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Method for self-stabilized precipitation polymerization in situ preparation of poly(4-ethenyl pyridine)polymer

A vinylpyridine, self-stabilizing precipitation technology, applied in pharmaceutical formulations, medical preparations with non-active ingredients, coatings, etc., to achieve the effects of clean surface, low cost and good stability

Active Publication Date: 2011-10-26
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] The purpose of the present invention is to solve the drawbacks caused by the use of stabilizers and other additives in the traditional precipitation polymerization method system, and to provide a kind of in-situ preparation of pellets using a recyclable organic solvent as the reaction medium and self-stabilizing precipitation polymerization system. Method for poly(4-vinylpyridine) polymer with controllable diameter and shape and system maintaining stable dispersion

Method used

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  • Method for self-stabilized precipitation polymerization in situ preparation of poly(4-ethenyl pyridine)polymer
  • Method for self-stabilized precipitation polymerization in situ preparation of poly(4-ethenyl pyridine)polymer
  • Method for self-stabilized precipitation polymerization in situ preparation of poly(4-ethenyl pyridine)polymer

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Experimental program
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Effect test

Embodiment 1

[0046] Add 2.625g of monomer 4-vinylpyridine, 0.0328g of initiator azobisisobutyronitrile, and 50ml of butyl acetate as the reaction medium into a 100ml three-necked flask, then put it in a water bath, and install a condenser The water pipe was connected with water, and the reaction temperature of the water bath was kept at 70°C, and the reaction was carried out under the protection of nitrogen for 8 hours. After the reaction, the obtained poly(4-vinylpyridine) polymer was centrifuged out from the emulsion by a centrifuge (4000 rpm, centrifugation time 10 min), cleaned and placed in a vacuum oven at 50°C for drying.

[0047] The average particle size of the obtained monodisperse P4VP particles was 502 nm, and the particle size distribution coefficient was 1.12%. , the yield is 78.85%, and its scanning electron micrograph is as figure 1 shown.

Embodiment 2

[0049] Put 2.625g of monomer 4-vinylpyridine, 0.0328g of initiator azobisisobutyronitrile, and 50ml of ethyl heptanoate as the reaction medium into a 100ml three-necked flask, then put it in a water bath, and put it on Condensate the water pipe and pass water, keep the reaction temperature of the water bath at 70°C, and react for 8 hours under the protection of nitrogen. After the reaction, the obtained poly(4-vinylpyridine) polymer was centrifuged out from the emulsion by a centrifuge (4000 rpm, centrifugation time 10 min), cleaned and placed in a vacuum oven at 50°C for drying.

[0050] The average particle diameter of gained monodisperse P4VP particle is 476nm, and particle size distribution coefficient is 1.43%, and productive rate is 69.42%, and its scanning electron micrograph is as follows figure 2 shown.

Embodiment 3

[0052] Add 2.625g of monomer 4-vinylpyridine, 0.0328g of initiator azobisisobutyronitrile, and 50ml of isoamyl acetate as the reaction medium into a 100ml three-necked flask, then put it in a water bath, and install Condensate the water pipe and pass water, keep the reaction temperature of the water bath at 70°C, and react for 8 hours under the protection of nitrogen. After the reaction, the obtained poly(4-vinylpyridine) polymer was centrifuged out from the emulsion by a centrifuge (4000 rpm, centrifugation time 10 min), cleaned and placed in a vacuum oven at 50°C for drying.

[0053] The average particle diameter of gained monodisperse P4VP particle is 492nm, and particle size distribution coefficient is 1.38%, and productive rate is 67.94%, and its scanning electron micrograph is as follows image 3 shown.

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Abstract

The invention discloses a method for self-stabilized precipitation polymerization in situ preparation of a poly(4-ethenyl pyridine)polymer, belonging to the field of polymer preparation. The method comprises the following steps: adding a monomer 4-ethenyl pyridine, an initiator and a reaction medium in a reaction container for fully dissolving and shaking, and then reacting at the temperature of 60-80 DEG C for 6-8 hours in the protection of nitrogen; and separating out the polymer from white lactescence through centrifugation or filtration so as to obtain white poly(4-ethenyl pyridine) powder. When the reaction medium is a single organic acid alkyl ester, a monodispersed particle with a grain size of 470-690nm is obtained; and when the reaction medium is a mixed solvent of organic acid alkyl ester, vinylacetate and cyclohexane, a serial type particle with a gain size of 500-1000nm is obtained. In the method, stirring and any stabilizer do not need to be added, a polymerization systemis capable of maintaining a self-stabilized dispersion state, the surface of the polymer particle is clean, and the polymer particle has good thermal resistance.

Description

technical field [0001] The invention specifically relates to a method for preparing poly(4-vinylpyridine) polymers in situ by self-stabilizing precipitation polymerization, which belongs to the field of polymer preparation. Background technique [0002] Since poly(4-vinylpyridine) (P4VP) has amino functional groups, it can be easily modified to be hydrophilic, acidic, basic and amphoteric, and the required ligands can also be simply connected. Therefore, it has a wide range of applications in drug carriers, chromatographic column packing, chemical separation, polymer catalysis, coatings, and the preparation of functional membranes. [0003] As an important functional chemical raw material, 4-vinylpyridine is widely used in various fields of polymer materials. For example, weakly basic ion exchange resins and ion exchange membranes can be produced by using 4-vinylpyridine monomers to separate heavy metal ions; graft copolymerization of the monomers with linear polymers can o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F126/06C08F2/06A61K47/32C09D139/08
Inventor 邓建元王剑杨万泰
Owner BEIJING UNIV OF CHEM TECH
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