Phosphorus-nitrogen-boron synergistic efficient flame retardant flexible curing agent and synthesis method thereof

A synthesis method and high flame retardant technology are applied in the field of phosphorus-nitrogen-boron synergistic high flame-retardant flexible curing agent and its synthesis field, which can solve the problem that the synthesis reaction temperature and flame retardant efficiency of polyester with low acid value cannot be synthesized. To solve the problems of synergistic flame retardant, inability to synthesize high acid value curing agent, etc., to achieve the effect of optimization of curing agent index parameters, strong adjustability, and obvious synergistic flame retardant effect

Active Publication Date: 2019-03-15
法拉新材料连云港有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Regarding synergistic flame retardant and flexibility, a flexible flame retardant curing agent is described in the patent CN201310245491.1, but this curing agent is synthesized by using multifunctional flame retardant materials, resulting in the viscosity of the curing agent being too large and acidic. The value range is narrow and it is impossible to synthesize low acid value polyester (acid value≤80mgKOH / g) and the synthesis reaction temperature cannot be too high (no more than 220°C); on the other hand, the flexibility of this curing agent is also significantly worse than that of the present invention The curing agent in the present invention, and the flame retardant efficiency can not reach the synergistic flame retardant of phosphorus, nitrogen and boron in the present invention
In CN201310245173.5, a phosphorus-nitrogen synergistic flame-retardant curing agent is also described. The curing agent is also synthesized by using a multifunctional flame-retardant material, which also leads to a large melt viscosity and a narrow acid value range of the curing agent, and Higher phosphorus content makes this invention unable to synthesize high acid value curing agent (acid value ≥ 150mgKOH / g), and has no advantage in flexibility

Method used

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  • Phosphorus-nitrogen-boron synergistic efficient flame retardant flexible curing agent and synthesis method thereof
  • Phosphorus-nitrogen-boron synergistic efficient flame retardant flexible curing agent and synthesis method thereof
  • Phosphorus-nitrogen-boron synergistic efficient flame retardant flexible curing agent and synthesis method thereof

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Embodiment 1

[0032] A kind of synthetic method with phosphorus-nitrogen-boron synergistic highly flame-retardant flexible curing agent (A), the steps are as follows:

[0033] (1) After the four-neck flask, stirrer, distillation column, condenser tube and temperature-controlled heating mantle are finished, add 95g of neopentyl glycol, raise the temperature to 110-130°C, stir and melt, add 244.4g of diethyl-(N, N-bis(2-hydroxyethyl)-aminomethyl)-phosphine oxide, 56.5g bis(hydroxymethyl)cadecaborane, after stirring evenly, the temperature was raised to 140°C;

[0034] (2) Add 40g of adipic acid, 257.8g of isophthalic acid and 0.69g of ethyl triphenylphosphine bromide, under the protection of nitrogen, slowly raise the temperature to 140°C for esterification reaction and by-product water flows out, and control distillation The column temperature is not higher than 100°C;

[0035] (3) Then carry out a segmented esterification reaction, 140~170°C for 1.5~3h, 170~200°C for 2~3h, 200~230°C for 1~...

Embodiment 2

[0040] A kind of synthetic method with phosphorus-nitrogen-boron synergistic highly flame-retardant flexible curing agent (B), the steps are as follows:

[0041] (1) After the four-necked flask, stirrer, distillation column, condenser tube and temperature-controlled heating mantle are finished, add 85g of neopentyl glycol, raise the temperature to 110-130°C, stir and melt, add 246.01g of diethyl-(N, N-bis(2-hydroxyethyl)-aminomethyl)-phosphine oxide, 37.36g bis(hydroxymethyl)cadecaborane, after stirring evenly, the temperature was raised to 140°C;

[0042] (2) Add 55.21g of adipic acid, 188.3g of isophthalic acid and 0.61g of ethyl triphenylphosphine bromide, under the protection of nitrogen, slowly raise the temperature to 140°C for esterification reaction and by-product water flows out, control The temperature of the distillation column is not higher than 100°C;

[0043] (3) Then carry out a segmented esterification reaction, 140~170°C for 1.5~3h, 170~200°C for 2~3h, 200~23...

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Abstract

The invention relates to a phosphorus-nitrogen-boron synergistic efficient flame retardant flexible curing agent and a synthesis method thereof. The curing agent comprises the following components: 5to 16.7 parts of polyhydric alcohol, 18.7 to 42.5 parts of a phosphorus-nitrogen reactive flame retardant, 3.7 to 14.3 parts of a boron reactive flame retardant, 28 to 39 parts of polyatomic acid, 0.03 to 0.25 part of a catalyst, and 8 to 32 parts of an end-capping reagent; the acid value of the curing agent is 50 to 200 mgKOH/g; the melt viscosity is 800 to 7000 mPa.s/180 DEG C; the softening point is 60 to 125 DEG C; the P content is 2.7 to 6.4 wt%%; the N content is 1.2 to 2.9 wt%; the B content is 2 to 8 wt%. The existence of phosphorus, nitrogen and boron flame retardant elements and flexible chain ensures that the curing agent has excellent flame retardant efficiency, flame retardant durability and flexibility.

Description

technical field [0001] The invention belongs to the field of electronic packaging materials, in particular to a phosphorus-nitrogen-boron synergistic highly flame-retardant flexible 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, c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/698C08G59/40
CPCC08G59/4078C08G63/6986
Inventor 崔宇
Owner 法拉新材料连云港有限公司
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