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Preparation method of carbon dioxide based block copolymer

A technology of block copolymers and carbon dioxide, which is applied in the field of preparation of carbon dioxide-based biodegradable block copolymers, can solve the problems of high cost, metal catalyst residue, low reaction efficiency, etc., and achieves no effect on performance and color, and wide range of raw materials , cheap effect

Active Publication Date: 2019-08-06
HUAZHONG UNIV OF SCI & TECH
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  • Abstract
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Problems solved by technology

[0006] In view of the above defects or improvement needs of the prior art, the present invention provides a method for preparing a carbon dioxide-based block copolymer, which uses cyclic anhydride monomers, lactone monomers, epoxy compounds and carbon dioxide as monomers , using a mixture of organic Lewis acid and organic Lewis base as a catalyst, and using a terminal hydroxyl compound as an initiator, the initiator initiates ring-opening copolymerization of cyclic anhydride monomers, lactone monomers, epoxy compounds and carbon dioxide, one step Carbon dioxide-based block copolymers are prepared by this method, which solves the technical problems in the preparation of biodegradable block copolymers in the prior art, such as lengthy process flow, low reaction efficiency, high cost, affecting yield, and metal catalyst residues.

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  • Preparation method of carbon dioxide based block copolymer
  • Preparation method of carbon dioxide based block copolymer
  • Preparation method of carbon dioxide based block copolymer

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preparation example Construction

[0039] In some embodiments, the preparation method of the present invention includes the following steps:

[0040] (1) In an anhydrous and oxygen-free environment, cyclic acid anhydride monomers, lactone monomers and epoxy compounds are mixed to obtain a monomer mixture;

[0041] (2) mixing the monomer mixture, the catalyst and the initiator to obtain a raw material mixture;

[0042] (3) charging carbon dioxide into the raw material mixed solution to cause a polymerization reaction, and after the reaction is completed, quench the reaction to obtain a crude product;

[0043] (4) adding the crude product into an organic solvent for precipitation, separating and drying the obtained precipitate to obtain the carbon dioxide-based block copolymer.

[0044] In some embodiments, the cyclic acid anhydride monomers are maleic anhydride, phthalic anhydride, 1-cyclopentene-1,2-dicarboxylic anhydride, cyclobutane dicarboxylic anhydride and bicyclo[2.2. 1] One or more of hept-5-ene-2,3-di...

Embodiment 1

[0073] A preparation method of a carbon dioxide-based biodegradable copolymer is as follows:

[0074] (1) In an anhydrous and oxygen-free environment, add 0.88g, 0.85g, and 6mL of phthalic anhydride, lactide, and cyclohexene oxide into the reaction kettle at a molar ratio of 1:1:10, Then add triethylborane, 1,8-diazabicycloundec-7-ene and water in a molar ratio of 2:1:2, and add 118 μL, 9 μL, and 2.1 μL, respectively. React at 80°C for 10 h, release carbon dioxide, react for another 2 h, then cool to room temperature, and feed air to terminate the reaction.

[0075] (2) Methanol was added to the crude product obtained in step (1), and magnetically stirred for more than 30 minutes to obtain a precipitated white solid, which was separated by filtration, and the obtained white solid was vacuum-dried at room temperature to constant weight.

[0076] (3) Use H NMR spectrum to characterize the structure of the block copolymer, and use gel permeation chromatography to characterize th...

Embodiment 2

[0088] A preparation method of a triblock carbon dioxide-based biodegradable block copolymer is as follows:

[0089] (1) In an anhydrous and oxygen-free environment, add 3.10g, 3.57g, and 6mL of maleic anhydride, ε-caprolactone, and ethylene oxide into the reaction kettle at a molar ratio of 1:1:5, Then add triethylamine, 4-dimethylaminopyridine and benzyl alcohol according to the molar ratio of 1:1:1, add 43.5μL, 38.20mg, 32.5μL respectively. Filled with 1MPa carbon dioxide. React at 80°C for 4h, release carbon dioxide, react for another 1h, then cool to room temperature, and feed air to terminate the reaction.

[0090] (2) Methanol was added to the crude product obtained in step (1), and magnetically stirred for more than 30 minutes to obtain a precipitated white solid, which was separated by filtration, and the obtained white solid was vacuum-dried at room temperature to constant weight.

[0091] (3) Use H NMR spectrum to characterize the structure of the block copolymer,...

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Abstract

The invention belongs to the technical field of polymer synthesis, and more particularly relates to a preparation method of a carbon dioxide-based biodegradable block copolymer. The carbon dioxide-based biodegradable block copolymer is prepared by using a cyclic anhydride monomer, a lactone monomer, an epoxy compound and carbon dioxide as monomers, using an organic Lewis acid and organic Lewis base mixture as a catalyst, and using a terminal hydroxyl compound as an initiator to initiate ring-opening copolymerization of the cyclic anhydride monomer, the lactone monomer, the epoxy compound and the carbon dioxide in one step. The preparation method can effectively utilize the carbon dioxide and convert the carbon dioxide into a practical polymer material. The obtained polymer has no metal residue, and the luster and performance of the polymer can be ensured. One-step feeding is adopted to avoid the problems of complicated steps and purification in the step-by-step synthesis of the block copolymer. Meanwhile, the carbon dioxide-based biodegradable block copolymer has high controllability in molecular weight and block length.

Description

technical field [0001] The invention belongs to the technical field of polymer synthesis, and more specifically relates to a preparation method of a carbon dioxide-based biodegradable block copolymer. Background technique [0002] Since the 1950s, with the rapid development of the field of polymer materials, plastic has become a low-cost, high-performance material and has been widely used, playing an increasingly important role in human society, and thus has an indispensible missing position. [0003] With the intensification of plastic usage, its negative problems are gradually exposed. The waste of a large amount of plastics has brought serious environmental problems and increasingly threatened human life and health. However, plastics have become an indispensable and important part of human society. To solve this problem, it is necessary to develop degradable plastics while ensuring superior performance in all aspects. [0004] Biodegradable plastics have attracted much...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G64/34C08G64/18C08G63/08C08G63/181C08G63/52C08G63/87
CPCC08G63/08C08G63/181C08G63/52C08G63/87C08G64/18C08G64/34
Inventor 周兴平张国超王勇解孝林
Owner HUAZHONG UNIV OF SCI & TECH
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