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Amphiphilic block polymer synthesis process based on cyclic lactone

A cyclic lactone and synthesis process technology, which is applied in the field of cyclic lactone-based amphiphilic block polymer synthesis process, can solve potential safety hazards, difficult to expand production, and difficult to obtain narrow dispersion high molecular weight amphiphilic It can solve the problems of volatile polymers, etc., to achieve the effect of single variable, simplify the feeding process, and save the preparation time.

Inactive Publication Date: 2016-11-09
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the preparation of PEG ring-opening lactone is generally vacuum-sealed tube polymerization. After feeding, it is necessary to vacuumize and ventilate nitrogen to create an anhydrous and oxygen-free vacuum environment. There are requirements for the vacuum resistance and explosion-proof of the reaction bottle, and the feeding After the completion, it is necessary to seal the tube with an open flame while vacuuming, which has potential safety hazards and is not easy to expand production
In addition, there is also a synthesis process that uses normal pressure and inert gas protection. The inert gas protection needs to be turned on until the end of the reaction, and it is usually difficult to obtain amphiphilic polymers with narrow dispersion and high molecular weight.

Method used

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  • Amphiphilic block polymer synthesis process based on cyclic lactone
  • Amphiphilic block polymer synthesis process based on cyclic lactone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] A. Put the reaction raw materials mPEG-OH, ε-caprolactone, stannous octoate, toluene, silanized polymer tube, hydrothermal synthesis reaction kettle, and stirring bar into an anhydrous and oxygen-free glove box ;

[0027] B. preparation volume ratio is 0.1% stannous octoate / toluene mixed solution in anhydrous and oxygen-free glove box;

[0028] C. Add 50 mg mPEG-OH and 450 mg ε-caprolactone into the silanized polymerization tube equipped with a stirring bar in an anhydrous and oxygen-free glove box, then add 1 mL of anhydrous toluene and 3.2 μL of 0.1% octanoic acid sulfide Tin / toluene mixed solution.

[0029] D. In an anhydrous and oxygen-free glove box, seal the polymerization tube containing the reaction reagent with tin foil and put it into the polytetrafluoroethylene liner, and fill the gap with tin foil to fix the polymerization tube in the liner, and then put Put the PTFE bushing into the kettle, then tighten the lid of the kettle, and then use the screw to tig...

Embodiment 2

[0036] A. Put the reaction raw materials mPEG-OH, L-lactide, stannous octoate, toluene, silanized polymer tube, hydrothermal synthesis reaction kettle, and stirring bar into an anhydrous oxygen-free glove box ;

[0037] B. preparation volume ratio is 0.1% stannous octoate / toluene mixed solution in anhydrous and oxygen-free glove box;

[0038] C. Add 300 mg mPEG-OH and 300 mg L-lactide into the silanized polymerization tube equipped with a stirring bar in an anhydrous and oxygen-free glove box, then add 1 mL of toluene solution, 20 μL of 0.1% stannous octoate / toluene mixed solution.

[0039] D. In an anhydrous and oxygen-free glove box, seal the polymerization tube containing the reaction reagent with tin foil and put it into the polytetrafluoroethylene liner, and fill the gap with tin foil to fix the polymerization tube in the liner, and then put Put the PTFE bushing into the kettle, then tighten the lid of the kettle, and then use the screw to tighten the lid of the kettl...

Embodiment 3

[0047] A. Put the reaction raw materials Mal-PEG-OH, lactide, stannous octoate, toluene, silanized polymerization tube, hydrothermal synthesis reaction kettle and stirring bar into anhydrous and oxygen-free gloves in the box;

[0048]B. preparation volume ratio is 0.05% stannous octoate / toluene mixed solution in anhydrous and oxygen-free glove box;

[0049] C. Add 300mg of Mal-PEG-OH and 300mg of L-lactide in a silanized polymerization tube equipped with a stirring bar in an anhydrous and oxygen-free glove box, and then add the mixed solution to make the lactide The molar ratio of lactide to stannous octoate is 1:0.1%.

[0050] D. In an anhydrous and oxygen-free glove box, seal the polymerization tube containing the reaction reagent with tin foil and put it into the polytetrafluoroethylene liner, and fill the gap with tin foil to fix the polymerization tube in the liner, and then put Put the PTFE bushing into the kettle, then tighten the lid of the kettle, and then use the s...

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Abstract

The invention relates to an amphiphilic block polymer synthesis process based on cyclic lactone. The amphiphilic block polymer synthesis process includes the following several steps that 1, stannous octoate is dissolved in toluene and is prepared into a stannous octoate solution for standby application; 2, the stannous octoate solution obtained in the step 1 is mixed with hydrophilic polyethylene glycol and the cyclic lactone, and an amphiphilic block polymer is obtained through heating reaction. Compared with the prior art, a hydrothermal synthesis reaction kettle serves as a reaction device, polymerization reaction is completed through one step, and the process is simple, safe and reliable. After the dosing ratio of the reaction raw materials is determined, the molecular weight of the reaction product is controlled only by adjusting the reaction time, and the process is single in variable and strong in controllability.

Description

technical field [0001] The invention relates to the field of polymer synthesis technology, in particular to a synthesis technology of amphiphilic block polymer based on cyclic lactone. Background technique [0002] Amphiphilic polymers are widely used in biomedicine and other fields due to their ability to self-assemble into nanoparticles under certain conditions. Currently, the most widely used amphiphilic polymer components are mainly polyethylene glycol (PEG) approved by the FDA and biodegradable polyesters (such as polycaprolactone, polylactic acid, etc.). Such amphiphilic polymers are usually obtained by reacting PEG containing special functional groups with its matching functional groups to obtain functionalized polyesters or using PEG ring-opening cyclic lactones. Among them, the synthesis method of ring-opening polymerization is more common. At present, the preparation of PEG ring-opening lactone is generally vacuum-sealed tube polymerization. After feeding, it is ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/664C08G63/78C08G63/82
CPCC08G63/664C08G63/78C08G63/785C08G63/823
Inventor 李永勇董海青刘萍
Owner TONGJI UNIV