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Preparation method of substituted acetylene helical polymer microspheres

A technology of acetylene polymer and acetylene helix, which is applied in the field of preparation of acetylene helix polymer microspheres, and can solve problems such as no precedent

Active Publication Date: 2014-07-30
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Although the suspension polymerization method has been widely used in the preparation of vinylic monomers, it has no precedent when it comes to acetylenic monomers, especially the preparation of pure substituted acetylene polymer microspheres.

Method used

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  • Preparation method of substituted acetylene helical polymer microspheres
  • Preparation method of substituted acetylene helical polymer microspheres
  • Preparation method of substituted acetylene helical polymer microspheres

Examples

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Effect test

example 1

[0046] Example 1: Dissolve 1g of polyvinyl alcohol (PVA) in 49g of deionized water to prepare an aqueous solution of PVA with a mass concentration of 2%, and dissolve 0.1g of monomer M1a containing chiral propargyl amide groups in 1mL of chloroform to form Solution, stirred under nitrogen atmosphere for 10 minutes, added 0.0022g rhodium metal catalyst in the above solution, the mol ratio of catalyst and monomer was 1:100, stirred under nitrogen atmosphere for 10 minutes, under nitrogen protection, the above solution was added dropwise to In the PVA aqueous solution, carry out mechanical stirring at a speed of 350rpm, keep the temperature at 0°C for 4 hours, then rise to 30°C for 12 hours, filter after the reaction, wash with deionized water and ethanol in sequence, and vacuum dry for 24 hours, that is Yellow polymer microspheres were obtained.

[0047] Result: the infrared spectrogram of example 1 is provided in the accompanying drawing figure 1 Curve a, photo of microspheres...

example 2

[0048] Example 2: The first step is to prepare the bis-alkynyl crosslinking agent M2, specifically as follows: adipic acid and propargyl alcohol are weighed according to the molar ratio of 1:3.5, and benzene is used as a solvent, and p-toluenesulfonic acid monohydrate is added as dehydration Refluxing reaction at 85°C for 3 hours, followed by extraction with saturated sodium bicarbonate solution and saturated sodium chloride solution, drying over anhydrous magnesium sulfate, and rotary evaporation to obtain a white solid, which is the diacetylenic crosslinking agent M2.

[0049] The second step is to prepare substituted acetylene helical polymer microspheres. Dissolve 1g of polyvinyl alcohol (PVA) in 49g of deionized water to prepare an aqueous solution of PVA with a mass concentration of 2%. Dissolve 0.1g of monomer M1a containing chiral propargyl amide groups in 1mL of chloroform to form a solution. Stir under atmosphere for 10 minutes, add 0.0047g diacetylenic crosslinking ...

example 3

[0051] Example 3: The first step is to prepare the bis-alkyne-based crosslinking agent M2, and the specific steps are the same as in Example 2.

[0052] The second step is to prepare substituted acetylene helical polymer microspheres. Dissolve 1g of polyvinyl alcohol (PVA) in 49g of deionized water to prepare an aqueous solution of PVA with a mass concentration of 2%. Dissolve 0.1g of monomer M1a containing chiral propargyl amide groups in 1mL of chloroform to form a solution. Stir under the atmosphere for 10 minutes, add 0.0094g diacetylenyl crosslinking agent to the above solution, stir under nitrogen atmosphere for 10 minutes, add 0.0026g rhodium metal catalyst to the above solution, the molar ratio of the catalyst to the total amount of the monomer crosslinking agent 1:100, stirred under nitrogen atmosphere for 10 minutes, under the protection of nitrogen, the above solution was added dropwise to the PVA aqueous solution, mechanically stirred at 350rpm, kept at 0°C for 4 h...

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Abstract

The invention discloses a preparation method of substituted acetylene helical polymer microspheres, and belongs to the field of high-molecular material. The preparation method comprises following steps: firstly, polyvinyl alcohol (PVA) is dissolved in deionized water so as to prepare a polyvinyl alcohol aqueous solution; substituted acetylene monomer is dissolved in dichloromethane, trichloromethane, or methylbenzene, and a rhodium metal catalyst is added, and an obtained mixture is stirred for 5 to 30min, and is added into the polyvinyl alcohol aqueous solution dropwise under nitrogen protection; an obtained mixed material is subjected to mechanical stirring, is reacted for 1 to 24h at a temperature of 0 to 60 DEG C, is filtered after reaction, is washed with deionized water and ethanol successively, and at last is subjected to vacuum drying for 12 to 24h so as to obtain yellow microspheres. According to the preparation method, the substituted acetylene helical polymer microspheres are prepared via suspension polymerization, application range of substituted acetylene helical polymer is enlarged, and the substituted acetylene helical polymer microspheres possess recoverability, and can be reused.

Description

technical field [0001] The invention belongs to the field of polymer materials and relates to a preparation method of substituted acetylene helical polymer microspheres. Background technique [0002] Polymer microsphere is a new type of functional material with excellent performance. It has a large specific surface area, strong adsorption capacity and excellent surface reactivity, so it is widely used in immunoassays, cell separation, immobilized enzymes, targeting In scientific researches such as pharmaceuticals and industrial applications such as advanced cosmetics and environmental protection materials. Traditional methods for preparing polymer microspheres mainly include emulsion polymerization, suspension polymerization, dispersion polymerization, etc. When using these polymerization methods to prepare polymer microspheres, a large amount of stabilizers or emulsifiers must be used in the reaction system, so the obtained The post-treatment of polymer microspheres is rel...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F238/00C08F2/20
Inventor 邓建平张海洋杨万泰宋洁璇任重磊
Owner BEIJING UNIV OF CHEM TECH
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