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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

AI Technical Summary

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 addition, in the process of processing, the batch material is easy to stick to the roller, and the mold release and lubricity are poor, which is not conducive to the continuous processing and production of the product
[0005] CN102503972B (2015-6-17) discloses a kind of methyl tin maleate and preparation method thereof, yet how to prepare green and safe tin methyl mercaptide preparation method that tin content is reduced, thermal stability is good still needs Improve

Method used

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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

Examples

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Effect test

Embodiment 1

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

[0036] (1) Tinization: Put metal tin and catalyst into a pressure-resistant and acid-resistant reaction kettle, then pass in methyl chloride and heat and mix evenly at 150°C, carry out halogenation reaction for 0.2h, then add redistribution agent tin tetrachloride and Raise the temperature to 235°C, pressurize to 0.5MPa to carry out the tinning reaction for 1 hour, then distill and accept the fraction with a gas temperature within 150°C, and then absorb it with pure water to obtain an aqueous solution of methyl tin chloride;

[0037] The methyl alkene chloride comprises dimethyl tin dichloride and monomethyl tin trichloride; the first catalyst is a mixture of quaternary ammonium salt phase transfer catalyst and dimethyl sulfide according to the molar mass ratio of 1:2; The weight of the first catalyst accounts for 1% of the weight of metallic tin.

[0038] (2) Synthesis: Add...

Embodiment 2

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

[0047](1) Tinization: Put metal tin and catalyst into a pressure-resistant and acid-resistant reactor, then pass in methyl chloride, heat and mix evenly at 170°C, carry out halogenation reaction for 0.4h, then add redistribution agent tin tetrachloride and Raise the temperature to 235-245°C, pressurize to 0.5-0.8MPa to carry out the tinning reaction for 2 hours, then distill and accept the fraction whose gas temperature is within 230°C, and then absorb it with pure water to obtain an aqueous solution of methyl tin chloride;

[0048] Methyl alkene chloride comprises dimethyl tin dichloride and monomethyl tin trichloride; The first catalyst is a mixture of quaternary ammonium salt phase transfer catalyst and dimethyl sulfide according to the molar mass ratio of 1: 3; The weight of the first catalyst accounts for 3% of the weight of metallic tin.

[0049] (2) Synthesis: add the...

Embodiment 3

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

[0058] (1) Tinization: Put metal tin and catalyst into a pressure-resistant and acid-resistant reaction kettle, then pass in methyl chloride and heat and mix evenly at 160°C, carry out halogenation reaction for 0.3h, then add redistribution agent tin tetrachloride and Raise the temperature to 240°C, pressurize to 0.6MPa to carry out the tinning reaction for 1.5 hours, then distill and accept the fraction whose gas temperature is within 200°C, and then absorb it with pure water to obtain an aqueous solution of methyl tin chloride;

[0059] The methyl alkene chloride comprises dimethyl tin dichloride and monomethyl tin trichloride; the first catalyst is a mixture of quaternary ammonium salt phase transfer catalyst and dimethyl sulfide according to the molar mass ratio of 1:2.5; The weight of the first catalyst accounts for 2% of the weight of metallic tin.

[0060] (2) Synthes...

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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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