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Method for synthesizing high-molecular-weight aliphatic polycarbonate

A polycarbonate and high molecular weight technology, applied in the field of high molecular weight aliphatic polycarbonate, can solve the problems of low raw material utilization rate, harsh reaction conditions, DMC loss, etc., achieve low production cost, less usage, and reduce equipment cost Effect

Active Publication Date: 2013-07-17
CHANGZHOU INST OF CHEM +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] CN101643542A discloses that dimethyl carbonate (DMC) and aliphatic dihydric alcohol transesterification method have synthesized the aliphatic polycarbonate of high molecular weight, but this reaction condition is harsh, and the DMC boiling point of one of raw material is lower, can be mixed with methanol Boiling, so under the reaction conditions, DMC is easy to volatilize and lose from the reactor, and the utilization rate of raw materials is low; diethyl carbonate (DEC) and aliphatic glycol transesterification method DEC will not azeotrope with ethanol, and ethanol Non-toxic, but DEC can enter the body through the gastrointestinal tract, skin and respiratory tract, showing moderate toxicity
Bayer company once proposed to utilize the method for subsection polymerization to improve the molecular weight (CN 1454915A) of polymer, but did not obtain ideal result, the molecular weight of the polymer prepared is all less than 100000g / mol, and this process route is longer, and energy consumption is higher high

Method used

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  • Method for synthesizing high-molecular-weight aliphatic polycarbonate
  • Method for synthesizing high-molecular-weight aliphatic polycarbonate
  • Method for synthesizing high-molecular-weight aliphatic polycarbonate

Examples

Experimental program
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Effect test

Embodiment 1

[0033] Under normal pressure, add 118g 1,4-butanediol, 215g diphenyl carbonate, and 0.1g zinc sulfate into a reactor equipped with heating and stirring system, temperature measurement system and fractionation system, and stir under nitrogen atmosphere. The temperature was gradually raised to 170°C, the by-product phenol was fractionally distilled out in time, and the reaction was refluxed for 2 hours until the by-product phenol was no longer distilled, and 0.001 g of stabilizer antioxidant 1010 was added. Then, the pressure of the system was gradually reduced to 1000Pa. After a certain time of reaction, the reaction temperature of the system was gradually increased to 190℃, and the pressure of the system was reduced to 100Pa. The polycondensation was carried out for 5h. The milky white solid was finally obtained as aliphatic polycarbonate with number average molecular weight. It is 62900g / mol and the intrinsic viscosity is 1.11dl / g. The aliphatic polycarbonate 1 The H-NMR spect...

Embodiment 2

[0035] Under normal pressure conditions, 130g 1,4-butanediol, 215g diphenyl carbonate, and 1.05g zinc chloride were added to a reactor equipped with a heating and stirring system, a temperature measurement system, and a fractionation system. Under a nitrogen atmosphere Stir and gradually raise the temperature to 200°C, fractionate the by-product phenol in time, reflux for 5 hours, until the by-product phenol no longer distills, add 0.001g stabilizer antioxidant 1010. Then, the pressure of the system was gradually reduced to 700Pa. After a certain time of reaction, the reaction temperature of the system was gradually increased to 210°C, and the pressure of the system was reduced to 30Pa. The polycondensation was carried out for 10 hours. The white solid was finally obtained as aliphatic polycarbonate with number average molecular weight. It is 209200g / mol, and the intrinsic viscosity is 1.89dl / g.

Embodiment 3

[0037] Under normal pressure conditions, 150g of 1,4-butanediol, 215g of diphenyl carbonate, and 0.5g of zinc stearate were added to a reactor equipped with a heating and stirring system, a temperature measurement system, and a fractionation system. In a nitrogen atmosphere Under stirring and gradually raising the temperature to 140°C, the by-product phenol was fractionally distilled in time, and the by-product phenol was refluxed for 6 hours until the by-product phenol was no longer distilled, and 0.001 g of stabilizer antioxidant 1010 was added. Then, the pressure of the system was gradually reduced to 2000Pa. After a certain time of reaction, the reaction temperature of the system was gradually increased to 210℃, and the pressure of the system was reduced to 30Pa. The polycondensation was carried out for 6h. The milky white solid was finally obtained as polycarbonate with a number average molecular weight of 113500g. / mol, the intrinsic viscosity is 1.54dl / g.

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Abstract

The invention discloses a method for synthesizing high-molecular-weight aliphatic polycarbonate through a trans-esterification method. The invention relates to a multi-stage trans-esterification reaction of aliphatic or alicyclic diol and diphenyl carbonate, and the high-molecular-weight aliphatic polycarbonate is formed by condensation during a process for removing a reaction byproduct phenol. Through the regulation upon the diol type or the ratio of mixed diol, polycarbonates with different structures can be obtained. The method provided by the invention has the advantages of simple preparation method, short reaction time, low catalyst dose, good product color, high device utilization rate, reduced production cost, and low pollution. The byproduct phenyl can be recycled and reused. Therefore, possibilities are provided for large-scale production and application of polycarbonate synthesized through the trans-esterification method. With the method, the obtained high-molecular-weight aliphatic polycarbonate is white solid with good heat resistance. The high-molecular-weight aliphatic polycarbonate can be completely biodegraded, and can be used as raw materials in polyurethane or polyester elastomer preparations, packaging material in food industries, additive in rubber industries, and medicine sustained-release agent, sutures lines, and bone fixation materials in the medical field.

Description

Technical field [0001] The invention relates to a high molecular weight aliphatic polycarbonate, and relates to a method for preparing high molecular weight aliphatic polycarbonate by transesterification condensation of diphenyl carbonate and aliphatic or alicyclic polyhydric alcohol. Background technique [0002] Aliphatic polycarbonate (APC) is an important part of polyester polymer. It is a kind of surface erosion material, which can be completely biodegradable, has good physical and mechanical properties, dielectric properties and biocompatibility, and There are many types, by changing the main chain chemical structure and introducing side chain functional groups, the polymer can have a wide range of physical, chemical and biological properties to meet different needs. In addition, because it is rich in carbon dioxide units, the heat of combustion is significantly lower than other polymers, and the flame retardancy is good. It can be gradually degraded into neutral glycol an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G64/38C08G64/30
Inventor 李会玲吴集钱贾树勇王公应蒋琪
Owner CHANGZHOU INST OF CHEM
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