Preparation method of electronic grade triglycidyl isocyanurate

A technology of triglycidyl isocyanurate, applied in the direction of organic chemistry, can solve the problems of low product purity and unsuitability for large-scale industrial production, and achieve the effect of improving product purity

Active Publication Date: 2011-09-07
HUANGSHAN HUAHUI TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The products obtained by these common methods are only common-grade TGIC, the product purity is low, and it is not suitable for large-scale industrial production

Method used

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  • Preparation method of electronic grade triglycidyl isocyanurate
  • Preparation method of electronic grade triglycidyl isocyanurate
  • Preparation method of electronic grade triglycidyl isocyanurate

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preparation example Construction

[0010] A preparation method of electronic grade triglycidyl isocyanurate, comprising the following steps:

[0011] a, drop into epichlorohydrin, cyanuric acid, quaternary ammonium salt phase transfer catalyst, water in proportion, wherein the molar ratio of cyanuric acid and epichlorohydrin is 1: 11~1: 17, and the quaternary ammonium salt phase transfer catalyst is The mass of cyanuric acid is 4-10%, the water is 5-10% of the volume of epichlorohydrin, the heating temperature is controlled at 80-120°C, and the reaction is stirred for 4-6 hours. Under the excess condition of epichlorohydrin, carry out synthetic reaction, its reaction formula is:

[0012]

[0013] Among them, CA is cyanuric acid, and ECH is epichlorohydrin. Under the condition of stirring, the mixed liquid reacts continuously and gradually becomes clear and transparent, and serves as the raw material for the subsequent cyclization reaction.

[0014] B, add caustic soda in described a reaction system, the mo...

Embodiment 1

[0021] a. Under the condition of excessive epichlorohydrin, input cyanuric acid and tetramethylammonium chloride in proportion, wherein the molar ratio of cyanuric acid and epichlorohydrin is 1:11, and the quality of tetramethylammonium chloride is cyanuric acid 4% of the mass of uric acid, 5% of the volume of epichlorohydrin by water, heating and temperature control at 80° C., and stirring for 4 hours.

[0022] b. Add caustic soda to the reaction system of a, the molar ratio of caustic soda and cyanuric acid is 1:3, the temperature is controlled at 15°C, the reaction time is 100min, and then the solid salt is removed by pressure filtration.

[0023] c. After the reaction is over, under reduced pressure, the cyclization solution is distilled to remove epichlorohydrin through the reaction kettle, and then further removed through high-vacuum thin film evaporator distillation to remove epichlorohydrin, and the crude product is then crystallized, centrifuged, Electronic grade trig...

Embodiment 2

[0025] a. Under the condition of excessive epichlorohydrin, the mixture of cyanuric acid, tetramethylammonium chloride and benzyltriethylammonium chloride is input in proportion, wherein the molar ratio of cyanuric acid and epichlorohydrin is 1 : 17, the quality of the mixture of tetramethylammonium chloride and benzyltriethylammonium chloride is 10% of the mass of cyanuric acid, water is 10% of the volume of epichlorohydrin, heating and temperature control is at 120 ℃, stirring Reaction 6h.

[0026] b. Add caustic soda to the reaction system of a, the molar ratio of caustic soda and cyanuric acid is 1:3.5, the temperature is controlled at 20°C, the reaction time is 150min, and then the solid salt is removed by pressure filtration.

[0027] c. After the reaction is over, under reduced pressure, the cyclization solution is distilled to remove epichlorohydrin through the reaction kettle, and then further removed through high-vacuum thin film evaporator distillation to remove epi...

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Abstract

The invention mainly aims to provide a preparation method of electronic grade triglycidyl isocyanurate (TGIC). In order to realize the aim, the technical scheme in the invention is as follows: the preparation method of electronic grade TGIC comprises the following steps: a) adding epichlorohydrin, cyanuric acid, quaternary ammonium salt phase transfer catalyst and water according to a ratio, heating and stirring to react; b) adding flake caustic soda in the reaction system obtained in the step a) to react, then performing pressure filtration to remove solid salt; and c) performing vacuum distillation after the reaction, then using a high vacuum film evaporator to distill and remove epichlorohydrin, crystallizing the coarse product, centrifuging, grinding, and drying to obtain electronic grade TGIC. According to the treatment method provided by the invention, the purity of the TGIC product can be effectively increased, and the purity of TGIC can be increased from 92% to more than 99%, which reaches the electronic grade.

Description

technical field [0001] The invention relates to a preparation method of electronic-grade triglycidyl isocyanurate, which belongs to the technical field of organic chemical industry. Background technique [0002] Triglycidyl isocyanurate (TGIC for short) is a heteropolyepoxide, the scientific name is three (2,3-epoxypropyl)-s-triazine-2,4,6-(1H,3H,5H )-triketone. In addition to being used as powder coating curing agent, TGIC products are also used in medicine, electronics and other industries. Among them, electronic grade TGIC is mainly used in electronic inks, sealants for photosensitive materials, and raw materials for photoimaging solder resist inks. Although there are many domestic TGIC producers at present, they are all produced by the traditional two-step method. It is difficult to control the water generated by the reaction in the cyclization stage, which leads to intensified side reactions, low product purity, high chlorine content, and poor quality. . Because the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D405/14
Inventor 方向宏林光伟杨志萍
Owner HUANGSHAN HUAHUI TECH
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