CN100999833A - Production process of poly-phenyl thio-ether fibre - Google Patents

Production process of poly-phenyl thio-ether fibre Download PDF

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CN100999833A
CN100999833A CN 200710019567 CN200710019567A CN100999833A CN 100999833 A CN100999833 A CN 100999833A CN 200710019567 CN200710019567 CN 200710019567 CN 200710019567 A CN200710019567 A CN 200710019567A CN 100999833 A CN100999833 A CN 100999833A
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polyphenylene sulfide
temperature
fiber
producing
spinning
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CN100523321C (en
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周仪
王琴云
周建平
何卫星
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江苏省纺织研究所有限公司
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Abstract

The process of producing polyphenylene sulfide fiber adopts excellent linear polyphenylene sulfide material, and includes melt spinning at 280-350 deg.c, heating with one heater at 250-320 deg.c during spinning, controlling the maintaining and cooling temperature reasonably, controlling the fiber winding speed at 300-1500 m/min, drafting the wound fiber at 80-280 deg.c, and settling at 150-300 deg.c. The present invention can produce polyphenylene sulfide fiber with high breaking strength, great elongation at break, excellent hot air shrinkage, etc. and is suitable for production of polyphenylene sulfide fiber.

Description

一种聚苯硫醚纤维的生产方法 A method of producing a polyphenylene sulfide fiber

技术领域 FIELD

本发明涉及纺织化纤行业,特别是特种纤维生产行业,具体地说是一种聚合物经熔融纺丝,拉伸定型后生成一种特种纤维,更具体地说是一种聚苯硫醚聚合物经熔融纺丝,拉伸定型后生成聚苯硫醚纤维的方法。 The present invention relates to the textile fiber industry, especially special fiber production industry, in particular a polymer is melt-spun, stretched shape after produce a special fiber, more particularly a polyphenylene sulfide polymer by melt spinning, polyphenylene sulfide fiber shape after stretching generation.

背景技术 Background technique

聚苯硫醚是一种特种工程材料,早在上世纪70年代就已实现了工业化生产,随着合成技术的提高,聚苯硫醚的性能不断提升,特别是线性聚苯硫醚的成功开发,使得聚苯硫醚纤维的工业化生产成为现实。 Polyphenylene sulfide is a special engineering materials, as early as the 1970s had achieved industrial production, with the improvement of synthesis of technology, performance polyphenylene sulfide on the rise, especially linear polyphenylene sulfide successful development so polyphenylene sulfide fiber industrial production become a reality. 由于聚苯硫醚纤维具有良好的热稳定性,可长期工作于190℃高温下;良好的阻燃性,极限氧指数大于31,正常情况下不燃烧,燃烧时发烟量低;良好的耐化学性,200℃以下尚未发现合适溶剂,仅次于PTFE;以及良好的蠕变性和电气性能等。 Since the polyphenylene sulfide fibers having good thermal stability, long-term work at a high temperature 190 deg.] C; good flame resistance, limiting oxygen index greater than 31, under normal circumstances without combustion, low smoke development upon combustion; good resistance chemical, below 200 ℃ not yet found a suitable solvent, after the PTFE; and creep resistance and good electrical properties. 使得聚苯硫醚纤维可广泛用作水泥、造纸、钢铁、燃煤电厂、垃圾焚烧厂等行业的高温过滤材料,以及耐高温防火服、缝纫线等产品。 Such that polyphenylene sulfide fibers can be widely used as high-temperature filter material cement, paper, steel, coal-fired power plants, incinerators and other industries, as well as high temperature fire suits, sewing and other products.

由于聚苯硫醚目前还未发现有合适的溶剂,因此聚苯硫醚纤维的工业化生产目前主要以熔融纺丝为主,这样不仅可以避免干、湿法纺丝所产生的溶剂回收等环境问题,同时还可以节省生产成本。 Since the polyphenylene sulfide has not yet found a suitable solvent, for industrial production of polyphenylene sulfide fibers mainly oriented in melt spinning, so not only to avoid dry, wet spinning solvent recovery arising from environmental issues such as , but also can save production costs. 另外由于聚苯硫醚熔点较高,加工温度相对较高,结晶度高等自身的一些特点,所以其熔融纺丝以及牵伸定型等工艺也存在特殊之处,特别是聚苯硫醚长丝不同于短纤维生产,它不仅对纺丝及牵伸定型等工艺有着特殊的要求,同时对聚苯硫醚原料也有着较高要求。 In addition, as higher melting point of polyphenylene sulfide, a relatively high processing temperatures, and high degree of crystallinity of some characteristics of their own, so the melt spinning and drawing process is also present special features like shape, especially a polyphenylene sulfide filaments of different in the production of staple fibers, which have special requirements not only on the spinning and drawing processes like shape, while a polyphenylene sulfide material also has a high requirement.

在国内,目前对聚苯硫醚纤维熔融纺丝的研究不多,特别是聚苯硫醚长丝纤维的纺丝更少,专利CN 1603477A提供的方法,适合于聚苯硫醚短纤维的生产,对于聚苯硫长丝纤维并不合适。 In China, research on the current melt-spun fibers of polyphenylene sulfide is not more, in particular polyphenylene sulfide filament spinning less, the method provided in Patent CN 1603477A, ​​is suitable for the production of polyphenylene sulfide staple fibers for polyphenylene sulfide filament fibers is not suitable.

发明内容 SUMMARY

本发明的目的是提供一种聚苯硫醚纤维的生产方法,特别是聚苯硫醚长丝纤维的生产方法,用本方法生产的聚苯硫醚纤维的制成率高,纤维的断裂强度、断裂伸长,干热收缩等性能都较优。 Object of the present invention is to provide a polyphenylene sulfide fiber production methods, especially for the production of polyphenylene sulfide filament fibers made by the present process for producing a high polyphenylene sulfide fiber, breaking strength of the fiber , breaking elongation, the dry heat shrinkage and other properties are better.

按照本发明提供的技术方案,聚苯硫醚纤维的生产方法包括a、切片预结晶及干燥:将线性结构的聚苯硫醚切片在真空转鼓或连续的干燥器中进行预结晶及干燥;在真空转鼓中进行预结晶及干燥时,真空度≤10KPa,温度控制在60~220℃;时间在2~48小时;在连续干燥器中进行预结晶和干燥时,干燥气体的露点控制在5℃以下,风温控制在15~200℃,时间在2~24小时;在线性结构的聚苯硫醚中, According to the aspect of the present invention provides, method of producing the polyphenylene sulfide fibers comprising a, pre-crystallization and drying sections: linear polyphenylene sulfide structure sections and dried in a pre-crystallized or continuous vacuum drum drier; when the pre-crystallized and dried in a vacuum drum, the vacuum degree ≤10KPa, temperature controlled at 60 ~ 220 ℃; time of 2 to 48 hours; in a continuous pre-dryer crystallization and drying, the drying gas dew point control the following 5 ℃, air temperature controlled at 15 ~ 200 ℃, time is 2 to 24 hours; linear polyphenylene sulfide structure, 单元的含量≥70%(mol/mol),分子量分散指数Mw/Mn≤5,熔融指数在10~800g/10min;b、熔融纺丝:将上述预结晶及干燥后的聚苯硫醚切片在螺杆纺丝设备中进行纺丝,纺丝温度280~350℃,喷丝板的喷丝孔孔径在0.1~1.0mm,喷丝孔长度与直径(L/D)比为2.0~10.0;c、缓冷及冷却:熔体从螺杆纺丝设备的喷丝板喷出后,分别经过一个保温缓冷区和一个冷却区,形成纺丝;其中保温缓冷区位于喷丝板下1~50cm,在保温缓冷区内设置有加热装置,保温缓冷区的温度控制在200~350℃;冷却区主要由以空气、N2、CO2中的一种或几中气体为冷却媒介组成的一个风冷区,风温控制在10~80℃;d、卷绕:经过冷却的纤维在按常规方法上油后进行卷绕,纺丝卷绕的速度控制在100~3000m/min;e、牵伸定型:在牵伸机中经过1~3道的牵伸过程,总牵伸倍率控制在1.5~8倍,牵伸温度为80~280 Content of ≥70% (mol / mol) units, a molecular weight dispersion index Mw / Mn≤5, a melt index of 10 ~ 800g / 10min; b, melt spinning: The above-described pre-crystallized and dried polyphenylene sulfide slices screw spinning apparatus for spinning a spinning temperature of 280 ~ 350 ℃, spinneret hole diameter spinneret at 0.1 ~ 1.0mm, the nozzle hole length to diameter (L / D) ratio of 2.0 ~ 10.0; c, cooling and slow cooling: after discharging from the spinneret screw melt spinning apparatus, respectively, through a heat slow cooling zone and a cooling zone to form a spinning; wherein heat slow cooling zone located below the spinneret 1 ~ 50cm, insulation slow cooling zone provided with a heating means, the temperature of heat slow cooling zone controlled at 200 ~ 350 ℃; consisting essentially of an air-cooled cooling zone with air, N2, CO2, one or several gas cooling medium consisting of zone, air temperature controlled at 10 ~ 80 ℃; d, wound: the cooled fibers wound in a conventional manner by the oil, in the spinning winding speed control 100 ~ 3000m / min; e, setting the draft : in the process of drafting drawing through the machine 1 to 3, the total draw ratio controlled to 1.5 to 8 times, draw temperature of 80 to 280 ,定型温度控制在150~300℃,牵伸速度控制在100~1000m/min,制成聚苯硫醚纤维,该聚苯硫醚纤维的单纤维线密度在0.5~10dtex。 , Setting temperature controlled at 150 ~ 300 ℃, drawing speed control 100 ~ 1000m / min, made of polyphenylene sulfide fibers, monofilament linear density of the polyphenylene sulfide fibers 0.5 ~ 10dtex.

本发明所选用的聚苯硫醚原料是一种线性结构的聚合物,并含 The selected material of the present invention is a polyphenylene sulfide polymer of a linear structure, and containing 结构单元,为充分体现聚苯硫醚自身的特点,在原料中上述结构单元的含量≥70%(mol/mol),最好能≥90%(mol/mol)。 Structural units, to fully reflect the polyphenylene sulfide own characteristics, the content of the feedstock in the structural units of ≥70% (mol / mol), preferably capable of ≥90% (mol / mol). 为充分体现线性聚合物的特点,所选的聚苯硫醚原料中,三官能团以上的基团含量应≤1%,能≤0.1%更好,最好能≤0.01%。 In order to fully reflect the characteristics of linear polymers, polyphenylene sulfide material selected, the group having three or more functional groups content should ≤1%, better able ≤0.1%, preferably ≤0.01%.

本发明所选的聚苯硫醚原料其分子量分布指数Mw/Mn≤5,分子量分布指数Mw/Mn≤2较好,最好是分子量分布指数Mw/Mn≤1.5,分子量分布指数过大,纺丝困难,纤维性能差。 Selected material of the present invention is a polyphenylene sulfide having a molecular weight distribution index Mw / Mn≤5, molecular weight distribution index Mw / Mn≤2 preferably, more preferably a molecular weight distribution index Mw / Mn≤1.5, molecular weight distribution index is too large, spinning silk difficulties, poor fiber properties.

本发明所选的聚苯硫醚原料其熔融指数(MFR)应在10~800g/10min,在15~500g/10min更好,最好在20~300g/10min,(测试标准:ASTM D1238-00)。 Selected material of the present invention is a polyphenylene sulfide having a melt index (MFR) should be 10 ~ 800g / 10min, at 15 ~ 500g / 10min, and most preferably at 20 ~ 300g / 10min, (Test Standard: ASTM D1238-00 ). 熔融指数过大,纤维难于成型,同时纤维的断裂强度较低。 Melt index is too large, the fiber molding difficult, while the lower breaking strength of the fiber. 相反熔融指数过低,原料挤出困难,难于加工。 Instead melt index is too low, the extruded material is difficult, difficult to process.

为方便熔融纺丝加工,本发明所选的聚苯硫醚原料最好选用切片形式而非粉末状态。 To facilitate the melt spinning process, the selected material of the present invention is preferably a polyphenylene sulfide powder form rather than a slice selection state. 为避免聚苯硫醚原料在螺杆的熔融挤出过程中产生堵料、压力波动、氧化、降解、交联等情况,在进行熔融纺丝前,最好对聚苯硫醚原料切片进行预结晶及干燥。 To prevent blocking material to produce a polyphenylene sulfide material in a molten screw extrusion process, pressure fluctuations, oxidation, degradation, crosslinking and the like, before carrying out melt spinning is preferably a polyphenylene sulfide material sections of the pre-crystallization and dry. 这个过程可以在真空转鼓中进行,也可以在连续的干燥器中进行。 This process may be performed in a vacuum drum may be performed in a continuous drier.

若选用在真空转鼓中进行聚苯硫醚原料切片的预结晶及干燥,其真空度需≤10KPa,或≤100Pa,最好≤10Pa;温度可以控制在60~220℃,最好为100~200℃;这一过程的时间一般控制在2~48小时,最好为4~24小时。 If the pre-selected for the crystallization of polyphenylene sulfide material slices and dried in a vacuum drum, degree of vacuum required ≤10KPa, or ≤100Pa, preferably ≤10Pa; the temperature can be controlled at 60 ~ 220 ℃, preferably 100 to 200 ℃; time control in this process is generally 2 to 48 hours, preferably 4 to 24 hours. 真空度不高,或露点温度高,干燥效果差,影响纺丝。 The degree of vacuum is not high, the dew point temperature or higher, the drying effect is poor, affecting spinning. 温度过高时间过长容易产生原料的氧化、交联等现象,改变原料的特性,影响纺丝及纤维性能;温度过低或时间过短,预结晶及干燥效果差,同样影响纺丝及纤维性能。 Temperature is too high for too long prone to oxidation phenomena, the crosslinked material or the like, to change the nature of the material, affect spinning and fiber properties; temperature is too low or the time is too short, poor drying and pre-crystallized, and also affects fiber spinning performance.

本发明中经干燥后的聚苯硫醚原料切片,在280~350℃进行熔融纺丝,纺丝温度主要取决于原料的特性,为减少聚苯硫醚的氧化,尽量减少其在螺杆及纺丝组件中的停留时间。 In the present invention, the polyphenylene sulfide material was dried chips, melt-spun at 280 ~ 350 ℃, spinning temperature depends on the nature of the material, to reduce oxidation of polyphenylene sulfide, and minimize the spinning screw the residence time wire assembly. 为提高聚苯硫醚的可纺性,须对喷丝板组件作如下调整,喷丝板上的喷丝孔孔径在0.1~1.0mm,喷丝孔长径(L/D)比在2.0~10.0较为合适,最好孔径在0.3~0.6mm,L/D在3.0~8.0。 To improve the spinnability polyphenylene sulfide, of the spinneret assembly should be adjusted as follows, spinneret hole diameter spinneret at 0.1 ~ 1.0mm, length of the nozzle hole diameter (L / D) ratio of 2.0 ~ 10.0 more appropriate pore size is preferably in the 0.3 ~ 0.6mm, L / D of 3.0 to 8.0.

本发明所说的聚苯硫醚纤维经喷丝孔挤出后首先通过一个保温缓冷区,这一区域主要是由一个加热装置组成,其位置在喷丝板下1~50cm,最好在5~30cm处,沿纤维通过方向安装;这一加热装置的长度为5~150cm,最好在20~100cm,这一保温缓冷区的温度控制在200~350℃,最好控制在250~320℃。 The present invention means a polyphenylene sulfide fiber after extrusion through the spinneret orifices through a first heat slow cooling zone, the region primarily consists of a heating unit, a position at which the nozzle plate 1 ~ 50cm, preferably 5 ~ 30cm, the mounting direction along the fiber by; the length of the heating means 5 ~ 150cm, preferably 20 ~ 100cm, the temperature of the heat slow cooling zone is controlled at 200 ~ 350 ℃, preferably at 250 to control 320 ℃.

本发明所说的加热装置其加热方式主要是电加热、联苯加热、油浴加热、红外线加热、热风加热等;其外形主要有保温筒式、套管式等,为了操作的便利性可以将其制成可开合的形式;此外对于红外线加热以及热风保温可以采用多孔面板及蜂窝面板的形式。 It said heating apparatus of the present invention which heating is mainly electric heating, biphenyl heating, oil bath heating, infrared heating, hot air heating or the like; its appearance cartridge main insulation, the sleeve type, etc., for the convenience of operation may be which is made in the form of openable closing; in addition to the hot air and infrared heating panels and a honeycomb form of a porous insulation panels may be employed.

本发明所说的聚苯硫醚纤维通过一个保温缓冷区后继续通过一个冷却区,其形式主要是风冷,风温控制在10~80℃,最好控制在20~50℃,冷却媒介主要为空气、N2或CO2,经此冷却后的聚苯硫醚纤维需上油处理,最后进行卷绕。 The present invention means a polyphenylene sulfide fibers after incubation continues through slow cooling zone through a cooling zone, which is the main form of air, the air temperature controlled at 10 ~ 80 ℃, preferably controlled at 20 ~ 50 ℃, cooling medium primary air, N2 or CO2, after this the required oil cooling polyphenylene sulfide fibers, and finally wound.

本发明所说的聚苯硫醚纤维其卷绕速度控制在100~3000m/min,根据聚苯硫醚原料的不同以及纤维单丝的粗细,其卷绕速度可以控制在200~2000m/min,通常其卷绕速度控制在300~1500m/min。 The present invention means a polyphenylene sulfide fiber which is wound on the speed control 100 ~ 3000m / min, according to the different thickness and single fibers of polyphenylene sulfide material, the winding speed can be controlled at 200 ~ 2000m / min, typically in its winding speed control 300 ~ 1500m / min. 纺丝速度太大,会造成纺丝张力大,成型差,毛丝多,不利于正常卷绕及后道加工。 The spinning speed is too large, it will cause the spinning tension, poor shape, wool yarn and more, is not conducive to the normal winding and after processing.

本发明所说的聚苯硫纤维其牵伸定型过程是一个在高于聚苯硫醚玻璃化温度环境中进行牵伸、定型的过程。 The present invention is said polyphenylene sulfide fiber which is a process of shaping the drawing above the glass transition temperature of the polyphenylene sulfide environment drafting, shaping process. 其加热媒介主要有电加热、过热蒸汽以及油浴。 Its main heating medium electric heating, an oil bath and superheated steam.

本发明所说的牵伸可以是1~3道的一个牵伸过程,根据聚苯硫醚纤维最终应用的不同,其牵伸温度、牵伸倍率及牵伸速度有所不同。 The present invention may be a draft of said drafting process 1 to 3, depending on the final application of the polyphenylene sulfide fibers, which draw temperature, draw rate and draw ratio is different. 总牵伸倍率控制在1.5~8倍,最好控制在2.5~6倍,牵伸温度为80~280℃,牵伸温度最好控制在90~250℃,定型温度控制在150~300℃,最好控制在180~280℃;牵伸速度控制在100~1000m/min,最好控制在200~800m/min。 The total draw ratio controlled to 1.5 to 8 times, preferably 2.5 to 6 times the control, drawing temperature is 80 ~ 280 ℃, drawing temperature is preferably controlled at 90 ~ 250 ℃, setting the temperature control in the 150 ~ 300 ℃, It is preferably controlled at 180 ~ 280 ℃; drawing speed is controlled 100 ~ 1000m / min, preferably controlled at 200 ~ 800m / min. 为进一步提高纤维的取向度和结晶度,同时为进一步降低纤维的干热收缩,其牵伸过程也可以通过2道或3道牵伸来进行,在进行多道牵伸过程中,其总牵伸倍数可以合理分配到每一道牵伸来完成。 To further enhance the orientation and crystallinity of the fibers, as well as further reducing the dry heat shrinkage fiber, which drawing processes may be performed by two or three drawing, drawing process during multi-channel, total pull extending multiple channels can be reasonably assigned to each drawing to complete. 如在2道牵伸过程中,第1道牵伸倍率为总牵伸倍率的0.1~20%,第2道牵伸倍率为总牵伸倍率的99.9~80%;在3道牵伸过程中,第1道牵伸倍率为总牵伸倍率的0.1~20%,第2道牵伸倍率为总牵伸倍率的99.8~70%;第3道牵伸倍率为总牵伸倍率的0.1~10%。 As in the two drawing process, a draw ratio of 0.1 to 20% of the total draw ratio, the draw ratio of 2 to 99.9 to 80% of the total draw ratio; 3 in the drafting process , a first draw ratio of 0.1 to 20% of the total draw ratio, the draw ratio of 2 to 99.8% of the total draw ratio to 70; a draw ratio of 3 total draw ratio of 0.1 to 10 %. 由上述过程所生产的聚苯硫醚纤维,其断裂强度、断裂伸长,干热收缩等性能都较优。 Produced by the process of a polyphenylene sulfide fiber, breaking strength, breaking elongation, the dry heat shrinkage and other properties are better.

本发明所说的聚苯硫醚纤维其最终的单纤维线密度在0.5~10dtex,最好控制在1~8dtex,最常用的线密度控制在1.5~6dtex;每束聚苯硫醚纤维可以有10~100根单纤维组成,最终应用也可有多束聚苯硫醚纤维合股而成。 The present invention is a polyphenylene sulfide fibers of said final monofilament linear density 0.5 ~ 10dtex, preferably controlled at 1 ~ 8dtex, most commonly in the line density control 1.5 ~ 6dtex; polyphenylene sulfide fibers per bundle can 10 to 100 individual fibers, the final application may be multiple beam polyphenylene sulfide fibers plied together.

本发明的特点在于,选用性能优良的聚苯硫醚原料,利用现有的化纤长丝生产设备,经过少许改造后即可以用于聚苯硫醚长丝纤维的生产,通过严格控制生产工艺,即可生产出性能优良的聚苯硫醚长丝纤维,生产设备的投入费用低,生产过程易管理,产品质量好。 Feature of the present invention is that the choice of a polyphenylene sulfide material with excellent performance, the use of conventional synthetic filament production equipment, through a little after the transformation can be used for the production of polyphenylene sulfide filament fibers, by strictly controlling the production process, to produce high performance polyphenylene sulfide filament fiber, low input costs of production equipment, production process easy to manage, good product quality.

具体实施方式 Detailed ways

实施例1聚苯硫醚原料切片采用线性聚苯硫醚,分子量分散指数Mw/Mn=1.9;熔融指数在44.6g/10min(ASTM D1238-00)。 Example 1 using a linear polyphenylene sulfide material sections polyphenylene sulfide, a molecular weight dispersion index Mw / Mn = 1.9; melt index 44.6g / 10min (ASTM D1238-00). 在熔融纺丝前,上述原料先在真空转鼓中进行预结晶及干燥,其温度为90~150℃,时间为24小时,真空度保持在≤1Pa。 , The raw material prior to melt-spinning in the pre-crystallized in vacuum drum dried and, at a temperature of 90 ~ 150 ℃, time of 24 hours, the degree of vacuum is maintained at ≤1Pa. 纺丝时螺杆温度:260~320℃;箱体温度:325℃;喷丝板孔径:0.35mm;长径比(L/D):4;保温缓冷区采用电加热保温套,保温缓冷区温度:280℃;冷却区的冷却风温度:25℃;卷绕速度:2000m/min;牵伸速度:600m/min;牵伸倍率:2倍,牵伸温度:100℃;定型温度:220℃。 Spinning screw temperature: 260 ~ 320 ℃; cabinet temperature: 325 ℃; spinneret pore diameter: 0.35mm; aspect ratio (L / D): 4; heat slow cooling zone electric heating jacket insulation, heat slow cooling zone temperature: 280 deg.] C; temperature of the cooling zone of cooling air: 25 deg.] C; winding speed: 2000m / min; drawing speed: 600m / min; draw ratio: 2 times, draw temperature: 100 deg.] C; fixing temperature: 220 ℃.

由上述原料及工艺所制得的聚苯硫醚纤维性能如下:纤维线密度:79.0dtex/18f;断裂强度:3.09cN/dtex;断裂伸长:24.2%;干热收缩:13.2%。 By the materials and processes the obtained polyphenylene sulfide fiber properties are as follows: Fiber linear density: 79.0dtex / 18f; breaking strength: 3.09cN / dtex; breaking elongation: 24.2%; dry heat shrinkage: 13.2%.

实施例2聚苯硫醚原料及其它工艺均与例1相同,喷丝板孔径:0.4mm;长径比(L/D):6。 Example 2 polyphenylene sulfide material, and other processes were the same as in Example 1, spinneret aperture: 0.4mm; aspect ratio (L / D): 6. 所制聚苯硫醚纤维性能如下:纤维线密度:110.2dtex/24f;断裂强度:3.25cN/dtex;断裂伸长:25.3%,干热收缩:14.1%。 Polyphenylene sulfide fibers prepared following properties: fiber linear density: 110.2dtex / 24f; breaking strength: 3.25cN / dtex; breaking elongation: 25.3%, a dry heat shrinkage: 14.1%.

实施例3聚苯硫醚原料切片采用线性聚苯硫醚,分子量分散指数Mw/Mn=1.7;熔融指数在25.2g/10min(ASTM D1238-00)。 Embodiment Example 3 polyphenylene sulfide material slices linear polyphenylene sulfide, a molecular weight dispersion index Mw / Mn = 1.7; melt index 25.2g / 10min (ASTM D1238-00). 其它工艺均与例1相同,喷丝板孔径:0.4mm;长径比(L/D):6;卷绕速度:1000m/min;牵伸速度:300m/min;分二道牵伸,各道的牵伸倍率分别为1.05,3.1,各道的牵伸温度分别为:100℃,120℃;定型温度为:250℃。 Other processes are the same as in Example 1, spinneret aperture: 0.4mm; aspect ratio (L / D): 6; winding speed: 1000m / min; drawing speed: 300m / min; drawing two points, each channel respectively 1.05,3.1 draw ratio, drawing temperature of each channel were: 100 ℃, 120 ℃; setting temperature: 250 ℃. 所制聚苯硫醚纤维性能如下:纤维线密度:115.3dtex/24f;断裂强度:3.51cN/dtex;断裂伸长:22.7%,干热收缩:11.6%。 Polyphenylene sulfide fibers prepared following properties: fiber linear density: 115.3dtex / 24f; breaking strength: 3.51cN / dtex; breaking elongation: 22.7%, a dry heat shrinkage: 11.6%.

实施例4聚苯硫醚原料切片采用线性聚苯硫醚,分子量分散指数Mw/Mn=2.5;熔融指数在62.8g/10min(ASTM D1238-00)。 Example 4 Example polyphenylene sulfide material slices linear polyphenylene sulfide, a molecular weight dispersion index Mw / Mn = 2.5; melt index 62.8g / 10min (ASTM D1238-00). 其它工艺均与例1相同,喷丝板孔径:0.4mm;长径比(L/D):6;卷绕速度:800m/min;牵伸速度:300m/min;分二道牵伸,各道的牵伸倍率分别为1.08,3.5,各道的牵伸温度分别为:100℃,120℃;定型温度为:250℃。 Other processes are the same as in Example 1, spinneret aperture: 0.4mm; aspect ratio (L / D): 6; winding speed: 800m / min; drawing speed: 300m / min; drawing two points, each channel respectively 1.08,3.5 draw ratio, drawing temperature of each channel were: 100 ℃, 120 ℃; setting temperature: 250 ℃. 所制聚苯硫醚纤维性能如下:纤维线密度:113.2dtex/24f;断裂强度:3.27cN/dtex;断裂伸长:24.7%,干热收缩:9.1%。 Polyphenylene sulfide fibers prepared following properties: fiber linear density: 113.2dtex / 24f; breaking strength: 3.27cN / dtex; breaking elongation: 24.7%, a dry heat shrinkage: 9.1%.

实施例5聚苯硫醚原料切片采用线性聚苯硫醚,分子量分散指数Mw/Mn=2.1;熔融指数在90.7g/10min(ASTM D1238-00)。 Example 5 linear polyphenylene sulfide material sections polyphenylene sulfide, a molecular weight dispersion index Mw / Mn = 2.1; melt index 90.7g / 10min (ASTM D1238-00). 其它工艺均与例1相同,纺丝时螺杆温度:260~300℃;箱体温度:315℃;喷丝板孔径:0.4mm;长径比(L/D):6;保温缓冷区采用电加热保温套,保温缓冷区温度:285℃;卷绕速度:1500m/min;牵伸速度:300m/min;分三道牵伸,各道的牵伸倍率分别为1.1,3.0,1.03各道的牵伸温度分别为:100℃,120℃,160℃;定型温度为:260℃。 Other processes are the same as in Example 1, the screw spinning temperature: 260 ~ 300 ℃; cabinet temperature: 315 ℃; spinneret pore diameter: 0.4mm; aspect ratio (L / D): 6; slow cooling zone using heat electric heating jacket insulation, heat slow cooling zone temperature: 285 ℃; winding speed: 1500m / min; drawing speed: 300m / min; drawing three min, the draw ratio of each channel are each 1.1,3.0,1.03 draw temperature channel were: 100 ℃, 120 ℃, 160 ℃; setting temperature: 260 ℃. 所制聚苯硫醚纤维性能如下:纤维线密度:112.8dtex/24f;断裂强度:3.93cN/dtex;断裂伸长:20.4%,干热收缩:7.8%。 Polyphenylene sulfide fibers prepared following properties: fiber linear density: 112.8dtex / 24f; breaking strength: 3.93cN / dtex; breaking elongation: 20.4%, a dry heat shrinkage: 7.8%.

实施例6聚苯硫醚原料切片采用线性聚苯硫醚,分子量分散指数Mw/Mn=1.8;熔融指数在160.6g/10min(ASTM D1238-00)。 Example 6 Example polyphenylene sulfide material slices linear polyphenylene sulfide, a molecular weight dispersion index Mw / Mn = 1.8; melt index 160.6g / 10min (ASTM D1238-00). 其它工艺均与例2相同,保温缓冷区采用电加热保温套,保温缓冷区温度:285℃;卷绕速度:1200m/min;牵伸速度:300m/min;分三道牵伸,各道的牵伸倍率分别为1.08,3.3,1.03各道的牵伸;定型温度为:255℃。 Other processes were the same as in Example 2, heat slow cooling zone electric heating jacket insulation, heat slow cooling zone temperature: 285 ℃; winding speed: 1200m / min; drawing speed: 300m / min; drawing three points, each Road draw ratio are drawn 1.08,3.3,1.03 each channel; setting temperature: 255 ℃. 所制聚苯硫醚纤维性能如下:纤维线密度:116.7dtex/24f;断裂强度:3.85cN/dtex;断裂伸长:21.6%,干热收缩:6.6%。 Polyphenylene sulfide fibers prepared following properties: fiber linear density: 116.7dtex / 24f; breaking strength: 3.85cN / dtex; breaking elongation: 21.6%, a dry heat shrinkage: 6.6%.

实施例7聚苯硫醚原料切片采用线性聚苯硫醚,分子量分散指数Mw/Mn=1.6;熔融指数在180.1g/10min(ASTM D1238-00)。 Example 7 A linear polyphenylene sulfide material sections polyphenylene sulfide, a molecular weight dispersion index Mw / Mn = 1.6; melt index 180.1g / 10min (ASTM D1238-00). 其它工艺均与例6相同,卷绕速度:1200m/min;牵伸速度:300m/min;牵伸倍率为3.8;牵伸温度:120℃;定型温度为:260℃。 Other processes are the same as in Example 6, winding speed: 1200m / min; drawing speed: 300m / min; draw ratio of 3.8; draw temperature: 120 ℃; setting temperature: 260 ℃. 所制聚苯硫醚纤维性能如下:纤维线密度:114.8dtex/24f;断裂强度:3.65cN/dtex;断裂伸长:23.6%,干热收缩:9.8%。 Polyphenylene sulfide fibers prepared following properties: fiber linear density: 114.8dtex / 24f; breaking strength: 3.65cN / dtex; breaking elongation: 23.6%, a dry heat shrinkage: 9.8%.

实施例8聚苯硫醚原料切片采用线性聚苯硫醚,分子量分散指数Mw/Mn=2.0;熔融指数在220.5g/10min(ASTM D1238-00)。 Example 8 Example polyphenylene sulfide material slices linear polyphenylene sulfide, a molecular weight dispersion index Mw / Mn = 2.0; melt index 220.5g / 10min (ASTM D1238-00). 其它工艺均与例6相同,保温缓冷区采用电加热保温套,保温缓冷区温度:280℃;卷绕速度:1000m/min;牵伸速度:300m/min;牵伸倍率为3.9;牵伸温度:110℃;定型温度为:260℃。 Other processes were the same as in Example 6, the cold zone heat slow electric heating jacket insulation, heat slow cooling zone temperature: 280 ℃; winding speed: 1000m / min; drawing speed: 300m / min; draw ratio of 3.9; pull stretching temperature: 110 ℃; setting temperature: 260 ℃. 所制聚苯硫醚纤维性能如下:纤维线密度:118.8dtex/24f;断裂强度:3.27cN/dtex;断裂伸长:25.6%,干热收缩:11.8%。 Polyphenylene sulfide fibers prepared following properties: fiber linear density: 118.8dtex / 24f; breaking strength: 3.27cN / dtex; breaking elongation: 25.6%, a dry heat shrinkage: 11.8%.

Claims (10)

1.一种聚苯硫醚纤维的生产方法,a、切片预结晶及干燥:将线性结构的聚苯硫醚切片在真空转鼓或连续的干燥器中进行预结晶及干燥;在真空转鼓中进行预结晶及干燥时,真空度≤10KPa,温度控制在60~220℃;时间在2~48小时;在连续干燥器中进行预结晶和干燥时,干燥气体的露点控制在5℃以下,风温控制在15~200°,时间在2~24小时;在线性结构的聚苯硫醚中, 1. A method of producing a polyphenylene sulfide fiber, a, pre-crystallization and drying sections: linear polyphenylene sulfide structure sections and dried in a pre-crystallized or continuous vacuum drum drier; vacuum drum in pre-crystallization and drying, the degree of vacuum ≤10KPa, temperature controlled at 60 ~ 220 ℃; time of 2 to 48 hours; pre-crystallization and drying, the drying gas dew point controlled at 5 ℃ continuous drier, air temperature controlled at 15 ~ 200 °, at the time of 2 to 24 hours; linear polyphenylene sulfide structure, 单元的含量≥70%(mol/mol),分子量分散指数Mw/Mn≤5,熔融指数在10~800g/10min;b、熔融纺丝:将上述预结晶及干燥后的聚苯硫醚切片在螺杆纺丝设备中进行纺丝,纺丝温度280~350℃,喷丝板的喷丝孔孔径在0.1~1.0mm,喷丝孔长度与直径(L/D)比为2.0~10.0;c、缓冷及冷却:熔体从螺杆纺丝设备的喷丝板喷出后,分别经过一个保温缓冷区和一个冷却区,形成纺丝;其中保温缓冷区位于喷丝板下1~50cm,在保温缓冷区内设置有加热装置,保温缓冷区的温度控制在200~350℃;冷却区主要由以空气、N2、CO2中的一种或几中气体为冷却媒介组成的一个风冷区,风温控制在10~80℃;d、卷绕:经过冷却的纤维在按常规方法上油后进行卷绕,纺丝卷绕的速度控制在100~3000m/min;e、牵伸定型:在牵伸机中经过1~3道的牵伸过程,总牵伸倍率控制在1.5~8倍,牵伸温度为80~280 Content of ≥70% (mol / mol) units, a molecular weight dispersion index Mw / Mn≤5, a melt index of 10 ~ 800g / 10min; b, melt spinning: The above-described pre-crystallized and dried polyphenylene sulfide slices screw spinning apparatus for spinning a spinning temperature of 280 ~ 350 ℃, spinneret hole diameter spinneret at 0.1 ~ 1.0mm, the nozzle hole length to diameter (L / D) ratio of 2.0 ~ 10.0; c, cooling and slow cooling: after discharging from the spinneret screw melt spinning apparatus, respectively, through a heat slow cooling zone and a cooling zone to form a spinning; wherein heat slow cooling zone located below the spinneret 1 ~ 50cm, insulation slow cooling zone provided with a heating means, the temperature of heat slow cooling zone controlled at 200 ~ 350 ℃; consisting essentially of an air-cooled cooling zone with air, N2, CO2, one or several gas cooling medium consisting of zone, air temperature controlled at 10 ~ 80 ℃; d, wound: the cooled fibers wound in a conventional manner by the oil, in the spinning winding speed control 100 ~ 3000m / min; e, setting the draft : in the process of drafting drawing through the machine 1 to 3, the total draw ratio controlled to 1.5 to 8 times, draw temperature of 80 to 280 ,定型温度控制在150~300℃,牵伸速度控制在100~1000m/min,制成聚苯硫醚纤维,该聚苯硫醚纤维的单纤维线密度在0.5~10dtex。 , Setting temperature controlled at 150 ~ 300 ℃, drawing speed control 100 ~ 1000m / min, made of polyphenylene sulfide fibers, monofilament linear density of the polyphenylene sulfide fibers 0.5 ~ 10dtex.
2.如权利要求1所述聚苯硫醚纤维的生产方法,其特征是:线性结构的聚苯硫醚中, 2. The method of producing a polyphenylene sulfide fiber as claimed in claim, characterized in that: a linear polyphenylene sulfide structure, 单元的含量≥90%(mol/mol),分子量分散指数Mw/Mn≤2,熔融指数在20~300g/10min(ASTM D1238-00)。 Content of units ≥90% (mol / mol), a molecular weight dispersion index Mw / Mn≤2, a melt index of 20 ~ 300g / 10min (ASTM D1238-00).
3.如权利要求1所述聚苯硫醚纤维的生产方法,其特征是:喷丝板的喷丝孔孔径在0.3~0.6mm,喷丝孔长度与直径(L/D)比为3.0~8.0。 3. The method of producing a polyphenylene sulfide fiber as claimed in claim, characterized in that: the nozzle hole diameter of the spinneret 0.3 ~ 0.6mm, the nozzle hole length to diameter (L / D) ratio of 3.0 to 8.0.
4.如权利要求1所述聚苯硫醚纤维的生产方法,其特征是:加热装置主要是可开合的保温筒或保温套管,其加热方式主要是电加热、联苯加热、油浴加热;或者,加热装置为多孔面板或蜂窝面板,加热方式为红外线加热或热风加热。 4. The method for producing a polyphenylene sulfide fiber as claimed in claim, characterized in that: the main heating means is retractable cylindrical insulation or insulation sleeve, which is heated mainly through electrical heating, biphenyl heated in an oil bath heating; Alternatively, the heating means is a porous honeycomb panel or panels, for the heating hot air heating or infrared heating.
5.如权利要求1所述聚苯硫醚纤维的生产方法,其特征是:在牵伸定型时,总牵伸倍率控制在2.5~6倍;牵伸温度在90~250℃,定型温度控制在180~280℃,牵伸速度控制在200~800m/min。 Temperature control in setting the draw temperature 90 ~ 250 ℃,; shape during drawing, the total draw ratio of 2.5 to 6 times the control: The method as claimed in producing the polyphenylene sulfide fiber of claim 1, characterized in that at 180 ~ 280 ℃, drawing speed control 200 ~ 800m / min.
6.如权利要求1所述聚苯硫醚纤维的生产方法,其特征是:在采用2道牵伸过程时,总牵伸倍率的0.1~20%在第1道牵伸过程中牵伸,总牵伸倍率的99.9~80%在第2道牵伸过程中牵伸。 6. The method of producing a polyphenylene sulfide fiber as claimed in claim, characterized in that: in the drafting process when using two, 0.1 to 20% of the total draw ratio in the first drawing process in a drawing, the total draw ratio of 99.9 to 80% of the draft in the drafting process of the two.
7.如权利要求1所述聚苯硫醚纤维的生产方法,其特征是:在采用3道牵伸过程时,总牵伸倍率的0.1~20%在第一道牵伸过程中牵伸,总牵伸倍率的99.8~70%在第2道牵伸过程中牵伸,总牵伸倍率的0.1~10%在第3道牵伸过程中牵伸。 7. The method for producing a polyphenylene sulfide fiber as claimed in claim, characterized in that: in the drafting process when using 3, from 0.1 to 20% of the total draw ratio of the draft in the drafting process of the first channel, the total draw ratio of 99.8 to 70% of the draft in the drafting process 2, the total draw ratio of 0.1 to 10% of the draft in the drafting process 3.
8.如权利要求1所述聚苯硫醚纤维的生产方法,其特征是:聚苯硫醚纤维是指由10~400根单纤维组成的单一长丝丝束,或者由上述丝束合股成的聚苯硫醚纤维长丝丝束。 8. The method of producing a polyphenylene sulfide fiber as claimed in claim, characterized in that: polyphenylene sulfide fibers which are single-filament yarn composed of 10 to 400 individual fibers or strands into the above partnership polyphenylene sulfide fiber filament tow.
9.如权利要求1所述聚苯硫醚纤维的生产方法,其特征是:保温缓冷区位于喷丝板下5~30cm处,保温缓冷区的温度控制在250~320℃。 9. The method of producing a polyphenylene sulfide fiber as claimed in claim, characterized in that: heat slow cooling zone located at 5 ~ 30cm below the spinneret, the temperature of heat slow cooling zone controlled at 250 ~ 320 ℃.
10.如权利要求1所述聚苯硫醚纤维的生产方法,其特征是:线性结构的聚苯硫醚中, 10. The method of producing a polyphenylene sulfide fiber as claimed in claim, characterized in that: a linear polyphenylene sulfide structure, 单元的含量≥90%(mol/mo1),分子量分散指数Mw/Mn≤2,熔融指数在20~300g/10min(ASTM D1238-00)。 Content of units ≥90% (mol / mo1), a molecular weight dispersion index Mw / Mn≤2, a melt index of 20 ~ 300g / 10min (ASTM D1238-00).
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