CN109574874A - 一种苯甲醛及其衍生物亚胺类潜固剂 - Google Patents

一种苯甲醛及其衍生物亚胺类潜固剂 Download PDF

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CN109574874A
CN109574874A CN201910054046.4A CN201910054046A CN109574874A CN 109574874 A CN109574874 A CN 109574874A CN 201910054046 A CN201910054046 A CN 201910054046A CN 109574874 A CN109574874 A CN 109574874A
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严萍
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Shandong Fuyuan New Materials Technology Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C251/00Compounds containing nitrogen atoms doubly-bound to a carbon skeleton
    • C07C251/02Compounds containing nitrogen atoms doubly-bound to a carbon skeleton containing imino groups
    • C07C251/24Compounds containing nitrogen atoms doubly-bound to a carbon skeleton containing imino groups having carbon atoms of imino groups bound to carbon atoms of six-membered aromatic rings
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C249/00Preparation of compounds containing nitrogen atoms doubly-bound to a carbon skeleton
    • C07C249/02Preparation of compounds containing nitrogen atoms doubly-bound to a carbon skeleton of compounds containing imino groups
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40High-molecular-weight compounds
    • C08G18/48Polyethers
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/70Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
    • C08G18/72Polyisocyanates or polyisothiocyanates
    • C08G18/74Polyisocyanates or polyisothiocyanates cyclic
    • C08G18/76Polyisocyanates or polyisothiocyanates cyclic aromatic
    • C08G18/7657Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings
    • C08G18/7664Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings containing alkylene polyphenyl groups
    • C08G18/7671Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings containing alkylene polyphenyl groups containing only one alkylene bisphenyl group

Abstract

本发明涉及一种潜固剂,由聚醚胺与苯甲醛或其衍生物合成,本发明采用了工业上常见的聚醚胺类化合物作为胺类交联基团提供者,用有效降低产品成本并兼顾了生产过程中环境保护;同时采用苯甲醛及常见烷基衍生物作为氨基保护剂,形成苯甲醛类双亚胺基团,能够同时兼顾上述的稳定性与活性要求,形成一种性能优异的双二亚胺类潜固剂。

Description

一种苯甲醛及其衍生物亚胺类潜固剂
技术领域
本发明属于化工合成技术领域,具体涉及一种苯甲醛及其衍生物亚胺类潜固剂。
背景技术
潜固剂,又称潜固化剂、潜伏固化剂,在聚氨酯体系中通过与水(或湿气)优先于异氰酸酯基反应产生活性基团,然后活性基团与异氰酸酯基迅速交联固化成膜,达到固化效果。潜固剂既要有一定的稳定性(产品储存期稳定性要求),又要能在固化时间段内能优先于异氰酸酯基与水反应形成活性交联基团(固化效果要求)。专利EP0965604,US5749627,DE4021659等所提出的单、双噁唑烷等不同类型潜固剂,与上述潜固剂相比,双二亚胺是较为符合上述要求的一类产品。
发明内容
针对现有技术中存在的问题,本发明的目的在于提供一种效果优异的潜固剂。
具体的,该潜固剂由聚醚胺与苯甲醛或其衍生物合成。
所述苯甲醛或其衍生物为其中R=CmH2m+1,m=0-7。
所述聚醚胺为其中n=2-5;
优选的,聚醚胺为聚醚胺D230。
潜固剂结构式为:
式中:
具体的合成过程为:
将聚醚胺和按摩尔比1:1.8-2.2混合,加入带水剂,加热回流分水,加热回流温度为90-150摄氏度;反应完成后将带水剂蒸出。
带水剂蒸出过程为:先常压蒸馏,蒸出30%-40%后进行减压蒸馏,压力为-0.1MPa。
上述合成反应中,所述带水剂用量为原料总质量的20-200%。优选为30-40%。带水剂的用量越多,反应速度越快,但是后期带水剂蒸出能耗大、时间长。
上述合成反应中,所述带水剂为:苯、甲苯、二甲苯、石油醚、环已烷、氯仿、四氯化碳、异丙醚中的一种或几种的混合物。
本发明采用了工业上常见的聚醚胺类化合物作为胺类交联基团提供者,用有效降低产品成本并兼顾了生产过程中环境保护;同时采用苯甲醛及常见烷基衍生物作为氨基保护剂,形成苯甲醛类双亚胺基团,能够同时兼顾上述的稳定性与活性要求,形成一种性能优异的双二亚胺类潜固剂。
具体实施方式
将聚醚胺(实施例中采用聚醚胺D230)和(R=CmH2m+1,m=0-7)按摩尔比1:1.8-2.2混合,加入带水剂,加热回流分水,加热回流温度为90-150摄氏度;反应完成后将带水剂蒸出。原料及参数如下表。
使用上述实施例制备的潜固剂,以二苯甲基二异氰酸酯(MDI)和聚醚多元醇(PPG)为原料合成聚氨酯预聚体。具体步骤为:
在1000mL装有搅拌、温度、真空和加热装置的三口烧瓶中加入90g PPG,75g氯化石蜡,225g钙粉,升温至110℃,真空干燥1小时,然后降温至80℃,顺次加入28g MDI-50,75g芳烃溶剂,并保持在该温度下搅拌反应3小时,加入0.5g T-9(辛酸亚锡),继续反应3小时,降温至60℃,加入5g前表中制备所得新型潜伏性固化剂,搅拌30min,混合均匀,降温至室温,密封保存24小时。
预聚体浇入模具,自然流平,在标准状态下固化,记录表干时间,完全固化时间。脱模后测试扯断伸长率、拉伸强度、撕裂强度。
产品应用试验效果
以上所述,仅是本发明的较佳实施例而已,并非是对本发明作其它形式的限制,任何熟悉本专业的技术人员可能利用上述揭示的技术内容加以变更或改型为等同变化的等效实施例。但是凡是未脱离本发明技术方案内容,依据本发明的技术实质对以上实施例所作的任何简单修改、等同变化与改型,仍属于本发明技术方案的保护范围。

Claims (10)

1.一种潜固剂,其特征在于,由聚醚胺与苯甲醛或其衍生物合成。
2.根据权利要求1所述的潜固剂,其特征在于,所述苯甲醛或其衍生物为其中R=CmH2m+1,m=0-7。
3.一种权利要求1或2所述的潜固剂的制备方法,其特征在于,由聚醚胺、苯甲醛或其衍生物、带水剂一起加热回流,反应完成后脱水,之后将带水剂蒸出。
4.根据权利要求3所述的潜固剂的制备方法,其特征在于,所述聚醚胺与苯甲醛或其衍生物的摩尔比为1:1.8-2.2。
5.根据权利要求3所述的潜固剂的制备方法,其特征在于,反应过程是:将聚醚胺与苯甲醛或其衍生物的摩尔比为1:1.8-2.2混合,加入带水剂,加热回流分水,加热回流温度为90-150摄氏度;反应完成后将带水剂蒸出。
6.根据权利要求5所述的潜固剂的制备方法,其特征在于,带水剂蒸出过程为:先常压蒸馏,蒸出30%-40%后进行减压蒸馏,压力为-0.1MPa。
7.根据权利要求5所述的潜固剂的制备方法,其特征在于,所述带水剂用量为原料总质量的20-200%。
8.根据权利要求7所述的潜固剂的制备方法,其特征在于,所述带水剂用量为原料总质量的30-40%。
9.根据权利要求5所述的潜固剂的制备方法,其特征在于,所述带水剂为:苯、甲苯、二甲苯、石油醚、环已烷、氯仿、四氯化碳、异丙醚中的一种或几种的混合物。
10.一种权利要求5-9任一项所述方法制备的潜固剂,其特征在于,用于聚氨酯以及环氧树脂的生产。
CN201910054046.4A 2018-02-04 2019-01-21 一种苯甲醛及其衍生物亚胺类潜固剂 Pending CN109574874A (zh)

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Application publication date: 20190405