A kind of synthetic method of high molecular weight polycarbonate and its catalyst and application

A synthesis method and technology of polycarbonate, applied in the field of synthesis of high-molecular-weight polycarbonate, can solve the problems of poor quality of synthetic polymers and cumbersome process, and achieve moderate strength of surface basic sites, wide application range and abundant quantity Effect

Active Publication Date: 2020-03-27
CHENGDU ORGANIC CHEM CO LTD CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The object of the present invention is to provide a method for synthesizing high-quality polycarbonate more simply, conveniently and efficiently, aiming at the disadvantages of cumbersome process and poor quality of synthetic polymers in the two-step transesterification polycondensation method for synthesizing polycarbonate

Method used

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  • A kind of synthetic method of high molecular weight polycarbonate and its catalyst and application
  • A kind of synthetic method of high molecular weight polycarbonate and its catalyst and application
  • A kind of synthetic method of high molecular weight polycarbonate and its catalyst and application

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Experimental program
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Effect test

Embodiment 1

[0038] MgO was synthesized by co-precipitation method: Mg(NO 3 ) 2 .6H 2 O was dissolved in deionized water to make a uniform solution with a molar concentration of metal ions of 1.0 mol / L. Then 1.0mol / L Na 2 CO 3 Slowly added dropwise to the above mixed solution. Adjust the pH value of the precipitation mother liquor to 9.5, filter after aging for 12.0 hours, and roast the obtained white precipitate at 450° C. for 4.0 hours to obtain MgO.

[0039] Be that diphenyl carbonate and 1,4-butanediol that molar ratio is 1:1, and catalyst MgO join in the reactor, and wherein MgO consumption is reaction mass gross weight (being diphenyl carbonate and 1,4-butane 0.1‰ of the weight sum of diols), in N 2 After dissolving at 120°C in the atmosphere, stir rapidly for 0.5h. Then reduce the pressure of the reaction system to 100 Pa, and raise the reaction temperature to 200°C for 2.5 hours to obtain the aliphatic polycarbonate. The obtained product is a white solid, which can be seen ...

Embodiment 2

[0041] The preparation method of MgO is with embodiment 1.

[0042] Diphenyl carbonate and bisphenol A with a molar ratio of 0.95:1, and catalyst MgO are added to the reactor, wherein the MgO consumption is 0.08‰ of the total weight of the reaction material, at N 2 Rapid stirring was carried out at 120° C. for 20 min in the atmosphere. Then the pressure of the reaction system was reduced to 50 Pa, and then the reaction temperature was raised to 260° C. for 1.0 hour to stop the reaction, and the obtained white polymer was aromatic polycarbonate. The molecular weight M of the polymer was tested by gel chromatography w =8 000, the yield was 94%.

Embodiment 3

[0044] Mg(OAc) 2 Directly placed at 500°C and calcined for 6.0h to obtain MgO as a catalyst.

[0045] Add diphenyl carbonate and 1,4-butanediol with a molar ratio of 1:1, and catalyst MgO into the reactor, wherein the amount of catalyst used is 0.1‰ of the total weight of the reaction material, at N 2 After dissolving at 120°C in the atmosphere, stir rapidly for 0.5h. Then reduce the pressure of the reaction system to 100 Pa, and raise the reaction temperature to 220°C for 2.5 hours to obtain the aliphatic polycarbonate. The molecular weight M of the polymer was tested by gel chromatography w =29300, corresponding to a yield of 93.8%.

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Abstract

The invention relates to a method for synthesizing high-molecular-weight polycarbonate and its catalyst and application in the technical field of polymer synthesis. The method of the invention is a method for synthesizing high-molecular-weight polycarbonate by taking diphenyl carbonate and glycol as raw materials through one-step melt transesterification polycondensation reaction. This method can be widely used in aliphatic polycarbonate, aromatic polycarbonate, isosorbide-based polycarbonate and tricyclodecane dimethanol-based polycarbonate. After the transesterification polycondensation reaction is completed, the catalyst can be directly left in the polymer as an inorganic filler without separation and subsequent treatment. The catalyst is selected from metal oxides and / or composite oxides of metal and aluminum, wherein the metal is selected from at least one of alkaline earth metals and zinc. Compared with the existing homogeneous catalyst systems such as titanium base, transition metal salt and strong base, the catalyst adopted in the invention has the advantages of simple preparation method, low toxicity, good color of the synthesized polymer and no catalyst separation process.

Description

technical field [0001] The invention relates to the technical field of polymer synthesis, and more particularly, relates to a synthesis method of high molecular weight polycarbonate and its catalyst and application. Background technique [0002] Aromatic polycarbonate (PC) synthesized by phosgene method using bisphenol A as raw material has been widely used in the fields of automobile manufacturing, aerospace and medical equipment as engineering plastics, and has become the fastest growing among the five major engineering plastics General engineering plastics. With the improvement of people's awareness of environmental protection, the process of synthesizing PC through transesterification polycondensation process using dimethyl carbonate (DMC) or diphenyl carbonate (DPC) as carbonyl source and bisphenol A as raw material has begun to be applied to industrial production process. . Referring to this process, the technical route of synthesizing aliphatic polycarbonates (APCs)...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G64/30C08K3/22C08K3/26
CPCC08G64/305C08G64/307C08K3/22C08K3/26C08K2003/222
Inventor 王公应王自庆杨先贵刘绍英李建国
Owner CHENGDU ORGANIC CHEM CO LTD CHINESE ACAD OF SCI
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