CN116103779A - 一种高耐热聚酰亚胺纤维及其制备方法 - Google Patents
一种高耐热聚酰亚胺纤维及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种高耐热聚酰亚胺纤维及其制备方法。制备包括如下步骤:S1:将三乙胺异氰酸酯水合物、二胺和二酐进行聚合反应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:初生丝经环化、牵伸处理,得到高耐热聚酰亚胺纤维。本发明使用含有功能性官能团的单体三乙胺异氰酸酯水合物在聚合过程中靶向封端,控制聚合体系的聚合度,同时在聚酰亚胺初生丝环化牵伸阶段的高温环境下释放小分子激活功能性官能团继续参与反应,局部形成体型结构,大幅度提高纤维的强度和耐热性能。
Description
技术领域
本发明涉及纤维制备技术领域,尤其涉及一种高耐热聚酰亚胺纤维及其制备方法。
背景技术
现有技术中虽然聚酰亚胺纤维可以耐高温,但是其在高温下的强度保持率不是很好,这在一定程度在限制了其应用,故需要进一步继续提高聚酰亚胺纤维的耐热性能。
发明内容
本发明的目的在于,针对现有技术的上述不足,提出一种高耐热聚酰亚胺纤维及其制备方法。
本发明的一种高耐热聚酰亚胺纤维的制备方法,包括如下步骤:
S1:将靶向封端剂三乙胺异氰酸酯水合物、二胺和二酐进行聚合反应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:初生丝经环化、牵伸处理,得到高耐热聚酰亚胺纤维;
其中,所述三乙胺异氰酸酯水合物的结构式为:
进一步的,所述三乙胺异氰酸酯水合物通过原料三乙胺水溶液和三苯基甲烷三异氰酸酯在氮气环境下,温度0-80℃下反应制得。
进一步的,所述三乙胺异氰酸酯水合物和二胺的质量比为0.001-0.01;二胺和二酐的质量比为0.99-1.01。
进一步的,步骤S2中脱泡环境为负压,范围(-0.1-0MPa),采用连续的平板流动器脱泡。
进一步的,步骤S2中,聚酰胺酸纺丝原液粘度控制在3000-4000p。
进一步的,步骤S2中,纺丝采用干法纺丝或湿法纺丝。
进一步的,步骤S3中,环化温度范围在250-450℃;环化时间范围在60-300s。
进一步的,步骤S3中,牵伸温度范围在300-550℃。
进一步的,步骤S3中,牵伸倍数范围在1.1-2.5。
进一步的,步骤S1中,二胺和二酐的种类大于等于2种,其中,二胺选自3,4’-二氨基二苯醚(3,4-ODA)、4,4’-二氨基二苯醚(4,4-ODA)、4,4’-二氨基二本砜(4,4’-DDS)、二氨基苯甲烷(MDA)、间苯二胺(MPDA)、对苯二胺(PDA)、5-氨基-2-(4-氨基苯基)苯并咪唑(BIA)、5-氨基-2-(4-氨基苯基)苯并噁唑(BOA)、1,4-双(4-氨基苯氧基)苯(1,4-BAB)、2,4-双[(4-氨基苯氧基)苯基]丙烷(4-BAPP)、4,4-二氨基苯酰替苯胺(4,4-DABA)、1,4-双(4-氨基苯氧基)-2叔丁基苯(BATB),二酐选自均苯四甲酸二酐(PMDA)、联苯四甲酸二酐(BPDA)。
采用上述的制备方法制备的高耐热聚酰亚胺纤维。
本发明使用含有功能性官能团的单体三乙胺异氰酸酯水合物在聚合过程中靶向封端,控制聚合体系的聚合度,同时在聚酰亚胺初生丝环化牵伸阶段的高温环境下释放小分子二氧化碳,三乙胺,激活异氰酸酯继续与端氨基反应,局部形成体型结构,大幅度提高纤维的强度和耐热性能。
本发明通过调整靶向封端剂三乙胺异氰酸酯水合物的配比,可以调整纤维分子链内体型结构单元的比例,从而得到一系列断裂强度及耐热性能优异的聚酰亚胺纤维。通过二胺、二酐单体的选择,两种或多种单体组合,不同的原料配比,不同的纺丝及后处理工艺等能得到多个系列的聚酰亚胺产品。
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
一种高耐热聚酰亚胺纤维的制作方法,包括以下步骤:
(1)自制三乙胺异氰酸酯水合物;
(2)在聚合设备中,根据聚合工艺单完成聚合操作及原液(聚酰胺酸溶液)熟化操作;
(3)原液通过脱泡器在-0.045MPa环境下完成平板流动脱泡;
(4)脱泡原液进入干法纺丝系统,调整纺丝工艺纺出初生丝;
(5)初生丝进入后处理300℃环化200s,450℃1.5倍牵伸阶段,进一步发生反应,微观结构中产生一定比例的体型结构单元,制得成品聚酰亚胺纤维。
步骤(2)中关键工艺参数
实施例2
一种高耐热聚酰亚胺纤维的制作方法,包括以下步骤:
(1)自制三乙胺异氰酸酯水合物;
(2)在聚合设备中,根据聚合工艺单完成聚合操作及原液(聚酰胺酸溶液)熟化操作;
(3)原液通过脱泡器在-0.06MPa环境下完成平板流动脱泡;
(4)脱泡原液进入干法纺丝系统,调整纺丝工艺纺出初生丝;
(5)初生丝进入后处理350℃环化250s,400℃1.8倍牵伸阶段,进一步发生反应,微观结构中产生一定比例的体型结构单元,制得成品聚酰亚胺纤维。
步骤(2)中关键工艺参数
实施例3
一种高耐热聚酰亚胺纤维的制作方法,包括以下步骤:
(1)在实验室中自制三乙胺异氰酸酯水合物;
(2)在聚合设备中,根据聚合工艺单完成聚合操作及原液(聚酰胺酸溶液)熟化操作;
(3)原液通过脱泡器在-0.05MPa环境下完成平板流动脱泡;
(4)脱泡原液进入湿法纺丝系统,调整纺丝工艺纺出初生丝;
(5)初生丝进入后处理250℃环化300s,450℃1.6倍牵伸阶段,进一步发生反应,微观结构中产生一定比例的体型结构单元,制得成品聚酰亚胺纤维。
步骤(2)中关键工艺参数
实施例4
一种高耐热聚酰亚胺纤维的制作方法,包括以下步骤:
(1)在实验室中自制三乙胺异氰酸酯水合物;
(2)在聚合设备中,根据聚合工艺单完成聚合操作及原液(聚酰胺酸溶液)熟化操作;
(3)原液通过脱泡器在-0.045MPa环境下完成平板流动脱泡;
(4)脱泡原液进入干法纺丝系统,调整纺丝工艺纺出初生丝;
(5)初生丝进入后处理320℃环化200s,480℃1.3倍牵伸阶段,进一步发生反应,微观结构中产生一定比例的体型结构单元,制得成品聚酰亚胺纤维。
步骤(2)中关键工艺参数
实施例5
一种高耐热聚酰亚胺纤维的制作方法,包括以下步骤:
(1)在实验室中自制三乙胺异氰酸酯水合物;
(2)在聚合设备中,根据聚合工艺单完成聚合操作及原液(聚酰胺酸溶液)熟化操作;
(3)原液通过脱泡器在-0.08MPa环境下完成平板流动脱泡;
(4)脱泡原液进入干法纺丝系统,调整纺丝工艺纺出初生丝;
(5)初生丝进入后处理350℃环化280s,460℃ 1.7倍牵伸阶段,进一步发生反应,微观结构中产生一定比例的体型结构单元,制得成品聚酰亚胺纤维。
步骤(2)中关键工艺参数
对比例1
在实施例1的聚合反应中不加入三乙胺异氰酸酯水合物,其他工艺与实施例相同,制备得到聚酰亚胺纤维。
将实施例1-5和对比例1制备的样品的检测指标并入下面的指标对照表中。
实施例1、2、3、4、5与对比例1取样检测指标对照表
从上表可知,少量封端剂的加入,对于原料成本可忽略不计,不增加额外成本前提下,本发明提高了聚酰亚胺耐热性能及断裂强度,提升产品性能指标明显。
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 (10)
2.如权利要求1所述的制备方法,其特征在于,所述三乙胺异氰酸酯水合物通过原料三乙胺水溶液和三苯基甲烷三异氰酸酯在氮气环境下,温度0-80℃下反应制得。
3.如权利要求1所述的制备方法,其特征在于,所述三乙胺异氰酸酯水合物和二胺的质量比为0.001-0.01;二胺和二酐的质量比为0.99-1.01。
4.如权利要求1所述的制备方法,其特征在于:步骤S2中脱泡环境为负压,范围(-0.1-0MPa),采用连续的平板流动器脱泡。
5.如权利要求1所述的制备方法,其特征在于:步骤S2中,聚酰胺酸纺丝原液粘度控制在3000-4000p。
6.如权利要求1所述的制备方法,其特征在于:步骤S3中,环化温度范围在250-450℃;环化时间范围在60-300s。
7.如权利要求1所述的制备方法,其特征在于:步骤S3中,牵伸温度范围在300-550℃。
8.如权利要求1所述的制备方法,其特征在于:步骤S3中,牵伸倍数范围在1.1-2.5。
9.如权利要求1所述的制备方法,其特征在于,步骤S1中,二胺和二酐的种类大于等于2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。
10.采用权利要求1-9任一项所述的制备方法制备的高耐热聚酰亚胺纤维。
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