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

A vinylpyridine, self-stabilizing precipitation technology, applied in the directions of pharmaceutical formulations, inactive medical preparations, coatings, etc., to achieve the effects of easy implementation, good stability, and narrow particle size distribution

Active Publication Date: 2013-03-13
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 for in situ preparation of poly(4-ethenyl pyridine)polymer
  • Method for self-stabilized precipitation polymerization for in situ preparation of poly(4-ethenyl pyridine)polymer
  • Method for self-stabilized precipitation polymerization for in situ preparation of poly(4-ethenyl pyridine)polymer

Examples

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, and 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 obt...

Claims

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Application Information

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Patent Type & Authority Patents(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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