Preparation method of flame retardant sike dimethyl haloethoxysilicate compound

A technology of dimethyl haloethoxysilicate and compound, which is applied in the field of preparation of flame retardant dimethyl haloethoxysilicate compound, can solve the threat of people's life and property safety, fire and other problems, to achieve the effect of high flame retardant element content, high flame retardant efficiency and low volatility

Active Publication Date: 2019-04-16
苏州阳桥新型材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Most of these polymer materials are flammable and often cause fires, posing a serious threat to people's lives and property.

Method used

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  • Preparation method of flame retardant sike dimethyl haloethoxysilicate compound
  • Preparation method of flame retardant sike dimethyl haloethoxysilicate compound
  • Preparation method of flame retardant sike dimethyl haloethoxysilicate compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Embodiment 1 In the 250ml four-necked bottle that stirrer, thermometer and condensation tube are housed, and drying tube and hydrogen halide absorption device are equipped with at the top of condensation tube, replace the air in the bottle with nitrogen, add 8.74g (0.0333 mol) tris(2-hydroxyethyl) isocyanurate and 100ml dioxane, add 12.91g (0.1mol) dimethyldichlorosilane below 30°C, heat up to 70°C, keep warm for 5h; wait for HCl After the gas is released, cool down to below 30°C, add 8.05g (0.1mol) 2-chloroethanol dropwise, and control the reaction temperature not higher than 40°C at the rate of addition, raise the temperature to 100°C after dropping, and keep the temperature for 6 hours; wait for HCl After the gas is released, add 0.25g of melamine, adjust the pH of the system to 5-6, filter with suction, and distill the filtrate under reduced pressure to remove the solvent and a small amount of low boiling point substances to obtain Sac dimethyl chloroethoxysilicate, ...

Embodiment 2

[0037] Example 2 In a 250ml four-necked bottle equipped with a stirrer, a thermometer and a condensation tube, and a drying tube and a hydrogen halide absorption device on the top of the condensation tube, replace the air in the bottle with nitrogen, and add 8.74g (0.0333 mol) tris(2-hydroxyethyl)isocyanurate and 150ml tetrahydrofuran, add 12.91g (0.1mol) dimethyldichlorosilane below 30°C, raise the temperature to 50°C, and keep the reaction for 9h; wait until the HCl gas is released Finally, cool down to below 30°C, add 8.59g (0.1067mol) 2-chloroethanol dropwise, control the reaction temperature not higher than 40°C at the rate of addition, raise the temperature to 60°C after dropping, keep the temperature for 12 hours; wait until the HCl gas is released Finally, add 0.5g melamine, adjust the pH of the system to 5-6, filter with suction, and distill off the filtrate under reduced pressure to remove the solvent, excess 2-chloroethanol and a small amount of low boiling point, an...

Embodiment 3

[0038] Example 3 In a 250ml four-necked bottle equipped with a stirrer, a thermometer and a condensation tube, and a drying tube and a hydrogen halide absorption device on the top of the condensation tube, replace the air in the bottle with nitrogen, and add 8.74g (0.0333 mol) tris(2-hydroxyethyl)isocyanurate and 120ml acetonitrile, add 12.91g (0.1mol) dimethyldichlorosilane below 30°C, heat up to 60°C, keep warm for 8h; wait until the HCl gas is released After that, cool down to below 30°C, add 9.39g (0.1167mol) 2-chloroethanol dropwise, control the reaction temperature not higher than 40°C with the dropping speed, raise the temperature to 80°C after dropping, keep the temperature for 8 hours; wait until the HCl gas is released Finally, add 0.8g melamine, adjust the pH of the system to 5-6, filter with suction, and distill off the filtrate under reduced pressure to remove solvent, excess 2-chloroethanol and a small amount of low boiling point, and obtain Sac dimethyl chloroeth...

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Abstract

The invention relates to a preparation method of a sencor dimethyl halogenate ethyoxyl silicate ester compound serving as a flame retardant. The structural formula of the compound is shown in the specification, wherein Y is Cl or Br. The preparation method comprises steps as follows: dimethyl dichlorosilane has a reaction with tri(2-hydroxyethyl) isocyanurate in an organic solvent under the protection of nitrogen at the temperature of 50-70 DEG C for 5-9h and then has a reaction with 2-halogenated ethyl alcohol at the temperature of 60-100 DEG C for 6-14h; alternatively, dimethyl dibromosilane has a reaction with tri(2-hydroxyethyl) isocyanurate in an organic solvent at the temperature of 40-70 DEG C for 4-7h and then has a reaction with 2-halogenated ethyl alcohol at the temperature of 40-100 DEG C for 6-12h; sencor dimethyl halogenate ethyoxyl silicate ester is obtained after purification. The flame retardant has high flame retardancy, the char-forming effect is good, the compound is suitable for being used as a flame-retardant plasticizer of polyvinyl chloride, polyurethane, epoxy resin, unsaturated resin and the like, the production process is simple, the cost is low, and the industrial production is easy to realize.

Description

technical field [0001] The invention relates to a preparation method of a flame retardant Sike dimethyl haloethoxysilicate compound, in particular to tris{2-[dimethyl(2-chloroethoxy)silyloxy]ethyl A process for the preparation of tris{2-[dimethyl(2-bromoethoxy)silyloxy]ethyl}isocyanurate compounds suitable for use as polyvinyl chloride , polyurethane, epoxy resin, unsaturated resin and other flame retardant plasticizers. Background technique [0002] With the development of the national economy and the improvement of people's living standards, the application fields of synthetic polymer materials are becoming more and more extensive. Most of these polymer materials are flammable, often cause fires, and pose a serious threat to people's lives and property. In order to solve the flammability of synthetic materials and ensure the safety of synthetic materials, the most effective way is to add flame retardants. Due to the small amount of halogenated flame retardants, low pric...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/18C08K5/5455C08K5/544
Inventor 王彦林龚胜杨海军
Owner 苏州阳桥新型材料有限公司
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