CN116103780B - 一种高韧高强聚酰亚胺纤维及其制备方法 - Google Patents
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Abstract
本发明公开了一种高韧高强聚酰亚胺纤维的制备方法。制备方法包括如下步骤:S1:将二胺和二酐进行聚合反应后得到高粘度范围的聚合原液,然后熟化得到聚酰胺酸纺丝原液;S2:将聚酰胺酸纺丝原液脱泡后进行纺丝得到初生丝;S3:初生丝高温环化及超声波低温牵伸工艺下,纤维中的结晶度达到一定比例,制得聚酰亚胺纤维。本发明通过严格控制聚合度得到平均分子量大于100000g/mol特殊大分子聚酰亚胺结构,采用高温熟化方式将聚合原液熟化至可纺粘度,纺丝后采用高温环化、超声波低温牵伸方式处理后,得到高韧高强聚酰亚胺纤维,保证高强高模性能同时提高其柔韧性,提高纤维伸长率,改善加工性能。
Description
技术领域
本发明涉及纤维制备技术领域,尤其涉及一种高韧高强聚酰亚胺纤维及其制备方法。
背景技术
现有技术中的高强高模聚酰亚胺纤维手感偏硬,伸长率较低,在提高纤维强度时牺牲了纤维的柔韧性,降低了纤维的伸长率,纤维的强度和伸长率没办法同时得到提升。
发明内容
本发明的目的在于,针对现有技术的上述不足,提出一种高韧高强聚酰亚胺纤维及其制备方法。
本发明的一种高韧高强聚酰亚胺纤维的制备方法,包括如下步骤:
S1:将二胺和二酐进行聚合反应后得到粘度范围在2000000cp-1000000cp的聚合原液,然后熟化得到聚酰胺酸纺丝原液;
S2:将聚酰胺酸纺丝原液脱泡后进行纺丝得到初生丝;
S3:初生丝环化及超声波牵伸工艺下,纤维中的结晶度达到一定比例,制得高韧高强聚酰亚胺纤维;环化温度为300-400℃;牵伸温度为200-350℃。
进一步的,步骤S3中,纤维中的结晶度达到25-30%。
进一步的,聚合原液的聚合度范围在0.999-1。
进一步的,步骤S1中熟化的温度为50-60℃。
进一步的,聚酰胺酸纺丝原的可纺粘度范围在250000-550000cp。
进一步的,超声波频率范围在50-500kHz。
进一步的,所述方法中多种原料为二胺和二酐,其种类大于等于4种;其中,二胺选自3,4’-二氨基二苯醚、4,4’-二氨基二苯醚、4,4’-二氨基二本砜、二氨基苯甲烷、间苯二胺、对苯二胺、5-氨基-2-(4-氨基苯基)苯并咪唑、5-氨基-2-(4-氨基苯基)苯并噁唑、1,4-双(4-氨基苯氧基)苯、2,4-双[(4-氨基苯氧基)苯基]丙烷、4,4-二氨基苯酰替苯胺、1,4-双(4-氨基苯氧基)-2叔丁基苯,二酐选自均苯四甲酸二酐、联苯四甲酸二酐。
采用上述的制备方法制备的高韧高强聚酰亚胺纤维。
现有技术中,聚合原液的粘度会直观的反映出聚合体系中平均分子量的大小,体系中大分子越多,原液粘度越大,现有技术中的聚合原液的粘度一般在200000-1000000cp,本发明将聚合原液的粘度制备的远远超过现有技术中的粘度,通过严格控制聚合度得到平均分子量大于100000g/mol特殊大分子聚酰亚胺结构,采用高温熟化方式将聚合原液熟化至可纺粘度,纺丝后采用高温环化(相对现有技术的环化温度)、超声波低温(相对现有技术的牵伸温度)牵伸方式处理后,得到高韧高强聚酰亚胺纤维,保证聚酰亚胺纤维高强高模性能同时提高其柔韧性,提高纤维伸长率,改善加工性能。
具体实施方式
以下是本发明的具体实施例,对本发明的技术方案作进一步的描述,但本发明并不限于这些实施例。
实施例1
一种高韧高强聚酰亚胺纤维的制备方法,包括以下步骤:
(1)根据聚合工艺单完成聚合操作及原液(聚酰胺酸溶液)52℃下恒温熟化;
(2)原液通过脱泡器在-0.1MPa的环境下脱泡12h;
(3)脱泡原液进入干法纺丝系统,调整纺丝工艺纺出初生丝;
(4)初生丝进入后处理环化牵伸阶段,进一步发生反应,在320℃高温环化及超声波(80KHZ)低温(230℃)牵伸工艺下,纤维中的结晶度达到一定比例,制得成品聚酰亚胺纤维。
步骤(1)中关键工艺参数
实施例2
一种高韧高强聚酰亚胺纤维的制备方法,包括以下步骤:
(1)根据聚合工艺单完成聚合操作及原液(聚酰胺酸溶液)55℃下恒温熟化;
(2)原液通过脱泡器在-0.06MPa的环境下脱泡16h;
(3)脱泡原液进入干法纺丝系统,调整纺丝工艺纺出初生丝;
(4)初生丝进入后处理环化牵伸阶段,进一步发生反应,在300℃高温环化及超声波(120KHZ)低温(250℃)牵伸工艺下,纤维中的结晶度达到一定比例,制得成品聚酰亚胺纤维。
步骤(1)中关键工艺参数
实施例3
一种高韧高强聚酰亚胺纤维的制备方法,包括以下步骤:
(1)根据聚合工艺单完成聚合操作及原液(聚酰胺酸溶液)54℃下恒温熟化;
(2)原液通过脱泡器在-0.08MPa的环境下脱泡12h;
(3)脱泡原液进入湿法纺丝系统,调整纺丝工艺纺出初生丝;
(4)初生丝进入后处理环化牵伸阶段,进一步发生反应,在350℃高温环化及超声波(120KHZ)低温(280℃)牵伸工艺下,纤维中的结晶度达到一定比例,制得成品聚酰亚胺纤维。
步骤(1)中关键工艺参数
实施例4
一种高韧高强聚酰亚胺纤维的制备方法,包括以下步骤:
(1)根据聚合工艺单完成聚合操作及原液(聚酰胺酸溶液)51℃下恒温熟化;
(2)原液通过脱泡器在-0.1MPa的环境下脱泡8h;
(3)脱泡原液进入干喷湿纺纺丝系统,调整纺丝工艺纺出初生丝;
(4)初生丝进入后处理环化牵伸阶段,进一步发生反应,在315℃高温环化及超声波(60KHZ)低温(260℃)牵伸工艺下,纤维中的结晶度达到一定比例,制得成品聚酰亚胺纤维。
步骤(1)中关键工艺参数
实施例5
一种高韧高强聚酰亚胺纤维的制备方法,包括以下步骤:
(1)根据聚合工艺单完成聚合操作及原液(聚酰胺酸溶液)52℃下恒温熟化;
(2)原液通过脱泡器在-0.1MPa的环境下脱泡10h;
(3)脱泡原液进入干法纺丝系统,调整纺丝工艺纺出初生丝;
(4)初生丝进入后处理环化牵伸阶段,进一步发生反应,在300℃高温环化及超声波(80KHZ)低温(250℃)牵伸工艺下,纤维中的结晶度达到一定比例,制得成品聚酰亚胺纤维。
步骤(1)中关键工艺参数
实施例6
一种高韧高强聚酰亚胺纤维的制备方法,包括以下步骤:
(1)根据聚合工艺单完成聚合操作及原液(聚酰胺酸溶液)52℃下恒温熟化;
(2)原液通过脱泡器在-0.1MPa的环境下脱泡8h;
(3)脱泡原液进入干法纺丝系统,调整纺丝工艺纺出初生丝;
(4)初生丝进入后处理环化牵伸阶段,进一步发生反应,在330℃高温环化及超声波(100KHZ)低温(280℃)牵伸工艺下,纤维中的结晶度达到一定比例,制得成品聚酰亚胺纤维。
步骤(1)中关键工艺参数
对比例1
根据聚合工艺单完成聚合操作,聚合原液的粘度为1000000cp,得到原液(聚酰胺酸溶液)48℃下恒温熟化;然后脱泡纺丝,在250℃环化,在350℃牵伸制得成品聚酰亚胺纤维。
对比文件1其他工艺参数与实施例1相同。
对实施例1、2、3、4、5、6与对比例1的聚酰亚胺纤维取样检测,得到下表:
实施例1、2、3、4、5、6与与对比例1的聚酰亚胺纤维取样检测指标对照表
以上未涉及之处,适用于现有技术。
虽然已经通过示例对本发明的一些特定实施例进行了详细说明,但是本领域的技术人员应该理解,以上示例仅是为了进行说明,而不是为了限制本发明的范围,本发明所属技术领域的技术人员可以对所描述的具体实施例来做出各种各样的修改或补充或采用类似的方式替代,但并不会偏离本发明的方向或者超越所附权利要求书所定义的范围。本领域的技术人员应该理解,凡是依据本发明的技术实质对以上实施方式所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围。
Claims (6)
1.一种高韧高强聚酰亚胺纤维的制备方法,其特征在于,包括如下步骤:
S1:将二胺和二酐进行聚合反应后得到粘度范围在2000000 cP-10000000 cP的聚合原液,然后熟化得到聚酰胺酸纺丝原液;
S2:将聚酰胺酸纺丝原液脱泡后进行纺丝得到初生丝;
S3:初生丝环化及超声波牵伸工艺下,纤维中的结晶度达到一定比例,制得高韧高强聚酰亚胺纤维;环化温度为300-400℃;牵伸温度为200-350℃;
步骤S1中熟化的温度为50-60℃;
聚酰胺酸纺丝原液的可纺粘度范围在250000-550000 cP。
2.如权利要求1所述的制备方法,其特征在于,步骤S3中,纤维中的结晶度达到25-30%。
3.如权利要求1所述的制备方法,其特征在于,聚合原液的聚合度范围在0.999-1。
4.如权利要求1所述的制备方法,其特征在于,超声波频率范围在50-500kHz。
5.如权利要求1所述的制备方法,其特征在于,所述方法中原料为二胺和二酐,原料种类大于等于4种;其中,二胺选自3,4’-二氨基二苯醚、4,4’-二氨基二苯醚、4,4’-二氨基二苯砜、二氨基苯甲烷、间苯二胺、对苯二胺、5-氨基-2-(4-氨基苯基)苯并咪唑、5-氨基-2-(4-氨基苯基)苯并噁唑、1,4-双(4-氨基苯氧基)苯、2,4-双[(4-氨基苯氧基)苯基]丙烷、4,4-二氨基苯酰替苯胺、1,4-双(4-氨基苯氧基)-2叔丁基苯,二酐选自均苯四甲酸二酐、联苯四甲酸二酐。
6.采用权利要求1-5任一项所述的制备方法制备的高韧高强聚酰亚胺纤维。
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