Method for preparing polycarbonate under catalysis of ionic liquid

A technology of ionic liquid and polycarbonate, which is applied in the field of catalyzed preparation of polycarbonate by ionic liquid, which can solve problems such as toxicity, limited application, and environmental pollution

Active Publication Date: 2021-05-18
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, these catalysts have certain toxicity, which may not only cause environmental pollution, but also remain in the synthetic

Method used

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  • Method for preparing polycarbonate under catalysis of ionic liquid
  • Method for preparing polycarbonate under catalysis of ionic liquid
  • Method for preparing polycarbonate under catalysis of ionic liquid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0063] In this example, isosorbide and dimethyl carbonate are used as raw materials to prepare a polycarbonate under the catalysis of amide ionic liquid, and the reaction formula is as follows:

[0064]

[0065] The preparation method comprises the following steps:

[0066] (1) Transesterification stage: under nitrogen atmosphere and normal pressure, add 7.3g (0.05mol) isosorbide, 22.5g (0.25mol) dimethyl carbonate and tetrabutylphosphorus phthaloyl to the reaction flask Imine (0.0005mol, 0.2025g), react the reaction mixture at 160°C for 2h, then slowly raise the temperature to 180°C, react for 0.5h, volatilize the unreacted dimethyl carbonate and low boiling point product methanol, and obtain the prepolymer ;

[0067] (2) Polycondensation stage: the temperature in step (1) is raised from 180°C to 250°C, the vacuum is slowly reduced to 50Pa, and the reaction is carried out for 1.5h to obtain the product isosorbide polycarbonate;

[0068] Molecular weight test: The GPC tes...

Embodiment 2

[0072] The difference between this example and example 1 is that the catalyst used is tetrabutylphosphoglutarimide (0.0005mol, 0.1855g), and other conditions are exactly the same as those of example 1.

[0073] Molecular weight test: The GPC test result of the product shows that the number average molecular weight of polycarbonate M n 22000g / mol, weight average molecular weight M w It is 37000g / mol.

[0074] Thermal performance test: The DSC test results of the product show that the glass transition temperature T of polycarbonate g It is 163°C.

[0075] NMR test: methylation selectivity 0.7%, methyl esterification selectivity 99.3%.

Embodiment 3

[0077] The difference between this example and Example 1 is that the catalyst used is tetrabutylphosphine hexahydrophthalimide (0.0005mol, 0.2055g), and other conditions are exactly the same as those of Example 1.

[0078] Molecular weight test: The GPC test result of the product shows that the number average molecular weight of polycarbonate M n 20000g / mol, weight average molecular weight M w It is 33000g / mol.

[0079] Thermal performance test: The DSC test results of the product show that the glass transition temperature T of polycarbonate g is 160°C.

[0080] NMR test: methylation selectivity 1.3%, methyl esterification selectivity 98.7%.

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Abstract

The invention relates to a method for preparing polycarbonate through catalysis of an ionic liquid. The method comprises the following step: carrying out a melt polymerization reaction on diester carbonate and a dihydroxy compound under the action of an amide ionic liquid catalyst to generate polycarbonate. According to the method disclosed by the invention, the amide ionic liquid catalyst with high catalytic activity, good selectivity and excellent thermal stability is obtained by taking an amide-containing compound as an anion and tetraalkylphosphorus as a cation, and polycarbonate with a large molecular weight and a high glass-transition temperature is obtained through catalysis. The method disclosed by the invention is mild in reaction condition, designable in catalyst structure and relatively high in reaction rate; a solvent is not needed in the reaction process, virulent phosgene is not used, and environmental pollution is avoided; and a product obtained by the reaction is free of catalyst residue and toxic substances, and the method is a green and environment-friendly low-cost polycarbonate preparation process.

Description

technical field [0001] The invention belongs to the technical field of polymer preparation, and relates to a method for preparing polycarbonate by catalyzing an ionic liquid. Background technique [0002] Polycarbonate (PC) is a high-performance polymer containing carbonate groups in its molecular chain. Due to its special structure, it has good transparency, excellent dimensional stability and outstanding impact resistance. It is widely used in optical components, electronic appliances, auto parts, building materials, aerospace and other fields, and is the thermoplastic engineering plastic with the fastest growing demand among the five major engineering plastics. However, currently commonly used polycarbonate not only needs to be prepared by using petrochemical product bisphenol A and highly toxic chemical phosgene, but also because its production raw material bisphenol A has estrogen effect and chronic toxic effect, which limits its application in food. Applications in ar...

Claims

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Application Information

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IPC IPC(8): C08G64/30
CPCC08G64/305C08G64/307
Inventor 徐菲方文娟张锁江霍锋杨子锋王卫卫张振才孙玮
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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