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Method for preparing dimethyltin chloride

A technology of dimethyl tin dichloride and tetramethyl ammonium chloride, which is applied in the direction of tin organic compounds, can solve the problems of high requirements for reaction conditions, inconvenient source of raw materials, inability to prepare by itself, etc., and achieve the conversion rate of raw materials High efficiency, protection of reaction equipment, and low cost

Inactive Publication Date: 2010-12-22
WEIFANG YIHUA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the prior art, the method steps for preparing dimethyl tin dichloride are cumbersome, the sources of raw materials are inconvenient, the requirements for reaction conditions are relatively high, and the yield is also low
For units with relatively large demand, because they cannot be prepared by themselves, they need to be purchased, which increases the production cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] In the autoclave equipped with agitator, thermometer, pressure gauge and conduit, add 120 kilograms of flake tin, 25 kilograms of tetramethylammonium chloride catalyst and 28 kilograms of tin tetrachloride and seal it, and heat up to 130 After ℃, stop heating; then stir at a speed of 100rpm and start to add 150 kg of methyl chloride (the gas of chloride has been dried by an adsorption drier, and the desiccant in the dryer adopts silica gel to obtain a water content of the gas of chloride≤500ppm) , continue to heat up to 210 ° C, pressure 1.3Mpa, stop adding chloromethane and continue to stir the reaction for 5 hours to obtain gaseous dimethyl tin dichloride; finally carry out falling film absorption to control the temperature of gaseous dimethyl tin dichloride The temperature is 220°C, the pressure is 1.6Mpa, 180 kg of water is used as the absorption liquid, and the water is circulated by a water pump in a vacuum state to carry out falling film absorption of gaseous dime...

Embodiment 2

[0018] In the autoclave equipped with agitator, thermometer, pressure gauge and conduit, add 35 kilograms of flake tin, 7 kilograms of tetramethylammonium chloride catalyst and 7.5 kilograms of tin tetrachloride and seal it, and heat up to 110 Stop heating after ℃; Stir with the speed of 90rpm then and begin to add 45 kilograms of methyl chloride (the gas of chloride has been dried through the adsorption drier, and the desiccant in the dryer adopts silica gel to obtain the water content≤500ppm of the gas of chloride), Continue to heat up to 200 DEG C, pressure 1.2Mpa, stop adding chloromethane and continue stirring reaction for 3 hours to obtain gaseous dimethyltin dichloride; finally carry out falling film absorption, control the temperature of gaseous dimethyltin dichloride as 210°C, pressure 1.1Mpa, using 50 kg of water as the absorbing liquid, and using a water pump to circulate the water in a vacuum state to absorb gaseous dimethyl tin dichloride by falling film, and the a...

Embodiment 3

[0020] In the autoclave equipped with agitator, thermometer, pressure gauge and conduit, add 102 kg of flake tin, 20 kg of tetrabutylammonium chloride catalyst and 23.8 kg of tin tetrachloride and seal it, and heat up to 100 Stop heating after ℃, stir with the speed of 130rpm and start to add 120 kilograms of methyl chloride (the gas of chloride has been dried through the adsorption dryer, and the desiccant in the dryer adopts silica gel to obtain the water content of the gas of chloride≤500ppm), heat up To 250°C, pressure 1.1Mpa, stop adding methyl chloride and continue to stir for 4 hours to produce gaseous dimethyltin dichloride; finally carry out falling film absorption, control the temperature of gaseous dimethyltindichloride to 250°C , the pressure is 1.6Mpa, 150 kg of water is used as the absorbing liquid, and a water pump is used to circulate the water in a vacuum state to carry out falling film absorption of gaseous dimethyl tin dichloride. The absorption time is 5 hou...

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Abstract

The invention discloses a method for preparing dimethyltin chloride, which comprises the following steps of: 1) heating tin, a catalyst and tin tetrachloride with a weight ratio of 1:0.1-0.5:0.1-0.3 to between 100 and 170 DEG C under the airtight condition, wherein the catalyst is tetramethylammonium chloride or tetrabutylammonium chloride; 2) adding chloromethane with stirring, continuing to raise the temperature to between 170 and 250 DEG C under the pressure of 0.9 to 1.7MPa, stopping adding the chloromethane and then continuing to stir for 1 to 5 hours to prepare gaseous dimethyltin chloride; and 3) performing falling film absorption on the gaseous dimethyltin chloride for 1 to 6 hours by using water as absorption liquid under the conditions that the temperature of the gaseous dimethyltin chloride is between 180 and 260 DEG C and the pressure is 0.9 to 1.7MPa to obtain aqueous solution of the dimethyltin chloride. By a direct synthesis method, a process is simple, production cost is greatly reduced and a product is nontoxic and meets the requirement of environmental protection.

Description

technical field [0001] The invention relates to the technical field of chemical industry, in particular to a preparation method of dimethyl tin dichloride. Background technique [0002] The intermediate dimethyl tin dichloride (DMCT) is in the state of aqueous solution, and it is widely used in magnesium or alloy corrosion inhibitors, glass coatings, electroluminescent materials and catalysts. As an intermediate, DMCT can be further synthesized and processed into vinyl halide resin, especially polyvinyl chloride resin (PVC) heat stabilizer-methyltin mercaptide, which is highly efficient, low-toxic, and highly transparent. In the prior art, the method steps for preparing dimethyl tin dichloride are cumbersome, the sources of raw materials are inconvenient, the requirements for reaction conditions are relatively high, and the yield is also low. For units with relatively large demand, because they cannot be prepared by themselves, they need to be purchased, which increases the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/22
Inventor 张冶
Owner WEIFANG YIHUA CHEM
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