JPS61278558A - Polyester composition - Google Patents
Polyester compositionInfo
- Publication number
- JPS61278558A JPS61278558A JP12054185A JP12054185A JPS61278558A JP S61278558 A JPS61278558 A JP S61278558A JP 12054185 A JP12054185 A JP 12054185A JP 12054185 A JP12054185 A JP 12054185A JP S61278558 A JPS61278558 A JP S61278558A
- Authority
- JP
- Japan
- Prior art keywords
- titanium nitride
- glycol
- slurry
- acid
- polyester
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Landscapes
- Manufacture Of Macromolecular Shaped Articles (AREA)
- Shaping By String And By Release Of Stress In Plastics And The Like (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Polyesters Or Polycarbonates (AREA)
- Artificial Filaments (AREA)
Abstract
Description
【発明の詳細な説明】
［技術分野］
本発明は芳香族ジカルボン酸を主とする二官能性酸成分
と少なくとも一種のグリコール成分よりなるポリエステ
ル組成物に関するものであり、更に詳しくは表面の均一
性および遮光性に優れた繊維、フィルム用あるいはその
他の成形品に適した黒原着ポリエステル組成物に関する
ものである。Detailed Description of the Invention [Technical Field] The present invention relates to a polyester composition comprising a bifunctional acid component mainly consisting of an aromatic dicarboxylic acid and at least one glycol component. The present invention also relates to a black spun-dyed polyester composition that has excellent light-shielding properties and is suitable for use in fibers, films, and other molded products.
［従来技術及びその問題点］
今日工業的に製造されているポリエステル、例えばポリ
エチレンテレフタレートを主成分とするポリエステルは
優れた物理的、化学的特性を有しており、繊維、フィル
ム、およびその他の成形品として広く使用されている。[Prior art and its problems] Polyesters produced industrially today, such as polyesters based on polyethylene terephthalate, have excellent physical and chemical properties and are suitable for use in fibers, films, and other moldings. It is widely used as a product.
これらポリエステル繊維あるいはフィルム等を製造し、
更に加工する際、繊維あるいはフィルム等の成形品の滑
り性が必要であり、このため、ポリエステル中に二酸化
チタン、シリカ等の微粒子を配合せしめ、成形品の表面
に適度の凹凸を与えて成形品の表面滑性を向上させるこ
とが通常行なわれている。Manufacture these polyester fibers or films,
During further processing, it is necessary for molded products such as fibers or films to have slipperiness. For this reason, fine particles such as titanium dioxide and silica are blended into polyester to give the surface of the molded product an appropriate level of roughness. It is common practice to improve the surface smoothness of.
ざらに、ポリエステルを黒く着色させたり、また遮光性
を付与し、ポリエステル成形品の付加価値を高めるため
、例えば、特開昭４８−９３６４８号公報、特開昭５０
−６２２９６＠公報などにはカーボンブラックを添加す
ることが知られている。In order to increase the added value of polyester molded products by coloring polyester black or imparting light-shielding properties, for example, JP-A-48-93648, JP-A-50
It is known to add carbon black, such as in -62296@publication.
しかしながら、カーボンブラックは極めて凝集性が強く
、そのためポリエステルの製造工程中に添加した場合に
は、分散が不充分であるという欠点を有している。ポリ
マ中に凝集粒子が存在すると紡糸時の糸切れの原因とな
ったり、またガイドや口金の摩耗等の問題が生じ、フィ
ルムにおいては粗大突起、フィッシュアイ等の原因とな
る。特に繊維においてはファインデニール化が進行し、
フィルムにおいては磁気記録用フィルムなどフィルム表
面の高性能化が要求され、黒原着および遮光性を有し、
かつ粒子の分散性の良好なポリエステルが待望されてい
るのが現状である。However, carbon black has extremely strong agglomeration properties, and therefore has the disadvantage of insufficient dispersion when added during the polyester manufacturing process. The presence of aggregated particles in the polymer causes thread breakage during spinning, causes problems such as abrasion of guides and spinnerets, and causes coarse protrusions, fish eyes, etc. in films. Especially in fibers, fine denier is progressing,
For films, such as magnetic recording films, high performance film surfaces are required, and black coloring and light-shielding properties are required.
At present, there is a long-awaited demand for a polyester having good particle dispersibility.
本発明者らは上記実状に鑑み鋭意検討した結果、微粒子
状窒化チタンがポリマ中での分散性、黒原着性、遮光性
および易滑性付与の効果に優れているとの知見を得て本
発明に達したものである。As a result of intensive studies in view of the above-mentioned circumstances, the inventors of the present invention have found that fine particulate titanium nitride has excellent dispersibility in polymers, black adhesion, light shielding properties, and imparting slipperiness. This is an invention.
［発明の目的］
本発明の目的は上記した従来技術では達成できなかった
黒原着および遮光性を有し、かつ粒子の分散性にも優れ
たポリエステル組成物を提供することにある。更に別の
目的は易滑性に優れたポリエステル組成物を提供するこ
とにある。[Object of the Invention] An object of the present invention is to provide a polyester composition that has black coloring and light-shielding properties that could not be achieved with the conventional techniques described above, and also has excellent particle dispersibility. Yet another object is to provide a polyester composition with excellent slipperiness.
［発明の構成］
本発明の前記目的は芳香族ジカルボン酸を主とする二官
能性酸成分と少なくとも一種のグリコール成分よりなる
ポリエステルであり、かつ微粒子状窒化チタンを含有し
てなるポリエステル組成物によって達成できる。[Structure of the Invention] The object of the present invention is to provide a polyester composition comprising a bifunctional acid component mainly consisting of an aromatic dicarboxylic acid and at least one glycol component, and containing fine particulate titanium nitride. It can be achieved.
本発明において用いられる芳香族ジカルボン酸成分とし
てはテレフタル酸、２，６−ナフタリンジカルボン酸、
１，２−ビス（２−クロロフェノキシ）エタン−４，４
′ −カルボン酸を挙げることができ、２０モル％以
下のインフタル酸、５−ナトリウムスルホ−イソフタル
酸、アジピン酸等の共重合成分を含むことができる。Aromatic dicarboxylic acid components used in the present invention include terephthalic acid, 2,6-naphthalene dicarboxylic acid,
1,2-bis(2-chlorophenoxy)ethane-4,4
'-carboxylic acids, and may contain up to 20 mol % of copolymerized components such as inphthalic acid, 5-sodium sulfo-isophthalic acid, and adipic acid.
また、グリコール成分としてはエチレングリコールを主
たる成分とするがその他ブチレングリコール、ジエチレ
ングリコール、プロピレングリコール、ポリエチレング
リコール、１，４−シクロヘキサンジメタツール等を主
成分または共重合成分として含んでいてもよい。The glycol component mainly contains ethylene glycol, but may also contain butylene glycol, diethylene glycol, propylene glycol, polyethylene glycol, 1,4-cyclohexane dimetatool, etc. as a main component or as a copolymer component.
本発明で用いる微粒子状の窒化チタンとじては最大粒子
径１０μｍ以下、好ましくは５μｍ以下であるが、これ
は通常金属チタンまたは酸化チタンを窒素中で加熱する
ことにより得られる。The fine particle titanium nitride used in the present invention has a maximum particle size of 10 μm or less, preferably 5 μm or less, and is usually obtained by heating metallic titanium or titanium oxide in nitrogen.
本発明でポリエステルに含有させる微粒子状の窒化チタ
ンの量はｏ、 ｏｉ〜２０重量％、好ましくは０．０５
〜１０重量％である。In the present invention, the amount of finely divided titanium nitride contained in the polyester is o, oi to 20% by weight, preferably 0.05% by weight.
~10% by weight.
窒化チタンの添加はポリエステル製造工程の任意の段階
、任意の方法で行なわれる。しかし、重合開始前、エス
テル化またはエステル交換反応で比較的低分子量の中間
体を製造する段階あるいはこれらを更に減圧または不活
性気流中で重縮合反応させて繊維またはフィルム形成能
を有する高重合体を得る段階等のポリエステル重合開始
前から重合反応中の段階で添加するのが操作上有利でお
る。この時、種々の分散媒、一般には、エチレングリコ
ールに均一に分散させたスラリ状態で添加するのが好ま
しい。Addition of titanium nitride can be carried out at any stage of the polyester manufacturing process and by any method. However, before the start of polymerization, a step of producing relatively low molecular weight intermediates through esterification or transesterification, or a polycondensation reaction of these intermediates under reduced pressure or an inert gas flow, produces a high polymer capable of forming fibers or films. It is operationally advantageous to add it before the start of polyester polymerization and during the polymerization reaction, such as in the step of obtaining . At this time, it is preferable to add it in the form of a slurry uniformly dispersed in various dispersion media, generally ethylene glycol.
エチレングリコール等の分散媒への分散には、種々の分
散法、例えば、高速分散機、超高速分散機、コロイドミ
ル、ウルトラターレックス、ホモジナイザー、サンドミ
ル、アトライタ、ロールミル等を用いて分散するのが好
ましい。特に超音波分散機やサンドミル、ロールミル等
の分散機が凝集粒子を微分散できるために有利であり好
ましい。For dispersion in a dispersion medium such as ethylene glycol, various dispersion methods can be used, such as a high-speed dispersion machine, an ultra-high-speed dispersion machine, a colloid mill, an ultraturrex, a homogenizer, a sand mill, an attritor, a roll mill, etc. preferable. In particular, a dispersing machine such as an ultrasonic dispersing machine, a sand mill, or a roll mill is advantageous and preferable because it can finely disperse aggregated particles.
最も好ましくは媒体攪拌型分散法の採用である。媒体攪
拌型分散に用いる媒体粒子としてはガラスピーズ、ある
いはジルコニア、チタニアなどからなるセラミックス粒
子などが用いられる。該粒子は窒化チタン粒子より大き
いことが好ましく、更に好ましくは平均粒子径が０．５
ｍｍ以下、０．０１ｍｍ以上、一層好ましくはｏ、 ：
ｓｍｍ以下０．０２ ｍｍ以上である。また、分散粒子
に粒子状物を共存させ、周速６ｍ／秒以上、好ましくは
Ｂ１１１／秒以上で高速攪拌下で分散することが好まし
い。Most preferably, a medium agitation type dispersion method is employed. As the medium particles used in the medium stirring type dispersion, glass beads, ceramic particles made of zirconia, titania, etc. are used. The particles are preferably larger than titanium nitride particles, and more preferably have an average particle diameter of 0.5.
mm or less, 0.01 mm or more, more preferably o:
smm or less and 0.02 mm or more. Further, it is preferable to cause particulate matter to coexist with the dispersed particles, and to disperse the particles under high-speed stirring at a circumferential speed of 6 m/sec or more, preferably B111/sec or more.
また、分散時にはリン酸、アルカリ化合物、ポリアルキ
レングリコール等の分散剤を使用するとスラリおよびポ
リマ中の窒化チタンの再凝集を防止でき、特に好ましい
６
ざらに窒化チタンをスラリとして調製する際には０．１
〜５０重量％含有したスラリ、より好ましくは１〜３０
重量％含有のスラリとして調製するのが好ましい。In addition, when dispersing, using a dispersing agent such as phosphoric acid, an alkali compound, or polyalkylene glycol can prevent re-agglomeration of titanium nitride in the slurry and polymer, which is particularly preferred. .1
Slurry containing ~50% by weight, more preferably 1~30% by weight
Preferably, it is prepared as a slurry containing % by weight.
また、ポリエステルの溶融成形時に混合する方法も簡便
である。Furthermore, the method of mixing during melt molding of polyester is also simple.
［発明の効果］
本発明は上記したように、芳香族ジカルボン酸を主とす
る二官能性酸成分と少なくとも一種のグリコール成分よ
りなるポリエステルに微粒子状窒化チタンを含有してな
る組成物であり、本発明の組成物によって次のような効
果が発揮される。[Effects of the Invention] As described above, the present invention is a composition comprising fine particulate titanium nitride in a polyester consisting of a bifunctional acid component mainly consisting of an aromatic dicarboxylic acid and at least one glycol component, The composition of the present invention exhibits the following effects.
（１）窒化チタンの微粒子はポリエステル中で極めて均
一に分散させることができるので、本発明の組成物から
得られる繊維、フィルムあるいは成形品は相互間の易滑
性に優れ、巻き取り等の操作が容易であり、押出しなど
の成形時に成形機の目詰りや糸切れ等のトラブルが生じ
ない。(1) Fine particles of titanium nitride can be dispersed extremely uniformly in polyester, so fibers, films, or molded products obtained from the composition of the present invention have excellent mutual slipping properties, and operations such as winding It is easy to use, and troubles such as clogging of the molding machine and thread breakage do not occur during molding such as extrusion.
（２）窒化チタンを含有していることによって、ポリエ
ステルの軟化点おるいは重合度に何ら劣るところはない
ため、本発明の組成物は通常の成形法で容易に成形を行
なうことができる。(2) Since the composition of the present invention contains titanium nitride, there is no inferiority in the softening point or degree of polymerization of polyester, and therefore, the composition of the present invention can be easily molded by ordinary molding methods.
（３）カーボンブラックに比較して分散性が良好である
ため、表面特性が良好で、かつ脱落等が少ない良好な黒
原着糸や黒原着フィルムおよび遮光性フィルムとするこ
とができる。(3) Since the dispersibility is better than that of carbon black, it is possible to produce black spun-dyed yarn, black spun-dyed film, and light-shielding film with good surface properties and less shedding.
次に実施例を挙げて本発明を説明するが、実施例中の［
η］はフェノール：テトラクロルエタンが１：１（重量
比）の混合溶媒中３０℃で求めた極限粘度である。Next, the present invention will be explained with reference to Examples.
η] is the intrinsic viscosity determined at 30° C. in a mixed solvent of 1:1 (weight ratio) phenol:tetrachloroethane.
実施例１
平均−次粒子径０．２μｍ１最大−次粒子径１．０μｍ
の窒化チタン１０部、エチレングリコール１００部を添
加し、ホモジナイザーにて高速攪拌してスラリを作成し
た。Example 1 Average particle size: 0.2 μm 1 Maximum particle size: 1.0 μm
10 parts of titanium nitride and 100 parts of ethylene glycol were added and stirred at high speed with a homogenizer to prepare a slurry.
該スラリを五十嵐機械（株）製サンドグラインダーで処
理し、窒化チタンのエチレングリコールスラリを調製し
た。続いて、１μｍの目開きのフィルターでスラリを濾
過した。得られたスラリ粒子の粒径分布を遠心式粒子径
測定装置（堀場製作所製 ＣＡＰＡ ５００）で測定す
ると、平均粒径は０．２μｍであった。The slurry was processed with a sand grinder manufactured by Igarashi Kikai Co., Ltd. to prepare an ethylene glycol slurry of titanium nitride. Subsequently, the slurry was filtered through a filter with a 1 μm opening. When the particle size distribution of the obtained slurry particles was measured using a centrifugal particle size measuring device (CAPA 500 manufactured by Horiba, Ltd.), the average particle size was 0.2 μm.
ジメチルテレフタレート１００部とエチレングリコール
６５部に触媒として酢酸マンガン０．０３８部、（０，
０３０モル％対ジメジメチルテレフタレート加え、１５
０〜２４０’Ｃで４時間メタノールを留去しつつエステ
ル交換反応を行なった。次いで、調製した窒化チタンの
グリコールスラリ１１部（窒化チタンとして１重量％対
ジメチルテレフタレート）、リン酸トリメチル０．０２
２部および重合触媒として０．０４部の三酸化アンチモ
ンを添加した後、１ｍ１ｌｌＨ（ＩＩ以下の高真空下で
３．５時間重縮合反応を行ない［η］＝０．６４０、軟
化点＝ ２６２．８℃のポリマを得た。ハンター型色差
計を用いて測定したポリマのＬ値は１４．０． ａ値は
−０，３、ｂ値は−０，３であり、黒色として優れたも
のであった。100 parts of dimethyl terephthalate and 65 parts of ethylene glycol, 0.038 part of manganese acetate as a catalyst, (0,
030 mol% to dimedimethyl terephthalate plus 15
The transesterification reaction was carried out at 0 to 240'C for 4 hours while distilling methanol off. Next, 11 parts of the prepared glycol slurry of titanium nitride (1% by weight as titanium nitride to dimethyl terephthalate), 0.02 parts of trimethyl phosphate
After adding 2 parts of antimony trioxide and 0.04 parts of antimony trioxide as a polymerization catalyst, a polycondensation reaction was carried out for 3.5 hours under a high vacuum of 1 ml 1 H (II or less) [η] = 0.640, softening point = 262. A polymer was obtained at 8°C.The L value of the polymer measured using a Hunter color difference meter was 14.0.The a value was -0.3, the b value was -0.3, and it was excellent as a black color. there were.
また、ポリマを２枚のカバーガラスの間に挾み２８０℃
にて溶融プレスし、急冷した俊、顕微鏡観察した結果は
粒子が均一に分布し、１μｍを越える凝集粒子、粗大粒
子は存在しなかった。In addition, the polymer was sandwiched between two cover glasses and heated to 280°C.
After melt pressing and quenching, microscopic observation revealed that the particles were uniformly distributed, with no aggregated particles or coarse particles larger than 1 μm.
比較実施例１
実施例１で窒化チタンに変えて一次粒子径０．１μｍの
カーボンブラックを用いる以外は実施例１と同様にして
スラリを調製した。スラリを１μｍの目開きのフィルタ
でスラリを濾過したが、目詰りを生じ、濾過できなかっ
たので、５μｍの目開きのフィルタで濾過を行なった。Comparative Example 1 A slurry was prepared in the same manner as in Example 1, except that carbon black with a primary particle size of 0.1 μm was used instead of titanium nitride. The slurry was filtered through a filter with an opening of 1 .mu.m, but the slurry became clogged and could not be filtered, so it was filtered with a filter with an opening of 5 .mu.m.
得られたスラリ粒子の粒径分布を測定した結果平均粒径
は０．７μｍであった。As a result of measuring the particle size distribution of the obtained slurry particles, the average particle size was 0.7 μm.
次に、カーボンブラックのスラリを用いて実施例１と同
様にしてカーボンブラック含有量１重量％、［η］ ＝
０．６４３、軟化点＝ ２６２．５℃のポリマを得た
。Next, using a carbon black slurry, the carbon black content was 1% by weight, [η] =
A polymer with a softening point of 0.643° C. and a softening point of 262.5° C. was obtained.
ハンター型色差計を用いて測定したＬ値は２０．Ｏ，ａ
値は、＋０．１、ｂ値は−１，１であり、黒味が不足し
ていた。また、ポリマ中の粒子の分散状態を実施例１と
同様にして観察した結果、３μｍを越える凝集粒子が多
数点在し、粒子の分散性は不良であった。The L value measured using a Hunter type color difference meter is 20. O,a
The value was +0.1, the b value was -1.1, and the blackness was insufficient. Furthermore, as a result of observing the dispersion state of particles in the polymer in the same manner as in Example 1, many aggregated particles exceeding 3 μm were scattered, and the dispersibility of the particles was poor.
実施例２
平均−次粒子径０．１μｍ、最大粒子径０．８μｍの窒
化チタン１０部とエチレングリコール１００部、リンｉ
ｌ Ｏ，０１部およびテトラエチルアンモニウム水酸化
物０．０６部を添加し、ざらに平均直径０．１ｍｍのガ
ラスピーズを１００部添加し、３０ｏｏｒｐｍで３時間
攪拌してスラリを調製した。Example 2 10 parts of titanium nitride with an average primary particle size of 0.1 μm and a maximum particle size of 0.8 μm, 100 parts of ethylene glycol, and phosphorus i
1 part of 1 O and 0.06 part of tetraethylammonium hydroxide were added, and 100 parts of glass beads having an average diameter of 0.1 mm were added thereto, followed by stirring at 30 oorpm for 3 hours to prepare a slurry.
攪拌終了後、４００メツシユの金網でガラスピーズを分
離し、得られた窒化チタンのエチレングリコールスラリ
を目開き１．０μｍのフィルりで濾過した。After stirring, the glass beads were separated using a 400-mesh wire mesh, and the resulting slurry of titanium nitride in ethylene glycol was filtered through a filter with an opening of 1.0 μm.
得られたスラリ中の粒子の粒径分布を実施例１と同様に
して測定すると平均粒子径は０．１２μｍであった。The particle size distribution of the particles in the obtained slurry was measured in the same manner as in Example 1, and the average particle size was 0.12 μm.
エチレングリコールユニット／テレフタル酸ユニットモ
ル比１．２、反応率９８％のビス−β−ヒドロキシエチ
ルテレフタレート１７６部を反応器に２４０℃で貯貿し
、常圧でテレフタル酸１４４部とエチレングリコール６
４．６部（エチレングリコール／テレフタル酸モル比１
．２０ ＞のスラリを一定速度で連続的に３時間４５分
かけて供給した。スラリ供給中は反応系を２３０〜２４
５℃にコントロールして反応させながら、生成する水は
精留塔を通して連続的に留去した。スラリ供給終了後、
反応温度を２４５℃にコントロールしながら１時間反応
を継続して反応を完結させた。176 parts of bis-β-hydroxyethyl terephthalate with a molar ratio of ethylene glycol unit/terephthalic acid unit of 1.2 and a reaction rate of 98% was stored in a reactor at 240°C, and 144 parts of terephthalic acid and 6 parts of ethylene glycol were added at normal pressure.
4.6 parts (ethylene glycol/terephthalic acid molar ratio 1
．． 20> of the slurry was continuously fed at a constant rate over a period of 3 hours and 45 minutes. During slurry supply, the reaction system is heated to 230-24
While the reaction was controlled at 5° C., the water produced was continuously distilled off through a rectification column. After finishing slurry supply,
The reaction was continued for 1 hour while controlling the reaction temperature at 245°C to complete the reaction.
反応終了後反応生成物の５０重量％（１７６部）を次の
反応槽に移し、リン酸０．０２１部（リン原子の量とし
て生成するポリマに基づいた添加量４０ｐｐＨｌ ）を
添加した後、三酸化アンチモン０．０５部（アンチモン
原子の量として生成するポリマに基づいた添加１２５０
ｐＩ）ＩＩＩ＞を添加し、ざらに窒化チタンのエチレン
グリコールスラリ１８．４部（窒化チタンとして生成す
るポリマに基づいた添加量１重量％）を添加して、その
後７０分で０．０３ｍｍ Ｈｇに減圧すると同時に１３
０分で２８８℃まで昇温しで２８８℃、０．０３ｍｍ
＠ｇ下で重縮合せしめ、［η］＝０．６５３、軟化点＝
２６１．５℃のポリマを得た。ハンター型色差計を用
いて測定したＬ値は１Ｂ、０． ａ値は−０，２、ｂ値
はＯｌＯであり、黒色として優れたものであった。After the completion of the reaction, 50% by weight (176 parts) of the reaction product was transferred to the next reaction tank, and after adding 0.021 part of phosphoric acid (40 ppHl based on the amount of phosphorus atoms produced in the polymer), 0.05 parts of antimony oxide (addition based on the amount of antimony atoms formed in the polymer 1250
18.4 parts of an ethylene glycol slurry of titanium nitride (1% by weight based on the polymer produced as titanium nitride) was then added to 0.03 mm Hg over 70 minutes. 13 at the same time as decompressing
Temperature increased to 288℃ in 0 minutes, 288℃, 0.03mm
Polycondensation under @g, [η] = 0.653, softening point =
A polymer having a temperature of 261.5°C was obtained. The L value measured using a Hunter type color difference meter is 1B, 0. The a value was -0.2, the b value was OIO, and it was an excellent black color.
また、ポリマ中の粒子の分散状態を実施例１と同様にし
て観察した結果、粒子は均一に分布し、１μｍを越える
粗大凝集粒子は存在しなかった。Furthermore, the dispersion state of the particles in the polymer was observed in the same manner as in Example 1, and as a result, the particles were uniformly distributed, and there were no coarse agglomerated particles exceeding 1 μm.
実施例３および比較実施例２
実施例２で得たポリマを窒素雰囲気中１２０℃で５時間
乾燥した後、エクストルーダ型溶融紡糸機を用いて、溶
融温度２９０℃、滞留時間２０分、紡糸速度６０００ｍ
／分、ノズル孔数１２個の条件で紡糸し、マルチフィ
ラメント糸を得た。Example 3 and Comparative Example 2 After drying the polymer obtained in Example 2 at 120°C in a nitrogen atmosphere for 5 hours, using an extruder type melt spinning machine, the polymer was heated at a melting temperature of 290°C, a residence time of 20 minutes, and a spinning speed of 6000 m.
A multifilament yarn was obtained by spinning at 12 nozzle holes per minute.
紡糸性は良好であり、２日以上紡糸を継続しても糸切れ
の発生は皆無であった。また紡糸機内圧力はほとんど上
昇しなかった。The spinnability was good, and no yarn breakage occurred even after spinning for two days or more. Moreover, the pressure inside the spinning machine hardly increased.
また、得られたフィラメントのＬ値は１８．０で好適な
黒色であった。Furthermore, the obtained filament had an L value of 18.0 and a suitable black color.
一方、比較実施例１で得たポリマを用いて、同様に紡糸
を行なった結果、糸切れが頻発し、また紡糸機内圧も１
日で急激に上昇した。On the other hand, when spinning was performed in the same manner using the polymer obtained in Comparative Example 1, yarn breakage occurred frequently and the internal pressure of the spinning machine was 1.
It rose sharply by day.
実施例４および比較実施例３
実施例１で得たポリマを２９０℃で溶融押出し、９０℃
で縦方向に３．０倍、１３０℃で横方向に３．０倍延伸
した後、２２０℃で熱処理し、５０μｍの厚さのフィル
ムを作成した。得られたフィルムの９００部ｍでの透過
率は１．０％で十分な遮光性を有していた。Example 4 and Comparative Example 3 The polymer obtained in Example 1 was melt extruded at 290°C and extruded at 90°C.
The film was stretched 3.0 times in the longitudinal direction and 3.0 times in the transverse direction at 130° C., and then heat treated at 220° C. to produce a film with a thickness of 50 μm. The resulting film had a transmittance of 1.0% at 900 parts m, and had sufficient light-shielding properties.
Claims (1)
とも一種のグリコール成分よりなるポリエステルであり
、かつ微粒子状窒化チタンを含有してなるポリエステル
組成物。A polyester composition comprising a bifunctional acid component mainly consisting of an aromatic dicarboxylic acid and at least one type of glycol component, and containing particulate titanium nitride.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP12054185A JPH0670165B2 (en) | 1985-06-05 | 1985-06-05 | Polyester composition |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP12054185A JPH0670165B2 (en) | 1985-06-05 | 1985-06-05 | Polyester composition |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS61278558A true JPS61278558A (en) | 1986-12-09 |
| JPH0670165B2 JPH0670165B2 (en) | 1994-09-07 |
Family
ID=14788843
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP12054185A Expired - Fee Related JPH0670165B2 (en) | 1985-06-05 | 1985-06-05 | Polyester composition |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0670165B2 (en) |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1848761A2 (en) | 2004-11-12 | 2007-10-31 | Eastman Chemical Company | Polyester polymer and copolymer compositions containing titanium nitride particles |
| US7300967B2 (en) | 2004-11-12 | 2007-11-27 | Eastman Chemical Company | Polyester polymer and copolymer compositions containing metallic titanium particles |
| JP2008534739A (en) * | 2005-03-31 | 2008-08-28 | イーストマン ケミカル カンパニー | Polyester polymer and copolymer compositions comprising particles of one or more transition metal compounds |
| WO2008123097A1 (en) * | 2007-03-20 | 2008-10-16 | Toray Industries, Inc. | Black resin composition, resin black matrix, color filter and liquid crystal display |
| TWI404761B (en) * | 2005-09-16 | 2013-08-11 | Grupo Petrotemex Sa De Cv | Aluminum/alkaline or alkali/titanium containing polyesters having improved reheat, color and clarity |
| US8987408B2 (en) | 2005-06-16 | 2015-03-24 | Grupo Petrotemex, S.A. De C.V. | High intrinsic viscosity melt phase polyester polymers with acceptable acetaldehyde generation rates |
| EP2926992A1 (en) | 2014-03-24 | 2015-10-07 | Mitsubishi Polyester Film GmbH | White biaxially oriented polyester film with increased thermal conductivity |
| DE102014206696A1 (en) | 2014-04-07 | 2015-10-08 | Mitsubishi Polyester Film Gmbh | White biaxially oriented polyester film with increased thermal conductivity |
| US9267007B2 (en) | 2005-09-16 | 2016-02-23 | Grupo Petrotemex, S.A. De C.V. | Method for addition of additives into a polymer melt |
| CN115928250A (en) * | 2022-12-12 | 2023-04-07 | 南京众山电池电子有限公司 | Preparation method and application of polyester fiber insulating material |
-
1985
- 1985-06-05 JP JP12054185A patent/JPH0670165B2/en not_active Expired - Fee Related
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI392700B (en) * | 2004-11-12 | 2013-04-11 | 葛魯波派楚泰克斯公司 | Polyester polymer and copolymer compositions containing titanium nitride particles |
| US7300967B2 (en) | 2004-11-12 | 2007-11-27 | Eastman Chemical Company | Polyester polymer and copolymer compositions containing metallic titanium particles |
| US7368523B2 (en) * | 2004-11-12 | 2008-05-06 | Eastman Chemical Company | Polyester polymer and copolymer compositions containing titanium nitride particles |
| JP2008519903A (en) * | 2004-11-12 | 2008-06-12 | イーストマン ケミカル カンパニー | Polyester polymer and copolymer compositions comprising titanium nitride particles |
| EP1848761A2 (en) | 2004-11-12 | 2007-10-31 | Eastman Chemical Company | Polyester polymer and copolymer compositions containing titanium nitride particles |
| JP2008534739A (en) * | 2005-03-31 | 2008-08-28 | イーストマン ケミカル カンパニー | Polyester polymer and copolymer compositions comprising particles of one or more transition metal compounds |
| US8987408B2 (en) | 2005-06-16 | 2015-03-24 | Grupo Petrotemex, S.A. De C.V. | High intrinsic viscosity melt phase polyester polymers with acceptable acetaldehyde generation rates |
| TWI404761B (en) * | 2005-09-16 | 2013-08-11 | Grupo Petrotemex Sa De Cv | Aluminum/alkaline or alkali/titanium containing polyesters having improved reheat, color and clarity |
| US9267007B2 (en) | 2005-09-16 | 2016-02-23 | Grupo Petrotemex, S.A. De C.V. | Method for addition of additives into a polymer melt |
| US8329068B2 (en) | 2007-03-20 | 2012-12-11 | Toray Industries, Inc. | Black resin composition, resin black matrix, color filter and liquid crystal display |
| WO2008123097A1 (en) * | 2007-03-20 | 2008-10-16 | Toray Industries, Inc. | Black resin composition, resin black matrix, color filter and liquid crystal display |
| EP2926992A1 (en) | 2014-03-24 | 2015-10-07 | Mitsubishi Polyester Film GmbH | White biaxially oriented polyester film with increased thermal conductivity |
| DE102014206696A1 (en) | 2014-04-07 | 2015-10-08 | Mitsubishi Polyester Film Gmbh | White biaxially oriented polyester film with increased thermal conductivity |
| CN115928250A (en) * | 2022-12-12 | 2023-04-07 | 南京众山电池电子有限公司 | Preparation method and application of polyester fiber insulating material |
| CN115928250B (en) * | 2022-12-12 | 2024-05-28 | 南京众山电池电子有限公司 | Preparation method and application of polyester fiber insulating material |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0670165B2 (en) | 1994-09-07 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US4668732A (en) | Polyester composition and process for producing the same | |
| WO1998000365A1 (en) | Titanium oxide and resin composition | |
| JPS61278558A (en) | Polyester composition | |
| US4067855A (en) | Fiber and film forming polyester composition | |
| JPH0550534B2 (en) | ||
| JPS6411068B2 (en) | ||
| JP2560685B2 (en) | Method for producing polyester | |
| JPWO2006121121A1 (en) | Titanium oxide sol and method for producing polyalkylene terephthalate using the same | |
| JPS61278557A (en) | Pigmented polyester composition | |
| JPS5845227A (en) | Preparation of polyester having excellent particle dispersibility | |
| JP2919539B2 (en) | Polyester production method | |
| JPS5946254B2 (en) | Method for producing polyester with excellent particle dispersibility | |
| JPH05132611A (en) | Polyester composition for yarn | |
| JP3148351B2 (en) | Polyethylene naphthalate composition | |
| JP2645472B2 (en) | Method for producing polyester composition and polyester composition | |
| JP3523419B2 (en) | Method for producing polyester excellent in fine particle dispersibility | |
| JPS59100156A (en) | Production of polyester composition | |
| JPH0243764B2 (en) | HORIESUTERUSOSEIBUTSUNOSEIZOHOHO | |
| JPS648087B2 (en) | ||
| US3376249A (en) | Process incorporating sodium pyrophosphate treated kaolinite within polyester | |
| JP3574826B2 (en) | Polyester resin composition and method for producing the same | |
| JPH0713134B2 (en) | Method for producing polyester | |
| JPH023420A (en) | Preparation of aromatic polyester | |
| JPH01153717A (en) | Production of polyester | |
| JPS6239166B2 (en) |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| LAPS | Cancellation because of no payment of annual fees |