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Flame retardant charring agent tetra(phosphono heterocyclic silicate methoxyl)silane compound and preparation method thereof

A technology of silane compound and trimethylol dimethyl silicate, which is applied in the field of tetrasilane compound, a flame-retardant char-forming agent, can solve the problems of flammable materials, hidden dangers of life and property safety, and achieve low cost and improved The effects of compatibility and good application development prospects

Inactive Publication Date: 2019-05-31
SUZHOU UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] With the development of polymer material science, plastics, rubber and fibers have been widely used in daily life, but most of these materials are easy to burn and often bring safety hazards to people's lives and property

Method used

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  • Flame retardant charring agent tetra(phosphono heterocyclic silicate methoxyl)silane compound and preparation method thereof
  • Flame retardant charring agent tetra(phosphono heterocyclic silicate methoxyl)silane compound and preparation method thereof
  • Flame retardant charring agent tetra(phosphono heterocyclic silicate methoxyl)silane compound and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0025] Example 1 In a 250ml four-neck flask equipped with a stirrer, a thermometer and a high-efficiency reflux condenser, and a hydrogen chloride absorption device at the top of the condenser, replace the air in the bottle with nitrogen, and add 39.2g (0.2mol) Trimethylolphosphine oxide cyclic ester of dimethyl silicate and 120ml of ethylene glycol dimethyl ether, after the trimethylol phosphine oxide cyclic ester of dimethyl silicate is dissolved and dispersed evenly, add 8.5g (0.05 mol) silicon tetrachloride, the dropping temperature does not exceed 50°C, after the dropping, raise the temperature to 85°C, keep the temperature for 12 hours, distill off the solvent under reduced pressure to obtain a turbid viscous liquid, cool it, and then pour the crude product into 120ml of ice water Stir rapidly for 30 minutes, let stand, and take off the lower layer of colorless viscous liquid to obtain the product flame-retardant char-forming agent tetrakis(phosphonoheterocyclic silicate ...

Embodiment 2

[0026] Example 2 In a 250ml four-neck flask equipped with a stirrer, a thermometer and a high-efficiency reflux condenser, and a hydrogen chloride absorbing device at the top of the condenser, replace the air in the bottle with nitrogen, and add 40.18g (0.205mol) Trimethylolphosphine oxide dimethylsilicate cyclic ester and 120ml acetonitrile, after trimethylolphosphine oxide cyclic dimethylsilicate is dissolved and dispersed evenly, add 8.5g (0.05mol) tetrachloride dropwise Silicon, the dropwise addition temperature does not exceed 50°C. After the dropwise addition, the temperature is raised to 80°C, and the temperature is kept for 12 hours. The solvent is distilled off under reduced pressure to obtain a turbid viscous liquid. After cooling, the crude product is poured into 120ml of ice water and stirred rapidly for 30 minutes, statically Place it, and take off the lower layer of colorless viscous liquid to obtain the product flame-retardant char-forming agent tetrakis(phosphon...

Embodiment 3

[0027] Example 3 In a 250ml four-neck flask equipped with a stirrer, a thermometer and a high-efficiency reflux condenser, and a hydrogen chloride absorbing device at the top of the condenser, replace the air in the bottle with nitrogen, and add 41.16g (0.21mol) Trimethylol phosphine oxide cyclic ester of dimethyl silicate and 120ml of dioxane, after the trimethylol phosphine oxide cyclic ester of dimethyl silicate is dissolved and dispersed evenly, add 8.5g (0.05mol) dropwise Silicon tetrachloride, the dropwise addition temperature does not exceed 50°C, after dropping, raise the temperature to 100°C, keep the temperature for 10 hours, distill off the solvent under reduced pressure to obtain a turbid viscous liquid, cool it, then pour the crude product into 120ml ice water and stir quickly After standing still for 30 minutes, the lower layer of colorless viscous liquid was taken to obtain the flame retardant char-forming agent tetrakis(phosphonoheterocyclic silicate methoxy)sil...

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Abstract

The invention relates to a flame retardant charring agent tetra(phosphono heterocyclic silicate methoxyl)silane compound and a preparation method thereof. The structural formula of the compound is represented in the description. The preparation method comprises following steps: adding dimethyl silicic acid trihydroxymethyl phosphine oxide cyclic ester and an organic solvent into a reactor with a hydrogen chloride absorbing device; dropwise adding silicon tetrachloride, controlling the mole ratio of silicon tetrachloride to dimethyl silicic acid trihydroxymethyl phosphine oxide cyclic ester ina range of 1:4 to 1:4.7, wherein the temperature is not higher than 50 DEG C during the dropwise addition process; after dropwise addition, raising the temperature to 80-150 DEG C, carrying out reactions at a constant temperature for 7 to 12 hours, and purifying the reaction product to obtain the flame retardant charring agent tetra(phosphono heterocyclic silicate methoxyl)silane compound. The compound is an excellent halogen-free phosphor-silicon synergetic flame retardant charring agent for polyvinyl alcohol, polyester, polyvinyl chloride, polyurethane, epoxy resin, unsaturated resin, and the like. The technology is simple, the equipment investment is little, and industrial production is easy to realize.

Description

technical field [0001] The present invention relates to a flame retardant char-forming agent tetrakis(phosphonoheterocyclic silicate methoxy)silane compound and a preparation method thereof, in particular to a flame-retardant char-forming agent tetrakis[1,1-dimethyl silicate Base-1-sila-2,6-dioxa-4-oxyl-4-phosphine-(4)-methylene] ester compound and preparation method thereof, the compound contains phosphorus and silicon double flame retardant elements , can be used as a flame retardant char-forming agent for polyvinyl alcohol, polyester, polyvinyl chloride, polyurethane, epoxy resin and unsaturated resin. Background technique [0002] With the development of polymer material science, plastics, rubber and fibers have been widely used in daily life, but most of these materials are easy to burn and often bring safety hazards to people's lives and property. Therefore, the research and development of flame retardants and flame retardant polymer materials has received people's at...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6596C08K5/549C08L63/00
Inventor 王彦林王世杰王天畅
Owner SUZHOU UNIV OF SCI & TECH
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