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Preparation method of hedgehog SiO2 hollow microsphere

A hollow microsphere and hedgehog technology, which is applied in the field of preparation of hedgehog-shaped SiO2 hollow microspheres, can solve the problems that the silica hollow microspheres cannot be satisfied, the types of block copolymers are limited, and the synthesis of copolymers is not easy. Easy to tune, wide application value, good effect

Inactive Publication Date: 2010-08-18
GUANGZHOU CHEM CO LTD CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are still some disadvantages in the method of preparing hollow silica microspheres by using block copolymers: (a) it is generally a diblock copolymer, and the control of structure and microsphere structure is difficult to balance, while the synthesis of triblock or above copolymers Not easy; (b) The types of commercially available block copolymers are limited, currently only P123, which cannot meet the requirements of assembling special microstructure silica hollow microspheres; (c) Utilize commercially available block copolymers to prepare special structure Silica microspheres generally need to add additives, just like CTAB, SDS, etc., the system is more complicated and the operating conditions are harsh

Method used

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  • Preparation method of hedgehog SiO2 hollow microsphere

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] (1) Preparation of block polymer polyacrylic acid ethyl cinnamate 53-block-(polyacrylic acid 94-copolymerization-polystyrene 258)

[0038] Weigh 0.075g polyethyl cinnamate 53-intercalated-(tert-butyl acrylate 94-copolymerization-polystyrene 258), put it into a 50mL single-neck round bottom flask, add 10mL solvent dichloromethane, 2mL of trifluoroacetic acid, protected from light and hydrolyzed for 24 hours, to obtain polyacrylic acid ethyl cinnamate 53-intercalated-(polyacrylic acid 94-copolymerization-polystyrene 258), spin concentration to remove solvent and trifluoroacetic acid, and add a certain amount of dichloromethane, at room temperature to make it volatilize, the obtained sample is the block polymer polyacrylic acid ethyl cinnamate 53-block-(polyacrylic acid 94-copolymerization-polystyrene 258) in a refrigerator after vacuum drying for 24h save.

[0039] (2) SiO 2 Preparation of hollow microspheres

[0040] Take 0.002g polyacrylic acid ethyl cinnamate 53-int...

Embodiment 2

[0042] (1) Block polymer polyacrylic acid ethyl cinnamate 53-block-(polyacrylic acid 58-co-poly-poly-tert-butyl acrylate 36-co-polystyrene 258) (referred to as PCEA53-b-P(AA58-co-tBA36 Preparation of -co-Sty258))

[0043] Weigh 0.025g of polyethyl cinnamate 53-intercalated-(tert-butyl acrylate 94-co-polystyrene 258) (referred to as PCEA53-b-P(tBA94-co-Sty258) and put it into a 50mL single-necked round Add 10mL of dichloromethane and 2mL of trifluoroacetic acid into a bottom flask, and hydrolyze for 5 hours in the dark to obtain polyacrylic acid ethyl cinnamate 53-intercalated-(polyacrylic acid 58-copolymerized-polyacrylic acid tert-butyl ester 36-copolymerized-polyacrylic acid Styrene 258) (referred to as PCEA53-b-P (AA58-co-tBA36-co-Sty258)), rotary concentration to remove solvent and trifluoroacetic acid, a certain amount of dichloromethane was added to it, and it was volatilized at room temperature, and the obtained The sample PCEA53-b-P (AA58-co-tBA36-co-Sty258) was vacuu...

Embodiment 3

[0047] (1) Preparation of block polymer polyacrylic acid ethyl cinnamate 53-block-(polyacrylic acid 94-copolymerization-polystyrene 258) (referred to as PCEA53-b-P(AA94-co-Sty258)

[0048] Weigh 0.050g polyethyl cinnamate 53-intercalated-(tert-butyl acrylate 94-co-polystyrene 258) (referred to as PCEA53-b-P(tBA94-co-Sty258)), put it into a 50mL single Add 10mL of dichloromethane and 2mL of trifluoroacetic acid into a round-bottomed flask, and hydrolyze in the dark for 24 hours to obtain polyacrylic acid ethyl cinnamate 53-intercalated-(polyacrylic acid 94-copolymerized-polystyrene 258), (PCEA53 -b-P(AA94-co-Sty258)), spin concentration to remove solvent and trifluoroacetic acid, add a certain amount of dichloromethane to it, and make it volatilize at room temperature, the resulting sample is PCEA53-b-P(AA94-co-Sty258 ) after vacuum drying for 24 h and stored in the refrigerator.

[0049] (2) SiO 2 Preparation of hollow microspheres

[0050] Take 0.005g polyacrylic acid ethy...

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Abstract

The invention discloses a hedgehog SiO2 hollow microsphere and preparation method thereof. Block polymer is taken as soft template; block polymer solution is added into organic solvent / water two-phase system, so as to form stable emulsion, co-guiding agent and silicon source are dissolved in organic solvent and mixed to be uniform, and the emulsion is added; under the conditions of faintly acid and alkalescence, silicon precursor is hydrolyzed and condensed; then drying and calcination subsequent treatment are carried out; and finally the hedgedog SiO2 hollow microsphere is obtained. The invention is easy to implement and is economic and practicable, the grain diameter distribution of the prepared hedgedog SiO2 hollow microsphere is uniform, and the cavity diameter and spinous density are adjustable.

Description

technical field [0001] The invention relates to the field of inorganic materials, in particular to a hedgehog-shaped SiO 2 Preparation method of hollow microspheres. Background technique [0002] Hollow spheres have the characteristics of low density, large specific surface area, high surface activity, and strong surface permeability. It has important commercial value and broad application prospects in the fields of active catalysts and catalyst supports. SiO 2 It has the advantages of non-toxicity and good biocompatibility, so SiO 2 Hollow spheres have good development prospects. [0003] Currently, SiO 2 The preparation method of the hollow sphere is mainly the template method, including the hard template method and the soft template method. The advantage of the hard template method is that it has a narrow particle size distribution; but its disadvantage is that the regularity and thickness of the hollow microsphere shell largely depend on the surface properties of t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/18
Inventor 胡继文李银辉
Owner GUANGZHOU CHEM CO LTD CHINESE ACADEMY OF SCI
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