Unlock instant, AI-driven research and patent intelligence for your innovation.

Low-chlorine electronic-grade TGIC and preparation method thereof

An electronic-grade sodium chloride technology, applied in organic chemistry, etc., can solve problems such as excessive content of organic by-products, insufficient purity of sodium chloride, unsatisfactory reaction efficiency, etc., and achieve simplified reaction steps, excellent protection, and yield high rate effect

Pending Publication Date: 2021-08-20
HUANGSHAN HUAHUI TECH
View PDF1 Cites 1 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] For this reason, the technical problem to be solved by the present invention is to provide a low-cost method for preparing low-chlorine electronic grade TGIC, so as to solve the problems that there are many by-products and unsatisfactory reaction efficiency in the synthesis TGIC process in the prior art;
[0008] The third technical problem to be solved by the present invention is to provide a high-purity by-product sodium chloride to solve the problems of insufficient purity of sodium chloride and excessive content of organic by-products in the process product

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Low-chlorine electronic-grade TGIC and preparation method thereof
  • Low-chlorine electronic-grade TGIC and preparation method thereof
  • Low-chlorine electronic-grade TGIC and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] In the reaction device, add sodium cyanate and epichlorohydrin with a molar ratio of 1:2.5 and mix well, and follow the n 催化剂 :n 氰酸钠 =0.08:1 ratio, add catalyst (hexadecyltrimethylammonium bromide: sodium carbonate = 1:2) and mix well, control the system temperature at 105°C for high-temperature reflux reaction for 2h; after the reaction, cool the reaction product to At room temperature, remove sodium chloride by suction filtration, then collect the filtrate and carry out vacuum distillation under negative pressure conditions (-0.098Mpa) to remove solvent and unreacted epichlorohydrin, and further add 2 times the mass of sodium cyanate Ethanol is used as the crystallization solvent, crystallization treatment is carried out at 5°C, suction filtration and drying are carried out to obtain high-purity electronic-grade TGIC products in the form of white powdery solid particles.

[0026] After the sodium chloride obtained by centrifugation is dried in a vacuum oven to recove...

Embodiment 2

[0028] In the reaction device, add sodium cyanate and epichlorohydrin with a molar ratio of 1:3.4 and mix well, and follow the n 催化剂 :n 氰酸钠 = 0.1:1 ratio of catalyst (hexadecyltrimethylammonium bromide: sodium carbonate = 1:3) was mixed, and the temperature of the system was controlled at 106°C for high-temperature reflux reaction for 1.7h; after the reaction, the reaction product was cooled to room temperature, remove sodium chloride by suction filtration, then collect the filtrate and carry out vacuum distillation under negative pressure conditions (-0.098Mpa) to remove solvent and unreacted epichlorohydrin, and further add 3 times the mass of sodium cyanate A certain amount of methanol is used as a crystallization solvent, crystallization treatment is carried out at 0°C, centrifuged and then dried to obtain a high-purity electronic-grade TGIC product of white powdery solid particles.

[0029] After the sodium chloride obtained by centrifugal separation is dried in a vacuum...

Embodiment 3

[0031] In the reflux reaction device, add sodium cyanate and epichlorohydrin with a molar ratio of 1:4.3 and mix well, and follow the n 催化剂 :n 氰酸钠 = 0.12:1 ratio, add catalyst (cetyltrimethylammonium bromide: sodium carbonate = 1:2.5) and mix well, control the system temperature at 107°C for high temperature reaction for 1.3h; after the reaction, cool the reaction product to At room temperature, remove sodium chloride through centrifugation, then collect the filtrate and carry out vacuum distillation under negative pressure conditions (-0.098Mpa) to remove solvent and unreacted epichlorohydrin, and further add 3 times the amount of sodium cyanate. Ethanol is the crystallization solvent, crystallization treatment is carried out at -5°C, centrifuged and then dried to obtain high-purity electronic-grade TGIC products with white powdery solid particles.

[0032] After the sodium chloride obtained after centrifugation is dried in a vacuum oven to recover the solvent (120° C.), whe...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention belongs to the technical field of curing agents, and particularly relates to a method for preparing low-chlorine electronic-grade TGIC and a high-purity byproduct sodium chloride at low cost. According to the method for preparing the low-chlorine electronic-grade TGIC at low cost, sodium cyanate and epoxy chloropropane are used as reaction raw materials, catalysis is carried out at a high temperature by using a transfer catalyst, and a substitution reaction of the sodium cyanate and the epoxy chloropropane and a trimerization cyclization reaction of a reaction intermediate are sequentially carried out, so that the required TGIC product is prepared. In the whole reaction, the epichlorohydrin is used as a reaction raw material and a reaction solvent at the same time, other solvents or water do not need to be additionally introduced, the reaction can be carried out at high temperature, the reaction efficiency is improved, the condition of ring opening of epoxy groups of the product caused by a large amount of water in the system is avoided, few by-products are generated in the whole reaction, the yield of the target product is high, and the purity of the prepared TGIC product is high.

Description

technical field [0001] The invention belongs to the technical field of curing agents, specifically relates to a low-chlorine electronic grade TGIC and high-purity by-product sodium chloride, and further discloses a low-cost method for preparing low-chlorine electronic-grade TGIC and high-purity by-product sodium chloride. Background technique [0002] Triglycidyl isocyanurate, also known as tris (2,3-epoxypropyl) isocyanurate, referred to as TGIC, commonly known as "Bick", is an important cyanuric acid derivative. Since TGIC has three highly active epoxy groups and the triazine ring is also very stable, TGIC not only has the physical and chemical properties of general epoxy resins, but also can be used with epoxy curing agents such as amines, carboxylic acids, phenolic anhydrides, etc. It produces a curing reaction; it can also generate cross-linked insoluble and infusible materials, and the curing reaction speed is faster; and compared with the usual epoxy resin, TGIC has a...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): C07D405/14
CPCC07D405/14
Inventor 林光伟杨志萍项纯何领
Owner HUANGSHAN HUAHUI TECH