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Dimethyl silicate pentaerythritol ester compound as fire retardant and preparation method thereof

A technology of pentaerythritol dimethylsilicate and pentaerythritol, which is applied in chemical instruments and methods, compounds of elements of Group 4/14 of the periodic table, organic chemistry, etc., can solve the limitation of halogen-based flame retardants, secondary hazards, A large amount of hydrogen halide gas and other problems, to achieve the effect of good compatibility, low cost, good application and development prospects

Active Publication Date: 2015-06-17
HUZHOU RUIGAO NEW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Practice shows that halogen-containing flame retardants will produce a lot of smoke and toxic corrosive hydrogen halide gas during combustion, causing secondary hazards
Therefore, the application of halogenated flame retardants is limited to a certain extent.

Method used

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  • Dimethyl silicate pentaerythritol ester compound as fire retardant and preparation method thereof
  • Dimethyl silicate pentaerythritol ester compound as fire retardant and preparation method thereof
  • Dimethyl silicate pentaerythritol ester compound as fire retardant and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Example 1 In a 100ml four-neck flask equipped with a stirrer, a thermometer, a high-efficiency reflux condenser and a drying tube and a hydrogen chloride absorption device at the upper mouth of the condenser, add 30ml of ethylene glycol dimethyl ether and 6.8g (0.05mol ) pentaerythritol, stirred and heated to 75°C to fully dissolve the pentaerythritol, then cooled to 40°C, added dropwise 12.9g (0.1mol) of dimethyldichlorosilane, and the dropping process controlled the temperature not to exceed 50°C. Insulate at 50°C for 2 hours, then raise the temperature to 70°C, heat for 8 hours, stir and cool to 30°C, filter with suction, recover the solvent, wash the filter cake with water to remove the attached free acid, and dry the filter cake to obtain a white solid dimethyl Pentaerythritol silicate, product yield 92.6%.

Embodiment 2

[0027] Example 2 Add 40ml of acetonitrile and 6.8g (0.05mol) of pentaerythritol in a 100ml four-neck flask equipped with a stirrer, a thermometer, a high-efficiency reflux condenser and a drying tube and a hydrogen chloride absorption device at the upper mouth of the condenser, and stir and heat To 75°C, fully dissolve pentaerythritol, then lower the temperature to 40°C, add 12.9g (0.1mol) dimethyldichlorosilane dropwise, control the temperature during the dropwise addition to not exceed 50°C, after the drop, raise the temperature to 60°C, Insulate for 2 hours, then heat up to 80°C, heat for 6 hours, stir and cool to 30°C, filter with suction, recover the solvent, wash the filter cake with water to remove the attached free acid, dry the filter cake to obtain white solid pentaerythritol dimethyl silicate ester, the product yield is 93.5%.

Embodiment 3

[0028] Example 3 Add 50ml of dichloroethane and 6.8g (0.05mol) of pentaerythritol in a 100ml four-necked flask equipped with a stirrer, a thermometer, a high-efficiency reflux condenser and a drying tube and a hydrogen chloride absorption device at the upper mouth of the condenser , stirred and heated to 75°C to fully dissolve the pentaerythritol, then lower the temperature to 40°C, add 12.9g (0.1mol) dimethyldichlorosilane dropwise, and control the temperature during the dropwise addition to not exceed 50°C. 60°C, keep warm for 2h, then raise the temperature to 82°C, keep warm for 6h, stir and cool to 30°C, filter with suction, recover the solvent, wash the filter cake with water to remove the attached free acid, dry the filter cake to obtain a white solid dimethyl Pentaerythritol silicate, product yield 94.2%.

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Abstract

The invention relates to a dimethyl silicate pentaerythritol ester compound as a fire retardant, and a preparation method thereof. The structural formula of the compound is shown in the description. The preparation method comprises the following steps: sufficiently dissolving pentaerythritol in an organic solvent, in a temperature environment of 50 DEG C or below, dropwise adding dimethyl dichlorosilane or dimethyldibromosilane; after dropwise adding, heating to 50-80 DEG C; performing a heat preservation reaction for 2 hours; then performing a heat preservation reaction for 4-8 hours at 70-130 DEG C; performing purification so as to obtain a white solid dimethyl silicate pentaerythritol ester. The dimethyl silicate pentaerythritol ester disclosed by the invention is high in flame resistant efficacy, is good in charring performance, is suitable for being used as a fire retardant of polyolefine, polyurethane, an epoxy resin , an unsaturated resin and the like. The production technology is simple, the investment in equipment is small, the raw materials are easy to obtain, the cost is low, and the industrialized production is easy to realize.

Description

technical field [0001] The invention relates to a flame retardant pentaerythritol dimethyl silicate compound and a preparation method thereof. Pentaerythritol dimethylsilicate is a halogen-free silicone flame retardant, suitable for use as a flame retardant for materials such as polyolefins, polyurethanes, epoxy resins, and unsaturated resins. Background technique [0002] In recent years, synthetic organic polymer materials have been widely used in electronics, electrical, machinery, transportation and chemical industries. However, due to the flammability of the polymer material itself, it also brings great safety hazards while bringing convenience to people. In order to improve the flammability of synthetic materials, the development and application of flame retardants have attracted more and more attention. Practice shows that halogen-containing flame retardants will produce a lot of smoke and toxic corrosive hydrogen halide gas during combustion, causing secondary haza...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/18C08K5/549C08L67/02
Inventor 王彦林王世杰唐诗
Owner HUZHOU RUIGAO NEW MATERIALS CO LTD
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