸酯纖維之混用布料所未曾具有的特 本紙張尺度適用中國國家梢準(CNS )八川:仏(210/ ) 〇Τ一 568965 五、發明説明(22 ) ' 徵°即’可得到常壓下可利用例如陽離子及/或分散染料 進行染色,以及具有目前所沒有之柔軟,伸縮性等獨特質 感的布料。 特別是具有,能利用陽離子或分散染料中任何一種或 者雙方染料使本發明之聚酯纖維染成深色的特性之範圍下 1 ’就不污承聚尿烷彈性纖維而可進行染色及,具有不同於 混用尼龍纖維與聚尿烷彈性纖維所代表之伸縮纖維的布料 之柔軟性或觸感觀點,又以例如混用此聚三甲撐對苯二甲 酸酯纖維與聚尿烷彈性.纖維所代表之伸縮纖維的布料特別 佳。 本發明之布料,即包含上述混用布,料,其形態,製編 織方法並無特別限制,可利用已知之方法製得。例如,利 用本發明之聚酯纖維爲經絲或緯絲的平編物,雙面編物等 編物’或針織,棉經等編物等,又,可進行交撚,合絲或 混染。 本發明所使用的伸縮纖維並無特別限制,其例如,經 乾式紡絲或熔融紡絲之聚尿烷彈性纖維,或者聚丁撐對苯 二甲酸酯纖維,聚四甲二醇共聚合之聚丁撐對苯二甲酸酯 纖維所代表的聚酯系彈性纖維等。至於使用伸縮纖維之混 用布料中的本發明之聚酯纖維的含有率並無特別限制,較 佳爲60〜98%。 本發明之布料亦包含混用布料,例如經一般法的洗淨 ,組裝,染色,最後固定等過程後仍可進行染色。另外, 必要時於洗淨後,染色前可進行鹼減量處理。I 1 9 0 ° C is preferable, and more preferably 1 1 0 to 1 1 8 ° C. If the heat treatment temperature is lower than 90 ° C, the fibers will not be sufficiently crystallized and the elastic recovery will be deteriorated. If the temperature is higher than 200 ° C, it will not be stretched by cutting off the heat-treated layer. -Ordered by the Ministry of Education's secondary bid, printed by the Hezhu Club. The straightforward method will be explained below by way of example. In other words, the use of a thermal insulation field with a length of 2 to 80 cm maintained at an ambient temperature of 30 to 200 ° C below the spinning orifice is used to suppress intense cooling of the molten composite yarn extruded from the spinning orifice. The molten composite yarn is rapidly cooled to become a solid composite yarn, and then wound up with a first roller heated at a rotation speed of 3 0 0 to 3 0 0 Om / mi η, and using the first roller and speed The second roller, which is faster than the first roller, is stretched 1 to 5 to 3 times, and then wound up by a coiler that is slower than the second roller. In addition, if necessary, mixed dyeing treatment can be performed in the spinning process. In addition, it is also possible to take unstretched at a spinning speed of 3 0 ~~ 3 0 〇〇〇〇〇m / mi η, and then take up by the first roller ·, the second roller described above. In the method, after the polymer is melt extruded, the extruded molten composite yarn cannot be quenched directly at the spinning mouth, but it needs to be maintained at 30 ~ 2 0 ° C through the ambient temperature set below the spinning mouth. In the thermal insulation field with a length of 2 to 80 cm, it is better to supply the solid composite yarn obtained by quenching the molten composite yarn to the elongation step after the rapid cooling. Pass ------ __---„I, I, ·--------•… II. One one one one-one,-This paper size applies to China National Generation Rate (CNS) Λ Chuan: ½ (210〆? W,-22-568965 V. Description of the invention (20) The purpose of this thermal insulation field is to suppress the formation of fine crystals or extremely oriented amorphous parts of the polymer due to rapid cooling, and it is easy to extend the step. An extended amorphous structure is obtained, so the present invention can complete the necessary fiber properties. Because polytrimethylene terephthalate has a faster crystallization than, for example, polyethylene terephthalate and polyester Speed, so slow cooling is an extremely effective method for suppressing the formation of fine crystals or extremely uniform amorphous parts. If it is lower than 30 ° C, it will be difficult to increase the extension ratio due to rapid cooling. It is also easy to cause wire breakage when it is higher than 200 ° C. The temperature in this insulation field is preferably 40 ~ 200 ° C, and more preferably 50 ~ 150 ° C. In addition, the insulation The length of the field is preferably 5 ~ 30 cm. For the spinning speed of silk, the winding speed of the first roller is 300 ~ 3000m / mi η. If the spinning speed is low At 300 m / mi η, although it has excellent spinning stability, the productivity is significantly reduced today. When it exceeds 300 m / mi η, the amount of amorphous part before winding is increased. Orientation or partial crystallization, which cannot increase the stretching ratio in the stretching step, therefore, the molecules cannot be oriented and it is not easy to obtain sufficient silk strength. This speed is again preferably 1 500 to 2700 m / mi η. The amorphous part of the fiber is gently oriented, so the speed of the winder is lower than that of the first roller. Therefore, it can reduce the large shrinkage of the polyethylene terephthalate fiber. The structure is easy to absorb the dye, so it can improve the dyeability. In addition, the tension-free ratio (winding speed / second roller speed) is 0. 95 ~ 0.99, and 0. 95 ~ 0.98 is better. The speed of the second roller, which is determined by the stretching magnification, is generally 6 0 0 This paper size is applicable to the Chinese National Decline (CNS) Λ4 丨 丨: 仏 (2K) x2V ·?: ,, #) '~ ο ^ Γ —… — 568965 V. Explanation of the invention (21) · 60 Q 〇m / mi η. Also, the extension ratio between the first roller and the second roller 1 · 3 ~ 3 times and 2 ~ 2 · 7 times are better. If the stretching ratio is lower than 1.3 times, the polymer cannot be fully oriented by stretching. Therefore, the strength or elastic recovery of the obtained fiber will be reduced. When it exceeds 3 times, it will raise hair quickly and cannot stretch stably. The temperature of the first roller is 40 ~ 70 ° C, because it is easy to stretch in this temperature range. Among them, 50 ° to 60 ° C is preferred. The purpose of the second roller is to perform thermosetting, so the temperature is set to 120 to 160. (:. If the temperature is lower than 120 ° C, it will lack heat fixability and will easily become thermally deformed, change the fiber over time and reduce the color rendering. When it exceeds 160 ° C, it will cause fluff or In the case of broken yarns, spinning cannot be performed stably. Among them, 120 ° C to 150 ° C is preferred. In order to obtain sufficient homogeneity and quality of the obtained fiber, the above-mentioned general method and straightening are most importantly applied. The best conditions shown in the method. In addition, the parameters of the fiber quality obtained by evaluating the applicable spinning conditions can be, for example, u%. U% is a parameter representing the homogeneity of the fiber cross section, and the above-mentioned better are applicable. The U% obtained under the conditions may be less than 2.5%, and may be less than 1.5% depending on the occasion. When the polyester fiber obtained above is used alone or as a part of the material of the cloth, excellent softness can be obtained. Stretchy and color-producing cloth. There are no particular restrictions on other fibers used as the material of the cloth, but it is especially mixed and used as the elastic fiber represented by polyurethane elastic fiber, cellulose fiber, wool, and silk. , Acetate, can To the special paper size that nylon or polyethylene terephthalate fiber mixed cloth has not possessed, it is applicable to China National Standards (CNS) Yagawa: 仏 (210 /) 〇Τ 一 568965 Ⅴ Description of the invention ( 22) 'Characterization' means that fabrics can be dyed under normal pressure using, for example, cationic and / or disperse dyes, and have unique textures such as softness, stretchability, etc. that are not currently available. Especially, cationic or disperse dyes can be used Any one or both of the dyes make the polyester fiber of the present invention in a range of dark characteristics. 1 ', it can stain the polyurethane elastic fiber without staining, and it has elasticity different from that of nylon fiber and polyurethane. From the viewpoint of softness and touch of the fabric of the stretchable fiber represented by the fiber, for example, the use of the polytrimethylene terephthalate fiber and polyurethane elasticity is mixed. The cloth of the stretchable fiber represented by the fiber is particularly preferable. The cloth, which includes the above-mentioned mixed cloth, material, its form, and knitting method is not particularly limited, and can be produced by a known method. For example, using the polymer of the present invention The fibers are warp or weft knitted fabrics, double knitted fabrics and other knitted fabrics, knitted fabrics, cotton warp knitted fabrics, etc., and can be twisted, plied or mixed. The stretchable fiber used in the present invention is not particularly limited. , For example, dry-spun or melt-spun polyurethane elastic fibers, or polybutylene terephthalate fibers, polytetramethylene glycol copolymerized polybutylene terephthalate fibers Representative polyester-based elastic fibers, etc. As for the content of the polyester fiber of the present invention in a mixed cloth using stretchable fibers, there is no particular limitation, and it is preferably 60 to 98%. The cloth of the present invention also includes a mixed cloth, such as After general washing, assembly, dyeing, and final fixing, dyeing can still be performed. In addition, after washing, if necessary, alkali reduction treatment can be performed before dyeing.
本纸ί長尺度適用中國國家代準(CNS ) Λ川:仏() ^ ocT 568965 五、發明説明(23 ) 進行洗淨之溫度可爲4 0〜9 8 °C。特別是混用伸縮 纖維’最好能於無張力的同時進行洗淨,如此一來可提昇 彈性。 染色前後的熱固定是可省略一部分或兩方均省略,但 ’就提升布料之形態安定性,染色性觀點,又以進行兩方 爲佳。熱固定之溫度爲120〜190 °C,又以140〜 1 8 0 °C爲佳,熱固定之時間爲1 0秒〜5分鐘,又以 2 0秒〜3分鐘爲佳。 染色時無需載液,進行之溫度爲7 0〜1 .5 0°C,又 以9 0〜1 2 0 °C爲佳,特別佳爲9 0〜,1 0 0 °C。爲了 使染色均質化,可利用乙酸或氫氧化鈉等調整染料之p Η ,同時又以使用由表面活性劑所構成之分散劑而特別佳。 另外,使用陽離子染料時;爲了提升染色物之鮮明度,又 以將硫酸鈉,硝酸鈉,硫酸鉀,硫酸鈣等鹼金屬或鹼土類 金屬加入染浴中特別佳。 經沪部中史枰冷^Μ.τ.消贽合β社印¥The long scale of this paper is applicable to China National Standards (CNS) Λchuan: 仏 () ^ ocT 568965 V. Description of the invention (23) The temperature for cleaning can be 40 ~ 98 ° C. In particular, it is preferable that the mixed stretchable fiber 'can be washed without tension, so that the elasticity can be improved. The heat fixation before and after the dyeing can be omitted for a part or both, but it is better to perform the two methods from the viewpoint of improving the cloth's form stability and dyeability. The temperature for thermal fixation is 120 ~ 190 ° C, and preferably 140 ~ 180 ° C. The time for thermal fixation is 10 seconds to 5 minutes, and preferably 20 seconds to 3 minutes. No carrier liquid is required for dyeing, and the temperature is 70 ~ 1.5 ° C, and 90 ~ 120 ° C is preferred, especially 90 ~ 100 ° C. In order to homogenize the dyeing, it is possible to adjust the p Η of the dye by using acetic acid or sodium hydroxide, and it is particularly preferable to use a dispersant composed of a surfactant. In addition, when using a cationic dye, in order to improve the sharpness of the dyed matter, it is particularly preferable to add an alkali metal or alkaline earth metal such as sodium sulfate, sodium nitrate, potassium sulfate, calcium sulfate to the dyeing bath. By Shanghai Department of Chinese History 枰 冷 ^ Μ.τ. 消. 合 β 社 印 ¥
In —I— 1 - = I -I- - - - I - - I 1 - --: II— I Is ----——1 TJ -" (¾^間¾%¾之>.|&小項朽^寫本 n ) 染色後可利用已知之方法進行皂洗或還原洗淨。特別 是混用伸縮纖維之情形下,就能去除污染聚尿烷彈性纖維 之分散染料而提升布料的堅牢性觀點,重要的係於對常壓 分散染料’可染性纖維及聚尿烷彈性纖維所形成之混用布料 進行染色時,進行還原性纖維洗淨。其方法可爲已知之方 法,例如於磺酸鈉或氫氧化鈉等鹼性水溶液中,利用氫化 硫化鈉等還原劑進行處理。 下面爲,常壓下能利用陽離子染料,分散染料中任何 一種或雙方染料染成深色之本發明的聚三甲撐對苯二甲酸 I ·__ _ — - ―一一 1 ' —一 ·*" " · ^ JT-* J U · - 1· ~ r … Β *-π ' - *** · ""****—— 木紙张尺度適用中國國家C準(CNS ) ) - 26 - 568965 五、發明説明(24 ) 酯系纖維的使用形態之例子。 (1 )混用本發明之聚三甲撐對苯二甲酸酯系纖維與 聚尿烷彈性纖維所代表之伸縮纖維,羊毛,絲綢,乙酸鹽 等耐熱性較低之纖維時,可於不損耐熱性較低之纖維的性 能下’於常壓下染成深色。特別是混用聚三甲撐對苯二甲 酸酯系纖維與聚尿烷彈性纖維時,可創作出具有不同於混 用尼龍纖維之布料的柔軟性及觸感,並兼具易攜特性之新 感覺的衣料。 經滅部中史桴冷^nc.t.消资合竹社印鉍 (2 ) —般的聚三甲撐對苯二甲酸酯纖維與聚尿烷彈 性纖維之混用布料需於1 1 〇〜1 2 〇 °c下進行染色,因 此會使聚尿烷彈性纖維產生熱劣化,且只能以分散染料進 行染色。又,利用分散染料對混用聚尿烷彈性纖維之布料 進行染色時,聚尿烷彈性纖維所吸取的分散染料會比聚三 甲撐對苯二甲酸酯纖維多,且無法牢固地固著於聚尿烷彈 性纖維。例如,乾洗或洗濯下,易造成纖維分散染料移除 而污染周邊衣料,或造成染料脫離而使混用布料退色之降 低染色性堅固性情形。但,使用常壓下能利用陽離子染料 ,分散染料中任何一種或兩方染料染成深色的本發明之聚 三甲撐對苯二甲酸酯纖維時,可解決前述問題。 即,第一種方法爲,使用本發明之常壓陽離子染料可 染的聚三甲撐對苯二甲酸酯。 聚尿烷彈性纖維無法以陽離子染料進行染色。但,使 用常壓下能利用陽離子染料進行染色之聚三甲撐對苯二甲 酸酯纖維時,會選擇性僅對聚三甲撐對苯二甲酸酯系纖維 木紙张尺度適用中國國家I?牟(CNS ) Λ.,1丨⑽(TTo aoV/ :,、n ) 1 〇7T~ 568965 五、發明説明(25 ) 進行染色,故不會有上述問題。 第二種的方法爲,使用本發明之常壓分散染料可染的 聚三甲撐對苯二甲酸酯纖維。其因爲,可將聚三甲撐對苯 二甲酸酯系纖維改質爲具有常壓分散染料可染性,故能抑 制分散染料移行到聚尿烷彈性纖維上。 (3 )混用聚尿烷彈性纖維所代表之伸縮纖維的一例 爲’具強勒性之褲襪。但,此業界缺少專門染色工場中進 行一般高壓染色時m必備的高壓染色釜。而使用本發明之 常壓陽離子染料可染性或常壓分散染料可染性之聚三甲撐 對苯二甲酸酯纖維時,具有無需增加新設備之,可直接轉 用尼龍纖維交編褲襪所使用的常壓染色釜之設備上的優點 。又’此設備上的優點對工業上具有極重要之效果。 經y部中史(?次^,-"〈^-消贽合0社印¥ 11— I ........ i -- - I - - f ! j I (¾而之:λτΛΦ項本 D ) (4 )使用本發明之聚三甲撐對苯二甲酸酯系纖維而 得到的布料,例如能具有比目前混用尼龍纖維及聚尿烷彈 性纖維之布料更柔軟之觸感及無尼龍纖維特有的僵硬感。 另外’具有輕伸縮性及優良顯色性,因此可得到一種具有 新感覺的衣料。又,聚三甲撐對苯二甲酸酯系纖維具有較 高的熱固定性及優良耐變黃性。因這些特性不會造成尼龍 纖維特有之問題,故可得到處理性優良之衣料。’ (5 )混用本發明之聚酯纖維與纖維素纖g時,亦具 有卓越成效。·其因爲,使用反應染料對纖維素纖維進行染 色時’右染浴溫度超過1 0 0 C時易造成反應染料分解。 而使用本發明之聚三甲撐對苯二甲酸酯系纖維時,常壓下 可利用陽離子染料或分散染料,反應染料進行一段一浴染In —I— 1-= I -I-----I--I 1--:: II— I Is ----—— 1 TJ-" (¾ ^ 间 ¾% ¾ 之 >. | & Small item ^ Manuscript n) After dyeing, soaping or reduction washing can be performed by known methods. In particular, the use of stretchable fibers can remove the disperse dye that contaminates polyurethane elastic fibers and improve the fastness of the cloth. The important point is that the atmospheric pressure disperse dyes can be dyed and polyurethane elastic fibers. When the formed mixed cloth is dyed, the reducing fibers are washed. The method may be a known method, for example, treatment with a reducing agent such as sodium hydride in an alkaline aqueous solution such as sodium sulfonate or sodium hydroxide. The following is a polytrimethylene terephthalate of the present invention that can be dyed to a dark color by using cationic dyes, disperse dyes, or both of them under normal pressure. I · __ _ —-— —One 1 1 — — * " " ^ JT- * JU ·-1 · ~ r… Β * -π '-*** · " " **** —— The standard of wood and paper is applicable to China National Standard (CNS))- 26-568965 V. Description of the Invention (24) An example of the use form of ester fiber. (1) When the polytrimethylene terephthalate-based fibers of the present invention are mixed with the elastic fibers represented by polyurethane elastic fibers, wool, silk, acetate and other heat-resistant fibers, the heat resistance is not impaired. Low-performing fibers are dyed dark at atmospheric pressure. Especially when polytrimethylene terephthalate fiber and polyurethane elastic fiber are mixed, it can create a new feeling that has softness and touch different from the fabric mixed with nylon fiber and has easy portability. Lining. Shi Jie Leng from the Ministry of Economic Affairs ^ nc.t. Consumer Bismuth Co., Ltd. printed bismuth (2)-General trimethyl terephthalate fiber and polyurethane elastic fiber mixed cloth needs to be 1 1 〇 ~ Dyeing at 120 ° C will cause thermal degradation of polyurethane elastic fibers and can only be dyed with disperse dyes. In addition, when disperse dyes are used to dye fabrics mixed with polyurethane elastic fibers, polyurethane elastic fibers can absorb more disperse dyes than polytrimethylene terephthalate fibers and cannot be firmly fixed to the polymer. Urethane elastic fiber. For example, under dry cleaning or washing, it is easy to cause the fiber disperse dyes to be removed and contaminate the surrounding clothing, or to cause the dyes to detach, which will cause the mixed fabrics to fade and reduce the strongness of dyeing. However, when the polytrimethylene terephthalate fiber of the present invention can be dyed to a dark color using cationic dyes, disperse dyes, or both dyes under normal pressure, the aforementioned problems can be solved. That is, the first method is a polytrimethylene terephthalate dyeable with the atmospheric cationic dye of the present invention. Polyurethane elastic fibers cannot be dyed with cationic dyes. However, when using polytrimethylene terephthalate fibers that can be dyed with cationic dyes under normal pressure, it will selectively apply only China's national I? Mu (CNS) Λ., 1 丨 ⑽ (TTo aoV /: ,, n) 1 〇7T ~ 568965 V. Description of the invention (25) Dyeing, so there will be no above problems. The second method is to use polytrimethylene terephthalate fiber which can be dyed using the atmospheric pressure disperse dye of the present invention. This is because polytrimethylene terephthalate-based fibers can be modified to have normal-pressure disperse dyeability, so that disperse dyes can be prevented from migrating to polyurethane elastic fibers. (3) An example of a stretchable fiber typified by a mixed polyurethane elastic fiber is a pantyhose with strong tenacity. However, the industry lacks a high-pressure dyeing kettle necessary for general high-pressure dyeing in specialized dyeing factories. When using the polytrimethylene terephthalate fiber capable of dyeing atmospheric pressure cationic dyes or normal pressure disperse dyes of the present invention, it is possible to directly switch to nylon fiber cross-knitting tights without adding new equipment. Advantages of the equipment used in the atmospheric dyeing kettle. Also, the advantages of this device have extremely important effects on industry. The history of the y ministry (? 次 ^,-" <^-消 贽 合 0 社 印 ¥ 11— I ........ i--I--f! J I (¾ and: λτΛΦ Item D) (4) The cloth obtained by using the polytrimethylene terephthalate fiber of the present invention, for example, can have a softer feel and a softer touch than the cloths currently mixed with nylon fibers and polyurethane elastic fibers, and There is no rigidity peculiar to nylon fibers. In addition, it has light stretchability and excellent color rendering properties, so a new feeling can be obtained. In addition, polytrimethylene terephthalate fibers have high heat fixability. And excellent yellowing resistance. Because these characteristics do not cause problems specific to nylon fibers, a cloth with excellent handleability can be obtained. '(5) The polyester fiber and cellulose fiber g of the present invention also have excellent results when mixed. · When using reactive dyes to dye cellulose fibers, the reaction dye will easily decompose when the temperature of the right dyeing bath exceeds 100 ° C. When using the polytrimethylene terephthalate fiber of the present invention, Cationic or disperse dyes and reactive dyes can be used for one-stage one-bath dyeing under normal pressure
本纸張尺度適用中國國家iu參(CNS ) Λ4 4:,½ ( 210,) - 9ftT 568965 Λ 7 ________ _ ]]Ί 五、發明説明(26 ) 色。所得之布料則可兼具纖維素特有之乾爽感及來自聚三 甲撐對苯二甲酸酯的柔軟性,故能得到新感覺衣料。 (6 )本發明之聚酯纖維可單獨適甩於編織物,而目 所得之布料可具有豐富之柔軟性,優良之伸縮性及顯色性 。另外,1 0 0 °c以上進行染色時亦不會產生問題,故可 以1 0 0 t:以上進行染色。 、 又’本發明之聚酯纖維具有其爲陽離子染料可染性之 纖維及,能工業性地抑制鹼減量之量與速度的特徵。因此 鹼減量之本發明的聚酯纖維可具有更柔之柔軟性及,因其 纖維表面存在數// m程度之微細孔,故可具有乾爽感與染 色鮮明之持徵。又,本發明的常壓分散染料可染性之聚酯 纖維亦具有相近的鹼減量特性。 , 以上所述之本發明的聚三甲撐對苯二甲酸酯可依據上 述使用樣態而使用於外衣,內衣類,裏布,褲子等衣料, 或地毯用原絲,芯心,飾品等資材上。 Μ滅部屮史抒冷^h_T.^贽合竹杜印¾ --------A---^---r ^ (^尤閱讀背而之注本D ) 下面將以實施例詳細說明本發明,但非限於此例。又 ,實施例中的主要測定値及評估値係利用下列測定方法, 評估方法而得到。 (1 )測定極限黏度 測定此極限黏度〔7/〕之方式爲,利用奧斯特瓦爾德 黏度管,於3 5 °C下使用〇 —氯苯醋而細得。 (2 )測定損耗正接 1、纸张尺度適用中國國家)!·隼(CNS )八叫仏(2ϋ yfl ) . 29 - ~ 568965 五、發明説明(27 ) 利用歐里耶提克公司製雷歐白佛隆,於乾燥空氣中, 測定周波數1 1 Ο Η Z ,升溫速度5 °C / m i η下,測定 各溫度下損耗正接(t a η δ )及動態彈性率。再由此結 果求取損耗正接與溫度曲線,並由此曲線上求取損耗正接 之峰溫度的Tmax(°c)。 (3 )測定彈性率 -裝· 依據:f I S — L - 1 〇 1 3測定彈性率。 (4 )測定熔點 、-口 利用精工電子公司製DSC,於20 °C / mi η之昇 溫速度,1 0 0毫升/ m i η之氮氣氣流下測定。並以熔 解之峰的峰値溫度爲熔點。 ' (5 )測定彈性回復率 將纖維固定於夾頭間距爲2 0 c m之拉伸試驗機上, 以拉長率至2 0%之拉伸速度2 0 cm/m i η拉長1分 鐘後放置。其後再以同速度收縮,並捐繪出應力-應數曲 線。又,以收縮中應力爲0時之拉伸度爲殘留拉伸度(X )。而彈性回復率係利用下列式求取。 彈性回復率=-|~Χ X 100(%) (6 )測定b値 本紙张尺度適用中國國家枝-導(CNS ) MWWU ( 210 κ ?cp ;./; 5 "30^"" 568965 五、發明説明(28 ) 利用b値測定所得纖維的黃色程度。又,b値係利用 斯卡試驗機(股)的色彩電腦而測得。若b値愈大表示黃 色愈多。 (7 )染色性評估試驗 ① 評估陽離子染料對聚酯纖維染色性 試料爲聚酯纖維的一口編物圓編,天竺,規格2 8 ) ’利用含斯克阿隆魯4 0 0 (花王公司製,非離子表面活 性劑)2 g / d之溫水(浴比χ : 5 0 )進行7 〇 °C, 2 0分鐘洗淨處理後,利用轉鼓乾燥機使其乾燥。其次利 用針式拉幅進行1 8 0 °C,3 0秒的熱固定處理。其後使 用卡揚庫里魯藍一 GSL-ED (日本化藥(股)製陽離 子染料)對所得之物進行4 % 〇 w f ,浴比'1 : 5 0, 9 5 °C,3 0分鐘的染色處理。並加入添加劑之乙酸 0 · 2 5 g /<d及硫酸鈉3 g / d,以調整P Η値。 ② 評估分散染料對聚酯纖維之染色性 經溁部中史標蟫^只工消资合竹社印狀 --------t—— 5式料爲聚醋纖維的一 口編物(圓編,天竺’規格2 8 )’利用含2 g / d之斯克阿隆魯4 0 0的溫水(浴比1 :5 0 )進行7 0 °c,2 0分鐘的洗淨處理後、利用轉鼓 乾燥機使其乾燥。其次利用針式拉幅機進行1 8 0 °C, 3 0秒之熱固定處理。其後使用卡揚隆聚酯藍一 3 R S F (曰本化藥公司製,分散染料)6 % 〇 w ί進行浴比1 : 50 ’ 9 5°C ’ 6〇分鐘的染色處理。並加入分散劑之尼 卡薩索魯7 0 0 〇 (日華化學公司製,陰離子性表面活性 紙张尺度適用中國國fΑ^^Γ(7κΓ:7ν·;;« Γ 〇7"f — 568965 Λ 7 五、發明説明(29 ) - 劑)0 · 5g/d及,調整pH用之乙酸〇 · 25毫开/ 1與乙酸鈉1 g/d,以使pH爲5。 求取抽空率之方式爲,利用分光光度計求取染料原料 之吸光度A,染色後之染液的吸光度a後,以下列式求取 。所採用的吸光度爲,此染色之最大吸收波長5 8 〇 n 11 m 下的値。 抽空率=(A— a)/Axl〇〇 (%)The dimensions of this paper are applicable to Chinese national ginseng (CNS) Λ4 4:, ½ (210,)-9ftT 568965 Λ 7 ________ _]] Ί 5. Description of the invention (26) color. The obtained cloth can have both a dry feeling peculiar to cellulose and a softness derived from polytrimethylene terephthalate, so that a new feeling cloth can be obtained. (6) The polyester fiber of the present invention can be suitable for being thrown on a woven fabric alone, and the obtained cloth can have rich softness, excellent stretchability and color rendering. In addition, dyeing at temperatures above 100 ° C does not cause any problems, so dyeing at temperatures above 100 t: is possible. The polyester fiber of the present invention is characterized in that it is a cationic dyeable fiber and that it can industrially suppress the amount and speed of alkali reduction. Therefore, the alkali-reduced polyester fiber of the present invention can have more softness and softness, and because the surface of the fiber has micropores of about several meters per meter, it can have the characteristics of dryness and vivid dyeing. In addition, the polyester fiber capable of dyeing the atmospheric-pressure disperse dye of the present invention has similar alkali-reducing properties. According to the above-mentioned polytrimethylene terephthalate of the present invention, it can be used in outerwear, underwear, lining, trousers and other materials according to the above-mentioned usage patterns, or raw materials for carpets, cores, jewelry and other materials. on. M 灭 部 屮 史 史 冷 ^ h_T. ^ 贽 合 竹 杜 印 ¾ -------- A --- ^ --- r ^ (^ You read the note to the back of this book D) The following will be implemented Examples illustrate the present invention in detail, but are not limited to this example. The main measurements and evaluations in the examples are obtained by the following measurement methods and evaluation methods. (1) Determination of the limiting viscosity The method of measuring the limiting viscosity [7 /] is to use an Osterwald viscosity tube and use 0-chlorobenzene vinegar at 35 ° C to obtain a fine. (2) Measurement of loss positive 1. Paper size is applicable to China) !! (CNS) 八 叫 仏 (2ϋ yfl). 29-~ 568965 V. Description of the invention (27) Use of Leo White Furon manufactured by Oriyetic Corporation In a dry air, measure the number of cycles 1 1 Ο Η Z and the temperature increase rate 5 ° C / mi η, and measure the loss positive connection (ta η δ) and dynamic elasticity at each temperature. From this result, the curve of loss positive connection and temperature is obtained, and from this curve, the peak temperature Tmax (° c) of the loss positive connection is obtained. (3) Measurement of modulus of elasticity-Installation and basis: f I S — L-103. The modulus of elasticity was measured. (4) Measurement of melting point Measured using DSC manufactured by Seiko Instruments Inc. at a temperature rising rate of 20 ° C / mi η under a nitrogen gas flow of 100 ml / m η. The melting point of the melting peak is used as the melting point. '(5) Determine the elastic recovery rate and fix the fiber on a tensile tester with a chuck spacing of 20 cm, and stretch it at a stretching rate of 20% to 20% at a speed of 20 cm / mi η and leave it for 1 minute . Thereafter, it was contracted at the same speed and the stress-response curve was donated. In addition, the degree of elongation when the stress during shrinkage is 0 is taken as the residual elongation (X). The elastic recovery rate is obtained by the following formula. Elastic response rate =-| ~ X X 100 (%) (6) Determination of b 値 Paper size Applicable to China National Branch-Guide (CNS) MWWU (210 κ? Cp;.; 5 " 30 ^ " " 568965 V. Description of the invention (28) The degree of yellowness of the obtained fiber is measured by using b 値. In addition, b 値 is measured using a color computer of a ska tester (strand). A larger b 大 indicates more yellow. (7 ) Dyeability evaluation test ① The sample used to evaluate the dyeability of cationic dyes on polyester fibers is a knit of polyester fiber, Tianzhu, size 2 8) 'Using SK Alonglu 4 0 0 (manufactured by Kao Corporation, non-ionic surface) Active agent) 2 g / d warm water (bath ratio χ: 50) was washed at 70 ° C for 20 minutes, and then dried with a drum dryer. Secondly, the pin-type stenter was used for heat fixing at 180 ° C for 30 seconds. Thereafter, the obtained product was subjected to 4% 〇wf using Kayan Kurilu blue GSL-ED (a cationic dye made by Nippon Kayaku Co., Ltd.), and the bath ratio was' 1: 50, 95 ° C, 30 minutes. Dyeing treatment. Add acetic acid 0 · 25 g / < d and sodium sulfate 3 g / d as additives to adjust PΗ 値. ② Assessing the dyeability of disperse dyes on polyester fibers by the Ministry of Economic History in the Ministry of Economics and Industry ^ ^ Gongzhuzi Hezhu Bamboo Printing -------- t—— Type 5 is a knit of polyester fiber ( Circular knitting, Tianzhu "Specification 2 8) 'After using 2 g / d of Akelulu 4 0 0 warm water (bath ratio 1: 5 0) for 7 0 ° C, 20 minutes of washing treatment, It was dried with a drum dryer. Secondly, a pin tenter was used for heat fixing at 180 ° C for 30 seconds. Thereafter, a dyeing treatment with a bath ratio of 1:50 '9 5 ° C' for 60 minutes was performed using Kayanlon Polyester Blue-3R S F (manufactured by Japan Chemical Co., Ltd., disperse dye) 6%. And dispersant is added Nicasa Solu 7 0 0 〇 (manufactured by Nichia Chemical Co., Ltd., anionic surface-active paper scale applicable to the Chinese country fΑ ^^ Γ (7κΓ: 7ν · ;; «Γ 〇7 " f — 568965 Λ 7 V. Description of the invention (29)-Agent) 0 · 5g / d and acetic acid used for pH adjustment 0.25mK // 1 and sodium acetate 1g / d so that the pH is 5. Find the evacuation rate of The method is to use a spectrophotometer to obtain the absorbance A of the dye material, and then obtain the absorbance a of the dyeing solution after the dyeing, and then use the following formula. The absorbance used is the maximum absorption wavelength of this dyeing at 5 8 〇n 11 m値。 Evacuation rate = (A— a) / Ax100 (%)
'4·'、· "V --口 表示染成何種程度之深色度則是利用K / S進行評估 。又此値係由,測定染色後之樣品布料的分光反射率後, 以下列之Kubelka-Munk式求取。若此値愈大表示深色效果 愈大,即,愈能顯色。所採用的R爲,此染料之最大吸收 波長下的値。'4 ·', · " V --- mouth The degree of darkness that indicates the degree of dyeing is evaluated using K / S. In this case, after measuring the spectral reflectance of the sample cloth after dyeing, it is determined by the following Kubelka-Munk formula. A larger value means that the darker effect is greater, that is, the color can be developed. The R used is 値 at the maximum absorption wavelength of this dye.
K/S=(l— R)2/2R 另外,染成黑色時的明亮度則係利用L値進行評估。 (8 )染色堅牢度試驗 染色纖維之堅牢性試驗係利用(6 )之方法所製得的 染色一口編物進行評估。 其中,乾洗堅牢度則係依據J I S - L 一 04 6 〇 , 耐光堅牢度係依據J I S — L - 0 8 4 2,洗濯堅牢度係 本紙张尺度適用中國國家牦準(CNS ) Λ川:仏(2丨0 X :?〔厂;广_ 〇9 568965 五、發明説明(3〇 ) 依據J I S — L 一 0 8 4 4,而乾,濕摩擦堅牢度則係依 據J I S - L 一 〇 8 4 9。另外,'乾洗堅牢度亦進行液污 染試驗。 .(9 )測定U % 利用謝魯佩卡烏斯塔公司製USTER TESTER3而測得。 〔實施例1〕 ' 於2 2 0 °C下利用三甲二醇(以下簡稱爲「τ M G」 經靖部中史梓汶^h.T.消贽合^:社印y )1144重量份,二甲基對苯二甲酸酯(以下簡稱爲「 •DMT」)1 3 0 0重量份,5 —磺基間苯二酸四丁基鱗 鹽(以下簡稱爲「S ί Ρ Ρ」)5 7重量份(對全部酸成 分之總克分子數爲2 m ο 1 % ),醚形成抑制劑之乙酸鋰 〇 · 4 3重量份,著色抑制劑之乙酸鈷〇 .丨3重量份, 酯交換觸媒之鈦四丁氧化物1 · 3重量份進行酯交換反應 。其次於27 0°C,減壓度爲0 · 5 t 〇 r r下利用聚縮 合觸媒之鈦四丁氧化物1·3重量份,熱安定劑之三甲基 亞磷酸鹽0·065重量份進行聚縮合,得聚合物。又, .所得聚合物之極限黏度爲0 . 6 1。 ♦ 使所得聚合物片乾燥後,利用具有3 6個圓剖面之孔 (直徑0 · 2 3 m m )的紡口,以紡絲溫度2 6 5。(:,紡 絲速度1 2 0 0 m / m i η進行肪絲’得未延伸絲。其後 於熱滾軸5 0 °C,熱板1 4 0 °C,延伸倍率3 · 0倍,延 伸速度6 0 0 m / m i η下對所得未延伸絲進行延撚,得 本紙张尺度適用中國國家棍) λ4ΜμΓΓΤ)〇7^γ/ ;χ I: )' Ι γΓΓ ……— 568965 Λ7K / S = (l—R) 2 / 2R In addition, the brightness when dyed to black is evaluated using L 値. (8) Dyeing fastness test The fastness test of the dyed fiber was evaluated by using the dyed bite knitted fabric prepared by the method of (6). Among them, the fastness to dry cleaning is based on JIS-L 04 06, the light fastness is based on JIS — L-0 8 42, and the fastness to washing is based on this paper. The Chinese National Standard (CNS) is applicable Λ 川: 仏 ( 2 丨 0 X :? [Factory; Guang_ 〇9 568965 V. Description of the invention (3〇) is based on JIS — L 0 0 4 4 and the fastness of dry and wet friction is based on JIS-L 108 8 9 In addition, 'the fastness to dry cleaning was also subjected to a liquid contamination test. (9) The U% was measured using USTER TESTER 3 manufactured by Cherupe Kausta. [Example 1]' Using trimethylamine at 220 ° C 1144 parts by weight of alcohol (hereinafter referred to as "τ MG" by Shi Ziwen in the Ministry of Economic Affairs of China, ^ hT ^: Sheyin y), dimethyl terephthalate (hereinafter referred to as "• DMT") 1 3 0 0 parts by weight, 5 -sulfoisophthalic acid tetrabutyl scale salt (hereinafter referred to as "S ί ΡΡ") 5 7 parts by weight (total gram number of all acid components is 2 m ο 1% ), Lithium acetate 0.43 parts by weight of ether formation inhibitor, cobalt acetate 0.3 parts by weight of coloration inhibitor, titanium tetrabutoxide of transesterification catalyst 1.3 The transesterification reaction was carried out in parts. Next was 2.7 parts by weight of titanium tetrabutoxide using a polycondensation catalyst at 27 ° C and a decompression degree of 0.5 t rr. The polymer was polycondensed at 0. 065 parts by weight of phosphate to obtain a polymer. In addition, the limiting viscosity of the obtained polymer was 0.6 1. ♦ After the obtained polymer sheet was dried, pores (diameters having 36 circular cross sections) were used. 0 · 2 3 mm), at a spinning temperature of 2 6 5. (:, Spinning speed of 1 2 0 0 m / mi η is performed to obtain unstretched yarn. Then it is heated at 50 ° C, hot plate 1 40 ° C, drawing ratio 3.0 · times, drawing speed of the unstretched yarn at a drawing speed of 600 m / mi η, the paper size is applicable to the Chinese national stick) λ4ΜμΓΓΤ) 〇7 ^ γ /; χ I:) 'Ι γΓΓ …… — 568965 Λ7
--_ _________ IP --- · - 一 - *- ,—,_,, w — —_ - 五、發明説明(31 ) 5 〇 d / 3 6 f之延伸絲。結果所得纖維之物性爲,熔點 23l°c,密度 1 · 32g/cm3,強度 3 · 4g/d, 延伸度37%,丁1113又11〇。(:,1;%1.2%,彈性 率2 2 g / d,彈性回復率8 7 %。又,延伸絲之Q / R 値爲0 . 2 5,故符合式(1 )。另外,纖維之b値爲 6·ι〇--_ _________ IP --- ·-a-*-,-, _ ,, w — —_-5. Description of the invention (31) 5 〇 d / 3 6 f extension wire. As a result, the physical properties of the obtained fiber were: a melting point of 23 l ° C, a density of 1.32 g / cm3, a strength of 3.4 g / d, an elongation of 37%, and a density of 1113 and 110. (:, 1;% 1.2%, elasticity rate 2 2 g / d, elastic recovery rate 87%. Also, the Q / R 値 of the extension yarn is 0.25, so it conforms to the formula (1). In addition, the fiber b 値 is 6.
I 此實施例所製得之聚酯纖維的9 5 °C,3 0分鐘下之 陽離子染料之抽空率爲7 2 %的大値,可得非常鮮明之染 色物。I The polyester fiber obtained in this example was 95 ° C, and the cathodic dye evacuation rate at 30 minutes was 72%, and a very clear dye was obtained.
、1T 由染色後之一口編物的乾洗堅牢度得知,此染色物不 退色,又,液污染爲4 - 5級。另外,具有良好之耐光堅 牢度(4 — 5級),乾、濕摩擦堅牢度(5級),洗濯堅 牢度(5級)。 〔實施例2〜7〕 經消部中次桴冷局ι,ηΐ 、合竹社印聚 .除了改變酯形成性磺酸鹽化合物之種類及共聚合比率 外,其他同實施例1之方法進行聚合’紡絲。所得纖維之 試驗,評估試驗結果如表1所示。結果任何一個實施例之 纖維均符合式(1 ),因此具有良好之染色性,堅牢性, 諸物性。 〔比較例1〕 除了未使用s I p p外,1其他同實施例1 ,得聚三甲 撐對苯二甲酸酯均聚物。所得聚合物之極限黏度爲 本纸张尺度適用中國國家d- ( CNS) 仏.(210X 2‘-厂Λ G ) - 34 - 568965 五、發明説明(32、 — — 〇 · 6 3。其次,同實施例1進行紡絲,延伸,得纖維。 結果所得纖維爲,熔點2 3 6 °C,T m a X 1 1 1 t,強 度3 · 6g/d ’延伸度35%,彈性率23g/d,彈 性回復率8 8 %。又,纖維之Q / R値爲〇 · 2 6,故符 合式(1 )。 但’此比較例所得之聚酯纖維的9 5 °C,3 0分'鐘下 之陽離子染料之抽空率爲6%,故無法染成深色。 〔比較例2〕 除了調製SIPP之共聚合比率爲〇·3克分子%的 聚合物外’其他同實施例1進行紡絲。所得纖維之試驗, 評估結果如表1所示。結果酯形成性磺酸鹽化合物之共聚 合比率低於0 · 5克分子%,纖維之9 5 °C,3 0分鐘下 的陽離子染料之抽空率爲3 0%,因此無法染成深色。- 〔比較例3〕 除了將S I P P之共聚合比率改爲6克分子%外,其 他同實施例1之方法進行聚合,紡絲,以調製成纖維。其 試驗,評估結果如表1所不。又,此聚合物於肪絲時產生 多量的斷絲情形,故紡絲性差。另外,纖維於9 5 °C下進 行染色時,會因絲收縮而變硬,故無法得到觸感良好之布 料。所得布料之乾洗堅牢度比實施例低。 〔比較例4〕 除了將延伸倍率改爲3 · 3倍外,其他同實施例1。 本紙张尺度適用中國國家核Ϊ ( CNS ) Λ4Η:仏(21〇v?^;;\j; ! . 35^~ —_ 計t閃讀艿而之>14,-|.-;1:^]'巧叻{^本力 -訂· 568965 五、發明説明(33 ) 結果所得纖維之定:向適當而使T m a X超過1 1 5 t。陽 離子染料之抽空率爲4 5 %。又,所得纖維會造成多數起 毛現象。 經滴部中次標砣而以.1:消贽合竹社印來 本紙张尺度適用中國國家柷卑(CNS ) A.m’仏·( ) -36- 568965 — )Γ' T __ 产,_ - I I · * - ------------ _ _ · _· »———»· * · · ··— - 五、發明説明(35 ) 〔比較例5〕 除了將熱滾軸之溫度改爲2 5 °C外,其他同實施例1 之方法進行聚合,紡絲。結果延伸時產生多量的斷絲情形 ,故無法連續得到纖維。又,除了將熱滾軸之溫度改爲 8 0 t外,其他同實施例1之方法進行聚合,紡絲。結果 延伸時熱滾軸會使絲熔著而產生大量的單絲斷裂情形,故 所得之纖維會有很多起毛現象。U %爲3 . 2之較差値。 〔比較例6〕 除了將熱板之溫度改爲7 0 °C外,其他同實施例1之 方法進行聚合,紡絲。結果得無斷絲,起毛等問題之纖維 。但,所得纖維之彈性回復率爲較低的5 5 %,Q / R値 爲0 · 4 9,故無法符合式(1 ) 。 ^ ,〔比較例7〕 除了將熱板之溫度改爲2 0 0 °C外,其他同實施例1 之方法進行聚合,紡絲。結果纖維會因熱板而切斷,故無 法延伸。 ‘ 〔比較例8〕 ' 除了將延伸倍率改爲2 · 3倍及,熱板溫度改爲 1 8 0 °C外,其他同實施例1之方法進行聚合,紡絲。結 果可得無斷絲,起毛等問題之纖維。但,所得纖維之彈性 回復率爲較低48%,Q/R値爲〇 · 5 2,故無法符合 木ϋ尺度適用中國國家彳^ ( CNS ) Α4Π;^ ( 210>; ?g· ; i'· ) ^一…—1T is known from the fastness of dry-cleaning a knitted fabric after dyeing. The dyed material does not fade, and the liquid pollution is grade 4-5. In addition, it has good light fastness (level 4-5), dry and wet rubbing fastness (level 5), and washing fastness (level 5). [Examples 2 to 7] In the consumer department, the heat treatment was carried out in the middle stage, ηΐ, and Hezhusha Printing Co., except that the type and copolymerization ratio of the ester-forming sulfonate compound were changed, and the method was performed in the same manner as in Example 1. Polymer 'spinning. The test and evaluation results of the obtained fibers are shown in Table 1. As a result, the fibers of any of the examples conformed to the formula (1), and therefore had good dyeability, fastness, and various physical properties. [Comparative Example 1] A polytrimethylene terephthalate homopolymer was obtained in the same manner as in Example 1 except that s I p p was not used. The limiting viscosity of the obtained polymer is based on the paper standard applicable to Chinese national d- (CNS) 仏. (210X 2'-factory Λ G)-34-568965 V. Description of the invention (32,--0 · 63. Second, the same Example 1 was spun and stretched to obtain fibers. As a result, the fibers obtained had a melting point of 2 3 6 ° C, T ma X 1 1 1 t, a strength of 3 · 6 g / d, an elongation of 35%, and an elastic modulus of 23 g / d. The elastic recovery rate is 88%. In addition, the fiber Q / R 値 is 0.26, so it conforms to the formula (1). However, the polyester fiber obtained in this comparative example is below 95 ° C for 30 minutes. The cationic dye had an evacuation rate of 6%, so it could not be dyed in a dark color. [Comparative Example 2] Spinning was performed in the same manner as in Example 1 except that a polymer having a copolymerization ratio of SIPP of 0.3 mol% was prepared. The test results of the obtained fibers are shown in Table 1. As a result, the copolymerization ratio of the ester-forming sulfonate compound was lower than 0.5 mol%, the fiber was 95 ° C, and the cationic dye was evacuated in 30 minutes. The rate is 30%, so it cannot be dyed in dark colors.-[Comparative Example 3] Except that the copolymerization ratio of SIPP was changed to 6 mol%, the other The method of Example 1 was polymerized and spun to prepare fibers. The test and evaluation results are not shown in Table 1. In addition, the polymer produced a large number of yarn breaks in the fat yarn, so the spinnability was poor. In addition, When the fiber is dyed at 95 ° C, it will harden due to the shrinkage of the silk, so a cloth with good feel cannot be obtained. The dry-cleaning fastness of the obtained cloth is lower than that of the example. [Comparative Example 4] In addition to changing the stretching ratio to 3 · 3 times, the other is the same as in Example 1. The paper size is applicable to China National Nuclear Tritium (CNS) Λ4Η: 仏 (21〇v? ^ ;; \ j;!. 35 ^ ~ —_ Count t flash read No. > 14,-| .-; 1: ^] 'Qiaorat {^ Benli-Order · 568965 V. Description of the invention (33) The result of the determination of the fiber: T ma X exceeds 1 1 5 t as appropriate The cathodic dye evacuation rate is 45%. In addition, the obtained fiber will cause most fluffing phenomenon. After the standard of the drop department, the paper is printed with .1: printed by Hezhu Society. This paper applies to the Chinese national standard (CNS). ) A.m '仏 · () -36- 568965 —) Γ' T __ Product, _-II · *------------- _ _ · _ · »———» · * · · · · —-5. Description of the invention (35) [Comparative Example 5] Except that the temperature of the hot roller was changed to 25 ° C, the polymerization was performed in the same manner as in Example 1 and spinning was performed. As a result, a large number of yarn breaks occurred during stretching, so it could not be obtained continuously. The fibers were polymerized and spun in the same manner as in Example 1 except that the temperature of the hot roller was changed to 80 t. As a result, the hot roller can cause the filaments to fuse and cause a large number of filament breaks during stretching, so the resulting fiber will have a lot of fluffing. U% is a relatively low rate of 3.2. [Comparative Example 6] The polymerization and spinning were carried out in the same manner as in Example 1 except that the temperature of the hot plate was changed to 70 ° C. The result is a fiber without problems such as broken filaments and fluff. However, the elastic recovery rate of the obtained fiber was lower 55%, and Q / R 値 was 0.49, so it could not meet the formula (1). ^ [Comparative Example 7] Except that the temperature of the hot plate was changed to 200 ° C, the polymerization and spinning were performed in the same manner as in Example 1. As a result, the fibers are cut by the hot plate and cannot be stretched. ‘[Comparative Example 8] 'Except that the stretching ratio was changed to 2.3 times and the hot plate temperature was changed to 180 ° C, the polymerization and spinning were performed in the same manner as in Example 1. As a result, a fiber having no problems such as broken wires or fluff can be obtained. However, the elastic recovery rate of the obtained fiber was 48% lower, and Q / R 値 was 0.52, so it could not meet the standard of Chinaϋϋ (CNS) Α4Π; ^ (210 >;? G ·; i '·) ^ 一 ...—
568965568965
A 7 IP 五、發明説明(36 ) 式(1 )。 〔比較例9〕 利用中2 · 5克分子%之5 —鈉磺基間苯二酸共聚合 而成的聚乙烯對苯二甲酸酯纖維進行紡絲。所得纖維爲, 強度4 · 2g/d,延伸度30%’彈性率l〇〇g/d ,彈性回復率31%,Q/R値3 · 2,Tmax 131 °C,又,陽離子染料之95 °C,30分鐘下的抽空 率爲3 6 %。 〔參考例1〕 除了不用乙酸鈷,三甲基亞磷酸鹽外,其他同實施例 1。此時纖維物性雖未改變,但,纖維之b値爲1 1 · 2 ,故會變黃。 〔實施例8〕 使實施例2所得之聚合物乾燥後,使水分成爲 5 0 p P m,再以2 8 5 t:進行熔融,並經由一層排列的 36個直徑〇·23mm之孔的紡口擠出。其次,讓擠出 之熔融複合絲通過長5 c m,溫度1 〇 〇 °C之保溫領域_ ,以風速0 · 4 m / m i η之風使其急冷,得固體複合絲 。其後,讓固體複合絲通過加熱至6 0 °C之回轉速度爲 2 1 0 0 m / m i η的第一滾軸與加熱至1 3 3 °C之回轉 速度爲4 3 0 0 m / m i η的第二滾軸之間,以進行熱延 本纸張尺度適用中國國家«卑(CNS ) Λ州仏(210OV:、ν ) ΟΠ 568965 五、發明説明(π ) 伸及熱固定,接著以4 1 8 0 m / m i η捲取。結果所得 纖維爲雙絲之7 5 d / 7 2 ί。 、 又’所得纖維之物性爲,強度3 · 1 g / d,延伸率 4 1 %,U % 〇 · 7 %,彈性囘復率8 9 %,Q / R値 0 · 25,Tmax 109°C,且 95°C,30 分鐘下 陽離子染料之抽空率98%,b値6.5。 〔實施例9〕 使用實施例1之聚酯纖維與2 1 0旦之勒依卡(旭化 成工業(股)製聚尿烷系伸縮纖維)編成經編物。編成之 規格爲28G ,聚酯纖維之束長爲l〇8〇mm/480 回,伸縮纖維爲1 1 2 m m / 4 8 0回,又,投梭密度 90回/英寸。又,聚酯纖維之混率設定爲75 · 5%。 對所得生機進行9 0 °C,2分鐘的無張力洗淨後,進行 經求部中火桴消费合竹社印於 I ϋ I I - -.....-.....I n · J1-1 n 1:1 -I- -1----——i 丁 、vy,v-0 (1^1間-¾^:而之注 項 本 m ) 1 6 0 °C ’ 1分鐘乾熱固定。其後將染料之卡揚庫里魯黑 B S - E D (日本化藥(股·)製陽離子染料)加入使用分 散劑之提斯巴- T L (明成化學(股)製非離子性活性劑 )lg/Ι之,添加硫酸鈉50g/l及碳酸鈉I5g/ d而使p Η調整爲1 1的水溶液中,以作爲染液。接著於 染色濃度爲8%owf ,浴比1 : 50下進行9 5°C,1 小時染色處理。染色後於古藍阿普P (三洋化成工業(股 )製非離子性表面活性劑)1 g / 1 ,浴比1 : 5 0, 8 0 °C下進行1 0分鐘的皂洗處理。並利用一般方法進行 加工。所得染色物之L値爲1 1 · 2,能充分染色。染色 ^氏张尺度適用中國國t樣嗥(CNS ) Λ心丨( 210x?t ) . 4〇T" 568965 A 7 五、發明説明(38 ) n m I - II 丨丨,I · J “卜――- - II: - I TW, ,"v 、-口 v^.ly^T $ f 之·;τ-*1;ϋη·:ί:"功、*ί>:7 本 D ) 物之染色堅牢性方面爲,洗濯堅牢度5級,濕摩擦堅牢度 5級,耐光堅牢度4至5級。又,此染色編物且柔軟性及 *豐富的伸縮性,且具有擴.張,腰身之優良質感。 〔實施例1 0〕 使用實施例2之聚酯纖維,並重覆實施例9之操作方 式。所得染色物之L値爲10 . 9,可充分染色。此染色 物之染色堅牢性爲,洗濯堅牢性5級' 濕摩擦堅牢性5級 ,耐光堅牢性4至5級。染色物具柔軟性及豐富伸縮性, 且具有擴張,腰身之優良質感。 〔比較例1 0〕 使用比較例1所製成之聚三甲撐對苯二甲酸酯纖維, 並同實施例9編成編物。 對所得生機進行9 0 °C,2分鐘的無張力洗淨處理, .再進行1 6 0 °C,1分鐘的乾熱處理。又,爲了染成深色 而使泰阿尼庫斯黑BG-FS (泰斯塔日本公司製分散染 料)8 0 % 〇 w ί ’並於存在染色助劑之尼卡散索魯特 1 2 0 0 〇 · 5g/l ,經乙酸調整而使ΡΗ爲6 ,浴 比1 : 3 0之情形下進行9 5 °C,6 0分鐘的染色處理。 所得染色物之濕摩擦堅牢性爲2級,且具有遊離的污染伸 縮纖維之分散染料。‘ 另外’使用比較例9所製成之纖維,並重覆實施例9 之操作方式。所得布料明顯變硬,L値爲2 1 ,故只能染 本紙张尺度適用中國國[ΓΓ; μ‘1 “:认--------------------- 568965A 7 IP 5. Description of the invention (36) Formula (1). [Comparative Example 9] Polyethylene terephthalate fibers obtained by copolymerizing 5-sodium sulfoisophthalic acid of 2.5 g% by weight were used for spinning. The fiber obtained was a strength of 4 · 2g / d, an elongation of 30%, an elastic modulus of 100g / d, an elastic recovery rate of 31%, a Q / R 値 3 · 2, a Tmax of 131 ° C, and a cationic dye of 95%. The evacuation rate at 30 ° C for 30 minutes was 36%. [Reference Example 1] Except that cobalt acetate and trimethylphosphite were not used, the procedure was the same as in Example 1. Although the physical properties of the fiber were not changed at this time, since the fiber's b 値 was 1 1 · 2, it turned yellow. [Example 8] After the polymer obtained in Example 2 was dried, the moisture was changed to 50 p P m, and the polymer was melted at 2 8 5 t: and passed through a layer of 36 holes with a diameter of 23 mm in diameter. Mouth squeezed. Secondly, the extruded molten composite yarn was passed through a thermal insulation field with a length of 5 cm and a temperature of 1000 ° C, and was rapidly cooled by a wind with a wind speed of 0.4 m / m i η to obtain a solid composite yarn. Thereafter, the solid composite yarn was passed through a first roller heated to 60 ° C with a rotation speed of 2 100 m / mi η and a rotary speed heated to 1 3 3 ° C was 4 3 0 0 m / mi η is used between the second rollers for heat-rolling. The paper size is applicable to the Chinese country «Base (CNS) Λ 州 仏 (210OV :, ν) ΟΠ 568965 V. Description of the invention (π) stretching and heat fixing, and then 4 1 8 0 m / mi η Take-up. As a result, the obtained fiber was 7 5 d / 7 2 ί. The physical properties of the obtained fiber are: strength 3.1 g / d, elongation 41%, U% 0.7%, elastic recovery rate 89%, Q / R 値 0 · 25, Tmax 109 ° C And, at 95 ° C, the evacuation rate of the cationic dye is 98% at 30 minutes, b 値 6.5. [Example 9] A warp knitted fabric was prepared by using the polyester fiber of Example 1 and Leica (210 urethane-based stretchable fiber manufactured by Asahi Kasei Corporation). The specifications are 28G, the bundle length of polyester fiber is 108mm / 480 times, the stretch fiber is 112mm / 480 times, and the shuttle density is 90 times / inch. The blend ratio of the polyester fibers was set to 75.5%. After the obtained vitality was washed at 90 ° C for 2 minutes without tension, it was printed on I ϋ II--....-..... I n · J1-1 n 1: 1 -I- -1 ----—— i Ding, vy, v-0 (1 ^ 1 room-¾ ^: while the note item m) 1 6 0 ° C '1 minute Dry heat fixation. Then Kayan Kurilu Black BS-ED (a cationic dye made by Nippon Kayaku Co., Ltd.) was added to Tishba-TL (a non-ionic active agent made by Meisei Chemical Co., Ltd.) using a dispersant. Lg In addition, 50 g / l of sodium sulfate and 15 g / d of sodium carbonate were added to adjust p 为 to an aqueous solution of 1 1 as a dyeing solution. Next, dyeing was performed at 95 ° C for 1 hour at a dyeing concentration of 8% owf and a bath ratio of 1:50. After dyeing, soaping treatment was performed at Gulan Apu P (non-ionic surfactant manufactured by Sanyo Chemical Industry Co., Ltd.) 1 g / 1 at a bath ratio of 1: 50, 80 ° C for 10 minutes. And use the general method for processing. The L 値 of the obtained dyed matter was 1 1 · 2 and it was sufficiently dyed. Stained ^ 's Zhang scale is applicable to China's t-like sample (CNS) Λ heart 丨 (210x? T). 4〇T " 568965 A 7 V. Description of the invention (38) nm I-II 丨 丨, I · J "Bu― ―--II:-I TW,, " v 、-口 v ^ .ly ^ T $ f z; τ- * 1; ϋη ·: ί: " Gong, * ί >: 7 D) In terms of dyeing fastness, washing fastness is 5th grade, wet rubbing fastness is 5th grade, light fastness is 4 to 5th grade. Also, this dyed knit is soft and has a lot of elasticity, and it has expansion. Zhang, waist [Excellent texture] [Example 10] The polyester fiber of Example 2 was used, and the operation method of Example 9 was repeated. The L 値 of the obtained dyed matter was 10.9, which can be fully dyed. The dyeing fastness of this dyed matter For washing fastness grade 5 'wet rubbing fastness grade 5 and light fastness grade 4 to 5. The dyed material has softness and rich elasticity, and has a good texture of expansion and waist. 〔Comparative example 1 0〕 Use comparison The polytrimethylene terephthalate fiber prepared in Example 1 was knitted into the same fabric as in Example 9. The obtained vitality was subjected to a tension-free washing treatment at 90 ° C for 2 minutes. 1 60 ° C, dry heat treatment for 1 minute. In order to dye dark colors, Tai Anikus Black BG-FS (disperse dyes manufactured by Taistar Japan Co., Ltd.) 80% 〇w Dyeing aid of Nika Sansolut 1 2 0 0 5 g / l, adjusted to pH 6 with acetic acid, and dyed at 9 5 ° C for 60 minutes with a bath ratio of 1: 30 The wet rubbing fastness of the obtained dyed material is Grade 2, and it has a disperse dye that disperses contaminated and stretchable fibers that are free of contamination. In addition, 'the fiber made in Comparative Example 9 is used, and the operation method of Example 9 is repeated. The obtained cloth becomes significantly changed. Hard, L 値 is 2 1, so it can only be dyed on this paper. Applicable to China [ΓΓ; μ'1 ": Recognition --------------------- 568965
IP 五、發明説明(39 ) 成薄色。 又,爲了比較,同實施例9將一般方法所紡成的尼龍 6纖維與勒依卡編成經編物,再利用卡揚隆黑B G L (曰 本化藥(股)製酸性染料)7 % 〇 w ί進行1 0 0 °C, 6 0分鐘的染色處理。所得染色布料之耐光堅牢度爲2至 3級。 〔實施例1 1〕 以實施例1所製得之7 5 d / 3 6 ί的聚酯纖維爲經 絲,並以7 5 d / 4 4 f之銅氨人造絲零緯絲’以製成平 編物(經 1 4 0 條/ 2 5 · 4 m m,緯 8 0 條/ 2 5 . 4 m m )。再利用常法對此平編物進行洗洗淨處理。水洗後 進行1 8 0 °C,3 0秒的加壓固定處理,其後’於不用載 液之情形下,利用陽離子染料,反應染料進行一段一浴染 色處理。所使用之染料爲,卡揚庫里魯黑BS — ED (曰 本化藥(股)製,陽離子染料)及得里馬雷藍一 x 一 S G N (三得(股)製,反應染料)。又,將染料加入使 用分散劑的提斯巴—T L (明成化學(股)製)1 g / 1 之,添加硫酸鈉5 0 g / 1及碳酸鈉1 5 g / 1而使P Η 調整爲1 1的水溶液中,以作爲染液。並於濃度2 % 〇 w f ,浴比1 : 5 0下進行1 0 0 °C,1小時之染色處理。 染色後於古藍阿普P (三洋化成工業(股)製)1 g / 1 ,浴比1 ·· 5 0下進,行8 0 °C,1 〇分鐘的皂洗處理。其 後以常法進行加工。所得染色物可均勻染色,爲鮮明的染 本紙張尺度適用中國國家代牟(CNS ) /\4#仏(&厂 ~ 568965 五、發明説明(42 ) 一 ··— — 同實施例9 ’ 1 1製成織編物,結果可得具有同實施 例9 ’ 1 1之優良質感的布料。 、 〔實施例1 4〕 •裝 剪斷實施例2所得之纖維,得纖維長3 9rnm之短纖 維。以同實施例所製得之2 〇 d / 2 f的複合絲爲芯,並 將此纖維配置於鞘上,得複合混率爲1 1重量%之複合絲 。其次’以此複合絲爲經絲(織密度1 4 6條/ 2 5 · 4 mm) ’緯絲(織密度7 7條/ 2 5 · 4 m m )製成織物 ’再依據實施例9之方法進行9 5。(:下的染色處理。 、11 結果染色布料可染成K/S爲2·5 · 3之深色。又, 所得布料具有優良之擴張,腰身及排斥性。 〔實施例1 5〕 於氮氣中對實施例2所得之聚合物進行2 0 0 °C, 2 4小時的固相聚合,得極限黏度丨· 〇之聚合物。同實 .施例1進行紡絲,結果得具有強度4 _ 0 g / d,伸度 Μ#•部中失忭消贽合竹社印狀 3 2 %,U % 1 · 〇 %,彈性率2 3 g / d,彈性回復率 91%’Q/R 値 〇 · 25 ,Tmax 110°C,b 値 4 · 3之物性的纖維。 〔實施例1 6〕IP 5. Description of the invention (39) Thin color. For comparison, the nylon 6 fiber spun by conventional methods and Leica were knitted into warp knits in the same manner as in Example 9, and then Kayan Long Black BGL (an acid dye made by Benwa Pharmaceutical Co., Ltd.) was used. 7% Perform dyeing at 100 ° C for 60 minutes. The fastness to light of the obtained dyed cloth was grades 2 to 3. [Example 1 1] The 7 5 d / 3 6 ί polyester fiber obtained in Example 1 was used as a warp yarn, and 7 5 d / 4 4 f copper ammonia rayon zero weft yarn was used to make Plain knitted fabric (warp 140 pieces / 25 · 4 mm, weft 80 pieces / 25. 4 mm). Then, the plain knitted fabric is washed and washed by a conventional method. After being washed with water, a pressure fixing treatment at 180 ° C for 30 seconds was performed, and thereafter, a cationic dye and a reactive dye were used for one-stage one-bath dyeing treatment without using a carrier liquid. The dyes used are Kayan Kurilu black BS — ED (a cationic dye made by Japan Chemical Co., Ltd.) and delimare blue one x one S G N (reactive dye made by Suntory (stock)). In addition, the dye was added to 1 g / 1 of Tesba-TL (manufactured by Meisei Chemical Co., Ltd.) using a dispersant, and sodium sulfate 50 g / 1 and sodium carbonate 15 g / 1 were added to adjust P Η to 1 1 in an aqueous solution as a dyeing solution. The dyeing treatment was performed at 100 ° C for 1 hour at a concentration of 2% 〇 w f at a bath ratio of 1: 50. After dyeing, go to ancient blue A P (Sanyo Kasei Kogyo Co., Ltd.) 1 g / 1, the bath ratio is 1 · · 50, and proceed to 80 ° C, soaping treatment for 10 minutes. Thereafter, it is processed by a conventional method. The obtained dyed material can be uniformly dyed, and the paper is of a clear dyeing standard. Applicable to China National Mould (CNS) / \ 4 # 仏 (& factory ~ 568965 5. V. Description of the invention (42) 1 ·· —— — Same as Example 9 ′ 11 1 was made into a woven fabric, and as a result, a cloth having the same excellent texture as in Example 9 ′ 1 1 was obtained. [Example 1 4] • The fiber obtained in Example 2 was cut to obtain short fibers with a fiber length of 39 nm. Take the 20 d / 2 f composite yarn prepared in the same example as the core, and arrange this fiber on the sheath to obtain a composite yarn with a composite mixing ratio of 11% by weight. Secondly, take this composite yarn as a warp Silk (weaving density of 1 4 6/2 5 · 4 mm) 'weft (weaving density of 7 7/2 5 · 4 mm) to make a fabric' and then proceeding to 9 5 according to the method of Example 9. (: the following Dyeing treatment, 11 Results The dyed cloth can be dyed into a dark color with K / S of 2.5, 3. Also, the obtained cloth has excellent expansion, waist and repellency. [Example 1 5] The examples were tested in nitrogen. The polymer obtained in 2 was subjected to solid-state polymerization at 200 ° C for 24 hours to obtain a polymer having a limiting viscosity 丨 · 〇. It was the same as in Example 1. Silk, the result is to have strength 4 _ 0 g / d, elongation M # • Department of 忭 忭 忭 忭 合 竹 社 印 状 32 2%, U% 1 · 〇%, elastic modulus 2 3 g / d, elastic recovery A fiber with a yield of 91% 'Q / R 値 0.25 ·, Tmax 110 ° C, b 値 4 · 3. [Example 16]
於22〇。(:下使用TMG1Q31重量份,1 ,4 — 丁二醇(以下簡稱爲「4」)1 0 6重量份,D Μ T 本紙张尺度適用中國國家枝卑(CNS ) A4R仏(210,' V丨;、 -45- 568965 s A /At 22 o. (: Using TMG1Q31 parts by weight, 1,4-butanediol (hereinafter referred to as "4") 106 parts by weight, D Μ T This paper is applicable to China National Zhibei (CNS) A4R 仏 (210, 'V丨;, -45- 568965 s A /
____ IP *----—— _____ _ 五、發明説明(43 ) ·— 一 ··———— 1 3 0 0重量份,鈦四丁氧化物1 · 3重量份進行酯交換 後’加入二甲基磷酸鹽〇 · 〇 1重量%,並於2 5〇 t:, 減壓度0 · 5 t 〇 r r下進行聚縮合,得聚合物。結果所 得聚合物之極限黏度爲〇 · 8。又,利用N M R測定之聚 合物中的4 G成分爲4 · 1重量%。 使所ί守水口物片乾丨架後’利用具有3 6個圓剖面之孔 (直徑0 · 2 3 m m )的紡口,以紡絲性溫度2 6 5 t:, .裝. 紡絲性速度1 2 0 0 m / m i η進行紡絲性,得未延伸絲 。其次,以熱滾軸6 0 °C,熱板1 4 0 °C,延伸倍率 、-口 2 · 9倍’延伸速度6 0 〇 m / m i η方式對此未延伸絲 進行延撚,得5 0 d / 3. 6 ί之延伸絲。結果纖維物性爲 ,熔點 224°C,Tmax 98°C,強度 3 · 6g/d ,延伸度4 0 %,U % 1 · 2 %,彈性率2 3 g / d ,彈 性回復率8 3 %,b値4 · 5。又,此纖維之Q / R値爲 0.28,故符合式(1)。 另外,·本實施例之聚酯纖維的9 5 t,6 0分鐘下之 分散染料的抽空率爲7 8%,爲高抽空率。 由染色後一口編物之乾洗堅牢度得知此染色物不退色 ,又,液污染爲3 . 5級,另外具有良好之耐光堅牢度( 5至4級),乾,濕摩擦堅牢度(5級),洗濯堅牢度( 5級)。 〔實施例1 7〜2 1〕 除了改變乙二醇種類及,乙二醇類與T M G之比率外 木紙張尺度適用中國國家枒準(CNS ) /\.川:仏(210少) - 46 · 568965 五、發明説明(44 ) ,其他同實施例1 6之方法進行聚合,紡絲。又,所得纖 維之各項試驗,評估結果如表2所示。即,任何一種均爲 符合式(1 )之纖維,且具有良好之染色性,染色堅牢性 ,諸物性。 〔比較例1 2〕 -裝·____ IP * ----—— _____ _ V. Description of the invention (43) ····· ———— 1 3 0 0 parts by weight, titanium tetrabutoxide 1 · 3 parts by weight after transesterification 'added Dimethyl phosphate was 0.001% by weight, and polycondensation was performed at 250 ° C and a reduced pressure of 0.5 ° T rr to obtain a polymer. As a result, the limiting viscosity of the obtained polymer was 0.8. The 4 G component in the polymer measured by N M R was 4 · 1% by weight. After the water-retaining mouthpiece is dried, the spinning mouth with 36 holes (diameter 0 · 23 mm in diameter) with a circular cross section is used to spin at a temperature of 2 6 5 t :,. Spinnability was obtained at a speed of 12 00 m / mi η, and an undrawn yarn was obtained. Next, the unstretched yarn was twisted with a hot roller at 60 ° C, a hot plate at 140 ° C, and a draw ratio of -2 · 9 times the elongation speed of 600 mm / mi to obtain 5 0 d / 3. 6 ί of extension wire. Results The physical properties of the fiber were: melting point 224 ° C, Tmax 98 ° C, strength 3.6g / d, elongation 40%, U% 1.2%, elastic modulus 23g / d, elastic recovery rate 83%, b 値 4 · 5. Since Q / R 値 of this fiber is 0.28, it conforms to the formula (1). In addition, the evacuation rate of the disperse dye in the polyester fiber of this example at 9 5 t and 60 minutes was 78%, which was a high evacuation rate. It is known from the fastness of dry cleaning of a knitted fabric after dyeing that the dyed material does not fade, and the liquid pollution is grade 3.5, and it has good light fastness (grade 5 to 4), and fastness to dry and wet friction (grade 5). ), Wash fastness (level 5). [Example 1 7 ~ 2 1] In addition to changing the type of ethylene glycol and the ratio of ethylene glycol to TMG, the Chinese paper standard (CNS) / \. Sichuan: 仏 (less than 210)-46 · 568965 V. Description of the invention (44), others are polymerized and spun in the same manner as in Example 16. Table 2 shows the evaluation results of the obtained fibers. That is, any of them is a fiber conforming to the formula (1), and has good dyeability, fastness to dyeing, and various physical properties. [Comparative Example 1 2]-Loading ·
、1T 使用比較例1之聚合物,並依據實施例1調,製纖維, 再利用上述(7 )染色性評合試驗②之分散染料評估聚酯 纖維的染色性。但,此比較例所得之聚酯纖維的T m a X 超過1 Ο 2 °C。此纖維之9 5 °C,6 0分鐘下的分散染料 之抽空率爲3 6 %,故無法染成深色。又,將染液濃度改 爲0 · 5%〇 w f時’可將抽空率提升爲8 1%。由此得 知,聚三甲撐對苯二甲酸酯纖維對低濃度之分散染料雖具 有常壓可染性,但,提高染料濃度時不具常壓可染性。 〔比較例1 3〕 經漭部中央標w'合竹社印於 除了改變T M G與4 G之比率外,其他同實施例1 6 之方法進行聚合,紡絲。結果如表2所示。又,其4 G成 分之比率低於1 · 5重量%,纖維之Tma X爲1 〇 6°C 。9 5 °C,6分鐘下之分散染料的抽空率較低,故無法染 成深色。 本纸张尺度適用中國國家彳1隼(CNS ) AWd ( 210 X 、 568965 A;1T uses the polymer of Comparative Example 1 to prepare fibers according to Example 1, and then uses the disperse dye of the above (7) dyeability evaluation test ② to evaluate the dyeability of polyester fibers. However, the T m a X of the polyester fiber obtained in this comparative example exceeds 10 2 ° C. The disperse dye evacuation rate of this fiber at 95 ° C and 60 minutes is 36%, so it cannot be dyed dark. When the concentration of the dye solution was changed to 0. 5% 0 wf ', the evacuation rate was increased to 81%. From this, it is known that although polytrimethylene terephthalate fiber has normal pressure dyeability for low-concentration disperse dyes, it does not have normal pressure dyeability when the dye concentration is increased. [Comparative Example 1 3] Printed on the central part of the crotch, w 'Hezhu Co., Ltd. Except that the ratio of T M G to 4 G was changed, polymerization was performed in the same manner as in Example 16 and spinning was performed. The results are shown in Table 2. The ratio of the 4 G component was less than 1.5% by weight, and the Tma X of the fiber was 106 ° C. 9 The disperse dye has a low evacuation rate at 5 ° C for 6 minutes, so it cannot be dyed dark. The size of this paper is applicable to China's national standard (CNS) AWd (210 X, 568965 A);
Γ~—^ 1P 五、發明説明(46 ) t比較例1 4〕 除了改變T M G與4 G之比率外,其他同實施例1 6 進行聚合,紡絲·。所得纖維之物性,評估結果如表2所示 ° 4 G成分之比率爲1〇 · 3重量%。纖維之丁 max爲 8 5 °C以下,雖具有高抽空率,但乾洗堅牢度爲非常差之 1級。 〔比較例1 5〕 除了以六甲二醇(以下簡稱爲6 G )取代4 G及,改 變T M G與6 G之比率外,其他同實施例1 6之方法進行 聚合,紡絲。所得纖維之試驗,評估結果如表2所示。聚 合物之6G成分的比率爲8·7重量%。雖然此纖維之 Tma X爲8 5°C以下,9 5Τ:,60分鐘下進行染色時 ’抽空率超過7 0%,但乾洗堅牢度爲非常差之1級。又 ’纖維之熔點爲2 1 °C之較低値,因此進行假撚加工等加 工時,絲會熔著於加熱器上而無法進行加工。 〔比較例1 6〕 除了以環己烷二甲醇(以下簡稱爲C 6 — 2 G )取代 4 G及改變T M G與C 6 - 2 G之比率外,其他同實施例 1 6之方法進行聚合,紡絲。結果如表2所示。C 6 — 2 G成分之比率爲1 2 · 6重量%。又,此絲之彈性率爲 24g/d,彈性回復率爲34%,Q/R値爲〇 · 71 ,故不符合式(1 )。由此絲而製得之布料缺乏彈性回復 本紙張尺度適用中國國家).?卑(CNS ) ( 21〇> j; f ~~aqZ~ 568965 五、發明説明(47 ) 性。另外,纖維之T m a X爲6 2 °C,9 5 °C,6 0分鐘 下進行染色時,會使布料收縮變硬。 〔比較例1 7〕 ’除了以乙二醇(以卞簡稱爲2 G )取代4 G及改變 T M G與2 G之比率外,其他同實施例1 6之方法進行聚 合,紡絲。結果如表2所示。所得聚合物會變黃,所得纖 維之b値亦爲1 8 · 3的黃色,因此無法使用於需具有白 度之內衣等用途。 〔實施例2 2〕 利用實施例1 6之聚酯纖維及2 1 0旦之勒依卡(旭 化成工業製的聚尿烷系伸縮纖維)製成經編物。此編物之 編成規格爲2 8 G,聚酯纖維之束長爲1 〇 8 Omm/ 480回,伸縮纖維爲1 1 2mm/480回,投梭密度 爲90回/英寸。另外,聚酯纖維之混率設定爲75·5 %。 對所得生機進行9 0 °C,2分鐘無張力洗淨處理後, 進行1 6 0°C,1分鐘的乾熱固定處理。接著於存在泰阿 尼庫斯黑BG—FS (泰斯塔日本公司製分散染料) 8%〇wf ,染色助劑之尼卡散索魯特1200 〇·5 g / 1之情形下,於經乙酸調整而使p Η爲6,浴比1 ·· 30下進行9 5 °C,6 0分鐘染色處理。 所得染色製品之黑色明亮度L値爲1 1 . 7 ,能充分 本紙张尺度適用中Ϊ國家^^ ( CNS ) AAn]i^ (Τί〇77^Λ/; ! ~5〇Τ' 568965 五、發明説明(48 ) 顯色。染色製品之物性爲,洗濯堅牢度5級,濕摩擦堅牢 度4級’耐光堅牢度4級,並且具有柔軟性及豐富的伸縮 感及擴張,腰身等質感。 〔比較例1 8〕 爲了比較,同實施例2 2利用一般法所紡成之尼龍6 纖維與勒依卡製成經編物,並使用酸性染料之卡揚隆黑 B G L (日本化藥公司製的酸性染料)7 % 〇 w f進行 9 5 °C,6 0分鐘的染色處理。所得染色製品之L値爲 1 2 · 3。此布料之耐光堅牢度爲2至3級。 / · 〔實施例2 3〕 以實施例1 6所製得之7 5 d / 3 6 f的聚酯纖維爲 經絲,以7 5 d / 4 4 ί之銅氨人造絲爲緯絲,以製成平 織物(織密度中經1 4 0條/ 2 5 . 4 m m,緯8 0條/ 2 5 . 4. m m )。利用常法對此平織物進行洗淨處理,絲 光處理。此絲光處理一般係於常溫下,浸泡於7 5 %之氫 氧化鈉水溶液中進行。中和,水洗,1 8 0 t,3 0秒之 加壓固定後,於不使用·載液之情形下,進行分散染料及反 • / 應染料之一段一浴染色處理。所使用之分散染料爲卡揚隆 聚酯藍一BRSF (日本化藥公司製,分散染料),反應 染料爲得里馬雷藍一 X — S GN (三得公司製,反應染料 )。又,將染色加入使用分散劑之提斯巴一 T L (明成化 學公司製)1 g / 1之添加硫酸鈉5 0 g / 1 ,碳酸鈉 -11 11- - - 1 : - _ - · 11 I - ,4:'-、 ------ ------- ------- ------ --- n^i ^ J 、^乃 、=口 («先1^)-¾^:而之;i息t項項寫本Β ) 本紙张尺度適用中國國家;[|專(cns ) Λ4η:仏.(21〇X ?~ ? :、、h ) - 51 - 568965 Λ7 五、發明説明(49 ) I m —II ---—....... n I -- - —Is I—I I-------------- \~w- ,、^v 、-0 (^1間:而之/i^d.-T項·-¾切寫本 Ή ) 1 5 g / 1而將p Η調整爲1 1的水溶液中,以作爲染液 。並於染料濃度2 % 〇 w f ,浴比1 : 5 0下進行9 5 °C ,1小時染色。染色後於得藍阿普P (三洋化成公司製的 非離子性表面活性劑)1 g / 1 ,浴比1 : 5 0下進行 8 0 °C,1 0分鐘的皂洗處理。染色後並利用常法進行加 工。 * 所得染色物除了可均勻染色外,還具有柔軟觸感及乾 爽感,即具有目前織布所未有的良好質感。染色物之K/ S爲22 · 7 ,乾洗堅牢度爲3至4級,濕摩擦堅牢度爲 4級,耐光堅牢度爲4級。 又,使用實施例1 6所製得之7 5 d / 3 6 f的聚酯 纖維爲經,緯絲,以製成平織物,並進行染色加工。,所得 布料雖不具乾爽感,但極柔軟,布料之緯方向上具有7 % 程度的拉伸1生。 〔實施例2 4〕 將實施例1 6之聚酯纖維撚成3 0 0 T / m後,利用 滾筒附糊以作爲經絲,又,以二乙酸鹽(1 0 0 d / 1 5 0 f )爲緯絲,以製成平織物(經1 2 0條/ 25· 4mm,緯 80 條/ 25 · 4mm)。 * 聚酯纖維用之分散染料爲卡揚隆聚酯藍一3RSF( 日本化藥公司製),二乙酸鹽用之分散染料爲卡揚隆飛斯 特藍一 RD200 (日本化藥公司製)。又,染料濃度各 爲5 % 〇 w ί ,並於弱酸性,存在分散劑下進行9 5 °C之 本纸張尺度適;則國噚家枒冬(CNS ) AW:仏(210x :、丨;) _ 52 _ 568965 五、發明説明(5〇 ) 一段一浴染色。染色後利用蘇打灰1 g / 1 ’非離子洗淨 劑0 · 5g/l之弱鹼浴進,行7〇°C,20分鐘的皂洗 處理。結果所得染色物之K / S爲2 2 · 2,故爲優良品 。另外,染色物之乾洗堅牢度爲3至4級,耐光堅牢度爲 4級,且觸感柔軟及具有優良之鮮明性。 〔實施例2 5〕 於2 2 0 °C下利用D Μ T 1 1 7 0重量份,間苯二 酸二甲酯130重量份,TMG 763重量份,鈦四丁 氧化物1·3重量份進行酯交換後,加入三甲基亞磷酸鹽 0 · 01重量份,並於260 °C,減壓度爲 0 · 5 t 〇 r r下進行聚縮合,得聚合物。所得聚合物之 極限黏度爲0 · 8。又,利用N M R測定之聚合物中的間 苯二酸成分爲6 . 2重量%。 使所得聚合物片乾燥後,利用具有3 6個圓剖面之孔 (直徑0 · 2 3 m m )的紡口,以紡絲溫度2 6 5 °C,紡 絲性速度1 2 0 0 m / m i η進行紡絲,以製成未延伸絲 經滅部中史栉冷妁h.T-消於合竹讧印奴 。其次於熱滾軸6 0 °C,熱板1 4 0 °C,延伸倍率2 · 9 倍,延伸速度6 0 0 m / m i n下對所得未延伸絲進行延 撚,得5 0 d / 3 6 f之延伸絲。結果纖維之物性爲,熔 點 219°C,Tmax l〇0°C,強度 3 · 5g/d , 延伸度4 3 % ’ U % 1 · 〇 %,彈性率2 4 g / d,彈 性回復率8 2 %,b値7 · 6。又,纖維之q / R値爲 0 · 2 9,故符合式(1 )。此實施例之聚酯纖維的 I、紙張尺度適用中國國家^準(CNS ) Λ圳仏—— 568965 A'/ ________ — ΙΓ 五、發明説明(51 ) 9 5°C,6 0分鐘之分散染料的抽空率爲8 1%,顯示其 具有高抽空率。由染色後之一 口編物的乾洗堅固性得知, 此染色物不退色,液污染爲3級。另外,染色物之染色堅 牢性方面則具有良好之耐光堅牢度(4至5級),乾,濕 摩擦堅牢度(.5級),洗濯堅牢度(5級)。 〔實施例2 6〜3 1〕 除了變更二羧酸衍生物之種類外,其他同實施例2 5 之方法進行聚合,紡絲。結果如表3所示。由內容得知任 何一種纖維均·爲符合式(1 )之纖維,且具有良好之染色 性,堅牢性,諸物性。 · 〔比較例1 9 ,2 0〕 除了改變間苯二酸二甲酯之共聚合比率外,其他同實 施例2 5。所得纖維之試驗,哥估結果如表3所示。因比 較例1 9之共聚合比率過低,故纖維之染色性較差,又… 比較例2 0之共聚合比率過高,故降低乾洗堅牢性。 本紙張尺度適用中國國家柃绛(CNS ) A川( 210 X ) . 54 568965 A 7 五、發明説明(52 ) JD v〇 un cn OQ 〇6 VO cr; un 1 MD DC堅牢 度 CO 寸 c〇 CO cn cn m 寸 τ·__·Η 抽空率 g 5S in m 〇〇 VO S 芝. MD CTn g 〇 oo p 1- -Η cs i—H CN 1 扁 Tmax P g 1 Η g r—H vo CSJ On ON oo v〇 oo u〇 OO g r ~· Η ON <〇 〇 〇 o OO CNI c5 cn CO o ON O r—H CN vo CN c5 o 彈性回 復率 岂 •CO oo m oo g M3 OO S5 ON oo o 彈性率 s25 (Nl CO cn Csl csj CO csl 2 延伸率 g CO ζ} OQ 1—tH o 強度 运 v25 wn … wn cn CN CN 極限黏度 /~\ \_/ ο 5S c5 l〇 o g o r- o g o g o g o 熔點 〇〇 >w/ CNl VO CS1 csi Csl CN * CN CN o Csl CN Csl VO csi csl 共聚合成分 重量% Οί νο 04 VO 寸· 〇· cn oo OO m o4 \ i 種類 11 m 11 擀餾 gE Ε- 間苯二酸二 甲酯 間苯二酸二 甲酯 1 1 M 根 ffi- 11 氍 11 ίΏ氍 癸二酸二甲 酯 1,4-環己烷 二羧酸 間苯二酸二 甲酯 間苯二酸二 甲酯 實施例25 實施例26 實施例27 實施例28 實施例29 實施例30 實施例31 比較例19 比較例20 、11 本纸张尺度適用中國國家朽率(CNS ) Λ4化仏(2】0> ) _ 55^ 568965 五、發明説明(53 ) · 〔參考例2〕 除了不用三甲基磷酸鹽外,其他同實施例2 9。雖然 所得纖維之纖維物性未改變,但纖維之b値爲1 2 · 3, 即稍爲變黃。 〔實施例3 2〕 利用實施例2 5之聚酯纖維及2 1 0旦之勒依卡(旭 化成工業製聚尿烷系伸縮纖維)製成經編物。編成規格爲 28G ’聚酯纖維之束長爲i〇8〇mm/480回,伸 縮纖維爲1 1 2mm/4 8 0回,投梭密度爲9 0回/英 吋。又,聚酯纖維之混率設定爲7 5 · 5 %。 對所得生機進行9 0 °C,2分鐘的無張力洗淨,再進 行1 6 0 °C,1分鐘的乾熱固定。其後於存在泰阿尼庫斯 黑BG - FS (泰斯塔日本公司製分散染料)8%owf ’染色助劑之尼卡散索魯特1 2 0 0 (日華化學公司製染 色助劑)0 · 5 g / 1之情形下,於p Η經乙酸調整爲6 ,浴比1 : 3 0下進行9 5 X:,6 0分鐘的染色處理。 所得染色製品之黑色明亮度L値爲1 1 · 3 ,能充分 顯色。又,染色物之洗濯堅牢度爲5級,濕摩擦堅牢度爲 4級,耐光堅牢度爲4級。另外,染色物具有柔軟性及豐 富的伸縮感,且具有擴張及腰身之質感。 〔實施例3 3〕Γ ~ — ^ 1P V. Description of the invention (46) t Comparative Example 1 4] Except changing the ratio of T M G to 4 G, the polymerization was performed in the same manner as in Example 16 and spinning was performed. The physical properties of the obtained fibers were shown in Table 2. The ratio of the 4 G component was 10 · 3% by weight. The fiber dmax is below 8 5 ° C. Although it has a high evacuation rate, the fastness to dry cleaning is very poor. [Comparative Example 15] Polymerization and spinning were carried out in the same manner as in Example 16 except that 4 G was replaced with hexamethylene glycol (hereinafter abbreviated as 6 G) and the ratio of T M G to 6 G was changed. The test and evaluation results of the obtained fibers are shown in Table 2. The ratio of the 6G component of the polymer was 8.7% by weight. Although the Tma X of this fiber is below 85 ° C, 95 ° T: when dyeing at 60 minutes, the evacuation rate exceeds 70%, but the fastness to dry cleaning is very poor. Moreover, the melting point of the fiber is as low as 21 ° C. Therefore, during processing such as false twist processing, the yarn is fused to the heater and cannot be processed. [Comparative Example 16] Polymerization was performed in the same manner as in Example 16 except that 4 G was replaced with cyclohexanedimethanol (hereinafter referred to as C 6-2 G) and the ratio of TMG to C 6-2 G was changed. Spinning. The results are shown in Table 2. The ratio of the C 6-2 G component was 1 2 · 6% by weight. In addition, the elasticity of this yarn was 24 g / d, the elastic recovery was 34%, and Q / R 値 was 0.71, so it did not meet the formula (1). The fabric made from this silk lacks elasticity, and the paper size is applicable to the Chinese country.) (CNS) (21〇) j; f ~~ aqZ ~ 568965 V. Description of the invention (47). In addition, the fiber T ma X is 6 2 ° C, 9 5 ° C, and dyeing at 60 minutes will make the fabric shrink and harden. [Comparative Example 17] 'Except for the replacement with ethylene glycol (referred to as 2 G for 卞) Except for 4 G and changing the ratio of TMG to 2 G, the polymerization and spinning were carried out in the same manner as in Example 16. The results are shown in Table 2. The obtained polymer turned yellow, and the b 値 of the obtained fiber was also 1 8 · The yellow color of 3 cannot be used for underwear and other applications that require whiteness. [Example 2 2] The polyester fiber of Example 16 and the Leica of 2 10 denier (polyurethane system manufactured by Asahi Kasei Industrial Co., Ltd.) were used. Stretching fiber) is made into warp knitting fabric. The knitting specification of this knitting fabric is 2 8 G, the bundle length of polyester fiber is 1.08 Omm / 480 times, the stretching fiber is 1 12 mm / 480 times, and the shuttle density is 90 times / Inches. In addition, the blend ratio of polyester fibers is set to 75.5%. The obtained raw materials are subjected to a 90 ° C, 2-minute tension-free washing treatment, and then to 160 ° C, 1 minute dry heat fixation treatment. Then in the presence of Taianikus black BG-FS (dispersed dyes manufactured by Taistar Japan Co., Ltd.) 8% 〇wf, Nika Sansolut 1200 〇 · In the case of 5 g / 1, p Η was adjusted to 6 with acetic acid, and dyeing was performed at 95 ° C for 60 minutes at a bath ratio of 1 ·· 30. The black brightness L 値 of the obtained dyed product was 1 1 7. It can be used in this paper on the basis of the standard of China ^^ (CNS) AAn] i ^ (Τί〇77 ^ Λ /;! ~ 5〇Τ '568965 V. Description of the invention (48) Color development. Physical properties of dyed products For washing fastness level 5, wet rubbing fastness level 4 'light fastness level 4 and it has softness and rich texture of stretch and expand, waist and other textures. [Comparative Example 1 8] For comparison, the same as Example 2 2 Nylon 6 fiber spun from general method and Leica are used to make warp knitting, and Kayan Long Black BGL (acid dye manufactured by Nippon Kayaku Co., Ltd.) is used at 5% at 9 5 ° C. 60 minutes of dyeing treatment. The L 値 of the obtained dyed product is 1 2 · 3. The light fastness of this cloth is 2 to 3 grades. 2 3] The 7 5 d / 3 6 f polyester fiber prepared in Example 16 was used as a warp, and the 7 5 d / 4 4 之 copper ammonia rayon was used as a weft to make a flat fabric ( In the weaving density, 140 warps / 25.4 mm, and weft 80 warps / 25. 4. mm). This plain fabric is subjected to a washing treatment and a mercerizing treatment by a conventional method. This mercerizing treatment is generally performed at room temperature by immersion in a 75% aqueous solution of sodium hydroxide. After neutralization, washing, 180 t, 30 seconds of pressure fixation, disperse dyes and reactive dyes should be dyed in one bath without using a carrier liquid. The disperse dye used was Kayanlon Polyester Blue-BRSF (dispersed dye manufactured by Nippon Kayaku Co., Ltd.), and the reaction dye was delime blue-X-S GN (made by Suntory Co., Ltd., reactive dye). In addition, 1 g / 1 of Tesba-TL (manufactured by Meisei Chemical Co., Ltd.) using a dispersant was added, and sodium sulfate 50 g / 1, sodium carbonate -11 11---1:-_-· 11 I -, 4: '-, ------ ------- ------- ------ --- n ^ i ^ J, ^ 乃, = 口 («先1 ^)-¾ ^: And; i-item t-scripts B) This paper size is applicable to Chinese countries; [| 专 (cns) Λ4η: 仏. (21〇X? ~?: ,, h)-51- 568965 Λ7 V. Description of the invention (49) I m —II -----....... n I--—Is I—I I -------------- \ ~ w- ,, ^ v, -0 (where ^ 1: and /i^d.-T item--¾ cut script Ή) 1 5 g / 1 and adjust p Η to an aqueous solution of 1 to As a dye solution. Dyeing was performed at 95 ° C for 1 hour at a dye concentration of 2% 〇 w f and a bath ratio of 1: 50. After dyeing, a blue soap P (a nonionic surfactant manufactured by Sanyo Kasei Co., Ltd.) 1 g / 1 was subjected to a soaping treatment at 80 ° C for 10 minutes at a bath ratio of 1:50. After dyeing, processing is performed by a conventional method. * In addition to the uniform dyeing, the obtained dyed material also has a soft touch and a dry feel, that is, a good texture not found in current woven fabrics. The K / S of the dyed material is 22.7, the dry fastness is 3 to 4, the wet rubbing fastness is 4 and the light fastness is 4. In addition, the polyester fibers of 7 5 d / 3 6 f obtained in Example 16 were used as warp and weft to form a plain fabric, and dyeing was performed. Although the obtained cloth does not have a dry feeling, it is extremely soft. The cloth has a stretch of about 7% in the weft direction. [Example 2 4] After the polyester fiber of Example 16 was twisted to 3 0 T / m, a paste was used as a warp yarn, and diacetate (1 0 0 d / 1 5 0 f ) Are weft yarns to make plain fabrics (warp 120/25 · 4mm, weft 80/25 · 4mm). * The disperse dye for polyester fiber is Kayanlon Polyester Blue-3RSF (manufactured by Nippon Kayaku Co., Ltd.), and the disperse dye for diacetate is Kayanlong Feisite Blue-RD200 (manufactured by Nippon Kayaku Co., Ltd.). In addition, the dye concentration is 5% 〇w ί, and the paper is properly sized at 9 5 ° C in the presence of a dispersant under weak acidity; then the country's home winter (CNS) AW: 仏 (210x :, 丨;) _ 52 _ 568965 V. Description of the invention (50) One-stage one-bath dyeing. After dyeing, a weak alkali bath of 1 g / 1 'non-ionic detergent 0.5 g / l in soda ash was used for bathing at 70 ° C for 20 minutes. As a result, the K / S of the obtained dyed product was 2 2 · 2 and was therefore excellent. In addition, the fastness to dry cleaning is 3 to 4 and the fastness to light is 4 and the touch is soft and has excellent sharpness. [Example 2 5] D M T 1 1 70 parts by weight, 130 parts by weight of dimethyl isophthalate, 763 parts by weight of TMG, and 1.3 parts by weight of titanium tetrabutoxide at 220 ° C After transesterification, 0.01 part by weight of trimethylphosphite was added, and polycondensation was performed at 260 ° C and a reduced pressure of 0.5 t rr to obtain a polymer. The limiting viscosity of the obtained polymer was 0 · 8. The isophthalic acid component in the polymer measured by N M R was 6.2% by weight. After the obtained polymer sheet was dried, a spinning orifice having 36 circular cross-section holes (diameter 0.23 mm) was used at a spinning temperature of 2 65 ° C and a spinning speed of 1220 m / mi. η was spun to make unstretched silk warp in the cold warp hT-Yu-Yuzhu Yinnu. Secondly, the unstretched yarn was twisted at 60 ° C, 140 ° C on a hot plate, 2 · 9 times draw ratio, and 600 m / min draw speed to obtain 5 0 d / 3 6 f's extended filament. Results The physical properties of the fibers were: melting point 219 ° C, Tmax 100 ° C, strength 3.5 g / d, elongation 43% 'U% 1.0%, elastic modulus 24 g / d, elastic recovery rate 8 2%, b 値 7 · 6. Since q / R 値 of the fiber is 0 · 2 9, it satisfies the formula (1). The I and paper dimensions of the polyester fiber in this embodiment are applicable to the Chinese National Standard (CNS) Λzhen 仏 —— 568965 A '/ ________ — ΙΓ 5. Description of the invention (51) 9 5 ° C, 60 minutes of disperse dye The evacuation rate is 8 1%, which shows that it has a high evacuation rate. It is known from the dry-cleaning solidity of one of the knitted fabrics after dyeing that the dyed material does not fade, and the liquid pollution is level 3. In addition, the dyeing fastness of the dyed material has good light fastness (grade 4 to 5), dry and wet rubbing fastness (.5 grade), and washing fastness (grade 5). [Example 2 6 to 3 1] Except that the type of the dicarboxylic acid derivative was changed, the polymerization and spinning were performed in the same manner as in Example 25. The results are shown in Table 3. According to the content, it was found that any fiber is a fiber conforming to the formula (1), and has good dyeability, fastness, and various physical properties. [Comparative Examples 19, 20] Except that the copolymerization ratio of dimethyl isophthalate was changed, the others were the same as those in Example 25. The test results of the obtained fibers are shown in Table 3. Because the copolymerization ratio of Comparative Example 19 is too low, the dyeability of the fiber is poor, and ... The copolymerization ratio of Comparative Example 20 is too high, so the fastness to dry cleaning is reduced. This paper is applicable to China National Standard (CNS) A Sichuan (210 X). 54 568965 A 7 V. Description of the invention (52) JD v〇un cn OQ 〇6 VO cr; un 1 MD DC fastness CO inch c〇 CO cn cn m inch τ · __ · Η Evacuation rate g 5S in m 〇〇VO S 芝. MD CTn g 〇oo p 1- -Η cs i—H CN 1 Flat Tmax P g 1 Η gr—H vo CSJ On ON oo v〇oo u〇OO gr ~ · Η ON < 〇〇〇o OO CNI c5 cn CO o ON O r—H CN vo CN c5 o Flexible recovery rate • CO oo m oo g M3 OO S5 ON oo o Elasticity s25 (Nl CO cn Csl csj CO csl 2 Elongation g CO ζ) OQ 1—tH o Strength v25 wn… wn cn CN CN Limit viscosity / ~ \ \ _ / ο 5S c5 l〇ogo r- ogogogo Melting point 〇〇 > w / CNl VO CS1 csi Csl CN * CN CN o Csl CN Csl VO csi csl Copolymerization weight% 〇ί νο 04 VO inch · 〇 cn oo OO m o4 \ i Type 11 m 11 Rolling gE Ε-dimethyl isophthalate dimethyl isophthalate 1 1 M root ffi- 11 氍 11 ίΏ 氍 sebacate dimethyl 1,4-cyclohexanedicarboxylic acid dimethyl isophthalate Isophthalic acid Dimethyl Example 25 Example 26 Example 27 Example 28 Example 29 Example 30 Example 31 Comparative Example 19 Comparative Examples 20 and 11 The paper size is applicable to the Chinese National Decay Rate (CNS) Λ4Chemical (2) 0 >) _ 55 ^ 568965 V. Description of the invention (53) · [Reference Example 2] Except that trimethyl phosphate is not used, the same as in Example 2 9. Although the fiber physical properties of the obtained fiber are not changed, b 値 of the fiber is 1 2 · 3, which is slightly yellowed. [Example 3 2] The warp knitted fabric was made of the polyester fiber of Example 2 5 and 2 100 denier ika (polyurethane stretchable fiber manufactured by Asahi Kasei Industrial Co., Ltd.). . The bundle length of 28G 'polyester fiber is 108mm / 480 times, the stretch fiber is 112mm / 480 times, and the shuttle density is 90 times / inch. The mixing ratio of the polyester fibers was set to 75.5%. The obtained vitality was washed at 90 ° C for 2 minutes without tension, and then fixed at 160 ° C for 1 minute. After that, there existed Tayanikus Black BG-FS (disperse dyes made by TESTA Japan Co., Ltd.) 8% owf 'dyeing aid of Nika Sansolut 1 2 0 0 (dyeing aid made by Nichiwa Chemical Co., Ltd. ) In the case of 0.5 g / 1, the dyeing treatment was performed at 9: 5 X: for 60 minutes at pΗ with acetic acid adjusted to 6 and a bath ratio of 1:30. The blackness L 値 of the obtained dyed product was 1 1 · 3, which was sufficient for color development. In addition, the washing fastness of the dyed matter is 5th grade, the wet rubbing fastness is 4th grade, and the light fastness is 4th grade. In addition, the dyed material has softness and rich stretch feeling, and has the texture of expansion and waist. [Example 3 3]
於220°C下利用DMT 1300重量份,TMG 1、纸张尺度適用中國國r;if準(cns ) ^Γ(1Τ〇77^7:χ}' ϋΤ— — -------- ^先間^^:而之/1总和^Utilizing 1300 parts by weight of DMT at 220 ° C, TMG 1, paper size applies to China; if quasi (cns) ^ Γ (1Τ〇77 ^ 7: χ} 'ϋΤ — — -------- ^ Xianma ^^: And the sum of / 1 ^
V 本TJC 、1Τ 經潆部中史桴沒局Μ工消资合Μ社印於 568965 五、發明説明(6〇 ) 具有柔軟性之纖維素材。 因具有上述性能,因此,本發明之聚三甲撐對苯二甲 酸酯系纖維適用爲,製造與聚尿烷彈性纖維所代表之伸縮 纖維’羊毛,絲綢,乙酸鹽等耐熱性較低之纖維素材,或 常壓下可染色之纖維素纖維等混用布料之堅牢染色物的纖 維材料。即’與前述低耐熱纖維混用後所製成的布料製品 能&不損及纖維特性之情形下利用汎用常壓設備以簡單方 法製造堅牢染色布料,此乃本發明對產業上所具有的特徵 效用。 本紙張尺度適用中國國CN\S ) Λ4川仏(2】0, : G )V. TJC, 1T, printed by the Ministry of History, China, Japan, Japan, Japan, 568965, etc. 5. Description of the invention (60) Fiber material with softness. Due to the above-mentioned properties, the polytrimethylene terephthalate fiber of the present invention is suitable for the production of stretchable fibers such as wool, silk, and acetate, which are represented by polyurethane elastic fibers. Fiber materials, or cellulose fibers that can be dyed under normal pressure, such as fibrous materials, which are used to firmly dye fabrics. That is, 'the cloth product made by mixing with the aforementioned low heat-resistant fiber can & without impairing the fiber characteristics, use a general-purpose normal pressure equipment to manufacture a firmly dyed cloth in a simple method, which is the industrial characteristic of the present invention utility. This paper size applies to China CN \ S) 44 川 仏 (2】 0,: G)
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TW87114836A TW568965B (en) | 1997-09-10 | 1998-09-07 | A polyester fiber and fabric made thereof |
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1998
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