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Method for preparing mixture of methyl tin chloride

A technology of methyl tin chloride and mixture, which is applied in the direction of tin organic compounds, can solve the problems of increasing production cost, reducing the conversion rate of raw material tin, etc., and achieve the effect of increasing conversion rate, reducing the amount of waste residue, and high content

Inactive Publication Date: 2015-04-08
HUBEI NANXING CHEM GENERAL FACTORY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The other is that when trace moisture exists in the reaction system, tin tetrachloride reacts with tin powder to generate tin dichloride, and its reaction formula is: SnCL4+Sn→SnCL2; Tin melt will form a layer of film on the surface of tin powder or tin sheet to prevent tin powder from continuing to react with methyl chloride, which will generate a large amount of waste residue at the bottom of the reaction vessel, and these waste residues cannot be used, thus greatly reducing the conversion rate of raw material tin , which increases the production cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Add metal tin powder 1800g, Tetramethylammonium chloride or dimethyl sulfide 8g as catalyzer in the 10L stainless steel pressure-resistant reaction vessel that high-speed stirrer is housed, pass into the upper floor air in the methyl chloride replacement reaction vessel; Then, Seal the reaction vessel, start the heating device and high-speed stirrer, when the temperature in the reaction vessel reaches 180°C, inject methyl chloride from the bottom of the reaction vessel, tin powder and methyl chloride start to react, when the pressure in the reaction vessel reaches 2.5MPa , stop injecting methyl chloride, and when the temperature in the reaction vessel reaches 250° C., adjust the heating device so that the temperature in the reaction vessel remains between 250 and 280° C. Inject a certain amount of nitrogen into the reaction vessel to fill the upper space in the reaction vessel, then start to inject tin tetrachloride, after injecting 3400g tin tetrachloride, stop injectin...

Embodiment 2

[0032] Add metal tin powder 150kg, Tetramethylammonium chloride or dimethyl sulfide 1.5kg as catalyzer in the 800L stainless steel pressure-resistant reaction vessel that high-speed stirrer is housed, pass into the upper floor air in the methyl chloride displacement reaction vessel; Then , seal the reaction vessel, start the heating device and high-speed stirrer, when the temperature in the reaction vessel reaches 180°C, inject methyl chloride from the bottom of the reaction vessel, tin powder and methyl chloride start to react, when the pressure in the reaction vessel reaches 2.5MPa , stop injecting methyl chloride, and when the temperature in the reaction vessel reaches 250° C., adjust the heating device so that the temperature in the reaction vessel remains between 250 and 280° C. Inject a certain amount of nitrogen into the reaction vessel, to fill the head space in the said reaction vessel, then start to inject tin tetrachloride, when injecting 275kg tin tetrachloride, sto...

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PUM

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Abstract

The invention discloses a method for preparing a mixture of methyl tin chloride, which comprises the following steps of: heating tin and catalyst in a reaction vessel; injecting chloromethane when the temperature in the reaction vessel reaches 180 DEG C; keeping temperature between 250 and 280 DEG C when the temperature in the reaction vessel reaches 250 DEG C; and then injecting stannic chloride; stopping injecting the stannic chloride when the ratio of the molar weight of the stannic chloride to the molar weight of the tin is more than 0.9; sealing the reaction vessel, keeping the temperature, and reacting for one hour; transferring the materials in the reaction vessel into a distilling container; distilling the materials in the reaction vessel under the state of 130-160 DEG C temperature and 6-10 KPa pressure; and absorbing the material steam by water, thereby obtaining an aqueous solution of the mixture of methyl tin chloride, wherein the content of methyl trichlorosilane is high. According to the method provided by the invention, the waste residues in the synthetic reaction are efficiently reduced, the conversion rate of raw material tin is increased, and meanwhile, the decomposition of the methyl trichlorosilane is efficiently reduced.

Description

technical field [0001] The invention belongs to the field of fine chemical production, and relates to a preparation method of a methyltin chloride mixture. The content of monomethyltin trichloride in the methyltin chloride mixture obtained by the preparation method is high. Background technique [0002] Organotin compounds have been used as PVC plastic stabilizers for six or seven years. U.S. patent documents US3222317 and US3396185 describe the production and use of butyltin and octyltin heat stabilizers. Production process and usage examples of methyl tin alkoxide. After nearly 30 years of development, methyltin mercaptide has gradually become the mainstream product in the organic tin stabilizer industry. Now the commonly used methyltin mercaptides are dimethyl dithiolate tin and monomethyl trithiolate tin mixture, wherein the proportion of tin trithiolate is 20-30%. [0003] With the continuous optimization of plastic processing equipment, high-efficiency, high-speed ex...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/22
Inventor 李建丰韩永和李尖王友王爱红龙守奎钟新乐高勇
Owner HUBEI NANXING CHEM GENERAL FACTORY