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Preparation method of biodegradable block copolymer

A block copolymer and biodegradation technology, applied in the field of preparation of biodegradable block copolymers, can solve the problems of cumbersome synthesis process, high production cost, increased activity, etc., and achieve simple operation, improved mechanical properties, and improved activity. Effect

Active Publication Date: 2019-05-21
HUAZHONG UNIV OF SCI & TECH
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  • Description
  • Claims
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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 biodegradable block copolymer, which uses a composite catalyst of a non-metallic Lewis acid and a non-metallic Lewis base to prepare a block copolymer. Non-toxic and biodegradable block copolymers without metal catalyst residues can be obtained through the method polymerization, and there is a synergistic effect between the composite catalysts, which increases the activity of monomers and initiators, and can realize ring-opening homopolymerization of epoxy monomers to obtain Polyether block expands the structural type of block copolymers, and can prepare tri-block copolymers and penta-block copolymers with richer structural types containing polyether blocks, so that non-metallic catalysts solve the problems that traditional metal catalysts are difficult to achieve. Completely remove the difficult problem, and at the same time solve the technical problems of cumbersome traditional synthesis process and high production cost of multi-block copolymers

Method used

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preparation example Construction

[0034] The invention provides a method for preparing a biodegradable block copolymer. By using a hydroxyl terminal compound as an initiator, a non-metallic Lewis acid and a Lewis base catalyst are used to synergistically catalyze epoxy monomers, acid anhydride monomers and lactones Biodegradable block copolymers were prepared by one-step polymerization of similar monomers. The concrete realization steps of this technical scheme are as follows:

[0035] (1) Under anaerobic conditions, add epoxy monomers, lactone monomers, and acid anhydride monomers into the reactor according to a certain ratio to obtain a monomer mixture; determine according to the needs of the target block copolymer The mixing ratio. In some embodiments, the molar ratio of the anhydride monomer to the epoxy monomer is 50:500 to 200:500; the molar ratio of the lactone monomer to the epoxy monomer is 50:500~200:500.

[0036] (2) mixing the monomer mixture described in step (1) with the initiator to obtain a ...

Embodiment 1

[0069] A kind of preparation method of degradable triblock copolymer comprises the following steps:

[0070] (1) Under anhydrous and oxygen-free conditions, mix ε-caprolactone, 1,2-cyclohexanedioic anhydride, 1,2-epoxybutane, and deionized water in a molar ratio of 50:100:500:10 Take 0.5ml, 1.29g, 3.6mL, and 15μL respectively, and add them to a 10mL reaction kettle in turn, and then add the catalyst triethylboron (85μL, 1mol / L) and 1,5,7-triazide bicyclo (4.4.0 ) dec-5-ene (60mg) was added to the reaction system in a molar ratio of 1:5, stirred and reacted at 100°C for 48h, then the reactor was cooled to room temperature, and air was introduced to terminate the reaction. The reaction solution was yellow and viscous thick.

[0071] (2) Dissolve the reaction solution in step (1) in 10 mL of dichloromethane, slowly drop it into cold methanol solution to precipitate a polymer, filter and separate to obtain a white polymer, and dry it in a vacuum oven at 40°C to constant weight ....

Embodiment 2

[0080] A kind of preparation method of degradable triblock copolymer comprises the following steps:

[0081] (1) Under anhydrous and oxygen-free conditions, take 1.20g, 3mL, and 1.5μL of lactide, propylene oxide, and deionized water in a molar ratio of 100:500:1, respectively, and add them to a 10mL reaction kettle in sequence. Add the catalyst triethylboron (170 μL, 1mol / L) and 7-methyl-1,5,7-triazabicyclo (4.4.0) dec-5-ene (12 μL) in a molar ratio of 2:1 into the reaction system, stirred and reacted at 40°C for 72 hours, then cooled the reactor to room temperature, and added dilute hydrochloric acid to terminate the reaction, the reaction solution was yellow and relatively viscous.

[0082] (2) Dissolve the reaction solution in step (1) in 10 mL of dichloromethane, slowly drop it into cold methanol solution to precipitate a polymer, filter and separate to obtain a white polymer, and dry it in a vacuum oven at 40°C to constant weight .

[0083] (3) H NMR spectrum and C NMR ...

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Abstract

The invention belongs to the technical field of macromolecular synthesis and particularly relates to a preparation method of a biodegradable block copolymer. The biodegradable block copolymer is prepared by taking a hydroxyl terminal compound as an initiator and performing synergistic catalysis on an epoxy monomer, an anhydride monomer and a lactone monomer by using nonmetallic lewis acid and lewis base catalysts through one-step polymerization. The preparation method of the biodegradable block copolymer has the following beneficial effects: due to use of the nonmetallic lewis acid and lewis base catalysts, the problem of medal residues of the block copolymer can be solved; furthermore, triblock copolymers and pentablock copolymers containing polyether blocks and with rich structure typescan be prepared. The purification problem that the fractional step method needs to charge for many times and wastes time and energy can be solved by a one-step method, the production efficiency can beimproved and the production cost can be reduced. The biodegradable block copolymer prepared by the method is controllable in relative 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 biodegradable block copolymer. Background technique [0002] With the rapid development of the economy, the excessive use of petroleum-based plastics has produced a large amount of plastic waste, which has caused serious pollution to the environment because it is not biodegradable. However, the national economy and daily life are inseparable from plastics. The development of biodegradable materials with good mechanical properties and thermal stability is of great significance to the environment and society. [0003] At present, biodegradable materials are mainly polyester and polycarbonate materials, such as polylactic acid and polypropylene carbonate. They are non-toxic and have good biocompatibility, and have good application prospects in the fields of food packaging, medical treatment and engineering plastics. However, the...

Claims

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Application Information

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IPC IPC(8): C08G63/60C08G63/664
Inventor 解孝林朱帅帅王勇廖永贵周兴平
Owner HUAZHONG UNIV OF SCI & TECH
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