Preparation method of flame retardant plasticizer dimethyl silicate di(1,3-dihaloisopropyl) ester compound

A technology of dimethyl silicic acid and flame retardant plasticizer is applied in the field of preparation of silicone and halogen synergistic flame retardant plasticizer dimethyl silicate diester compound, which can solve the limitation of use of halogen-based flame retardants, It is difficult to find alternatives and other problems to achieve the effect of good application development prospects, good symmetry, and simple equipment

Active Publication Date: 2017-10-17
HUZHOU RUIGAO NEW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The use of halogenated flame retardants has been restricted since the European Union announced in 1986 that PBDE flame retardants produced dioxins (Dioxin) when they were burned.
However, due to the excellent comprehensive cost performance of halogenated flame retardants, and it is difficult to find ideal substitutes, research and development of high-efficiency halogenated flame retardants to reduce the amount of flame retardants and reduce the generation of harmful gases during combustion has become a halogenated flame retardant. Important research direction of fuel

Method used

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  • Preparation method of flame retardant plasticizer dimethyl silicate di(1,3-dihaloisopropyl) ester compound
  • Preparation method of flame retardant plasticizer dimethyl silicate di(1,3-dihaloisopropyl) ester compound
  • Preparation method of flame retardant plasticizer dimethyl silicate di(1,3-dihaloisopropyl) ester compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Example 1 In a 250ml four-necked bottle equipped with a stirrer, a thermometer and a condenser tube, and a drying tube and a hydrogen chloride absorption device at the top of the condenser tube, replace the air in the bottle with nitrogen, and add 6.45g (0.05mol ) dimethyldichlorosilane and 65ml of acetonitrile, add dropwise 21.79g (0.1mol) of 1,3-dibromoisopropanol, and control the reaction temperature at a rate not higher than 30°C. React for 8 hours; after the HCl gas is released, add 0.24g 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 dimethyl silicate bis(1,3- Dibromoisopropyl) ester, yield 89.6%.

Embodiment 2

[0034]Example 2 In a 250ml four-necked bottle equipped with a stirrer, a thermometer and a condenser tube, and a drying tube and a hydrogen chloride absorption device at the top of the condenser tube, replace the air in the bottle with nitrogen, and add 6.45g (0.05mol ) dimethyldichlorosilane and 55ml dichloroethane, add dropwise 23.97g (0.11mol) 1,3-dibromoisopropanol, control the reaction temperature with the dropping rate not higher than 30°C, and raise the temperature to 70°C after dropping ℃, heat preservation reaction for 5h; after the HCl gas is released, add 0.49g 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 excess 1,3-dibromoisopropanol (recycled and used ) and a small amount of low boiling point substances to obtain bis(1,3-dibromoisopropyl) dimethyl silicate with a yield of 92.2%.

Embodiment 3

[0035] Example 3 In a 250ml four-necked bottle equipped with a stirrer, a thermometer and a condenser tube, and a drying tube and a hydrogen chloride absorption device at the top of the condenser tube, replace the air in the bottle with nitrogen, and add 6.45g (0.05mol ) dimethyldichlorosilane and 40ml tetrahydrofuran, add 27.24g (0.125mol) 1,3-dibromoisopropanol dropwise, and control the reaction temperature at a rate not higher than 30°C. React for 9 hours; after the HCl gas is released, add 0.73g of melamine, adjust the pH of the system to 5-6, filter with suction, distill the filtrate under reduced pressure to remove the solvent, excess 1,3-dibromoisopropanol (recycled) and a small amount of Low-boiling point products yielded bis(1,3-dibromoisopropyl) dimethyl silicate with a yield of 90.7%.

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Abstract

The invention relates to a preparation method of a flame-retardant plasticizer bis(1,3-dihaloisopropyl) dimethyl silicate compound. The structure of the compound is shown in the following formula: where X=Cl or Br. The preparation method is as follows: under the protection of nitrogen, in the temperature range of 30 DEG C to 70 DEG C, the molar ratio of dimethyldichlorosilane or dimethyldibromosilane and 1,3-dihaloisosilane is 1:2 to 3. Propanol is reacted in an organic solvent for 5-9 hours, and after purification, bis(1,3-dihaloisopropyl) dimethyl silicate is obtained. The bis(1,3-dihaloisopropyl) dimethyl silicate of the invention has high flame retardant performance and good compatibility with polymer materials, and is suitable for use as polyvinyl chloride, polyurethane, epoxy resin, unsaturated resin, etc. The flame retardant plasticizer has the advantages of simple production process, low cost and easy industrialized production.

Description

technical field [0001] The invention relates to a preparation method of organosilicon and halogen synergistic flame retardant plasticizer dimethyl silicate bis(1,3-dihaloisopropyl) ester compound. The compound is suitable as a flame retardant plasticizer for polyvinyl chloride, polyurethane, epoxy resin, unsaturated resin, etc. Background technique [0002] The rapid development of the world economy, the continuous improvement of people's living standards and the enhancement of safety and fire awareness have promoted the rapid development of the flame retardant industry. Since the European Union announced in 1986 that PBDE flame retardants produced dioxins (Dioxin) when burned, the use of halogenated flame retardants has been restricted. However, due to the excellent comprehensive cost performance of halogenated flame retardants, and it is difficult to find ideal substitutes, research and development of high-efficiency halogenated flame retardants to reduce the amount of fl...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/18C08K5/5419C08L27/06
Inventor 王彦林杨海军
Owner HUZHOU RUIGAO NEW MATERIALS CO LTD
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