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Preparation method based on citric acid for copolycarbonate

A technology of copolycarbonate and citric acid, which is applied in the fields of renewable resource utilization and green synthesis, can solve problems such as restricting the application of renewable resources, and achieve the effect of green environmental protection synthesis method, reduction of dependence on petroleum resources, and good rigidity.

Inactive Publication Date: 2020-02-11
TIANJIN UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there has been no report on the synthesis of copolycarbonates using derived monomers derived from citric acid from renewable resources, thus limiting the application of renewable resources in the production of copolycarbonates.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] A preparation method of citric acid-based copolycarbonate, using citric acid and diphenyl carbonate as raw materials, using lithium acetylacetonate as a catalyst, and realizing bulk polymerization at a temperature of 200-230°C and a vacuum condition of 0.5-0.8mbar , including the following steps.

[0029] (1) Add 60g (0.60mol) of concentrated sulfuric acid to a round-bottomed flask, slowly add 14g of citric acid under ice-cooling, slowly heat up to 30°C within 8h, react for 18h, add 40mL of dichloromethane under ice-bath conditions, and Add 40mL of methanol below ℃, stir at room temperature for 12h, then add 240mL of ice water, stir for 0.5h, let stand to separate, keep the organic phase, extract the water layer with 3×40mL dichloromethane, combine the organic layer, rotary evaporate, and reduce pressure Distillation gives dimethyl acetone dicarboxylate. 30 g (0.172 mol) of the obtained dimethyl acetone dicarboxylate was slowly added to 125 mL of methanol solution in w...

Embodiment 2

[0032] A preparation method of citric acid-based copolycarbonate, using citric acid and diphenyl carbonate as raw materials, using lithium acetylacetonate as a catalyst, and realizing bulk polymerization at a temperature of 200-230°C and a vacuum condition of 0.5-0.8mbar , including the following steps.

[0033] (1) Add 60g (0.60mol) of concentrated sulfuric acid into a round bottom flask, slowly add 14g of citric acid under ice bath, slowly heat up to 30°C within 8h, react for 18h, add 40mL of dichloromethane under ice bath conditions, Next, 40 mL of methanol was added and stirred at room temperature for 12 h. Then add 240mL of ice water, stir for 0.5h, let stand to separate layers, keep the organic phase, extract the water layer with 3×40mL dichloromethane, combine the organic layers, rotary evaporate, and distill under reduced pressure to obtain dimethyl acetone dicarboxylate. 30 g (0.172 mol) of the obtained dimethyl acetone dicarboxylate was slowly added to 125 mL of met...

Embodiment 3

[0036] A preparation method of citric acid-based copolycarbonate, using citric acid and diphenyl carbonate as raw materials, using lithium acetylacetonate as a catalyst, and realizing bulk polymerization at a temperature of 200-230°C and a vacuum condition of 0.5-0.8mbar , including the following steps.

[0037] (1) Add 60g (0.60mol) of concentrated sulfuric acid into a round bottom flask, slowly add 14g of citric acid under ice bath, slowly heat up to 30°C within 8h, react for 18h, add 40mL of dichloromethane under ice bath conditions, Add 40mL of methanol, stir at room temperature for 12h, then add 240mL of ice water, stir for 0.5h, let stand to separate layers, keep the organic phase, extract the water layer with 3×40mL dichloromethane, combine the organic layer, rotary evaporate, and distill under reduced pressure Dimethyl acetonedicarboxylate is obtained. 30 g (0.172 mol) of the obtained dimethyl acetone dicarboxylate was slowly added to 125 mL of methanol solution in wh...

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PUM

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Abstract

The invention discloses a preparation method based on citric acid for copolycarbonate. The method comprises the following steps: performing a reaction on citric acid and concentrated sulfuric acid toprepare dimethyl acetone dicarboxylate, performing a Weiss-Cook condensation reaction on the dimethyl acetone dicarboxylate and methylglyoxal to prepare an intermediate disodium salt, performing decarboxylation on the intermediate disodium salt by using a mixed solution of glacial acetic acid and hydrochloric acid to prepare 3a-methyltetrahydropenten-2,5(1H,3H)-dione, performing reduction on the 3a-methyltetrahydropenten-2,5(1H,3H)-dione by using sodium borohydride, performing extraction by using trichloromethane, performing methanol recrystallization to obtain 3a-methyloctahydropenten-2,5-diol, and performing bulk polymerization on the 3a-methyloctahydropenten-2,5-diol, diphenyl carbonate and aliphatic diol by using lithium acetylacetonate as a catalyst to obtain the 3a-methyloctahydropenten-2,5-diol copolycarbonate. The synthetic method provided by the invention has a simple process and mild reaction conditions, and the raw materials are environmentally friendly, cheap and easy to obtain.

Description

Technical field: [0001] The invention relates to the technical field of renewable resource utilization and green synthesis, in particular to a preparation method of citric acid-based copolycarbonate. [0002] Background of the invention: [0003] Polycarbonate (BPA-PC) is a thermoplastic engineering plastic with excellent comprehensive properties. It has excellent impact resistance, good dimensional stability, strong heat resistance and cold resistance. It can be used in a wide range of - Used in the temperature range of 100-140°C, it has excellent dielectric properties and good light transmission (the transmittance of visible light can reach 90%). It is the only product with good transparency among the five major engineering plastics, and it is also the growth rate in recent years. The fastest general-purpose engineering plastic. Polycarbonate is widely used in various fields of national economic development, mainly in optics, electronics, automobiles, construction, office ...

Claims

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Application Information

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IPC IPC(8): C08G64/30
CPCC08G64/305
Inventor 杨芷懿庞成才刘福德
Owner TIANJIN UNIVERSITY OF TECHNOLOGY
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