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Method for preparing polyisocyanate

A technology of polyisocyanate and isocyanate, which is applied in the field of preparation of polyisocyanate curing agent products, can solve the problems of insoluble matter, unfavorable application of downstream customers in cold regions, and easy precipitation of products, so as to reduce the fluorine content and the accumulation of fluorine , the effect of controlling the harm of fluorine

Active Publication Date: 2019-04-19
WANHUA CHEM GRP CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above-mentioned published patents all involve the use of fluorine in the preparation process of polyisocyanate, and the resulting product is prone to precipitation and insoluble matter when stored at low temperature, such as at -20°C. Therefore, the above-mentioned products are not conducive to downstream customers in cold regions. application

Method used

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  • Method for preparing polyisocyanate
  • Method for preparing polyisocyanate
  • Method for preparing polyisocyanate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0073] a) 800g HDI (hexamethylene diisocyanate) is placed in the round-bottomed flask equipped with reflux condenser, stirrer, thermometer and nitrogen inlet, after heating to 70°C, add 70wt% tetrabutylphosphine difluoride 0.5g of n-hexanol solution, and carry out self-polymerization reaction under constant stirring, and control the reaction temperature between 70-75°C; when the conversion rate of monomer in the self-polymerization reaction reaches 30%, immediately add tetrabutyl difluoride Phosphine equimolar amount of C 2 f 5 CH 2 O(CH 2 CH 2 O) 3 H, continue stirring for 15min to terminate the reaction;

[0074] b) Cool the terminated reaction liquid to -20°C, and filter it through a two-stage polytetrafluoroethylene filter element, the pore size of the above-mentioned polytetrafluoroethylene filter element is 50um;

[0075] c) Evaporate and remove the unreacted raw materials contained in the reaction liquid by using a thin-film evaporator at a temperature of 150° C. ...

Embodiment 2

[0088] a) 1000g HDI (hexamethylene diisocyanate) is placed in the round-bottomed flask equipped with reflux condenser, stirrer, thermometer and nitrogen inlet, add 50wt% tetramethylammonium difluoride after heating to 60 ℃ 0.8g of n-hexanol solution, and carry out self-polymerization reaction under constant stirring, and control the reaction temperature between 60-65°C; when the conversion rate of monomer in the self-polymerization reaction reaches 40%, immediately add ammonium equimolar amount of C 6 f 13 CH 2 CH 2 O(CH 2 CH 2 O) 4 H, continue stirring for 15min to terminate the reaction;

[0089] b) cooling the terminated reaction liquid to 10°C, and passing through two-stage polytetrafluoroethylene packing for adsorption, the particle size of the above polytetrafluoroethylene packing is 1.0 mm;

[0090] c) Extract the adsorbed reaction liquid with cyclohexane, the extraction temperature is 40° C., the mass ratio of n-hexane to the reaction liquid is 2:1, extract cont...

Embodiment 3

[0097] a) 1000g of pentamethylene diisocyanate is placed in a round-bottomed flask equipped with a reflux condenser, a stirrer, a thermometer and a nitrogen inlet, heated to 60°C, and 1g of n-hexanol solution of 60wt% tetrabutylammonium fluoride is added , and carry out the self-polymerization reaction under constant stirring, and control the reaction temperature between 60-65 ° C; when the conversion rate of the monomer in the self-polymerization reaction reaches 40%, immediately add C 3 f 7 CH 2 O(CH 2 CH 2 O) 10 H, continue stirring for 15min to terminate the reaction;

[0098] b) Cool the terminated reaction solution to -30°C, and filter through two-stage polytetrafluoroethylene filter bags, the pore size of the above-mentioned polytetrafluoroethylene filter bags is 70um;

[0099] c) Evaporate and remove the unreacted raw materials contained in the reaction liquid using a thin-film evaporator at a temperature of 150° C. and an absolute pressure of 100 Pa, so that the ...

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Abstract

The invention discloses a method for preparing polyisocyanate. The method comprises the following steps: isocyanate is subjected to a self-polymerization reaction under the catalysis of a fluorine-containing catalyst, and a terminator is added after the completion of the reaction to terminate the reaction in order to obtain a reaction solution; and the unreacted isocyanate monomer is removed to obtain the polyisocyanate, wherein the fluorine content of the polyisocyanate is controlled to be 80 ppm or below. The method controls the fluorine content of the product, avoids the turbidity phenomenon of the product during low-temperature storage, and effectively reduces the toxicity of fluorine in the system, device hazards and downstream harms.

Description

technical field [0001] The invention relates to a preparation method of a polyisocyanate curing agent product. Background technique [0002] The polyisocyanate prepared by polymerization of aliphatic diisocyanate monomer has been widely used in the polyurethane coating or adhesive industry. Through the polymerization of isocyanate itself, it can effectively reduce the harm of volatile isocyanate monomer to the human body. [0003] Isocyanate monomers can be polymerized to obtain uretdione (structural formula 1), trimer (structural formula 2), and iminooxadiazinedione (structural formula 3). The three structures have their own characteristics and affect the performance of the product. The viscosity of uretdione is the smallest, the functionality is small, the functionality of the trimer is large, the viscosity is large, and the viscosity of iminooxadiazinedione is smaller than that of the trimer, and the functionality is greater than that of uretdione. conducive to curing. ...

Claims

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Application Information

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IPC IPC(8): C07D251/34C07D273/04C08G18/02
CPCC07D251/34C07D273/04C08G18/02C08G18/022
Inventor 刘伟石滨尚永华王明永朱智诚辛光震薛勇勇陈杰孙晔黎源
Owner WANHUA CHEM GRP CO LTD
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