TW201040333A - Manufacturing method of cellulose fiber - Google Patents

Abstract

The present invention provides a manufacturing method of cellulose fiber, which can produce uniform cellulose solution at low temperature, and can further produce fiber by using the said cellulose solution. The processing method is mainly to dissolve little amount of cellulose powder in the liquid concentrated NMMO (N-methyl morpholin N-oxide), so as to reduce the solidification temperature of NMMO, then injecting the low-temperature liquid concentrated NMMO with the dissolved cellulose and the cellulose powder into a kneader, moisten and mix the cellulose in the kneader paste-like shape without depressurizing process, then provide it to an extruder for dissolving it into the uniform state, thereby producing the uniform cellulose solution even at low temperature, and further producing a cellulose product with excellent tenderness and strength.

Description

201040333 九、發明說明： 【發明所屬之技術領域】 本發鴨隸屬-纖維餘之技術領域，制係指即使 :::ss均勾的纖維素溶液，進而利用該纖維素溶液製造纖 【先前技術】 按，纖維素雖然與其他物質的親和力強，但如料分子 :者分，具有由牢_氫鍵形成的結晶結構，使用^的 ^使其轉’能魏_結_製錢較溶 」 (N_methyl ;; 5 ^ 稱NMMO)。 似1此間 • 械強度等特點，故廣泛應用於需以纖維素 • 巧前技術可知，拥氧化？基瑪_製造纖維♦纖維 藝，百先揭露於美國第3447935專利案中。 京纖、，隹的工 ° 4142913 ^ 4144080 ^素f液的製造方法，係利_蒸德溶脹 i==):r素溶液凝固(-=== _onw)(©恶)之後，用擠㈣爾來製造纖 方法利用擠出機，雖缝夠實現溶解卫藝έ化;/ = 過進行預先片（chip)化的先行工藝，所t必須經 量消耗:，且在前體的溫度及濕度的控斤上存要二長的時間，能 術方法’係先製造含水量為5 %〜1 7 %重量3固離 後，再將其㈣核«_起· 201040333 ‘维，再用擠出機將前體溶解，以此來製造 置。且固能气」ίΐ為了運廷和儲存前體需要複雜的冷卻裝 it f基瑪溶劑的製造和保管方面也存在問題。 Ο Ο 以及5_83號美國專利案，其揭=號 ，罝除去水枓中過置的水，以製造纖維素溶液，該 邊進行蒸發、溶解，所以會出現垂直方 肖耗大，由於纖維素的分解及氧化甲基瑪的變色ίί致 g效率性低’因此將此方法用於製造高強度的纖維時存=些 而專利文獻8〜1〇以及6係分別為專利號第5 5456748號，以及5888288號美國專利，其公開之^維素 制 造方法為’使用水平圓筒型高速擾拌機^⑹將^=二 ，板狀漿料和含水量為22%的氧化甲基瑪混合、溶脹f，在= 強制薄膜型蒸發裝置將高雌溶液中的水蒸發， 維素溶液。該方法中’必須另外對製造板狀漿料“ / ，抓_)進行控制，且水平圓筒型高速 ，= 出溶脹溶液等問題。作為解決此問題的方法，=^艮難^ 利號5通75號美國專利），公開了一種錢 :^ $ 201040333 旋推進器（conveyor screw)的水平圓筒型高速攪拌機。 而專利文獻1 2係專利號5948905號美國專利，1 術在於，為了通職含水涵23%的氧⑽ ^ 維素混合物_水蒸發來製造纖維素驗，—邊在減壓下= 秦發。該方法中包括多級艙室（chamber)。該專利的方法 ） -個擒室(chamber)中的喷嘴的直徑大、孔(h〇le)的數 Ο Ο 舱室的級數增加，喷嘴的直徑變小、孔的個數則變多，由择 加溶液的蒸發截面積’以提高水分喊發效率。該專利 乂 開了在最後-級即第8級使麟出機的方法。該方法具有如^ 足：各餘室的構成全部不同，用於驗室_移的螺旋^ 空處理程序過多，裝置變得複雜。 °°汉具 而專利文獻1 3係P CT國際公開w〇97/4779〇號真 料，其係在雙螺桿型擠出機中將纖維素粉末直接溶解於液態氧= 。曱基瑪溶劑，以製造雜素溶液的方法。在該方法巾，在保持 。(:的溫度下向該擠出機的第—個機筒(barrel)注人含水 %的液態氧化曱基碼，向調節成7 5t的擠出機其第三個機 供粉末纖維素之後，進行轉送、捏煉，並將溫度升高到工2 從而製，溶液。該方法中需要3個機筒以用於提供纖維素粉末和 乳化甲基碼，亚且為了溶解纖維素，還需要其他的機筒用於 溶解。實際上，因為溶脹和溶解幾乎是同時發生於狹小溶脹區 所以由於漿料粉末的;^全溶脹，導致產生含有未溶解的纖唯 顆粒的纖維素溶液的可能性高。雖然在製造少量的溶液時是， 的，但是在增加纖維素溶液的製造量的情況下，產生大量的未溶 解部分’因而存在必須增加對過濾系㈣投資問題和紡絲週掏變 短的問題。如果增加溶脹區間’則溶解區間變短，存在擠 機筒增加過多的缺點。即使增載入物台⑽⑻’通過增加螺桿的 L/D(length/diameter)，使擠出機的膨脹期間增長，但因為使用 201040333 Ο 同一個驅動軸，所以還是存在很難同時調節溶脹條件和溶解條 的缺點。 U 最後，專利文獻1 4係韓國公開專利2002-24689號專利案， ΐΐ開1以下的方法’使用被_冷空氣過度冷卻的“氧化、甲 基瑪，製作經溶脹的纖維素漿料粉末及液態氧化甲基 人 ^並使其溶解以製造高均勻f的纖維素溶液，但是在使用= ，時’不财能正確地控麵急冷的氧化甲基瑪的溫度，而丄ς 氧化t基瑪為高濃㈣m情含有的水分會凝結 = 能保持氧化甲基瑪的含水量均勻度。 σ 不 曰如上所述，習用創作揭露方法的特點在於，在最 曹 量化和能耗變多等問題’所述裝置例如有為了確 Β夺間來蒸發高減溶液中的水的裝置 箄' 、:留 還提出了使用含有重量約13%的水分驗亩= 解纖維素粉末的方法，但是這種方法存在如 土，、、直接冷 Ο 下缺點 曱基瑪的結晶化度即約8〇。。以上的狀態下 =㊁在2 ^氧化曱基麟纖維素的反應活性過高，導致纖維素不^ 洛脹而直接溶解，從而有朗未溶解成分之缺點’/、 發生 ，態學一^㈣上研究溶_轉的纖維素纖維，結 的厚度等 維素的浸透力存在差異。在財材纖維(贿ι 土= 根據使用的木材纖維的種類和漿 ^ 廷樣的傾向。因此，為了製造均勻的 ，2月匕看到 的溶劑充分地浸透於雜錢軸全部’㈣將所使用 兩王丨面積内，必須使纖維素鬆 201040333 ^差====== 合解的雜素雜。因此，調t的反麟錄成為製賴維纽_重要I乳化甲 【發明欲解決她課題】 现何 作先前技術方法複雜不利於大量生產， 因溶液 Ο Ο ，會發生纖維素分解以及氧化輸i變色等迻成产 切力且全面積地充分浸透於纏維去 低/m低剪 其無限制地溶脹後被溶解。、、·〜、、粗大組織和微細組織内，使 本發明為了解決類以往的問題，， 均勻的纖維素溶液的方法。 Μ 了在低>皿下也可以製造 【發明内容】 纖維ii ，維之®紗法』，該 m〇rph〇lin N-〇xide，簡稱N_〇T^^f=tthyl 低乳化甲基瑪的固化溫度後， ，降 素混合及溶脹，或者使纖維機壓過程地將纖維 將所述糊狀物提供給擠出機 在^^為糊狀物，然後本發明的-個特徵是使二煉^1了溶解。 及溶脹階段，但並不完全溶解.2置在捏煉機内進行混合 糊狀物，之德描银，或者在捏煉機中部分溶解，製作 工藝方法:成2出機。因此，與下述 工藝方法中’為了溶解纖維素，二大量的溶液’所述 素，並且僅使用擠出機，而所述擠基瑪溶解熱 解纖維 混合、溶 201040333 間。同時’與使用低濃度氧化甲基瑪進行混合、溶 相比，本發明具有機械裝置簡單的優點。旻錄置所構成的方法 液的==二最=方二=明均勻的纖维素溶 中溶解曹詈η 步(）’在液態濃縮氧化甲基瑪 溶液；+驟fR、0 Μ二5%的少量纖維素粉未製造氧化甲基瑪 液和纖i素粉有少量的纖維素粉柄氧化曱基瑪溶 Ο Ο #捏煉機，在捏煉軸無減壓過程地將纖維素 液通過紡絲喷嘴擠出紡絲後，通過空氣層 得的複人_1使賊職剌複合絲；以及步驟（D)，對獲 、稷口 4進仃水洗、乾燥和上油處理以及卷取等 根據本發明的另-最佳實施方式，步驟⑻中:祕 :=ί量：〜於 θ根據本备明的另一最佳實施方式，步驟（ ,丨、 態物基瑪™⑽〜提 的纖維素其二二⑷或者步驟⑻ 本發明，通過賴則（_如⑷的水分進行控制， 纖維素粉末化，麵態濃純彳吖基射溶解少量_维+粉 ΐ下==基瑪的固化温度變低。藉此能夠在== i夜在：ίί谷液提供給捏煉機，纖維素粉末和氧化甲基瑪 絲機内以低溫狀態順利地進行混合及溶脹。纟从 ’皿、氧化$基瑪溶液時，由於在初期混合及溶脹過程令纖維 201040333 Ο201040333 IX. Description of the invention: [Technical field to which the invention pertains] The present invention relates to the technical field of the fiber-to-fiber, and the system refers to a cellulose solution even if::ss is hooked, and then the cellulose solution is used to manufacture the fiber. 】 According to the cellulose, although the affinity with other substances is strong, but the material molecule: the minute, has a crystal structure formed by the strong hydrogen bond, using ^ ^ ^ to turn 'can Wei _ knot _ money is more soluble" (N_methyl ;; 5 ^ called NMMO). Similar to the characteristics of the mechanical strength, it is widely used in the need for cellulose. JIMA _ Manufacture of fiber ♦ fiber Art, Bai Xian was exposed in the US Patent No. 3,447,935. Jingfei, 隹 隹 ° 4142913 ^ 4144080 素 f f liquid manufacturing method, _ _ steam swell i ==): r solution solution solidification (-=== _onw) (© evil), after squeezing (four) Erlai's method of making fiber uses an extruder, although it is enough to achieve dissolution and sanitation; / = the advance process of pre-chip, t must be consumed: and the temperature and humidity of the precursor The control of the pound must last for two long periods of time. The method can be used to make the water content of 5% to 1.7 % by weight. After the solidification, the (four) core «_起· 201040333 'dimensional, and then extruded The machine dissolves the precursor to make it. And solid energy gas has a problem in the manufacture and storage of the solvent and the storage of the precursor. Ο Ο and U.S. Patent No. 5_83, which discloses that the water in the leeches is removed to produce a cellulose solution, which is evaporated and dissolved, so that the vertical square is consumed, due to the cellulose The disintegration and the discoloration of the oxidized methyl group are low in efficiency. Therefore, this method is used for the production of high-strength fibers, and the patent documents 8 to 1 and 6 are respectively patent No. 5 5456748, and U.S. Patent No. 5,888,288, the disclosure of which discloses the method of manufacturing a sulphate using a horizontal cylindrical high-speed scrambler ^(6), a plate-like slurry and an oxidized methyl group having a water content of 22%, and swelling In the = forced film type evaporation device to evaporate the water in the high female solution, the vitamin solution. In this method, 'there must be additional control for the manufacture of the plate-like slurry", and the horizontal cylindrical type is high-speed, and the swelling solution is solved. As a method for solving this problem, =^艮难^利号5 U.S. Patent No. 75, discloses a horizontal cylindrical high-speed mixer of the type: 201040333 Conveyor screw. Patent Document 1 2 is a U.S. Patent No. 5,948,905, and the operation is based on Aqueous culvert 23% oxygen (10) ^ vitamin mixture _ water evaporation to produce cellulose test, while under reduced pressure = Qinfa. The method includes a multi-stage chamber. The method of this patent) - a diverticulum The diameter of the nozzle in the chamber is large, the number of holes (h〇le) is increased, the number of stages of the chamber is increased, the diameter of the nozzle is reduced, and the number of holes is increased, and the evaporation cross-sectional area of the selective solution is Improve the efficiency of water shouting. This patent breaks the method of getting out of the machine at the final level, that is, the eighth level. The method has the same formula: the composition of each chamber is different, and the spiral for the chamber _ shift ^ There are too many empty processing programs and the device becomes complicated. °°Han and Patent Document 1 3 P CT International Publication No. 97/4779, which is a method in which a cellulose powder is directly dissolved in a liquid oxygen = hydrazine solvent to produce a heterogeneous solution in a twin-screw extruder. Method towel, at the temperature of (. at the temperature of the extruder, the first barrel of the extruder is filled with the liquid oxidized ruthenium base code, and the third machine is adjusted to the extruder of 7 5t. After the powdered cellulose is supplied, it is transferred, kneaded, and the temperature is raised to the solution 2, which requires 3 barrels for providing the cellulose powder and the emulsified methyl code, and to dissolve Cellulose, other barrels are needed for dissolution. In fact, because swelling and dissolution occur almost simultaneously in a narrow swelling zone, due to the full swelling of the slurry powder, a fiber containing undissolved fibrils is produced. The possibility of a solution is high. Although it is in the case of manufacturing a small amount of solution, in the case of increasing the amount of the cellulose solution produced, a large amount of undissolved portion is produced', so there is a need to increase the investment problem for the filtration system (4) and spinning Silk circumference becomes shorter Problem. If the swelling interval is increased, the dissolution interval becomes shorter, and there is a disadvantage that the extruder barrel is excessively increased. Even if the loading stage (10) (8)' is increased by the L/D (length/diameter) of the screw, the expansion period of the extruder is made. Growth, but because of the use of 201040333 Ο the same drive shaft, there are still some disadvantages that it is difficult to adjust the swelling conditions and the dissolution strip at the same time. U Finally, Patent Document 1 4 is a Korean Patent Publication No. 2002-24689, which is opened below 1 Method 'Using oxidized, methyl methacrylate, which is overcooled by cold air, to make a swollen cellulose pulp powder and a liquid oxidized methyl group and dissolve it to produce a highly uniform f cellulose solution, but in use = , when 'no money can correctly control the temperature of the surface of the oxidized methyl ketone, and 丄ς oxidize t kema is high concentration (four) m moisture containing water will condense = can maintain the water content uniformity of oxidized methyl. σ As described above, the conventional method of creating a disclosure method is characterized in that the device is subjected to the most quantitative and energy consumption problems, for example, the device has a device for evaporating the water in the high-reduction solution in order to surely usurp, : Retention is also made to use a method containing a moisture content of about 13% by weight to determine the cellulose powder, but this method exists as soil, and the degree of crystallization of the 曱 曱 玛 即 is about 8 〇. . In the above state = two in 2 ^ cerium sulfhydryl cellulose reactivity is too high, resulting in cellulose does not swell and directly dissolve, so that there are shortcomings of the lansin dissolved components / /, occur, state one ^ (four) On the study of the dissolution-transfer cellulose fibers, the thickness of the knots is different in the permeability of the vitamins. In the material of the material (bribe = soil = according to the type of wood fiber used and the tendency of the slabs of the slabs. Therefore, in order to make a uniform, the solvent seen in February is fully saturated with the junk shaft. In the area of the two kings, it is necessary to make the cellulose loose 201040333 ^ poor ====== the miscellaneous miscellaneous miscellaneous. Therefore, the reverse transcription of t is the system of Lai Weixin _ important I emulsification A [invention to solve Her subject] What is the previous technical method is not conducive to mass production, due to the solution 纤维素 Ο, cellulose decomposition and oxidation and discoloration will occur, and the whole area will be fully saturated in the entanglement to lower / m low The present invention is a method for dissolving a uniform cellulose solution in order to solve the conventional problems, and to dissolve it in an unrestricted manner, and to dissolve it in a large amount and in a fine structure. It is also possible to manufacture [invention] fiber ii, weizhi® yarn method, the m〇rph〇lin N-〇xide, abbreviated as N_〇T^^f=tthyl, after curing temperature of low-emulsification methylma, Mix and swell, or make the fiber press process The paste is supplied to the extruder as a paste, and then the feature of the present invention is that the two melts are dissolved. And the swelling phase, but not completely dissolved. 2 is placed in a kneader for mixing. The paste, the German silver, or partially dissolved in the kneader, the production process: 2 out of the machine. Therefore, in the following process, 'in order to dissolve the cellulose, two large amounts of the solution' And only the extruder is used, and the extruded keima dissolves the pyrolysis fibers to be mixed and dissolved between 201040333. At the same time, the invention has the advantage of simple mechanical means compared with mixing and dissolving with a low concentration of oxidized methyl ketone. The method liquid composed by the recording method == two most = square two = clear uniform cellulose dissolved in Cao 詈 step () 'concentrated oxidized methyl methine solution in liquid; + sfR, 0 Μ two 5% A small amount of cellulose powder is not made of oxidized methyl ketone liquid and fibrin powder. There is a small amount of cellulose powder sputum yttrium yttrium yt Ο 捏 # kneader, the cellulose liquid is passed through the kneading shaft without decompression process After the spinning nozzle is extruded and spun, the reptile _1 composite yarn is obtained through the air layer And step (D), washing, drying and oiling treatment, and coiling, etc., according to another preferred embodiment of the present invention, in step (8): secret: = ί: θ according to θ Another preferred embodiment of the present invention, the step (, 丨, 基 基 TM TM TM TM 提 提 提 提 提 提 提 纤维素 纤维素 纤维素 纤维素 纤维素 纤维素 纤维素 或者 或者 本 本 本 本 本 本 本 本 本 本 本 本 本 本 本 本 本 本 本 本 本 本 本 本 本 本 本Powdered, the surface of the concentrated pure ruthenium base dissolves a small amount of _ dimension + powder = == jima's curing temperature becomes lower. This can be supplied to the kneader, fiber at == i night: ίί谷液The powder and the oxidized methyl marsh machine are smoothly mixed and swelled at a low temperature. When 纟 from the dish, the oxidized $ Sigma solution, due to the initial mixing and swelling process, the fiber 201040333 Ο

G 素粉末或粉末固塊的表面急劇溶脹及溶解，會發生轤 凝聚現象。不僅如此，因為只她塊的表面溶== 内侧的粉末被溶解需要長時間，以至可能產生未溶解部分。但是， 根據發明的方法，使用在液態濃縮氧化甲基瑪中溶解有少量的纖 維素粉末的氧化甲基瑪時，通過氧化甲基瑪的固化溫度變低的效 杲，可以在低溫狀態下定量地注入氧化曱基瑪以進行混合，從而 能夠防止在纖維素粉末或粉末固塊的表面急劇地生成夕α卜膜。由 此，即使在低溫下也能夠製造均勻的纖維素溶液，所以可以在纺 絲時使用低溫均⑽齡素溶液，財卩制在擠出_纖维素在古 分解的特性’從而能夠製造出柔軟性和嶋異的纖: 本ί明中，可以將低比重職料簡單地注人到本 以及纖維素成型品生產量，通過直接注入重量約㈡= ΐίϊΓ基瑪，無需另外的減壓式水分蒸躲置，從而使裝置姓 構父件間早。同時，通過調節粉末狀的纖維素的大小和“ ί服i溶解ΐ形，避免因此導致纖維素形成未溶解的纖維素顆粒 *在捏煉機 •給雙軸擠 螺旋或所需盤(needing disk)的插人最小化？…「，能夠將反 粉末狀的纖維素之__而造成只麵維素的ί膜 狀。所以，篩檢程式的改換週期變短。進—步^ 中溶脹的纖維素糊狀物，在將體積最小化煉機 出機，可以減少雙軸擠出機内的螺桿排列的負^。即μ雙軸擠 素溶液的滞留時間的“窄，纖的， 利用在捏煉機巾持續顧剪切力財冑的 〜同蚪’ 溶解時間和溶解溫1，使原來的漿料聚合“、^夠降低 此能夠保持為高的分子量。藉此依據本發“ ς為 出具有優異物理性質的纖維素纖維。 、/ ，此夠a造 【實施方式】 201040333 兹為使魏進-步瞭解本發明之結構設計及 式再予說明於后： 2下請f考附圖對本發明進行具體地說明。 垂第1圖是概略地說明作為本發明的實施例的製程步驟圖，該 二施例中，在氧化曱基瑪中溶解少量纖維素，並在低溫下製造均 勻的纖維素溶液。 麻I 所使㈣纖維素粉末，使用帶刀桿的粉碎機成型粒 Ο Ο ± 之粉末，並焉選500//m以下。若粉末的粒徑超過 日難在捏煉機喊行穩狄分散，並且存在溶服需要 、首先，在濃縮液態氧化甲基瑪中溶解少量粒徑5000//m以下 素粉末。相對於濃驗·化甲基瑪，_素粉末的含量 ^重罝Ojl%〜5%，較佳設計為重量〇· 1%〜3%。纖維素粉末的含 里小於重量0. 01,%時，氧化甲基瑪的固化溫度的降低效果微小 ^性沒有幫助，與此關，如敎於重量5%，職化甲基瑪溶 f的粘度增大，在捏煉機内進行混合、溶脹所需的時間長。之後， ，用了般的方法對濃度為重量·〜3嶋氧化甲基瑪溶液進行濃 縮丄製作成含水量為$量⑽〜18%的濃驗態氧化f基瑪。當含 水ϊ小於10%時，費用增加，從而在成本方面不利，如果含水量大 於m ’則溶解性下降。織將溶解有少量齡素粉末的氧化甲基 ，溶液保持在5(TC〜95°C並注人到捏煉機中。接著’在捏煉機二 二減壓過程地職維素混合及雜，製佩錄，再提供給擠出 義：，使其在均勻狀態下溶解，從而製造均勻的纖維素溶液。 上述y里浴~於氧化曱基瑪之纖維素粉末，可以透過齒輪 或螺桿式供料機將溶解有少量該纖維綠末的氧化ψ基瑪溶 供給捏煉機，最佳方式係利用螺桿式供料機注入到捏煉機中。 ^上述在該捏煉機内混合及溶脹的纖維素溶液中，根據纖維素 聚合體的聚合度，相縣態輸Ψ基瑪，將轉素粉末的含量的 12 201040333The surface of the G powder or the powder solid swells and dissolves abruptly, and enthalpy condensation occurs. Not only that, because only the surface of her block is dissolved == the inner powder needs to be dissolved for a long time, so that an undissolved portion may be produced. However, according to the method of the present invention, when an oxidized methyl group in which a small amount of cellulose powder is dissolved in a liquid concentrated oxidized methyl group is used, the effect of lowering the curing temperature of the oxidized methyl group can be quantified at a low temperature. The cerium oxide base is injected to carry out mixing, so that it is possible to prevent the formation of a film on the surface of the cellulose powder or the powder solid. Thereby, even if a uniform cellulose solution can be produced even at a low temperature, it is possible to use a low-temperature (10)-n-nose solution at the time of spinning, and it is possible to manufacture a characteristic of the extrusion-cellulose in the ancient decomposition. Softness and strange fiber: In this case, the low-specific gravity material can be easily injected into the production of this and the cellulose molded product, and the direct injection weight is about (2) = ΐίϊΓ基玛, no additional decompression type moisture is needed. Steaming and hiding, so that the device surnamed the parent is early. At the same time, by adjusting the size of the powdered cellulose and "dissolving the ΐ shape, avoiding the cellulose to form undissolved cellulose particles* in the kneader; giving the biaxial extrusion spiral or the required disk (needing disk) ) The insertion is minimized?...", it is possible to make the anti-powdered cellulose __ a film that is only venetian. Therefore, the change cycle of the screening program becomes shorter. Swelling in the step ^ Cellulose paste, which minimizes the volume of the extruder, can reduce the negative arrangement of the screw arrangement in the twin-screw extruder. That is, the retention time of the μ biaxially extruded solution is "narrow, fibrous, utilized in pinching. The refining machine towel continues to take care of the shearing force of the same kind of dissolution time and the dissolution temperature of 1, so that the original slurry polymerization ", ^ can reduce this can maintain a high molecular weight. Cellulose fibers having excellent physical properties. [Embodiment] 201040333 In order to make Wei Jin-step understand the structural design and formula of the present invention, the present invention will be specifically described below. BRIEF DESCRIPTION OF THE DRAWINGS Fig. 1 is a schematic view showing a process step as an embodiment of the present invention, in which a small amount of cellulose is dissolved in cerium oxide and a uniform cellulose solution is produced at a low temperature. Hemp I (4) Cellulose powder, using a pulverizer with a shank to form a powder of 粒 Ο ±, and select 500//m or less. If the particle size of the powder exceeds the daily difficulty, it is required to be dispersed in the kneader, and there is a need for dissolution. First, a small amount of powder having a particle diameter of 5000//m or less is dissolved in the concentrated liquid oxidized methyl group. The content of the _-powder powder is from 罝Ojl% to 5%, preferably from 〇·1% to 3%. When the content of the cellulose powder is less than the weight of 0.01%, the effect of reducing the curing temperature of the oxidized methyl group is not helpful, and if it is less than 5% by weight, the methylation of the methyl group is f The viscosity is increased, and the time required for mixing and swelling in the kneader is long. Thereafter, the concentrated oxidized methyl group solution having a concentration of ~3 嶋 is concentrated in a conventional manner to prepare a concentrated oxidized f-kima having a water content of (10) to 18%. When the water content is less than 10%, the cost is increased, which is disadvantageous in terms of cost, and if the water content is more than m', the solubility is lowered. Weave the oxidized methyl group which will dissolve a small amount of aging powder, keep the solution at 5 (TC~95 °C and inject it into the kneader. Then 'mix in the kneading machine two or two decompression process , made by the extrusion, and then provided to the extrusion: it is dissolved in a uniform state to produce a uniform cellulose solution. The above y-bath ~ cellulose powder of yttrium yttrium can be transmitted through a gear or screw The feeder supplies a cerium oxide base dissolved in a small amount of the fiber green to the kneader, and the best mode is injected into the kneader by a screw feeder. ^The above mixing and swelling in the kneader In the cellulose solution, according to the degree of polymerization of the cellulose polymer, the phase of the state of the kiln, the content of the transgenic powder 12 201040333

漠度設定為重量5¾(〜9Λα/ A 内的纖維素粉末含量小。如果捏煉機 與此不同’如果大於20%，則難的物理性質， 不能得到均勻的溶液。、 〜、氧化甲基瑪進行溶解，從而 根據本發明，在步驟 然後在捏練機内無_過程地素洛液注入捏煉機， 之後，提供給擠出機，使脹，製作成物狀 的纖維素溶液。此時所换用狀您下洛解，從而製作均勾 Ο Ο ，的範圍内。如果機筒少二^l/d在12 纖維素溶液通過機筒的時間短，宏It /D小於12，則 如果機筒多於16個或者螺桿生未/谷解部分。與此不同， 力過大，有可能發生螺桿變形的情況。於64，則作用於螺桿的應 粉末中的弋)驟⑻的纖維素 混入諸如聚乙稀醇、雙乙梳取、冬成型物以功能性，可以 碳或者氯化解的添加劑。/者物-氧化鈦、二減石夕、 (ι)=;ί 裝通過乳報（5)之前’利用接觸式含水率測定 不赶$ 7 /乾驗室（2)的辆溫度進行㈣，俾使含水率 =超過y。通常所提供的漿料其含水率約娜〜丄〇 t各季節的含水率及溫度的變化，粉碎後的儲藏ΐ 〇)中儲_粉末麟素其含轉會產生偏差。如果含水率 13 201040333 •高’㈣之間容祕生凝聚現象，很難得到均句的、、容、签而0 -氧化甲基瑪/纖維素/水的組成出現偏差，通隹 仃紡絲的纖維的粗度也同時發生偏差，從 物。補.配在帶刀的粉碎機⑹的内部的=== ^ 粉末纖維素的粒徑，可以使則、於__的 巧以使用500_以下的粉末為最佳。粉末的粒徑大於_ A晴’在捏煉機内與氧化甲基瑪進行混合時，漿料之、 凝聚現象’、從而難以製造均勻的溶液。通過粉碎機（6 )並^ 〇的粉==素’通過送風裝置⑺提供給袋式雜程式、$ =Ute· ’將空氣被排出到外部，粉末狀的纖維素通） 闕(rotary valve) ( 9 )提供給_纖維素儲藏槽（工〇 ) 重量式計量裝置(1 1 )將粉末纖維素提供給捏煉機(2 裝程乂驟中生成並使用的氧化甲基瑪以重量20%〜35%的漠产 ==(乂):除去;:，炭化雜質等，儲= / _ ^& 1 8 )然後再從/辰縮i合的供給槽依次定量提供給3 ^薄膜下型濃縮塔（工9 )，最終製造出重量_〜·的氧化甲 〇,瑪水溶液。將濃縮的氧化甲基瑪提供給保持在阶的套管 (=ket)式儲藏槽（2 〇 )。將從套管式儲藏槽（2 〇 )中量取的 液態氧化曱基瑪和從精密重量式計量裝置（2丄）中量取的纖維 ，粉末提供給安裝有用於高減溶_組合攪拌器⑼砸碰― =er)的溶解槽（2 2 )，製造出溶解有重量〇· 01%〜5%程度的少 =維素氧化甲基瑪溶液，製造的溶缝至雜儲藏槽（2 通過齒輪泵（2 4 ；)與纖維素粉末—起被定量地提供給捏煉 機（2 5)内部。 ^ f於以熱介套管方式來保持溫度的捏煉機（2 5 )，可以將其 酿度調整在大致5〇。〇〜95。〇，根據溶解於所投入的氧化曱基瑪中 的纖維素的濃度和所使用的纖維素粉末的分子量以及最終的纖維 14 201040333 素、/辰度的不同，最佳溫度會有變化。用5〇°c〜95。〇的捏煉機（2 5)對^容解有少量纖維素的低溫氧化甲基瑪和纖維素粉未進行捏 煉’使氧化甲基瑪均勻地浸透在纖維素的全面積中，形成糊狀物。 隨著糊狀物的形成使纖維素溶脹，並開始部分溶解。通過強制轉 送裝置（1 2 )’由雙軸擠出機（2 6 )來提供糊狀物。將雙軸擠 出機£2 6)的内部溫度調整在6〇。(：〜1〇5。(：範圍内，由於溫度上 升和另切力，糊狀物内的纖維素被完全溶解。溶解的纖維素溶液 經過篩檢程式（2 7)後，通過喷嘴〔2 8)進行纺絲，最後經 〇 過水洗和乾燥，從而製作出纖維素纖維。 /μ ®第i Ϊ係表示氧化甲基瑪固化溫度根據纖維素濃度變化的變 =。由參考第3可知’即使僅溶解有少量（約0.0 二纖，ΐ，也能使氧化甲基瑪的固化溫度從75。。急劇地下降到 中曰1圖中的說明，根據本發明，在液態濃縮氧化曱基瑪 粉末’使氧化甲基瑪溶液的固化溫度變低。 溫度下’將氧化甲基瑪溶液以液態提供給 在低溫“纖唯;度範圍實施製程’而且可以 從而狀如末和氧甲基瑪溶液能順利地混合及溶脹。 〇均⑽纖絲面上生成細，最終仰魏溫下製造出 以下’為了能更明確地理解本發、 了 (a)纖維素溶液的均勻性 態為『二二 15 201040333The indifference is set to a weight of 53⁄4 (the content of cellulose powder in ~9Λα/A is small. If the kneader is different from this, if it is more than 20%, the physical properties are difficult, and a uniform solution cannot be obtained.) The solution is dissolved, so that, according to the present invention, the kneading solution is injected into the kneader in the step and then in the kneading machine, and then supplied to the extruder to be swollen to prepare a cellulose solution in the form of a substance. If you change the shape of the solution, you can make a range of Ο 。 , if the barrel is less than 2 l / d in 12 cellulose solution through the barrel for a short time, the macro It / D is less than 12, then There are more than 16 barrels or a screw-free/glutoscing part. Unlike this, if the force is too large, the deformation of the screw may occur. At 64, the cellulose in the powder of the screw is applied to the powder (8). Additives such as polyethylene glycol, double-ethyl comb, winter moldings that are functional, carbon or chlorinated. /Those things - titanium oxide, diminishing stone eve, (ι) =; ί before loading through the milk report (5) 'Using contact moisture content measurement does not catch $ 7 / dry room (2) temperature (4),俾 Make moisture content = exceed y. Generally, the slurry provided has a water content of about Na ~ 丄〇 t changes in water content and temperature in each season, and the storage of pulverized ΐ 〇 _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ If the water content is 13 201040333 • High (4) between the secret and the agglomeration phenomenon, it is difficult to get the uniform sentence, the capacity, the sign and the 0-oxidized methylma/cellulose/water composition deviation, the overnight spinning The thickness of the fiber also varies at the same time. It is preferable to use the powder of the powdered cellulose in the inside of the pulverizer (6) with a knife to make it possible to use a powder of 500 Å or less. When the particle size of the powder is larger than _A-clearing, the slurry is agglomerated when it is mixed with the oxidized methyl group in the kneader, so that it is difficult to produce a uniform solution. By the pulverizer (6) and the powder of the = = = 通过 通过 通过 通过 通过 通过 通过 通过 通过 通过 通过 通过 通过 通过 通过 rot rot rot rot rot rot rot rot rot rot rot rot rot rot rot rot rot rot rot rot rot rot rot rot rot rot rot rot rot rot rot (9) supplied to the _cellulose storage tank (worker), the gravimetric metering device (1 1 ) supplies the powdered cellulose to the kneader (2 oxidized methylma generated and used in the process of the process is 20% by weight ~35% of desert production == (乂): removal;: carbonization impurities, etc., storage = / _ ^ & 1 8 ) and then quantitatively supplied to the 3 ^ film subtype from the supply tank The concentration tower (Work 9) finally produced an oxidized formamidine and an aqueous solution of _~·. The concentrated oxidized methylma is supplied to a casing (=ket) type storage tank (2 〇) which is maintained in the order. The liquid cerium oxide gamma measured from the casing type storage tank (2 〇) and the fiber measured from the precision weight metering device (2 丄) are supplied to the mixer for the high-dissolution _ combination agitator (9) Bumping - = er) dissolution tank (2 2 ), producing a solution containing less than the weight 〇 · 01% ~ 5% less = vitamin oxidized methyloma solution, manufactured by the solution to the miscellaneous storage tank (2 through The gear pump (2 4 ;) is quantitatively supplied to the inside of the kneader (25) together with the cellulose powder. ^ f is a kneader (2 5 ) that maintains the temperature by means of a thermo-mechanical sleeve. The brewing degree is adjusted to be approximately 5 〇. 〇~95. 〇, according to the concentration of cellulose dissolved in the yttrium oxide yttrium and the molecular weight of the cellulose powder used and the final fiber 14 201040333 素, / 辰The optimum temperature will vary. The kneading machine (25) is used to knead the low-temperature oxidized methylma and cellulose powder with a small amount of cellulose. 'Making the oxidized methyl group evenly soaked in the entire area of the cellulose to form a paste. With the formation of the paste, the fiber The vitamins swell and begin to partially dissolve. The paste is supplied by a twin-screw extruder (2 6 ) by a forced transfer device (1 2 ). The internal temperature of the twin-screw extruder is adjusted to 6 Hey. (:~1〇5. (: Within the range, the cellulose in the paste is completely dissolved due to the temperature rise and the other shear force. The dissolved cellulose solution passes through the screening program (2 7) and passes through the nozzle [2] 8) Spinning, and finally washing and drying to prepare cellulose fibers. /μ® i-lane indicates that the curing temperature of the oxidized methyl group changes according to the cellulose concentration =. Even if only a small amount (about 0.0 fiber, ΐ, can be dissolved, the curing temperature of the oxidized methyl group can be reduced from 75.. sharply down to the description in the middle 曰1 diagram, according to the present invention, the cerium oxide is concentrated in the liquid state. The powder 'make the curing temperature of the oxidized methylma solution low. At the temperature, the oxidized methylmar solution is supplied in a liquid state to the low temperature "fibrous; range process" and can be used as a solution such as oxymethylmethyl It can be smoothly mixed and swelled. 〇 (10) The surface of the fibril is fine, and the following is produced at the final temperature. In order to understand the hair more clearly, (a) the uniformity of the cellulose solution is "two two." 15 201040333

J (b )重量平均聚合度（DPw) 溶解的纖維素其固有粘度『IV』可以用如下的方法測定。採 用烏氏(U berod)粘度計在25±0. 01X：下，測定根據ASTM D539-51T 製作的0. lg/dL〜〇. 6g/dL濃度的0.5M氫氧化銅乙二胺 (cupriethylenediamine hydroxide)溶液。 (c)利用下述方法測定本發明所製造的纖維素纖維的物理性質。 乾燥強度.107C、2小時乾燥之後的強度(g/d) 0 濕潤強度：以25°C、65RH%放置24小時後測定的強度(g/d) 凊參閱表1，其係實施例1〜12之表列圖，使用乾燥艙室， 將重里平均I合體為12〇〇的纖維素片（Buckeye)以6 · 5%〜 1 0%的含水率進行調節。然後，利用安裝有500//m的筛輪的粉 碎機製造直徑小於等於5〇〇 含水率為重量3· 5%〜7%的纖維素 - 粉末，接著通過薄膜降下濃縮塔，製造濃縮成重量87. 5%、9〇它 巧態，化曱基瑪。無態氧化甲基瑪的濃縮過程中，添加相對 ?辰縮液基瑪為重量的抗氧化劑，並使其溶解。 ，液態氧化曱基瑪及纖維素粉末量取到安裝★用於進行高枯 〇 的組合勝H的溶解槽’製作雜有重量G.Qi%〜2 維素的氧化甲基瑪溶液。然後，通過齒輪泵將所製造 Ϊ容液7注入捏煉機’該捏煉機内部溫度保持在5〇 旦料脾i用精密重量式的計量裝置來對纖維素粉末進行定 重煉機’以使相對全體溶液，纖維素糊狀物的 Γ的Ϊΐίΐ 所使用的捏煉機’其體積為約3几、旋轉 給同方二雙車 用製^的糊狀物被強制轉送並被提供 第-雜給部賴筒H偏3 2軸擠錢的直徑為47刪，其 溫度保持在95。(：〜105。&所製、生的^〜7〇C ’最終排出部的機筒 過篩檢程式，通過齒輪糊狀物在溶脹及溶解之後，通 ⑽泵被&供給喷嘴。為了對溶液的均勻性 16 201040333 Ϊ行Γ價’在從雙輛掩出機排出不久後的溶液轉送帶上進行取 為^用噴絲孔(orifice)直徑為15〇，孔間隔為i.5mm，孔數 9Qlnni000個的喷嘴將纖維素溶液排出。將空氣層的長度保持於 為’空氣層中用於吹向長絲的冷空氣的溫度和相對濕度分別設 到凑C、45RH%。然後，將風速調節成6. 5m/sec。被空氣層送流 得洛的長絲經過水洗、乾燥、上油處理以及卷取’將最終獲 、複絲的纖維度調節成1500旦尼爾（denier)。J (b) Weight average degree of polymerization (DPw) The intrinsic viscosity "IV" of the dissolved cellulose can be measured by the following method. Using a U berod viscometer at 25 ± 0. 01X: 0.5 lg / dL ~ 〇. 6g / dL concentration of 0.5M copper hydroxide ethylenediamine (cupriethylenediamine hydroxide) ) solution. (c) The physical properties of the cellulose fibers produced by the present invention were measured by the following methods. Drying strength. 107 C, strength after drying for 2 hours (g/d) 0 Wet strength: strength (g/d) measured after standing at 25 ° C, 65 RH% for 24 hours 凊 Refer to Table 1, which is Example 1~ In the table of Table 12, the cellulose sheet (Buckeye) having a 12-inch average I-synthesis was adjusted at a moisture content of 6 · 5% to 10% using a drying compartment. Then, a cellulose-powder having a water content of 5 5% to 7% by weight is prepared by using a pulverizer equipped with a 500/m sieve wheel, and then the concentration tower is lowered by a film to produce a concentrated weight. 87. 5%, 9 〇 it is a clever state, 曱 曱 曱 。. During the concentration process of the non-oxidized methyl ketone, an antioxidant is added to the weight of the condensate kima and dissolved. The amount of liquid cerium sulphate and cellulose powder is taken up and installed. ★ The dissolution tank for the combination of high cumin and sulphur H is made into an oxidized methyl methine solution with a weight of G.Qi% to 2 velocities. Then, the produced sputum liquid 7 is injected into the kneader by a gear pump. The internal temperature of the kneader is kept at 5 spleen, and the cellulose powder is subjected to a refining machine by a precision weight type metering device. For the whole solution, the kneading machine used for the cellulose paste is used. The kneader used has a volume of about 3, and the paste for the rotation of the same two-vehicle is forcibly transferred and supplied with the first miscellaneous. The diameter of the squeezing of the H-32 axis is 47, and the temperature is maintained at 95. (: ~105. & produced, raw ^~7〇C 'The final discharge part of the barrel screening program, after the gear paste is swollen and dissolved, the (10) pump is supplied to the nozzle. Uniformity of the solution 16 201040333 The price of the ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' The number of holes 9Qlnni000 nozzles discharges the cellulose solution. The length of the air layer is maintained at the temperature and relative humidity of the cold air used for blowing into the filaments in the air layer, respectively, to C, 45 RH%. The wind speed was adjusted to 6. 5 m/sec. The filaments fed by the air layer were washed, dried, oiled and coiled to adjust the fiber length of the final and multifilament to 1500 denier.

區分 實施 例 1 實施 例 2 實施 例 3 實施 例 4 實施 例 5 實施 例 6 實施 例 7 實施 例 8 實施 例 9 實施 例 10 實施 例 11 實施 例 12 〜溶液的 瑢解漿料濃度 0.01 0.1 0.1 0.5 0.5 0.5 1.2 1.2 1.2 1.2 2.0 2.5 ，M〇溶液的 —^C) 78 75 75 67 70 65 59 53 60 57 53 87 圼煉璣的输 ^〇C) 75 70 85 70 75 68 67 51 66 66 55 91 *煉镣的旋轉速 30 30 30 30 30 30 30 20 30 25 30 30 ^機的旋轉速 200 200 200 180 200 230 200 180 250 200 150 250 擠，的最終機 105 100 100 95 100 95 105 95 100 95 95 105 瑢_製造量 110 140 130 180 170 180 220 170 230 170 160 235 纖維素粉末的含 4.3 3.9 4.1 3.9 4.0 4.0 4.2 4.8 4.4 4.9 4.0 7.5 17 201040333 溶液的均勻性 —(1-5) 2 2 -~~~~―― 2 1 1 2 1 -~~— -1 1 3 2 2 長絲的聚合度 1010 1030 960 990 1000 970 1040 1020 Qlf) 1 non 1 ΛΟΠ ΟΟΛ 長絲的強度(δ/ίΓ) 7.0 7.3 6.7 7.1 7.0 6.5 7.0 7.5 Λ Q 1UZU c n 1 uzu n y〇\) n 〇 長絲的伸長率 (%) 5.9 6.1 ___ 5.4 6.2 6.7 6.4 5.7 5.9 U.^7 5.4 o.y 5.0 /.0 5.5 /.Z 6.5 用〆ί ί閱表2 ’其係實施例13〜2 2之表列圖。使 〇 2 3至：量平均聚合體為850的纖維素片(Buckeye)以 的Q%的含水率進行調節。然後，糊安裝有500#m ==::機製造直徑5°〇Μ以下、含水率為重量3.關 git;接著通過薄膜降下濃祕，製造濃縮成重量们 ㈣化甲基瑪。在液態氧化f基瑪的濃縮過程中， 目對祕祕氧化甲顧為重量G. _的抗·劑，並使其 解輸^基瑪域較粉末餘到安財跡高招度溶 量纖ii，11的溶ΐ槽’製作溶财重量g. 1%〜5%程度的少 ❹瑪溶液二=甲基瑪溶液。然後通過齒輪泵將所製造的氧化甲基 用梦JΓ “捏煉機’該捏煉機内部保持在5G°c〜95°C。利 αΓΪ重域的計量裝置來對雜素粉末進行定量，秋後將I、、主 n機’令_素嫌物的最料度為姆整體溶液重量、;；3 二、:人所使用的捏煉機，其體積為約3〇L、旋轉片的逮度為 出機印^用製^的^^^娜送並被提供給同方向的雙軸擠 雙轴擠機徑為47麵，第一個供給部的機筒 r H寺在㈣〜赃’最終排出部的機筒溫度保持在蚊〜⑽ 過造_狀物’在溶脹及溶解之後，通過篩檢程式，再通 ί ’被提供給喷嘴。為了對溶液的均勻性進行評估，在從 又軸擠出機排出不久後的溶液轉送帶上進行取樣。 攸 纖維素溶液利用喷絲孔(orifice)直徑為15〇_、孔間隔為Differentiation Example 1 Example 2 Example 3 Example 4 Example 5 Example 6 Example 7 Example 8 Example 9 Example 10 Example 11 Example 12 The concentration of the solution of the solution is 0.01 0.1 0.1 0.5 0.5 0.5 1.2 1.2 1.2 1.2 2.0 2.5, M〇 solution—^C) 78 75 75 67 70 65 59 53 60 57 53 87 圼 玑 输 〇 ) ) C) 75 70 85 70 75 68 67 51 66 66 55 91 * Rotating speed of smelting 30 30 30 30 30 30 30 20 30 25 30 30 ^ Rotation speed of machine 200 200 200 180 200 230 200 180 250 200 150 250 Extruded, final machine 105 100 100 95 100 95 105 95 100 95 95 105 瑢_Manufacture amount 110 140 130 180 170 180 220 170 230 170 160 235 Cellulose powder containing 4.3 3.9 4.1 3.9 4.0 4.0 4.2 4.8 4.4 4.9 4.0 7.5 17 201040333 Uniformity of solution - (1-5) 2 2 -~ ~~~—— 2 1 1 2 1 -~~— -1 1 3 2 2 Degree of polymerization of filaments 1010 1030 960 990 1000 970 1040 1020 Qlf) 1 non 1 ΛΟΠ ΟΟΛ Strength of filaments (δ/ίΓ) 7.0 7.3 6.7 7.1 7.0 6.5 7.0 7.5 Λ Q 1UZU cn 1 uzu ny〇\) n Elongation of filaments (%) 5.9 6.1 ___ 5.4 6.2 6.7 6 .4 5.7 5.9 U.^7 5.4 o.y 5.0 /.0 5.5 /.Z 6.5 〆 阅 表 2 2 ’ ’ ’ 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 The cellulose sheet (Buckeye) having a volume average polymer of 850 was adjusted to have a Q% moisture content. Then, the paste was installed with 500#m ==:: machine manufactured to have a diameter of 5° 〇Μ or less, and the water content was weighted by 3. git; and then the film was thickened and concentrated to produce a weight (4) methyl group. In the concentration process of liquid oxidized f-kimma, the secret oxidized carbamide is the anti-agent of weight G. _, and it is decomposed into the gamma-ma domain. , 11 of the dissolution tank 'to make a solvency weight g. 1% ~ 5% degree of gamma solution two = methyl methine solution. Then, the oxidized methyl group produced by the gear pump is used to quantify the impurity powder in the inside of the kneader by the "Job" of the dream J Γ "Kneader". After I, the main n machine 'order _ prime suspects the maximum material weight is the overall solution weight,; 3 2:: the kneader used by people, its volume is about 3 〇 L, the rotation of the film The degree is issued by the machine ^^^^Na and is supplied to the same direction of the twin-screw double-axis extruder with a diameter of 47 faces, and the first supply part of the barrel r H temple is at (four) ~赃' The temperature of the barrel of the final discharge is kept in the mosquito~(10) After the swelling and dissolution, it is passed through the screening program and then supplied to the nozzle. In order to evaluate the uniformity of the solution, The shaft extruder is sampled on the solution transfer belt for a short time. The cellulose solution has a diameter of 15 〇 _, and the pore spacing is

2UIU4UJJJ 2. 5mm、篩孔數為的個、+ 60刪，空氣層中用於吹4的噴嘴將其排出。空氣層的長度保持於 為23°C、55RH%。然長絲的冷空氣的溫度和相對濕度分別設 固浴的長絲經過水^=速調節成7m/sec。被空氣層送流到凝 複合絲的纖維度調節成二〇以:以及卷取’將最終獲得的 在實婦|丨2 2巾’除了朗重量平触合體為·的纖維素 片（Buckeye)之外，採用與實施例13〜21相同的方法實施。2UIU4UJJJ 2. 5mm, the number of mesh holes, + 60 cut, the nozzle for blowing 4 in the air layer will discharge it. The length of the air layer was maintained at 23 ° C and 55 RH%. However, the temperature and relative humidity of the cold air of the filaments were respectively adjusted to 7 m/sec by the speed of the water. The fiberiness that is sent to the condensed composite wire by the air layer is adjusted to two: to take up the cellulose film (Buckeye) that will be finally obtained in addition to the weight of the flat-contact body. The same procedures as in Examples 13 to 21 were carried out.

表2 區分 實施 例 13 實施 例 14 實施 例 15 實施 例 ^_16 實施 例 17 實施 例 18 實施 例 19 實施 例 20 實施 例 21 實施 例 22 NMMO溶液的溶 解漿料濃度(％) 0.1 0.1 0.5 0.5 1.2 1.2 1.2 2.0 3.0 5.0 NMMO溶液的捏 煉機注入溫度 CC) 75 75 67 70 63 65 65 61 55 52 捏煉機的溫度 ΓΟ 70 80 75 75 67 70 75 65 57 54 捏煉機的旋轉速 度(卬Π1) 一· 擠出機的旋轉速 度(rpm) 30 30 30 30 20 30 25 30 30 30 180 180 180 230 180 250 200 150 250 250 擠出機的最終機 筒溫度(。〇 ________ 溶液的製造量 100 95 95 100 95 100 105 95 105 100 160 160 210 220 180 220 190 170 180 240 (kg/hr) — 纖維素粉末的含 水率(％) ______- 4.9 4.3 3.7 4.5 4.9 4.2 5.3 4.9 4.5 4.7 201040333 溶液的均句性 丄 1〜5) ~~~^----- 1 2 1 1 1 1 2 2 2 1 長絲的聚合窗 J50 730 750 700 720 690 710 760 745 630 5.3 5.7 4.9 5.4 5.5 4.8 5.3 6.1 63 45 絲的伸格 ~~ ~~ 一 7.1 7.4 7.2 6.7 6.9 7.0 6.5 6.3 6.7 8.1 例表3的比較說明’除上述之外的其他條件，和實施 八溶解於不同的是’在比較例1〜5 +，沒有將漿料 〇歲纖维絲I基瑪中’將純粹的南溫氧化甲基瑪注入到捏煉機， 行混合及溶脹，利職出機使其溶解，從而製作 表3 區分 比較例 1 比較例 2 比較例 3 比較例 4 比較 例 5 比較 例 6 比較 例 7 比較 例 8 DP 1200 1200 1200 1200 850 850 850 850 NMMO溶液的溶解漿 料濃度(％) 0 0 0 0 0 0 0 0 NMMO溶液的捏煉機 注入溫度(°C) 95 一 — — 95 '~- — — 捏煉機的溫度(。〇 90 — — — 90 捏煉機的旋轉速度 (rpm) 30 — — — 25 — — _ 擠出機的旋轉速度 (rpm) 200 150 200 250 200 150 200 250 擠出機的最終機筒溫 度(。〇 105 95 95 95 105 100 95 105 溶液的製造量(kg/hr) 105 55 65 80 120 65 70 80 20 201040333 纖維素粉末的含水率 5.1 4.1 4.1 3.9 5.1 4.3 4.5 3.9 (%) 溶液的均勻性(1〜5) 3 3 2 4 3 4 2 2 長絲的聚合度 1020 1050 990 900 690 740 700 680 長絲的強度(g/d) 6.3 7.1 6.9 6.5 5.5 5.7 5.4 4.9 長絲的伸長率(％) 5.5 5.2 4.8 4.0 6.5 7.0 6.7 6.5 其次，在比較例6〜8中，與實施例不同地，沒有使用捏煉Table 2 Differentiation Example 13 Example 14 Example 15 Example ^_16 Example 17 Example 18 Example 19 Example 20 Example 21 Example 22 Dissolved slurry concentration of NMMO solution (%) 0.1 0.1 0.5 0.5 1.2 1.2 1.2 2.0 3.0 5.0 Kneader injection temperature of NMMO solution CC 75 75 67 70 63 65 65 61 55 52 Temperature of kneader ΓΟ 70 80 75 75 67 70 75 65 57 54 Rotating speed of kneader (卬Π1) I. Rotating speed of the extruder (rpm) 30 30 30 30 20 30 25 30 30 30 180 180 180 230 180 250 200 150 250 250 Final barrel temperature of the extruder (.〇________ The manufacturing volume of the solution 100 95 95 100 95 100 105 95 105 100 160 160 210 220 180 220 190 170 180 240 (kg/hr) — water content (%) of cellulose powder ______- 4.9 4.3 3.7 4.5 4.9 4.2 5.3 4.9 4.5 4.7 201040333丄1~5) ~~~^----- 1 2 1 1 1 1 2 2 2 1 Polymer window of filament J50 730 750 700 720 690 710 760 745 630 5.3 5.7 4.9 5.4 5.5 4.8 5.3 6.1 63 45 The extension of the wire ~~ ~~ A 7.1 7.4 7.2 6.7 6.9 7.0 6.5 6.3 6.7 8.1 Example comparison of Table 3 'Other conditions than the above, and the implementation of the eight dissolved in the difference is 'in the comparative example 1~5 +, there is no slurry in the old filiform I jima' will inject pure southern temperature oxidized methylma Go to the kneader, mix and swell, and dissolve it to make it dissolve. Thus, Table 3 is distinguished. Comparative Example 1 Comparative Example 2 Comparative Example 3 Comparative Example 4 Comparative Example 5 Comparative Example 6 Comparative Example 7 Comparative Example 8 DP 1200 1200 1200 1200 850 850 850 850 Dissolved slurry concentration of NMMO solution (%) 0 0 0 0 0 0 0 0 Kneader injection temperature of NMMO solution (°C) 95 I – 95 '~- — — Kneader temperature(. 〇90 — — — 90 Kneader Rotation Speed (rpm) 30 — — — 25 — — _ Rotating speed of the extruder (rpm) 200 150 200 250 200 150 200 250 Final barrel temperature of the extruder (. 〇105 95 95 95 105 100 95 105 Manufactured amount of solution (kg/hr) 105 55 65 80 120 65 70 80 20 201040333 Water content of cellulose powder 5.1 4.1 4.1 3.9 5.1 4.3 4.5 3.9 (%) Uniformity of solution ( 1~5) 3 3 2 4 3 4 2 2 Degree of polymerization of filaments 1020 1050 990 900 690 740 700 680 Strength of filaments (g/d) 6.3 7.1 6.9 6.5 5.5 5.7 5.4 4.9 Elongation of filaments (%) 5.5 5.2 4.8 4.0 6.5 7.0 6.7 6.5 Next, in Comparative Examples 6 to 8, unlike the examples, no kneading was used.

機，僅使用雙軸擠出機將保持於95〇c的重量86. 5%的液態氧化甲 基瑪注入到第1機筒内，然後在第3機筒將纖維素粉末注入側面 雙軸供給機進行混合、溶脹及溶解，同時調節雙轴擠出機的溫户， 從而製造纖維素溶液。 又 ，歸納上述喊明，本發明確實具有可專娜，銳法提出申Machine, using only a twin-screw extruder, the weight of 86 〇c is 86.5% of the liquid oxidized methylma is injected into the first barrel, and then the cellulose powder is injected into the side biaxial supply in the third barrel. The machine mixes, swells and dissolves while adjusting the temperature of the twin-screw extruder to produce a cellulose solution. In addition, summarizing the above-mentioned shouting, the present invention does have a special nature, and the sharp method proposes

【圖式之簡單說明】 第1圖.係為本發明在氧化曱基瑪（ΝΜΜ0)中溶解少量纖維 ^ 練末並製造㈣的齡溶液之步賴。 f 2圖」係為本發明整體製造製程簡㈣。 第3圖.係為本發明氧化甲基瑪^圓）的固化溫度隨 濃度變化的變化圖。 【圖式之圖號說明】 漿料片：（1 ) 乾燥空氣（3 ) 軋輥：（5 ；) 送風裝置:（7 ) 旋轉閥：（9 ) 計量裝置：（11) 精製塔（17) 薄膜降下型濃縮塔（1 乾燥艙室：（2 ) 含水率測定裝置：（4 ) 粉碎機：（6 ) 袋式篩檢程式：（8 ) 儲藏槽：（1 0 ) 強制轉送裝置：（1 2) 供給槽（18) 9 )套管式儲藏槽··（ 2 0 ) 21 201040333 計量裝置：（2 1) 溶液儲藏槽：（2 3 ) 捏煉機：（2 5 ) 師檢程式.（2 7 ) 溶解槽：（2 2 ) 齒輪泵：（2 4) 雙軸擠出機：（2 6 ) 喷嘴：（2 8 )[Simplified description of the drawing] Fig. 1 is a step of dissolving a small amount of fiber in the yttrium yttrium (ΝΜΜ0) of the present invention and preparing the (4) aged solution. The f 2 diagram is the overall manufacturing process of the invention (4). Fig. 3 is a graph showing changes in the curing temperature of the oxidized methyl group of the present invention as a function of concentration. [Illustration of the figure] Slurry: (1) Dry air (3) Roll: (5;) Air supply: (7) Rotary valve: (9) Metering device: (11) Refining tower (17) Film Lowering Concentration Tower (1 Drying compartment: (2) Moisture measuring device: (4) Crusher: (6) Bag screening program: (8) Storage tank: (1 0) Forced transfer device: (1 2) Supply tank (18) 9) Casing storage tank ··( 2 0 ) 21 201040333 Metering device: (2 1) Solution storage tank: (2 3 ) Kneader: (2 5 ) Inspection program. (2 7 Dissolution tank: (2 2 ) Gear pump: (2 4) Twin-screw extruder: (2 6 ) Nozzle: (2 8 )

22twenty two

Claims (1)

201040333 十、申清專利範園： 1、一種纖維素纖維之製造方法，包括以下製程： 々…Α在液恶〉辰縮氧化曱基瑪（N-methyl morpholin Ν-oxide， =，^ίΜΜΌ)中溶解少量◦ · ◦ 1〜5%的纖維素末，用 製造氧化曱基瑪溶液； 备机f i將該轉有少量的麟素粉末之氧化甲基瑪溶液和纖維 Ο Ο 機’在捏煉納無減壓過程地將纖維素混合、潤 成離物後，賴錄物提供給擠出機，得 氣接^凝直接以纺絲喷嘴擠出纺絲後，令其與空 等作^。·將獲得的複合絲進行械、麟、上油歧，以及卷取 其中二項所述之纖維素纖維之製造方法， 〜9 牲維素少1溶解後，液態氧化甲基瑪是以5 〇°c y 〇 U/皿度保持而進行供給。 苴4步:Τΐ專ΐϊ圍第1項所述之纖維素纖維之製造方法， 液和纖维件絲=^轉#少量_餘末的氧化甲基瑪溶 素各末的捏煉機，是保持在5⑽ 且請專利範圍第1項所述之纖維素纖維之製造方法， 其二巧===七 為10%〜18%。 〜合欲祁對於全體重量’其含水量 6、依申請專利範圍第1項 其中該步中，溶解有少素纖維之製造方法’ 由被保持在溫度5 0t：〜9 51的捏“所g甲基瑪^液依g 23 201040333 請專利範圍第1項所述之纖維素纖維之製造方法，其中該步驟B 或步驟C中，該纖維素粉末亦可混合其他高分子物質。 ❹ 〇 24201040333 X. Shenqing Patent Fanyuan: 1. A method for producing cellulose fibers, including the following processes: 々...Α 液 液 〉 〉 辰 辰 辰 辰 ( ( ( ( ( ( ( ( ( oxide oxide oxide oxide oxide oxide oxide oxide oxide oxide oxide oxide oxide oxide oxide oxide oxide oxide oxide oxide oxide oxide oxide oxide oxide oxide Dissolve a small amount of ◦ · ◦ 1~5% of cellulose ends to make yttrium yttrium solution; prepare the machine to convert a small amount of linoleum powder to oxidized methyl methine solution and fiber Ο 机 machine in kneading After the cellulose is mixed and wetted into a separator without a decompression process, the material is supplied to the extruder, and the gas is connected to the spinning nozzle directly after being spun by a spinning nozzle, and then it is made into an air. · The obtained composite yarn is subjected to mechanical, lining, oiling, and the production method of the cellulose fiber described in the above two, and the liquid oxidized methyl ke is 5 〇 after dissolving °cy 〇U/dish is maintained and supplied.苴4 Steps: The manufacturing method of the cellulose fiber described in Item 1 of the Τΐ , , 液 液 液 = = = = = = = = = 少量 少量 少量 少量 少量 少量 少量 少量 少量 少量 少量 少量The method for producing the cellulose fiber according to Item 1 of the patent scope is as follows: (2) ================================================= ~ 合 祁 祁 全体 全体 祁 祁 祁 祁 祁 祁 祁 祁 祁 祁 祁 祁 祁 祁 祁 祁 祁 祁 祁 祁 祁 祁 祁 祁 祁 祁 祁 祁 祁 祁 祁 祁 祁 祁 祁 祁 祁 祁 祁 祁 祁 祁 祁 祁 祁 其 其The method for producing a cellulose fiber according to the above item 1, wherein the cellulose powder may be mixed with other high molecular substances in the step B or the step C. ❹ 〇24