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Method for preparing polyisocyanate containing biuret structure with stable storage

A polyisocyanate, storage-stable technology, applied in the field of polyisocyanate preparation, can solve the problems of surrounding environment and construction personnel injury, high cost of aldoxime compounds, limited application and other problems, and achieve the effect of excellent long-term storage stability

Active Publication Date: 2016-05-25
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, the cost of aldoxime compounds is too high, which limits their application as industrial biuret reagents
[0008] Biuret products prepared by existing methods have the problem of increased residual monomer content during long-term storage, which has a great impact and harm on the surrounding environment and construction personnel

Method used

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  • Method for preparing polyisocyanate containing biuret structure with stable storage
  • Method for preparing polyisocyanate containing biuret structure with stable storage
  • Method for preparing polyisocyanate containing biuret structure with stable storage

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035]1) Dissolve 1.8g of 5-methyl-8-aminomethylquinoline and 2.86g of oxalic acid dihydrazide in 10.0g of water, preheat to 40°C, keep warm, and set aside;

[0036] 2) Under the protection of nitrogen, add 500g of hexamethylene diisocyanate (HDI) and 0.5g of diisopropyl phosphate into the reaction vessel, heat to 160°C, the dissolved 5-methyl-8-ammonia Add the water of methylquinoline and oxalic acid dihydrazide dropwise into the reaction vessel, and the dropping time is controlled at 50 minutes; after the dropwise addition, continue to stir and react at 160°C for 1 hour; then cool to below 35°C , blowing to obtain a biuret reaction solution;

[0037] 3) Enter the biuret reaction solution synthesized in step 2) into the secondary short-path evaporator separation device at a feed rate of 25mL / min to separate unreacted diisocyanate and polyisocyanate containing biuret structure, the first stage The separation temperature of the short-path evaporator is controlled at 140°C, the...

Embodiment 2

[0039] 1) Dissolve 1.02g of 5-chloro-8-aminomethylquinoline and 0.98g of adipic dihydrazide in 10.0g of water, preheat to 40°C, keep warm, and set aside;

[0040] 2) Under nitrogen protection, add 500g of hexamethylene diisocyanate (HDI) and 0.5g of diisopropyl phosphate into the reaction vessel, heat to 160°C, and dissolve 5-chloro-8-aminomethyl The water of quinoline and adipic acid dihydrazide was added dropwise into the reaction vessel, and the dropping time was controlled to be 50 minutes; after the dropwise addition, the stirring reaction was continued at 160°C for 1 hour; then cooled to below 35°C, and put The material obtains the biuret reaction liquid;

[0041] 3) Enter the biuret reaction solution synthesized in step 2) into the secondary short-path evaporator separation device at a feed rate of 25mL / min to separate unreacted diisocyanate and polyisocyanate containing biuret structure. The separation conditions are the same as Example 1: Dilute the polyisocyanate co...

Embodiment 3

[0043] 1) Dissolve 0.81g of 5-chloro-8-aminomethylquinoline and 0.07g of maleic hydrazide in 15.0g of water, preheat to 80°C, keep warm, and set aside;

[0044] 2) Under the protection of nitrogen, add 500g of hexamethylene diisocyanate (HDI) and 0.5g of diisopropyl phosphate into the reaction vessel, heat to 150°C, and dissolve the 5-chloro-8-aminomethyl The water of quinoline and maleic hydrazide was added dropwise into the reaction vessel, and the dropping time was controlled to be 60 minutes; after the dropping was completed, the stirring reaction was continued at 150°C for 1.5 hours; then cooled to below 35°C, and the material was discharged Obtain biuret reaction solution;

[0045] 3) Put the biuret reaction solution synthesized in step 2) into the secondary short-path evaporator separation device at a feed rate of 20mL / min to separate unreacted diisocyanate and polyisocyanate containing biuret structure. The separation conditions are the same as Example 1: Dilute the p...

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Abstract

The invention relates to a method for preparing polyisocyanate containing a biuret structure. The method uses a reaction of polyisocyanate and water under existence of a substituted 8-aminomethyl quinoline compound and a hydrazine derivative to prepare biuret-containing polyisocyanate. A color number of the produced product is lower than 20 Hazen, under synergism of the substituted 8-aminomethyl quinoline compound and the hydrazine derivative, product is stored for 6 months, increasing amount of the monomer content is less than 0.1 wt%, and the product has excellent long-term storage stability.

Description

technical field [0001] The present invention relates to the preparation of polyisocyanate containing biuret structure, more specifically to a preparation method of polyisocyanate containing biuret structure with low color number and good long-term storage stability. Background technique [0002] Aliphatic or alicyclic biuret polyisocyanate is widely used in the production of coating compositions, adhesives, sealants, foams, elastomers, fiber treatment agents, etc., the preparation method of aliphatic polyisocyanate with biuret structure It has been disclosed by German patent document DE1101394 since 1958. Further possible preparation methods are also disclosed in the review paper "The Synthesis of Aliphatic Polyisocyanates Containing Biuret, isocyanurate oruret dione backbones for use in coatings" (J. prakt. Chem, 336, 1994, 185-200), which discusses the advantages and disadvantages of these specific methods. [0003] The preparation of biuret-containing polyisocyanates is ...

Claims

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Application Information

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IPC IPC(8): C07D215/12C07D215/18
Inventor 王彪尚永华石滨李海军黎源华卫琦
Owner WANHUA CHEM GRP CO LTD
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