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

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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 t

Method used

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Examples

Experimental program
Comparison scheme
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Example Embodiment

[0017] Example 1】

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

[0019] Step 1, tetraethoxysilane is subjected to pressure reduction distillation;

[0020] Step 2, take the tetraethoxysilane in steps, adding a three-neck flask, anhydrous ethanol is added in a mass of tetraethoxysilane: anhydrous ethanol = 1: 2, and stirring at 40 ° C for 30 min;

[0021] Step three, sequentially add a stabilizer of 0.8%, 1.8% catalyst, 2.5% porolescent agent, and keep the stirring speed unchanged, stirred by stirring to 110 ° C.

[0022] Step 4, using a vacuum decompression distillation apparatus, under vacuum conditions 110Pa, pressure distillation 2H was carried out at a temperature 115 ° C, and all volatile substances were removed, i.e., polyethoxysilane;

[0023] Step 5. The preparation of the product is 10% aqueous ethanol, the control reaction temperature is 50 ° C and the stirring speed is 800 r / min, and the polyethoxysilane is s...

Example Embodiment

[0027] [Example 2]

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

[0029] Step 1, tetraethoxysilane is subjected to pressure reduction distillation;

[0030] Step 2, take the tetraethoxysilane in steps, adding a three-neck flask, anhydrous ethanol is added in a mass of tetraethoxysilane: anhydrous ethanol = 1: 2, and stirring at 40 ° C for 30 min;

[0031] Step three, adding a molar concentration of 1.2% to a stabilizer, 2.0% catalyst, 3.5% porolescent agent to maintain the stirring speed, stir for 80 min, and slowly warmed to 110 ° C.

[0032] Step 4, using a vacuum decompression distillation apparatus, under vacuum conditions 120Pa, the temperature of 125 ° C was evaporated for 2.5 h, and all volatile substances were removed, i.e., the polyethoxysilane was obtained.

[0033] Step 5, the preparation of the mass ratio of 20% ethanol, the control reaction temperature is 50 ° C and the stirring speed is 800 r / min, and the ...

Example Embodiment

[0037] [Example 3]

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

[0039] Step 1, tetraethoxysilane is subjected to pressure reduction distillation;

[0040] Step 2, take the tetraethoxysilane in steps, adding a three-neck flask, anhydrous ethanol is added in a mass of tetraethoxysilane: anhydrous ethanol = 1: 2, and stirring at 40 ° C for 30 min;

[0041] Step three, adding a molar concentration of 1.0% of a stabilizer, 1.9% catalyst, 3% porolescent agent, retaining the stirring speed, stirring at 120 mination, and then warmed to 110 ° C.

[0042] Step 4, using a vacuum decompression distillation apparatus, under vacuum conditions 115 Pa, the temperature of 120 ° C is reduced pressure, and all volatile substances are removed, i.e., to obtain polyethoxysilane;

[0043] Step 5. The preparation of the mass ratio of 15% of the ethanol solution, the control reaction temperature is 50 ° C and the stirring speed is 800 r / min, ...

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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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