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Preparation method of hybridized silica gel monolithic column

A hybrid silica gel and monolithic column technology, applied in the field of chromatographic separation, can solve the problems of difficult to prepare pore structure, difficult to master, complicated preparation, etc., and achieve the effect of good separation effect, increased strength, and improved flexural fracture

Inactive Publication Date: 2015-01-07
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the preparation of hybrid silica monolithic columns is relatively complicated and difficult to master. It is difficult to prepare monolithic columns with uniform pore structure and good continuity, and there are still great obstacles in the application of chromatographic separation.

Method used

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  • Preparation method of hybridized silica gel monolithic column
  • Preparation method of hybridized silica gel monolithic column
  • Preparation method of hybridized silica gel monolithic column

Examples

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Effect test

Embodiment 1

[0023] Weigh 0.70g PEG, add 10mL 0.01mol / L acetic acid solution, stir evenly, add 5.4mL TMOS and 1.8mL VTMS, stir for 1h in an ice bath at 0°C, vacuum for 20min, pour into a glass tube, and age at 40°C for 24 hours, and then heat-treated with 1 mol / L ammonia water at 120 °C to prepare mesopores. Then, the column was soaked in 0.1mol / L nitric acid solution for 3 hours, distilled water for 3 hours, and N,N-dimethylformamide for 5 hours. After taking it out, it was dried at 60°C for 10 hours, and the temperature was raised to 600°C at 1°C / min. Incubate for 2 hours to obtain a monolithic column bed of hybrid silica gel with a double-pore structure. A 50mm×4.6mm i.d. hybrid silica monolithic column was prepared by coating the silica gel monolithic column bed in a stainless steel column with epoxy resin material.

Embodiment 2

[0025] Weigh 0.70g PEG, add 10mL 0.01mol / L acetic acid solution, stir evenly, add 5.4mL TMOS and 2.7mL VTMS, stir for 1h in an ice bath at 0°C, vacuum for 20min, pour into a glass tube, and age at 40°C 24 h, and then heat-treated with 0.1 mol / L ammonia water at 120 °C to prepare mesopores. Then, the column was soaked in 0.1mol / L nitric acid solution for 3 hours, distilled water for 3 hours, and N,N-dimethylformamide for 5 hours. After taking it out, it was dried at 60°C for 10 hours, and the temperature was raised to 600°C at 1°C / min. Incubate for 2 hours to obtain a monolithic column bed of hybrid silica gel with a double-pore structure. A 50mm×4.6mm i.d. hybrid silica monolithic column was prepared by coating the silica gel monolithic column bed in a stainless steel column with epoxy resin material.

Embodiment 3

[0027] Weigh 0.70g PEG, add 10mL 0.01mol / L acetic acid solution, stir evenly, add 5.4mL TMOS and 1.8mL VTMS, stir for 1h in an ice bath at 0°C, vacuum for 20min, pour into a glass tube, and age at 40°C for 24 hours, and then heat-treated with 2 mol / L ammonia water at 120 °C to prepare mesopores. Then, the column was soaked in 0.1mol / L nitric acid solution for 3 hours, distilled water for 3 hours, and N,N-dimethylformamide for 5 hours. After taking it out, it was dried at 60°C for 10 hours, and the temperature was raised to 500°C at 1°C / min. After 2h, a monolithic column bed of hybrid silica gel with a double-pore structure was obtained. A 50mm×4.6mm i.d. hybrid silica monolithic column was prepared by coating the silica gel monolithic column bed in a stainless steel column with epoxy resin material. The nitrogen adsorption and desorption test results show that the nanometer average pore diameter of the column is 11.38nm, and the specific surface area is 248.9㎡ / g.

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Abstract

The invention discloses a preparation method of a hybridized silica gel monolithic column. The preparation method of the hybridized silica gel monolithic column comprises the following steps: firstly, weighing PEG (polyethylene glycol) with Mw of 10000, namely 0.70g of polyethylene glycol; adding 10mL of 0.01mol / L acetic acid solution; adding tetramethyl orthosilicate and vinyl trimethoxy silane according to a volume ratio ranging from (1:1)-(4:1); stirring in an ice bath and vacuumizing; pouring a mixture into a glass tube and aging at 40 DEG C for 24 hours; then carrying out heat treatment with 0.1mol / L-2mol / L ammonia water to prepare a column bed of a hybridized silica gel monolithic column; roasting at 400-700 DEG C after immersing to obtain the column bed with a double-pore structure of the hybridized silica gel monolithic column; and covering with an epoxy resin material and filling the column bed into a stainless steel column to prepare the hybridized silica gel monolithic column. According to the preparation method of the hybridized silica gel monolithic column, a phenomenon that the monolithic column is easy to bend and crack in a traditional preparation process is improved; and the average pore diameter of the monolithic column is 11.26nm and the specific surface area of the monolithic column is 315.7m<2> / g. Benzene can be effectively separated under a normal-phase chromatography mode and the number of theoretical plates is 10410N / m.

Description

technical field [0001] The invention belongs to chromatographic separation technology, more specifically, monolithic column liquid chromatography technology, and relates to a preparation method of silica gel hybrid monolithic column. Background technique [0002] Chromatography, as a separation and analysis technology and method, no matter what kind of separation mode it is, has been developed by leaps and bounds from technology to theory to application in various scientific fields. In the 21st century, with the rapid development and challenges of materials science, information science, environmental science, life science and other fields, people put forward higher requirements for chromatography technology. [0003] In the whole chromatographic system, it can be said that the monolithic column is the core. In order to adapt to the progress of science and technology and the development of industrial production, the monolithic column technology has also made great progress. ...

Claims

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Application Information

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IPC IPC(8): B01J20/10B01J20/30B01D15/20
CPCB01J20/103B01D15/20B01J20/28061B01J20/28083B01J20/28095
Inventor 龚彩荣张珊珊范国樑
Owner TIANJIN UNIV
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