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Preparation method of methyl tin ethyl mercaptan stearate

A technology of ester methyl tin and thioethanol, which is applied in the field of preparation of methyl tin thioethanol stearate, can solve the problems of difficult recovery of valuable by-products from wastewater, waste of resources, and lower yields, and achieve the goal of manufacturing Low cost, stable product quality, and little harm

Active Publication Date: 2017-06-23
云南锡业锡化工材料有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has added sulfide in the preparation of sulfurized fatty acid mercaptoethanol ester methyl tin, and common sulfide (sodium sulfide) has strong stink, and is bigger to the harm of human body, and, after adding sulfide, must be in waste water Introducing other metal salts into the waste water, making it difficult to recover valuable by-products in the wastewater, wasting resources
In addition, the method is to carry out the synthesis reaction under alkaline conditions, and under alkaline environment, the ester group structure in the fatty acid mercaptoethanol ester is very prone to saponification reaction, reducing the yield

Method used

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  • Preparation method of methyl tin ethyl mercaptan stearate
  • Preparation method of methyl tin ethyl mercaptan stearate
  • Preparation method of methyl tin ethyl mercaptan stearate

Examples

Experimental program
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Effect test

Embodiment 1

[0020] Put 2395kg of mercaptoethanol stearate into the reaction kettle, heat and stir the mixture, when the temperature reaches 55°C, start to drop methyl tin chloride aqueous solution and ammonia water, and adjust the acidity of the reaction system between 2 and 5; maintain Reaction system temperature and the stability of acidity, continue dripping methyl tin chloride aqueous solution and ammoniacal liquor, when dropping into the monomethyl tin trichloride aqueous solution 1200kg of mass concentration 45%, stop dripping ammoniacal liquor, leave standstill phase separation; The phase was washed with water at 60°C, and then stood still to separate the phases; the organic matter was distilled under reduced pressure at a temperature between 60°C and 90°C to remove water and other low-boiling impurities, and then filtered, cooled, and shaped to obtain the following: image 3 The pure product 2572kg of the trithioethanol stearate monomethyl tin of shown structure. The yield is 98.2...

Embodiment 2

[0025] Put 1777kg of mercaptoethanol stearate into the reaction kettle, heat and stir the mixture, when the temperature reaches 65°C, start to add methyltin chloride aqueous solution and ammonia water dropwise, and adjust the acidity of the reaction system between 2 and 5; maintain Reaction system temperature and the stability of acidity, continue dripping methyl tin chloride aqueous solution and ammoniacal liquor, when dropping into the dimethyl tin dichloride aqueous solution 1000kg of mass concentration 55%, stop dripping ammoniacal liquor, leave standstill phase separation; The phase was washed with water at 50°C, and then stood still to separate the phases; the organic matter was distilled under reduced pressure at a temperature between 90°C and 100°C to remove water and other low-boiling impurities, and then filtered, cooled, and shaped to obtain the following: image 3 The pure product 2089kg of the dithioethanol stearate dimethyl tin of shown structure. The yield is 99...

Embodiment 3

[0030] Put 1308kg of mercaptoethanol stearate into the reaction kettle, heat and stir the mixture, when the temperature reaches 60°C, start to add methyl tin chloride aqueous solution and ammonia water dropwise, and adjust the acidity of the reaction system between 2 and 5; maintain Reaction system temperature and the stability of acidity, continue to drop methyl tin chloride aqueous solution and ammoniacal liquor, when dropping into 800kg methyl tin chloride aqueous solution (the mass concentration of dimethyl tin dichloride is 30%, monomethyl trichloride When the mass concentration of tin is 15%), stop dripping ammonia water, and stand for phase separation; get the organic phase and wash it with water at 70°C, then stand for phase separation; the organic matter is distilled under reduced pressure at a temperature between 95°C and 105°C to remove water Wait for the low-boiling point impurities, then filter, cool, and shape to obtain 1477kg of the mixture of dithioethanol stear...

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Abstract

The invention provides a preparation method of methyl tin ethyl mercaptan stearate. The preparation method comprises the following steps: adding ethyl mercaptan stearate into a reaction kettle; heating and stirring a mixture; when the temperature reaches 50 DEG C to 70 DEG C, starting to dropwise add a methyl tin chloride water solution and ammonia water; adjusting the acidity of a reaction system to be 2 to 5; keeping the temperature and acidity of the reaction system stable; continually dropwise adding the methyl tin chloride water solution and the ammonia water; when all the water solution is added, stopping dropwise adding the ammonia water, and standing and carrying out phase splitting; taking an organic phase and washing with water; standing and carrying out phase splitting again; decompressing and distilling at temperature ranging from 60 DEG C to 140 DEG C to remove impurities with low boiling points from organics; filtering, cooling and shaping to obtain the methyl tin ethyl mercaptan stearate. According to the preparation method provided by the invention, decomposition of an ester group under strong acidic and alkaline environments is avoided, the reaction yield can be effectively improved and a valent byproduct ammonium chloride in wastewater can be recycled; the preparation method of the methyl tin ethyl mercaptan stearate has the advantages of high yield, low manufacturing cost, stable product quality, small damages and the like.

Description

technical field [0001] The invention relates to the technical field of preparation methods of methyl tin thioethanol stearate. Background technique [0002] At room temperature, methyl tin thioethanol stearate is a colorless or light yellow solid, which can be used as a heat stabilizer for the processing of PVC pipes, profiles, sheets, films, etc. It has good lubricating properties and low odor , low tin content, low manufacturing cost, good transparency and other advantages. [0003] At present, there are few documents reporting methyltin thioethanol stearate and its preparation method at home and abroad. Chinese patent CN104629208A discloses a preparation method of composite solid methyl tin PVC heat stabilizer, which uses fatty acid mercaptoethanol ester, methyl tin chloride mixture and sulfide to form sulfurized fatty acid mercaptoethanol ester through condensation reaction in aqueous solution Methyl tin, finally mixed with fatty acid metal salts. This method has adde...

Claims

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Application Information

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IPC IPC(8): C07F7/22
CPCC07F7/226
Inventor 易强顺李祥彦郭应辉胡洋刘莉
Owner 云南锡业锡化工材料有限责任公司