Preparation method of high-purity porous spherical silica gel filler

A porous spherical, silica gel technology, applied in the field of silica gel adsorption packing, can solve the problems of low bonding efficiency, small active points or catalytic points, and it is difficult to avoid the interference of metal impurities, and achieves the effect of good regularity and good chromatographic performance.

Inactive Publication Date: 2019-06-11
青岛硕远硅胶科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

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. The metal impurities in the silica gel structure usually affect the acidity of silanol, forming a heterogeneous structure, and chelating with the system. Complexation occurs, even if pickling is performed twice, it is difficult to avoid the interference of metal impurities, especially in the process of bonding, this effect makes the bonding efficiency not high, and some metals may become small The active point or catalytic point of the filler matrix can produce catalytic effect and non-specific adsorption

Method used

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  • Preparation method of high-purity porous spherical silica gel filler
  • Preparation method of high-purity porous spherical silica gel filler

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Embodiment 1

[0023] A preparation method of high-purity porous spherical silica gel filler, comprising the following preparation steps:

[0024] Step 1: Purify tetraethoxysilane by distillation under reduced pressure, and then collect it in a clean and dry ground container for later use;

[0025] Step 2: Weigh the purified tetraethoxysilane obtained in step 1, add it to a three-necked flask, add absolute ethanol according to the mass ratio of tetraethoxysilane: absolute ethanol = 1:1.5, and put it at 30°C Stir for 40min, the stirring speed is 350r / min;

[0026] Step 3, add 1.0% stabilizer cyclohexane, 2.0% catalyst hexamethylenetetramine, and 3.0% porogen to the above system in turn, keep the stirring speed constant, stir for 60 minutes, and slowly heat up to 120 ℃, then pass nitrogen to protect, continue to stir and react for 24h to obtain the product after reaction; the porogen is a mixture of polyethylene glycol 400 and sorbitan monooleate with a molar ratio of 2:1, and the The poroge...

Embodiment 2

[0032] A preparation method of high-purity porous spherical silica gel filler, comprising the following preparation steps:

[0033] Step 1: Purify tetraethoxysilane by distillation under reduced pressure, and then collect it in a clean and dry ground container for later use;

[0034] Step 2: Weigh the purified tetraethoxysilane obtained in step 1, add it to a three-necked flask, add absolute ethanol according to the mass ratio of tetraethoxysilane: absolute ethanol = 1:1.5, and put it at 30°C Stir for 40min, the stirring speed is 300r / min;

[0035] Step 3, adding 0.5% stabilizer 2-methylpentane, 1.8% catalyst N,N-dimethylcyclohexylamine, and 2.0% porogen to the above system in sequence, keeping the stirring speed constant, Stir for 60 minutes, slowly raise the temperature to 120°C, then pass nitrogen for protection, continue to stir and react for 24 hours, and obtain the product after the reaction; the porogen is polyethylene glycol 400 and sorbitan monooleate with a molar ra...

Embodiment 3

[0041]A preparation method of high-purity porous spherical silica gel filler, comprising the following preparation steps:

[0042] Step 1: Purify tetraethoxysilane by distillation under reduced pressure, and then collect it in a clean and dry ground container for later use;

[0043] Step 2: Weigh the purified tetraethoxysilane obtained in step 1, add it to a three-necked flask, add absolute ethanol according to the mass ratio of tetraethoxysilane: absolute ethanol = 1:1.5, and put it at 30°C Stir for 40min, the stirring speed is 400r / min;

[0044] Step 3: Add the stabilizer cyclopropane with a molar concentration of 1.5%, 2.3% catalyst N,N-dimethylbenzylamine, and 4.0% porogen to the above system in sequence, keep the stirring speed constant, stir for 60 minutes, and slowly heat up to 120° C., and then pass nitrogen for protection, and continue to stir and react for 24 hours to obtain the reacted product; the porogen is a mixture of polyethylene glycol 400 and sorbitan monool...

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Abstract

The invention discloses a preparation method of a high-purity porous spherical silica gel filler, comprising the following preparation steps: purification of raw material tetraethoxysilane, synthesisand post-treatment of polyethoxysilane, synthesis of the high-purity spherical silica filler, and washing aging, roasting and drying. The invention provides the preparation method of the high-purity porous spherical silica gel filler. The spherical silica gel prepared by the preparation method has good regularity, and the metal impurity content in the porous high-purity silica gel is determined byusing an ICP full spectrum direct reading plasma emission spectrometer, and is as follows: Al: 3.5 mg/kg, Ca: 1 mg/kg, Fe: 1.5 mg/kg, Mg: 2.0 mg/kg, and Na: 1 mg/kg. The metal impurity content is lower than that of domestic silica gel, and the chromatographic performance is good. Under normal-phase and reversed-phase conditions, the column efficiency is about 65,000, and the peak shape is symmetrical. The high-purity porous spherical silica gel filler can be widely used as a chromatographic filler matrix for rapid separation of chemical or biological macromolecules.

Description

technical field [0001] The invention relates to the technical field of silica gel adsorption packing, in particular to a preparation method of high-purity porous spherical silica gel packing. Background technique [0002] Silica gel is an inorganic matrix filler. The main chemical composition is silica. The structure of silica gel is extremely stable. It is widely found in minerals such as sand and granite. Natural silica exists in the form of crystalline and amorphous structures. In addition to the very high mechanical strength, good filling stability and excellent chemical stability of silica gel, the surface of silica gel has special surface chemical characteristics. The surface of silica gel is also rich in silanol, and the silicon atoms exposed on the surface of silica gel tend to For tetrahedral ligands with oxygen atoms, the coordination is usually completed by combining monovalent hydroxyl groups, that is, the formation of surface silanol groups. The existence of sil...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/10B01J20/28B01J20/30B01D15/20
Inventor 刘增强
Owner 青岛硕远硅胶科技有限公司
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