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Preparation of methyltin stabiliser

A technology of methyl tin stabilizer and dimethyl tin dichloride, which is applied in the direction of tin organic compounds, can solve the problems of continuous processing and production of unfavorable products, poor mold release, poor lubricity, and easy sticking of batch materials to rolls, etc., to achieve The effect of good product stability, high transparency, and easy production control

Active Publication Date: 2011-09-14
YANGZHOU HATAIKE TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0015] 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%. During the process, 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 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; the cost of methyl tin is mainly due to the relatively high cost of tin, how to reduce the content of tin in the product , enhance the stabilizing effect of methyl tin, and reduce the content of methyl tin in PVC products, which gives us a scientific research direction

Method used

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  • Preparation of methyltin stabiliser
  • Preparation of methyltin stabiliser
  • Preparation of methyltin stabiliser

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] After mixing 118 grams (1mol) of succinic acid (or malonic acid, or glutaric acid) with 172 grams (2.2mol) of 2-mercaptoethanol, add 200 grams of toluene, then add 0.5 grams of p-toluenesulfonic acid to reflux , after completion of the reaction, wash three times with 200ml of water, after drying, evaporate the solvent, extract low-boiling solvent and water under high vacuum, obtain 226 grams of dimercaptoethyl succinate, yield 95%.

[0050]Drop 238 grams (1mol) of dimercaptoethyl succinate into a 1:4 mixed aqueous solution of monomethyltin trichloride: dimethyltin dichloride with a chlorine equivalent of 1 mole, at a temperature of 25 to 40°C , use ammonia solution (or sodium hydroxide solution or sodium bicarbonate solution) to adjust the pH value of the system to 7-8. After esterification, the temperature was 40-60°C for 4 hours. After the reaction, the water phase was separated, and the organic phase was washed 3 times with 300 grams of water. The water phase was sep...

Embodiment 2

[0054] After mixing 146 grams (1mol) of adipic acid with 148 grams (1.9mol) of 2-mercaptoethanol (or 3-mercaptopropanol, 2-methyl-2-mercaptoethanol, or 4-mercaptobutanol), add 200 grams Toluene (or sherwood oil or n-hexane or hexanaphthene or chloroform or benzene), then add 2 grams of benzenesulfonic acid or methanesulfonic acid) backflow, after completion of the reaction, wash three times with 200ml water, after drying, evaporate the solvent, The low-boiling point solvent and water were extracted under high vacuum to obtain 250 g of dimercaptoethyl adipate, with a yield of 94%.

[0055] Add 266 grams (1 mol) of dimercaptoethyl adipate dropwise into a 1:6 mixed aqueous solution of monomethyl tin trichloride: dimethyl tin dichloride with a chlorine equivalent of 1 mole at a temperature of 0 to 30°C , use ammonia solution (or sodium hydroxide solution or sodium bicarbonate solution) to adjust the pH value of the system to 7-8. After esterification, the temperature was 60-90°C ...

Embodiment 3

[0059] After mixing 146 grams (1mol) of adipic acid with 312 grams (4mol) of 2-mercaptoethanol (or 2-methyl-2-mercaptoethanol, or 4-mercaptobutanol), add 400 grams of n-hexane or cyclohexane or Chloroform or benzene), then add 5 grams of benzenesulfonic acid or methylsulfonic acid) to reflux, after the reaction is complete, wash three times with 200ml of water, after drying, evaporate the solvent, and extract the low-boiling solvent and water under high vacuum to obtain 250 grams of hexane Dimercaptoethyl diacid, yield 94%.

[0060] Add 266 grams (1 mol) of dimercaptoethyl adipate dropwise into a 1:2 mixed aqueous solution of monomethyl tin trichloride: dimethyl tin dichloride with a chlorine equivalent of 1 mole, at a temperature of 0 to 30°C , use ammonia solution (or sodium hydroxide solution or sodium bicarbonate solution) to adjust the pH value of the system to 7-8. After esterification, the temperature was 60-90 °C for 6 hours. After the reaction, the water phase was se...

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Abstract

The invention provides a methyl tin stabilizer and a method for preparing the same and relates to the technical field of organic chemistry. The method comprises: in the presence of a catalyst, mixing and refluxing an alkyl diacid, mercaptoethanol and a solvent; after the reaction finishes, washing the solution with water and obtaining a dimercaptoester; and adding the obtained dimercaptoester into an aqueous solution of methyltin trichloride or / and dimethyltin dichloride, adjusting the pH value of the system by using an alkaline solution, carrying out an pre-esterification reaction before heat preservation, heating for carrying out a post-esterification reaction, washing an organic phrase after the reaction finishes, separating the organic phrase from a water phrase, carrying out vacuum water removal and obtaining the methyl tin stabilizer. The methyl tin stabilizer has high transparency, weather resistance, compatibility, pressure analysis, non-toxicity, excellent high-temperature stability and low tin content. The low tin-content methyl tin has higher thermal stability than the prior methyl tin, so final PVC products can achieve the same stability with even smaller amount of added methyl tin stabilizer, the use of tin is reduced and the production costs of terminal clients are reduced at last.

Description

technical field [0001] The invention relates to the technical field of organic chemical industry, in particular to the technical field of organotin heat stabilizer used for preparing polyvinyl chloride. Background technique [0002] Polyvinyl chloride (PVC) has excellent corrosion resistance, flame retardancy and high mechanical properties, and because of its low price, rich sources of raw materials, and mature manufacturing technology, its products are widely used in light industry, machinery, electronics, construction, textiles, It is an ideal substitute for steel and wood in industries such as aviation, medicine and food packaging. [0003] Since the polyvinyl chloride structure contains double bonds, branch points, and initiator residues, it will be degraded with the dehydrochlorination reaction when heated to 100°C. molecular crosslinking. In order to minimize the loss of chemical and physical properties of PVC during processing, it is necessary to add some chemical s...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/22C08K5/58
Inventor 江以桦张业武成贞辉赵根根李艳军
Owner YANGZHOU HATAIKE TECH
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