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Polyaspartate, and preparation method and application thereof

A technology of aspartic acid ester and maleic acid diol ester, which is applied in the field of polymer synthesis, can solve the problems of high esterification temperature, poor coating performance, short construction operation time, etc., and achieve high esterification conversion rate , Conducive to construction penetration, improve the effect of mechanical properties

Pending Publication Date: 2021-10-26
浙江艾特普科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Yet adopt the method in the prior art, there is following problem when preparing the reaction raw material dialkyl maleate of polyaspartate: 1, when maleic anhydride reacts with alcohol, the esterification temperature is high, easily produces trans The structure is not conducive to the subsequent reaction with primary amines, resulting in insufficient conversion of primary amines, so when used in coatings, the early viscosity increases rapidly, and the construction operation time is short; and the product is easily oxidized at high temperature, which affects product quality; 2. Maleic anhydride Esterification with alcohol is difficult, accompanied by reverse reaction, the synthesized dialkyl maleate has a high acid value, and when the polyaspartic acid ester made from it is used in coatings, it is easy to react with isocyanate curing agent to generate carbon dioxide. The coating is easy to generate bubbles, and the coating performance is not good; 3. When maleic anhydride and alcohol are esterified, the solvent needs to be removed with water, which is not environmentally friendly; 4. The polyaspartic acid synthesized by the method in the prior art Most of the ester resins are two-functional resins, and the ratio range of the curing agent and the curing agent is narrow. The mechanical properties of the cured coating are not good, which is not conducive to the use of coatings.

Method used

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  • Polyaspartate, and preparation method and application thereof
  • Polyaspartate, and preparation method and application thereof
  • Polyaspartate, and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] A kind of polyaspartic acid ester, structural formula is:

[0041]

[0042] Among them, R 1 , R 2 , R 3 and R 4 is methyl; R 5 for polyether groups.

[0043] Its preparation method comprises the following steps:

[0044] (1) Add maleic anhydride, polymerization inhibitor p-hydroxyanisole (MEHQ), catalyst triphenylphosphine into the flask, drop propylene oxide, the mol ratio of maleic anhydride and propylene oxide is 1:2.1, The addition amount of MEHQ is 0.02% of the total mass of the reactants, and the addition amount of triphenylphosphine is 0.02% of the total mass of the reactants; the addition rate of propylene oxide is controlled so that the reaction temperature does not exceed 60 ° C, and the addition is completed at 70 ° C Insulate for 2 hours, measure the acid value every 0.5 hours, and wait until the acid value reaches 2mgKOH / g to discharge to obtain diol maleate;

[0045] (2) Add polyetheramine D400 to the flask, and add sodium methoxide, the amount o...

Embodiment 2

[0047] A kind of polyaspartic acid ester, structural formula is:

[0048]

[0049] Among them, R 1 and R 2 for hydrogen, R 3 and R 4 is methyl; R 5 For n-hexyl.

[0050] Its preparation method comprises the following steps:

[0051] (1) Add maleic anhydride, polymerization inhibitor p-hydroxyanisole (MEHQ), and catalyst triphenylphosphine into the flask, add dropwise a mixture of ethylene oxide and propylene oxide, maleic anhydride, ethylene oxide The mol ratio with propylene oxide is 1:1:1, and the addition amount of MEHQ is 0.02% of reactant gross mass, and the addition amount of triphenylphosphine is 0.01% of reactant gross mass; The drop rate of oxypropane is such that the reaction temperature does not exceed 60°C. After the dropwise addition, keep the temperature at 60°C for 6h, and measure the acid value every 0.5h. When the acid value reaches 2mgKOH / g, the material is discharged to obtain diol maleate;

[0052] (2) Add 1,6-hexamethylenediamine into the flask, ...

Embodiment 3

[0054] A kind of polyaspartic acid ester, structural formula is:

[0055]

[0056] Among them, R 1 , R, R 3 and R 4 Respectively hydrogen, methyl, ethyl and cyclopentyl; R 5 For cycloalkyl.

[0057] Its preparation method comprises the following steps:

[0058] (1) Add maleic anhydride, polymerization inhibitor p-hydroxyanisole (MEHQ), and catalyst triphenylphosphine into the flask, and drop propylene oxide and ethylene oxide with a molar ratio of 1:1:1:1 , a mixture of butylene oxide and 1,2-epoxycyclopentane, the molar ratio of maleic anhydride and epoxy groups in the mixture is 1:2.4, the amount of MEHQ added is 0.02% of the total mass of reactants, triphenyl The addition amount of base phosphine is 0.1% of the total mass of reactants; control the dropping speed of the epoxy mixture so that the reaction temperature does not exceed 60°C, keep the temperature at 70°C for 2h after dropping, measure the acid value every 0.5h, and wait until the acid value reaches 2mgKO...

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Abstract

The invention discloses a polyaspartate, and a preparation method and application thereof. The preparation method comprises the following steps: (1) reacting maleic anhydride with an epoxy monomer to obtain maleic acid glycol ester; and (2) reacting the maleic acid glycol ester obtained in the step (1) with primary amine to obtain the polyaspartate. After the polyaspartate and an isocyanate curing agent are mixed to obtain a polyaspartate polyurea coating. Maleic anhydride is modified with the epoxy monomer to synthesize maleic acid glycol ester, and then maleic acid glycol ester reacts with the primary amine, so that polyfunctional polyaspartate can be prepared, and the mechanical property of the coating is improved; and the synthesized maleic acid glycol ester has no trans structure, the acid value of the product is low, the viscosity of the prepared coating is slowly increased, and the construction permeation is facilitated.

Description

technical field [0001] The invention relates to the field of polymer synthesis, in particular to a polyaspartic acid ester and its preparation method and application. Background technique [0002] Polyaspartic acid ester resin is a special kind of steric hindered secondary amine compound. Its steric hindrance and inductive effect work together to reduce the activity of secondary amine when it reacts with -NCO. Compared with traditional polyurea materials, It has longer construction time and higher paint film adhesion. Polyaspartic ester resin is combined with aliphatic isocyanate curing agent, and the prepared polyaspartic ester polyurea coating has excellent mechanical properties and aging resistance, which is more excellent than general hydroxyl resin and epoxy resin. drying speed. [0003] Polyaspartic acid esters in the prior art are generally obtained through the reaction of dialkyl maleate and fatty primary amines, and dialkyl maleate is prepared by esterification of...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C229/24C07C227/06C08G65/332C09D175/02
CPCC07C229/24C08G65/3322C09D175/02C08G2150/00
Inventor 朱银邦赵军子卢鹏飞徐轶
Owner 浙江艾特普科技有限公司
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