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Method for preparing surface patterned SiO2 hollow microsphere

A silicon dioxide and surface patterning technology, applied in the field of chemistry or physics, can solve the problems of difficult formation of a single type of particles, poor self-assembly stability, poor dispersion, etc., to achieve a feasible process, short reaction time, and simple operation Effect

Inactive Publication Date: 2009-07-01
SHAANXI NORMAL UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For example, the method of removing polymer cores to synthesize hollow microspheres has many procedures, but its size is controllable; using molecular self-assembly as a template, the preparation process is simple, but due to the poor stability of self-assembly, it is not easy to form a single type of particle. and poor dispersion

Method used

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  • Method for preparing surface patterned SiO2 hollow microsphere
  • Method for preparing surface patterned SiO2 hollow microsphere
  • Method for preparing surface patterned SiO2 hollow microsphere

Examples

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Comparison scheme
Effect test

Embodiment 1

[0038] This embodiment provides the preparation method of surface patterned silicon dioxide hollow microspheres, and its process steps are as follows:

[0039] 1. Preparation of mixed surfactants

[0040] Mix Span-80 and Tween-80 at a weight ratio of 5:1 to prepare a mixed surfactant.

[0041] 2. Preparation of synthetic template oil phase

[0042] Add the mixed surfactant prepared in step 1 into a three-necked flask filled with n-heptane, and mix the mixed surfactant and n-heptane at a weight ratio of 1:122 to prepare a synthetic template oil phase.

[0043] 3. Preparation of emulsion

[0044] Put the synthetic template oil phase prepared in step 2 into a three-necked flask, stir with a stirrer at a stirring speed of 360-400 rpm, and inject N at a flow rate of 2-3ml / min. 2 , emulsified at 25 ° C for 40 to 60 minutes to make an emulsion.

[0045] 4. Preparation of water phase

[0046] Mix N,N'-methylene dienamide, ammonium persulfate, and N-isopropylacrylamide in a molar ra...

Embodiment 2

[0058] In the process step 2 of this embodiment, the mixed surfactant and n-heptane are mixed in a weight ratio of 1:115 to form a synthetic template oil phase. In step 3, the emulsification temperature was 18°C. In process step 4, the molar ratio of acrylic acid to NaOH is 1:0.3 to prepare a sodium acrylate aqueous solution with a concentration of 23%. In process step 8, the reaction time was 2 hours. In process step 9, the calcination temperature is 300° C., and the calcination time is 5 hours. Other processing steps are identical with embodiment 1.

Embodiment 3

[0060] In the process step 2 of this embodiment, the mixed surfactant and n-heptane are mixed in a weight ratio of 1:130 to prepare a synthetic template oil phase. In step 3, the emulsification temperature was 30°C. In process step 4, the molar ratio of acrylic acid to NaOH is 1:1 to prepare a sodium acrylate aqueous solution with a concentration of 23%. In process step 8, the reaction time was 12 hours. In process step 9, the calcination temperature is 550° C., and the calcination time is 3 hours. Other processing steps are identical with embodiment 1.

[0061] In order to determine the best processing step of the present invention, the inventor has carried out a large amount of laboratory research tests, and various test situations are as follows:

[0062] 1. Effect of reaction time on the shell thickness of silica hollow microspheres

[0063] Swell the copolymerized microgel with 2.5mL of ammonia water with a concentration of 25-28%, and add it to the deposited oil phas...

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Abstract

A method for preparing surface-patterned silica hollow microspheres, comprising preparing a mixed surfactant, preparing a synthetic template oil phase, preparing an emulsion, preparing an aqueous phase, preparing a copolymerized microgel, preparing a swollen copolymerized microgel, The steps of preparing a mixed solution of tetraethoxy-n-silane and n-heptane, preparing surface-patterned silicon dioxide polymer composite microspheres, and preparing surface-patterned silicon dioxide hollow microspheres. Compared with the existing preparation method, the present invention has the advantages of reasonable design, feasible process, simple operation, easy control of SiO2 shell thickness, short reaction time, etc. The surface patterned silica hollow microspheres prepared by the present invention have the advantages of The advantages of large specific surface and relatively small mass can be widely used in biomedicine, wave absorption and shock absorption, catalyst loading, rapid enrichment and separation, sensing technology, environmental protection, marine mining and other fields.

Description

technical field [0001] The invention belongs to the technical field of chemical or physical methods, and in particular relates to the manufacture of colloid chemical microcapsules or microspheres. Background technique [0002] Silica hollow microsphere materials have special properties different from those prepared by other methods, such as strong surface modification and easy separation, so they have become a large class of materials widely used in the field of colloid and material science. There are many reports on the preparation methods of silica hollow microspheres at home and abroad. There are mainly two methods, that is, to prepare core / shell composite microspheres first, and then remove the internal polymer core through calcination or dissolution; The self-assembled body is a template, and the hollow microsphere material is obtained through a self-assembled method. Both approaches have their pros and cons. For example, the method of removing polymer cores to synthe...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J13/02
Inventor 胡道道杨菊香房喻白超良沈淑坤宋少飞孙永亮
Owner SHAANXI NORMAL UNIV
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