CN104774308A - 一种熔纺氨纶切片的制备方法 - Google Patents
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Abstract
本发明公开了一种熔纺氨纶切片的制备方法,此方法由一种新合成的脂肪族/芳香族混合型聚酯多元醇与聚醚多元醇的混合物、脂肪族二醇、二异氰酸酯在双螺杆挤出机中反应制的,产品具有分子量高,分子量分布窄的特点,利用本方法制备的切片生产的熔纺氨纶性能接近或超越干纺法生产的氨纶。
Description
技术领域
本发明涉及一种新型熔纺氨纶切片的制备方法。
背景技术
氨纶作为一种高弹性纤维材料,在纺织行业具有广泛的用途,目前,氨纶主要采用干法纺丝(干纺)和熔融纺丝(熔纺)两种工艺生产,熔纺氨纶设备投资少、投产周期短、生产流程简单、产量高、成本低、尤其是无污染等优势受到人们的普遍关注,在国际上被称为绿色氨纶。
由于熔纺氨纶加工温度高,与干纺氨纶相比,回弹性与耐热性均差一些,为了提高熔纺氨纶的性能需要对其上游产品——聚氨酯切片进行改性,以提高最终产品性能,中国专利申请CN01115739在氨纶切片中加入纳米粉体共混后,用于纺丝,能够提高熔纺氨纶的热性能和力学性能;中国专利申请CN200410065487采用在聚酯切片中混入交联剂、热稳定剂等助剂的方法来提高熔纺氨纶的性能;但聚氨酯切片和助剂等共混均一度难于控制,熔纺氨纶品质控制较难。
发明内容
本发明目的是提供一种在力学性能、耐热性能方面接近干纺氨纶的熔纺氨纶切片。
具体技术方案如下:
一种熔纺氨纶切片的制备方法,其是将混合多元醇、脂肪族二醇和异氰酸酯按照1:(0.5~2):(1.4~3)的摩尔比加入长径比为45~85的反应型双螺杆挤出机中,制得熔纺氨纶切片。
作为优选方案,所述混合多元醇包括聚酯多元醇和聚醚多元醇。
作为优选方案,所述聚酯多元醇和聚醚多元醇的摩尔比为(50~80):20。
所述聚醚多元醇的分子量为1000Da~5000Da。
作为优选方案,所述聚醚多元醇为聚四亚甲基醚二醇、聚乙二醇、聚丙二醇的一种或几种。
作为优选方案,所述聚酯多元醇制备方法如下:
a) 将摩尔比为(10~25):(25~40):(55~75)的芳香族二酸、脂肪族二酸和1,4-丁二醇加入制浆釜中,在氮气保护下,于20~60℃的温度下打浆,直至混合均匀;
b) 将步骤a)得到的产物压入酯化釜,在常压氮气保护下,于100~270℃搅拌反应1~4小时,并将生产的水冷凝排出,得到澄清透明液体;
c) 将步骤b)得到的澄清透明液体用氮气压入缩聚釜,在100Pa~40kPa的真空度下,于200℃~250℃反应0.5h~12h,放料,得到聚酯多元醇。
作为优选方案,所述芳香族二酸包括邻苯二甲酸、对苯二甲酸、间苯二甲酸和萘二酸的一种或几种。
作为优选方案,所述脂肪族二酸包括乙二酸、丙二酸、丁二酸、己二酸、癸二酸的一种或几种。
作为优选方案,所述脂肪族二醇为1,4-丁二醇、1,4-环己烷二甲醇中的一种或两种。
作为优选方案,所述异氰酸酯为4,4’-二苯基甲烷二异氰酸酯、甲苯二异氰酸、六次甲基二异氰酸酯、异氟尔酮二异氰酸酯和(4,4’-二环己甲烷)二异氰酸酯的一种或几种。
本发明的优点是制备的切片产品重均分子量≥500kDa,分子量分布≤1.9,与市面上其他熔纺氨纶比较弹性回复率较高,性能接近或超越干纺氨纶,如表1所示:
规格 | 平均伸长率(%) | 断裂强力(CN) | 强度 (CN/dtex) | 300%应力( CN) | 弹性回复率(%) | 沸水收缩率(%) |
15D | 480-530 | 20-24 | 1.2-1.5 | 8—10 | 89-91 | 11—12 |
20D | 480-520 | 25-35 | 1.2—1.4 | 10—12 | 89-91 | 11—12 |
40D | 460—510 | 48—52 | 1.2—1.3 | 17---20 | 89-91 | 11—12 |
表1。
具体实施方式
下面结合实施例对本发明作进一步描述,但本发明的保护范围不仅局限于实施例。
实施例1
在氮气保护下,将对苯二甲酸:己二酸:1,4-丁二醇按摩尔比10:40:70的比例在50℃条件下搅拌至均匀;用氮气将混合液压致酯化釜,迅速升温至100℃开始反应,在2h内将温度升至235℃,并排出生成水分,得澄清液体;将此液体压入缩聚釜,保持温度230℃,迅速减压至30kPa,保持温度不变,将压力在1h内逐步降低到100Pa,反应结束,得聚酯多元醇,分子量分子量3000Da。
将得到的聚酯多元醇与分子量2000的聚四亚甲基醚二醇按摩尔比70:20共混均匀,得混合醇;用计量泵按摩尔比1.03:0.97:2的比例将混合多元醇、1,4-丁二醇、六次甲基二异氰酸酯打入长径比为65的反应双螺杆中,反应温度120~190℃,水下造粒,干燥、包装后的产品。重均分子量650kDa,分子量分布:1.7。
实施例2
在氮气保护下,将邻苯二甲酸:丁二酸:1,4-丁二醇按摩尔比15:35:60的比例在60℃条件下搅拌至均匀;用氮气将混合液压致酯化釜,迅速升温至100℃开始反应,在2h内将温度升至260℃,并排出生成水分,得澄清液体;将此液体压入缩聚釜,保持温度245℃,迅速减压至30kPa,保持温度不变,将压力在1h内逐步降低到100Pa,反应结束,得聚酯多元醇,分子量分子量4000Da。
将得到的聚酯多元醇与分子量1000的聚四亚甲基醚二醇按摩尔比50:20共混均匀,得混合醇;用计量泵按摩尔比1.03:0.97:2的比例将混合多元醇、1,4-环己烷二甲醇、4,4’-二苯基甲烷二异氰酸酯打入长径比为75的反应双螺杆中,反应温度120~190℃,水下造粒,干燥、包装后的产品。重均分子量500kDa,分子量分布:1.9。
实施例3
在氮气保护下,将对苯二甲酸:戊二酸:1,4-丁二醇按摩尔比55:55:75的比例在60℃条件下搅拌至均匀;用氮气将混合液压致酯化釜,迅速升温至100℃开始反应,在2h内将温度升至240℃,并排出生成水分,得澄清液体;将此液体压入缩聚釜,保持温度235℃,迅速减压至30kPa,保持温度不变,将压力在1h内逐步降低到100Pa,反应结束,得聚酯多元醇,分子量分子量2000Da。
将得到的聚酯多元醇与分子量5000的聚乙二醇按摩尔比80:20共混均匀,得混合醇;用计量泵按摩尔比1.03:0.97:2的比例将混合多元醇、1,4-环己烷二甲醇与1,4-丁二醇混合物、4,4’-二苯基甲烷二异氰酸酯打入长径比为85的反应双螺杆中,反应温度120~190℃,水下造粒,干燥、包装后的产品。重均分子量520kDa,分子量分布:1.6。
最后应说明的是:以上实施例仅用以说明本发明而并非限制本发明所描述的技术方案;因此,尽管本说明书参照上述的各个实施例对本发明已进行了详细的说明,但是,本领域的普通技术人员应当理解,仍然可以对本发明进行修改或等同替换;而一切不脱离本发明的精神和范围的技术方案及其改进,其均应涵盖在本发明的权利要求范围中。
Claims (10)
1.一种熔纺氨纶切片的制备方法,其特征在于,是将混合多元醇、脂肪族二醇和异氰酸酯按照1:(0.5~2):(1.4~3)的摩尔比加入长径比为45~85的反应型双螺杆挤出机中,制得熔纺氨纶切片。
2.根据权利要求1所述的制备方法,其特征在于:所述混合多元醇包括聚酯多元醇和聚醚多元醇。
3.根据权利要求2所述的制备方法,其特征在于:所述聚酯多元醇和聚醚多元醇的摩尔比为(50~80):20。
4.根据权利要求2或3所述的制备方法,其特征在于:所述聚醚多元醇的分子量为1000Da~5000Da。
5.根据权利要求4所述的制备方法,其特征在于:所述聚醚多元醇为聚四亚甲基醚二醇、聚乙二醇、聚丙二醇的一种或几种。
6.根据权利要求2或3所述的制备方法,其特征在于:所述聚酯多元醇制备方法如下:
a) 将摩尔比为(10~25):(25~40):(55~75)的芳香族二酸、脂肪族二酸和1,4-丁二醇加入制浆釜中,在氮气保护下,于20~60℃的温度下打浆,直至混合均匀;
b) 将步骤a)得到的产物压入酯化釜,在常压氮气保护下,于100~270℃搅拌反应1~4小时,并将生产的水冷凝排出,得到澄清透明液体;
c) 将步骤b)得到的澄清透明液体用氮气压入缩聚釜,在100Pa~40kPa的真空度下,于200℃~250℃反应0.5h~12h,放料,得到聚酯多元醇。
7.根据权利要求6所述的制备方法,其特征在于:所述芳香族二酸包括邻苯二甲酸、对苯二甲酸、间苯二甲酸和萘二酸的一种或几种。
8.根据权利要求6所述的制备方法,其特征在于:所述脂肪族二酸包括乙二酸、丙二酸、丁二酸、己二酸、癸二酸的一种或几种。
9.根据权利要求1所述的制备方法,其特征在于:所述脂肪族二醇为1,4-丁二醇、1,4-环己烷二甲醇中的一种或两种。
10.根据权利要求1所述的制备方法,其特征在于:所述异氰酸酯为4,4’-二苯基甲烷二异氰酸酯、甲苯二异氰酸、六次甲基二异氰酸酯、异氟尔酮二异氰酸酯和(4,4’-二环己甲烷)二异氰酸酯的一种或几种。
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CN108192070A (zh) * | 2018-01-18 | 2018-06-22 | 河北邦泰氨纶科技有限公司 | 一种具有抗菌性能的熔纺氨纶切片 |
CN108264626A (zh) * | 2018-01-18 | 2018-07-10 | 河北邦泰氨纶科技有限公司 | 一种高回弹氨纶切片 |
CN114230753A (zh) * | 2021-12-09 | 2022-03-25 | 烟台泰和新材料股份有限公司 | 一种聚醚酯型熔纺氨纶切片的制备方法 |
CN114790275A (zh) * | 2022-05-16 | 2022-07-26 | 金俊平 | 一种力学性能优良的耐高温熔纺氨纶切片及其制备方法 |
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