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N-B synergistic high-flame-resistance type curing agent and synthesis method thereof

A synthesis method and curing agent technology are applied in the field of N-B synergistic high flame retardant curing agent and its synthesis field to achieve the effects of excellent flame retardancy, easy compatibility and excellent processability

Active Publication Date: 2018-08-21
吴天航
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Boron-based flame retardants are also divided into two categories: additive type and reactive type. Zinc borate is a representative of additive type flame retardants and is widely used, but it also has the defects of additive type flame retardants.

Method used

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  • N-B synergistic high-flame-resistance type curing agent and synthesis method thereof
  • N-B synergistic high-flame-resistance type curing agent and synthesis method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] A kind of synthetic method of N-B synergistic high flame retardant curing agent (A), the steps are as follows:

[0035] (1) After finishing the four-neck flask, stirrer, distillation column, condenser tube and temperature-controlled heating mantle, add 120g of neopentyl glycol and 168.21g of 1,3-dimethylol-5,5-dimethylhydantoin, and raise the temperature To 110~130℃, stirring and melting;

[0036] (2) Add 85.48g of 3-carboxyphenylboronic acid and 0.37g of ethyltriphenylphosphine bromide; slowly raise the temperature to 150°C under nitrogen, and distill out by-product water. During the reaction, control the temperature of the distillation column to not exceed 100°C, and then carry out segmented esterification reaction, 150~160°C for 1~3h, 160~170°C for 1~2h;

[0037](3) Cool down to 150°C, add 248.83g of isophthalic acid, 84.18g of adipic acid and 0.33g of ethyltriphenylphosphine bromide, slowly raise the temperature to 150°C under nitrogen, and carry out a segmented es...

Embodiment 2

[0042] A kind of synthetic method of multi-branched N-P synergistic flame retardant flexible curing agent (B), the steps are as follows:

[0043] (1) After finishing the four-neck flask, stirrer, distillation column, condenser tube and temperature-controlled heating mantle, add 105g of neopentyl glycol and 184.33g of 1,3-dimethylol-5,5-dimethylhydantoin, and raise the temperature To 110~130℃, stirring and melting;

[0044] (2) Add 76.32g of 3-carboxyphenylboronic acid and 0.36g of ethyltriphenylphosphine bromide; slowly raise the temperature to 150°C under nitrogen, and distill out by-product water. During the reaction, control the temperature of the distillation column to not exceed 100°C, and then carry out segmented esterification reaction, 150~160°C for 1~3h, 160~170°C for 1~2h;

[0045] (3) Cool down to 150°C, add 239.26g of isophthalic acid, 105.23g of adipic acid and 0.34g of ethyltriphenylphosphine bromide, slowly raise the temperature to 150°C under nitrogen, and car...

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Abstract

The invention relates to an N-B synergistic high-flame-resistance type curing agent and a synthesis method thereof. The N-B synergistic high-flame-resistance type curing agent is prepared from polyol,a reaction type nitrogen-containing compound, a reaction type boron-containing compound, polybasic acid, a catalyst and an end-capping agent by a sectional type synthesis method and by adjusting theproportion of the components, the reaction temperature and the reaction time. In the curing agent, the acid value range is 80 to 180 mgKOH / g, the melt viscosity range is 800 to 6000 mPa*s / 180 DEG C, the softening point range is 75 to 125 DEG C, the N content range is 1.9 to 4.8 percent by weight and the B content range is 0.35 to 1.05 percent by weight. The curing agent has a nitrogen (N) and boron (B) flame-resistant element non-migratory and multi-branched structure, so that the curing agent has excellent flame resistance and flame-resistant durability, is easy to crystallize, low in viscosity and easily compatible, is applied to an electronic packaging material and can realize zero halogen, zero phosphorus, flame resistance and excellent flame-resistant durability of the electronic packaging material.

Description

technical field [0001] The invention belongs to the field of electronic packaging materials, in particular to an N-B synergistic highly flame-retardant curing agent and a synthesis method thereof. Background technique [0002] Epoxy resin refers to a polymer containing two or more epoxy groups, with aliphatic, alicyclic or aromatic organic compounds as the backbone and formed by the reaction of epoxy groups; epoxy groups can be located in the molecular chain The end, middle or ring structure of the segment; it is one of the most widely used matrix resins in polymer matrix composites. Due to the special molecular structure of epoxy resin, epoxy resin has excellent adhesion, heat resistance, chemical resistance and excellent electrical insulation properties, and is easy to process, low shrinkage, small linear expansion coefficient and low cost. Advantages such as low cost. Widely used in the packaging of electronic components such as varistors, ceramic capacitors, diodes, an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/698C08G63/78C08G59/42C08L63/00
CPCC08G59/4276C08G63/6986C08G63/78C08L63/00C08L2203/206
Inventor 吴天航
Owner 吴天航
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