Preparation method of pentaerythritol double ring dimethyl silicate compound serving as fire retardant

A technology of dimethyl silicate and pentaerythritol, which is applied in chemical instruments and methods, compounds of Group 4/14 elements of the periodic table, organic chemistry, etc., can solve problems such as secondary hazards, and achieve low cost and compatibility. The effect of good performance and simple preparation method

Inactive Publication Date: 2015-06-17
苏州阳桥新型材料有限公司
View PDF1 Cites 5 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Practice has shown that the flame retardant materials prepared by modifying halogen-containing flame retardants will produce a large amount of smoke and toxic corrosive hydrogen halide gas during the combustion process, causing secondary hazards, so halogen-based flame retardants have received certain attention in many aspects. degree of limitation

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Preparation method of pentaerythritol double ring dimethyl silicate compound serving as fire retardant
  • Preparation method of pentaerythritol double ring dimethyl silicate compound serving as fire retardant
  • Preparation method of pentaerythritol double ring dimethyl silicate compound serving as fire retardant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Example 1 In a 150ml four-necked flask equipped with a stirrer, a thermometer, and a high-efficiency fractionation device, add 13.62g (0.1mol) pentaerythritol, 24.04g (0.2mol) dimethyldimethoxysilane and 40ml toluene, and heat up to Start the boiling fractionation reaction at 80°C, control the temperature at the top of the fractionation column to not be higher than 65°C, and continuously separate the generated methanol. As the reaction progresses, the free dimethyldimethoxysilane decreases, and the temperature of the reaction system gradually increases. Insulate and react at 110°C for about 7 hours. When the fractionated methanol reaches the theoretical amount, stop the reaction, cool, filter with suction, rinse the filter cake with water three times, drain it, and dry the filter cake to obtain a white solid pentaerythritol bicyclodimethylsilane Ester, product yield 95.0%.

Embodiment 2

[0021] Example 2 In a 150ml four-neck flask equipped with a stirrer, a thermometer, and a high-efficiency fractionation device, add 13.62g (0.1mol) of pentaerythritol, 24.04g (0.2mol) of dimethyldimethoxysilane and 50ml of dimethylbenzene, and heat up Start the boiling fractionation reaction at 80°C, control the top temperature of the fractionation column to not be higher than 65°C, and continuously separate the generated methanol. As the reaction progresses, the free dimethyldimethoxysilane decreases, and the temperature of the reaction system gradually increases , keep the reaction at 140°C for about 6 hours, when the fractionated methanol reaches the theoretical amount, stop the reaction, cool, filter with suction, rinse the filter cake with water three times, drain it, and dry the filter cake to obtain a white solid pentaerythritol bicyclodimethyl Silicate, product yield 98.5%.

Embodiment 3

[0022] Example 3 In a 150ml four-neck flask equipped with a stirrer, a thermometer, and a high-efficiency fractionation device, add 13.62g (0.1mol) of pentaerythritol, 24.04g (0.2mol) of dimethyldimethoxysilane and 50ml of tetrachloroethane , the temperature is raised to 80°C to start the boiling fractionation reaction, and the temperature at the top of the fractionation column is controlled not to be higher than 65°C, and the generated methanol is continuously separated. As the reaction progresses, the free dimethyldimethoxysilane decreases, and the temperature of the reaction system gradually Raise the temperature and keep it warm at 130°C for about 7 hours. When the fractionated methanol reaches the theoretical amount, stop the reaction, cool, filter with suction, rinse the filter cake with water three times, drain it, and dry the filter cake to obtain a white solid pentaerythritol bicyclodi Methyl silicate, product yield 96.6%.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

Abstract

The invention relates to a preparation method of a pentaerythritol double ring dimethyl silicate compound serving as a fire retardant. The structure of the compound is shown in the following formula.The preparation method comprises the following steps: in a reactor provided with a high efficiency fraction collector, adding dimethyl dimethoxy silicon alkane and pentaerythritol with a molar ratio of 1 to 2, and an appropriate amount of anorganic solvent, controlling the temperature of a top of a fractionating column not to be higher than 65 DEG C, continuously separating generated methanol, and when the fractionated methanol achieves a theory amount, performing purification so as to obtain a white solid pentaerythritol double ring dimethyl silicate . The compound disclosed by the invention is high in flame resistant efficacy, is good in carbon forming performance, and is suitable for being used as the fire retardant of polyolefine, polyurethane, an epoxy resin, an unsaturated resin and the like. The production technology is simple, the investment of equipment is few, the raw materials are east to obtain, the cost is low, and the industrialized production is easy to realize.

Description

technical field [0001] The invention relates to a preparation method of a flame retardant pentaerythritol bicyclodimethyl silicate compound. Pentaerythritol bicyclodimethylsilicate 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] The wide application of synthetic organic polymer materials has greatly improved and enriched people's lives, but because most of the synthetic polymer materials themselves are flammable, it brings convenience to people and also brings great fire safety hazards . In order to improve the flammability of synthetic materials, the development and application of flame retardants have attracted more and more attention. Practice has shown that the flame retardant materials prepared by modifying halogen-containing flame retardants will produce a large amount of smoke and toxic corrosive hydrogen halide gas ...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/18C08K5/549C08L27/06
Inventor 王彦林张东娣王世杰唐诗
Owner 苏州阳桥新型材料有限公司
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap