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Method for preparing polymer microspheres

A technology of polymer and polymerization inhibitor, applied in the field of materials, can solve the problems of large amount of inhibitor added, limited application, difficult to clean, etc., and achieve good dimensional uniformity and the effect of inhibiting emulsion polymerization.

Inactive Publication Date: 2011-04-20
SERVICE CENT OF COMMLIZATION OF RES FINDINGS HAIAN COUNTY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the suspension polymerization process of polymer microspheres, the effect of water-soluble inorganic inhibitors is weak, and the addition amount of inhibitors is relatively large, especially as the diameter of the microspheres obtained by suspension polymerization is smaller, the effect of water-soluble inorganic inhibitors The weaker the inhibitory effect
Patent JP-A-61-255,355 uses water-soluble mercapto compounds to inhibit emulsion polymerization and achieved good results, but due to its unpleasant smell, this unpleasant smell is not easy to clean in the product, so its application is limited

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Equipped with stirrer, condensate return pipe, thermometer, inert gas N 2 Fill in the reactor of mouth, add the deionized water of 800g, with 8g polyvinyl alcohol and 8g composite emulsion polymerization inhibitor (comprising 3.2g 3,4,5-trihydroxybenzoic acid, 3.6g hexamethylenetetramine, 1.2 g NaCl) in deionized water and filled with nitrogen. Then add 79.5g styrene and 0.5g divinylbenzene, stir, the temperature rises to 70°, add 8g benzoyl peroxide, keep the constant temperature at 70°, stir and react for 6 hours, the stirring speed is 5000 rpm. After the reaction, the liquid-solid phase was separated by centrifugal filtration, dried and pulverized to obtain microspheres with an average particle size of 50 μm.

Embodiment 2

[0018] Equipped with stirrer, condensate return pipe, thermometer, inert gas N 2 Fill in the reactor of inlet, add the deionized water of 400g, 4g polyvinylpyrrolidone and 0.8g composite emulsion polymerization inhibitor (comprising 0.72g 3,4,5-trihydroxybenzoic acid, 0.04g hexamethylenetetramine, 0.04g sodium chloride) in deionized water, filled with nitrogen. Then add 79g methyl methacrylate, 1g trimethylolpropane triacrylate, stir, the temperature rises to 90°, add 0.8g methyl ethyl ketone peroxide, keep the temperature at 90°, stir and react for 3 hours, the stirring speed is 2500 rpm point. After the reaction, the liquid-solid phase was separated by centrifugal filtration, dried and pulverized to obtain microspheres with an average particle size of 100 μm.

Embodiment 3

[0020] Equipped with stirrer, condensate return pipe, thermometer, inert gas N 2 In the reactor of filling mouth, add the deionized water of 800g, 0.8g carboxymethyl cellulose and 4g composite emulsion polymerization inhibitor (comprising 1.6g 3,4,5-trihydroxybenzoic acid, 2g hexamethylenetetramine , 0.4g sodium chloride). Then add 55g styrene, 20g methyl acrylate, 5g divinylbenzene, stir, the temperature rises to 90°, add 4g azobisisobutyronitrile, keep the temperature at 80°, stir and react for 4.5 hours, the stirring speed is 2000 rpm point. After the reaction, centrifugal filtration was used to separate liquid and solid phases, and after drying and crushing, microspheres with an average particle size of 150 μm were obtained.

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PUM

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Abstract

The invention relates to a method for preparing polymer microspheres. The method comprises: mixing composite emulsion polymerization inhibitor, stabilizing agent and de-ionized water in a reaction kettle, then introducing nitrogen into the mixture, adding a polymer monomer into the mixture, stirring the mixture, raising temperature to a reaction temperature between 70 and 90 DEG C, adding an initiating agent into the mixture, and thermostatically stirring the mixture to react for 3 to 6 hours under the reaction temperature; and after the reaction is finished, filtering, drying and crushing the reactants to form the polymer microspheres, wherein the composite emulsion polymerization inhibitor comprises the following components in percentage by weight: 40 to 90 percent of 3, 4, 5-trihydroxybenzoic acid, 5 to 50 percent of hexamethylene tetramine, and 5 to 15 percent of sodium chloride. The composite emulsion polymerization inhibitor is added during suspension polymerization, and can effectively inhibit the occurrence of emulsion polymerization during suspension polymerization for preparing polystyrene microspheres and polyacrylic acid microspheres; and the prepared microspheres have good size evenness.

Description

technical field [0001] The invention belongs to the field of material technology, and relates to a method for preparing polymer microspheres, in particular to a polymer microsphere with uniform size obtained by suspension polymerization of styrene monomer or acrylic monomer in the presence of an emulsion polymerization inhibitor. ball technique. Background technique [0002] Polymer microspheres play a special and key role in many important fields because of their special size and structure. Microspheres with different particle sizes and shapes are responsible for different functions, and are widely used in many fields such as coatings, paper surface processing, plastic additives, and building materials. For example, polymethyl methacrylate microspheres can be made into an anti-blocking opening agent for polyolefin films (in polyolefin resin, after mixing polymethyl methacrylate microsphere particles, it is formed into a film. At this time, on the surface of the film Very ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J13/14
Inventor 聂秋林袁求理
Owner SERVICE CENT OF COMMLIZATION OF RES FINDINGS HAIAN COUNTY