Method for synthesizing esterthio tin stabilizer

A technology of tin ester mercaptide and isooctyl acetate, which is applied in the field of synthesizing tin tin mercaptide to achieve the effects of energy saving, safety in the synthesis process and reduction of possibility

Inactive Publication Date: 2010-05-12
SHANGHAI UNIV OF ENG SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The technical problem to be solved by this invention is to provide a kind of method of synthetic ester group tin mercaptide, to solve the defective in the prior art

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] In a 500ml four-necked flask equipped with a stirring bar, a dropping funnel, and a thermometer, add 52g of methyl acrylate, 0.88g of hydroquinone, and 200ml of a mixed solvent of tetrahydrofuran and chloroform (20ml of tetrahydrofuran), and add it while stirring. 36g Sn powder. After stirring evenly, open the valve of the HCl gas generator, and slowly pass in excess dry hydrogen chloride gas. React at room temperature, and continue to react for 1 hour after the tin powder is completely converted. After the reaction was completed, a small amount of insoluble impurities were removed by suction filtration. The solvent was evaporated under reduced pressure, the solvent was recovered and reused, and the crude product was purified 2 to 3 times. 77 g of bis-(β-methoxyformylethyl)tin dichloride were obtained as a white powder. The conversion of Sn was 100%, and the yield was 70%.

[0037] Product performance: the melting point is 132.3°C, the Sn content is 31.68%, and the ...

Embodiment 2

[0041] In a 500ml four-necked flask equipped with a stirring bar, a dropping funnel, and a thermometer, add 43.6g of butyl acrylate, 0.3g of hydroquinone, and 200ml of tetrahydrofuran and chloroform mixed solvent (60ml of tetrahydrofuran), and add while stirring. 20g Sn powder. After stirring evenly, open the valve of the HCl gas generator, and slowly pass in excess dry hydrogen chloride gas. React at room temperature, and continue to react for 0.5 to 1 hour after the tin powder is completely converted. After the reaction was completed, trace impurities were removed by suction filtration. The solvent was evaporated under reduced pressure, and the solvent was recovered for reuse. 73 g of bis-(β-butoxyformylethyl)tin dichloride was obtained as a colorless transparent liquid. The conversion rate of Sn is 100%, and the yield rate is over 90%. Product performance: Sn content is 25.68%, and the structure of the product is correct as detected by infrared spectrometer and nuclear ...

Embodiment 3

[0043] Product performance test of embodiment 3: the tin content of the product of embodiment 1: 15.98%, the sulfur content: 8.28%; the tin content of the product of embodiment 2 is 14.54%, the sulfur content is 7.71%. Static thermal stability (Congo red method): Add 2phr product to 100phrPVC, appropriate amount of plasticizer and lubricant, plasticize in an open mill for 5min, cut into 2×2×1mm squares, put into a test tube about 5cm, Put a strip of Congo red test paper 2-3cm above the sample, and put the test tube in an oil bath at 190+2°C. The thermal stability time of embodiment 1 product is 61min, and the thermal stability time of embodiment 2 product is 55min; Dynamic thermal stability (rheometer test) and processing stability: add 2phr product in 100phrPVC, plasticizer, lubricant amount , After mixing evenly, put it into the mixing chamber of the rheometer, at 180-190°C, with a rotation speed of 30rpm. The dynamic thermal stability time of embodiment 1 product / PVC syste...

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Abstract

The invention discloses a method for synthesizing esterthio tin stabilizer. Firstly, the bichloride of intermediate compound tin is synthesized, and then the bichloride of tin reacts with isooctyl thioglycolate, phase transfer catalyst, organic solvent and inorganic alkaline solution to synthesize the esterthio tin stabilizer with stable quality and superior performance. The method better solves the problem that the esterthio tin stabilizer under long term standing is easy to deposit, change color, have severe odour and the like, has mild and simple synthesis condition and is easy to realize industrialized production.

Description

technical field [0001] The invention relates to the field of chemical synthesis, in particular to a method for synthesizing ester-based tin mercaptide. Background technique [0002] x-[β-methyl(butyl)oxyformylethyl], y-(isooctyl mercaptoacetate) tin (abbreviated as ester-based tin mercaptide) is a thermal material of PVC and its copolymers that are widely used and have excellent performance. Stabilizer, the synthetic method that U.S. Patent US4080363 proposes is to synthesize intermediate first, and the synthetic of intermediate is to adopt tin powder, methyl acrylate and hydrogen chloride gas as raw material, ether is solvent, reacts in ice-salt bath, after reaction finishes, filter Remove unreacted tin powder, then use CH 3 C1 3 Carry out extraction, obtain intermediate di-(beta-methoxyformyl ethyl) tin dichloride after distilling off solvent; Then intermediate and isooctyl thioglycolate and NaHCO 3 The reaction produces ester-based tin mercaptide. The disadvantage of ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/22B01J31/02C08K5/58
Inventor 张书华
Owner SHANGHAI UNIV OF ENG SCI
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