A kind of preparation method and application of pentaerythritol methylphenylthiosilicate

A technology of pentaerythritol silicate and methyl phenyl thio group, which is applied in the chemical field, can solve the problem that the flame retardant performance cannot meet the production requirements, etc., and achieves the effects of meeting the requirements of flame retardancy, improving the flame retardancy and simple preparation method.

Active Publication Date: 2020-10-20
SUZHOU UNIV OF SCI & TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing flame retardants usually only meet the requirements of a certain aspect, and the flame retardant properties sometimes cannot meet the production needs

Method used

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  • A kind of preparation method and application of pentaerythritol methylphenylthiosilicate

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Effect test

Embodiment 1

[0017] Preparation of intermediate: In a 100mL three-necked round-bottomed flask equipped with a stirrer, thermometer, dropping funnel, reflux condenser and hydrogen chloride absorption device, add 50mL of diethylene glycol dimethyl ether as a solvent and 0.1mol (13.62g) For pentaerythritol, add 0.1mol (14.95g) methyltrichlorosilane dropwise under stirring in an ice-water bath, and control the reaction temperature of the system not higher than 50°C. Reaction at 140°C for 4h. After no hydrogen chloride gas is released, most of the diethylene glycol dimethyl ether is distilled off under reduced pressure to obtain a white viscous liquid, which is cooled and crystallized, filtered, washed with dichloroethane, and dried to obtain a white solid formazan pentaerythritol silicate (CSRC).

[0018] Preparation of sodium benzenethiol: at room temperature, add 0.1mol (11.0g) of benzenethiol to an anhydrous and dry Erlenmeyer flask, then add 0.1mol (2.3g) of sodium particles, and shake sl...

Embodiment 2

[0021] Preparation of intermediate: In a 100mL three-necked round-bottomed flask equipped with a stirrer, thermometer, dropping funnel, reflux condenser and hydrogen chloride absorption device, add 50mL of diethylene glycol dimethyl ether as a solvent and 0.1mol (13.62g) For pentaerythritol, add 0.1mol (14.95g) methyltrichlorosilane drop by drop under stirring in an ice-water bath, control the reaction temperature of the system not higher than 50°C, slowly raise the temperature to 65°C after dropping, keep warm for 1.5h , heated to 150 ° C for 4.5 h. After no hydrogen chloride gas is released, most of the diethylene glycol dimethyl ether is distilled off under reduced pressure to obtain a white viscous liquid, which is cooled and crystallized, filtered, washed with dichloroethane, and dried to obtain a white solid formazan pentaerythritol silicate (CSRC).

[0022] Preparation of sodium benzenethiol: at room temperature, add 0.1mol (11.0g) of benzenethiol to an anhydrous and d...

Embodiment 3

[0025] Preparation of intermediate: In a 100mL three-necked round-bottomed flask equipped with a stirrer, thermometer, dropping funnel, reflux condenser and hydrogen chloride absorption device, add 50mL of diethylene glycol dimethyl ether as a solvent and 0.1mol (13.62g) For pentaerythritol, add 0.1mol (14.95g) methyltrichlorosilane drop by drop under stirring in an ice-water bath. Reaction at 160°C for 5h. After no hydrogen chloride gas is released, most of the diethylene glycol dimethyl ether is distilled off under reduced pressure to obtain a white viscous liquid, which is cooled and crystallized, filtered, washed with dichloroethane, and dried to obtain a white solid formazan pentaerythritol silicate (CSRC).

[0026] Preparation of sodium benzenethiol: at room temperature, add 0.1mol (11.0g) of benzenethiol to an anhydrous and dry Erlenmeyer flask, then add 0.1mol (2.3g) of sodium particles, and shake slowly until there are no bubbles Generate, stand still.

[0027] Pre...

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Abstract

The invention discloses a preparation method of pentaerythritol methyl phenylthiosilicate, which comprises the following steps: preparing an intermediate: adding a diethylene glycol dimethyl ether solvent and pentaerythritol in a three-necked round bottom flask, and stirring in an ice water bath condition; dropwise adding methyltrichlorosilane; removing part of diethylene glycol dimethyl ether through vacuum distillation to obtain a white viscous liquid; standing for cooling to room temperature and filtering the white viscous liquid to obtain produced crystals; washing and drying the crystalsto obtain the intermediate; preparing sodium benzenethiolate; adding the intermediate to a round bottom flask, adding the diethylene glycol dimethyl ether solvent and zinc chloride; dropwise adding concentrated hydrochloric acid while stirring to obtain an organic phase layer solution; adding a catalyst to the organic phase layer solution, adding sodium benzenethiolate to the organic phase layer solution to obtain a white solid pentaerythritol methyl phenylthiosilicate. The invention also discloses application of pentaerythritol methyl phenylthiosilicate.

Description

technical field [0001] The invention relates to the fields of chemistry and the like, in particular to a preparation method and application of pentaerythritol methylphenylthiosilicate. Background technique [0002] With the advancement of science and technology, synthetic materials have been widely used in people's lives, and their flammability has brought people increasingly serious fire hazards, thus promoting the development of flame-retardant materials. Flame retardants, functional additives that endow flammable polymers with flame retardancy, are mainly designed for the flame retardancy of polymer materials. [0003] It is a substance that can increase the flame resistance of polymer materials. It is mainly used in polymer materials such as plastics, rubber, fibers, etc., and most of these materials are combustible. Especially for plastics, if they are to be used in transportation, construction, electrical equipment, aviation, spaceflight, etc., it is urgent to solve t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/18C08K5/549
CPCC07F7/1892C08K5/549
Inventor 程宏英相鹏伟赵明王彦林
Owner SUZHOU UNIV OF SCI & TECH
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