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Preparation method of silica gel filler

A spherical silica gel, silica gel technology, applied in chemical instruments and methods, silicon compounds, alkali metal oxides/hydroxides, etc., can solve the problem of low bonding efficiency, small active points or catalytic points, affecting the chemical properties of silica gel surface and other problems to achieve good chromatographic performance

Pending Publication Date: 2021-06-22
南京宜凯瑞新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] However, due to the existence of impurities such as silanol and metal ions that often remain in silica gel, the surface chemical properties of silica gel are affected, and the interference of metal impurities in the silica gel structure makes the bonding efficiency not high, and some metals may become small active points. Or catalytic sites, which enable the packing matrix to produce catalytic effects and non-specific adsorption

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] A preparation method for a spherical silica gel filler, comprising the following preparation steps:

[0019] Step 1, purifying tetraethoxysilane by distillation under reduced pressure;

[0020] Step 2, take the tetraethoxysilane in step 1, add it to a three-necked flask, add absolute ethanol according to the mass ratio of tetraethoxysilane: absolute ethanol = 1:2, and stir at 40°C for 30 minutes;

[0021] Step 3, add a molar concentration of 0.8% stabilizer, 1.8% catalyst, and 2.5% porogen to the above system in turn, keep the stirring speed constant, stir for 80 minutes, and slowly heat up to 110°C;

[0022] Step 4, use a vacuum vacuum distillation device to carry out vacuum distillation at a temperature of 115°C for 2 hours under a vacuum condition of 110 Pa, and remove all volatile substances to obtain polyethoxysilane;

[0023] Step 5, preparing an aqueous ethanol solution with a mass ratio of 10%, controlling the reaction temperature to 50°C and a stirring speed o...

Embodiment 2

[0028] A preparation method for a spherical silica gel filler, comprising the following preparation steps:

[0029] Step 1, purifying tetraethoxysilane by distillation under reduced pressure;

[0030] Step 2, take the tetraethoxysilane in step 1, add it to a three-necked flask, add absolute ethanol according to the mass ratio of tetraethoxysilane: absolute ethanol = 1:2, and stir at 40°C for 30 minutes;

[0031] Step 3, adding a molar concentration of 1.2% stabilizer, 2.0% catalyst, and 3.5% porogen to the above system in turn, keep the stirring speed constant, stir for 80min, and slowly heat up to 110°C;

[0032] Step 4, use a vacuum vacuum distillation device to carry out vacuum distillation at a temperature of 125°C for 2.5 hours under vacuum conditions of 120 Pa, and remove all volatile substances to obtain polyethoxysilane;

[0033] Step 5, preparing an aqueous ethanol solution with a mass ratio of 20%, controlling the reaction temperature to 50°C and a stirring speed of...

Embodiment 3

[0038] A preparation method for a spherical silica gel filler, comprising the following preparation steps:

[0039] Step 1, purifying tetraethoxysilane by distillation under reduced pressure;

[0040] Step 2, take the tetraethoxysilane in step 1, add it to a three-necked flask, add absolute ethanol according to the mass ratio of tetraethoxysilane: absolute ethanol = 1:2, and stir at 40°C for 30 minutes;

[0041] Step 3: Add 1.0% stabilizer, 1.9% catalyst, and 3% porogen to the above system in turn, keep the stirring speed constant, stir for 80 minutes, and slowly raise the temperature to 110°C;

[0042] Step 4, use a vacuum vacuum distillation device to carry out vacuum distillation at a temperature of 120°C for 2 hours under vacuum conditions of 115 Pa, and remove all volatile substances to obtain polyethoxysilane;

[0043] Step 5, preparing an aqueous ethanol solution with a mass ratio of 15%, controlling the reaction temperature to 50°C and a stirring speed of 800r / min, sl...

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PUM

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Abstract

The invention discloses a preparation method of a spherical silica gel filler. The preparation method comprises the following preparation steps: purification of a raw material tetraethoxysilane, synthesis and post-treatment of polyethoxysilane, and synthesis and drying of the spherical silica gel filler. According to the preparation method of the spherical silica gel filler provided by the invention, the spherical silica gel prepared by the preparation method is good in regularity and chromatographic performance, and can be widely applied as a chromatographic filler matrix for rapidly separating chemical or biological macromolecules.

Description

technical field [0001] The invention relates to the technical field of silica gel adsorption fillers, in particular to a method for preparing spherical silica gel fillers. Background technique [0002] Silica gel is an inorganic matrix filler, the main chemical composition is silicon dioxide, which has very high mechanical strength, good filling stability and excellent chemical stability. In addition, the surface of silica gel has special surface chemical properties, and the surface of silica gel is also Rich in silanol, it is the basis for the surface chemical bonding or modification of silica gel. The process of filtering silica gel as a filler is essentially a process of interaction between solute, mobile phase and stationary phase. [0003] However, due to the existence of impurities such as silanol and metal ions that often remain in silica gel, the surface chemical properties of silica gel are affected, and the interference of metal impurities in the silica gel structu...

Claims

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Application Information

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IPC IPC(8): B01J20/30B01J20/10B01J20/28
CPCB01J20/103B01J20/28019B01J20/28054
Inventor 石鹏杰王家兵周颂阳周中凯
Owner 南京宜凯瑞新材料有限公司
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