Method for preparing hyperbranched polymer through dual click chemistry

A technology of hyperbranched polymers and click chemistry, which is applied in the field of synthesis of hyperbranched polymers, can solve the problems of hyperbranched polymers that need to be expanded, monomers that cannot be purchased commercially, and chemical reactions that are limited, so as to achieve a wide range of applicable monomers , high repeatability and simple process

Active Publication Date: 2011-09-14
杭州德烯科技集团有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although new progress has been reported, there are still key difficulties that need to be overcome: 1. The reported monomer coupling strategy enables the synthesis of hyperbranched polymers by conventional polycondensation methods using commercial asymmetric monomers , represents a great progress in the synthesis strategy, but the reported chemical reactions are limited, and the variety of hyperbranched polymers to be

Method used

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  • Method for preparing hyperbranched polymer through dual click chemistry
  • Method for preparing hyperbranched polymer through dual click chemistry
  • Method for preparing hyperbranched polymer through dual click chemistry

Examples

Experimental program
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Embodiment 1

[0020] Step 1), under nitrogen protection, hexanedithiol (3.01 g, 20 mmol), ethyl acetate (17.62 g, 200 mmol), triethylamine (1.01 g, 10 mmol), propylene acrylate were added successively in the reactor Alkyne ester (2.20 g, 20 mmol), at 30 o C for 5 hours, evaporated under reduced pressure to remove ethyl acetate and triethylamine;

[0021] Step 2), under nitrogen protection, the product obtained in step 1) was dissolved in 20 mL of toluene, and 4 mol% of thermosensitive free radical initiator azobisisobutyronitrile (131.3 mg) was added, at 65 o C polymerization reaction 3 hours, obtain hyperbranched polymer (number average molecular weight is 7200; weight average molecular weight is 104800; degree of branching 0.76) through methanol precipitation, separation, drying.

Embodiment 2

[0023] Step 1), under nitrogen protection, hexanedithiol (3.01 g, 20 mmol), ethyl acetate (17.62 g, 200 mmol), triethylamine (4.04 g, 40 mmol), propylene acrylate were added successively in the reactor Alkyne ester (2.20 g, 20 mmol), at 10 o C for 5 hours, evaporated under reduced pressure to remove ethyl acetate and triethylamine;

[0024] Step 2), under nitrogen protection, the product obtained in step 1) was dissolved in 20 mL of toluene, and 4 mol% of thermosensitive free radical initiator azobisisobutyronitrile (131.3 mg) was added, at 65 o C polymerized for 3 hours, precipitated with methanol, separated and dried to obtain a hyperbranched polymer.

Embodiment 3

[0026] Step 1), under nitrogen protection, add hexanedithiol (3.01 g, 20 mmol), ethyl acetate (0.17 g, 2 mmol), triethylamine (1.23 g, 22 mmol), propylene acrylate in the reactor successively Alkyne ester (2.20 g, 20 mmol), at 40 o C for 0.5 hours, evaporated under reduced pressure to remove ethyl acetate and triethylamine;

[0027] Step 2), under nitrogen protection, the product obtained in step 1) was dissolved in 20 mL of toluene, and 4 mol% of thermosensitive free radical initiator azobisisobutyronitrile (131.3 mg) was added, at 65 o C polymerized for 3 hours, precipitated with methanol, separated and dried to obtain a hyperbranched polymer.

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Abstract

The invention discloses a method for preparing a hyperbranched polymer through dual click chemistry. The method comprises the following steps of: 1) adding one mole of bis(thiol) compound, 0.1 to 10 moles of solvent, 0.05 to 2 moles of base catalyst, and 0.9 to 1.1 moles of compound containing alkynyl and alkenyl into a reactor sequentially under the protection of nitrogen, performing sulfydryl-alkene addition reaction at the temperature of between 10 and 40 DEG C for 0.5 to 24 hours, and performing reduced pressure evaporation to remove the solvent; and 2) dissolving the product obtained in the step 1) in 0.25 to 10 moles of solvent under the protection of nitrogen, adding 0.005 to 0.05 mole of photosensitive radical initiator or thermosensitive radical initiator, irradiating by ultraviolet light or heating at the temperature of between 40 and 90 DEG C to produce radical, performing sulfydryl-alkene addition polymerization reaction for 0.5 to 24 hours, and precipitating, separating and drying to obtain the hyperbranched polymer. The method has the advantages of no need of complex AB2 monomer synthesis and purification steps, high speed and efficiency, convenience, wide application range and the like. The obtained hyperbranched polymer containing a large amount of thioether bonds has wide application prospect in the fields of biomedical carriers, high-performance materials, additives and the like.

Description

technical field [0001] The invention relates to a method for preparing a hyperbranched polymer by double-click chemistry, in particular to a method for synthesizing a hyperbranched polymer containing thioether and alkynyl. Background technique [0002] Since the 1980s, hyperbranched polymers have attracted more and more research interest. It is a class of highly branched macromolecules with a three-dimensional ellipsoidal structure, and it is called highly branched polymers together with dendrimers. Compared with linear polymers, it has many unique properties, such as: high solubility, low viscosity, internal branched backbone, internal cavity, binding sites, a large number of terminal functional groups, etc. Compared with dendrimers, its synthesis method is simpler, and it also makes the molecular design more variable. The continuous development of synthesis has promoted its application in the fields of processing aids, coatings, pharmaceutical carriers, metal nanocatalys...

Claims

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Application Information

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IPC IPC(8): C08G75/04C08G75/045
Inventor 韩金高超
Owner 杭州德烯科技集团有限公司
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