CN106543911A - 酪素‑聚氨酯乳液胶膜的制备方法 - Google Patents

酪素‑聚氨酯乳液胶膜的制备方法 Download PDF

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CN106543911A
CN106543911A CN201611125441.XA CN201611125441A CN106543911A CN 106543911 A CN106543911 A CN 106543911A CN 201611125441 A CN201611125441 A CN 201611125441A CN 106543911 A CN106543911 A CN 106543911A
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王耀斌
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Abstract

本发明酪素‑聚氨酯乳液胶膜的制备方法涉及聚氨酯工业领域，具体涉及酪素‑聚氨酯乳液胶膜的制备方法，包括以下步骤：酪素液的配制，在装有冷凝器、搅拌和温度计的三口烧瓶中加入水和干酪素，缓慢搅拌升温至65度，使酪素溶胀，加入三乙胺溶液，调节pH值为9‑10，待酪素溶胀呈半透明体系后继续恒温搅拌1h，得酪素液，冷却备用；聚氨酯预聚体及酪素‑聚氨酯乳液的制备，在干燥氮气保护下，将异佛尔酮二异氰酸酯和真空脱水后的聚四氢呋喃醚二醇加入带有温度计、搅拌杆和冷凝管的四口烧瓶中，混合均匀后，升温至88‑92度反应2h，本发明操作简单，加工方便，且能够提高产品性能，保证产品质量，安全可靠。

Description

酪素-聚氨酯乳液胶膜的制备方法
技术领域
本发明涉及聚氨酯工业领域，具体涉及酪素-聚氨酯乳液胶膜的制备方法。
背景技术
水性聚氨酯因其优异的性能和环保性已得到了广泛应用。随着新材料如生物医用材料、航天材料等的开发，水性聚氨酯的应用领域也在不断扩展。由于聚氨酯软硬段的热力学不相容性，聚氨酯表现出特殊的微相分离结构，使得其可以出现一个甚至两个Ｔg。聚氨酯材料的聚集态结构一般是软段区为连续相，硬段区为分散相，同时硬段区充当着物理交联点的作用，因此材料可以表现出特殊的强而韧的特性。
近年来，对水性聚氨酯软段改性的研究较多，主要集中在聚醚和聚酯多元醇的选择和改性方面；对于硬段，除了用不同的异氰酸酯和亲水基团等作为改变硬段的重要手段外，还可以通过改变硬段含量来探究水性聚氨酯结构与性能的变化。干酪素是一种含磷蛋白质，其结构与普通蛋白质相似，是由氨基酸以肽键相连接的天然高分子，存在较多的活性基团易与NCO封端的水性聚氨酯发生反应，生成交联结构。用酪素对水性聚氨酯进行改性，改性后的水性聚氨酯性能有较大的提升，成膜的光泽度以及强度也有明显的提高。对于水性聚氨酯本身硬段含量的变化对性能的影响研究较少。
发明内容
本发明目的在于提供一种操作简单，加工方便，且能够提高产品性能，保证产品质量，安全可靠的酪素-聚氨酯乳液胶膜的制备方法。
本发明酪素-聚氨酯乳液胶膜的制备方法，包括以下步骤：
第一步，酪素液的配制
在装有冷凝器、搅拌和温度计的三口烧瓶中加入水和干酪素，缓慢搅拌升温至65度，使酪素溶胀，加入三乙胺溶液，调节pH 值为9-10，待酪素溶胀呈半透明体系后继续恒温搅拌1h，得酪素液，冷却备用；
第二步，聚氨酯预聚体及酪素-聚氨酯乳液的制备
在干燥氮气保护下，将异佛尔酮二异氰酸酯和真空脱水后的聚四氢呋喃醚二醇加入带有温度计、搅拌杆和冷凝管的四口烧瓶中，混合均匀后，升温至88-92度反应2h，加入二羟甲基丙酸、一缩二乙二醇及丙酮调节粘度，然后加入催化剂辛酸亚锡和二月桂酸二丁基锡各数滴，68-72度反应，采用二正丁胺滴定法确定残留的NCO含量达到理论值即为反应终点，降温至40度出料；将聚氨酯预聚体用三乙胺中和，加入酪素液，在冰水浴中乳化30min，得到酪素-聚氨酯乳液；
第三步，酪素-聚氨酯乳液胶膜的制备
将合成的酪素-聚氨酯乳液倒入水平放置的自制聚四氟乙烯板槽中，室温干燥1周后取出胶膜，放入真空干燥箱中45度下烘干直至恒重，取出自然冷却，放入干燥器中备用。
优选地，第一步中水和干酪素的比例为9:1。
本发明操作简单，加工方便，且能够提高产品性能，保证产品质量，安全可靠。
具体实施方式
实施例一：
本发明酪素-聚氨酯乳液胶膜的制备方法，包括以下步骤：
第一步，酪素液的配制
在装有冷凝器、搅拌和温度计的三口烧瓶中加入水和干酪素，缓慢搅拌升温至65度，使酪素溶胀，加入三乙胺溶液，调节pH 值为9-10，待酪素溶胀呈半透明体系后继续恒温搅拌1h，得酪素液，冷却备用；
第二步，聚氨酯预聚体及酪素-聚氨酯乳液的制备
在干燥氮气保护下，将异佛尔酮二异氰酸酯和真空脱水后的聚四氢呋喃醚二醇加入带有温度计、搅拌杆和冷凝管的四口烧瓶中，混合均匀后，升温至88-92度反应2h，加入二羟甲基丙酸、一缩二乙二醇及丙酮调节粘度，然后加入催化剂辛酸亚锡和二月桂酸二丁基锡各数滴，68-72度反应，采用二正丁胺滴定法确定残留的NCO含量达到理论值即为反应终点，降温至40度出料；将聚氨酯预聚体用三乙胺中和，加入酪素液，在冰水浴中乳化30min，得到酪素-聚氨酯乳液；
第三步，酪素-聚氨酯乳液胶膜的制备
将合成的酪素-聚氨酯乳液倒入水平放置的自制聚四氟乙烯板槽中，室温干燥1周后取出胶膜，放入真空干燥箱中45度下烘干直至恒重，取出自然冷却，放入干燥器中备用。
实施例二：
本发明酪素-聚氨酯乳液胶膜的制备方法，包括以下步骤：
第一步，酪素液的配制
在装有冷凝器、搅拌和温度计的三口烧瓶中加入水和干酪素，缓慢搅拌升温至65度，使酪素溶胀，加入三乙胺溶液，调节pH 值为9-10，待酪素溶胀呈半透明体系后继续恒温搅拌1h，得酪素液，冷却备用；
第二步，聚氨酯预聚体及酪素-聚氨酯乳液的制备
在干燥氮气保护下，将异佛尔酮二异氰酸酯和真空脱水后的聚四氢呋喃醚二醇加入带有温度计、搅拌杆和冷凝管的四口烧瓶中，混合均匀后，升温至88-92度反应2h，加入二羟甲基丙酸、一缩二乙二醇及丙酮调节粘度，然后加入催化剂辛酸亚锡和二月桂酸二丁基锡各数滴，68-72度反应，采用二正丁胺滴定法确定残留的NCO含量达到理论值即为反应终点，降温至40度出料；将聚氨酯预聚体用三乙胺中和，加入酪素液，在冰水浴中乳化30min，得到酪素-聚氨酯乳液；
第三步，酪素-聚氨酯乳液胶膜的制备
将合成的酪素-聚氨酯乳液倒入水平放置的自制聚四氟乙烯板槽中，室温干燥1周后取出胶膜，放入真空干燥箱中45度下烘干直至恒重，取出自然冷却，放入干燥器中备用。
第一步中水和干酪素的比例为9:1。
本发明操作简单，加工方便，且能够提高产品性能，保证产品质量，安全可靠。

Claims (2)

1.一种酪素-聚氨酯乳液胶膜的制备方法，其特征在于，包括以下步骤：
第一步，酪素液的配制
在装有冷凝器、搅拌和温度计的三口烧瓶中加入水和干酪素，缓慢搅拌升温至65度，使酪素溶胀，加入三乙胺溶液，调节pH 值为9-10，待酪素溶胀呈半透明体系后继续恒温搅拌1h，得酪素液，冷却备用；
第二步，聚氨酯预聚体及酪素-聚氨酯乳液的制备
在干燥氮气保护下，将异佛尔酮二异氰酸酯和真空脱水后的聚四氢呋喃醚二醇加入带有温度计、搅拌杆和冷凝管的四口烧瓶中，混合均匀后，升温至88-92度反应2h，加入二羟甲基丙酸、一缩二乙二醇及丙酮调节粘度，然后加入催化剂辛酸亚锡和二月桂酸二丁基锡各数滴，68-72度反应，采用二正丁胺滴定法确定残留的NCO含量达到理论值即为反应终点，降温至40度出料；将聚氨酯预聚体用三乙胺中和，加入酪素液，在冰水浴中乳化30min，得到酪素-聚氨酯乳液；
第三步，酪素-聚氨酯乳液胶膜的制备
将合成的酪素-聚氨酯乳液倒入水平放置的自制聚四氟乙烯板槽中，室温干燥1周后取出胶膜，放入真空干燥箱中45度下烘干直至恒重，取出自然冷却，放入干燥器中备用。
2.如权利要求1所述酪素-聚氨酯乳液胶膜的制备方法，其特征在于，第一步中水和干酪素的比例为9:1。
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108676350A (zh) * 2018-04-26 2018-10-19 阜南县慧宏柳木工艺品有限公司 一种柳条去皮机输送辊用塑胶的制备方法
CN110003425A (zh) * 2019-02-28 2019-07-12 常州五荣化工有限公司 一种生物可降解聚氨酯复合材料的制备方法
CN110359300A (zh) * 2019-08-22 2019-10-22 辽宁恒星精细化工有限公司 棉织物双色效应涂层胶及双色效应涂层整理方法
CN116172303A (zh) * 2023-04-21 2023-05-30 比音勒芬服饰股份有限公司 一种具有三角梅形态的防滑耐磨eva鞋底

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108676350A (zh) * 2018-04-26 2018-10-19 阜南县慧宏柳木工艺品有限公司 一种柳条去皮机输送辊用塑胶的制备方法
CN110003425A (zh) * 2019-02-28 2019-07-12 常州五荣化工有限公司 一种生物可降解聚氨酯复合材料的制备方法
CN110359300A (zh) * 2019-08-22 2019-10-22 辽宁恒星精细化工有限公司 棉织物双色效应涂层胶及双色效应涂层整理方法
CN110359300B (zh) * 2019-08-22 2021-08-24 辽宁恒星精细化工有限公司 棉织物双色效应涂层胶及双色效应涂层整理方法
CN116172303A (zh) * 2023-04-21 2023-05-30 比音勒芬服饰股份有限公司 一种具有三角梅形态的防滑耐磨eva鞋底

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