Flame retardant tetra(thiophosphonic heterocyclic silicate methoxide) silane compound and preparation method thereof

A technology of silane compound and trimethylolphosphine sulfide dimethylsilicate, applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., can solve flammable, life and property problems Fire hazards and other problems, to achieve the effect of improving compatibility, improving flame retardant charcoal efficiency, and low cost

Inactive Publication Date: 2019-06-14
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 science and technology, synthetic polymer materials such as plastics, rubber and fibers have been widely used in daily life, but most of these materials are flammable and often bring fire hazards to people's lives and property

Method used

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  • Flame retardant tetra(thiophosphonic heterocyclic silicate methoxide) silane compound and preparation method thereof
  • Flame retardant tetra(thiophosphonic heterocyclic silicate methoxide) silane compound and preparation method thereof
  • Flame retardant tetra(thiophosphonic heterocyclic silicate methoxide) silane compound and preparation method thereof

Examples

Experimental program
Comparison scheme
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 absorbing device at the top of the condenser, replace the air in the bottle with nitrogen, and add 42.4g (0.2mol) Trimethylol phosphine sulfide dimethyl silicate and 120ml ethylene glycol dimethyl ether, after trimethylol phosphine sulfide 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 tetrakis(thiophosphonoheterocyclic silicate methoxy)silane. The yield was 77.5%, and the flas...

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 43.46g (0.205mol) Trimethylol phosphine sulfide dimethyl silicate and 120ml acetonitrile, after trimethylol phosphine sulfide dimethyl silicate 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 Set, and take off the lower layer of colorless viscous liquid to obtain the product flame retardant tetrakis (thiophosphonoheterocyclic silicate methoxy)...

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 44.52g (0.21mol) Trimethylol phosphine sulfide dimethyl silicate and 120ml dioxane, after trimethylol phosphine sulfide dimethyl silicate is dissolved and dispersed evenly, add 8.5g (0.05mol) dropwise Silicon tetrachloride, the dropping temperature does not exceed 50°C, after the 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 of ice water and stir quickly After standing still for 30 minutes, the lower layer of colorless viscous liquid was removed to obtain the product flame retardant tetrakis(thiophosphonoheterocyclic silicate methoxy)silane. The yield was 87.1%, and the flash p...

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Abstract

The invention relates to a flame retardant tetra(thiophosphonic heterocyclic silicate methoxide) silane compound and a preparation method thereof. The structure of the compound is shown as a formula in the description. The preparation method comprises the following steps of adding dimethyl silicate trimethylol phosphine sulfide cyclic ester and organic solvents into a reaction vessel provided witha hydrogen chloride absorption device; then, dripping silicon tetrachloride; controlling the mol ratio of the silicon tetrachloride to the dimethyl silicate trimethylol phosphine sulfide cyclic esterto be 1:4-1:4.7; controlling the dripping temperature not to exceed 50 DEG C; after the dripping completion, raising the temperature to 80 to 150 DEG C; performing heat insulation reaction for 7 to 12h; performing purification treatment to obtain a product of the flame retardant of tetra(thiophosphonic heterocyclic silicate methoxide) silane. The compound is an excellent halogen-free phosphorus silicon and sulphur flame retardant, and can be used as a flame retardant char forming agent of polyvinyl alcohol, polyester, polyvinyl chloride, polyurethane, epoxy resin, unsaturated resin and the like; the process is simple; the equipment investment is low; the industrialized production can be easily realized.

Description

technical field [0001] The invention relates to a flame retardant tetrakis (thiophosphonoheterocyclic silicate methoxy) silane compound and a preparation method thereof, in particular to a flame retardant tetrakis[1,1-dimethyl -1-sila-2,6-dioxa-4-thio-4-phosphine-(4)-methylene] ester compound and its preparation method, the compound contains phosphorus, silicon, sulfur triple flame retardant It 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 science and technology, synthetic polymer materials such as plastics, rubber and fibers have been widely used in daily life, but most of these materials are flammable and often bring fire hazards to people's lives and property. Therefore, the research and development of flame retardants has received people's attention. Due to the increasing improvement of flame retardant regula...

Claims

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Application Information

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