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Preparation method and application of amphiphilic thermo-responsive block copolymer

A temperature-sensitive block and polymer technology, applied in the field of polymers, can solve the problems of few types of temperature-sensitive polymers, rare research, high low critical phase transition temperature, etc.

Inactive Publication Date: 2018-12-14
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] There are few types of commercial thermosensitive polymers, and the low critical phase transition temperature is high, which makes it difficult to meet diversified practical applications
Nowadays, considerable progress has been made in designing and synthesizing new temperature-responsive polymer systems through RAFT polymerization, but there are not many studies on the construction of regenerative two-phase aqueous systems from the prepared temperature-responsive polymers.

Method used

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  • Preparation method and application of amphiphilic thermo-responsive block copolymer
  • Preparation method and application of amphiphilic thermo-responsive block copolymer
  • Preparation method and application of amphiphilic thermo-responsive block copolymer

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Step (1): Preparation of RAFT reagent (BTPA)

[0035] In aqueous potassium hydroxide solution (104mg / mL, 31.25mL), add 3-mercaptopropionic acid (2.5mL, 28.75mmol) dropwise, then add carbon disulfide (3.75mL, 28.75mmol) dropwise, and place at room temperature Reaction 5h. Benzyl bromide (4.95g, 28.75mmol) was added, and the reaction was refluxed at 85°C for 12h. After the reaction, the mixture was cooled to room temperature, chloroform (70.0 mL) was added, and excess hydrochloric acid was added to adjust the pH value, and the organic layer was repeatedly washed with a large amount of distilled water, and the organic layer was rotary evaporated to obtain a yellow solid.

[0036] Step (2): Preparation of Macromolecular Chain Transfer Agent Based on Polyethylene Glycol Monomethyl Ether

[0037] Dry polyethylene glycol monomethyl ether (15.0 g, 3.0 mmol) was dissolved in 30.0 mL of anhydrous toluene, and a large amount of solvent was removed by azeotropic distillation at 5...

Embodiment 2

[0041] Step (1) and step (2) are with embodiment 1;

[0042] Step (3): Preparation of thermosensitive block polymer PEG-b-PNIPAM

[0043] Polyethylene glycol monomethyl ether macromolecular chain transfer agent (0.315g, 0.06mmol), N-isopropylacrylamide (NIPAM, 0.6675g, 6mmol) and azobisisobutyronitrile (AIBN, 4mg, 24μmol ) was dissolved in 1,4-dioxane (3.0 mL) and added to a one-necked flask. The mixture was sealed under vacuum after three freeze-pump-thaw cycles. React in an oil bath at 80°C for 12 hours, quench the polymerization with liquid nitrogen, unseal the tube, dilute with 1,4-dioxane, and precipitate the mixture with excess ether. The above dissolution-precipitation cycle was repeated three times to obtain a light yellow thermosensitive block polymer PEG-b-PNIPAM.

Embodiment 3

[0045] Step (1) and step (2) are with embodiment 1;

[0046] Step (3): Preparation of thermosensitive block polymer PEG-b-PNIPAM

[0047] Polyethylene glycol monomethyl ether macromolecular chain transfer agent (0.21g, 0.04mmol), N-isopropylacrylamide (NIPAM, 0.445g, 4mmol) and azobisisobutyronitrile (AIBN, 3mg, 18μmol ) was dissolved in 1,4-dioxane (2.0 mL) and added to a one-necked flask. The mixture was sealed under vacuum after three freeze-pump-thaw cycles. React in an oil bath at 75°C for 22 hours, quench the polymerization with liquid nitrogen, unseal the tube, dilute with 1,4-dioxane, and precipitate the mixture with excess ether. The above dissolution-precipitation cycle was repeated three times to obtain a light yellow thermosensitive block polymer PEG-b-PNIPAM.

[0048] Such as figure 1 Shown is the synthetic process schematic diagram (a) of the RAFT reagent (BTPA) prepared in embodiment 1, the synthetic process schematic diagram (b) of the macromolecular chain ...

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Abstract

The invention belongs to the technical field of polymers and relates to a preparation method and an application of an amphiphilic thermo-responsive block copolymer. The amphiphilic thermo-responsive block copolymer comprises water-soluble PEG (polyethylene glycol) blocks and thermo-responsive PNIPAM (poly(N-isopropylacrylamide)) blocks. The thermo-responsive block copolymer material is prepared through steps as follows: firstly, trithio ester containing carboxyl is prepared and then subjected to esterification reaction with ethylene glycol monomethyl ether, a PEG macromolecular chain transferagent is prepared, finally, N-isopropyl acrylamide monomers are polymerized to the PEG macromolecular chain transfer agent through RAFT polymerization, and the thermo-responsive block copolymer with narrow distribution width index and proper lower critical solution temperature is synthesized. The prepared polymer has the advantages of narrow distribution width index, proper lower critical solutiontemperature and the like; the thermo-responsive block copolymer and organic salt establish a regenerative two-phase aqueous system, and the polymer has characteristics that split-phase temperature islow, operating conditions are mild, the polymer is easy to recycle and the like.

Description

technical field [0001] The invention belongs to the technical field of polymers, and relates to a preparation method and application of an amphiphilic temperature-sensitive block polymer. Background technique [0002] Based on the two-phase aqueous system, it has broad application prospects in the fields of medicine, food, extraction and separation of natural active substances and its own excellent characteristics, such as large water content, fast phase separation, low cost and simple operation. The separation and enrichment method widely used in recent years. The first development of the two-phase aqueous system is the polymer-polymer system, most of which use dextran as a phase forming agent, which has high cost and high viscosity, and then salt is used instead of dextran to develop the polymer-salt system, hydrophilic organic solvent-salt system and ionic liquid-salt system, although these three systems reduce the cost and viscosity, they still cannot realize the recove...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F293/00
CPCC08F293/005C08F2438/03
Inventor 李文轩刘园园王蕾智文静王赟韩娟倪良
Owner JIANGSU UNIV
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