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Synthesis method of amphiphilic polyethylene glycol-polycyclic lactone copolymer containing multiple bromine functional groups and preparation method of thermosensitive polymer

A technology of polyethylene glycol and cyclic lactone, which is used in the preparation of temperature-sensitive polymers and the synthesis of amphiphilic polyethylene glycol-polycyclic lactone copolymers, which can solve the problem of uncontrollable graft chain grafting Density, unfavorable polymer material synthesis, unfavorable promotion and use, etc., to achieve the effect of controllable reaction process and results, easy operation and promotion, and convenient operation

Active Publication Date: 2017-07-07
SICHUAN UNIVERSITY OF SCIENCE AND ENGINEERING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, there are two major problems in the above-mentioned technology. One is that the operation process is cumbersome, and it is impossible to adopt a simple one-step reaction to introduce multiple reactive functional group side groups on the main chain of polyethylene glycol, and based on this to graft or other polymers. Modification to prepare functional polymer materials, which makes the above technology unfavorable for popularization and use; second, it is not easy to adjust the graft density of grafted chains by adjusting the density of functional group side groups, which is also not conducive to polymer materials with different needs. Synthesis

Method used

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  • Synthesis method of amphiphilic polyethylene glycol-polycyclic lactone copolymer containing multiple bromine functional groups and preparation method of thermosensitive polymer
  • Synthesis method of amphiphilic polyethylene glycol-polycyclic lactone copolymer containing multiple bromine functional groups and preparation method of thermosensitive polymer
  • Synthesis method of amphiphilic polyethylene glycol-polycyclic lactone copolymer containing multiple bromine functional groups and preparation method of thermosensitive polymer

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Embodiment 1

[0049] Synthesis of amphiphilic polyethylene glycol-polycyclic lactone copolymers containing multiple bromine functional groups in the main chain:

[0050] Weigh 500mg double-terminal hydroxyl PEG2000 in such as figure 1 Add polytetrafluoroethylene magnets to the eggplant-shaped reaction bottle shown, and then add 10ml of toluene, connect the vacuum distillation device, place the eggplant-shaped reaction bottle in an oil bath at 140°C, and turn on the magnetic stirring. After about 20 minutes, , the azeotrope of toluene and water and excess toluene were distilled off. Connect the eggplant-shaped bottle with a vacuum line, vacuumize in sequence (vacuum degree: -0.09MPa)-argon, and use a disposable syringe to separate the dried α-bromo-γ-butylene in the state of argon. Add 0.46ml of lactone and 1.63ml of ε-caprolactone to the eggplant-shaped reaction bottle, and add the catalyst Sn(Oct) dropwise with a disposable dropper 2 About 40 mg, heat the reaction system to 120°C, turn o...

Embodiment 2

[0053] Amphiphilic thermosensitive polymers were synthesized by atom transfer radical polymerization (ATRP):

[0054] according to figure 2 Copolymer A: PEG-P(CL-r-BL) 1 The area ratio of d peak and f+g peak in the H-NMR spectrum can be calculated that each polymer chain in polymer A contains 12 bromine functional groups.

[0055] Take polymer A 0.427g (containing 0.4mmol Br wherein), 0.057g CuBr (0.4mmol), 0.138g PMDETA (0.8mmol, 0.166ml PMDETA) and dissolve in 5mlDMF (dimethylformamide) and place in the reaction flask, Then add 0.453g NIPAM (4.0mmol NIPAM); freeze the reaction bottle (1-2min at -196°C)-vacuumize-argon gas cycle three times to remove oxygen, and continue to pass argon gas for 15min; close the reaction bottle , and then placed the reaction bottle in a 90°C oil bath, turned on magnetic stirring, and stopped the reaction after 8 hours of reaction. Dilute the solution with THF (tetrahydrofuran) and pass it through a neutral alumina column to remove copper sal...

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Abstract

The invention relates to a synthetic method for an amphiphilic polyethylene glycol (PEG)-polycyclic lactone copolymer including multiple bromine functional groups and a thermo-sensitive polymer preparing method. Double-terminal hydroxyl polyethylene glycol is used as an initiator, alpha-bromine-gamma-butyrolactone and epsilon-caprolactone are used as monomers, stannous octoate is used as a catalyst, the copolymer with a main chain including the multiple bromine functional groups is prepared at one step through the controllable ring opening polymerization (ROP) method, and the synthetic method is convenient, fast and controllable. The bromine functional groups on the main chain of the copolymer are used as the initiator, an atom transfer radical polymerization (ATRP) method is adopted, N-isopropylacrylamide (NIPAM) is used as the monomer, CuBr / PMDETA is used as the catalytic system, and accordingly a PEG-P(CL-r-BL)-g-PNIPAM thermo-sensitive polymer is prepared. The low critical consolute temperature (LCST) is adjusted by adjusting the proportion of hydrophilicity and hydrophobicity chain segments in the copolymer, so that the temperature is close to the temperature of a human body. The synthetic method and the preparing method have a good application prospect in the field of temperature response drug controlled release.

Description

technical field [0001] The invention belongs to the technical field of polymer material preparation, especially the preparation of medical polymer materials, and specifically relates to a synthesis method of amphiphilic polyethylene glycol-polycyclic lactone copolymer containing multiple bromine functional groups and its temperature-sensitive polymerization method of preparation. Background technique [0002] Polyethylene glycol (PEG) is a polymer with high hydrophilicity and good biocompatibility. The immunogenicity of PEG is very low, it will not cause serious antigenic reaction of the immune system in the human body, and PEG with a molecular weight of less than 10,000 can be quickly excreted through metabolism, does not accumulate in the body, and has no toxic side effects. Therefore, PEG has been approved by the US Food and Drug Administration (FDA) and is widely used in the field of biomedicine. Due to the good flexibility and high hydrophilicity of PEG molecular chai...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F283/02C08F220/54C08F220/34C08G63/664C08G63/78C08G63/85
Inventor 高晨张雪梅李新跃鲁越阳龑杨迁
Owner SICHUAN UNIVERSITY OF SCIENCE AND ENGINEERING
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