CN107674177A - 聚氨酯固化剂生产工艺 - Google Patents

聚氨酯固化剂生产工艺 Download PDF

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CN107674177A
CN107674177A CN201711061290.0A CN201711061290A CN107674177A CN 107674177 A CN107674177 A CN 107674177A CN 201711061290 A CN201711061290 A CN 201711061290A CN 107674177 A CN107674177 A CN 107674177A
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应建忠
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Yongjia Xincheng Technology Service Co Ltd
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Yongjia Xincheng Technology Service Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/30—Low-molecular-weight compounds
    • C08G18/34—Carboxylic acids; Esters thereof with monohydroxyl compounds
    • C08G18/348—Hydroxycarboxylic acids
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40—High-molecular-weight compounds
    • C08G18/48—Polyethers
    • C08G18/4833—Polyethers containing oxyethylene units
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
    • C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
    • C08G18/6666—Compounds of group C08G18/48 or C08G18/52
    • C08G18/6692—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/34
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
    • C08G18/72—Polyisocyanates or polyisothiocyanates
    • C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
    • C08G18/76—Polyisocyanates or polyisothiocyanates cyclic aromatic
    • C08G18/7614—Polyisocyanates or polyisothiocyanates cyclic aromatic containing only one aromatic ring

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Abstract

本发明涉及一种聚氨酯固化剂生产工艺，其反应物包括聚乙二醇，二异氰酸酯，极性非质子化强溶剂，抗氧化剂、催化剂和中和剂、二羟基羧酸亲水扩链剂；主要是采用滴加反应的制备方法，羟基基团和异氰酸酯基团反应平稳，最终形成性质稳定、储存稳定的产品；产品固含量为90%、异氰酸根含量为12.5%；具有固含量高、异氰酸根含量高、水溶性和乳化效果好、性能稳定等特点。

Description

聚氨酯固化剂生产工艺
技术领域
本发明属于高分子材料领域，尤其涉及一种水性聚氨酯及其制备方法。
背景技术
水性聚氨酯乳液或分散体的应用越来越广，水性化产品的性能在某些方面体现出溶剂型产品难以比拟的优势。但单组份的水性聚氨酯具有一定的热熔胶的特性，在某些应用上需要采用水性固化剂与其混用，在受热时与活性基团反应，以达到将其成膜后的性能固化的目的。因此，亲水性的异氰酸酯固化剂也得到了相应的发展。亲水性异氰酸酯固化剂的设计一般是在多异氰酸酯中加入亲水性的基团，以达到水中乳化的目的。然而，现有水性聚氨酯固化剂制备的产品普遍存在水溶性较差、乳化效果不好、固含量低、产品稳定性和一致性差等缺点。
发明内容
本发明针对现有技术的缺点，通过对树脂结构的改良，制备出具有线形结构，接触水时具有相突变、自乳化功能的树脂溶液，得到固含量高、异氰酸根含量高，水溶性和乳化效果好的聚氨酯固化剂生产工艺。
本发明聚氨酯固化剂生产工艺的反应物包括聚乙二醇，二异氰酸酯，极性非质子化强溶剂，抗氧化剂、催化剂和中和剂；主要是采用以下生产工艺：
1）投料分子量400的聚乙二醇，916份入1500L备料釜，升温至1150C，抽真空脱水0.5小时，打开回流冷凝阀，通入氮气保护；
2）中速搅拌下，投料230份N,N-二甲基甲酰胺、91.6份2，2-二羟基丙酸、2份催化剂和4份抗氧化剂入以上备料釜，搅拌30分钟至无色液体，自然冷却备用；
3）在3000L反应釜中，通入氮气保护，打开回流阀，投料1035份甲苯二异氰酸酯，中速搅拌下，升温至800C；
4）在3小时内，缓慢滴加备料釜中物料入以上反应釜，滴加结束后，保持800C继续反应，保温2小时至异氰酸根达到设定含量；
5）关闭热水阀，打开冷却水阀，将物料降温至500C以下时，投料62份三乙胺，并充分搅拌15分钟；
6）在冷却至室温状态时，隔绝空气情况下过滤包装。
本发明的优点是采用滴加反应的制备方法，羟基基团和异氰酸酯基团反应平稳，最终形成性质稳定、储存稳定的产品；产品固含量为90%、异氰酸根含量为12.5%；具有固含量高、异氰酸根含量高、水溶性和乳化效果好、性能稳定等特点。
具体实施方式
本发明聚氨酯固化剂生产工艺的反应物包括聚乙二醇，二异氰酸酯，极性非质子化强溶剂，抗氧化剂、催化剂和中和剂；主要是采用以下生产工艺：
1）投料分子量400的聚乙二醇，916份入1500L备料釜，升温至1150C，抽真空脱水0.5小时，打开回流冷凝阀，通入氮气保护；
2）中速搅拌下，投料230份N,N-二甲基甲酰胺、91.6份2，2-二羟基丙酸、2份催化剂和4份抗氧化剂入以上备料釜，搅拌30分钟至无色液体，自然冷却备用；
3）在3000L反应釜中，通入氮气保护，打开回流阀，投料1035份甲苯二异氰酸酯，中速搅拌下，升温至800C；
4）在3小时内，缓慢滴加备料釜中物料入以上反应釜，滴加结束后，保持800C继续反应，保温2小时至异氰酸根达到设定含量；
5）关闭热水阀，打开冷却水阀，将物料降温至500C以下时，投料62份三乙胺，并充分搅拌15分钟；
6）在冷却至室温状态时，隔绝空气情况下过滤包装。
本发明生产工艺中所述的“份”为一个质量单位，一般采用1Kg为一个质量单位；本发明生产工艺中各种物质成分的比例为相对较佳值，各种时间设定是相对较佳时间；各物质的投放量可根据反应釜容量或批量大小按比例增减。

Claims (1)

1.一种聚氨酯固化剂生产工艺，其特征是：
1）投料分子量400的聚乙二醇，916份入1500L备料釜，升温至1150C，抽真空脱水0.5小时，打开回流冷凝阀，通入氮气保护；
2）中速搅拌下，投料230份N,N-二甲基甲酰胺、91.6份2，2-二羟基丙酸、2份催化剂和4份抗氧化剂入以上备料釜，搅拌30分钟至无色液体，自然冷却备用；
3）在3000L反应釜中，通入氮气保护，打开回流阀，投料1035份甲苯二异氰酸酯，中速搅拌下，升温至800C；
4）在3小时内，缓慢滴加备料釜中物料入以上反应釜，滴加结束后，保持800C继续反应，保温2小时至异氰酸根达到设定含量；
5）关闭热水阀，打开冷却水阀，将物料降温至500C以下时，投料62份三乙胺，并充分搅拌15分钟；
6）在冷却至室温状态时，隔绝空气情况下过滤包装。
CN201711061290.0A 2017-11-02 2017-11-02 聚氨酯固化剂生产工艺 Withdrawn CN107674177A (zh)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109942791A (zh) * 2019-02-22 2019-06-28 上海稻畑精细化工有限公司 一种聚氨酯固化剂的制备工艺

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109942791A (zh) * 2019-02-22 2019-06-28 上海稻畑精细化工有限公司 一种聚氨酯固化剂的制备工艺

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