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mesoporous sio 2 Preparation method of surface-initiated boron affinity imprinted polymer material and its application in extraction of shikimic acid

An imprinted polymer and surface-initiated technology, which is applied in the preparation of organic compounds, chemical instruments and methods, and carboxylate preparation, etc., can solve the problems that the single-weight recognition ability of imprinted polymers is difficult to achieve deep separation and purification, and the composition is complex. , to achieve effective separation, increase adsorption efficiency, and good application prospects

Active Publication Date: 2021-07-20
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the complex components of the shikimic acid extract, it is difficult to meet the requirements of deep separation and purification only by the single-fold recognition ability of the imprinted polymer.

Method used

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  • mesoporous sio <sub>2</sub> Preparation method of surface-initiated boron affinity imprinted polymer material and its application in extraction of shikimic acid
  • mesoporous sio <sub>2</sub> Preparation method of surface-initiated boron affinity imprinted polymer material and its application in extraction of shikimic acid
  • mesoporous sio <sub>2</sub> Preparation method of surface-initiated boron affinity imprinted polymer material and its application in extraction of shikimic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] A mesoporous SiO 2 A method for preparing a surface-induced boron affinity imprinted polymer material, comprising the following steps:

[0033] a) According to the solid-to-liquid ratio (5mmol: 0.5mL: 30mL), dissolve TEOS and n-pentanol in cyclohexane, stir thoroughly and quickly add CTAB and urea to the above solution according to the molar ratio (0.2:1), add 30mL of deionized water, stirred for 30min, transferred to a hydrothermal reaction kettle, placed in a blast drying oven at 80°C, reacted for 2h, centrifuged, washed three times with acetone and distilled water, dried and placed in a tube Furnace roasting, the roasting temperature is 300°C, the roasting time is 4h, and the heating rate is 1°C / min;

[0034] b) Dissolve 0.1g of the above-prepared silicon material and 0.5mL of KH570 in 70mL of absolute ethanol, ultrasonically disperse for 0.5h, reflux at 40°C for 12h under mechanical stirring, centrifuge, wash with distilled water five times, vacuum at 30°C Dried t...

Embodiment 2

[0038] A mesoporous SiO 2 A method for preparing a surface-induced boron affinity imprinted polymer material, comprising the following steps:

[0039] a) According to the solid-to-liquid ratio (12mmol: 2mL: 30mL), dissolve TEOS and n-pentanol in cyclohexane, stir thoroughly and quickly add CTAB and urea to the above solution according to the molar ratio (0.4:1), add 30mL Deionized water, stirred for 30 minutes, transferred to a hydrothermal reaction kettle, placed in a blast drying oven at 100°C, reacted for 6 hours, centrifuged, washed with acetone and distilled water three times, dried and placed in a tube furnace Roasting, the firing temperature is 400°C, the firing time is 5h, and the heating rate is 1°C / min;

[0040] b) Dissolve 0.1g of the above-prepared silicon material and 2mL of KH570 in 70mL of absolute ethanol, under mechanical stirring, reflux at 75°C for 15h, centrifuge, wash with distilled water five times, and dry in vacuum at 30°C to obtain vinyl modification ...

Embodiment 3

[0044] A mesoporous SiO 2 A method for preparing a surface-induced boron affinity imprinted polymer material, comprising the following steps:

[0045] a) Dissolve TEOS and n-pentanol in cyclohexane according to the solid-to-liquid ratio (15mmol: 1.5mL: 30mL), and after stirring thoroughly, quickly add CTAB and urea to the above solution according to the molar ratio (0.6:1), and add 30mL of deionized water, stirred for 30min, transferred to a hydrothermal reaction kettle, placed in a blast drying oven at 120°C, reacted for 4h, centrifuged, washed three times with acetone and distilled water, dried and placed in a tube Furnace roasting, the roasting temperature is 550°C, the roasting time is 6h, and the heating rate is 1°C / min;

[0046] b) Dissolve 0.1g of the above-prepared silicon material and 2mL of KH570 in 70mL of absolute ethanol, under mechanical stirring, reflux at 60°C for 24h, centrifuge, wash with distilled water five times, and dry in vacuum at 30°C to obtain vinyl ...

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Abstract

The invention belongs to the field of resource utilization and chemical separation technology, and relates to mesoporous SiO 2 A method for preparing a surface-induced boron affinity imprinted polymer material, including dissolving TEOS and n-pentanol in cyclohexane, fully stirring to form a uniform solution, quickly adding CTAB and urea, adding deionized water, and performing a hydrothermal reaction at 80-180°C 2-6 hours, after drying, place the prepared silicon material in a tube furnace at 300-650°C for 4-8 hours; then dissolve the silicon material and KH570 in absolute ethanol, and reflux at 40-100°C for 12-48 hours , vacuum-dried to obtain vinyl-modified silicon material; dissolve it in acetonitrile solution, add shikimic acid, VPBA, cross-linking agent EGDMA, and initiator AIBN to react and then centrifuge. The material is based on a mesoporous silicon material, and a molecularly imprinted polymer is prepared on its surface to introduce a dual recognition mechanism, so that shikimic acid with a cis-dihydroxy structure is enriched on the surface of the material, and the effective separation of shikimic acid is realized. It has a good application prospect in the field of enrichment separation and purification of natural products with cis-dihydroxy structure.

Description

technical field [0001] The invention belongs to the field of resource utilization and chemical separation technology, and relates to materials and preparation methods for selectively separating shikimic acid in environmental plant tissues, in particular to mesoporous SiO 2 Preparation method of surface-induced boron affinity imprinted polymer material and its application to extract shikimic acid. Background technique [0002] Shikimic acid is widely distributed in nature and has high medical value. Its chemical structure is 3,4,5-trihydroxy-1-cyclohexene-1-carboxylic acid. The content of shikimic acid in star anise is the highest (about 10%), and it is regarded as the best resource plant for extracting shikimic acid. Studies have shown that shikimic acid has anti-tumor, anti-thrombotic, cerebral ischemia and anti-inflammatory effects. Using shikimic acid as a raw material can produce the only weapon against avian influenza virus-patented drug GS4104 (Tamiflu) through chemic...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F230/08C08F230/06C08F222/14B01J20/26B01J20/30B01D15/08C07C51/487C07C62/32
CPCB01D15/08B01J20/268C07C51/487C08F222/1006C08F230/08C07C2601/16C07C62/32
Inventor 邱凤仙朱瑶毛凯丽荣坚张涛杨冬亚潘建明
Owner JIANGSU UNIV
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