Hollow microsphere and its preparation method

A microsphere and hollow technology, applied in the field of hollow microspheres and their preparation, can solve the problems of cumbersome process, compound hollow microspheres have not yet been synthesized, and difficulty in industrialization

Inactive Publication Date: 2012-11-07
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The core-shell structure template method is a widely used method to prepare hollow spheres, but the bottleneck problems such as strict preparation conditions, cumbersome process, easy shell rupture when removing the template, and difficulty in industrialization have seriously affected the application of hollow spheres.
[0005] In industry, spray-drying technology has been widely used in the preparation of powder materials, but the reports about spray-drying technology to prepare hollow microspheres mainly focus on the research on the spray-drying process of specific compounds, most of the compounds (such as Phenolic) hollow microspheres have not yet been synthesized

Method used

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  • Hollow microsphere and its preparation method
  • Hollow microsphere and its preparation method

Examples

Experimental program
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Effect test

Embodiment 1

[0049] Embodiment 1, utilizing method one to prepare hollow microspheres

[0050] 1) 9.0g inorganic precursor TEOS (tetraethyl orthosilicate Si(OCH 2 CH 3 ) 4 ) and 3.0 mL of hydrochloric acid with a concentration of 2 mol / L were dissolved in 87 g of acetone, and after reflux at 60°C for 4 hours, 1 g of ethyl 2-cyanoacrylate was added and mixed evenly to obtain a mixed solution; the obtained mixed solution was pumped into The air-flow spray drying equipment adopts the co-current drying method for drying. The atomization device of the spray dryer adopts a two-flow nozzle, and the feeding speed of the mixed liquid is 15mL / min; the gas flow rate of the nozzle is controlled by the pressure of the compressed air, and the gas flow rate It is 30L / h; control the feed temperature (i.e. the air inlet temperature) to 25°C, and the outlet air is separated and emptied by a primary vortex to obtain hollow microspheres a;

[0051] The SEM photograph of this hollow microsphere a is as fi...

Embodiment 2

[0054] According to the same experimental conditions and step 1) as in Example 1, only step 2) the acetone used in the soaking step is replaced with hydrofluoric acid with a mass percentage concentration of 10%, and the hollow microspheres are removed after soaking with this hydrofluoric acid Silica in a, the material that obtains the wall that the present invention provides is the hollow microsphere of polyethyl 2-cyanoacrylate, and its SEM picture is as follows Figure 4 shown. Depend on Figure 4 It can be seen that the particle size of the microspheres is 500nm-50μm. After the treatment with hydrofluoric acid, the microspheres adhere to each other, and a small amount of microspheres collapse or even rupture.

Embodiment 3

[0056] According to the same experimental conditions and step 1) as in Example 1, only after step 1) and before step 2), the obtained hollow microsphere a was heat-treated at 350° C. for 24 hours to obtain hollow microsphere b. After the same step 2) as in Example 1, the material forming the wall provided by the present invention is a hollow microsphere of silicon dioxide. SEM observation shows that the particle diameter of the microsphere is 500nm-50 μm, and the wall is 100nm- 1 μm.

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Abstract

The invention discloses a hollow microsphere and its preparation method. In allusion to disadvantages of a traditional core-shell template method for preparation of a hollow microsphere, an alkene monomer with a rapid polymerization characteristic is fully utilized and a spray drying technology is combined in the invention. According to the preparation method, a layer of polymer shell is rapidly formed on the surface of a liquid drop, and by the utilization of a solvent for evaporation-induction, a shell formation substance grows on the interior surface of the polymer shell. Therefore, the hollow microsphere with a composite structure is prepared. Through adjusting experiment conditions and material components, the composition, structure and properties of the hollow microsphere are controllable. The method provided by the invention is a hollow microsphere preparation method with certain universality.

Description

technical field [0001] The invention relates to the field of material preparation, and relates to a class of hollow microspheres and a preparation method thereof. Background technique [0002] In recent years, due to the unique optical, electrical, mechanical, chemical and other properties brought about by changes in the size, composition, and structural order of materials, a large number of researches on materials with special functions have been carried out. [0003] Hollow sphere materials have attracted extensive attention of researchers due to their important theoretical and practical application values. The cavity inside the hollow sphere can be coated with a large number of guest molecules or nanoparticles, and can be used as a capsule material in the fields of medicine, cosmetics, fragrances, paints, inks, etc.; it can also be used as a confined reaction vessel, dye dispersant, lightweight filler , sound-absorbing materials, heat storage and flame-retardant material...

Claims

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Application Information

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IPC IPC(8): B01J13/02
Inventor 杨振忠沈轲梁福鑫刘继广
Owner INST OF CHEM CHINESE ACAD OF SCI
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