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Amido containing polyaspartate and preparation method thereof

A technology of amido-containing polyaspartic acid ester and aspartic acid ester, which is applied in the field of amido-containing polyaspartic acid ester and its preparation, can solve the problem of long synthesis time, low conversion rate, and inability to supply timely goods and other issues, to achieve the effect of improving the construction period and its application fields, broad prospects for industrialization, and expanding the scope of application

Inactive Publication Date: 2019-06-07
江西高信前沿科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It effectively solves the problems of low short-term conversion rate, long synthesis time, untimely supply, difficulty in industrial production or low performance of cured products in the existing technology.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Add 105 g (0.5 mol) of 4,4'-diaminocyclohexylmethane into a four-necked flask equipped with a stirrer, a heating device, an addition funnel, and a nitrogen inlet, protect it with nitrogen, raise the temperature to 80°C, and dissolve 172 g (1.0 mol) diethyl maleate was dropped into the four-neck flask through the addition funnel at a constant speed within 3 hours. After the addition was complete, the reaction was incubated for 24 hours. At this point 97% of the 4,4'-diaminocyclohexylmethane was converted to polyaspartate. Add 7.3 grams (0.05 mol) of adipic acid to the four-necked flask at one time, raise the temperature to 180°C and keep it for 1 hour, and when it is cooled to 110°C, vacuumize and dehydrate it under the condition of negative pressure of 0.05MPa for 1 hour, and obtain transparent, shallow Yellow liquid, the reaction is 100% complete.

Embodiment 2

[0031]Add 119 g (0.5 mol) of 3,3'-dimethyl-4,4'-diaminocyclohexylmethane into a four-necked flask equipped with a stirrer, a heating device, an addition funnel, and a nitrogen inlet, and pass nitrogen protection , the temperature was raised to 100°C, and 228.28 g (1.0 mol) of dibutyl maleate was dropped into the four-neck flask through the addition funnel at a constant speed within 3 hours. After the addition was complete, the reaction was incubated for 24 hours. At this point 86% of the 3,3'-dimethyl-4,4'-diaminocyclohexylmethane was converted to polyaspartate. Add 11.81 g (0.1 mol) of succinic acid to the four-neck flask at one time, raise the temperature to 180°C and keep it for 1 hour, and when it is cooled to 110°C, vacuumize and dehydrate it under the condition of negative pressure of 0.05MPa for 1 hour to obtain transparent, shallow Yellow liquid, the reaction is 100% complete.

Embodiment 3

[0033] Add 115 g (0.5 mol) of polyetheramine D-230 into a four-neck flask equipped with a stirrer, a heating device, an addition funnel and a nitrogen inlet, protect it with nitrogen, raise the temperature to 90 ° C, and dissolve 172 g (1.0 mol) Diethyl fumarate was dropped into the four-neck flask through the addition funnel at a constant speed within 3 hours. After the addition was complete, the reaction was incubated for 24 hours. At this point 88% of the polyetheramine D-230 was converted to polyaspartate. Add 23.12 (0.15mol) grams of hexahydrophthalic anhydride to the four-necked flask at one time, raise the temperature to 180°C and keep it for 1 hour. Yellow liquid, the reaction is 100% complete.

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PUM

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Abstract

The invention discloses amido containing polyaspartate and a preparation method thereof. The preparation method is characterized by comprising following steps: (1) carrying out Michael addition reactions between unsaturated dicarboxylate and primary amine at a temperature of 30 to 130 DEG C to generate aspartate oligomer; (2) carrying out amidation reactions between the product generated in the step (1) and dicarboxylic acid at a temperature of 120 to 220 DEG C to generate amido containing polyaspartic acid; and (3) removing micromolecular water from the product generated in the step (2) at atemperature of 100 to 120 DEG C under a negative pressure of 0.04 to 0.06 MPa to obtain the final product namely amido containing polyaspartate. The prepared amido containing polyaspartate and isocyanate are used to prepare polyurea, which has the characteristics of long gelation time and convenience for construction.

Description

technical field [0001] The invention relates to an amide group-containing polyaspartic acid ester and a preparation method thereof. The produced amide group-containing polyaspartic acid ester is mixed with an isocyanate prepolymer or an isocyanate curing agent to prepare polyurea. Background technique [0002] Polyaspartate polyurea is a new type of aliphatic polyurea with low activity, slow response and high performance. It effectively solves the shortcomings of traditional polyurea, such as excessive reaction speed, poor adhesion, complex coating molding, performance degradation, special equipment required for construction, and difficult operation. It is called the third-generation polyurea. Polyaspartic ester polyurea is very different from traditional polyurea and two-component polyurethane coatings in terms of construction and coating performance. For example, the reaction speed can be adjusted, and the gel time can range from a few minutes to several hours. It can be ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/00C08G18/64
Inventor 闫福安张彪葛建中袁维金
Owner 江西高信前沿科技有限公司