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Preparation method of dimethyl silicate acid di(1,3-dichloroixopropyl) ester compound serving as flame-retardant plasticizer

A technology of dimethyl silicic acid and flame retardant plasticizer, which is applied in the field of preparation of organosilicon and halogen synergistic flame retardant plasticizer dimethyl silicate diester compound, can solve the problem of difficult to find substitutes, halogen-based retardant Combustible use restrictions and other issues, to achieve the effect of good symmetry, good application and development prospects, and simple equipment

Active Publication Date: 2015-06-03
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 dimethyl silicate acid di(1,3-dichloroixopropyl) ester compound serving as flame-retardant plasticizer
  • Preparation method of dimethyl silicate acid di(1,3-dichloroixopropyl) ester compound serving as flame-retardant plasticizer
  • Preparation method of dimethyl silicate acid di(1,3-dichloroixopropyl) ester compound serving as flame-retardant plasticizer

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 dimethyl silicate acid di(1,3-dichloroixopropyl) ester compound serving as a flame-retardant plasticizer. The structural formula of the compound is shown in the specification, wherein X is Cl or Br. The preparation method comprises the steps as follows: dimethyl dichloro-silicane or dimethyl dibromo-silane and 1,3-dichloro isopropanol in the mole ratio of 1:(2-3) have a reaction in an organic solvent under the protection of nitrogen for 5-9h at the temperature ranging from 30 DEG C to 70 DEG C, and dimethyl silicate acid di(1,3-dichloroixopropyl) ester is obtained after purification. Dimethyl silicate acid di(1,3-dichloroixopropyl) ester has high flame ratardancy and good compatibility with macromolecular materials and is suitable for being used as the 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 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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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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