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Silica gel chromatographic packing for separation of alkaline compound and preparation method of silica gel chromatographic packing

A technology for silica gel chromatography and compounds, applied in separation methods, chemical instruments and methods, solid adsorbent liquid separation, etc., can solve the problems of unsatisfactory reproducibility and stability of chromatographic packing materials, and achieve good separation selectivity and preparation methods Simple and stable effect

Active Publication Date: 2015-11-25
浙江月旭材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, since this method adopts the method of copolymerization reaction, there are problems such as unsatisfactory reproducibility and stability of the prepared chromatographic filler.

Method used

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  • Silica gel chromatographic packing for separation of alkaline compound and preparation method of silica gel chromatographic packing
  • Silica gel chromatographic packing for separation of alkaline compound and preparation method of silica gel chromatographic packing
  • Silica gel chromatographic packing for separation of alkaline compound and preparation method of silica gel chromatographic packing

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preparation example Construction

[0034] The invention provides a preparation method of silica gel chromatography packing for separating basic compounds, comprising: reacting silica gel with a mixture of non-polar silane coupling agent and polar silane coupling agent to prepare the silica gel chromatography packing; wherein, The non-polar silane coupling agent contains three hydrolyzable groups, and the polar silane coupling agent contains one hydrolyzable group; or the non-polar silane coupling agent contains one hydrolyzable group, so The polar silane coupling agent contains three hydrolyzable groups.

[0035] In one embodiment of the present invention, the chemical formula of the non-polar silane coupling agent is: X(Si)(CH 3 ) 2 R 1 , X is a hydrolyzable group, R 1 Selected from alkyl groups containing 1 to 20 carbon atoms, substituted alkyl groups containing phenyl groups containing 1 to 20 carbon atoms, substituted alkyl groups containing pentafluorophenyl groups containing 1 to 20 carbon atoms, or pe...

preparation example 1

[0065] (1) Add 100 g of silica gel (5 μm, purchased from DAISO, Japan) into a 2 L glass reaction vessel, add 1000 mL of distilled water, stir for 30 minutes, filter, and repeat this step twice. Then add 1000mL of hydrofluoric acid aqueous solution with a mass ratio of 0.08%, stir for 24 hours, wash with distilled water until neutral, finally add 1000mL of acetone to wash, filter, and dry at 110°C for 12 hours to obtain activated silica gel;

[0066] (2) Weigh 100g of activated silica gel (5μm, Specific surface area: 300m 2 / g), placed in a 2L glass material reaction vessel; 5g of ultrapure water was added to the reaction vessel, and stirred at 170 rpm for more than 30 minutes to obtain hydrated silica gel;

[0067](3) Add the hydrated silica gel prepared in step (2) to the glass material reaction vessel, and add 800mL of dry anhydrous toluene solvent, stir evenly at 170 rpm and add 24.45g of octadecyltrichlorosilane and 3.593g of a mixture of two silane reagents, chloroprop...

preparation example 2

[0071] (1) Add 100 g of silica gel (5 μm, purchased from DAISO, Japan) into a 2 L glass reaction vessel, add 1000 mL of distilled water, stir for 30 minutes, filter, and repeat this step twice. Then add 900mL of hydrofluoric acid aqueous solution with a mass ratio of 0.06%, stir for 24 hours, wash with distilled water until neutral, finally add 1000mL of acetone to wash, filter, and dry at 110°C for 12 hours to obtain activated silica gel;

[0072] (2) Weigh 100g of activated silica gel (5μm, Specific surface area: 300m 2 / g), placed in a 2L reaction vessel; 8g of ultrapure water was added to the glass reaction vessel, and stirred at 250 rpm for 30 minutes to obtain hydrated silica gel;

[0073] (3) Add the hydrated silica gel prepared in step (2) to the glass material reaction vessel, and add 800mL of dry anhydrous toluene solvent, stir at 170 rpm and add 26.07g of octadecyltrichlorosilane and 3. 111g of a mixture of 4-chlorobutyldimethylchlorosilane and two silane reagent...

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Abstract

The invention provides silica gel chromatographic packing for separation of an alkaline compound and a preparation method of the silica gel chromatographic packing. The method comprises the following step: reacting silica gel with a mixture of a nonpolar silane coupling agent and a polar silane coupling agent to prepare the silica gel chromatographic packing. The chromatographic packing prepared by the preparation method of the silica gel chromatographic packing for separation of the alkaline compound provided by the invention can provide acting forces in various forms such as hydrophobic effect, hydrogen bonding effect, electrostatic attraction and ionic exchange, and has better separation selectivity compared with conventional reversed-phase chromatographic packing.

Description

technical field [0001] The invention relates to a silica gel-based reversed-phase chromatographic filler and a preparation method thereof, in particular to a silica gel chromatographic filler for separating basic compounds and a preparation method thereof. Background technique [0002] High performance liquid chromatography (HPLC) is an efficient, novel and rapid analytical separation technique developed in the 1970s. Since Kirkland first used the prepared silica gel reversed-phase chromatographic packing for high-performance liquid chromatography (HPLC) separation in 1971, reversed-phase high-performance liquid chromatography (RP-HPLC) has become an important tool in chemical engineering, food hygiene, drug testing, environmental monitoring, etc. The most commonly used analytical separation method in many fields. According to statistics, about 80% of separations are performed in reversed-phase mode. However, in the general separation mode, because the surface of the silic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/22B01J20/30B01D15/32
Inventor 薛昆鹏赵岳星姚立新余冲
Owner 浙江月旭材料科技有限公司
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