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Method for preparing polyester by catalyzing cyclic anhydride/epoxide ring opening alternate copolymerization with potassium acetate

A technology of potassium acetate catalyzing cyclic anhydrides and epoxides, which is applied in the field of polyester preparation, can solve the problems of high biological toxicity and high price, and achieve the effects of low biological toxicity, low price and simple preparation method

Active Publication Date: 2020-11-10
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical problem to be solved by the present invention is to use low-cost, non-biotoxic potassium acetate to catalyze the alternating copolymerization of cyclic anhydrides and epoxides to prepare biodegradable polyester materials in view of the high biotoxicity and high price of existing catalytic systems.

Method used

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  • Method for preparing polyester by catalyzing cyclic anhydride/epoxide ring opening alternate copolymerization with potassium acetate
  • Method for preparing polyester by catalyzing cyclic anhydride/epoxide ring opening alternate copolymerization with potassium acetate
  • Method for preparing polyester by catalyzing cyclic anhydride/epoxide ring opening alternate copolymerization with potassium acetate

Examples

Experimental program
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Effect test

Embodiment 1

[0142]

[0143] The preparation method of polyphthalate-cyclohexanediol in the present embodiment comprises the following steps:

[0144] (1) Under an inert atmosphere, add 15 μmol of potassium acetate catalyst, 1500 μmol of phthalic anhydride and 7500 μmol of cyclohexene oxide into a dry 15mL reactor, stir for 5 minutes, stabilize the reaction temperature to 110°C, and vigorously stir Lower polymerization reaction 6 hours;

[0145] (2) After the polymerization is completed, cool the reactor to room temperature, and pour the reaction system in the reactor into 500 mL of methanol for sedimentation. Then, it is filtered, washed and vacuum-dried to obtain polyphthalate-cyclohexanediol ester.

[0146] The polymerization time was 6 hours, and the conversion rate of phthalic anhydride monomer reached 100%. The product obtained above was subjected to GPC analysis and NMR analysis. Such as figure 1 As shown, the product obtained in Example 1 of the present invention is a polyes...

Embodiment 2

[0148]

[0149] The preparation method of poly-1,2-propylene glycol phthalate in the present embodiment comprises the following steps:

[0150] (1) Under an inert atmosphere, add 15 μmol of potassium acetate catalyst, 1500 μmol of phthalic anhydride and 7500 μmol of propylene oxide into a dry 15mL reactor, stir for 5 minutes, stabilize the reaction temperature to 110°C, and Polymerization for 8 hours;

[0151] (2) After the polymerization is completed, cool the reactor to room temperature, and pour the reaction system in the reactor into 500 mL of methanol for sedimentation. Then it is filtered, washed and vacuum-dried to obtain poly-1,2-propylene glycol phthalate.

[0152] The polymerization time was 8 hours, and the conversion rate of phthalic anhydride monomer reached 100%. The product obtained above was subjected to GPC analysis and NMR analysis. Such as figure 2 As shown, the product obtained in Example 2 of the present invention is a polyester having a structure ...

Embodiment 3

[0154]

[0155] The preparation method of poly-1,2-propylene glycol phthalate in the present embodiment comprises the following steps:

[0156](1) In an inert atmosphere, add 15 μmol potassium acetate catalyst, 15000 μmol phthalic anhydride and 75000 μmol propylene oxide into a dry 15 mL reactor, stir for 5 minutes, stabilize the reaction temperature to 110 ° C, and Polymerization for 72 hours;

[0157] (2) After the polymerization is completed, cool the reactor to room temperature, and pour the reaction system in the reactor into 1000 mL of methanol for sedimentation. Then it is filtered, washed and vacuum-dried to obtain poly-1,2-propylene glycol phthalate.

[0158] The polymerization time was 72 hours, and the conversion rate of phthalic anhydride monomer reached 100%. The product obtained above was subjected to GPC analysis and NMR analysis. Such as figure 2 As shown, the product obtained in Example 3 of the present invention is a polyester having a structure of fo...

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Abstract

The invention relates to a method for preparing polyester by catalyzing cyclic anhydride / epoxide ring opening alternate copolymerization with potassium acetate. According to the method, potassium acetate catalyzes an epoxy compound and cyclic anhydride to be subjected to ring-opening alternate copolymerization to synthesize polyester, wherein potassium acetate is used as a catalyst to catalyze thecopolymerization of the cyclic anhydride and the epoxy compound, the reaction formula is defined in the specification, R1 and R2 are anhydride substituents, are the same or different, and simultaneously or independently are a hydrogen atom, a double bond, a benzene ring or a norbornene ring, and R3 and R4 are epoxy compound substituents, and are simultaneously or independently H, methyl, benzenering or cyclohexyl. The preparation method comprises the following steps: carrying out a polymerization reaction on excessive epoxide, cyclic anhydride and potassium acetate by using a normal-pressurebulk polymerization method, precipitating the polymer, filtering, and drying. Compared with the existing metal organic catalyst and non-metal organic catalyst, the potassium acetate provided by the invention has low biotoxicity, low price and simple preparation method, and has great application prospects.

Description

technical field [0001] The invention relates to a method for preparing polyester by catalyzing ring-opening and alternating copolymerization of cyclic anhydride / epoxide with potassium acetate. Background technique [0002] Polyester is a very common polymer material, which can be divided into semi-aromatic polyester and aliphatic polyester from the chain structure. Among them, semi-aromatic polyester is often used in packaging materials, engineering plastics and fibers due to its good mechanical strength and barrier properties. Aliphatic polyesters are an important class of degradable materials, which have attracted extensive attention due to their wide range of monomer sources, most of which are derived from renewable resources. Aliphatic polyesters are considered as an alternative to petroleum-based polymer materials. The main methods of synthesizing polyesters are stepwise polymerization and chain growth polymerization. Gradual polymerization mainly refers to the gradu...

Claims

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Application Information

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IPC IPC(8): C08G63/83C08G63/42
CPCC08G63/42C08G63/83
Inventor 王彬陈崇民李悦生
Owner TIANJIN UNIV
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