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A Method for Preparing Polymer Networks Using Bulk Click Chemistry System

A click chemistry reaction and polymer technology, which is applied in the field of bulk click chemistry system to prepare polymer network, can solve the problems of irregular cross-linked network structure, low mechanical strength of gel network, different degree of reaction, etc., so as to reduce microscopic defects. The effect of preventing the formation of macroscopic defects and reducing the diffusion time

Inactive Publication Date: 2015-10-28
SOUTHEAST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the traditional click chemical reaction process, it takes time for the ligand to diffuse and bind the ligand to the metal catalyst.
The click reaction reacts immediately as long as there is a metal catalyst and a ligand. When the ligand diffuses to the place where there is a metal catalyst, it reacts quickly to form a polymer gel network, and the formation of the polymer gel network hinders the metal catalyst and ligand. The further diffusion of the body, so that the reaction degree of each point in the system is different when the reaction occurs, especially the degree of reaction in the gel network is low, so that the formed polymer gel network forms a lot of defects, so that the cross-linked network structure Irregular
There are even large particle-shaped metal catalysts in some places, so that a large number of macropore defects appear in the gel network. It is because of the appearance of such macropore defects that the mechanical strength of the gel network is not high, and it is easy to break and other fatal defects. limit its application

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] a) Synthesis of azido compounds: Accurately weigh 10 g of polyethylene glycol (M n =2000) was dissolved in 50ml of anhydrous dichloromethane, ice-bathed, and the temperature of the system was lowered to 0°C. After stirring for 3 hours, freshly distilled thionyl chloride (2ml) was weighed and dissolved in 20ml of anhydrous dichloromethane. Slowly drop the thionyl chloride and dichloromethane solution into the polyethylene glycol dichloromethane solution for about 20 minutes at 0°C using a constant-pressure floor liquid funnel. Add 0.2ml neopyridine to the system. Slowly warm up to room temperature, and react for 24 hours under magnetic stirring. After the reaction was completed, the pyridine hydrochloride generated during the system reaction was filtered off, and dichloromethane and excess thionyl chloride were removed by distillation under reduced pressure. The resulting product was precipitated in a large amount of ether, filtered to obtain linear polyethylene glyco...

Embodiment 2

[0030] The basic process is the same as in Example 1, the difference is that:

[0031] In step 1), the linear polyethylene glycol (M n = 2000) is 0.25g (0.125mmol), 0.0259g (0.09mmol) pentaerythroxypropargyl ether, ultrasonic vibration at 50 ° C until completely dissolved, adding metal catalyst nano cuprous chloride (1.25mg, 0.125mmol), N, N, N', N", N"-pentamethyldiethylenetriamine ligand (1.25mmol).

[0032] In step 2), the reaction temperature is 50° C., and the reaction time is 4 hours to form a polymer gel network compound.

[0033] The rest are completely consistent with Example 1.

Embodiment 3

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

[0036] In step a), synthesis of azide compounds: Accurately weigh 10 g of polyethylene glycol (M n =4000) was dissolved in 50ml of anhydrous dichloromethane, ice-bathed, and the temperature of the system was lowered to 0°C. After stirring for 3 hours, freshly distilled thionyl chloride (1ml) was weighed and dissolved in 20ml of anhydrous dichloromethane. Slowly drop the thionyl chloride and dichloromethane solution into the polyethylene glycol dichloromethane solution for about 20 minutes at 0°C using a constant-pressure floor liquid funnel. Add 0.2ml neopyridine to the system. Slowly warm up to room temperature, and react for 24 hours under magnetic stirring. After the reaction was completed, the pyridine hydrochloride generated during the system reaction was filtered off, and dichloromethane and excess thionyl chloride were removed by distillation under reduced pressure. The resulting product...

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Abstract

The invention discloses a method for preparing a polymer network by utilizing a bulk click chemical system. The method comprises the following step of carrying out click reaction on an organic compound containing three or more than three multi-terminal alkynyl and an organic compound containing at least two terminal azido in the presence of a nanoscale metal catalyst to obtain the polymer network. The method disclosed by the invention is simple in operation, high in click efficiency and rapid in reaction; the polymer network prepared by adopting the method disclosed by the invention is few in macroscopic and microcosmic defects and the regularity of the polymer network is increased, so that the physical strength and the mechanical strength of the polymer network are increased.

Description

technical field [0001] The invention belongs to the field of polymer synthesis methods, and relates to a method for preparing a polymer network by a bulk click chemistry system. Background technique [0002] Polymer gel network structure, especially hydrogel, has the most similar properties to biological soft tissue and has good biocompatibility. Hydrogel is a three-dimensional network structure formed by the cross-linking of hydrophilic polymers with high permeability. In the gaps of the polymer gel network, some metabolites and oxygen small molecule substances can transmit information and substances. It is precisely because of the intelligence of this kind of polymer gel network gel that it may be applied in many fields, especially in biomedical fields such as drug sustained release and biological tissue engineering. Many gel-like tissues and organs in the human body operate mechanically in harsh dynamic physiological environments. For example, articular cartilage is sub...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G73/08
Inventor 付国东钱珊珊姚芳
Owner SOUTHEAST UNIV
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