Porous spherical silica chromatography filler and preparing method thereof

A technology of porous spherical and silica gel chromatography, which is applied in chemical instruments and methods, and other chemical processes, can solve the problems of affecting the output of microspheres with target particle size and increasing production costs, and achieves high yield, easy control of conditions, and excellent preparation process. simple effect

Active Publication Date: 2016-12-14
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although these hollow spheres and strips can be eliminated by subsequent particle classification methods, they will seriously affect the yield of microspheres with target particle size and increase production costs

Method used

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  • Porous spherical silica chromatography filler and preparing method thereof
  • Porous spherical silica chromatography filler and preparing method thereof
  • Porous spherical silica chromatography filler and preparing method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] The preparation method of porous spherical silica gel chromatographic filler, comprises the steps:

[0035] (1) Add absolute ethanol and tetraethyl orthosilicate (TEOS, 104 g) into a three-necked flask at a molar ratio of 1, stir and mix at 500 rpm to obtain a mixed solution;

[0036] (2) Add 0.1M hydrochloric acid aqueous solution to the mixed solution, stir at 30°C for 0.5h, and distill off the solvent under reduced pressure to obtain a polysiloxane prepolymer; The molar ratios are 0.5, 1.0, 1.5, 2.0 respectively;

[0037](3) The viscosity modifier solution is a continuous phase; the dispersion phase polysiloxane prepolymer is dispersed into the continuous phase at a ratio of 0.2 by volume, and stirred evenly to obtain an emulsion dispersion system;

[0038] Viscosity modifier solution is the solution of the polyethylene glycol 10000 aqueous solution that mass ratio is 0.5% surfactant triton X-100 and mass concentration,

[0039] (4) Add concentrated ammonia water i...

Embodiment 2

[0046] The preparation method of porous spherical silica gel chromatographic filler, comprises the steps:

[0047] (1) Add absolute ethanol and ethyl silicate-40 (TES-40, 48g) into a three-necked flask at a molar ratio of 4, stir and mix at 500 rpm to obtain a mixed solution;

[0048] (2) Add 0.1M hydrochloric acid aqueous solution to the mixed solution, stir at 30°C for 1h, and distill off the solvent under reduced pressure to obtain a polysiloxane prepolymer; the water in the hydrochloric acid aqueous solution and ethyl silicate-40 The molar ratio is 1.2;

[0049] (3) Mix absolute ethanol and viscosity modifier solution uniformly by volume ratio 0.5 to make continuous phase; disperse phase polysiloxane prepolymer into said continuous phase by volume ratio 0.2, stir evenly to obtain emulsion dispersion system;

[0050] The viscosity regulator solutions are respectively polyethylene glycol 200 aqueous solution, polyethylene glycol 2000 aqueous solution, polyethylene glycol 4...

Embodiment 3

[0056] The preparation method of porous spherical silica gel chromatographic filler, comprises the steps:

[0057] (1) Add absolute ethanol and ethyl silicate-40 (TES-40, 48g) into a three-necked flask at a molar ratio of 4, stir and mix at 500 rpm to obtain a mixed solution;

[0058] (2) Add 0.1M hydrochloric acid aqueous solution to the mixed solution, stir at 30°C for 1h, and distill off the solvent under reduced pressure to obtain a polysiloxane prepolymer; the water in the hydrochloric acid aqueous solution and ethyl silicate-40 The molar ratio is 1.2;

[0059] (3) Mix absolute ethanol and viscosity modifier solution uniformly by volume ratio 0.5 to make continuous phase; disperse phase polysiloxane prepolymer into said continuous phase by volume ratio 0.2, stir evenly to obtain emulsion dispersion system;

[0060] Described viscosity modifier solution is the solution of the polyethylene glycol 10000 aqueous solution that mass ratio is 5% surfactant and mass concentrati...

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Abstract

The invention discloses porous spherical silica chromatography filler and a preparing method thereof. The method includes the steps that 1, absolute ethyl alcohol and a first component are mixed to obtain a mixed solution; 2, a hydrochloric acid water solution is added into the mixed solution and stirred, solvent is removed to obtain a polysiloxane prepolymer; 3, absolute ethyl alcohol and viscosity modifier are prepared into a continuous phase, the polysiloxane prepolymer is dispersed into the continuous phase to obtain an emulsion dispersing system; 4, strong ammonia water is added into the emulsion dispersing system and stirred for reaction, the mixture stands for ageing and is filtered to collect microspheres, and the microspheres are washed and dried to obtain spherical silica microspheres; 5, the spherical silica microspheres are dispersed in deionized water; 6, strong ammonia water is added into the spherical silica microsphere dispersion liquid and stirred, solid is collected, washed, dried and calcined to obtain the porous spherical silica chromatography filler. The filler is in a regular sphere shape and narrow in particle size distribution and can be used in normal-phase chromatography and other separating modes. The preparing method is simple and high in yield, and conditions are easy to control.

Description

technical field [0001] The invention relates to a porous spherical silica gel chromatographic packing and a preparation method thereof, belonging to the preparation technology of the porous spherical silica gel chromatography packing. Background technique [0002] High performance liquid chromatography is one of the most important laboratory separation and analysis techniques, and it has been widely used in food, medicine, environment, chemical industry and other fields. A liquid chromatograph consists of key components such as a high-pressure infusion pump, an injection valve, a chromatographic column, and a detector. An infusion pump is used to drive the liquid mobile phase through the column. After the sample enters the chromatographic column through the injection valve, it is carried by the mobile phase through the chromatographic column. Due to the difference in the distribution coefficients of different compounds between the chromatographic stationary phase and the m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/283B01J20/30
CPCB01J20/283B01J2220/54
Inventor 万谦宏刘世鹏周秀丽霍志霞王晓欢李瑞沙陈磊
Owner TIANJIN UNIV
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