CN107384291A - 一种可快速固化的水性聚氨酯纸板胶黏剂及其制备方法 - Google Patents

一种可快速固化的水性聚氨酯纸板胶黏剂及其制备方法 Download PDF

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CN107384291A
CN107384291A CN201611204993.XA CN201611204993A CN107384291A CN 107384291 A CN107384291 A CN 107384291A CN 201611204993 A CN201611204993 A CN 201611204993A CN 107384291 A CN107384291 A CN 107384291A
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王强
查道友
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Anqing Decheng Chemical Co Ltd
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Abstract

本发明公开一种可快速固化的水性聚氨酯纸板胶黏剂，由以下重量份的原料组成：聚乙二醇45‑60，二环己基甲烷二异氰酸酯25‑35，粗碱木质素4‑11，10％NaOH溶液适量，10％盐酸溶液适量，异佛尔酮二异氰酸酯8‑17，二月桂酸二丁基锡0.4‑0.8，丙酮适量，二乙醇胺10‑25，桐油4‑10，乙醇钠0.4‑0.8，二羟甲基丙酸3‑8，N‑甲基吡咯烷酮适量，N‑甲基二乙醇胺2‑9，三乙胺12‑25，松香树脂乳液1‑4，蒸馏水适量，膨润土3‑10，十八酸0.6‑2，碳酸钠0.1‑0.4，云母粉1‑3。本发明在水性聚氨酯胶黏剂中引入经‑NCO基团修饰的木质素，增加胶黏剂对纸张的粘合力，另一方能提高水性聚氨酯胶黏剂的耐水性能，产品具有粘结牢度好、无霉烂等特点。

Description

一种可快速固化的水性聚氨酯纸板胶黏剂及其制备方法
技术领域
本发明涉及胶黏剂领域，确切地说是一种可快速固化的水性聚氨酯纸板胶黏剂及其制备方法。
背景技术
物体的粘接，就是靠胶中的高分子体间的拉力来实现的，胶中的溶剂载着高分子体慢慢地浸入到物体的组织内，当胶水中的溶剂消失后，胶水中的高分子体就依靠相互间的拉力，将两个物体紧紧的结合，现有的纸张粘合剂诸多存在返潮、霉烂等现象，特别是影响纸张的手感以及存在严重的环保问题。
聚氨酯胶黏剂具有软硬度等性能，可调节性好，耐低温，柔韧性好，粘接强度大等优点，但是，目前在整个聚氨酯胶黏剂领域中以溶剂型聚氨酯胶黏剂为主，其缺点是有机溶剂气味大，易挥发，使用时造成空气污染、易燃、或多或少具有毒性等，因此近年来各国聚氨酯材料研究人员花费相当大的精力进行水性聚氨酯胶黏剂的开发和研究。水性聚氨酯是一种聚氨酯粒子分散于水中的二元胶体体系。水性聚氨酯以水为介质，具有安全、不燃烧、无公害的独特优点。
刘璐、任志勇等人在其《羟基化桐油衍生的两性聚氨酯水分散体的制备和性能研究》一文中，以聚乙二醇(PEG-800)、N-甲基二乙醇胺(MDEA)、二羟甲基丙酸(DMPA)、4,4'-二环己基甲烷二异氰酸酯(HMDI)和羟基化桐油(HTO)等为原料，合成了羟基化桐油衍生的两性聚氨酯(HTO-ZPUD)，通过后交联提高水性两性聚氨酯的耐水性和耐溶剂性，但其粘性不足。
因此，本发明在水性聚氨酯胶黏剂中引入经-NCO基团修饰的木质素，增加胶黏剂对纸张的粘合力，另一方能提高水性聚氨酯胶黏剂的耐水性能。
发明内容
针对现有技术的不足，本发明的目的在于提供一种可快速固化的水性聚氨酯纸板胶黏剂及其制备方法。
一种可快速固化的水性聚氨酯纸板胶黏剂，由以下重量份的原料组成：聚乙二醇45-60份，二环己基甲烷二异氰酸酯25-35份，粗碱木质素4-11份，10％NaOH溶液适量，10％盐酸溶液适量，异佛尔酮二异氰酸酯8-17份，二月桂酸二丁基锡0.4-0.8份，丙酮适量，二乙醇胺10-25份，桐油4-10份，乙醇钠0.4-0.8份，二羟甲基丙酸3-8份，N-甲基吡咯烷酮适量，N-甲基二乙醇胺2-9份，三乙胺12-25份，松香树脂乳液1-4份，蒸馏水适量，膨润土3-10份，十八酸0.6-2份，碳酸钠0.1-0.4份，云母粉1-3份。
具体步骤如下：
(1)-NCO基木质素的制备：
①、将粗碱木质素配制成浓度为30％的水溶液，用质量分数为10％NaOH溶液调节pH至13-14，使碱木质素充分溶解后除去不溶物，然后用10％盐酸溶液于55-65℃下调pH至2-3，沉淀出碱木质素，过滤，反复用蒸馏水洗涤沉淀至中性，于50-70℃真空干燥，得碱木质素备用；
②、在带磁力揽拌的单口瓶中加入异佛尔酮二异氰酸酯、二月桂酸二丁基锡、丙酮以及上述碱木质素，充分搅拌后，在30-50℃超声分散1-3小时，然后在50-60℃回流反应3-5小时，冷却至室温，分离、丙酮洗涤，将滤饼在70-85℃下真空干燥3-4小时，研磨后即得到-NCO基木质素；
(2)羟基化桐油的制备：
将桐油和二乙醇胺加入装有搅拌器、回流冷凝管、温度计和氮气保护的四口烧瓶中，于40-55℃下加入乙醇钠，之后控制反应温度在105-125℃之间，回流搅拌2-5小时，得到羟基化桐油；
(3)羟基化桐油改性水性聚氨酯/木质素复合乳液的制备：
将聚乙二醇置于四口烧瓶中升温110-130℃真空下脱水2-3小时，在氮气环境下降温至50-70℃，加入二环己基甲烷二异氰酸酯、步骤(1)-NCO基木质素搅拌反应0.5-2小时，滴加溶有二羟甲基丙酸的N-甲基吡咯烷酮溶液，控温在75-85℃下搅拌反应50-70分钟，降温在70-80℃，加入步骤(2)羟基化桐油和N-甲基二乙醇胺，反应1-2小时，加入三乙胺中和15-25分钟，加热至70-90℃加水乳化，得到羟基化桐油改性水性聚氨酯/木质素复合乳液；
(4)改性膨润土的制备：
①将膨润土加水打浆，打浆后浆液浓度为10-15wt％，然后加入碳酸钠及10％NaOH溶液，充分搅拌反应0.5-1.5小时，形成人工钠基土，调节pH至9-11，待用；
②配制10-20％的十八酸皂液，在常温不断搅拌下，将十八酸皂液缓慢加入膨润土浆液中，待充分搅拌、混合均匀后，缓慢升温到60-80℃，在碱性条件下充分反应2-4小时，再经10％盐酸溶液中和，并脱水、水洗，得到改性膨润土；
(5)将步骤(3)复合乳液加入松香树脂乳液、云母粉以及步骤(4)改性膨润土，抽真空至真空度为0.5-0.8MPa，以300-500r/min的速率高速搅拌混合20-30分钟，得到所述水性聚氨酯胶黏剂。
与现有技术相比，本发明具有以下优点：
(1)木质素是一种具有三维网状立体结构的复杂的聚酚类物质，分子中含有丰富的醇羟基和酚羟基等活性基团，本发明中利用这些活性基团与异氰酸酯反应，获得表面被-NCO基团修饰的木质素，之后参与水性聚氨酯的合成反应得到生物质基水性聚氨酯乳液，可与纸张中的羟基发生化学反应，从而产生良好的粘结效果，又能赋予胶黏剂生物降解性能，环保效果好，另外-NCO基团修饰的木质素可与聚乙二醇、羟基化桐油发生反应，使得链段之间的相互作用增强，提升交联强度，耐水性得到提高，包装盒粘合后不返潮、无霉烂，不影响纸张手感。
(2)羟基化桐油可看做含三个共轭双键的长疏水支链，将其引入聚氨酯成为含双键桐油水性聚氨酯乳液，其实质是向聚氨酯中引入了含双键长疏水支链，使得疏水缔合作用明显，对胶黏剂的增稠性越好，制备的水性聚氨酯胶黏剂具有初始粘性好，粘接强度高等特点，同时双键的引入可提高胶体的交联密度，使产品的耐水、耐溶剂性显著提升。
(3)本发明中加入改性处理后的膨润土，增强了胶黏剂产品的粘结力，并明显提高了固化速率，对不同纸质适应性强，用其粘结的纸箱受潮、水浸不开胶，长途运输和仓储破损率低，适用于各种产品的包装。
具体实施方式
一种可快速固化的水性聚氨酯纸板胶黏剂，由以下重量份的原料组成：聚乙二醇55，二环己基甲烷二异氰酸酯30，粗碱木质素9，10％NaOH溶液适量，10％盐酸溶液适量，异佛尔酮二异氰酸酯12，二月桂酸二丁基锡0.6，丙酮适量，二乙醇胺20，桐油9，乙醇钠0.7，二羟甲基丙酸6，N-甲基吡咯烷酮适量，N-甲基二乙醇胺7，三乙胺18，松香树脂乳液3，蒸馏水适量，膨润土8，十八酸1，碳酸钠0.3，云母粉2。
具体步骤如下：
(1)-NCO基木质素的制备：
①、将粗碱木质素配制成浓度为30％的水溶液，用质量分数为10％NaOH溶液调节pH至13-14，使碱木质素充分溶解后除去不溶物，然后用10％盐酸溶液于60℃下调pH至2-3，沉淀出碱木质素，过滤，反复用蒸馏水洗涤沉淀至中性，于65℃真空干燥，得碱木质素备用；
②、在带磁力揽拌的单口瓶中加入异佛尔酮二异氰酸酯、二月桂酸二丁基锡、丙酮以及上述碱木质素，充分搅拌后，在40℃超声分散2小时，然后在55℃回流反应4小时，冷却至室温，分离、丙酮洗涤，将滤饼在80℃下真空干燥4小时，研磨后即得到-NCO基木质素；
(2)羟基化桐油的制备：
将桐油和二乙醇胺加入装有搅拌器、回流冷凝管、温度计和氮气保护的四口烧瓶中，于50℃下加入乙醇钠，之后控制反应温度在115℃之间，回流搅拌4小时，得到羟基化桐油；
(3)羟基化桐油改性水性聚氨酯/木质素复合乳液的制备：
将聚乙二醇置于四口烧瓶中升温120℃真空下脱水3小时，在氮气环境下降温至60℃，加入二环己基甲烷二异氰酸酯、步骤(1)-NCO基木质素搅拌反应1小时，滴加溶有二羟甲基丙酸的N-甲基吡咯烷酮溶液，控温在80℃下搅拌反应60分钟，降温在75℃，加入步骤(2)羟基化桐油和N-甲基二乙醇胺，反应1.5小时，加入三乙胺中和20分钟，加热至80℃加水乳化，得到羟基化桐油改性水性聚氨酯/木质素复合乳液；
(4)改性膨润土的制备：
①将膨润土加水打浆，打浆后浆液浓度为15wt％，然后加入碳酸钠及10％NaOH溶液，充分搅拌反应1小时，形成人工钠基土，调节pH至10，待用；
②配制15％的十八酸皂液，在常温不断搅拌下，将十八酸皂液缓慢加入膨润土浆液中，待充分搅拌、混合均匀后，缓慢升温到70℃，在碱性条件下充分反应3小时，再经10％盐酸溶液中和，并脱水、水洗，得到改性膨润土；
(5)将步骤(3)复合乳液加入松香树脂乳液、云母粉以及步骤(4)改性膨润土，抽真空至真空度为0.7MPa，以400r/min的速率高速搅拌混合25分钟，得到所述水性聚氨酯胶黏剂。
按照具体实施例制备的制备的水性聚氨酯胶黏剂，对其进行性能测试，结果如下：
粘结固化时间(30℃)：<45min，剥离强度：106N/(2.5cm)，初始粘度(25℃)：10360mPa·s。

Claims (2)

1.一种可快速固化的水性聚氨酯纸板胶黏剂，其特征在于，由以下重量份的原料组成：聚乙二醇45-60份，二环己基甲烷二异氰酸酯25-35份，粗碱木质素4-11份，10％NaOH溶液适量，10％盐酸溶液适量，异佛尔酮二异氰酸酯8-17份，二月桂酸二丁基锡0.4-0.8份，丙酮适量，二乙醇胺10-25份，桐油4-10份，乙醇钠0.4-0.8份，二羟甲基丙酸3-8份，N-甲基吡咯烷酮适量，N-甲基二乙醇胺2-9份，三乙胺12-25份，松香树脂乳液1-4份，蒸馏水适量，膨润土3-10份，十八酸0.6-2份，碳酸钠0.1-0.4份，云母粉1-3份。
2.根据权利要求书1所述的一种可快速固化的水性聚氨酯纸板胶黏剂的制备方法，其特征在于，具体步骤如下：
(1)-NCO基木质素的制备：
①、将粗碱木质素配制成浓度为30％的水溶液，用质量分数为10％NaOH溶液调节pH至13-14，使碱木质素充分溶解后除去不溶物，然后用10％盐酸溶液于55-65℃下调pH至2-3，沉淀出碱木质素，过滤，反复用蒸馏水洗涤沉淀至中性，于50-70℃真空干燥，得碱木质素备用；
②、在带磁力揽拌的单口瓶中加入异佛尔酮二异氰酸酯、二月桂酸二丁基锡、丙酮以及上述碱木质素，充分搅拌后，在30-50℃超声分散1-3小时，然后在50-60℃回流反应3-5小时，冷却至室温，分离、丙酮洗涤，将滤饼在70-85℃下真空干燥3-4小时，研磨后即得到-NCO基木质素；
(2)羟基化桐油的制备：
将桐油和二乙醇胺加入装有搅拌器、回流冷凝管、温度计和氮气保护的四口烧瓶中，于40-55℃下加入乙醇钠，之后控制反应温度在105-125℃之间，回流搅拌2-5小时，得到羟基化桐油；
(3)羟基化桐油改性水性聚氨酯/木质素复合乳液的制备：
将聚乙二醇置于四口烧瓶中升温110-130℃真空下脱水2-3小时，在氮气环境下降温至50-70℃，加入二环己基甲烷二异氰酸酯、步骤(1)-NCO基木质素搅拌反应0.5-2小时，滴加溶有二羟甲基丙酸的N-甲基吡咯烷酮溶液，控温在75-85℃下搅拌反应50-70分钟，降温在70-80℃，加入步骤(2)羟基化桐油和N-甲基二乙醇胺，反应1-2小时，加入三乙胺中和15-25分钟，加热至70-90℃加水乳化，得到羟基化桐油改性水性聚氨酯/木质素复合乳液；
(4)改性膨润土的制备：
①将膨润土加水打浆，打浆后浆液浓度为10-15wt％，然后加入碳酸钠及10％NaOH溶液，充分搅拌反应0.5-1.5小时，形成人工钠基土，调节pH至9-11，待用；
②配制10-20％的十八酸皂液，在常温不断搅拌下，将十八酸皂液缓慢加入膨润土浆液中，待充分搅拌、混合均匀后，缓慢升温到60-80℃，在碱性条件下充分反应2-4小时，再经10％盐酸溶液中和，并脱水、水洗，得到改性膨润土；
(5)将步骤(3)复合乳液加入松香树脂乳液、云母粉以及步骤(4)改性膨润土，抽真空至真空度为0.5-0.8MPa，以300-500r/min的速率高速搅拌混合20-30分钟，得到所述水性聚氨酯胶黏剂。
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