Method of preparing polyaspartic ester

A technology of aspartic acid ester and dibasic acid ester, which is applied in the preparation of cyanide reaction, chemical instruments and methods, and the preparation of organic compounds. It can solve the problem of slow reaction speed, high reaction temperature, and inability to directly improve the conversion of primary amine rate and other issues

Active Publication Date: 2020-04-10
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chinese published patent CN109320681 reports that the conversion rate of primary amines is improved by introducing acrylate in the late stage of the reaction, and the primary amines can be quickly eliminated through the introduction of highly active electrophilic groups; Chinese published patent CN102250343A reports the use of supported alkali metal fluorine Compound catalyzed method for synthesizing polyaspartate, the reaction rate has been improved, but in the later stage of the reaction, glycidyl tertiary carbonic acid ester needs to be added

Method used

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  • Method of preparing polyaspartic ester
  • Method of preparing polyaspartic ester
  • Method of preparing polyaspartic ester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038]

[0039] (1) By mass parts, 40 parts of indium trifluoromethanesulfonate and 15 parts of indium chloride, 10 parts of copper trifluoromethanesulfonate, 5 parts of aluminum trifluoromethanesulfonate and 30 parts of aluminum oxide Disperse together in 120 parts of ethanol, stir at 55°C for 3h, distill off the solvent at 1kPa and 40°C under reduced pressure, dry the product in vacuum at 30°C for 5h, and roast it in a nitrogen atmosphere at 450°C for 3h to obtain the supported Lewis acid catalyst.

[0040] (2) Add 344.60g (2.0mol) of isophorone diamine into the 2 In the reaction kettle of the gas line pipe and the bubbler, the system was continuously purged with nitrogen and the bubbler was observed to bubble, and the stirring was started and the temperature of the reactor was controlled at 35°C, and 723.16g (4.2mol) of maleic acid di Ethyl ester was slowly and uniformly added to the reactor within 2 hours. After the addition was complete, 2.76 g of supported Lewis acid c...

Embodiment 2

[0044]

[0045] (1) By mass parts, 45 parts of indium trifluoromethanesulfonate and 13 parts of indium chloride, 8 parts of copper trifluoromethanesulfonate, 5 parts of aluminum trifluoromethanesulfonate and 29 parts of aluminum oxide Disperse together in 150 parts of ethanol, stir at 60°C for 3.5h, distill and remove the solvent under reduced pressure at 1kPa at 40°C, dry the product in vacuum at 40°C for 3h, then roast at 500°C for 3h in a nitrogen atmosphere to obtain a supported type Lewis acid catalyst.

[0046] (2) Add 420.72g (2.0mol) 4,4'-diaminodicyclohexylmethane into the 2 In the reaction kettle of the gas line pipe and the bubbler, the system was continuously purged with nitrogen and the bubbler was observed to bubble, and the stirring was started and the temperature of the reactor was controlled at 40°C, and 723.16g (4.2mol) of maleic acid di Ethyl ester was slowly and uniformly added to the reactor within 2 hours. After the addition was completed, 5.05 g of s...

Embodiment 3

[0050]

[0051] (1) By mass parts, 60 parts of indium trifluoromethanesulfonate and 5 parts of indium chloride, 8 parts of copper trifluoromethanesulfonate, 7 parts of aluminum trifluoromethanesulfonate and 20 parts of aluminum oxide Disperse together in 200 parts of ethanol, stir at 60°C for 4h, distill off the solvent at 1kPa, 40°C under reduced pressure, dry the product in vacuum at 50°C for 5h, and roast it in a nitrogen atmosphere at 550°C for 4h to obtain the supported Lewis acid catalyst.

[0052] (2) Add 476.82g (2.0mol) 3,3'-dimethyl-4,4'-diaminodicyclohexylmethane into the 2 In the reaction kettle of the gas line pipe and the bubbler, the system was continuously purged with nitrogen and the bubbler was observed to bubble, and the stirring was started and the temperature of the reactor was controlled at 50°C, and 723.16g (4.2mol) of maleic acid di Ethyl ester was slowly and uniformly added to the reactor within 2 hours. After the addition was completed, 23.84 g of...

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Abstract

The invention discloses a method of preparing polyaspartic ester. The preparation method comprises the following steps: (1) organic primary amine and unsaturated dibasic acid ester are subjected to Michael addition reaction under the catalysis of a supported Lewis acid catalyst, and (2) a catalyst and excessive unsaturated dibasic acid ester are removed from the reaction solution obtained in the step (1) to obtain polyaspartic ester, wherein the supported Lewis acid catalyst comprises 40-60 wt% of indium trifluoromethanesulfonate, 10-30 wt% of one or more of indium chloride, copper trifluoromethanesulfonate, aluminum trifluoromethanesulfonate and zinc trifluoromethanesulfonate, and the balance of a carrier, and the content is based on the total weight of the catalyst. Raw materials of thecatalyst are common and easy to obtain, the preparation method is simple and convenient, and the method has the advantages of good catalytic activity, high primary amine conversion rate, simplicity and convenience in operation, high product quality and the like when used for preparing polyaspartic ester.

Description

technical field [0001] The invention belongs to the field of organic chemical synthesis, and in particular relates to a method for preparing polyaspartate. Background technique [0002] Polyaspartic Acid Ester (PAE) is synthesized by Michael addition reaction of diamine and maleic acid ester, and compounded with low viscosity isocyanate curing agent to obtain polyaspartic acid ester polyurea , known as the third-generation polyurea, due to the steric hindrance and inductive effect of the ester group in polyaspartate, and through structural design, its gel time can be adjusted from minutes to hours. As a new type of high-performance material, PAE polyurea has the advantages of high solid content, ultra-fast drying, and no need for catalysts compared with traditional polyurethane materials. It is widely used in related fields with high quality requirements for anti-corrosion, waterproof, wear-resistant and weather resistance. . [0003] It is well known in the art that the r...

Claims

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Application Information

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IPC IPC(8): C07C227/08C07C229/24C08G18/32B01J31/26B01J31/04
CPCC07C227/08C08G18/3234B01J31/0227B01J31/26C07C2601/14B01J2231/32C07C229/24
Inventor 王加琦张鹏飞习林潘亚男王文黄存贺袁帅黄少峰崔乾刘超何金同
Owner WANHUA CHEM GRP CO LTD
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