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Green methyl tin mercaptide compound

A technology of tin methyl mercaptide and complexes, which is applied in the directions of tin organic compounds, compounds of elements of Group 4/14 of the periodic table, chemical instruments and methods, etc. Improvement, mold release, poor lubricity, etc., to increase the effect of yellowing resistance, excellent dispersion and stability, and high transparency

Inactive Publication Date: 2016-10-12
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 its preparation method, but how to prepare the green tin methyl mercaptide compound with reduced tin content and good thermal stability still needs to be improved

Method used

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  • Green methyl tin mercaptide compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Green tin methyl mercaptide compound, which is prepared by the following steps:

[0041] (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;

[0042] The methyl alkene chloride comprises dimethyl tin dichloride and monomethyl tin trichloride; the first catalyst is a mixture of tetrabutyl ammonium bromide and dimethyl sulfide according to the molar mass ratio of 1:2; the second The weight of a catalyst accounts for 1% of the weight of metallic tin.

[0043] (2) Synthesis: add the obtained methyl tin chlorid...

Embodiment 2

[0054] Green tin methyl mercaptide compound, which is prepared by the following steps:

[0055] (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;

[0056] Methyl olefin chloride comprises dimethyl tin dichloride and monomethyl tin trichloride; The first catalyst is the mixture of tetrabutyl ammonium chloride and dimethyl sulfide according to the molar mass ratio of 1: 3; The weight of a catalyst accounts for 3% of the metal tin weight.

[0057] (2) Synthesis: add the obtained methyl tin chloride aqueous solutio...

Embodiment 3

[0068] Green tin methyl mercaptide compound, which is prepared by the following steps:

[0069] (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;

[0070] Methyl olefin chlorides include dimethyl tin dichloride and monomethyl tin trichloride; the first catalyst is a mixture of trioctyl methyl ammonium chloride and dimethyl sulfide in a molar mass ratio of 1:2.5 ; The weight of the first catalyst accounts for 2% of the metal tin weight.

[0071] (2) Synthesis: add the obtained methyl tin chloride aqueous so...

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Abstract

The invention relates to an organic tin substance, in particular to a green methyl tin mercaptide compound. The compound is prepared in steps as follows: (1) tinning: metal tin and a catalyst are placed into a reaction kettle, then chloromethane is introduced, the mixture is heated and mixed evenly at the temperature of 150-170 DEG C for a halogenating reaction for 0.2-0.4 h, then a redistribution agent is added, and the mixture is heated and pressurized for a tinning reaction; (2) synthesis: an obtained methyl tin chloride aqueous solution is added to isooctyl thioglycolate, a second catalyst, alkane diacid and a regulator are added, a reaction is conducted, the pH value is adjusted to range from 7 to 9, and then the mixture is heated to 60-70 DEG C for a reaction for 3-4 h and is left to stand, cooled and layered; the regulator is prepared from 6-9 parts of a first compound regulator by mass, 7-11 parts of a second compound regulator by mass and 8-14 parts of a third compound regulator by mass; (3) water washing; (4) distillation. The product has the yellowing resistance and volatile separation resistance, is good in heat stability and has the low tin content.

Description

technical field [0001] The invention relates to a preparation method of organic tin substances, in particular to a green tin methyl mercaptide compound. 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 products due to its uniq...

Claims

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Application Information

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