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Silicic acid tetra (dichloropropyl) ester compound and preparation method thereof

A synergistic technology of epichlorohydrin and silicon halide, applied in the direction of silicon organic compounds, etc., to achieve good application prospects, small investment and low cost

Active Publication Date: 2012-06-27
南通敏孝文化传播有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the preparation and development of flame retardants using silicon tetrachloride as a raw material, there have been no reports so far

Method used

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  • Silicic acid tetra (dichloropropyl) ester compound and preparation method thereof
  • Silicic acid tetra (dichloropropyl) ester compound and preparation method thereof
  • Silicic acid tetra (dichloropropyl) ester compound and preparation method thereof

Examples

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Effect test

preparation example 1

[0040] Preparation Example 1 In a 250ml four-neck flask equipped with a stirrer and a drying tube, nitrogen protection was introduced, 0.80mol of epichlorohydrin was added, stirred, and the initial temperature was 25° C. The reaction is carried out and the temperature is gradually increased), and then the temperature is slowly raised to 50 ° C. After maintaining the temperature for 8 hours, the excess reactant is distilled off, cooled, and the liquid obtained by filtering is tetrakis (dichloropropyl) silicate. The yield is 93%, the decomposition temperature is 267±5°C, and the flash point (open cup) is 260±5°C. The degree of Baume is 45.53 (14°C), the density is 1.455 (14°C), and the refractive index is n D 20 = 1.4966.

preparation example 2

[0041] Preparation Example 2 In a 250ml four-necked flask equipped with a stirrer and a drying tube, pass through nitrogen protection, add 0.6mol of epichlorohydrin, stir, and start to drop 0.10mol of silicon tetrachloride at an initial temperature of 25°C (with The reaction is carried out and the temperature is gradually increased), and then the temperature is slowly raised to 70 ° C. After maintaining the temperature for 6 hours, the excess reactant is distilled off, cooled, and the liquid obtained by filtering is tetrakis (dichloropropyl) silicate. The yield is 95%, the decomposition temperature is 267±5°C, and the flash point (open cup) is 260±5°C. The degree of Baume is 45.53 (14°C), the density is 1.455 (14°C), and the refractive index is n D 20 = 1.4966.

preparation example 3

[0042] Preparation Example 3 In a 250ml three-neck flask equipped with a stirrer and a drying tube, feed nitrogen protection, add 0.50mol of epichlorohydrin, stir, and start to drop 0.10mol of silicon tetrachloride (with the reaction Gradually increase the temperature), then slowly heat up to 90°C, and after maintaining the temperature for 4 hours, distill off the excess reactant, cool, and filter the resulting liquid to be tetra(dichloropropyl)silicate, with a yield of 95 %, the decomposition temperature is 267±5°C, and the flash point (open cup) is 260±5°C. The degree of Baume is 45.53 (14°C), the density is 1.455 (14°C), and the refractive index is n D 20 =1.4966

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Abstract

The invention relates to a silicic acid tetra (dichloropropyl) ester compound and a preparation method thereof, the structure of the polymer is as shown in the following formula, wherein n is not less than 0 and not more than 4, and the synthetic method is as follows: respectively dripping silicon tetrachloride epoxy with epichlorohydrin, 1,3-dichloro-2-propanol or 2,3-dichloropropanol under the nitrogen protection and at the initial temperature of 25 DEG C, then carrying out direct reaction or reaction in an organic solvent under the heating condition, then purifying reaction products and preparing the silicic acid tetra (dichloropropyl) ester. The silicic acid tetra (dichloropropyl) ester has high thermal stability and good compatibility with polymer material, thereby being an excellentflame retardant plasticizer. Simultaneously, the synthesis process is simple, the equipment investment is low, and the cost is low, thereby being conductive to environmental protection and particularly having great significance for solving the pollution of a large amount of silicon tetrachloride produced by polysilicon.

Description

technical field [0001] The invention relates to a silicon-halogen synergistic flame retardant and its preparation process, in particular to a tetra(dichloropropyl)silicate compound and its preparation method. The compound can be used as polyvinyl chloride, polyester, polyurethane, epoxy Flame retardant plasticizer for resin, FRP resin, paint and other materials. Background technique [0002] The utilization of solar energy is an inevitable way of energy development, and the large-scale production of polysilicon (photovoltaic industry) is the fundamental industry to realize the conversion of solar energy. However, producing one ton of polysilicon will produce 15-20 tons of silicon tetrachloride pollutants. At present, how to deal with industrial waste silicon tetrachloride has become a bottleneck restricting the development of my country's solar polysilicon industry (photovoltaic industry). Due to the imperfection of domestic supporting facilities, silicon tetrachloride is ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/04C08L27/06C08K5/5415
Inventor 王彦林刁建高
Owner 南通敏孝文化传播有限公司
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