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Water-based blocked polyisocyanate crosslinking agent of highly branched structure and preparation method thereof

A polyisocyanate, highly branched technology, applied in the field of polymer materials, can solve the problem that the effective active group does not reach the ideal level, and achieve the effect of increasing the content of active groups, wide application prospects, and increasing solid content

Active Publication Date: 2014-06-18
上海浩登材料股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, a series of water-based blocked polyisocyanate crosslinking agents researched and developed by Bayer are mainly linear products, and the effective active groups contained in them have not reached the ideal level.

Method used

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  • Water-based blocked polyisocyanate crosslinking agent of highly branched structure and preparation method thereof
  • Water-based blocked polyisocyanate crosslinking agent of highly branched structure and preparation method thereof
  • Water-based blocked polyisocyanate crosslinking agent of highly branched structure and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] Under nitrogen protection and mechanical stirring, 18 parts of hexamethylene diisocyanate, 0.6% of dibutyltin dilaurate and 15 parts of methyl ethyl ketone were successively added to the four-necked flask, slowly rising to 65°C, and 1. Slowly add 5 parts of triethanolamine to the reaction system dropwise within one hour, and keep warm for 0.5 hours. The product at this time is used as the first step product; add 15 parts of triethanolamine and 12 parts of butanone in the four-necked flask, and then Slowly add the product of the first step within 1.5 hours, the reaction temperature is 60°C, and keep warm for 0.5 hours, and the product at this time is used as the product of the second step; add 35 parts of hexamethylene diisocyanate to the four-necked flask, Slowly add the second-step product dropwise within 1 hour, and keep warm at 60°C for 0.5 hours after the dropwise addition; keep the temperature constant, then add 4 parts of polyethylene glycol 600 dropwise to the sys...

Embodiment 2

[0049] Under nitrogen protection and mechanical stirring, successively add 16 parts of isophorone diisocyanate, 0.5% of stannous octoate and 15 parts of acetone into the four-necked flask, slowly rise to 65 ° C, within 1. hour 4.5 parts of triethanolamine are slowly added dropwise to the reaction system, and the temperature is maintained for 0.5 hours. The product at this time is used as the product of the first step; The product of the first step, the reaction temperature is 65°C, heat preservation for 0.5 hours, the product at this time is used as the product of the second step; add 35 parts of isophorone diisocyanate to the four-necked flask, slowly add the second step within 1.5 hours For the second-step product, keep the temperature at 65°C for 0.5 hours after the dropwise addition; keep the temperature constant, then add 6.5 parts of polyethylene glycol 400 dropwise to the system within 0.5 hours, and keep the temperature for 0.5 hours; add 32.6 parts of 2-ethyl-4-methyl...

Embodiment 3

[0051] Under nitrogen protection and mechanical stirring, 20 parts of toluene diisocyanate, 0.5% of dibutyltin dilaurate and 10 parts of N-methyl-2-pyrrolidone were successively added to the four-necked flask, slowly rising to 60 ℃, 4 parts of triethanolamine are slowly added dropwise to the reaction system within 1. hour, and the temperature is maintained for 0.5 hours. The product at this time is taken as the first step product; 12 parts of triethanolamine and 10 parts of N Methyl-2-pyrrolidone, then slowly add the product of the first step dropwise within 1 hour, the reaction temperature is 60 ° C, keep warm for 0.5 hours, the product at this time is used as the product of the second step; add 40 parts of toluene to the four-necked flask In the diisocyanate, slowly add the second-step product dropwise within 1 hour, and keep the temperature at 60°C for 0.5 hour after the dropwise addition; keep the temperature constant, and then add 8 parts of polyethylene glycol 800 dropwis...

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Abstract

The invention discloses a water-based blocked polyisocyanate crosslinking agent of a highly branched structure and a preparation method thereof. The preparation method comprises the following steps: blocking triethanolamine through diisocyanate, blocking isocyanate end group of the last step by using triethanolamine in the reversed-phase feeding manner to form a branch-type hydroxyl-blocked skeleton, reacting the skeleton with diisocyanate to convert blocking groups into isocyanate groups, carrying out chain extension by using polyethylene glycol, blocking an active isocyanate group by using imidazole derivatives and finally neutralizing amine on the skeleton structure by using acid to increase the water solubility of the crosslinking agent. The crosslinking agent has the advantages that the highly branched structure is adopted, so that the solid content and the active group content of the crosslinking agent can be increased by a large margin and the curing strength of the crosslinking agent is effectively increased; in addition, the defect that the material is embrittled during curing of the crosslinking agent can be overcome due to the introduction of the flexible polyethylene glycol chain, so that the crosslinking agent has a broad application prospect in the water-based paint curing field.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and in particular relates to a water-based blocked polyisocyanate crosslinking agent with a highly branched structure and a preparation method thereof. Background technique [0002] The blocking of isocyanates can be traced back to a research paper published by S. Petersen in the 1950s. In the development history of more than 50 years, blocked polyisocyanate has been widely used in various industries such as aerospace, automobile, paper making, chemical equipment and textile. Blocked polyisocyanate crosslinking agent, as an important branch in the application of blocked isocyanate, has also experienced a relatively long development process. [0003] Although the early isocyanate cross-linking agents contained several effective isocyanate-reactive groups on one molecule, they did not block the highly active groups. This cross-linking agent was phased out due to its short construction ti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G18/80C08G18/83C08G18/73C08G18/75C08G18/76C08G18/32C08G18/48
CPCC08G18/4833C08G18/807C08G18/833
Inventor 韦军沈健蒋乙峰孙详
Owner 上海浩登材料股份有限公司
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