CN102990901A - 聚对苯甲酰聚对苯二胺树脂聚合用组合式双螺杆挤出机 - Google Patents

聚对苯甲酰聚对苯二胺树脂聚合用组合式双螺杆挤出机 Download PDF

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CN102990901A
CN102990901A CN2012105943192A CN201210594319A CN102990901A CN 102990901 A CN102990901 A CN 102990901A CN 2012105943192 A CN2012105943192 A CN 2012105943192A CN 201210594319 A CN201210594319 A CN 201210594319A CN 102990901 A CN102990901 A CN 102990901A
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screw extruder
poly
phenylenediamine
double screw
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CN102990901B (zh
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余木火
孔海娟
滕翠青
张蕊
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Hebei Silicon Valley chemical Co., Ltd.
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Donghua University
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
    • B29C48/375—Plasticisers, homogenisers or feeders comprising two or more stages
    • B29C48/39—Plasticisers, homogenisers or feeders comprising two or more stages a first extruder feeding the melt into an intermediate location of a second extruder
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
    • B29C48/375—Plasticisers, homogenisers or feeders comprising two or more stages
    • B29C48/385—Plasticisers, homogenisers or feeders comprising two or more stages using two or more serially arranged screws in separate barrels
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
    • B29C48/395—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders
    • B29C48/40—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders using two or more parallel screws or at least two parallel non-intermeshing screws, e.g. twin screw extruders
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/78—Thermal treatment of the extrusion moulding material or of preformed parts or layers, e.g. by heating or cooling
    • B29C48/875—Thermal treatment of the extrusion moulding material or of preformed parts or layers, e.g. by heating or cooling for achieving a non-uniform temperature distribution, e.g. using barrels having both cooling and heating zones
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/92—Measuring, controlling or regulating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00—Indexing scheme relating to extrusion moulding
    • B29C2948/92—Measuring, controlling or regulating
    • B29C2948/92504—Controlled parameter
    • B29C2948/92704—Temperature
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00—Indexing scheme relating to extrusion moulding
    • B29C2948/92—Measuring, controlling or regulating
    • B29C2948/92819—Location or phase of control
    • B29C2948/92857—Extrusion unit
    • B29C2948/92876—Feeding, melting, plasticising or pumping zones, e.g. the melt itself
    • B29C2948/92895—Barrel or housing

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Abstract

本发明涉及一种聚对苯甲酰聚对苯二胺树脂聚合用组合式双螺杆挤出机，由两阶双螺杆T型组合而成；其中，一阶双螺杆挤出机的螺纹结构为异向啮合，二阶双螺杆挤出机的螺纹结构为同向啮合。本发明可以预缩聚时提高混合效果减少剪切，使分子量分布均匀；反应过程中脱挥段设计，聚合后端加大剪切，控制相转变；实现了粉料连续稳定聚合；本发明可以实现更好的散热，得到聚合物的分子量高，而且分布窄，能够得到稳定聚合物。

Description

聚对苯甲酰聚对苯二胺树脂聚合用组合式双螺杆挤出机
技术领域
本发明属于聚对苯甲酰聚对苯二胺树脂化工设备领域，特别涉及一种聚对苯甲酰聚对苯二胺树脂聚合用组合式双螺杆挤出机。 
背景技术
芳纶纤维具有超高强度、高模量、耐高温、耐酸碱、质量轻等优良性能，其中比强度是刚的5~6倍，模量是钢丝和玻璃纤维的2~3倍，韧性是钢丝的2倍，而质量仅为钢丝的1/5左右。芳纶是综合性能优良、产量最大、应用最广的高性能纤维，在高性能纤维中占有重要的地位，在国防，航空航天，汽车减重节能减排，新能源开发和经济建设等方面具有不可替代的作用。 
USP5726257公开了一种间歇式制备聚对苯二甲酰对苯二胺树脂的方法，该方法是对苯二胺和对苯二甲酰氯在N-甲基吡咯烷酮溶剂体系中，分批聚合制备树脂，反应首先在一根同时具有搅拌和造粒作用的聚合齿轮的圆柱形反应容器中进行，当对苯二甲酰氯加入时，反应体系受到漩涡搅拌，生成聚合物被粉碎，聚合反应和聚合物的粉碎在同一容器中进行。漩涡状的搅拌方式能够保证反应体系充分混合，反应迅速进行，得到较高粘度的聚合物。这种方法制备的对苯二甲酰对苯二胺树脂只能分批进行，效率比较低且难得到性能稳定的树脂聚合物。 
CN101265326公开了一种对苯二甲酰对苯二胺树脂的制备方法以及设备，即先将对苯二胺溶解后，用三轴自清洁型预反应器，然后将对苯二甲酰氯按一定比例加入到预反应器中，并加入吡啶类酸吸收剂进行反应，反应完全后挤出，然后在静置、洗涤、脱水、干燥后得到聚对苯二酰对苯二胺树脂，并公开了一种三轴自清洁预反应设备，制的了较高分子量的树脂，但是此反应是间歇式反应。 
目前，对苯二甲酰对苯二铵树脂的合成工业上主要是通过在双螺杆挤出机中进行低温缩聚反应合成的。在聚合过程单体的纯度及分数以及加入的助溶剂和产生的小分子的脱除对反应都有很大的影响。且随着聚合反应的进行，体系粘度增加，产生凝胶现象，聚合物由于端基包埋无法进一步反应，致使生成的聚合物的分子量较小，且分布比较宽。 
发明内容
本发明所要解决的技术问题是提供一种聚对苯甲酰聚对苯二胺树脂聚合用组合式双螺杆挤出机，该组合式双螺杆挤出机预缩聚时提高混合效果减少剪切，使分子量分布均匀；反应过程中脱挥段设计，聚合后端加大剪切，控制相转变；实现了粉料连续稳定聚合；可以实现更好的散热，得到聚合物的分子量高，而且分布窄，能够得到稳定聚合物。 
本发明的一种聚对苯甲酰聚对苯二胺树脂聚合用组合式双螺杆挤出机，由两阶双螺杆T型组合而成如图所示；其中，一阶双螺杆挤出机的螺纹结构为异向啮合，二阶双螺杆挤出机的螺纹结构为同向啮合。 
所述一阶双螺杆挤出机的螺杆直径为100~130mm，长径比为12~16，转速为200~400rpm，物料停留时间为10~30s。 
所述二阶双螺杆挤出机的螺杆直径为100~150mm，长径比为40~60，转速为40~300rpm，物料停留时间为3~15min。 
所述一(Ⅰ)阶双螺杆挤出机的冷却温度为-15~15℃。 
所述二(Ⅱ)阶双螺杆挤出机分三个温度区，温度设定为-5~5℃，0~20℃，30~50℃。 
所述一阶双螺杆挤出机后段开孔，通过抽真空脱除聚合物中产生的副产物氯化氢小分子。 
本发明一阶双螺杆挤出机为预缩聚反应器，用来将对苯二胺溶解和部分对苯二甲酰氯预缩聚；合成一定粘度的预聚物，然后将预聚物和剩余的对苯二甲酰加入第二阶双螺杆中进一步反应。第二阶双螺杆挤出机是主缩聚反应器，并在其后段开孔抽真空脱除反应产生的副产物氯化氢小分子，且具有三段不同的螺纹段组成，具有最佳混合、输送、脱挥的效果。 
有益效果
本发明可以预缩聚时提高混合效果减少剪切，使分子量分布均匀；反应过程中脱挥段设计，聚合后端加大剪切，控制相转变；实现了粉料连续稳定聚合；本发明可以实现更好的散热，得到聚合物的分子量高，而且分布窄，能够得到稳定聚合物。 
附图说明
图1为本发明组合式双螺杆挤出机示意图； 
图2a为I阶螺杆螺纹结构示意图；图2b为Ⅱ阶螺杆螺纹结构示意图。 
具体实施方式
下面结合具体实施例，进一步阐述本发明。应理解，这些实施例仅用于说明本发明而不用于限制本发明的范围。此外应理解，在阅读了本发明讲授的内容之后，本领域技术人员可以对本发明作各种改动或修改，这些等价形式同样落于本申请所附权利要求书所限定的范围。 
实施例1 
本实施例提供的一种聚对苯甲酰聚对苯二胺树脂聚合用组合式双螺杆挤出机，由两阶双螺杆T型组合而成；其中，一阶双螺杆挤出机的螺纹结构为异向啮合，二阶双螺杆挤出机的螺纹结构为同向啮合。一阶双螺杆挤出机后段开孔，通过抽真空脱除聚合物中产生的副产物氯化氢小分子。 
在50L带夹套的不锈钢反应釜中加入15Kg无水N-甲基吡咯烷酮，加入1Kg经高温活化 的无水氯化钙，完成溶解后，通过液体计量加料系统将预制成的溶剂加入到第一台双螺杆中，冷却至15℃，加入0.65kg对苯二胺粉末加入到直径120mm,长径比14，转速300rpm第一阶双螺杆反应器中至溶解，然后将冷却到-10℃，加入对苯二甲酰氯0.325Kg进行预聚，停留30s，将低聚物和吡啶分别以290g/min，7g/min的流量以计量泵同时加入直径为100mm,长径比48，转速为150rpm的双螺杆挤出机中，控制双螺杆三段温度分别为-5℃，5℃，40℃。12min可以挤出淡黄色面包屑状的聚合体，通过多次水洗除去溶剂后真空干燥得到对苯二甲酰对苯二胺粉末，测得其比浓对数粘度为6.5dl/g。 
对比例 
在50L带夹套的不锈钢反应釜中加入15Kg无水N-甲基吡咯烷酮，加入1Kg经高温活化的无水氯化钙，加入0.65kg对苯二胺粉末搅拌溶解，然后将冷却到-10℃，加入对苯二甲酰氯0.325Kg进行预聚，然后低聚物和剩余的0.905kg对苯二甲酰氯一起加入到入直径为100mm,长径比48，转速为150转的双螺杆挤出机中，控制双螺杆三段温度分别为-5℃，5℃，40℃。约12min中可以挤出淡黄色面包屑状的聚合体，通过多次水洗除去溶剂后真空干燥得到对苯二甲酰对苯二胺粉末，测得其比浓对数粘度为6.0dl/g。

Claims (6)

1.一种聚对苯甲酰聚对苯二胺树脂聚合用组合式双螺杆挤出机，其特征在于：由两阶双螺杆T型组合而成；其中，一阶双螺杆挤出机的螺纹结构为异向啮合，二阶双螺杆挤出机的螺纹结构为同向啮合。
2.根据权利要求1所述的一种聚对苯甲酰聚对苯二胺树脂聚合用组合式双螺杆挤出机，其特征在于：所述一阶双螺杆挤出机的螺杆直径为100~130mm，长径比为12~16，转速为200~400rpm，物料停留时间为10~30s。
3.根据权利要求1所述的一种聚对苯甲酰聚对苯二胺树脂聚合用组合式双螺杆挤出机，其特征在于：所述二阶双螺杆挤出机的螺杆直径为100~150mm，长径比为40~60，转速为40~300rpm，物料停留时间为3~15min。
4.根据权利要求1所述的一种聚对苯甲酰聚对苯二胺树脂聚合用组合式双螺杆挤出机，其特征在于：所述一阶双螺杆挤出机的冷却温度为-15~15℃。
5.根据权利要求1所述的一种聚对苯甲酰聚对苯二胺树脂聚合用组合式双螺杆挤出机，其特征在于：所述二阶双螺杆挤出机分三个温度区，温度设定为-5~5℃，0~20℃，30~50℃。
6.根据权利要求1所述的一种聚对苯甲酰聚对苯二胺树脂聚合用组合式双螺杆挤出机，其特征在于：所述一阶双螺杆挤出机后段开孔，通过抽真空脱除聚合物中产生的副产物氯化氢小分子。
CN201210594319.2A 2012-12-31 2012-12-31 聚对苯甲酰聚对苯二胺树脂聚合用组合式双螺杆挤出机 Expired - Fee Related CN102990901B (zh)

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CN108623803A (zh) * 2018-06-22 2018-10-09 清华大学 聚对苯二甲酰对苯二胺高浓度连续稳定聚合方法及其系统
CN109012528A (zh) * 2018-08-14 2018-12-18 无锡创彩光学材料有限公司 一种管式反应器及用其制备单分散聚酰胺酸溶液的方法
CN109295506A (zh) * 2018-09-13 2019-02-01 清华大学 一种对位芳纶纺丝原液配制系统及其配制方法

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108623803A (zh) * 2018-06-22 2018-10-09 清华大学 聚对苯二甲酰对苯二胺高浓度连续稳定聚合方法及其系统
CN109012528A (zh) * 2018-08-14 2018-12-18 无锡创彩光学材料有限公司 一种管式反应器及用其制备单分散聚酰胺酸溶液的方法
CN109012528B (zh) * 2018-08-14 2024-03-08 无锡创彩光学材料有限公司 一种管式反应器及用其制备单分散聚酰胺酸溶液的方法
CN109295506A (zh) * 2018-09-13 2019-02-01 清华大学 一种对位芳纶纺丝原液配制系统及其配制方法
CN109295506B (zh) * 2018-09-13 2020-07-28 清华大学 一种对位芳纶纺丝原液配制系统及其配制方法

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