Unlock instant, AI-driven research and patent intelligence for your innovation.

A kind of method of synthesizing high molecular weight aliphatic polycarbonate

A high-molecular-weight polycarbonate technology, applied in the field of high-molecular-weight aliphatic polycarbonate, can solve the problems of low raw material utilization, harsh reaction conditions, and long process routes, and achieve low production costs, less usage, and simplified processes The effect of the route

Active Publication Date: 2015-12-02
CHANGZHOU INST OF CHEM +1
View PDF5 Cites 1 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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 of staged polymerization to improve the molecular weight of polymer (CN1454915A), but did not obtain ideal result, the molecular weight of the prepared polymer is all less than 100000g / mol, and this process route is longer, and energy consumption is higher

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • A kind of method of synthesizing high molecular weight aliphatic polycarbonate
  • A kind of method of synthesizing high molecular weight aliphatic polycarbonate
  • A kind of method of synthesizing high molecular weight aliphatic polycarbonate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Under normal pressure, add 118g of 1,4-butanediol, 215g of diphenyl carbonate, and 0.1g of zinc sulfate into a reactor equipped with a heating and stirring system, a temperature measuring system and a fractionation system, and stir under a nitrogen atmosphere And gradually raise the temperature to 170°C, distill out the by-product phenol in time, reflux for 2 hours, until the by-product phenol no longer distills out, add 0.001g of stabilizer antioxidant 1010. Then, gradually reduce the system pressure to 1000Pa. After a certain period of reaction, gradually increase the system reaction temperature to 190°C, reduce the system pressure to 100Pa, polycondensate for 5 hours, and finally obtain a milky white solid that is aliphatic polycarbonate. It is 62900g / mol, and the intrinsic viscosity is 1.11dl / g. The aliphatic polycarbonate 1 The H-NMR spectrum is attached figure 1 As shown, the FT-IR spectrum is attached figure 2 Shown, GPC characterization see attached image ...

Embodiment 2

[0035] Under normal pressure conditions, 130g of 1,4-butanediol, 215g of diphenyl carbonate, and 1.05g of zinc chloride were added to a reactor equipped with a heating and stirring system, a temperature measuring system and a fractionation system, and the Stir and gradually raise the temperature to 200°C, fractionally distill out the by-product phenol in time, and reflux for 5 hours until the by-product phenol no longer distills out, then add 0.001g of stabilizer antioxidant 1010. Then, gradually reduce the system pressure to 700Pa, after a certain period of reaction, gradually increase the system reaction temperature to 210 ° C, reduce the system pressure to 30Pa, polycondensate for 10 hours, and finally obtain a white solid that is aliphatic polycarbonate, its number average molecular weight It is 209200g / mol, and the intrinsic viscosity is 1.89dl / g.

Embodiment 3

[0037] Under normal pressure, 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 measuring system, and a fractionation system. Stir under low temperature and gradually raise the temperature to 140°C, distill out the by-product phenol in time, reflux for 6 hours, until the by-product phenol no longer distills out, add 0.001g of stabilizer antioxidant 1010. Then, gradually reduce the system pressure to 2000Pa, after a certain period of reaction, gradually increase the system reaction temperature to 210°C, reduce the system pressure to 30Pa, polycondensate for 6 hours, and finally obtain a milky white solid, which is polycarbonate, and its number average molecular weight is 113500g / mol, the intrinsic viscosity is 1.54dl / g.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

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 through 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, can be completely biodegradable, has good physical and mechanical properties, dielectric properties and biocompatibility, and There are many kinds. By changing the chemical structure of the main chain 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, due to the rich carbon dioxide units, the heat of combustion is significantly lower than other polymers, and the flame retardancy is good. And it can undergo hydrolysis, alcoholysis and...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(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