Mesoporous silica (SiO2) and preparation method thereof

A mesoporous silica and mesoporous technology, applied in the field of silica gel fillers, can solve the problems of complex preparation process, high cost, and increased production cost, and achieve the effect of simplifying the original process

Active Publication Date: 2019-10-18
中谱科技(福州)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The development of this material mainly stems from the fact that in the 1960s, Stober et al. used alkali-catalyzed hydrolysis of ethyl orthosilicate to prepare SiO2 materials, and SiO2 prepared by the sol-gel method. Not only has high purity, but also has good uniformity. The disadvantage is that the preparation process takes a long time, the cost is high, and the prepared SiO2 has no pores. If it is us

Method used

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  • Mesoporous silica (SiO2) and preparation method thereof
  • Mesoporous silica (SiO2) and preparation method thereof
  • Mesoporous silica (SiO2) and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] (1) First weigh 3g of TX-100 surfactant, then add it into 50mL of sulfuric acid solution (3mol / L) and stir vigorously at 50°C for 24h (stirring speed is 600r / min) to fully dissolve it. After the stirring was completed, 10 mL of porogen ethanol was added and the stirring was continued for 12 h to obtain a mixed solution A. Then add olivine with a certain particle size (0.5mm) to the above mixed solution A, and continue to stir vigorously at 50°C for 24h (stirring rate is 700r / min), after the stirring is completed, the obtained mesoporous silicon precursor is decanted It is separated from unreacted substances, and at the same time, the impurity components in olivine are also dissolved by acid, and aged at 60°C for 12h. Among them, the TX-100 surfactant promotes the silicon in olivine to form an ordered combination by virtue of its special amphiphilicity, and the porogen effectively fills the combination, and then continues to separate the aged silicon precursor Wash with...

Embodiment 2

[0032] (1) First weigh 4g of TX-10 surfactant, then add it into 55mL of sulfuric acid solution (4mol / L) and stir vigorously at 40°C for 24h (stirring speed is 500r / min) to fully dissolve it. After the stirring was completed, 8 mL of porogen glycerol was added and the stirring was continued for 16 h to obtain a mixed solution A. Next, olivine with a certain particle size (0.8mm) was added to the above mixed solution A, and continued to stir vigorously at 40°C for 16h (stirring rate was 600r / min), and after the stirring was completed, the obtained mesoporous silicon precursor was decanted It is separated from unreacted substances, and at the same time, the impurity components in olivine are also dissolved by acid, and aged at 60 ° C for 8 hours. Among them, the TX-100 surfactant promotes the silicon in olivine to form an ordered combination by virtue of its special amphiphilicity, and the porogen effectively fills the combination, and then continues to separate the aged silicon ...

Embodiment 3

[0035] (1) First weigh 3.5g of SE-10 surfactant, then add it into 40mL of hydrochloric acid solution (5mol / L) and stir vigorously at 35°C for 24h (stirring speed is 400r / min) to fully dissolve it. After the stirring was completed, 5 mL of porogen heptane was added and the stirring was continued for 10 h to obtain a mixed solution A. Next, serpentine with a certain particle size (1.0mm) was added to the above mixed solution A, and continued to stir vigorously at 35°C for 16h (stirring rate was 500r / min). After the stirring was completed, the obtained mesoporous silicon precursor was decanted The body is separated from the unreacted substance, and at the same time, the impurity components in the serpentine are also dissolved by acid, and aged at 60 ° C for 10 h. Among them, the TX-100 surfactant promotes the silicon in the serpentine to form an ordered combination by virtue of its special amphiphilicity, and the porogen effectively fills the combination, and then continues to re...

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Abstract

The invention provides mesoporous silica (SiO2) and a preparation method and application thereof, and belongs to the field of silicone fillers. The specific surface area of the mesoporous SiO2 is 367-407 m2/g, and the average pore diameter is 11.26-13.65 nm; and the content of surface hydroxyl is 0.498-0.541 mmol/g. The method for preparing the mesoporous SiO2 comprises the steps: a natural mineral (olivine or serpentine) is adopted as a silicon source, the mesoporous SiO2 is prepared through a one-step method, firstly the natural mineral silicon source is added into an acid, surfactant and porogenic agent mixed solution, the mixture is stirred for a period of time at the specific temperature to sufficiently react, after reacting is completed, centrifugal separation is conducted, a silicon-containing precursor is obtained, the silicon-containing precursor is subjected to still standing, filtered, washed and dried and then calcined at the high temperature, then the mesoporous SiO2 is obtained, and then the obtained mesoporous SiO2 is bonded to C18 and then used for high performance liquid chromatography fillers.

Description

technical field [0001] The invention belongs to the field of silica gel fillers, and in particular relates to a mesoporous silica and a preparation method thereof. Background technique [0002] With the continuous development of science and technology fields such as machinery, optics and electronics, the separation of various substances by chromatography has been rapidly developed and widely used in various industries. In particular, high performance liquid chromatography (HPLC), as an important branch of chromatography, has played a pivotal role in the fields of food, biology, medicine and chemical industry, and has become an indispensable detection method in current research. In this field, the chromatographic column plays a very key role, and the chromatographic column packing, as the key to restricting the separation performance of high performance liquid chromatography, has become the direction of the majority of researchers. [0003] At present, commonly used chromato...

Claims

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Application Information

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IPC IPC(8): C01B33/12B01D15/20
CPCC01B33/12B01D15/206C01P2006/12C01P2006/16
Inventor 张基明
Owner 中谱科技(福州)有限公司
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