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Method for synthesising grafted copolymer by simultaneous chemoenzymatic process and one-pot process

A technology of graft copolymer and chemical enzymatic method, which is applied in the field of synthesis and preparation of polymer materials

Inactive Publication Date: 2015-02-18
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the use of enzymatic polymerization and click chemistry for simultaneous one-pot synthesis has not been reported

Method used

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  • Method for synthesising grafted copolymer by simultaneous chemoenzymatic process and one-pot process
  • Method for synthesising grafted copolymer by simultaneous chemoenzymatic process and one-pot process
  • Method for synthesising grafted copolymer by simultaneous chemoenzymatic process and one-pot process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Embodiment 1: chemical enzymatic method simultaneously one pot synthesis brush type graft copolymer PHAZPMA-g-(PCL) (PEG)

[0044] Synthesis of multifunctional macromolecular initiator PHAZPMA:

[0045] The solid components in the reaction system include: atom transfer radical polymerization catalyst system CuCl (0.06mg) and bpy (0.018mg) were transferred to a 50mL reaction bottle under the protection of argon. The liquid components in the reaction system: add argon to the reaction bottle after fully deoxygenating, in which: initiator 2-bromoisobutyrate ethyl 30 μL, atom transfer radical polymerization monomer glycidyl methacrylate (GMA) 2mL, solvent dimethylformamide (DMF) 1.4mL, seal the reaction bottle and place it in a 60°C oil bath with constant temperature and magnetic stirring for reaction. After reacting for 1-24h according to the required molecular weight, dissolve the mixture in chloroform Over neutral Al 2 o 3 The atom transfer radical polymerization catal...

Embodiment 2

[0059] Example 2: One-pot synthesis of centipede-like copolymer PHAZPMA-g-(P10-HD) (PEG) by chemical enzymatic method

[0060] The multifunctional initiator was synthesized as in Example 1.

[0061] Alkyne-PEO 2000 ) is synthesized with embodiment 1.

[0062] The reaction bottle was subjected to strict baking, vacuum degassing and argon cooling, and after repeating three times, the solid component in the reaction system was added: lipase Novozyme435 (enzymatically polymerized monomer 10-hydroxydecanoic acid (10-HD ) 5% by weight), activated molecular sieves ( Molecular sieve, activated by firing in a muffle furnace at 1000°C), catalyst system cuprous chloride / 2,2-bipyridine (CuCl / bpy), sealed. After three times of vacuum degassing and filling with argon, the liquid components: 10-hydroxydecanoic acid (10-HD) (7.52g), Alkyne-PEO 2000 Dissolve the polyfunctional macromolecular initiator PHAZPMA in 4mL of toluene, pass through argon gas to fully remove oxygen, use a sample i...

Embodiment 3

[0063] Embodiment 3: chemical enzymatic method one pot synthesis centipede shape copolymer PHAZPMA-g-(PCL) (FA)

[0064] The synthesis of multifunctional initiator PHAZPMA is as in Example 1.

[0065] Synthesis of Alkyne-Folic Acid (Alkyne-FA):

[0066] Weigh 0.50g folic acid (FA), dissolve it in 20mL DMSO, transfer to a 50mL reaction bottle, add 0.30g pentynoic acid (large excess), EDC0.58g, DMAP0.12g, place the reaction bottle at room temperature, Stir magnetically for 24h. After the reaction is over, use 1mol / L hydrochloric acid to wash the product solution repeatedly, then wash with water several times and concentrate, add chloroform to dissolve and add an appropriate amount of MgSO 4 Dry, filter to remove MgSO 4 , After distilling off the filtrate, put it into a vacuum oven for drying. Yield 82%.

[0067]

[0068] The reaction bottle was subjected to strict baking, vacuum degassing and argon cooling, and after repeated three times, the solid components in the reac...

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Abstract

The invention discloses a method for synthesising a grafted copolymer by simultaneous chemoenzymatic process and one-pot process, and belongs to the technical field of synthesis and preparation for a high-molecular material. The preparation method is a method for synthesising a polymer by simultaneous chemoenzymatic process and one-pot process, which combines enzymatic polymerization with click chemistry, and comprises the specific steps of preparing a polyfunctional high-molecular initiator, synthesising a click chain segment, and synthesising a brush-type grafted copolymer, wherein the prepared polyfunctional high-molecular initiator is polyepoxypropyl methacrylate after being subjected to loop opening by sodium azide, one side of the prepared polyfunctional high-molecular initiator is hydroxyl capable of initiating enzymatic polymerization, and the other side of the prepared polyfunctional high-molecular initiator is an azide group used for initiating a click chemical reaction. With the adoption of the method disclosed by the invention, the cockamamie steps of stepwise polymerization and sequential one-pot synthesis processes are avoided, separation and purification for an intermediate compound needed in multi-step operations are avoided, the pollution brought by a solvent is reduced, and the production cost is reduced; and a simpler as well as more convenient, efficient and energy-saving method is provided for synthesising a functional block polymer.

Description

technical field [0001] The invention belongs to the technical field of polymer material synthesis and preparation, and adopts a "chemical enzymatic method and simultaneous one-pot synthesis" grafted brush copolymer combined with enzymatic ring-opening polymerization and click chemistry. Background technique [0002] Brush-type graft copolymers are a class of structured polymers with unique structures and properties. They are not only widely used in biomedical materials, adhesives, additives, coatings, etc., but also used to prepare nanomaterials , inorganic mesoporous molecular sieves, etc. In recent years, scientists have synthesized a large number of block, comb, and centipede copolymers, and conducted extensive research on their physical and chemical properties and potential applications. [0003] Brush-type graft copolymers are generally divided into three synthetic methods: (1) macromonomer copolymerization, the macromonomer polymer with double construction is used as ...

Claims

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Application Information

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IPC IPC(8): C08G81/02C08F120/32C08F8/30C08F8/32C12P7/62
CPCY02P20/10
Inventor 李亚鹏祝明李玉祥撒宗朋王玉珍王静媛
Owner JILIN UNIV
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