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A kind of preparation method of hollow porous microsphere

A porous microsphere, hollow technology, applied in the field of materials, can solve the problems of difficult separation and purification of products, high time cost, long time, etc.

Active Publication Date: 2021-09-14
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The in-situ polymerization preparation method has the problems of complicated operation, difficult product separation and purification, low yield, high time cost, and difficult to control the porous structure.
The existing modified preparation methods often need to combine extraction, solvent evaporation, etching, dialysis and other subsequent treatment processes, the process is complicated, the time is long and the yield is low

Method used

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  • A kind of preparation method of hollow porous microsphere
  • A kind of preparation method of hollow porous microsphere
  • A kind of preparation method of hollow porous microsphere

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preparation example Construction

[0021] The invention provides a method for preparing hollow porous microspheres, which specifically includes the following steps: using sulfonic acid type polystyrene cation exchange resin particles as raw materials, cracking them at a temperature of 350-550°C in a nitrogen or nitrogen-oxygen atmosphere 1-60min to obtain hollow porous microspheres. It should be pointed out that the reactor for pyrolysis of resin particles is a common electric heating device, which can be a muffle furnace or a tube furnace.

[0022] During the cracking process of the sulfonic acid polystyrene series cation exchange resin particles, the temperature difference between the inside and the outside surface of the particles is 1-200°C. Under this temperature difference, the sulfonic acid group is removed inside the resin particle to form sulfur dioxide, and the exposed polystyrene-divinyl phenyl body is cracked to form holes; The matrix is ​​cross-linked to form a stable structure.

[0023] The sulf...

Embodiment 1

[0037] A preparation method of hollow porous microspheres, the specific steps are as follows: using Amberlite IRN-97H sulfonic acid type cation exchange resin with a cross-linking degree of 8% and an average particle diameter of 0.5 mm as a raw material, vacuum drying at 105°C for 4 hours. The dried resin particles were put into a tube furnace for pyrolysis, the pyrolysis temperature was 450°C, the pyrolysis time was 20min, and the pyrolysis atmosphere was a nitrogen-oxygen mixture with an oxygen concentration of 3vt%. Under this condition, the temperature difference between the inside and outside surface of the resin particle was 110°C. After the reaction is over, the product is cooled naturally to obtain hollow porous microspheres.

[0038] The product was sliced, and the structure of the cut surface of the product was observed with a scanning electron microscope, such as figure 1 shown. The outer shell of the prepared product remains in a complete spherical shape, and the...

Embodiment 2

[0040] A preparation method of hollow porous microspheres, the specific steps are as follows: using Amberlite IRN-97H sulfonic acid type cation exchange resin with a cross-linking degree of 8% and an average particle diameter of 0.5 mm as a raw material, vacuum drying at 105°C for 4 hours. The dried resin particles were put into a tube furnace for pyrolysis, the pyrolysis temperature was 450°C, the pyrolysis time was 30min, and the pyrolysis atmosphere was a nitrogen-oxygen mixture with an oxygen concentration of 5vt%. Under this condition, the temperature difference between the inside and outside surface of the resin particle is 80°C. After the reaction is over, the product is cooled naturally to obtain hollow porous microspheres.

[0041] The product was sliced, and the structure of the cut surface of the product was observed with a scanning electron microscope, such as figure 2 shown. The outer shell of the prepared product remains in a complete spherical shape, the inte...

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Abstract

The invention provides a method for preparing hollow porous microspheres, belonging to the technical field of materials. The preparation method of hollow porous microspheres of the present invention comprises the following steps: using sulfonic acid type polystyrene cation exchange resin particles as raw materials, cracking for 1-60min at a temperature of 350-550°C in nitrogen or nitrogen-oxygen atmosphere, to obtain Hollow porous microspheres. The shell of the prepared product remains intact, and the interior is hollow and forms a uniformly distributed pore structure. By changing the cleavage reaction conditions, the number and distribution of pores inside the formed hollow porous polymer microspheres can be effectively regulated, so as to be suitable for different application fields.

Description

technical field [0001] The invention belongs to the technical field of materials, and in particular relates to a preparation method of hollow porous microspheres. Background technique [0002] Hollow porous polymer microspheres have the characteristics of high specific surface area, low density, and adjustable pore size due to their special hollow interior, uniform arrangement of pores, and stable shell structure. , Adsorption separation, radioactive waste resin disposal and other fields have a wide range of applications. At present, the preparation of porous polymer microspheres is mainly divided into two categories, one is the in-situ polymerization preparation method adding initiator and porogen, including suspension polymerization, precipitation polymerization, multi-step emulsion polymerization, dispersion polymerization, microfluidic Polymerization, etc.; the other is a modified preparation method that promotes the formation of a porous structure of the polymer throug...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J13/02
CPCB01J13/02
Inventor 黄正梁宋琦王洁杨勇杨遥孙婧元王靖岱阳永荣蒋斌波廖祖维唐振超
Owner ZHEJIANG UNIV