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Preparation method of polymer matrix controllable graded pore material

A polymer and hierarchical pore technology, which is applied in the field of inorganic, organic and polymer materials, can solve the problems that the pore size of the material is difficult to be effectively controlled, it is difficult to prepare porous microspheres with pores, and it depends on the external reaction conditions of the emulsifier. Achieve good industrialization development prospect, simple process and low cost

Inactive Publication Date: 2018-10-02
HEBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the porous copolymer system has been widely studied and applied, it is difficult to prepare porous microspheres with open pores, and the pore size of the material obtained by this method is difficult to be effectively controlled. The preparation process is more dependent on the molar ratio of the emulsifier and external in reaction conditions

Method used

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  • Preparation method of polymer matrix controllable graded pore material
  • Preparation method of polymer matrix controllable graded pore material
  • Preparation method of polymer matrix controllable graded pore material

Examples

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Effect test

Embodiment 1

[0046] Embodiment 1: the three-dimensional ordered macroporous copolymer (comparative example) that does not add porogen synthesis;

[0047] (1) Preparation of 200nm silica colloidal crystal template;

[0048] Utilize according to patent CN101691426A -Fink-Hohn synthesis method, add 127g of absolute ethanol, 30g of ammonia water with a mass fraction of 25%, and 60.5g of deionized water into a 500mL three-necked bottle equipped with mechanical stirring at room temperature (25°C), stir evenly, and then Quickly add 16.8 g of ethyl orthosilicate to the three-necked flask, and react at room temperature for 8 hours. Transfer the obtained suspension to a beaker, wait for the solvent to volatilize completely naturally, and obtain a colloidal silica template with an average particle size of 200nm, and finally sinter the template in a muffle furnace at 500°C for 3 hours, and slowly lower it to room temperature to obtain The silica colloidal crystal template with an average particle s...

Embodiment 2

[0053] Embodiment 2: Oligomer is used as porogen to synthesize hierarchical hole poly(styrene-divinylbenzene) copolymer HPP(St-DVB)-PPG;

[0054](1) The preparation of 200nm silica colloidal crystal template is the same as step (1) in the embodiment one;

[0055] (2) The oligomer polypropylene glycol (PPG) is used as a porogen to synthesize hierarchically porous poly(styrene-divinylbenzene) copolymer HPP(St-DVB)-PPG;

[0056] The sintered colloidal silica template obtained in the 10g dried step (1) is placed in the reactor, and 0.84g monomer and 3.8g crosslinking agent mixed solution (mass ratio DVB: St=9:2), 3mL polypropylene glycol (PPG) and 0.023g initiator azobisisobutyronitrile (AIBN) mixed solution was dispersed at a high speed of 6000r / min for 10min, then poured into the container, submerged in the sintered carbon dioxide Silica colloidal crystal template, after half an hour, put it in an oven at 65°C for 4h, then raise the temperature to 80°C for 24h, and the polymer / ...

Embodiment 3

[0059] Example 3: Using toluene and polypropylene glycol as porogens to synthesize hierarchically porous poly(styrene-divinylbenzene) copolymer HP P(St-DVB)-Toluene-PPG;

[0060] (1) The preparation of 200nm silica colloidal crystal template is the same as step (1) in the embodiment one;

[0061] (2) The polypropylene glycol in Example 2 was replaced by a mixture of toluene and polypropylene glycol, the feed ratio of toluene and polypropylene glycol was the volume ratio Toluene:PPG=1:6, and the remaining steps were referred to Example 2. Material HP PDVB-Toluene-PPG its nitrogen adsorption and desorption curve and pore size distribution see Image 6 , the type IV isotherm shows that the material has a mesoporous structure. According to the BJH pore size distribution diagram, the material has mesopores of about 2.5nm and mesopores of about 20nm, forming a hierarchical pore combining multi-scale mesopores and ordered macropores. structure. The specific surface area of ​​BET is...

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Abstract

The invention discloses a preparation method of a polymer matrix controllable graded pore material. The polymer matrix controllable graded pore material is prepared by combining a colloidal crystal template method with a pore-forming agent; in the process of synthesizing the graded pore copolymer, the final specific surface area and a pore structure of the control material are realized by properlycontrolling the proportions of a monomer, a crosslinking agent and the pore-forming agent. The polymer matrix graded pore material obtained by the invention selects a three-dimensional ordered macroporous copolymer as a skeleton; the pore wall is enabled to have a microporous and mesoporous structure by regulating the content ratio of all the components in a precursor, and thereby the graded porematerial is prepared. The average aperture variation range of the graded pore material is 4 to 8.5 nm, and the variation range of specific surface area is 100 to 700m<2> / g. According to the graded pore structure of combining three-dimensional ordered large holes with micropores and mesopores, the ordered macropores greatly improve the mass transfer efficiency of a material; abundant micropores and mesopores favorably improve the specific surface area and the utilization rate of the material, so that the material has a great potential application value in practical application.

Description

technical field [0001] The technical solution of the invention relates to the fields of inorganic, organic and polymer materials, and in particular to a preparation method of a polymer-based adjustable hierarchical pore material. Background technique [0002] Hierarchically Structure Porous Materials are multi-level materials that integrate micropores (<2nm), mesoporous (2-50nm), and macropores (>50nm) in one body. Level structure such as micropore-mesopore, micropore-macropore, and mesoporous-macropore integrated materials, or materials with tertiary structure micropore-mesopore-macropore integrated. The hierarchical pore structure makes up for the defects of the single-level pore structure to a certain extent. In addition, because of its large specific surface area, developed and interconnected multi-level pore structure and low density, it is excellent in diffusion and mass transfer. than other single-channel structures. In recent years, the design and synthesis o...

Claims

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Application Information

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IPC IPC(8): C08J9/28C08L25/08C08L25/18
CPCC08J9/28C08J2201/0462C08J2201/0502C08J2325/08C08J2325/18
Inventor 王小梅南学日张旭
Owner HEBEI UNIV OF TECH
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