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A kind of porous silicon oxide microsphere and its preparation method and application

A technology of porous silica and microspheres, which is applied in the field of silica gel packing, can solve the problems of long processing time and high preparation cost, and achieve the effects of large specific surface area, promotion of arrangement and polymerization, and good separation effect

Active Publication Date: 2020-12-08
中谱科技(福州)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In 1968, Stober et al. discovered the use of alkali-catalyzed hydrolysis of ethyl orthosilicate to prepare SiO 2 Microspheres, the microspheres prepared by this sol-gel method have high purity and good uniformity, but the preparation cost of this method is high, the processing time is long, and it is non-porous. If it is to be used as a liquid chromatography packing matrix, subsequent expansion is required. A series of operations such as holes

Method used

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  • A kind of porous silicon oxide microsphere and its preparation method and application
  • A kind of porous silicon oxide microsphere and its preparation method and application
  • A kind of porous silicon oxide microsphere and its preparation method and application

Examples

Experimental program
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Embodiment 1

[0037] (1) Preparation of microspheres: Reflux 12mL of absolute ethanol and 20mL of tetraethyl orthosilicate in a microwave synthesizer at 60°C, and drop in the mixed solution at a rate of 0.5mL / min while stirring with a peristaltic pump. Add 5mL of 0.1mol / L hydrochloric acid aqueous solution, let it stand for 20min after the dropwise addition, and then rotate the reaction solution at 50°C for 1h to obtain a partially hydrolyzed viscous oligomer; weigh 5g of oligomer and 30mg of F127 In a three-neck flask, add 20mL of isopropanol to prepare solution A, and at the same time, mix 1.5mL of ammonia water, 40.75mL of absolute ethanol and 2mL of distilled water through ultrasonic mixing to prepare solution B, and use a peristaltic pump at 1mL / min Slowly drop solution A into solution B at the speed of 300r / min, and reprocess it while stirring at 300r / min. After the dropwise addition is completed, let it stand for 30min, wash it with absolute ethanol for 5 times, and then place it in a...

Embodiment 2

[0040]Reflux 25mL of absolute ethanol and 20mL of ethyl orthosilicate in a microwave synthesizer at 60°C, and add 0.1mol / L of 3mL of hydrochloric acid dropwise into the mixed solution at a rate of 0.5mL / min while stirring with a peristaltic pump Aqueous solution, let it stand for 30 minutes after the dropwise addition, and then rotate the reaction solution at 55°C for 2 hours to obtain a partially hydrolyzed viscous oligomer; weigh 5g of the oligomer and 25mg of F108 in a three-necked flask, add 15mL of Prepare solution A with isopropanol. At the same time, mix 3mL of ammonia water, 42mL of absolute ethanol and 5mL of distilled water by ultrasonic mixing to form solution B. Slowly drip solution A into the In solution B, reprocess it while stirring at 250r / min. After the dropwise addition is completed, let it stand for 30min, centrifuge and wash it with absolute ethanol for 5 times, then place it in a vacuum drying oven at 100°C for 24h, and at 550°C Calcined for 4 hours to obt...

Embodiment 3

[0043] Reflux 30mL of absolute ethanol and 15mL of ethyl orthosilicate in a microwave synthesizer at 60°C, and add 0.1mol / L of 7mL of hydrochloric acid dropwise into the mixed solution at a rate of 0.5mL / min while stirring with a peristaltic pump Aqueous solution, let it stand for 25min after the dropwise addition, then rotate the reaction solution at 65°C for 0.5h to obtain a partially hydrolyzed viscous oligomer; weigh 5g oligomer and 20mg P123 in a three-necked flask, add 20mL Prepare solution A with isopropanol, and at the same time, mix 4.5mL of ammonia, 36mL of absolute ethanol and 3mL of distilled water by ultrasonic mixing to form solution B, slowly drop solution A at a speed of 0.8mL / min through a peristaltic pump Put it into solution B, and reprocess it while stirring at 400r / min. After the dropwise addition is completed, let it stand for 90min, wash it with absolute ethanol for 5 times, and then place it in a vacuum drying oven at 80°C for 36h. Calcined at 700°C for...

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Abstract

The invention provides porous silicon oxide microspheres and a preparation method and application thereof, and belongs to the field of silica gel fillers. The porous silicon oxide microspheres have aspecific surface area of 253-323 m<2> / g, an average pore diameter of 10.47-13.63 nanometers and a surface hydroxyl group content of 0.502-0.536 mmol / g. The method for preparing the porous silicon oxide microspheres comprises the steps that an organosilicone solution is put into a microwave synthesizer, after heating is performed to reflux, an acid solution is added dropwise for reflux mixing, andthen low-temperature rotary evaporation is performed to obtain an oligomer; after the oligomer is sufficiently mixed with a pore-forming agent, an alcohol solvent is added to prepare a solution A; ammonium hydroxide, an alcohol solvent and water are mixed to prepare a solution B; the solution A is slowly dropped into the solution B, reprocessing is carried out under stirring, after dropping is completed, standing, washing and drying are carried out, and the porous silicon oxide microspheres are obtained through high-temperature calcination.

Description

technical field [0001] The invention belongs to the field of silica gel fillers, and in particular relates to a porous silicon oxide microsphere and a preparation method and application thereof. Background technique [0002] Since the 1960s, with the continuous development of machinery, optics and electronics, chromatography has been greatly developed and widely used in various industries. Among them, high performance liquid chromatography (HPLC), as an important branch of chromatography, is an indispensable and important means of separation and detection in food, medical, chemical and other important fields. Chromatographic column packing, as the key to restricting the separation performance of high performance liquid chromatography, has become the direction of many researchers. [0003] At present, the commonly used chromatographic packing matrix can be divided into organic matrix, inorganic matrix and organic-inorganic composite matrix stationary phase according to diffe...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/283B01J20/28B01J20/30B01D15/20
CPCB01D15/206B01J20/28021B01J20/283
Inventor 张基明
Owner 中谱科技(福州)有限公司