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Preparation method of intermediate dimethoxy carbonic acid bisphenol A diester

A technology of dimethoxycarbonic acid bisphenol and intermediates, which is applied in the field of preparation of fine chemical intermediates, can solve the problems of low DmC selectivity and yield, unfavorable large-scale production, increase of polycondensation temperature and the like, and achieves short reaction time. , less by-products, good overall performance of polyester

Active Publication Date: 2012-05-09
TIANJIN POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although phenol can be effectively separated under high vacuum conditions, the polycondensation temperature still needs to be raised to 200-300°C
(2) The oxidative carbonylation method of bisphenol A (BPA): the oxidative carbonylation method of BPA and CO is also a method for non-phosgene synthesis of polycarbonate, but the PC molecular weight synthesized by this method is generally very low, according to literature reports , Mw can reach up to 5600, which is not conducive to large-scale production
DmC(1) is usually prepared by transesterification of DMC and BPA, due to the low selectivity and yield of DmC(1)

Method used

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  • Preparation method of intermediate dimethoxy carbonic acid bisphenol A diester
  • Preparation method of intermediate dimethoxy carbonic acid bisphenol A diester
  • Preparation method of intermediate dimethoxy carbonic acid bisphenol A diester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Feeding: DMC / BPA / (Ar) 2SnO=4mol / 1mol / 1.2g, react in an autoclave, replace the air in the autoclave with nitrogen, react at 220°C for 12 hours, and stir at a speed of 150R / Min. After the reaction is completed, the catalyst is filtered, and the excess DMC and by-product methanol are distilled off to obtain a white powder with a yield higher than 92%. Gained white powder is dissolved in the mixed liquid of methanol and water at 65 DEG C, the volume ratio of alcohol and water is controlled at 1: 1, and the colorless massive solid that cools out is the intermediate DmC (1) that the present invention seeks, The product purity is higher than 99.8%, and the yield is higher than 90%.

Embodiment 2

[0026] Feeding: DMC / BPA / (Ph) 2 SnO=8mol / 1mol / 8g, react in an autoclave, replace the air in the autoclave with nitrogen, react at 220°C for 6 hours, and stir at a speed of 100R / Min. The crude product recovery process is the same as in Example 1, and the yield is higher than 96%; the obtained white powder is dissolved in a mixture of methanol and water at 70°C, and the volume ratio of alcohol to water is controlled between 1:2, and a colorless block is precipitated after cooling The solid is DmC (1), the product purity is higher than 99.8%, and the yield is higher than 93%.

Embodiment 3

[0028] Feeding: DMC / BPA / (Ph) 2 SnO=12mol / 1mol / 6g, using atmospheric pressure kettle reaction, adopting the method of adding DMC dropwise to the BPA melt, the by-product methanol will be distilled after the reaction, and the reaction temperature is controlled at 200°C, the reaction is 8 hours, and the stirring speed is 150R / Min. The crude product recovery and recrystallization process are the same as in Example 1, the crude product yield is higher than 85%, the product purity is higher than 99.8%, and the recrystallization product yield is higher than 80%.

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Abstract

The invention discloses a preparation method of an intermediate dimethoxy carbonic acid bisphenol A diester. The intermediate is used for synthesis of polycarbonate. The preparation method is characterized in that DMC micromolecular carbonic ester and BPA are used as raw materials to react in the presence of an organo tin catalyst at the temperature of 140-250 DEG C and at normal pressure or high pressure for 0.5-48h so as to obtain a crude intermediate product; and the high-purity polycarbonate intermediate is prepared by an alcohol / water mixed solvent recrystallization method. The organo tin catalyst comprises (Ar)2SnX2, (Ar)2Sn(OH)X, (Ar)2SnO, R(Ph)SnO, R2SnX2, R2Sn(OH)X or R2SnO. The feed mole ratio of DMC to BPA is 2-20. The mass ratio of the organo tin catalyst to bisphenol A is 5 per thousand-10%. The alcohol / water mixed volume ratio is 1-3.

Description

technical field [0001] The invention relates to the preparation technology of fine chemical intermediates, in particular to a preparation method of the intermediate dimethoxycarbonic acid bisphenol A diester. This intermediate is used in the synthesis of polycarbonate. Background technique [0002] Polycarbonate (Polycarbonate, abbreviated as PC) is a colorless and transparent amorphous thermoplastic material. PC has the advantages of heat resistance, impact resistance, flame retardancy, transparency and excellent mechanical properties, so it has been widely used in glass assembly industry, automobile industry, electronic and electrical industry, office equipment, medical care, film and protective equipment. At present, PC at home and abroad is mainly prepared by the phosgene method. The phosgene method uses dichloromethane as a solvent, bisphenol A (BPA) and phosgene as raw materials, and reacts in the presence of NaOH. The products produced by this method are of high qu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/96C07C68/06C08G64/30
Inventor 李振环程博闻苏坤梅明军
Owner TIANJIN POLYTECHNIC UNIV
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