Method for preparing polyethylene glycol network gel by using mercapto-vinyl clicking system

A technology of polyethylene glycol and olefin click, which is applied in the field of preparing polyethylene glycol network gel by using mercapto-ene click system, can solve the problems of limiting the potential application of polymer gel materials, etc. Mild conditions, efficient and fast response

Active Publication Date: 2015-05-06
常州市交通设施有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The polymer gel materials prepared by the traditional click method cannot meet the requirements of these special functions, which limits the potential application of polymer gel materials in functional materials of life, environment and medical science

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] a) Synthesis of terminal mercapto compounds: 1g of dry 3-mercaptopropionic acid, 10mL of freshly steamed tetrahydrofuran were placed in a dry 100mL three-necked flask, and 0.72mL of freshly steamed SOCl was slowly added dropwise under ice-bath conditions 2 , Remove the ice bath and raise the temperature to 60°C for 4h. After the reaction was completed, excess SOCl was removed under reduced pressure 2 . N 2 Add 9.4g polyethylene glycol (M n=2000) of anhydrous THF solution 40mL, and 1.5mL of triethylamine was added dropwise, and the reaction system was carried out at 60°C for 8h. After the reaction was completed, cool to room temperature, remove salt by filtration, and remove most of THF by rotary evaporation. The residue was precipitated in a large amount of ether, and was filtered and dried to obtain the brown target product.

[0029] b) Synthesis of multi-terminal unsaturated carbon-carbon double bonds: Accurately weigh 10g polyethylene glycol (M n =2000) into a d...

Embodiment 2

[0035] The basic process is the same as in Example 1, the difference is that:

[0036] In step 1), the polyethylene glycol derivative (M n =10000) is 0.4g (0.04mmol), 0.16g (0.08mmol) end mercapto polyethylene glycol derivative (M n =2000), 5uL 1mol / L free radical initiator azobisisoheptanonitrile tetrahydrofuran solution, solvent 1mL tetrahydrofuran dissolved, under the protection of nitrogen, the reaction temperature is 70 ° C, the reaction time 1h to form a polymer gel network compound .

[0037] In step 2), the reacted polymer gel network is taken out, put into a methanol solution to remove unreacted reactants remaining in the polymer network, and a regular polymer network is obtained after drying.

[0038] The rest are completely consistent with Example 1.

Embodiment 3

[0040] The basic process is the same as in Example 1, the difference is that:

[0041] In step 1), the polyethylene glycol derivative (M n =10000) is 0.4g (0.04mmol), 0.2g (0.1mmol) terminal mercapto polyethylene glycol derivative (M n =2000), the tetrahydrofuran solution of 5uL 1mol / L free radical initiator benzoin dimethyl ether, solvent 1mL THF dissolving, under the protection of nitrogen, under the radiation of ultraviolet light, the reaction time 2min has formed polymer gel network compound.

[0042] The rest are completely consistent with Example 1.

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PUM

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Abstract

The invention discloses a method for preparing polyethylene glycol network gel by using a mercapto-vinyl clicking system. Free radicals are generated through initiating by using a free-radical initiator under the condition of a certain temperature or lighting, so as to synchronously catalyze a vinyl compound and a mercapto compound to be subjected to click reaction. According to the method disclosed by the invention, by using the controllability of the efficiency of initiation of the free radicals under the condition of temperature and lighting, a polyethylene glycol derivative containing three or more multiterminal unsaturated carbon-carbon double bonds and a polyethylene glycol derivative which at least contains two terminal mercapto groups are synthesized by using the method, so as to prepare a polyethylene glycol polymer gel network with a regular structure. According to the method disclosed by the invention, the operation is simple, reaction materials are easily obtained, reaction is rapid, and the reaction conditions are mild; the polymer network prepared by the method disclosed by the invention has the advantages of good biocompatibility, regular structure, high mechanical strength and the like.

Description

technical field [0001] The invention belongs to the field of polymer synthesis methods, and relates to a method for preparing polyethylene glycol network gel by using a mercapto-ene click system. Background technique [0002] The polymer gel network structure has a high degree of similarity to human tissue, biocompatibility and high permeability to nutrients and metabolites. In recent years, it has achieved great development in the fields of drug controlled release, material separation, tissue engineering scaffolds, light-adjusting materials, and medical transplant organs. Hydrogel is a three-dimensional network structure of hydrophilic polymers cross-linked, which can quickly absorb and retain most of the water and is insoluble in water. Some small molecular substances can move in the gap of the polymer three-dimensional network, similar to the biomembrane in the organism for the transmission of information and substances. Therefore, the polymer network with high strength...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G81/00C08J3/24C08G65/48
Inventor 刘晓飞杨英武杨英杰
Owner 常州市交通设施有限公司
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