Preparation method of high-purity spherical full-pore silica gel particles

A spherical and particle technology, applied in the field of preparation of high-purity spherical full-porous silica gel particles, can solve the problems of inability to meet large-scale industrial production, unfavorable to environmental protection, large particle size range, etc., and achieve pore size distribution that is controllable and avoided The effect of agglomeration, shape deformation, and uniform particle size

Active Publication Date: 2013-01-16
微纯生物科技(广州)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, domestic research institutes and institutions of higher learning in this field are far behind the international advanced level in terms of filler purity, particle strength, particle size and pore size and distribution, or can only Small-scale preparation in the laboratory cannot meet the needs of large-scale industrial production
[0004] For example: U.S. Patent 5,425,930 describes a method for preparing monodisperse high-purity spherical silica particles, but the particles prepared by this method are non-porous particles, which cannot meet the needs of modern high-performance liquid chromatography technology
U.S. Patent (Patent No. 7223473) document describes a method of preparing organic / inorganic hybrid silica particles, which produces particles with a wide range of particle sizes, resulting in low final yield and high cost
The Chinese patent (patent number 00134301.7) describes a method for preparing monodisperse full-porous spherical silica particles. This method first prepares organic-inorganic composite particles, and then burns at high temperature to remove the organic part. The process is relatively complicated. High temperature Burning not only consumes a lot of energy but is not conducive to environmental protection

Method used

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Embodiment 1

[0027] A preparation method of high-purity spherical full-porous silica gel particles: Add 200mL tetraethyl orthosilicate, 150mL absolute ethanol and 170mL deionized water into a 1L three-necked bottle, adjust the pH value to 3.5 with hydrochloric acid, and store at 26°C After stirring for 18 hours, the temperature was raised to 85° C. for distillation to remove ethanol, and a colorless liquid with a viscosity of 0.4 Pa·s was obtained after cooling to room temperature.

[0028] In a 1L three-necked flask, add 300g of deionized water, 80g of absolute ethanol and 7g of surfactant, among which 6.3g of Tween 20 and 0.7g of sodium dodecylbenzenesulfonate are mixed and stirred for 30 minutes to form a uniform water phase solution; in a 150mL beaker, take 75mL polytetraethoxysilane liquid (viscosity of 0.4Pa s) and 40mL cyclohexane and mix evenly to form an oil phase solution; add the oil phase solution to the water phase under mechanical stirring, and stir for 80 After 10 minutes, a...

Embodiment 2

[0030] A preparation method of high-purity spherical full-porous silica gel particles: Add 100mL tetraethyl orthosilicate, 100mL absolute ethanol and 80mL deionized water into a 1L three-necked bottle, adjust the pH value to 4 with hydrochloric acid, and set the temperature at 24°C After stirring for 19 hours, the temperature was raised to 95° C. for distillation to remove ethanol, and a colorless liquid with a viscosity of 0.3 Pa·s was obtained after cooling to room temperature.

[0031] In a 1L three-necked flask, add 400g of deionized water, 200g of absolute ethanol and 9g of surfactant, among which 8.1g of Tween 80 and 0.9g of sodium dodecylsulfonate are mixed, and stirred for 40 minutes to form a uniform aqueous phase solution ;In a 150mL beaker, take 50mL of polytetraethoxysilane liquid (viscosity is 0.3Pa s) and 40mL of aromatic alkanes and mix evenly to form an oil phase solution; add the oil phase solution to the water phase under mechanical stirring, and stir for 100 ...

Embodiment 3

[0033] A preparation method of high-purity spherical full-porous silica gel particles: add 2L tetraethyl orthosilicate, 1.5L absolute ethanol and 1.5L deionized water into a 10L container and mix, adjust the pH value to 2.5 with hydrochloric acid, and set the temperature at 25 After stirring at °C for 16 hours, the temperature was raised to 90°C for distillation to remove ethanol, and after cooling to room temperature, a colorless liquid with a viscosity of 0.25 Pa·s was obtained.

[0034]The process of industrialized production is: in a 20L reactor, add 6L deionized water, 1600g absolute ethanol and 150g surfactant, wherein 136g Triton X-100, 14g sodium dodecylbenzenesulfonate, stir for 30 minutes to form a homogeneous aqueous solution. In a 3L beaker, take 1.5L polytetraethoxysilane liquid (viscosity 0.25Pa·s) and mix with 1L n-heptane to form an oil phase solution. Add the oil phase solution to the water phase solution under mechanical stirring. The stirring machine is a d...

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Abstract

The invention provides a preparation method of high-purity spherical full-pore silica gel particles. The method is carried out according to the following steps of: hydrolyzing, polymerizing in advance, distilling, preparing a water phase, preparing an oil phase, synthesizing particles and grading. In the invention, ethyl orthosilicate is used as a raw material, silica sol with high concentration (which is greater than 90wt%) is obtained by hydrolyzing and polymerizing in advance under an acidic condition, and the yield is enhanced; the formula of emulsion is optimized through a method of emulsion polymerization by adopting a compounded surfactant, the stability of the emulsion and the monodispersity of liquid drops are enhanced, the agglomeration and the shape deformation of the particlesare avoided, and water is adopted as a reaction medium, which adapts to the requirement of environmental protection; in the preparation of the particles, a pore structure is naturally formed without burning organic components at high temperature to obtain a porous structure, which is simple, convenient and effective and protects the environment; the entire method has simple procedure, excellent repeatability and low cost; and the obtained material has high purity, good mechanical strength, uniform particle diameter, controllable size and narrow and controllable pore diameter distribution.

Description

technical field [0001] The invention relates to the preparation technology of silica gel, in particular to a preparation method of high-purity spherical full-pore silica gel particles. Background technique [0002] High-performance liquid chromatography is a chromatographic separation technology that uses liquid as the mobile phase and uses a chromatographic column with extremely fine particles and high-efficiency stationary phase. High-performance liquid chromatography has wide applicability to samples and is not limited by the volatility and thermal stability of the analytical object, thus making up for the shortcomings of gas chromatography. Among the currently known organic compounds, about 20% can be analyzed by gas chromatography, while 80% need to be analyzed by high performance liquid chromatography. High performance liquid chromatography is based on the classical chromatography, citing the theory of gas chromatography. Technically, the mobile phase is changed to h...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/18C08J9/28B01J20/286
Inventor 黄晓黄曦
Owner 微纯生物科技(广州)有限公司
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