High transparent anti-yellowing curing accelerator for epoxy resin and preparation method thereof

A technology of changing epoxy resin and curing accelerator, which is applied in the field of epoxy resin curing accelerator and its preparation, can solve the problem of not making the yellowing resistance of the cured product, not making the optical performance of the cured product, and limiting the practical application of the accelerator, etc. problem, to achieve the effect of excellent yellowing resistance, excellent yellowing resistance and high transparency

Active Publication Date: 2018-12-11
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Tertiary amines are not only mostly yellow compounds, but when used in transparent epoxy resin, the transparency of the obtained material is not good, and it is easy to cause yellowing of the cured product during high temperature curing and long-term use. Lin Yijun et al. The effect of curing accelerators on the properties of cured epoxy resins was studied, and Tian Xinghe et al. discussed the colorless and transparent properties of cured epoxy resins
However, under the action of moisture, halides have a corrosive effect on metals, and various harmful halides will be produced in long-term high-temperature environments
[0004] In recent years, environmentally friendly halogen-free special salt accelerators have also been widely studied, but the synthesis and production process of these special compounds is complicated, and the use of toxic raw materials and solutions mainly limits the practical application of these accelerators For related introductions, please refer to the synthesis and application of latent epoxy resin curing accelerator M—Cd by Zhang Yang et al. and the preparation and performance of triphenylphosphine latent accelerator by Xiao Yan et al.
[0005] There is an epoxy resin curing accelerator and preparation method thereof (publication number: CN106397740A) discloses a kind of epoxy resin curing accelerator prepared by the reaction of quaternary ammonium hydroxide and C2-C4 organic acid, this curing accelerator is not Contains halogen, and it has strong curing performance after being mixed with epoxy resin. It is equivalent to TEAB in terms of curing performance such as curing time, light transmittance and haze, but this patent does not do research on the yellowing resistance of the cured product
[0006] Another article on epoxy resin curing accelerator (publication number: CN107075088A) discloses a kind of epoxy resin curing accelerator composed of a quaternary phosphonium salt with a certain general formula, aimed at epoxy resin sealing materials used for electronic components such as semiconductors, The curing accelerator has excellent fluidity, high catalytic activity and excellent curability when the mold is filled, but this patent does not do research on the optical properties of the cured product

Method used

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  • High transparent anti-yellowing curing accelerator for epoxy resin and preparation method thereof
  • High transparent anti-yellowing curing accelerator for epoxy resin and preparation method thereof
  • High transparent anti-yellowing curing accelerator for epoxy resin and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0025] A kind of epoxy resin curing accelerator, its chemical formula is:

[0026]

[0027] A kind of preparation method of epoxy resin curing accelerator is:

[0028] Weigh 1 mol of tetramethylammonium hydroxide and dissolve it in water to form a tetramethylammonium hydroxide solution, put it in a beaker, add diethylene glycol and mix well, then slowly add 1.0mol of 2-ethylhexanoic acid into tetramethylammonium hydroxide In the mixture of aqueous solution of methyl ammonium hydroxide and diethylene glycol, while controlling the temperature at 20-60°C, aqueous solution of tetramethylammonium hydroxide, diethylene glycol and 2-ethylhexyl acid mixture. Add the aqueous solution of tetramethylammonium hydroxide, the mixed solution of diethylene glycol and 2-ethylhexanoic acid into the reaction kettle, replace the oxygen in the reaction kettle with inert gas, and then vacuumize and heat to reduce Pressure distillation to remove water while controlling the temperature at 90-100...

Embodiment 2

[0037] Weigh 1 mol of tetraethylammonium hydroxide and dissolve it in water to form tetraethylammonium hydroxide solution, put it in a beaker, add octanol to mix well, then slowly add 1.2mol of 2-methylheptanoic acid into tetraethylammonium hydroxide In the mixed solution of ammonium oxide aqueous solution and octanol, while controlling the temperature at 20-60°C, a mixed solution of tetraethylammonium hydroxide aqueous solution, octanol and 2-methylheptanoic acid is obtained. Add the mixed solution of tetraethylammonium hydroxide aqueous solution, octanol and 2-methylheptanoic acid in the reactor, replace the oxygen in the reactor with inert gas, then vacuumize, heat, and carry out decompression distillation to remove water. At the same time, the temperature is controlled at 90-100°C for 12 hours, and the residue in the reaction kettle after distillation is the epoxy resin curing accelerator.

[0038] Mix e51 epoxy resin, 4-methylhexahydrophthalic anhydride, and curing accele...

Embodiment 3

[0040] Weigh 1 mol of tetrapropylammonium hydroxide and dissolve it in water to form tetrapropylammonium hydroxide solution, place it in a beaker, add propanol and mix evenly, then slowly add 1.3mol of heptanoic acid into tetrapropylammonium hydroxide aqueous solution and In the mixed solution of propanol, while controlling the temperature at 20-60°C, a mixed solution of quaternary ammonium hydroxide aqueous solution, propanol and heptanoic acid is obtained. Add the mixed solution of tetrapropylammonium hydroxide aqueous solution, propanol and heptanoic acid in the reactor, replace the oxygen in the reactor with inert gas, then vacuumize, heat, and carry out decompression distillation to remove water, and control the temperature at the same time. 90-100°C for 12 hours, the residue in the reactor after distillation is the curing accelerator for epoxy resin.

[0041]Mix e51 epoxy resin, 4-methylhexahydrophthalic anhydride, and curing accelerator at a mass ratio of 100:90:1.4, fi...

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Abstract

The invention relates to a high transparent anti-yellowing curing accelerator for epoxy resin and preparation method thereof, and belongs to the technical field of curing accelerators for epoxy resin. The curing accelerator for the epoxy resin is prepared by mixing quaternary ammonium hydroxide, organic acid with carbon atom number of 5 to 10 and alcohol and performing reduced pressure distillation. The high transparent anti-yellowing curing accelerator for the epoxy resin provided by the invention, the initial transparency of a cured sample is high, the yellowing resistance is excellent. Thecommon curing accelerator, tertiary amine, is not only mostly yellow compound, when the common curing accelerator is used in transparent epoxy resin, the transparency of the obtained materials is notgood, moreover, the yellowing of a cured material in high temperature curing and long-term use is easy to cause. Epoxy resin cured material prepared by the curing accelerator provided by the invention is high in transparency, the color changes slowly when being exposed to high temperature for a long time, and has excellent yellowing resistance.

Description

technical field [0001] The invention relates to an epoxy resin curing accelerator and a preparation method thereof, in particular to a non-halogen, highly transparent, yellowing-resistant special epoxy resin curing accelerator and a preparation method thereof, belonging to the technology of epoxy resin curing accelerators field. Background technique [0002] Epoxy resin is a kind of thermosetting resin with excellent comprehensive performance. It is widely used in various fields such as electronic potting compound, adhesive and advanced composite material matrix. It has the characteristics of high transparency and yellowing resistance to ensure the light transmittance and high refraction of the device. The use of epoxy resin generally requires the addition of a curing agent for cross-linking and curing. The mechanical, electrical, and thermal properties of the anhydride-cured epoxy resin are better than those of the amine-cured one, but require a higher curing temperature a...

Claims

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Application Information

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IPC IPC(8): C08G59/68C08G59/42C07C211/63C07C53/128C07C51/41C07C209/68
CPCC07C53/128C07C211/63C08G59/4215C08G59/686
Inventor 陈小格李丽洁努尔加依那提·努尔动王子峰王梦寒田野张继超金韶华
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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