WO2013120415A1 - 超高分子量聚乙烯绳网用有色纤维制备方法 - Google Patents

超高分子量聚乙烯绳网用有色纤维制备方法 Download PDF

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WO2013120415A1
WO2013120415A1 PCT/CN2013/071246 CN2013071246W WO2013120415A1 WO 2013120415 A1 WO2013120415 A1 WO 2013120415A1 CN 2013071246 W CN2013071246 W CN 2013071246W WO 2013120415 A1 WO2013120415 A1 WO 2013120415A1
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molecular weight
colored
weight polyethylene
high molecular
ultra
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PCT/CN2013/071246
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English (en)
French (fr)
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陈成泗
许史安
王华海
李泉荣
陆展飞
周银环
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宁波大成新材料股份有限公司
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Publication of WO2013120415A1 publication Critical patent/WO2013120415A1/zh

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    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
    • D01F6/46—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polyolefins
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00—General methods for the manufacture of artificial filaments or the like
    • D01F1/02—Addition of substances to the spinning solution or to the melt
    • D01F1/04—Pigments

Definitions

  • the invention relates to the field of high performance fiber technology, and relates to a method for preparing a colored fiber for ultra high molecular weight polyethylene rope. Background technique
  • Ultra High Molecular Weight Polyethylene Fiber is one of the world's three high-tech fibers (carbon fiber, aramid, UHMWPE). It is a high-strength, low-strength, high-modulus high-performance fiber that was successfully developed in the late 1970s and industrialized in the 1980s. It has developed rapidly in the past 20 years, and its production technology has passed the jelly-spinning method. Production, the main preparation method is divided into two steps: First, the ultra-high molecular weight powder resin and a large amount of solvent are prepared into a super high molecular weight polyethylene mixed spinning solution, and the twin-screw extruder is used to extrude and solidify into ultra-high molecular weight.
  • Polyethylene jelly fiber Secondly, the jelly fiber is extracted, dried, and three times of super-heat drawing to obtain ultra-high molecular weight polyethylene fiber, the fiber is white, the fiber can not meet the application of marine engineering high-strength rope, fishing net, etc. Color requirements. Secondly, since the ultrahigh molecular weight polyethylene fiber has a high molecular density and a non-functional group surface is smooth, it cannot be dyed.
  • Chinese Patent Application discloses a method for preparing colored high-strength polyethylene fibers, which comprises adding ultra-high molecular weight polyethylene powder to white mineral oil, mixing with inorganic pigment, and then heating and spinning in a twin-screw extruder.
  • Ultra-high molecular weight polyethylene jelly fiber after extraction, drying and drawing to obtain colored high-strength polyethylene fiber, the method has the color pigment faded when the twin-screw is swollen at high temperature, and then the large amount of pigment is dissolved in the mineral oil solvent, Conducive to solvent recovery, high cost, light fiber color, poor uniformity and other defects.
  • Chinese patent application discloses a method for preparing ultra-high molecular weight polyethylene red fiber: (1) adding red nano-scale organic pigment to 4.5 million ultra-high molecular weight polyethylene powder, mixing and mixing to form ultra-high a colored polymer of molecular weight polyethylene; (2) a high-shear molecular weight polyethylene spinning mixture prepared by high-shearing of a colored polymer with 70# solvent white oil and an antioxidant; (3) spinning step (2) The silk mixture is fed into the screw extruder by a high shear pump, and the extruded spinning wire is used to solidify the colored frozen collagen filaments through a cold water bath, and then subjected to extraction drying and multi-stage heat drawing to obtain ultrahigh molecular weight polyethylene red fibers.
  • the disclosed technology First, the presence of nano-scale pigments is difficult to avoid mixing in a large amount of solvent white oil, affecting the quality of solvent recovery; Meet the production of red, yellow and orange fibers.
  • Chinese Patent Application (200910154196.9) discloses a method for producing ultrahigh molecular weight polyethylene colored fine denier fibers, which are extruded through a twin-screw extruder after three super-high molecular weight polyethylene colored emulsions prepared by matching schemes. It is sprayed in a water bath, then extracted, dried and ultra-stretched into ultra-high molecular weight polyethylene colored fine fibers.
  • the first disclosed technology is that nano-scale pigments are also melted under high temperature. It is difficult to avoid pigment mixing in a large amount of solvent white oil, which affects the quality of solvent recovery and the uniformity of colored fibers. Secondly, it can only meet the fineness of 2D ⁇ 2.5DX 164F. Fiber production. Summary of the invention
  • the invention relates to a method for preparing colored fiber for ultra high molecular weight polyethylene rope net, and the specific steps are as follows: 3 ⁇ 4 mouth:
  • step 1
  • Ultra-high molecular weight polyethylene resin and HDPE polyethylene and organic pigment toner are used to prepare ultra-high molecular weight polyethylene colored masterbatch by vented twin-screw extruder, and the prepared colored masterbatch is ground into ultrahigh molecular weight polyethylene. Powdered colored masterbatch;
  • Ultra-high molecular weight polyethylene resin is selected, white oil (mineral oil) is used as solvent, and the above ultra-high molecular weight polyethylene powdery colored master batch is added to prepare a colored spinning solution body: input into a swelling kettle for mixing and swelling, and continuous stirring is performed.
  • Ultra-high molecular weight polyethylene resin and ultra-high molecular weight polyethylene colored masterbatch reach the state of mixed milk, cool the swollen colored resin solution, and transport it to twin-screw extruder plasticizing extrusion spinning and water bath to solidify Molecular weight polyethylene colored jelly fiber;
  • the prepared ultra-high molecular weight polyethylene colored jelly fiber 1 first through the extraction process, using a hydrocarbon cleaning agent to extract and separate the white oil solvent; 2 the extracted nascent fiber is then subjected to hot air drying; 3 after drying the fiber After three hot stretching; 4 fiber shaping: After three hot stretching and then heat setting, finally, the ultra high molecular weight polyethylene fiber is wound into a cylinder to obtain a finished colored fiber.
  • the production method has the following advantages: First, the organic pigment is fully utilized, and the pigment is not easily mixed. In solvent white oil; Second, uniform coloration, high color fastness, resistance to long-term seawater immersion and anti-ultraviolet light; third is to meet the preparation of various colors, fiber size 1600D - 3200D multifilament, single filament fineness is 5 ⁇ 10 denier, the elongation is 4% ⁇ 4.5%, and the fiber breaking strength is 30 ⁇ 33g/D, which can meet the requirements of high-strength ropes and offshore fishing trawls, deep-sea breeding large fences.
  • the specifications are 1600D 300F, 2000D 300F, 2400D 320F, 3000D 320F, 3200D 320F. ⁇ V, a single-filament fineness of 5 to 10 denier, an elongation of 4% to 5%, and a strength average of >3 ( ⁇ /0) of colored ultra-high molecular weight polyethylene fiber, which can meet different specifications of rope and fishing net applications. . detailed description
  • the invention relates to a method for preparing colored fiber for ultra high molecular weight polyethylene rope net, and the specific steps are as follows: 3 ⁇ 4 mouth:
  • step 1
  • ultra-high molecular weight polyethylene resin with a molecular weight of 100-1.2 million plus HDPE polyethylene and organic pigment toner, the weight ratio is 10: 2: 1; the color of the toner can be prepared according to the requirements of the fishing net, such as: black, blue, green , brown, and so on.
  • the ultrahigh molecular weight polyethylene masterbatch was prepared by a vented twin-screw extruder, and the twin-screw was heated at 160 ° C to 180 ° C, and the extrusion speed was 120 to 160 rpm. The prepared masterbatch is then ground into an ultrahigh molecular weight polyethylene powdery colored masterbatch having a particle size of 20-30 mesh.
  • the swell tank is mixed and swelled, the swelling temperature is 90-115 ° C, the swelling time is 1.5 ⁇ 3 hours, and the stirring is continued, so that the ultra-high molecular weight polyethylene resin and the ultra-high molecular weight polyethylene colored master batch reach the mixed milk state, After the swollen colored resin solution is cooled to 50 ⁇ 60 °C, it is sent to the twin-screw extruder for plasticizing extrusion spinning and water bath to solidify. The water bath solidification time is 1 ⁇ 2 minutes, and the temperature is 4 °C ⁇ 8 °C. , preparing ultra-high molecular weight polyethylene colored jelly fiber, the diameter of the jelly fiber is 0.5 ⁇ 0.8mm.
  • the prepared ultrahigh molecular weight polyethylene colored jelly fiber 1 is extracted in a known manner Take, use hydrocarbon cleaning agent to extract and separate the white oil solvent; 2 extract the nascent fiber and then hot air drying, the hot air temperature is controlled at 60-80 °C; 3 after drying, the fiber is heated in a known manner Stretching, a total of three hot stretching, the first stretching ratio is 10 ⁇ 15 times, the hot air temperature is 120 ° C ⁇ 135 ° C; the second stretching ratio is 1.5 ⁇ 2 times, the hot air temperature is 125 ° C ⁇ 140 °C; The third draw ratio is 1.2-1.5 times, the hot air temperature is 130 °C ⁇ 150 °C; 4 The fiber is heat set according to the known method: The set temperature is 130 °C ⁇ 140 °C . After three times of hot drawing and heat setting, the ultrahigh molecular weight polyethylene fiber is wound into a cylinder filled with a color fiber finished product.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Textile Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Artificial Filaments (AREA)

Abstract

本发明涉及一种超高分子量聚乙烯绳网用有色纤维的制备方法。本发明分三个步骤实施： 1.采用超高分子量聚乙烯树脂加HDPE聚乙烯和有机颜料色粉，制备超高分子量聚乙烯粉状有色母料。2.用超高分子量聚乙烯树脂，选用白油作溶剂，再加上述超高分子量聚乙烯粉状有色母料，制备有色纺丝溶液体，进行混合溶胀，冷却后挤压喷丝和水浴凝固，制备超高分子量聚乙烯有色冻胶纤维。3.将已制备的超高分子量聚乙烯有色冻胶纤维：经萃取工序，进行热风烘干，干燥后再经三道热拉伸，最后纤维定型。有色超高分子量聚乙烯纤维，能满足不同规格的绳索和渔网应用。

Description

超高分子量聚乙烯绳网用有色纤维制备方法 技术领域
本发明涉及高性能纤维技术领域， 涉及一种超高分子量聚乙烯绳网 用有色纤维的制备方法。 背景技术
超高分子量聚乙烯纤维（ UHMWPE )是当今世界三大高科技纤维（碳 纤维、 芳纶、 UHMWPE )之一。 是上世纪 70年代末研制成功， 80年代 实现产业化的一种高强度、 低延伸、 高模量的高性能纤维， 近 20年来有 较快的发展， 其生产技术均通过冻胶纺丝法生产， 主要制备方法分为二 个步骤完成： 一是将超高分子量粉末树脂与大量溶剂配制超高分子量聚 乙烯混合纺丝液， 通过双螺杆挤压机， 挤出喷丝凝固成超高分子量聚乙 烯冻胶纤维； 二是将冻胶纤维经萃取、 干燥、 三道超倍热牵伸获得超高 分子量聚乙烯成品纤维， 纤维均为白色， 该纤维不能满足应用海洋工程 高强绳索、 渔网等颜色要求。 其次由于超高分子量聚乙烯纤维分子密度 高， 无官能团表面光滑， 也无法进行染色解决。
超高分子量聚乙烯制备有色纤维， 是当今行业专家的研究热点。 中国专利申请（ZL200810014184.1 )公开一种有色高强聚乙烯纤维 制备方法， 其将超高分子量聚乙烯粉末加入于白色矿物油， 再加无机颜 料混合后， 经双螺杆挤出机内加热纺制超高分子量聚乙烯冻胶纤维， 再 经萃取、 干燥及牵伸后获得有色高强聚乙烯纤维， 该方法存在无机颜料 在双螺杆高温溶胀时颜色淡化， 其次大量颜料溶解在矿物油溶剂中， 不 利于溶剂回收， 成本高， 纤维颜色浅， 均匀性差等缺陷。
中国专利申请（ 201110090622.4 )公开一种超高分子量聚乙烯红色纤 维的制备方法： （1)其将红色纳米级有机颜料加入到 450万超高分子量聚 乙烯粉末中， 进行充分搅拌混合， 形成超高分子量聚乙烯的有色聚合体； (2)再将有色聚合体与 70#溶剂白油及抗氧剂进行高剪切制备超高分子量 聚乙烯纺丝混合液； （3)将步骤 (2)纺丝混合液用高剪切泵输入螺杆挤压机， 挤出喷丝经冷水浴凝固有色冻胶原丝， 之后再经萃取干燥及多级热牵伸 获得超高分子量聚乙烯红色纤维。 该公开技术： 一是存在纳米级颜料难 以避免混合在大量溶剂白油中， 影响溶剂回收质量； 二是公开技术只能 满足红色、 黄色、 橙色纤维生产。
中国专利申请（ 200910154196.9 )公开一种超高分子量聚乙烯有色细 旦纤维的生产方法， 其三种实施匹配方案制备的超高分子量聚乙烯有色 乳状混合液后， 都经过双螺杆挤出机挤压喷丝水浴处理， 再经萃取、 干 燥、 超倍拉伸成超高分子量聚乙烯有色细旦纤维。 该公开技术一是同样 存在纳米级颜料在高温熔融下， 难以避免颜料混合在大量溶剂白油中， 影响溶剂回收质量和有色纤维的均匀性， 二是只能满足 2D ~ 2.5D X 164F 的细旦纤维生产。 发明内容
上述背景技术中提到的三项现有技术都存在缺陷， 而更不能满足应 用于高强绳索、 渔网的生产要求。 本发明的目的， 在于提供制备高强绳 索和高强渔网用的超高分子量聚乙烯有色纤维的制备方法。
本发明一种超高分子量聚乙烯绳网用有色纤维制备方法， 具体步骤 :¾口下：
步骤 1:
采用超高分子量聚乙烯树脂加 HDPE聚乙烯和有机颜料色粉， 用排 气式双螺杆挤出机制备超高分子量聚乙烯有色母粒， 再将制备的有色母 粒研磨成超高分子量聚乙烯粉状有色母料；
步骤 2:
选用超高分子量聚乙烯树脂， 选用白油 （矿物油）作溶剂， 再加上 述超高分子量聚乙烯粉状有色母料， 制备有色纺丝溶液体：输入溶胀釜进 行混合溶胀， 连续搅拌， 使超高分子量聚乙烯树脂与超高分子量聚乙烯 有色母料达到混合乳体状态， 将溶胀后的有色树脂溶液冷却， 输送到双 螺杆挤出机塑化挤压喷丝和水浴凝固， 制备超高分子量聚乙烯有色冻胶 纤维；
步骤 3:
将已制备的超高分子量聚乙烯有色冻胶纤维： ①先经萃取工序， 用 碳氢清洁剂将白油溶剂萃取分离； ②萃取后的初生纤维再进行热风烘干； ③经干燥后纤维再经三道热拉伸； ④纤维定型： 经三道热拉伸后再经热 定型， 最后将超高分子量聚乙烯纤维收卷成筒装， 得到有色纤维成品。
该生产方法具有如下优点： 一是有机颜料充分利用， 颜料不易混合 在溶剂白油中； 二是着色均匀、 色牢度高， 能耐海水长期浸泡和抗紫外 线光照等功能； 三是满足各种颜色的制备， 纤维规格 1600D - 3200D 复 丝， 单丝纤度为 5~10旦尼尔， 伸长率为 4%~4.5%, 纤维断裂强度为 30~33g/D, 能满足高强度绳索及远洋捕捞拖网、 深海养殖大型围网等使 用要求。
高强绳索、 渔网用超高分子量聚乙烯有色纤维， 颜色以黑色、 蓝色、 绿色、咖啡色为主的各种有色纤维，规格以 1600D 300F、 2000D 300F、 2400D 320F、 3000D 320F、 3200D 320F的粗旦紆维，单丝纤度为 5 ~ 10旦尼尔， 伸长率为 4%~5%, 强力平均>3(^/0的有色超高分子量聚 乙烯纤维， 能满足不同规格的绳索和渔网应用。 具体实施方式
本发明一种超高分子量聚乙烯绳网用有色纤维制备方法， 具体步骤 :¾口下：
步骤 1:
采用 100 ~ 120万分子量的超高分子量聚乙烯树脂加 HDPE聚乙烯和 有机颜料色粉， 其重量配比 10: 2: 1; 色粉颜色可根据渔网要求配制， 如： 黑色、 蓝色、 绿色、 咖啡色等等。 用排气式双螺杆挤出机制备超高 分子量聚乙烯色母粒， 双螺杆加温 160°C ~ 180°C, 挤出速度为每分钟 120 ~ 160转。再将制备的色母粒研磨成超高分子量聚乙烯粉状有色母料， 粉末粒度大小为 20-30目。
步骤 2:
选用 200 ~ 300万分子量超高分子量聚乙烯树脂， 选用 5#~10#白油 (矿物油）作溶剂， 再加上述超高分子量聚乙烯粉状有色母料， 制备有 色纺丝溶液体， 其重量配比为： 10:40:2 ~ 3。 输入溶胀釜进行混合溶胀， 溶胀温度为 90~115°C, 溶胀时间为 1.5~3小时， 连续搅拌， 使超高分 子量聚乙烯树脂与超高分子量聚乙烯有色母料达到混合乳体状态， 将溶 胀后的有色树脂溶液冷却至 50~60°C时， 输送到双螺杆挤出机塑化挤压 喷丝和水浴凝固， 水浴凝固时间为 1~2分钟， 温度为 4°C ~8°C, 制备超 高分子量聚乙烯有色冻胶纤维， 冻胶纤维直径 0.5 ~0.8mm。
步骤 3:
将已制备的超高分子量聚乙烯有色冻胶纤维： ①按已知方式进行萃 取， 萃取时采用碳氢清洁剂， 将白油溶剂萃取分离； ②萃取后的初生纤 维再进行热风烘干， 热风温度控制在 60-80 °C; ③经干燥后纤维按已知方 式进行热拉伸， 共进行三道热拉伸， 第一道拉伸倍数为 10 ~ 15倍， 热风 温度为 120°C ~ 135°C; 第二道拉伸倍数为 1.5 ~ 2倍， 热风温度 125°C ~ 140 °C; 第三道拉伸倍数为 1.2-1.5倍， 热风温度为 130°C ~150°C; ④按 已知方式对纤维进行热定型： 定型温度为 130°C ~140°C。 经三道热拉伸 和热定型后将超高分子量聚乙烯纤维收卷成筒装有色纤维成品。

Claims

权利 要求
1、 一种超高分子量聚乙烯绳网用有色纤维制备方法， 步骤如下： 步骤 1 :
采用超高分子量聚乙烯树脂加 HDPE聚乙烯和有机颜料色粉， 用排 气式双螺杆挤出机制备超高分子量聚乙烯有色母粒， 再将制备的有色母 粒研磨成超高分子量聚乙烯粉状有色母料；
步骤 2:
选用超高分子量聚乙烯树脂， 选用白油作溶剂， 再加步骤 1 所制备 超高分子量聚乙烯粉状有色母料， 制备有色纺丝溶液体：输入溶胀釜进行 混合溶胀， 连续搅拌， 使超高分子量聚乙烯树脂与超高分子量聚乙烯有 色母料达到混合乳体状态， 得到有色树脂溶液， 然后将溶胀后的有色树 脂溶液冷却， 输送到双螺杆挤出机塑化挤压喷丝和水浴凝固， 制备超高 分子量聚乙烯有色冻胶纤维；
步骤 3:
将已制备的超高分子量聚乙烯有色冻胶纤维： ①按已知方式进行萃 取， 萃取时采用碳氢清洁剂， 将白油溶剂萃取分离；； ②萃取后的初生纤 维再进行热风烘干； ③干燥后纤维按已知方式进行热拉伸， 共进行三道 热拉伸； ④按已知方式对纤维进行热定型： 经三道热拉伸后再经热定型， 得到有色纤维成品。
2、 根据权利要求 1所述的制备方法， 在所述步骤 1中：
采用 100 ~ 120万分子量的超高分子量聚乙烯树脂加 HDPE聚乙烯和 有机颜料色粉， 其重量配比 10: 2: 1。
3、 根据权利要求 1或 2所述的制备方法， 在所述步骤 1中： 双螺杆加温 160°C ~ 180 °C ,挤出速度为每分钟 120 ~ 160转； 再将制 备的色母粒研磨成超高分子量聚乙烯粉状有色母料， 粉末粒度大小为 20-30目。
4、 根据权利要求 1、 2或 3所述的制备方法， 在所述步骤 2中： 选用 200 ~ 300万分子量超高分子量聚乙烯树脂， 选用 5# ~ 10#白油 作溶剂， 再加上述超高分子量聚乙烯粉状有色母料， 制备有色纺丝溶液 体， 其重量配比为： 10:40:2 ~ 3。
5、 根据权利要求 1、 2、 3或 4所述的制备方法， 在所述步骤 2中： 溶胀釜溶胀温度为 90~115°C, 溶胀时间为 1.5 ~ 3小时， 将溶胀后 的有色树脂溶液冷却至 50~60°C时， 输送到双螺杆挤出机塑化挤压喷丝 和水浴凝固， 水浴凝固时间为 1~2分钟， 温度为 4°C ~8°C, 制备超高分 子量聚乙烯有色冻胶纤维， 冻胶纤维直径 0.5 ~0.8mm。
6、 根据权利要求 1所述的制备方法， 在所述步骤 3②中： 萃取后的 初生纤维进行热风烘干的热风温度控制在 60-80°C。
7、 根据权利要求 1或 6所述的制备方法， 在所述步骤 3③中： 纤维经三道热拉伸， 第一道拉伸倍数为 10~ 15 倍， 热风温度为
120°C ~ 135 °C； 第二道拉伸倍数为 1.5 ~ 2倍， 热风温度 125°C ~ 140 °C； 第三道拉伸倍数为 1.2 ~ 1.5倍， 热风温度为 130°C ~150°C。
8、 根据权利要求 1、 6或 7所述的制备方法， 在所述步骤 3④中： 纤 维定型温度为 130°C ~140°C。
PCT/CN2013/071246 2012-02-16 2013-02-01 超高分子量聚乙烯绳网用有色纤维制备方法 WO2013120415A1 (zh)

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