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Method for preparing hollow silicon dioxide microsphere with controllable wall thickness by taking polystyrene microsphere as template

A technology of polystyrene microspheres and silicon dioxide, which is applied in the production of silicon dioxide, silicon oxide, and bulk chemicals, can solve the problems of no inorganic hollow microspheres, and achieve uniform size, simple process, and easy operation easy effect

Inactive Publication Date: 2010-08-18
DO FLUORIDE CHEM CO LTD +1
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Problems solved by technology

But so far, there is no literature report on the preparation and modification of composite microspheres by using supercritical carbon dioxide to carry inorganic precursors into polymer microspheres, and there is no report on the use of supercritical carbon dioxide to carry inorganic precursors into polymer microspheres. Bibliographic reports on the preparation of inorganic hollow microspheres with controllable wall thickness

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  • Method for preparing hollow silicon dioxide microsphere with controllable wall thickness by taking polystyrene microsphere as template
  • Method for preparing hollow silicon dioxide microsphere with controllable wall thickness by taking polystyrene microsphere as template
  • Method for preparing hollow silicon dioxide microsphere with controllable wall thickness by taking polystyrene microsphere as template

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Embodiment 1

[0033] The cross-linked polystyrene microspheres were prepared by using EGDMA as a cross-linking agent, and the specific experimental process was as follows: a 250ml three-necked bottle equipped with a mechanical stirrer and a reflux condensing device was placed in a constant temperature water bath. Then add 90ml deionized water, 0.24gNaHCO 3 , 1.2ml methacrylic acid and 10ml styrene. The rate of mechanical stirring was maintained at 250 rpm under the protection of nitrogen and the temperature of the system was raised to 70°C. After constant temperature for 30 minutes, 10 ml of an aqueous solution dissolved with 0.08 g of potassium persulfate was added to the reaction system as an initiator. When the polymerization was carried out for 1 h, 0.3 ml of EGDMA was added as a cross-linking agent. Then polymerized at 70° C. for 24 hours to obtain cross-linked polystyrene microspheres with a cross-linking degree of 3%.

[0034]The degree of cross-linking of the polystyrene microsph...

Embodiment 2

[0037] In the present embodiment, it is specifically divided into the following 5 systems, and the wall thickness of the hollow silica microspheres is studied with the consumption of tetraethyl orthosilicate (system 1), the consumption of cross-linked polystyrene microspheres (system 2), Reaction time (system 3), system pressure (system 4), the variation trend of the addition amount (system 5) of tetraethyl orthosilicate in the hydrolysis process, specifically as follows:

[0038] Example 2.1 Add 2ml of tetraethyl orthosilicate (TEOS) to the bottom of a 50ml supercritical reactor at a constant temperature of 40°C. Take by weighing the cross-linked polystyrene microsphere that 0.2g embodiment 1 prepares simultaneously, be placed in the stainless steel cage supporting use with supercritical reactor after being wrapped with filter cloth, then stainless steel cage is placed on supercritical reactor (stainless steel The cage is 6 cm from the bottom of the reactor). Inject CO into ...

Embodiment 28

[0053] Embodiment 2.8 regulates the system pressure to 9Mpa, others are the same as embodiment 2.1.

[0054] Embodiment 2.9 regulates the system pressure to 25Mpa, and others are the same as embodiment 2.1.

[0055] figure 1 , 8 , 9 are respectively the transmission electron microscope picture (TEM) of embodiment 2.1, embodiment 2.8, embodiment 2.9 gained hollow carbon dioxide microspheres: as can be seen from this series of figures, along with system pressure becomes 10Mpa by 9Mpa, becomes again 25Mpa, the wall thickness of hollow silica microspheres correspondingly changes from 15nm to 20nm, and then to 29nm, indicating that as the system pressure increases, the wall thickness of hollow silica microspheres also increases to a certain extent.

[0056] System 5: The amount of fixed cross-linked polystyrene microspheres is 0.2g, the amount of ethyl orthosilicate is 2ml, the system pressure is 10Mpa, the reaction time is 10h, and the amount of ethyl orthosilicate added during ...

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Abstract

The invention discloses a method for preparing hollow silicon dioxide microsphere with controllable wall thickness by taking polystyrene microsphere as the template, which includes the steps of, according to weight / volume proportion, putting 0.05-0.5g of polystyrene microsphere and 1-8ml of tetraethoxysilane in a supercritical reactor with constant temperature of 25-60 DEG without contacting each other, introducing carbon dioxide to the supercritical reactor until the pressure reaches 9-25MPa, reacting for 1-10h, relieving the pressure to the normal pressure, opening the reactor to get out of the processed polystyrene microsphere to obtain compound microsphere, dispersing the compound microsphere in the mixture solution of 0.3-4ml of ammonia and 10ml of ethanol, at the same time adding 0-0.66ml of tetraethoxysilane to the mixture solution, hydrolyzing for 2-24h under 20-40 DEG C, separating the solid and the liquid of the system after the hydrolysis process, and sintering the compound microsphere which is separated out. In this way, the hollow silicon dioxide microsphere can be obtained. The method finishes the modification of the polymer microshere and the implantation of the inorganic presoma in one step, and is simple in process, simple and convenient to operate, energy-saving and environment-friendly, and the hollow silicon dioxide microsphere prepared through the method has controllable wall thickness.

Description

technical field [0001] The invention belongs to the technical field of preparation of inorganic hollow microspheres, and in particular relates to a method for preparing hollow silicon dioxide microspheres with controllable wall thickness by using polystyrene microspheres as templates. Background technique [0002] Because hollow silica microspheres have a wide range of application prospects in controlled release, artificial cells, lightweight fillers, catalysis and confinement reactors, etc., at the same time, they have good biocompatibility, low density and High thermal and mechanical stability and other characteristics, so the research on its preparation and properties has aroused the great interest of the majority of scientific and technical workers. At present, the conventional methods for preparing hollow silica microspheres mainly include layer-by-layer deposition method, polymer microsphere sulfonation method and so on. Although these methods can prepare hollow silic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/12
CPCY02P20/54
Inventor 李世江陈志民罗成果许群
Owner DO FLUORIDE CHEM CO LTD
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