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Preparation method of hexamethylene diisocyanate tripolymer curing agent

A trimerization technology of hexamethylene diisocyanate and isocyanate, applied in organic chemistry, polyurea/polyurethane coatings, coatings, etc., can solve the problems of high reaction temperature, low catalytic efficiency, easy to produce by-products, etc., and achieve catalytic High efficiency, increase heat transfer area, and save solvent cost

Inactive Publication Date: 2013-12-11
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The present invention provides a method for preparing a hexamethylene diisocyanate trimer curing agent in view of the shortcomings of the existing HDI trimer preparation method, such as high reaction temperature, low catalytic efficiency and easy production of by-products.

Method used

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  • Preparation method of hexamethylene diisocyanate tripolymer curing agent

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Effect test

Embodiment 1

[0026] Preparation of 2-hydroxyalkyl quaternary ammonium base: in parts by mass, under nitrogen protection, 38 parts of propylene oxide were added dropwise to a system of 65 parts of triethylamine and 12 parts of water within 1 h to maintain the system The temperature is 30°C. After the addition of propylene oxide was completed, the stirring continued for 12 hours. After the reaction was stopped, the yellow liquid in the lower layer was separated with a rotary evaporator to obtain the product 2-hydroxyalkyl quaternary ammonium base in the form of yellow oil. In the prior art, quaternary ammonium salt catalysts are used to catalyze aromatic highly active diisocyanates such as TDI. For aliphatic diisocyanates (such as HDI, IPDI) with weak monomer activity, the catalytic activity of quaternary ammonium salts is very small. Except for special quaternary ammonium salts with fatty chain segments (for example, 2-hydroxypropyltrimethylisooctanoic acid ammonium salt), which are oily ...

Embodiment 2

[0032] Preparation of 2-hydroxyalkyl quaternary ammonium base: under the protection of nitrogen, 25.94g of propylene oxide was added dropwise to 80g of trimethylamine aqueous solution (33% by mass), and the dropwise addition was completed in one hour. Stirring was continued at 35 °C for 24 h. After stopping the reaction, the yellow liquid in the lower layer was separated with a rotary evaporator to obtain the product 2-hydroxyalkyl quaternary ammonium base in the form of light yellow oil.

[0033] (1) Put 100g of HDI monomer into the reaction container under the protection of nitrogen, and dropwise add the trimerization catalyst 2-hydroxyalkyl quaternary ammonium base prepared by accounting for more than 0.2% of the mass of isocyanate monomer within 1.5h, maintain the temperature at 40°C, and keep it warm Stirring and reacting for 8h; when the mass percentage of free NCO groups was measured to be 35%, add a phosphoric acid polymerization inhibitor accounting for 0.3% of the ma...

Embodiment 3

[0036] The preparation method of 2-hydroxyalkyl quaternary ammonium base: use 72.11 parts of methyl propylene oxide, add dropwise to the mixed solution of 101.19 parts of triethylamine and 18 parts of water, and continuously stir at 40°C for 12h. After stopping the reaction, the yellow liquid in the lower layer was separated with a rotary evaporator to obtain the product 2-hydroxyalkyl quaternary ammonium base in the form of light yellow oil.

[0037] (1) Put 100g of HDI monomer into the reaction container under the protection of nitrogen, add the trimerization catalyst prepared by accounting for more than 0.5% of the mass of the isocyanate monomer dropwise within 1 hour, maintain the temperature at 80 ° C, keep stirring for 2 hours; measure the free NCO group When the mass percentage of the mass is 40%, add 0.5% acetyl chloride polymerization inhibitor accounting for the mass of the isocyanate monomer, and keep warm for 0.5h; stop the reaction, and after cooling down to room t...

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Abstract

The invention discloses a preparation method of a hexamethylene diisocyanate tripolymer curing agent, which comprises the following steps: putting an isocyanate monomer into a reaction vessel in a nitrogen gas protective atmosphere, dropwisely adding an isocyanate trimerization catalyst containing 2-hydroxyalkyl quaternary ammonium hydroxide within 1-1.5 hours, reacting while stirring at 30-80 DEG C for 2-24 hours, wherein the mass of the isocyanate trimerization catalyst accounts for 0.01-0.5% of that of the isocyanate monomer; when the mass percent of free NCO groups is measured to be 30-40%, adding an isocyanate trimerization inhibitor, wherein the mass of the isocyanate trimerization inhibitor accounts for 0.1-1% of that of the isocyanate monomer; and feeding the obtained polyurethane tripolymer curing agent into a separation device through a distributor at a feed rate of 1-20g / min, and separating to obtain the hexamethylene diisocyanate tripolymer curing agent. The curing agent disclosed by the invention is favorably compatible with resin, and has ultraviolet irradiation resistance, high compatibility, low viscosity and high mechanical strength.

Description

technical field [0001] The invention relates to a hexamethylene diisocyanate trimer curing agent, in particular to a preparation method of the hexamethylene diisocyanate trimer curing agent. Background technique [0002] Hexamethylene diisocyanate (HDI) trimer curing agent has excellent weather resistance, heat resistance and conforms to today's environmental protection requirements High solid content, low viscosity characteristics, has been developed and produced by several foreign companies recently, and some products have entered the Chinese market, such as Tolonate HDI90, Desmodur N3390 and so on. [0003] Qiu Shaojun and others catalyzed HDI with quaternary ammonium salt catalyst to prepare HDI trimer. When the mass fraction of the catalyst was 0.3%, a higher conversion rate was obtained; at the same time, it was found that the polymerization induction time was short when the catalyst was used. Scholl, Fujita, Kumada and Ueyanagi used quaternary ammonium salts as cata...

Claims

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Application Information

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IPC IPC(8): C08G18/79C07D251/30C09D175/04
Inventor 黄洪陈卓司徒粤杨东东张心亚
Owner SOUTH CHINA UNIV OF TECH
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