CN111074628B - 一种原位在线水扩链聚氨酯相变调温功能织物及其制备方法 - Google Patents

一种原位在线水扩链聚氨酯相变调温功能织物及其制备方法 Download PDF

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CN111074628B
CN111074628B CN201911348825.1A CN201911348825A CN111074628B CN 111074628 B CN111074628 B CN 111074628B CN 201911348825 A CN201911348825 A CN 201911348825A CN 111074628 B CN111074628 B CN 111074628B
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郭静
甘紫文
祁冉冉
管福成
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Abstract

一种原位在线水扩链聚氨酯相变调温功能织物及其制备方法，本发明涉及功能织物技术领域。本发明通过水扩链反应，以二苯基甲烷二异氰酸酯为聚氨酯合成用的反应原料，与甲苯、二月桂酸二丁基锡、聚乙二醇形成预聚体，再扩链形成软链段，从而对织物改性使其具有相变调温功能，本发明提供的方法制备的相变调温功能织物的相变焓为20‑50J/g，相转变温度为0‑32℃。与传统技术相比，本发明提供的方法具有工艺简单、节能、环境友好等特点，并且扩大了相变材料在实际应用领域的范围。

Description

一种原位在线水扩链聚氨酯相变调温功能织物及其制备方法
技术领域
本发明涉及功能织物技术领域，特别是一种原位在线水扩链聚氨酯相变调温功能织物及其制备方法。
背景技术
相变调温功能织物指的是对外界环境温度具有智能响应能力的纺织品。目前，相变调温织物的制备方法主要有共混纺丝法、中空纤维灌装法、复合纺丝法和后整理法，但是这些方法存在工艺复杂，条件苛刻，潜热低，对织物强力、手感、透气透湿性等影响大等问题，限制了其应用和发展。基于此本发明提出应用水扩链原位制备具有相变调温功能的纺织品。
发明内容
为解决上述问题，本发明通过水扩链反应原位聚合获得具有相变调温功能的聚氨酯预聚体，采用该预聚体制备相变调温功能织物，该制备过程具体如下：
S1.制备具有相变调温功能的聚氨酯预聚体
先将二苯基甲烷二异氰酸酯溶于甲苯，在180r/min条件下搅拌，并升温加热至80℃，混合均匀后，滴加少量二月桂酸二丁基锡，混合后得到溶液A；将聚乙二醇溶于甲苯得到溶液B，用恒滴漏斗将溶液B在指定时间内滴加到溶液A，滴完后继续反应一段时间；反应结束，将产物在3000r/min下离心6min，滤除杂质，得预聚体，将预聚体避水保存待用；
S2.制备具有相变调温功能织物
将预聚体加入浸液槽，将待浸润织物经导布辊导入浸液槽，浸液后织物重量为原始重量的120-200％，浸液后经压辊导出送入扩链槽，在扩链槽反应一定时间后，经压辊导出，进入熟化机，定温熟化之后，成卷，得到相变调温功能织物。
所述步骤S1中，溶液A各原料之间的配比是：二苯基甲烷二异氰酸酯与甲苯的摩尔比为1:180-1:220，二月桂酸二丁基锡与二苯基甲烷二异氰酸酯的摩尔比为1:100-1.2:100。
所述步骤S1中，溶液B由聚乙二醇和甲苯组成，聚乙二醇和甲苯摩尔比为1:100-1:300。
进一步的，所述步骤S1中，溶液A中二苯基甲烷二异氰酸酯与溶液B中聚乙二醇的摩尔比为2:0-2.2:1。溶液B的滴加时间为0.5h，溶液B滴加完毕继续反应时间为1.5-2h。
进一步的，所述步骤S1中，聚乙二醇的分子质量为1000-4000。
所述步骤S2中，待浸润织物为机织物，织物成分为棉、毛、丝、麻及其混纺织物。
所述步骤S2中，扩链接剂是由二甲基甲酰胺(DMF)、NaHCO3或者乙醇中任一种与水组成的混合物，其中DMF或NaHCO3或乙醇与水的质量混合比为10:90。本发明选择二甲基甲酰胺、NaHCO3和乙醇等对反应的贡献在于调节反应进程，从而得到交联度和氢键化程度不同的材料。在10-40℃的范围均可产生扩链反应，但在20-25℃下生成的膜弹性最好。
因此，所述步骤S2中，扩链反应温度为10-40℃，优选20-25℃，反应时间为2-5min；熟化温度为40-70℃，熟化时间为5-10min。
本发明同时请求保护上述方法制备的相变调温功能织物。
本发明中选择二苯基甲烷二异氰酸酯为聚氨酯合成用的反应原料，主要作用是与聚乙二醇反应，形成聚氨酯预聚体，在扩链之后构成聚氨酯大分子的硬链段。甲苯在本发明中的作用是：作为反应过程的溶剂和带水剂。二月桂酸二丁基锡在本发明的作用是：作为聚氨酯合成用的催化剂。本发明中聚乙二醇是相变物质，聚乙二醇首先与二苯基甲烷二异氰酸酯反应形成预聚体，再扩链形成软链段。限定聚乙二醇的分子质量在1000-4000可以有效控制相变聚氨酯的相变焓与相变温度。
有益效果：
本发明提供的方法制备的相变调温功能织物的相变焓为20-50J/g，相转变温度为0-32℃。与传统技术相比，本发明提供的方法具有工艺简单、节能、环境友好等特点，并且扩大了相变材料在实际应用领域的范围。
附图说明
图1为不同扩链方法获得聚氨酯的红外光谱。
图2为在20-25℃下生成的聚氨酯膜的弹性测试图，其中，图a为拉伸前的聚氨酯膜，图b为拉伸过程中聚氨酯膜，图c为拉伸后聚氨酯膜。
具体实施方式
下面通过具体实施例详述本发明，但不限制本发明的保护范围。如无特殊说明，本发明所采用的实验方法均为常规方法，所用实验器材、材料、试剂等均可从商业途径获得。
实施例1
将0.77摩尔二苯基甲烷二异氰酸酯溶于170摩尔甲苯，在180r/min条件下搅拌，并升温加热至80℃，混合均匀后，滴加0.0077摩尔二月桂酸二丁基锡，混合后得到溶液A；将0.35摩尔聚乙二醇2000溶于52.5摩尔甲苯得到溶液B，用0.5h将溶液B滴加到溶液A，滴完后继续反应1.5小时；反应结束，将产物在3000r/min下离心6min，滤除杂质，得预聚体，将预聚体加入浸液槽，将棉织物经导布辊送入浸液槽，压榨后(织物重量约为原始重量的150％)送入扩链槽，扩链剂由10质量份的乙醇与90质量份的水组成，织物在扩链槽20-25℃扩链反应2分钟后，经带压辊的导布辊导出，进入40℃红外线熟化机熟化5min后，导出成卷，得到相变焓为20J/g，相变温度为27.3℃的相变调温功能棉织物。
实施例2
将0.77摩尔二苯基甲烷二异氰酸酯溶于154摩尔甲苯，在180r/min条件下搅拌，并升温加热至80℃，混合均匀后，滴加0.008摩尔二月桂酸二丁基锡，混合后得到溶液A；将0.35摩尔聚乙二醇4000溶于105摩尔甲苯得到溶液B，用0.5h将溶液B滴加到溶液A，滴完后继续反应2小时；反应结束，将产物在3000r/min下离心6min，滤除杂质，得预聚体，将预聚体加入浸液槽，将真丝织物经导布辊送入浸液槽，压榨后(织物重量约为原始重量的200％)送入扩链槽，扩链剂由10质量份的二甲基甲酰胺与90质量份的水组成，真丝织物在扩链槽20-25℃扩链反应10分钟后，经带压辊的导布辊导出，进入70℃红外线熟化机熟化8min后，导出成卷成卷，得到结晶相变焓30.1J/g，结晶温度为31℃相变调温功能真丝织物。
实施例3
将0.70摩尔二苯基甲烷二异氰酸酯溶于140摩尔甲苯，在180r/min条件下搅拌，并升温加热至80℃，混合均匀后，滴加0.008摩尔二月桂酸二丁基锡，混合后得到溶液A；将0.35摩尔聚乙二醇3000溶于70摩尔甲苯得到溶液B，用0.5h将溶液B滴加到溶液A，滴完后继续反应2小时；反应结束，将产物在3000r/min下离心6min，滤除杂质，得预聚体，将预聚体加入浸液槽，将毛织物经导布辊送入浸液槽，压榨后(织物重量约为原始重量的180％)送入扩链槽，扩链剂由10质量份的碳酸钠与90质量份的水组成，织物在扩链槽20-25℃扩链反应5分钟后，经带压辊的导布辊导出，进入70℃红外线熟化机熟化10min后，导出成卷成卷，得到结晶相变焓30.1J/g，结晶温度为32℃相变调温功能毛织物。
实施例4
将0.70摩尔二苯基甲烷二异氰酸酯溶于154摩尔甲苯，在180r/min条件下搅拌，并升温加热至80℃，混合均匀后，滴加0.0084摩尔二月桂酸二丁基锡，混合后得到溶液A；将0.35摩尔聚乙二醇1000溶于35摩尔甲苯得到溶液B，用0.5h将溶液B滴加到溶液A，滴完后继续反应2小时；反应结束，将产物在3000r/min下离心6min，滤除杂质，得预聚体，将预聚体加入浸液槽，将毛织物经导布辊送入浸液槽，压榨后送入扩链槽，扩链剂由10质量份的乙醇与90质量份的水组成，织物在扩链槽20-25℃扩链反应5分钟后，经带压辊的导布辊导出，进入60℃红外线熟化机熟化10min后，导出成卷，得到结晶相变焓50J/g，结晶温度为27.2℃相变调温功能毛织物。
以上所述，仅为本发明创造较佳的具体实施方式，但本发明创造的保护范围并不局限于此，任何熟悉本技术领域的技术人员在本发明创造披露的技术范围内，根据本发明创造的技术方案及其发明构思加以等同替换或改变，都应涵盖在本发明创造的保护范围之内。

Claims (3)

1.一种原位在线水扩链聚氨酯相变调温功能织物的制备方法，其特征在于，包括以下步骤：
S1. 制备具有相变调温功能的聚氨酯预聚体
先将二苯基甲烷二异氰酸酯溶于甲苯，在180r/min条件下搅拌，并升温加热至80℃，混合均匀后，滴加少量二月桂酸二丁基锡，混合后得到溶液A；将聚乙二醇溶于甲苯得到溶液B，将溶液B滴加到溶液A，滴完后继续反应一段时间；反应结束，将产物离心，滤除杂质，得预聚体，将预聚体避水保存待用；
溶液A各原料之间的配比是：二苯基甲烷二异氰酸酯与甲苯的摩尔比为1:180-1:220，二月桂酸二丁基锡与二苯基甲烷二异氰酸酯的摩尔比为1.0:100-1.2:100；溶液B中聚乙二醇和甲苯摩尔比为1:100-1:300；聚乙二醇的分子质量为1000-4000；溶液A中二苯基甲烷二异氰酸酯与溶液B中聚乙二醇的摩尔比为2:0-2.2:1;
S2. 制备具有相变调温功能织物
将预聚体加入浸液槽，将待浸润织物经导布辊导入浸液槽，浸液后织物重量为原始重量的120-200%，浸液后经压辊导出送入扩链槽，在扩链槽反应一定时间后，经压辊导出，进入熟化机，定温熟化之后，成卷，得到相变调温功能织物；
待浸润织物为机织物，织物成分为棉、毛、丝、麻及其混纺织物；
所述扩链槽中加入的扩链剂是由DMF、NaHCO3或者乙醇中任一种与水组成的混合物，其中DMF或NaHCO3或乙醇与水的质量混合比为10:90；扩链反应温度为10-40℃，反应时间为2-5 min；熟化温度为40-70℃，熟化时间为5-10 min。
2.根据权利要求1所述的一种原位在线水扩链聚氨酯相变调温功能织物的制备方法，其特征在于，溶液B的滴加时间为0.5h，溶液B滴加完毕继续反应时间为1.5-2 h。
3.一种原位在线水扩链聚氨酯相变调温功能织物，其特征在于，是按照权利要求1所述的方法制备的。
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