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Preparation method of dimethyl silicic acid (chlorine acrylate) diester as flame resistant plastifier

A technology of dimethyl silicate and flame retardant plasticizer, which is applied in the field of flame retardant plasticizers, can solve problems such as difficulty in finding substitutes, and achieve good symmetry, good compatibility, and good stability

Inactive Publication Date: 2015-06-17
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

Since the European Union announced in 1986 that polybrominated diphenyl ether flame retardants produced carcinogenic toxic substances when burned, the use of halogenated flame retardants has been restricted to a certain extent.
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 their toxicity has become an important aspect of halogenated flame retardants. research direction

Method used

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  • Preparation method of dimethyl silicic acid (chlorine acrylate) diester as flame resistant plastifier
  • Preparation method of dimethyl silicic acid (chlorine acrylate) diester as flame resistant plastifier
  • Preparation method of dimethyl silicic acid (chlorine acrylate) diester as flame resistant plastifier

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] 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 9.45g (0.1mol ) chloropropanol, 65ml of dioxane, add 6.45g (0.05mol) of dimethyldichlorosilane dropwise, control the reaction temperature not higher than 20°C at the rate of addition, raise the temperature to 50°C after dropping, and keep the reaction for 7h; After the HCl gas is released, add 0.12 g of melamine to 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 matter to obtain di(monochloropropyl) dimethyl silicate. Yield 90.8%.

Embodiment 2

[0035] 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 10.40g (0.11mol ) Chloropropanol, 50ml acetonitrile, add 6.45g (0.05mol) dimethyldichlorosilane dropwise, control the reaction temperature not higher than 20°C with the drop rate, raise the temperature to 40°C after the drop, keep the temperature for 9h; wait for HCl gas After the release, add 0.25g melamine to adjust the pH of the system to 5-6, filter with suction, and distill the filtrate under reduced pressure to remove the solvent, excess chloropropanol (recycled for use) and a small amount of low boiling point substances to obtain dimethicic acid dimethicone (Monochloropropyl) ester, yield 91.4%.

Embodiment 3

[0036]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 11.82g (0.125mol ) Chloropropanol, 45ml ethylene glycol dimethyl ether, add 6.45g (0.05mol) dimethyldichlorosilane dropwise, control the reaction temperature not higher than 20°C with the dropping rate, raise the temperature to 70°C after dropping, and keep warm for reaction 5h; after the HCl gas is released, add 0.37g of melamine to adjust the pH of the system to 5-6, filter with suction, distill the filtrate under reduced pressure to remove the solvent, excess chloropropanol (recycled for use) and a small amount of low boiling point substances to obtain two Bis(monochloropropyl) methyl silicate, yield 93.7%.

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Abstract

The invention relates to a preparation method of dimethyl silicic acid (chlorine acrylate) diester as a flame resistant plastifier. The structure of the compound is shown in the formula (refer to the Specification), wherein OC3H6Cl refers to OCH2CHClCH3 and OCH(CH2Cl)CH3. The preparation method comprises the following steps: under nitrogen protection, the molar ratio of dimethyl dichlorosilane or dimethyl dibromo-silane to chloropropyl alcohol is 1:2-3, under the temperature of 20-90 DEG C, and in an organic solvent, the reaction is performed for 5-9 hours; through purification, the dimethyl silicic acid (chlorine acrylate) diester is obtained. The dimethyl silicic acid (chlorine acrylate) diester as the flame resistant plastifier, disclosed by the invention, is high in flame resistant efficacy, is good in plasticity, is suitable for the flame resistant plastifier of polyvinyl chloride, polyurethane, epoxy resin, unsaturated resin and the like, is simple in production technology, and is low in cost, and industrialized production is easy to realize.

Description

technical field [0001] The invention relates to a method for preparing a flame-retardant plasticizer di(monochloropropyl)silicate. The compound has the synergistic flame-retardant plasticizing effect of silicon and chlorine, and is suitable for polyvinyl chloride, polyurethane, Flame retardant plasticizer for epoxy resin, unsaturated resin, etc. Background technique [0002] With the rapid development of science and technology in the world, the continuous improvement of people's living standards and the enhancement of safety and fire prevention awareness, the flame retardant industry has developed rapidly. Since the European Union announced in 1986 that polybrominated diphenyl ether flame retardants produced carcinogenic toxic substances when burned, the use of halogenated flame retardants has been restricted to a certain extent. However, due to the excellent comprehensive cost performance of halogenated flame retardants, and it is difficult to find ideal substitutes, resea...

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 苏州阳桥新型材料有限公司
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