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A kind of preparation method of controllable water-absorbing silicon dioxide microsphere

A technology of silica and microspheres, applied in the direction of silica, silica, etc., can solve the problems of difficult control of water absorption, reduction of purification stability and repeatability, and difficulty in repeating purification results, etc., to achieve a simple and easy-to-control process , excellent mechanical stability, the effect of narrow pore size distribution

Active Publication Date: 2017-09-12
JIANGSU HECHENG ADVANCED MATERIALS
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  • Abstract
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Problems solved by technology

[0003] Traditional chromatographic separation often uses reversed-phase silica gel packing as the separation and purification matrix. The common ones are C18, C8, C6, phenyl, amino, cyano and other bonded phases, which can be used for the separation and purification of substances in biomedicine, chemical engineering and related fields. However, because this kind of stationary phase substrate often cooperates with organic solvent-water as the mobile phase for separation and purification, it is not suitable for use in the field of electronic material purification; although normal phase silica gel often uses organic solvents as mobile phase, normal phase silica gel has Strong hygroscopicity, and the purified sample may also contain water. Different water absorption rates seriously affect the adsorption performance of normal phase silica gel, making it difficult to repeat the purification results, greatly affecting the purification quality of the product, and reducing the stability and repeatability of the purification.
[0004] Patent No. ZL 2010 1 0207767.3 "A Preparation Method for High-Purity Spherical Fully Porous Silica Gel Particles" describes a synthesis and preparation process of a porous spherical silica gel medium. The particles synthesized by this method have a good mesoporous structure, but as It is difficult to control the water absorption when the normal phase packing is used; the patent No. ZL 20101 0208014.4 "Preparation method of trifunctional n-octadecyl bonded phase" describes a preparation method of tC18 reverse phase silica gel particles. Particles are suitable for the separation and purification of samples under water / organic systems, and have a wide range of applications, but it is difficult to control the moisture content in electronic materials

Method used

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  • A kind of preparation method of controllable water-absorbing silicon dioxide microsphere
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  • A kind of preparation method of controllable water-absorbing silicon dioxide microsphere

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Experimental program
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Effect test

Embodiment 1

[0043] Preparation of controllable water-absorbing silica microspheres

[0044] The preparation steps are as follows

[0045] 1) Add 281.25g of ethyl orthosilicate and 26.75g of triethoxymethylsilane into 217.68g of absolute ethanol, stir magnetically until completely dispersed and form a homogeneous phase.

[0046] 2) Add 52.84g of 0.1M HCl dropwise to the solution obtained in step 1) under magnetic stirring, raise the temperature to 70°C, and keep at this temperature for 20h to partially hydrolyze the silicon source to form a silica sol.

[0047] 3), the sol obtained in step 2) removes the solvent by rotary evaporation.

[0048] 4) Take 20 g of the sol obtained in step 3), add 1 g of toluene, and stir magnetically to make it homogeneous.

[0049] 5), step 4) the oil phase prepared is dispersed in 100g H 2 O and 2g of surfactant (HBL=14pan80:Tween80=1:10) in the aqueous phase. Emulsify for 3h under magnetic stirring at 500r / min.

[0050] 6) Add 15mL of ammonia water (15%...

Embodiment 2

[0054] Preparation of controllable water-absorbing silica microspheres

[0055] The preparation steps are as follows

[0056] 1) Add 156.25g of methyl orthosilicate and 133.72g of triethoxymethylsilane into 217.68g of absolute ethanol, stir magnetically until completely dispersed and form a homogeneous phase.

[0057] 2) Add 52.84g of 0.1M HCl dropwise to the solution obtained in step 1) under magnetic stirring, raise the temperature to 70°C, and keep at this temperature for 20h to partially hydrolyze the silicon source to form a silica sol.

[0058] 3), the sol obtained in step 2) removes the solvent by rotary evaporation.

[0059] 4) Take 20 g of the sol obtained in step 3), add 1 g of toluene, and stir magnetically to make it homogeneous.

[0060] 5), step 4) the oil phase prepared is dispersed in 100g H 2 O and 2g of surfactant (HBL=14pan80:Tween80=1:10) in the aqueous phase. Emulsify for 3h under magnetic stirring at 500r / min.

[0061] 6) Add 15mL of ammonia water (1...

Embodiment 3

[0065] Preparation of controllable water-absorbing silica microspheres

[0066] The preparation steps are as follows

[0067] 1) Add 31.25g of ethyl orthosilicate and 240.70g of triethoxymethylsilane into 217.68g of absolute ethanol, stir magnetically until completely dispersed and form a homogeneous phase.

[0068] 2) Add 52.84g of 0.1M HCl dropwise to the solution obtained in step 1) under magnetic stirring, raise the temperature to 70°C, and keep at this temperature for 20h to partially hydrolyze the silicon source to form a silica sol.

[0069] 3), the sol obtained in step 2) removes the solvent by rotary evaporation.

[0070] 4) Take 20 g of the sol obtained in step 3), add 1 g of toluene, and stir magnetically to make it homogeneous.

[0071] 5), step 4) the oil phase prepared is dispersed in 100g H 2 O and 2g of surfactant (HBL=14pan80:Tween80=1:10) in the aqueous phase. Emulsify for 3h under magnetic stirring at 500r / min.

[0072] 6) Add 15mL of ammonia water (15%...

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Abstract

The invention provides a method for preparing controllable water-absorbing silicon dioxide microspheres, and belongs to the technical field of chromatographic support particle synthesis. A controllable water-absorbing silicon dioxide material has a microsphere structure macroscopically and a mesoporous structure microscopically, and meanwhile synthesized hybridized silica gel has high a high-activity surface, narrow aperture distribution and excellent mechanical stability, and by adopting the method for preparing the controllable water-absorbing silicon dioxide microspheres, the silicon dioxide microspheres with controllable water-absorbing properties can be easily and conveniently prepared.

Description

technical field [0001] The invention belongs to the technical field of liquid chromatography stationary phase particle synthesis, in particular to a method for synthesizing controllable water-absorbing silica microspheres specially used in the field of electronic material purification. Background technique [0002] Electronic materials often have strict control standards for water content, such as liquid crystal materials, the doping of water will greatly affect its dielectric properties, thereby affecting the display effect, so it needs to be removed as much as possible. [0003] Traditional chromatographic separation often uses reversed-phase silica gel packing as the separation and purification matrix. The common ones are C18, C8, C6, phenyl, amino, cyano and other bonded phases, which can be used for the separation and purification of substances in biomedicine, chemical engineering and related fields. However, because this kind of stationary phase substrate often coopera...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B33/18
CPCC01B33/18C01P2004/32C01P2004/61
Inventor 黄晓康庄胡娟刘钰黄曦靳灿辉黄达
Owner JIANGSU HECHENG ADVANCED MATERIALS
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