CN101600756B - 使用双轴捏和机将芳族聚酰胺聚合物溶解在硫酸中的方法 - Google Patents

使用双轴捏和机将芳族聚酰胺聚合物溶解在硫酸中的方法 Download PDF

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CN101600756B
CN101600756B CN2008800037418A CN200880003741A CN101600756B CN 101600756 B CN101600756 B CN 101600756B CN 2008800037418 A CN2008800037418 A CN 2008800037418A CN 200880003741 A CN200880003741 A CN 200880003741A CN 101600756 B CN101600756 B CN 101600756B
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B·M·肯德尔斯
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Abstract

本发明涉及一种使用双轴捏和机在溶剂中溶解聚合物的方法，其包括以下步骤：a)将聚合物和溶剂计量进料到捏和机中；b)混合聚合物和溶剂以在溶剂中溶解聚合物得到溶液；c)将溶液脱气得到纺丝原液；d)将纺丝原液运送出捏和机，其中所述聚合物是芳族聚酰胺聚合物，溶剂是硫酸，且其中所述芳族聚酰胺聚合物在将硫酸计量进料到捏和机中之前计量进料到捏和机中。

Description

使用双轴捏和机将芳族聚酰胺聚合物溶解在硫酸中的方法
本发明关于一种使用双轴捏和机将芳族聚酰胺聚合物，更特别地是PTTA(聚对亚苯基对苯二甲酰胺)溶解在硫酸中的方法。
溶解芳族聚酰胺聚合物的方法在所属技术领域是已知的。常见方法包括将芳族聚酰胺聚合物溶解于反应器或捏和机中的液体硫酸中，并将所形成的溶液脱气，例如WO 00/77515中所述。该方法在85℃用时4小时，其导致芳族聚酰胺聚合物降解。或者根据US 5,599,623，将芳族聚酰胺聚合物溶解在硫酸中是在低温(低于25℃)下进行，例如使用冷冻硫酸冰，随后将所产生的固体溶液熔融并脱气。该方法用时6小时，因此具有大停留时间分布。该方法限于具有含量为17.5-19.8重量％的PTTA作为芳族聚酰胺聚合物的混合物。低于17.5重量％PPTA时，硫酸中形成了大量不合格材料。而且从TDC(对苯二酰二氯)和PPD(对苯二胺)，以及其它单体如DAPBI(5-(6)-氨基-2-(对氨基苯基)苯并咪唑)、CI-TDC(2-氯代对苯二酰二氯)和CI-PPD(2-氯-对苯二胺)获得的共聚物不能溶解或者仅能很困难地溶解，因为所形成的固体溶液变得太粘和/或形成不易于进一步加工的大块。这些已知方法因此具有固有的缺点。
WO 2006/045517中建议了一种改进。根据该方法PPTA或其共聚物被运送到双螺杆挤出机中，然后加入硫酸并且混合以将PPTA溶解在硫酸中。在膜形成并且脱气后，含有PPTA的纺丝原液离开双螺杆挤出机。该方法有一些其它缺点如在计量进料中发生小量偏差，这些偏差不能消除且在输出的PPTA浓度上为可见偏差。双螺杆挤出机的工作容积小，因此停留时间也短。为了恒定结果，需要严格的控制系统。而且双螺杆挤出机是昂贵的仪器，这使该方法在商业上的吸引力比较小。双螺杆挤出机是与双螺杆捏和机不同的仪器。螺杆和挤出机内表面之间的距离小。在捏和机中，主要的目的不在于将材料运送出捏和机，而是构建多个轴以彻底捏和材料。双轴捏和机的工作容积大，因此停留时间也长。这要求不同类型的轴，对于捏和运动，其相对较小且在轴和捏和机内表面之间有充足的空间。捏和机的剪切水平比挤出机中的低，这导致与挤出机相比为具有低能量损耗的方法。低能量损耗也意味着进行溶解方法所需的冷却能量低。
CN 1048710中公开了一种方法，其涉及通过将对苯二胺和对苯二甲酰氯混合到双轴混合器中以得到聚(对苯基二甲酰基对苯基二胺)的聚合方法。之后在排气双芯轴挤出机中对产物脱气。因此使用双轴混合器和双芯轴挤出机以从聚合反应得到聚合树脂，而不是用于将聚合物溶解在溶剂中以得到纺丝原液。
WO 96/34732公开了使用单轴捏和机。在这样的单轴捏和机中将聚合材料熔融并脱气。然而聚合材料首先必须在其可以进入单轴捏和机之前溶解，从而在添加聚合物之前将溶剂(硫酸)加入到单独的溶解单元中。这样的单轴捏和机不适合溶解芳族聚酰胺聚合物，而后者是本发明的主题。
本发明的目的在于提供一种不具有上述缺点的方法。为此目的，已经开发了一种新方法。本发明因此涉及一种使用双轴捏和机将芳族聚酰胺聚合物溶解在硫酸中的方法，其包括以下步骤：
a)将聚合物和溶剂计量进料至捏和机中；
b)混合聚合物和溶剂以将聚合物溶解在溶剂中得到溶液；
c)将该溶液脱气得到纺丝原液；
d)将纺丝原液运送出捏和机；
其中聚合物是芳族聚酰胺聚合物，溶剂是硫酸，其中在将硫酸计量进料至捏和机中之前将芳族聚酰胺聚合物计量进料至捏和机中。
将固体聚合物计量进料至捏和机中优选用回转阀进行，其具有的其它优点在于捏和机可以在用于脱气所形成纺丝原液的真空下工作。
本发明中所用双轴捏和机适合将任何芳族聚酰胺聚合物(包括共聚物)溶解在硫酸中。用TDC(对苯二酰二氯)和PPD(对苯二胺)制成的聚合物和共聚物是最合适的，但用另外包含单体如DAPBI(5-(6)-氨基-2-(对氨基苯基)-苯并咪唑)、CI-TDC(2-氯代对苯二酰二氯)、NDC(萘酰二氯)和CI-PPD(2-氯-对苯二胺)的单体形成的共聚物可以同样好地使用。所有这些和其它聚合物和共聚物在所属技术领域是公知的。
图1示意性说明了本发明。图1是双轴捏和机的示意图。
根据本发明实施方案，将芳族聚酰胺聚合物如图中表明的PPTA计量进料至捏和机的第一部分1，并且运送到运送装置2。聚合物然后通过回转阀3引入捏和机。硫酸通过位于阀3之后的入口4注入捏和机。将聚合物和硫酸引入捏和机的这种次序防止了PPTA(或者概括地说是芳族聚酰胺聚合物)入口的堵塞和堵盖的风险，因为PPTA和硫酸的混合会形成大块。通过首先将PPTA和然后是硫酸引入捏和机，混合和溶解过程将会同时发生。双轴捏和机相对于现有技术的优点在于使充分活塞流具有足够的停留时间以消除进料波动，提供充分混合并且同时清洁机筒。双轴捏和机(也称为两轴捏和机)包括两个共旋转轴，它们结合了清洁和捏和作用。也可以用两个共旋转轴，其中一个具有高的旋转速度用于清洁作用，而另一个具有低的旋转速度用于捏和作用。混合期间的热散逸和溶解聚合物中所出现的能量足以在几乎绝热的情况下实现整个过程。在芳族聚酰胺聚合物溶解在硫酸中之后，可以在捏和机6的部分5中通过使用真空泵7或者其它获得真空的装置使用低压将溶液脱气。因为芳族聚酰胺聚合物是由回转阀3计量进料的，所以溶解的聚合物可以在低压力下(例如在40毫巴绝对压力下)在双轴捏和机中脱气。脱气的溶液可以用作纺丝原液，且可以通过输出装置8在一定预定压力下从捏和机6运送出，输出装置8在图中绘制为卸料螺杆。
本发明的溶解方法优选在少于180分钟里进行。更通常情况下该方法进行45到120分钟，并且一般是45到60分钟。
该方法使得芳族聚酰胺聚合物以任何浓度溶解，因为没有固体溶液阶段，该阶段在使用低浓度或者使用共聚物时会引起大量不合格材料。
该方法也允许在溶液中使用纳米颗粒如纳米管。为了得到这样的纺丝原液，芳族聚酰胺聚合物与纳米颗粒混合且然后与硫酸混合，或者作为替换芳族聚酰胺聚合物的硫酸溶液与纳米颗粒混合。
此外，用于溶解过程的双轴捏和机设备比双螺杆挤出机或者其它已知路径所需要的其它设备更廉价。而且能量消耗低于现有技术中的方法。
本发明进一步以下述非限制性实施例进行示例性说明。
概要
芳族聚酰胺聚合物的计量进料在双轴捏和机的第一部分的开始处(图1：4)完成。因为双轴捏和机在用于溶液脱气的40毫巴的压力下工作，所以使用回转阀。
芳族聚酰胺聚合物的计量进料通过失重系统(测定重量的)进行。因为溶解设备具有与溶解时间(60分钟)相等的缓冲容量，所以不需要具有高精确性的计量进料体系。
硫酸的计量进料发生在双轴捏和机的第一部分的末端(图1：5)。硫酸通过压力阀引入到捏和机中，压力阀使得可以引入到在40毫巴压力下工作的双轴捏和机。液体硫酸的计量进料用齿轮泵或者3-头柱塞泵进行。硫酸流用科里奥利管进行测量，以后向控制泵频率以使得可以校正硫酸的计量进料。因为缓冲容量，所以不需要具有高精确性的计量体系。
将PPTA溶解在硫酸中
将PPTA溶解在硫酸中是在由耐受该方法的磨耗的材料制成的双轴捏和机中进行。
实施例1
将ηrel为5.01的x重量％PPTA计量进料到双轴捏和机中，并且将100-x重量％硫酸注入该双轴捏和机中。硫酸的纯度是99.8％。捏和机的速度是大约32和25.6rpm。用于脱气的真空度设定为40毫巴(绝对压力)。输出压力挤出机为4巴。溶解容量是30Kg/h。溶解过程的温度是85℃。制备了下述具有不同浓度和ηrel的纺丝原液。
  PPTA(x重量％)   ηrel
  17.7   4.59
  19.5   4.75
  18.7   4.88
  19.0   4.78
由于非常有限的降解，相对粘度仅有少量降低。
实施例2
将19.5重量％的从PPD和含有5摩尔％ηrel＝5.84的NDC(萘酰二氯)的TDC/NDC混合物制备而来的共聚物计量进料到双轴捏和机中。将81.5重量％硫酸注入容量为28.2Kg/h的该双轴捏和机中。捏和机速率是大约52/42rpm，且用于脱气的真空度是40-100毫巴(绝对压力)。输出压力挤出机为4巴。纺丝原液具有的ηrel为4.06-4.33。

Claims (11)

1.一种使用双轴捏和机在溶剂中溶解聚合物的方法，其包括以下步骤：
a)将聚合物和溶剂计量进料到捏和机中；
b)混合聚合物和溶剂以在溶剂中溶解聚合物得到溶液；
c)将溶液脱气得到纺丝原液；
d)将纺丝原液运送出捏和机，其中所述聚合物是芳族聚酰胺聚合物，溶剂是硫酸，且其中所述芳族聚酰胺聚合物在将硫酸计量进料到捏和机中之前计量进料到捏和机中。
2.如权利要求1所述的方法，其中所述芳族聚酰胺聚合物使用回转阀计量进料到捏和机中。
3.如权利要求1或2所述的方法，其中所述芳族聚酰胺聚合物从至少包含TDC和PPD的单体的混合物获得。
4.如权利要求1或2所述的方法，其中所述芳族聚酰胺聚合物是PPTA。
5.如权利要求1或2所述的方法，其中所述芳族聚酰胺聚合物在双轴捏和机中的停留时间少于180分钟。
6.如权利要求5所述的方法，其中所述芳族聚酰胺聚合物在双轴捏和机中的停留时间为45-120分钟。
7.如权利要求6所述的方法，其中所述芳族聚酰胺聚合物在双轴捏和机中的停留时间为45-60分钟。
8.如权利要求1或2所述的方法，其中所述芳族聚酰胺聚合物与纳米颗粒混合且然后与硫酸混合，或者其中所述芳族聚酰胺聚合物的硫酸溶液与纳米颗粒混合。
9.一种使用双轴捏和机在溶剂中溶解聚合物的方法，其包括以下步骤：
a)将聚合物和溶剂计量进料到捏和机中；
b)混合聚合物和溶剂以在溶剂中溶解聚合物得到溶液；
c)将溶液脱气得到纺丝原液；
d)将纺丝原液运送出捏和机，其中所述聚合物是芳族聚酰胺共聚物，溶剂是硫酸，且其中所述芳族聚酰胺共聚物在将硫酸计量进料到捏和机中之前计量进料到捏和机中。
10.如权利要求1或权利要求9所述的方法，其中聚合物和共聚物用TDC(对苯二酰二氯)和PPD(对苯二胺)制成，其中制成共聚物的单体另外包含其它单体。
11.如权利要求10所述的方法，其中其它单体为DAPBI(5-(6)-氨基-2-(对氨基苯基)-苯并咪唑)、CI-TDC(2-氯代对苯二酰二氯)、NDC(萘酰二氯)或CI-PPD(2-氯-对苯二胺)。
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