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Methyl tin reverse thioester and preparation method thereof

A technology of methyl tin and reverse thioester, applied in the direction of tin organic compounds, etc., can solve problems such as insufficient lubricity, and achieve the effects of improving initial coloration, delaying PVC degradation, and improving lubrication.

Active Publication Date: 2012-01-04
ZHEJIANG HIMPTON NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this type of stabilizer has insufficient lubricity due to the limitation of its own alkyl chain length, so it must be used in combination with a lubricant to achieve the best effect

Method used

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  • Methyl tin reverse thioester and preparation method thereof
  • Methyl tin reverse thioester and preparation method thereof
  • Methyl tin reverse thioester and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] 147g of isooctanoic acid, 78g of mercaptoethanol and 140g of hexanaphthene were mixed in a three-necked flask equipped with a thermometer, a stirrer and a reflux device, stirred, heated to 120°C, the reactant began to reflux, and slowly added dropwise 6g of vitriol oil (98.5 wt%), close the separatory funnel after the dropwise addition, reflux until there are no more drops of water hanging on the inner wall of the distillation column, cool to room temperature, then heat to about 80°C to distill off the solvent to obtain 204.2g of mercaptoethyl isooctanoate ;

[0039] In a three-necked flask equipped with a thermometer, a stirrer and a vacuum reflux device, 204.2 g of mercaptoethyl isooctanoate, 6 g of concentrated sulfuric acid (98.5 wt %) and 95 g of mercaptoacetic acid obtained above were mixed, stirred, heated to 70 ° C, and kept The vacuum degree is -0.062~-0.074MPa, react for 2 hours, no more water drips out of the water separator, cool to room temperature, wash wi...

Embodiment 2

[0044] Mix 150g of isooctanoic acid, 79.6g of mercaptoethanol and 150g of xylene in a three-necked flask equipped with a thermometer, a stirrer and a reflux device, stir, heat to 125°C, the reactant starts to reflux, and slowly add 8g of p-toluene dropwise Sulfonic acid, after the dropwise addition, close the separatory funnel, reflux until no more water droplets hang on the inner wall of the distillation column, cool to room temperature, and distill off the solvent at about 140°C to obtain 208.1 g of mercaptoethyl isooctanoate;

[0045] Mix 208.1g of mercaptoethyl isooctanoate, 8g of p-toluenesulfonic acid and 96g of mercaptoacetic acid in a three-neck flask equipped with a thermometer, a stirrer and a reflux device, stir, heat to 90°C, and maintain a vacuum of -0.068 ~-0.079MPa, reacted for 2.5 hours, no more water dripped out of the water separator, cooled to room temperature, washed with water, took out the oil phase, and distilled and dehydrated under reduced pressure to o...

Embodiment 3

[0051] 156g of isooctanoic acid, 81.9g of mercaptoethanol and 160g of ether were mixed in a three-necked flask equipped with a thermometer, a stirrer and a reflux device, stirred, heated to 130°C, the reactant began to reflux, and 10g of butyl titanate was slowly added dropwise, After the dropwise addition, close the separatory funnel, reflux until no more water droplets hang on the inner wall of the distillation column, cool to room temperature, and distill off the solvent at about 35°C to obtain 214.2 g of mercaptoethyl isooctanoate;

[0052] Mix 214.2g of mercaptoethyl isooctanoate, 100g of mercaptoacetic acid and 12g of butyl titanate in a three-necked flask equipped with a thermometer, a stirrer and a reflux device, stir, heat to 110°C, and keep the vacuum at -0.075~- 0.90MPa, reacted for 3 hours, no more water dripped out of the water separator, cooled to room temperature, washed with water, took out the oil phase, and dehydrated by distillation under reduced pressure to ...

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Abstract

The invention discloses methyl tin reverse thioester. The methyl tin reverse thioester is prepared by the following steps: mixing mercaptoethyl isooctoate, a catalyst and mercaptoacetic acid; stirring and heating to the temperature of between 70 and 150 DEG C; reacting in a condition that the vacuum degree is between minus 0.06 and minus 0.09MPa; reacting until no water drips from a water segregator; cooling to room temperature, cleaning with water to receive an oil phase; distilling and dehydrating in reduced pressure to obtain a thioester compound; stirring and mixing the thioester compound, methyl tin chloride and water, heating to the temperature of between 60 and 80 DEG C, and adding inorganic base to regulate the pH value to be 6 to 8; stirring to react for 4 to 6 hours, cleaning with water after the reaction is completed; filtering, and distilling filtrate in reduced pressure to prepare the methyl tin reverse thioester, wherein the methyl tin chloride is methyltin trichloride, dimethyltin dichloride or mixture of methyltin trichloride and dimethyltin dichloride. The methyl tin reverse thioester provided by the invention can be used as a vinyl halide resin thermal stabilizer.

Description

(1) Technical field [0001] The invention relates to a methyl tin retrothioester and a preparation method thereof. In particular, it relates to a methyl tin reverse thioester heat stabilizer for polyvinyl chloride (PVC) and a preparation method thereof. (2) Background technology [0002] Mercaptan methyl tin heat stabilizer is widely used in the processing of sheets, plates, pipes and hollow injection molding products due to its excellent stability, compatibility and weather resistance, and has an unshakable leading position in the field of heat stabilizers . [0003] As early as the 1970s, Morton Chemical Company of the United States developed dimethyl tin bis (isooctyl thioglycolate), namely TM ~ 181FS, which uses methyl tin chloride and isooctyl thioglycolate as raw material intermediates. It is prepared by Grignard reagent method, and the specific steps are described in detail in US3810868, US3887519 and US351966. At present, domestic manufacturers have improved their ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/22C08K5/57C08L27/06
Inventor 高尔金周天红唐伟瞿英俊王志勇孟建新陈建军
Owner ZHEJIANG HIMPTON NEW MATERIAL
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