Method for synthesizing segmented copolymer by coupling enzymatic catalysis and organic catalysis by virtue of micro reactor

A block copolymer and microreactor technology, which is applied in biochemical equipment and methods, bioreactor/fermenter combinations, specific-purpose bioreactors/fermenters, etc., can solve the problem of low conversion rate and reaction efficiency. Low problems, to achieve the effect of optimizing the process flow, controllable molecular weight, and improving molecular weight distribution

Active Publication Date: 2017-03-22
NANJING UNIV OF TECH
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

[0004] The technical problem to be solved in the present invention is to provide a method for synthesizing block copolymers by coupling enzyme catalysis and organic catalysis with a microreactor system to solve the shortcomings of low reaction efficiency and low conversion rate in the prior art.

Method used

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  • Method for synthesizing segmented copolymer by coupling enzymatic catalysis and organic catalysis by virtue of micro reactor
  • Method for synthesizing segmented copolymer by coupling enzymatic catalysis and organic catalysis by virtue of micro reactor
  • Method for synthesizing segmented copolymer by coupling enzymatic catalysis and organic catalysis by virtue of micro reactor

Examples

Experimental program
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Effect test

Embodiment 1

[0035]Fill 1.17 g of immobilized enzyme Novozyme 435 with a particle size of 0.3 to 0.9 mm into an immobilized enzyme microreactor with an inner diameter of 3.8 mm and a length of 300 mm (retention volume is 1.81 mL), using an inner diameter of 1 mm and a length of 9218.2 mm microchannel reactor (reserved volume is 7.24mL), connect the device, and flush the pipeline with toluene solvent after redistillation to remove water. Add ε-caprolactone (6.8484g, 6.65mL, 60mmol), benzyl alcohol (0.21mL, 2mmol), toluene (8.14mL) and δ-valerolactone to two flat-bottomed dry ampoules after removing water at high temperature (1.82mL, 20mmol), TBD (0.1mmol), toluene (13.18mL), after shaking and mixing, move them into the first material sampling device A and the second material sampling device B, and adjust the flow rate of A and B to be 0.362ml / min, the reaction temperatures in the two reactors were 60°C and 25°C respectively, and the reaction was started. After 25min, the reaction was stabl...

Embodiment 2

[0037] Fill 1.17 g of immobilized enzyme Novozyme 435 with a particle size of 0.3 to 0.9 mm into an immobilized enzyme microreactor with an inner diameter of 3.8 mm and a length of 300 mm (retention volume is 1.81 mL), using an inner diameter of 1 mm and a length of 18436.4 mm microchannel (retention volume is 14.48mL), connect the device, and flush the pipeline with toluene solvent after redistillation to remove water. Add ε-caprolactone (6.65mL, 60mmol), benzyl alcohol (0.21mL, 2mmol), 8.14mL toluene and δ-valerolactone (5.44mL, 60mmol ), 0.3mmol TBD, 9.56mL toluene, oscillated and mixed evenly, and moved into the first material sampling device A and the second material sampling device B, the flow rate of A and B was adjusted to 0.362ml / min, and the reaction temperature was 60°C and 25°C, start the reaction, wait for 25 minutes to stabilize the reaction, collect for 6 minutes, add 80mL of methanol and quencher solid benzoic acid (0.13mmol), stir and precipitate at low temper...

Embodiment 3

[0039] Fill 0.585 g of immobilized enzyme Novozyme 435 with a particle size of 0.3 to 0.9 mm into an immobilized enzyme microreactor with an inner diameter of 3.8 mm and a length of 150 mm (retention volume is 0.905 mL), using an inner diameter of 1 mm and a length of 3687 mm The microchannel reactor (retention volume is 2.90mL), connect the device, and flush the pipeline with the toluene solvent after distilling off the water. Add ε-caprolactone (6.65mL, 60mmol), benzyl alcohol (0.21mL, 2mmol), 8.14mL toluene and lactide (20mmol), DBU (0.02 mL, 0.1mmol), 14.98mL toluene, after shaking and mixing, move into the first material sampling device A and the second material sampling device B, control the flow rate of A and B to be 0.181ml / min, the reaction in the two reactors The temperature was 60°C and 25°C respectively, and the reaction was started. After 44 minutes, the reaction was stable and collected for 11 minutes. Then, 80 mL of methanol and 0.04 mmol of solid benzoic acid (...

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Abstract

The invention discloses a method for synthesizing a segmented copolymer by coupling enzymatic catalysis and organic catalysis by virtue of a micro reactor, and relates to the field of the synthesis of polymers. The method comprises the following steps: (a) dissolving a monomer 1 and an initiating agent in an organic solvent, pumping an obtained solution into an immobilized enzyme micro reactor, and conducting a full reaction; (b) dissolving a monomer 2 and an organic catalyst in an organic solvent, mixing an obtained solution and reaction liquid outputted from the step (a) in a mixer 4, pumping a mixed solution into a micro-channel reactor 5 and conducting a full reaction; and (c) adding a quenching agent and a third organic solvent to reaction liquid collected from the step (b), and conducting separating and purifying, so as to obtain the pure poly-monomer 1-poly-monomer 2 segmented copolymer. According to the method provided by the invention, the processes of the enzymatic catalysis and the organic catalysis are coupled by virtue of the micro reactor, so that advantages of the enzymatic catalysis and the organic catalysis are integrated, and subsequently reaction efficiency is greatly improved, reaction time is shortened an continuous production is achieved; and the method has the advantages of being safe, efficient, low in energy consumption, high in reaction rate, moderate in reaction conditions and the like.

Description

technical field [0001] The invention relates to polymer synthesis, in particular to a method for catalytically synthesizing block copolymers using a microreactor system. Background technique [0002] Block copolymers are linear copolymers formed by the alternating polymerization of different segments of chemical structure. It can combine the excellent properties of various polymers to obtain functional polymer materials with superior performance. At present, the methods for synthesizing block copolymers mainly include organic catalysis, metal catalysis and enzyme catalysis. There are two limitations in its preparation: 1) It is difficult to efficiently couple enzymes and organic catalysts in the same reaction system; 2) It is difficult to precisely and controllably construct the copolymeric structure. The enhancement of mass and heat transfer by microflow field technology and its continuous flow and low back-mixing characteristics provide good technical feasibility for bre...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C12P7/62C12M1/00C12M1/40C08G63/08C08G63/82C08G63/87
Inventor 郭凯黄卫军朱宁胡欣方正刘一寰
Owner NANJING UNIV OF TECH
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