CN106085333A - 一种复合膜用大豆油基无溶剂聚氨酯胶黏剂的制备方法 - Google Patents

一种复合膜用大豆油基无溶剂聚氨酯胶黏剂的制备方法 Download PDF

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CN106085333A
CN106085333A CN201610415064.7A CN201610415064A CN106085333A CN 106085333 A CN106085333 A CN 106085333A CN 201610415064 A CN201610415064 A CN 201610415064A CN 106085333 A CN106085333 A CN 106085333A
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张萍波
王宇奇
范明明
蒋平平
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Abstract

本发明公开了一种复合膜用大豆油基无溶剂聚氨酯胶黏剂的制备方法。该无溶剂型聚氨酯胶黏剂由固化剂(A组分)和主剂(B组分)组成，其中组分A为脂肪族类异氰酸酯与聚醚类多元醇制备的端基‑NCO预聚体，组分B为大豆油基聚酯多元醇，由改性油酸与环氧大豆油在无溶剂、无催化剂条件下开环接枝制得，两种组分按‑NCO/‑OH官能团配比，在常用的食品软包装塑料/塑料复合上具备良好的粘接性能。与传统的聚氨酯胶黏剂相比，本发明涉及的聚氨酯胶黏剂不含有溶剂和有机锡类催化剂，原料绿色可再生，制备方法安全环保，交联密度大，并具有良好的耐水性能。

Description

一种复合膜用大豆油基无溶剂聚氨酯胶黏剂的制备方法
技术领域
本发明涉及食品包装复合膜用聚氨酯胶黏剂领域，特别涉及到一种大豆油基无溶剂型聚氨酯胶黏剂的制备方法。
背景技术
在食品包装领域，单层的薄膜包装无法满足各种产品性能的要求，因此，以胶黏剂复合的多层复合膜受到广泛关注并迅速发展。聚氨酯胶黏剂对薄膜载体有良好的粘接性能，使用方便，并具有优良的柔韧性能和耐候性能，在软包装复合中占据主导地位。我国聚氨酯胶黏剂近年来发展迅速，但溶剂型聚氨酯胶黏剂仍占有很大的市场份额，虽然其在外观、粘接性和抗张力方面优点突出，但其使用大量溶剂，给环境和人们的健康带来危害。随着国家对VOCs限量的规定日趋严格以及节能减排、绿色化学的提倡，无溶剂聚氨酯胶黏剂成为未来的发展方向。
目前，无溶剂型聚氨酯胶黏剂主要以不可再生的石油类下游产物为原料。而大豆油作为生物基可再生、可降解的绿色原料，利用其制备交联程度高的聚酯多元醇倍受关注，这不仅能降低对石油类多元醇的依赖，还可将聚醚、聚酯多元醇优势互补，扩大复膜胶应用范围。另外，聚氨酯胶黏剂制备中普遍使用的催化剂和芳香族异氰酸酯也给食品卫生安全带来了很大的隐患。因此，采用不含苯环的脂肪族异氰酸酯和更为绿色环保的方法制备食品级聚氨酯胶黏剂具有重要的现实意义。
发明内容
本发明的目的在于提供一种无溶剂、绿色环保、性能良好的软包装复合用聚氨酯胶黏剂及其制备方法。
本发明是通过下述技术方案加以实现的，一种复合膜用大豆油基无溶剂聚氨酯胶黏剂的制备方法，该胶黏剂由A和B两种组分构成，具体制备过程包括，
(1)A组分的制备：在反应釜中加入摩尔比为2～4:1的脂肪族二异氰酸酯和真空脱水后的端基-OH聚醚多元醇，在氮气保护下搅拌并升温至50～70℃，待体系中NCO质量分数不再变化时停止搅拌，降温出料，密封包装；
(2)B组分的制备：将质量比为9.3～9.5:1的油酸和冰醋酸加入到反应设备中，缓慢升温至50～60℃后逐滴加入质量浓度为30％的过氧化氢溶液，冰醋酸与过氧化氢质量比为1:8，1～2h滴加完毕，再缓慢升温至95～100℃继续反应1～2h，降至室温后出料，产物水洗3～4次，分离出油相后，旋蒸将水除去，置于另一充满氮气的反应釜中，再将经过真空干燥的环氧值为6～6.3％的环氧大豆油加入上述充满氮气的反应釜，环氧大豆油与油酸质量比为2.3～2.5:1，缓慢升温至170～180℃，搅拌下进行开环反应6～7h，反应完毕降温出料，即得大豆油基聚酯多元醇，羟值160～180mg KOH/g。
本发明中，所述端基-NCO预聚体(A组分)的制备过程中不使用有机锡类催化剂，所述大豆油基聚酯多元醇制备过程中不使用溶剂和催化剂。
本发明中，所述脂肪族二异氰酸酯为1,6-已二异氰酸酯、异氟尔酮二异氰酸酯、甲基环己基二异氰酸酯、二环己基甲烷二异氰酸酯中的一种或几种混合。
本发明中，所述端-OH聚醚多元醇为分子量在400～2000的聚乙二醇、聚丙二醇、聚四氢呋喃二醇中的一种或几种混合。
本发明进一步提供了采用上述大豆油基无溶剂聚氨酯胶黏剂的制备方法得到的胶黏剂用于制备复合膜的工艺，是按-NCO/-OH官能团摩尔比1.1～1.3:1称取A、B组分，在40～50℃下混合均匀后进行复膜，然后在50～60℃下固化36～48h。
与现有技术相比，本发明的有益效果是：
1、本发明的无溶剂型聚氨酯胶黏剂生产和使用过程中不使用有机溶剂和催化剂，安全环保。
2、本发明使用绿色可再生、廉价易得的环氧大豆油为原料，降低了对石油类原料的依赖。
3、本发明制备的无溶剂聚氨酯胶黏剂引入大豆油基多元醇，交联程度高，耐水耐热性能较好。
具体实施方式
下面结合实施例对本发明作进一步描述，但本发明的保护范围不仅局限于实施例，该领域专业人员对本发明技术专利所做的改变，均应属于本发明的保护范围内。
本发明的-NCO基含量按照HG/T2409-1992标准进行检测；羟值按照ASTM D 4247-99标准进行检测；T型剥离强度按照GB/T2791-1995标准进行检测。
实施例1
制备A组分：在反应釜中依次加入50g的异氟尔酮二异氰酸酯和真空脱水后的60g分子量为800的聚乙二醇，在氮气保护下搅拌，升温至60℃，每隔30min取样，测其-NCO基含量，待体系中-NCO质量分数不再变化时停止搅拌，降温出料，密封包装。所得A组分-NCO含量＝15.8％。
制备B组分：将38g油酸和4g冰醋酸加入到反应釜中，缓慢升温至60℃后逐滴加入32g过氧化氢溶液(质量浓度30％)，2h后滴加完毕，再缓慢升温至95℃继续反应1.5h，降至室温后出料，产物水洗3次，分离出油相后，旋蒸将水除去，干燥待用。接着将100g真空干燥后的环氧大豆油与上述产物40g加入到充满氮气的反应釜中，缓慢升温至180℃进行开环反应，搅拌6.5h后降温出料，即得大豆油基聚酯多元醇，羟值173mg KOH/g。
按-NCO/-OH官能团摩尔比1.2:1称取A、B组分，在50℃下混合均匀后进行涂布复膜，然后在60℃下固化48h后测得BOPP/PE复合膜的T型剥离强度3.3N/15mm。
实施例2
制备A组分：在反应釜中依次加入38g的1,6-已二异氰酸酯和真空脱水后的56g分子量为1000的聚丙二醇，在氮气保护下搅拌，升温至45℃，每隔30min取样，测其-NCO基含量，待体系中-NCO质量分数不再变化时停止搅拌，降温出料，密封包装。所得A组分-NCO含量＝15.3％。
制备B组分：将30g油酸和3.2g冰醋酸加入到反应釜中，缓慢升温至55℃后逐滴加入26g过氧化氢溶液(质量浓度30％)，1.5h后滴加完毕，再缓慢升温至100℃继续反应1h，降至室温后出料，产物水洗4次，分离出油相后，旋蒸将水除去，干燥待用。接着将80g真空干燥后的环氧大豆油与上述产物34g加入到充满氮气的反应釜中，缓慢升温至170℃进行开环反应，搅拌7h后降温出料，即得大豆油基聚酯多元醇，羟值166mg KOH/g。
按-NCO/-OH官能团摩尔比1.1:1称取A、B组分，在45℃下混合均匀后进行涂布复膜，然后在60℃下固化48h后测得BOPP/PE复合膜的T型剥离强度3.0N/15mm。
实施例3
制备A组分：在反应釜中依次加入50g的二环己基甲烷二异氰酸酯和真空脱水后的38g分子量为600的聚四氢呋喃二醇，在氮气保护下搅拌，升温至50℃，每隔30min取样，测其-NCO基含量，待体系中-NCO质量分数不再变化时停止搅拌，降温出料，密封包装。所得A组分-NCO含量＝14.2％。
制备B组分：将40g油酸和4.3g冰醋酸加入到反应釜中，缓慢升温至60℃后逐滴加入34g过氧化氢溶液(质量浓度30％)，1h后滴加完毕，再缓慢升温至100℃继续反应1.5h，降至室温后出料，产物水洗3次，分离出油相后，旋蒸将水除去，干燥待用。接着将80g真空干燥后的环氧大豆油与上述产物33.5g加入到充满氮气的反应釜中，缓慢升温至175℃进行开环反应，搅拌7h后降温出料，即得大豆油基聚酯多元醇，羟值163mg KOH/g。
按-NCO/-OH官能团摩尔比1.3:1称取A、B组分，在50℃下混合均匀后进行涂布复膜，然后在60℃下固化36h后测得BOPP/PE复合膜的T型剥离强度3.5N/15mm。

Claims (4)

1.一种复合膜用大豆油基无溶剂聚氨酯胶黏剂的制备方法，该胶黏剂由A和B两种组分构成，其特征在于包括以下过程，
(1)A组分的制备：在反应釜中加入摩尔比为2～4:1的脂肪族二异氰酸酯和真空脱水后的端基-OH聚醚多元醇，在氮气保护下搅拌并升温至50～70℃，待体系中NCO质量分数不再变化时停止搅拌，降温出料，密封包装；
(2)B组分的制备：将质量比为9.3～9.5:1的油酸和冰醋酸加入到反应设备中，缓慢升温至50～60℃后逐滴加入质量浓度为30％的过氧化氢溶液，冰醋酸与过氧化氢质量比为1:8，1～2h滴加完毕，再缓慢升温至95～100℃继续反应1～2h，降至室温后出料，产物水洗3～4次，分离出油相后，旋蒸将水除去，置于另一充满氮气的反应釜中，再将经过真空干燥的环氧值为6～6.3％的环氧大豆油加入上述充满氮气的反应釜，环氧大豆油与油酸质量比为2.3～2.5:1，缓慢升温至170～180℃，搅拌下进行开环反应6～7h，反应完毕降温出料，即得大豆油基聚酯多元醇，羟值160～180mg KOH/g。
2.按权利要求1所述的制备方法，其特征在于，所述脂肪族二异氰酸酯为1,6-已二异氰酸酯、异氟尔酮二异氰酸酯、甲基环己基二异氰酸酯、二环己基甲烷二异氰酸酯中的一种或几种混合。
3.按权利要求1所述的制备方法，其特征在于，所述端-OH聚醚多元醇为分子量在400～2000的聚乙二醇、聚丙二醇、聚四氢呋喃二醇中的一种或几种混合。
4.按权利要求1所述的胶黏剂的制备方法得到的胶黏剂用于制备复合膜的工艺，其特征在于，按-NCO/-OH官能团摩尔比1.1～1.3:1称取A、B组分，在40～50℃下混合均匀后进行复膜，然后在50～60℃下固化36～48h。
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