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Polyaspartic acid ester composition as well as preparation method and application thereof

A polyaspartate, aspartate technology, applied in the direction of polyurea/polyurethane adhesives, polyurea/polyurethane coatings, adhesive types, etc., can solve the unclear effect of PAE performance, PAE The overall performance of the composition is reduced, and the content of by-products is increased.

Active Publication Date: 2021-06-01
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In order to improve the conversion rate of primary amines, existing technical solutions often use high temperature, catalysts or long-term reaction / storage, etc. However, under these working conditions, not only will it bring undesired catalyst residues, or lead to by-products The increase of the content will lead to the decline of the comprehensive performance of the PAE composition, and the influence of these trace components on the performance of the PAE is not clear

Method used

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  • Polyaspartic acid ester composition as well as preparation method and application thereof
  • Polyaspartic acid ester composition as well as preparation method and application thereof
  • Polyaspartic acid ester composition as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0096] Step1: Add 1162g (10mol) of 2-methylpentamethylenediamine into a 20L glass reactor. The reactor is equipped with a mechanical stirring paddle, a thermometer, a constant pressure dropping funnel, and a N 2 Gas line pipe, bubbler, 3444g (20mol) diethyl butenedioate recycle liquid obtained by the separation of previous batches is added to the constant pressure dropping funnel, and N is introduced into the system. 2 After 10 minutes, the air in the system was replaced; under the condition of stirring at 30°C, diethyl butenedioate was slowly dropped into the flask for 0.5h at a constant speed, and the reaction temperature was controlled at 30°C for 2 hours. Then, 3444 g (20 mol) of diethyl maleate was added to the constant pressure dropping funnel, the temperature of the reaction system was lowered to 25° C., the supplementary liquid was added dropwise at a constant speed for 0.5 h, and the reaction was continued at 25° C. for 5 h. Stop the reaction, then add 23g (0.5%) ant...

Embodiment 2

[0103] Step1: Add 1051.8g (5mol) 4,4'-diaminodicyclohexylmethane into a 20L glass reactor. The reactor is equipped with a mechanical stirring paddle, a thermometer, a constant pressure dropping funnel, and a N 2 Gas line pipe, bubbler, 4304g (25mol) diethyl butenedioate obtained by the separation of the previous batch was added to the constant pressure dropping funnel, and N was passed into the system. 2 After 10 minutes, replace the air in the system; slowly drop diethyl maleate into the flask under the condition of stirring at 45°C, drop it at a constant speed for 1 hour, and control the reaction temperature to 45°C for 3 hours. Then, 1722 g (10 mol) of diethyl maleate was added to the constant pressure dropping funnel, the temperature of the reaction system was lowered to 30° C., the supplementary solution was added dropwise at a constant speed for 1 hour, and the reaction was continued at 30° C. for 6 hours. Stop the reaction, then add 2.77g (0.1%) antioxidant RIANOX MD-1...

Embodiment 3

[0110] Step1: Add 1192g (5mol) 3,3'-dimethyl-4,4'-diaminodicyclohexylmethane into a 20L glass reactor, which is equipped with a mechanical stirring paddle, a thermometer, a constant pressure dropping funnel, Connected with N 2 Gas line pipe, bubbler, 5165g (30mol) diethyl butenedioate separated from the previous batch was added to the constant pressure dropping funnel, and N was introduced into the system. 2 After 10 minutes, replace the air in the system; slowly drop diethyl maleate into the flask under the condition of stirring at 50°C, drop it at a constant speed for 1 hour, and control the reaction temperature to 50°C for 4 hours. Then, 1722 g (10 mol) of diethyl maleate was added to the constant pressure dropping funnel, the temperature of the reaction system was lowered to 30° C., the supplementary liquid was added dropwise at a constant speed for 1 hour, and the reaction was continued at 30° C. for 8 hours. Stop the reaction, then add 2.91g (0.1%) antioxidant RIANOX M...

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Abstract

The invention provides a high-quality polyaspartic acid ester composition and a preparation method thereof. According to the method, by controlling the process, the ratio of the secondary amine value to the total amine value of the polyaspartic acid ester composition is 95%-99.9%, so that the gelation time of polyurea compounded by the polyaspartic acid ester composition is prolonged, the viscosity is moderate, and the adhesive force, impact resistance and weather resistance of a coated film are excellent.

Description

technical field [0001] The invention belongs to the field of polyaspartic acid esters, and in particular relates to a polyaspartic acid ester composition and its preparation method and application. Background technique [0002] Polyaspartic Ester (Polyaspartic Ester, PAE) is a special kind of sterically hindered secondary amine. Due to the steric hindrance and inductive effect of the ester group, the activity of the secondary amine when it reacts with NCO is reduced, and it is cured with low-viscosity isocyanate. The gel time of the agent can be adjusted from minutes to hours. Therefore, the disadvantages of short construction time, poor coating adhesion and many surface defects of traditional polyurea materials are overcome. [0003] PAE is synthesized by the Michael addition reaction of organic primary diamines and butenedioic acid diesters, as shown below: [0004] [0005] Literature (Advanced Materials Research. Vol 875-877, 2014, pp 165-170.) reported that the ord...

Claims

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Application Information

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IPC IPC(8): C09D175/02C09D7/61C09D175/04C09J175/02C09J175/04
CPCC09D175/02C09D7/61C09D175/04C09J175/02C09J175/04C08K2003/2241C08K2003/3045C08K3/22C08K3/30C08K3/34
Inventor 郑超李同和李晶李文滨宋国毅石滨尚永华黎源
Owner WANHUA CHEM GRP CO LTD
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