A kind of room temperature crosslinking agent and preparation method thereof

A cross-linking agent, room temperature technology, used in organic chemistry and other directions, can solve problems such as low efficiency, achieve the effect of simplifying steps, significant production advantages, and improving solubility and polarity

Active Publication Date: 2018-09-07
WUHAN QIANGLONG NEW CHEM MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by this invention is to provide a kind of high yield, the preparation technology of high-quality trimethylolpropane-three-(3-ethyleneimino)-propionate room temperature cross-linking agent, to solve existing The problem of low efficiency of technology in actual industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Put methyl isobutyl ketone and pentaerythritol solvent with a volume ratio of 1:2 into the three-necked reaction flask, replace with nitrogen, add trimethylolpropane triacrylate, ethyleneimine, formaldehyde under stirring at 150 rpm Hydroquinone and hexamethylenetetramine, then add lye dropwise to adjust the pH of the mixture to 8.0, then raise the temperature to 90°C, and react for 6 hours to obtain trimethylolpropane-tri-(3-ethyleneimine )-propionate room temperature crosslinking agent, wherein the mass ratio of trimethylolpropane triacrylate, ethyleneimine, methylhydroquinone and hexamethylenetetramine is: 30:19:5:0.3 .

Embodiment 2

[0016] Put methyl isobutyl ketone and pentaerythritol solvent with a volume ratio of 2:5 into a three-necked reaction flask, replace with nitrogen, add trimethylolpropane triacrylate, ethyleneimine, formaldehyde under stirring at 100 rpm Hydroquinone and hexamethylenetetramine, then add dropwise lye to adjust the pH of the mixture to 9.0, then raise the temperature to 100°C, and react for 5 hours to obtain trimethylolpropane-tri-(3-ethyleneimine )-propionate room temperature crosslinking agent, wherein the mass ratio of trimethylolpropane triacrylate, ethyleneimine, methylhydroquinone and hexamethylenetetramine is: 32:22:4:0.2 .

Embodiment 3

[0018] Put methyl isobutyl ketone and pentaerythritol solvent with a volume ratio of 1:3 into the three-necked reaction flask, replace with nitrogen, add trimethylolpropane triacrylate, ethyleneimine, formaldehyde under stirring at 180 rpm Hydroquinone and hexamethylenetetramine, and then add lye dropwise to adjust the pH of the mixture to 8.5, then raise the temperature to 110°C, and react for 4 hours to obtain trimethylolpropane-tri-(3-ethyleneimine )-propionate room temperature crosslinking agent, wherein the mass ratio of trimethylolpropane triacrylate, ethyleneimine, methylhydroquinone and hexamethylenetetramine is: 20:25:4:0.5 .

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Abstract

The invention provides a trimethylolpropane-tri-(3-ethylimidogen)-propionate room-temperature cross-linking agent and a preparation method thereof. A simple one-step synthesis process is adopted and comprises the following specific steps: adding methylisobutylketone and a pentaerythritol solvent into a three-opening reaction flask; after replacing with nitrogen gas, adding trimethylolpropane triacrylate, ethylenimine, methylnaphthohydroquinone and hexamethylenetetramine while stirring; dropping alkali liquid to adjust the pH of the mixture, and heating the mixture to a certain temperature and reacting for a certain time to obtain the trimethylolpropane-tri-(3-ethylimidogen)-propionate room-temperature cross-linking agent. With the adoption of the preparation method, the yield and quality of the product can be improved, the cost is reduced and the operation is simple and convenient, so that the preparation method is suitable for industrially producing the trimethylolpropane-tri-(3-ethylimidogen)-propionate room-temperature cross-linking agent.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a trimethylolpropane-tri-(3-ethyleneimino)-propionate room temperature crosslinking agent and a preparation method thereof. Background technique [0002] Aziridine trifunctional cross-linking agents were developed abroad in the 1970s, and were industrialized in the 1990s. At the end of the 20th century, such products began to enter our country. The addition method is the preferred method for the early production of this product. The transesterification method is only suitable for large-scale production, requires special equipment, and is technically difficult. Therefore, the investment scale is large, the operation requirements are strict, and the product quality is slightly better than that of the addition method. [0003] The biggest advantage of the aziridine crosslinking agent is that the dosage is small, the crosslinking activity and crosslinking dens...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D203/08
CPCC07D203/08
Inventor 施明李雪莲张兵杨铧李瑞
Owner WUHAN QIANGLONG NEW CHEM MATERIALS
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