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Cage-shaped organic silicon flame retardant charring agent and preparation method thereof

A technology of organosilicon and char-forming agent, which is applied in the fields of organic chemistry, chemical instruments and methods, coatings, etc., can solve the problem of less varieties of char-forming agents or flame-retardant char-forming agents, and achieves low cost and stable physical and chemical properties. , the effect of dense and stable carbon layer structure

Active Publication Date: 2011-08-10
SUZHOU UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, at present, there are few varieties of char-forming agents or flame-retardant char-forming agents with excellent cost performance.

Method used

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  • Cage-shaped organic silicon flame retardant charring agent and preparation method thereof
  • Cage-shaped organic silicon flame retardant charring agent and preparation method thereof
  • Cage-shaped organic silicon flame retardant charring agent and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0046] Example 1 In a 100ml four-neck flask equipped with a stirrer, a thermometer, a dropping funnel, a reflux condenser and a hydrogen chloride absorption device, add 0.1mol (12.01g) trimethylolethane and 45ml acetonitrile, start stirring, and At 25°C, add 0.1 mol (14.95g) methyltrichlorosilane dropwise within about 30 minutes, and then raise the temperature to 65°C and reflux for 1 hour after the drop. Then the temperature was raised to 80°C for reflux reaction for 16 hours. After the hydrogen chloride was released, it was crystallized by cooling, filtered and dried to obtain 1,4-dimethyl-1-sila-2,6,7-trioxabicyclo[2 ,2,2]-octane white solid. Its yield is 92%, and its decomposition temperature is 350±10°C.

Embodiment 2

[0047] Example 2 In a 100ml four-necked flask equipped with a stirrer, a thermometer, a dropping funnel, a reflux condenser, and a hydrogen chloride absorption device, add 0.1mol (12.01g) of trimethylolethane and 45ml of dioxane, and open the Stir, and add 0.1 mol (14.95 g) methyltrichlorosilane dropwise at 25°C within about 30 minutes, then raise the temperature to 65°C and reflux for 1 hour after the drop is complete. Then the temperature was raised to 102°C for reflux reaction for 14 hours. After the hydrogen chloride was released, it was crystallized by cooling, filtered and dried to obtain 1,4-dimethyl-1-sila-2,6,7-trioxabicyclo[2 ,2,2]-octane white solid. Its yield is 93%, and its decomposition temperature is 350±10°C.

Embodiment 3

[0048] Example 3 In a 100ml four-neck flask equipped with a stirrer, a thermometer, a dropping funnel, a reflux condenser and a hydrogen chloride absorption device, add 0.1mol (12.01g) trimethylolethane and 45ml toluene, start stirring, and At 25°C, add 0.1 mol (14.95g) methyltrichlorosilane dropwise within about 30 minutes, and then raise the temperature to 65°C and reflux for 1 hour after the drop. Then the temperature was raised to 112°C for reflux reaction for 14 hours. After the hydrogen chloride was released, it was crystallized by cooling, filtered, and dried to obtain 1,4-dimethyl-1-sila-2,6,7-trioxabicyclo[2 ,2,2]-octane white solid. Its yield is 93%, and its decomposition temperature is 350±10°C.

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Abstract

The invention relates to a cage-shaped organic silicon flame retardant charring agent, i.e. a 1,4-dimethyl-1-sila-2,6,7-trioxabicyclo[2,2,2]-octane compound, and a preparation method thereof. The compound has a structure shown as the following formula in the specification. The preparation method comprises the step of: reacting methyl trichlorosilane or methyltrimethoxysilane with trimethylolethane in an organic solvent to prepare 1,4-dimethyl-1-sila-2,6,7-trioxabicyclo[2,2,2]-octane. The cage-shaped organic silicon flame retardant charring agent is a novel halogen-free non-toxic flame retardant charring agent, which has high flame retardant performance and good charring performance, can effectively prevent the melting and the dropping of high polymer during combustion, and is stable in physical and chemical properties, good in compatibility with macromolecular materials, high in raw material availability, simple in process and easy for industrial production.

Description

technical field [0001] The present invention relates to a kind of cage organosilicon flame retardant char-forming agent compound and its preparation method, in particular to 1,4-dimethyl-1-sila-2,6,7-trioxabicyclo[2,2, 2]-octane and a preparation method thereof, the compound can be used as a flame-retardant char-forming agent for materials such as polyolefins, polyesters, polyurethanes, and coatings. Background technique [0002] The rapid development and wide application of flammable synthetic polymer materials has promoted the research of flame retardant materials. The amount of flame retardants is increasing at a rate of 20% every year. With the advancement of technology, strict requirements for high efficiency, halogen-free, non-toxic and smoke-free have been put forward for flame retardants in recent years. In particular, halogenated flame retardants have been greatly restricted, while phosphorus and nitrogen based flame retardants have received more attention. Due to...

Claims

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Application Information

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IPC IPC(8): C07F7/18C08K5/549C08L23/00C08L23/12C08L67/00C08L75/04C09D7/12
Inventor 王彦林游基飞王乐然
Owner SUZHOU UNIV OF SCI & TECH
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