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Method for preparing polycarbonate through catalysis of binuclear ionic liquid

A technology of ionic liquid and polycarbonate, which is applied in clean catalysis and green fields, can solve the problems that cannot be applied to the field of PC synthesis, cannot promote molecular chain condensation, and the catalyst has no reactivity.

Active Publication Date: 2021-03-12
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there are few reports on the synthesis of PC from dicationic ionic liquids. Patent document CN201010503499.X reports a sulfonic acid dinuclear imidazole-based ionic liquid and its catalytic method for preparing butylene succinate. Ionic liquids cannot be used in the field of PC synthesis due to the inability to promote the condensation of molecular chains in the polycondensation stage, resulting in a catalyst that is basically inactive.

Method used

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  • Method for preparing polycarbonate through catalysis of binuclear ionic liquid
  • Method for preparing polycarbonate through catalysis of binuclear ionic liquid
  • Method for preparing polycarbonate through catalysis of binuclear ionic liquid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0064] At room temperature, 10.70 g (50 mmol) of diphenyl carbonate (hereinafter referred to as "DPC") and 7.35 g (50 mmol) of isosorbide (hereinafter referred to as "ISO") were added to a 250 ml four-necked flask (ISO The molar ratio with DPC is 1:1), pass into nitrogen protection, heat up to 130°C and add catalyst bis-(3-methyl-1-imidazole)-ethylene bromide (isosorbide 1.5×10 moles of alcohol -5 ), the prepolymerization stage was kept at 130°C for 3h under normal pressure. The polycondensation stage reduces the pressure in the reactor to 1×10 -5 Mpa gradually raised the reaction temperature to 240° C., and continued the reaction for 15 minutes.

[0065] Concrete reaction formula is as follows, and the productive rate that obtains product A through calculation is 99%, and characterization analysis obtains that product A weight average molecular weight is 89800g / mol, and glass transition temperature is (T g )173℃, thermal decomposition temperature is (T d5％ ) 328°C.

[00...

Embodiment 2

[0068] Same as Example 1, except that the catalyst is bis-(3-methyl-1-imidazole)-propylene bromide, other conditions remain unchanged. The productive rate that obtains product A through calculation is 97%, and characterization analysis obtains product A weight-average molecular weight to be 82600g / mol, T g 172°C, T d5％ is 325°C.

Embodiment 3

[0070] Same as Example 1, except that the catalyst is bis-(3-methyl-1-imidazole)-butylene bromide, other conditions remain unchanged. The productive rate that obtains product A through calculation is 98%, and characterization analysis obtains product A weight-average molecular weight to be 84500g / mol, T g 169°C, T d5％It is 321°C.

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Abstract

The invention provides a method for preparing polycarbonate through catalysis of a binuclear ionic liquid, which comprises the following steps: by using a dihydroxy compound and a diester carbonate asraw materials, adding the raw materials into a reactor according to the molar ratio of (1: 0.9)-(1: 8), and synthesizing polycarbonate by using binuclear imidazolyl ionic liquid as a catalyst througha melt transesterification method under the protection of inert gas. Compared with literature reports, the weight-average molecular weight of the synthesized polycarbonate reaches 5 * 10 < 4 >-16 * 10 < 4 > g / mol, the transesterification time is shortened by 25%-50%, and the polycondensation time is shortened by 20%-40% by regulating the length of an alkyl chain between double imidazole rings andchanging the structure of anions under the synergistic catalytic action of anions and cations.

Description

technical field [0001] The invention relates to the field of green and clean catalysis, in particular to a method for preparing polycarbonate by catalyzing a binuclear ionic liquid. Background technique [0002] The catalysts currently used for the synthesis of polycarbonate are mainly organic base catalysts and metal catalysts. Among them, representative organic base catalysts include: 4-methylaminopyridine (CN102341363), triphenyl phosphite (CN103080201) and the like. Metal catalysts include alkali metal catalysts and alkaline earth metal catalysts. Such as sodium bicarbonate (JournalOf Applied Polymer Science: 2010, 134(30), 3658-3667; CN110461942), cesium carbonate (CN104094142), calcium acetate (CN107108873), zinc acetate (RSC ADVANCES, 2015, 5, 87311–87319) Wait. Compared with organic base catalysts, metal catalysts have higher reactivity, and the molecular weight of the synthesized polycarbonate is higher. However, metal catalysts often cause discoloration of prod...

Claims

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Application Information

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IPC IPC(8): C08G64/30
CPCC08G64/305C08G64/307
Inventor 徐菲王卫卫张锁江杨子锋张振才方文娟何宏艳
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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