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Process for synthesizing methyl tin chloride

A technology of monomethyltin tin trichloride and synthesis method, applied in directions such as tin organic compounds, can solve problems such as expensive catalyst price, and achieve the effects of low price, high purity, and shortening the process of synthesis

Active Publication Date: 2008-12-10
湖北犇星新能源材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the catalyst is more expensive

Method used

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  • Process for synthesizing methyl tin chloride

Examples

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Effect test

Embodiment 1

[0019] Example 1: Add 119g of metal tin powder and 3g of dimethyl sulfide into a stainless steel autoclave with stirring, pass through 10g of methyl chloride and raise the temperature to 180-230°C for reaction. After the consumption of methyl chloride is complete, add 35g of tin tetrachloride, continue to add 100g of methyl chloride and react at 180-230°C for 3-6 hours, then distill under reduced pressure to obtain 262.2g of methyl tin chloride, and the reaction yield is 99.32%.

Embodiment 2

[0020] Example 2: Add 131g of metal tin powder and 3.3g of dimethyl sulfide into a stainless steel autoclave with stirring, feed 11g of methyl chloride and raise the temperature to 180-230°C for reaction. After the methyl chloride is consumed, add 38.5g of tin tetrachloride, continue to add 110g of methyl chloride, react at 180-230°C for 3-6 hours, then distill under reduced pressure to obtain 288.1g of methyl tin chloride, the reaction yield is 99.22%.

Embodiment 3

[0021] Embodiment 3: Add 154.7g of metal tin powder and 3.9g of dimethyl sulfide in a stainless steel autoclave with stirring, feed 13g of methyl chloride and heat up to 180-230°C for reaction, after the consumption of methyl chloride is completed, then Add 45.5g of tin tetrachloride, continue to add 130g of methyl chloride and react at 180-230°C for 3-6 hours, then distill under reduced pressure to obtain 340.5g of methyl tin chloride, the reaction yield is 99.18%.

[0022] In the above-mentioned embodiment:

[0023] The tin powder is in the range of 10-50 meshes, and can be firstly mixed with the solvent methyl tin chloride at a temperature of 180-200°C.

[0024] The solvent methyl tin chloride can be composed of monomethyl tin trichloride and dimethyl tin dichloride, the weight ratio of the two is 15-25: 75-85, and generally 20: 80 is used for comparison it is good.

[0025] When the present invention is reacted in a stainless steel high-pressure reactor with stirring, th...

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Abstract

The invention discloses a method for synthesizing methyl tin chloride. The invention adopts a synthesizing method by high pressure and one-step catalysis. The method comprises the following specific steps that: dimethyl thioether is used as a catalyst; tin powder and the methyl tin chloride are evenly mixed in a stainless steel high-pressure reaction kettle at a temperature of between 180 and 200 DEG C, passed through with methyl chloride and heated to a temperature of between 180 and 230 DEG C for carrying out a first reaction; after the methyl chloride is consumed, tin tetrachloride is added and methyl chloride is passed through to the mixture for carrying out a second reaction for 3 to 6 hours; and the mixture is subjected to decompression and distillation to prepare the methyl tin chloride. The method changes the prior synthesizing method which uses a grignard reagent to synthesize the methyl tin chloride; as the adopted catalyst is low molecular thioether, the catalyst has cheap price, shortens the process of synthesizing a methyl tin intermediate product; and the synthesized methyl tin intermediate product has high purity, contains no other impurities and has a yield reaching over 99 percent.

Description

technical field [0001] The invention relates to the field of fine chemical production, in particular to a preparation process of methyl tin chloride. Background technique [0002] There are many patents on the use of organotin compounds in PVC resin as stabilizers, such as US patents 3222317, 3396185, etc., mainly butyltin and octyltin, because propyltin has an odor, and ethyltin is poisonous and replaced. [0003] In the 1970s, American Morton Chemical Company developed dimethyl tin bis(isooctyl thioglycolate), namely TM-181FS, which is a high-efficiency stabilizer for the preparation of PVC and PVC copolymers. [0004] There are many preparation methods for TM-181FS, and the synthesis of the methyl tin chloride intermediate of TM-181FS is the most critical step, which directly affects the quality of TM-181FS. Such as U.S. Patents 3810868, 3887519, 351966 and 4129584, etc., what they synthesized adopted was the Grignard reagent method, and the catalysts used were tetrabuty...

Claims

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Application Information

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IPC IPC(8): C07F7/22
Inventor 戴百雄吴勇宫廷徐善武刘勇王少培温志鹏张建广苏禾蒋俊
Owner 湖北犇星新能源材料有限公司
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