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Synthesis process of dimethyl tin dichloride

A technology of dimethyl tin dichloride and synthesis process, applied in the direction of tin organic compounds, etc., can solve the problems of environmental pollution, complex process, low yield of finished products, etc., achieve shortened reaction time, high product purity, and short synthesis time Effect

Active Publication Date: 2012-06-27
启东市强强贸易有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] But above-mentioned method technique is complicated, and the product produced is the mixture of monomethyl tin trichloride and dimethyl tin dichloride, is not suitable for producing high-purity dimethyl tin dichloride and has more side effects after using catalyst product, and at present, the reaction temperature of this method is high, the pressure is high, the risk is large, the yield of finished product is not high, and there is environmental pollution, which causes the current method to be unfavorable for industrial production and application

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] In the pressure reaction kettle equipped with a special stirrer, thermometer, pressure gauge and conduit, add 300 kg of tin particles, 30 kg of dimethyl sulfoxide, 10 kg of tin tetrachloride, and 200 kg of solid dimethyl tin dichloride kg, according to the heating rate of 1.5°C / min, the temperature is raised to 180°C, the pressure of methyl chloride is controlled between 0.9-1.3Mpa, the reaction is about 4 hours, the reaction temperature is controlled at 180-210°C, and the consumption of methyl chloride is about 300 kg. After the reaction is over, control the reaction temperature at 200-240°C, pressure 1.3-1.5Mpa, react for about 2 hours, then distill at atmospheric pressure, and receive the distillate with the gas temperature in the kettle between 188°C and 200°C to obtain dimethyl tin dichloride. The utilization rate of tin ingot is 96.5%; the yield of methyl tin is 98.9%, among which dimethyl tin dichloride accounts for 98.7%, methyl tin trichloride 1.2%, trimethyl t...

Embodiment 2

[0027] In a pressure reactor equipped with a special stirrer, a thermometer, a pressure gauge and a conduit, add 350 kilograms of tin particles, 5 kilograms of dimethyl sulfoxide, 10 kilograms of tin tetrachloride, and the solid dimethyl dichloride in Example 1. A total of 250 kilograms of tin chloride and the remaining black solid slag at the end of the distillation were raised to 188°C at a heating rate of 2°C / min, the reaction temperature was controlled at 180-210°C, and the pressure of methyl chloride was controlled between 0.9-1.3Mpa. React for about 4 hours, control the reaction temperature at 180-210 ° C, the consumption of methyl chloride is about 350 kg, the reaction is over, then control the reaction temperature at 200-240 ° C, pressure 1.3-1.5Mpa, react for about 2 hours, then normal pressure Distill and receive the fraction whose gas temperature in the tank is between 188°C and 200°C to obtain dimethyl tin dichloride. The utilization rate of tin ingot is 95.5%; the...

Embodiment 3

[0029] In the pressure reactor equipped with special stirrer, thermometer, pressure gauge and conduit, add 250 kilograms of tin particles, 30 kilograms of dimethyl sulfide, 10 kilograms of tin tetrachloride, the solid dimethyl A total of 200 kg of tin dichloride and the black solid slag remaining at the end of the distillation are raised to 180°C at a heating rate of 1.0°C / min, and the pressure of methyl chloride is controlled between 0.9-1.3Mpa. React for about 4 hours and control the reaction temperature. At 180-210°C, the consumption of methyl chloride is about 250 kg, the reaction is over, then control the reaction temperature at 200-240°C, pressure 1.3-1.5Mpa, react for about 2h, then distill at atmospheric pressure, and receive the gas temperature in the kettle In the distillate between 188°C and 200°C, dimethyl tin dichloride is obtained. The utilization rate of tin ingot is 97.1%; the yield of methyl tin is 99.0%, wherein dimethyl tin dichloride accounts for 98.7%, met...

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Abstract

The invention discloses a synthesis method of dimethyl tin dichloride, which comprises the following steps of: 1) adding tin, a catalyst and tin tetrachloride to a reactor, the amount of the catalyst being 5-15% of the weight of the tin, the amount of the tin tetrachloride being 1-10% of the weight of the tin, and heating to 160-190 DEG C according to a heating procedure; 2) under the conditions that the reaction temperature is controlled between 175 and 215 DEG C and the reaction pressure is controlled between 0.5 and 1.5MPa, stirring in the reactor, and adding vaporized methyl chloride gas until the completion of the reaction; 3) after the completion of the reaction, under the conditions that the reaction temperature is controlled between 180 and 250 DEG C, the reaction pressure is controlled between 1.3 and 1.5 MPa, obtaining the dimethyl tin dichloride by distillation. The high-purity dimethyl tin dichloride is prepared according to the invention and the method is capable of improving the utilization rate of tin ingots and the yield of methyl tin chloride. The method adopts a high-pressure method for one-step catalytic synthesis, and has the advantages of simple process, short reaction time, and high product purity.

Description

technical field [0001] The invention relates to the production field of fine chemicals, more specifically, the synthesis process of high-purity dimethyl tin dichloride. Background technique [0002] Dimethyltin dichloride (DMTC), English name: Dimethyltin Dichloride, CAS NO: 753-73-1, molecular formula: C 2 h 6 C1 2 Sn, relative molecular mass: 219.57. [0003] Dimethyl tin dichloride mixed with methyl tin trichloride is mainly used to produce methyl tin heat stabilizer, which is the main raw material for the production of methyl tin heat stabilizer; however, high-purity dimethyl tin dichloride With the development of science and technology in recent years, its use in magnesium or alloy corrosion inhibition, LOW-E glass coating, esterification reaction catalysis and other related fields is increasing year by year. And it has incomparable superiority when used on LOW-E glass coating. [0004] The traditional method for preparing dimethyl tin dichloride is not only cumber...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/22
Inventor 冯勇张建根
Owner 启东市强强贸易有限公司
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