Method for preparing C21dicarboxylic acid polyamide epoxy hardener from methyl eleostearate

A dibasic carboxylic acid polyamide, epoxy curing agent technology, applied in the field of preparation of C21 dibasic carboxylic acid polyamide epoxy curing agent, can solve the problem of low hardness of dimer acid polyamide resin epoxy cured product, preparation Problems such as large process energy consumption and poor heat resistance can achieve the effect of convenient distillation and purification, high strength and reduced energy consumption

Inactive Publication Date: 2008-10-08
INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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  • Summary
  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

[0005] In order to solve the existing C in the prior art 36 The hardness of the dimer acid polyamide resin epoxy cured product is not high and the heat resistance is poor, and the disadvantages of high energy consumption and low yield of the preparation process, the invention provides a method for preparing C 21 The preparation method of dibasic carboxylic acid polyamide epoxy curing agent,

Method used

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  • Method for preparing C21dicarboxylic acid polyamide epoxy hardener from methyl eleostearate
  • Method for preparing C21dicarboxylic acid polyamide epoxy hardener from methyl eleostearate
  • Method for preparing C21dicarboxylic acid polyamide epoxy hardener from methyl eleostearate

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Embodiment 1

[0028] A kind of preparation C 21 The preparation method of dibasic carboxylic acid polyamide epoxy curing agent comprises the following steps:

[0029] The first step: add 100 parts by mass of methyl chelate and 20.6 to 30.9 parts by mass of acrylic acid, and 0.5% to 1.5% of the mass of acrylic acid, and perform an addition reaction at 160 to 180 ° C for 2 to 3 hours, Vacuum distillation removes non-reactants, and decolorizing agent decolorizes to obtain C 21 Monomethyl dicarboxylate;

[0030] The second step: 1 mole of C obtained from the first step 21 Dibasic carboxylic acid monomethyl ester is added dropwise to 1.5-2 moles of polyamines at 140°C within 0.5 hours, and amidation reaction is carried out at 170-200°C. The reaction time is 5-6 hours, and vacuum distillation removes water and free Amine, get C 21 Dibasic carboxylic acid polyamide epoxy curing agent.

[0031] Wherein, acrylic acid can be 20.6~30.9 any mass parts, such as 20.6 mass parts, 26.3 mass parts or 3...

Embodiment 2

[0033] Add 100g of methyl lyceate and 24.7g of acrylic acid into a three-necked flask equipped with a magnetic stirrer, a thermometer and a reflux condenser, add hydroquinone accounting for 0.5% of the mass of acrylic acid as a polymerization inhibitor, and heat up to 180 ° C. Stir the reaction at rpm for 2 hours, distill under a vacuum of 2mmHg, remove fractions below 240°C, and decolorize with activated carbon to obtain C 21 106 g of monomethyl dicarboxylic acid.

Embodiment 3

[0035] Add 1% p-hydroxyanisole by mass of acrylic acid as a polymerization inhibitor, and the rest are the same as in Example 2.

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Abstract

The invention belongs to the preparation field of epoxy curing agents and discloses a method of preparing C21 dicarboxylates polyamide epoxy curing agent with methyl eleostearate as follows: the first step: 100 molar portions of methyl eleostearate, 20.6-30.9 molar portions of acrylic acid, and inhibitor accounting for 0.5% to 1.5% mass of the acrylic acid are processed with addition reaction at 160 to 180 DEG C for 2 to 3 hours; then the non-reactant is removed through vacuum distillation and the reactant is decolorized through depigmenting agent so as to obtain C21 dicarboxylic acid monomethyl ester. The second step: 1 mol of C21 dicarboxylic acid monomethyl ester obtained from the first step is added drop by drop into 1.5-2 mol of polyamine which is of 140 DEG C within 0.5 hour, then the mixture liquid is processed with amidation at 170 to 200 DEG C for 3 to 6 hours; later, water and free amine are removed through vacuum distillation, so the C21 dicarboxylates polyamide epoxy curing agent is obtained. The methyl eleostearate of the invention has an 85% yield, high reactivity and low energy consumption needed in the reactions; the prepared C21 dicarboxylates polyamide epoxy curing agent and the epoxy solid products have high strength and modulus and good heat-resistant performance.

Description

technical field [0001] The present invention relates to a kind of preparation method of epoxy resin curing agent, relate in particular to a kind of C 21 The preparation method of dibasic carboxylic acid polyamide epoxy curing agent. Background technique [0002] Epoxy resin has excellent technological properties, mechanical properties and physical properties. It is widely used in the fields of machinery, electricity, electronics, aviation, aerospace, chemical industry, transportation, construction, etc. . Epoxy resin has practical significance only when used together with curing agent, so the structure and quality of curing agent directly affect the performance and application of cured epoxy resin. The research and development of curing agents at home and abroad are far more active than the research and development of epoxy resin varieties. Every time a new curing agent is developed, it can solve a practical problem in one aspect, which is equivalent to developing a new cu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G69/26C08G59/44C08L63/00
Inventor 夏建陵黄坤李梅聂小安杨小华王定选
Owner INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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