Green and safe methyl tin mercaptide preparation method

A technology of methyl tin mercaptide and methyl tin, which is applied in the direction of chemical instruments and methods, tin organic compounds, compounds of group 4/14 elements of the periodic table, etc. There are some issues to be improved to achieve a good stable effect

Inactive Publication Date: 2016-09-07
ANHUI SHENGHUA XINAOTE CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Methyl tin (SM501) on the domestic market mainly contains 20% isooctyl methyl tin trimercaptoacetate and 80% isooctyl dimethyl tin dimercaptoacetate, and its tin content is 19.4, in actual During the processing, the methyl tin on the market will move from the inside of the product to the surface, and finally precipitate from the surface of the product, forming spots, which affects the fineness of the product. This is the so-called exudation (or sweating); In

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  • Green and safe methyl tin mercaptide preparation method
  • Green and safe methyl tin mercaptide preparation method
  • Green and safe methyl tin mercaptide preparation method

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[0034] Example one

[0035] The green and safe preparation method of methyl tin mercaptan includes the following steps:

[0036] (1) Tinning: Put metallic tin and catalyst into the pressure-proof and acid-proof reaction kettle, then pass in methyl chloride, heat and mix uniformly at 150℃, carry out the halogenation reaction for 0.2h, then add the redistributing agent tin tetrachloride and Heat up to 235°C and pressurize to 0.5MPa to carry out tinning reaction for 1 hour, then distill and accept the fraction with gas temperature within 150°C, and then absorb with pure water to obtain methyl tin chloride aqueous solution;

[0037] Methylene chlorides include dimethyl tin dichloride and monomethyl tin trichloride; the first catalyst is a mixture of quaternary ammonium salt phase transfer catalyst and dimethyl sulfide in a molar mass ratio of 1:2; The weight of the first catalyst accounts for 1% of the weight of metal tin.

[0038] (2) Synthesis: Add the obtained methyl tin chloride aque...

Example Embodiment

[0045] Example two

[0046] The green and safe preparation method of methyl tin mercaptan includes the following steps:

[0047] (1) Tinning: Put metallic tin and catalyst into the pressure and acid proof reactor, then pass in methyl chloride, heat and mix uniformly at 170℃, and carry out the halogenation reaction for 0.4h, then add the redistributing agent tin tetrachloride and mix The temperature is raised to 235-245°C, and the pressure is increased to 0.5-0.8MPa for tinning reaction for 2 hours, and then distilled and accepted the fraction with a gas temperature of 230°C, and then absorbed with pure water to obtain an aqueous solution of methyl tin chloride;

[0048] Methylene chloride includes dimethyl tin dichloride and monomethyl tin trichloride; the first catalyst is a mixture of quaternary ammonium salt phase transfer catalyst and dimethyl sulfide in a molar mass ratio of 1:3; The weight of the first catalyst accounts for 3% of the weight of the metal tin.

[0049] (2) Synthe...

Example Embodiment

[0056] Example three

[0057] The green and safe preparation method of methyl tin mercaptan includes the following steps:

[0058] (1) Tinning: Put metallic tin and catalyst into the pressure-proof and acid-proof reaction kettle, then pass in methyl chloride, heat and mix uniformly at 160℃, carry out the halogenation reaction for 0.3h, then add the redistributing agent tin tetrachloride and Heat up to 240°C and pressurize to 0.6MPa to carry out tinning reaction for 1.5 hours, then distill and accept the fraction with gas temperature within 200°C, and then absorb with pure water to obtain an aqueous solution of methyl tin chloride;

[0059] Methylene chloride includes dimethyl tin dichloride and monomethyl tin trichloride; the first catalyst is a mixture of quaternary ammonium salt phase transfer catalyst and dimethyl sulfide in a molar mass ratio of 1:2.5; The weight of the first catalyst accounts for 2% of the weight of the metal tin.

[0060] (2) Synthesis: Add the obtained methyl ...

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Abstract

The invention relates to a preparation method for organic tin type materials, in particular to a green and safe methyl tin mercaptide preparation method. The green and safe methyl tin mercaptide preparation method comprises the following steps: (1), tin processing: putting metal tin and a first catalyst into a reaction kettle, halogenating after charging methyl chloride, adding a redistribution agent to perform a tin reaction, distilling, receiving fractions with gas temperature of 150-230 DEG C, and using pure water to absorb, thereby obtaining a methyl tin chloride water solution; (2), synthesizing: adding the obtained methyl tin chloride water solution into isooctyl thioglycolate, adding a second catalyst, stirring to react at 5-15 DEG C for 0.2-0.4 hour, adding alkali liquid, continuously stirring to react till a pH value of a reaction system reaches 7-9, heating to 60-70 DEG C, reacting for 1-1.5 hours, standing, cooling down, and layering; (3), rinsing; (4) distilling. According to the green and safe methyl tin mercaptide preparation method, a product has high transparency, weather resistance, compatibility and volatilization precipitation resistance, and has good heat stability and low tin content.

Description

technical field [0001] The invention relates to a method for preparing organic tin substances, in particular to a method for preparing green and safe tin methyl mercaptide. 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] The main varieties of organotin are mono-alkyl tin, di-alkyl tin and tri-alkyl tin series, among which the tri-alkyl tin series is very toxic and cannot be used as a stabilizer; mono-alkyl tin has mono-methyl Tin, monobutyltin, monooctyltin, etc.; dialkyltin includes dimethyltin, dibutyltin, dioctyltin, etc. At present, the European Union has stipulated that the use of butyl tin and octyl tin series in PVC materials used in medical and food packaging is prohibited, while methyl tin series are still widely used in various high-grade PVC prod...

Claims

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Application Information

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IPC IPC(8): C07F7/22
CPCC07F7/226C07F7/2296
Inventor 李振杰杨立新焦健康宋建良
Owner ANHUI SHENGHUA XINAOTE CHEM CO LTD
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