Preparation method of inorganic-organic hybrid monolithic column

An organic hybrid, monolithic column technology, applied in chemical instruments and methods, separation methods, other chemical processes, etc., can solve the problems of uneven pore structure, small surface area, poor separation effect, etc., to achieve good separation effect, skeleton and Uniform pore size and short time-consuming effect

Inactive Publication Date: 2015-04-08
HEBEI UNIVERSITY
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

[0003] The purpose of the present invention is to provide a preparation method of an inorganic-organic hybrid monolithic column, to expand the high performance liquid chromatography monolithic column of the new polymerization system, and to solve the small surface area and uneven pore structure of the polymer material in the existing monolithic column and poor separation

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  • Preparation method of inorganic-organic hybrid monolithic column
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  • Preparation method of inorganic-organic hybrid monolithic column

Examples

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Embodiment 1

[0022] (1) Hydroxylation of nanodiamonds by Fenton’s reagent reflux method: take 6.95g FeSO 4 ·H 2 O, add a little (about 10-30ml) distilled water to dissolve completely, adjust the pH of the solution to 3.0 with concentrated sulfuric acid, add 0.1g of nano-diamonds with a particle size of 80 nm to the solution, stir and mix, add 42.5g dropwise while stirring H with a mass fraction of 30% 2 o 2 , making nanodiamonds in Fe 2+ : H 2 o 2 The molar ratio is 1:15, and the temperature is 80 °C for 5 h under reflux reaction to obtain hydroxylated nano-diamonds. The infrared spectrum is as follows figure 2 As shown in B, the infrared spectrum of the nano-diamond before the reaction is as follows figure 2 As shown in A;

[0023] (2) Take the hydroxyl nanodiamond prepared in step (1) and KH of the same mass as the hydroxyl nanodiamond 570 (γ-methacryloxypropyltrimethoxysilane) was mixed and dissolved in 30ml of ethanol with a concentration of 95% (v / v), ultrasonically treated ...

Embodiment 2

[0026] (1) Hydroxylation of nanodiamonds by Fenton’s reagent reflux method: Take 5.69g FeSO 4 , add a little (about 10-30ml) distilled water to dissolve completely, adjust the pH of the solution to 2.8 with concentrated sulfuric acid, add 0.1g of nano-diamonds with a particle size of 60 nm in the solution, stir and mix, add 34.8g of mass dropwise while stirring H with a score of 30% 2 o 2 , making nanodiamonds in Fe 2+ : H 2 o 2 The molar ratio is 1:15, and the temperature is 75°C for reflux reaction for 6 hours to obtain hydroxylated nano-diamonds;

[0027] (2) Take the hydroxyl nanodiamond prepared in step (1) and KH of the same mass as the hydroxyl nanodiamond 570 (γ-methacryloxypropyltrimethoxysilane) was mixed and dissolved in 30ml of ethanol with a concentration of 95% (v / v), ultrasonically treated for 1.5 hours, and reacted at a constant temperature of 55°C for 6.5 hours, and then the reaction The product was centrifuged at 15,000 r / min for 8 min, and unreacted KH...

Embodiment 3

[0030] (1) Hydroxylation of nanodiamonds by Fenton’s reagent reflux method: take 7.79g FeSO 4 ·H 2 O, add a little (about 10-30ml) distilled water to dissolve completely, adjust the pH of the solution to 3.2 with concentrated sulfuric acid, add 0.1g of nano-diamonds with a particle size of 80 nm to the solution, stir and mix, and add 47.6g dropwise while stirring H with a mass fraction of 30% 2 o 2 , making nanodiamonds in Fe 2+ : H 2 o 2 The molar ratio is 1:15, and the temperature is 85°C for reflux reaction for 4 hours to obtain hydroxylated nano-diamonds;

[0031] (2) Take the hydroxyl nanodiamond prepared in step (1) and KH of the same mass as the hydroxyl nanodiamond 570 (γ-methacryloxypropyltrimethoxysilane) mixed and dissolved in 30ml of ethanol with a concentration of 95% (v / v), ultrasonically treated for 2.5 hours, and reacted at a constant temperature of 65°C for 5.5 hours, and then the reaction The product was centrifuged at 15,000 r / min for 8 min, and unrea...

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Abstract

The invention relates to a preparation method of an inorganic-organic hybrid monolithic column. The preparation method comprises the following steps: A. adjusting the pH value of Fe<2+> compound containing aqueous solution, adding with nano-diamond, adding with H2O2 and reacting to obtain hydroxyl nano diamond; B. mixing the hydroxyl nano diamond with KH570, dissolving into ethyl alcohol, carrying out ultrasonic treatment, reacting, centrifuging, washing, and drying to obtain the coupled hydroxylized nano diamond; C. mixing the coupled hydroxylized nano diamond, dipentaerythritolhexaacrylate, a cross-linking agent, an initiator and a pore-foaming agent, injecting the mixture into a stainless steel column, and reacting for 1-1.5h; and D. connecting the stainless steel column with a high-pressure infusion pump, flushing, and drying to obtain the inorganic-organic hybrid monolithic column. The preparation method has simple process, the reaction condition can be realized easily, the operability is good, the prepared monolithic column has uniform framework and pore diameter, has good separation effect and can be used for separating complex samples under a wide-temperature-range condition, and the application field of the monolithic column can be expanded greatly.

Description

technical field [0001] The invention relates to a preparation method of a high performance liquid chromatography monolithic column, in particular to a preparation method of an inorganic-organic hybrid high performance liquid chromatography monolithic column. Background technique [0002] High-performance liquid chromatography (HPLC) is a new chromatographic separation and analysis technique developed in the early 1970s. It has the characteristics of high separation efficiency, good selectivity, high sensitivity, fast analysis speed, and wide application range. HPLC has become an important separation and analysis technology in chemistry, biochemistry, medicine, industry, agriculture, environmental protection and other disciplines, and is an indispensable technology in the hands of analytical chemistry, biochemistry and environmental chemistry workers. The monolithic column is a continuous bed stationary phase that uses organic or inorganic polymerization methods to perform in...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D15/22B01J20/285B01J20/30
Inventor 刘海燕魏爱乐闫宏远
Owner HEBEI UNIVERSITY
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