Preparation method of bisphenol A solid phase extractant based on dummy template covalently imprinted silica gel

A solid-phase extraction agent and pseudo-template technology, applied in the field of preparation of bisphenol A solid-phase extraction agent, can solve the problem of template leakage of non-specific recognition sites and the like, and achieve the effect of high selective recognition ability

Inactive Publication Date: 2014-10-29
WUHAN TEXTILE UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In recent years, people have used covalent imprinting or pseudo-template non-covalent imprinting techniques to prepare selective solid pha...

Method used

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  • Preparation method of bisphenol A solid phase extractant based on dummy template covalently imprinted silica gel
  • Preparation method of bisphenol A solid phase extractant based on dummy template covalently imprinted silica gel
  • Preparation method of bisphenol A solid phase extractant based on dummy template covalently imprinted silica gel

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Experimental program
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Embodiment 1

[0029] (1) Under the protection of nitrogen, add hexafluorobisphenol A and 3-propylisocyanotriethoxysilane, hexafluorobisphenol A and 3-propylisocyanotriethoxy to anhydrous tetrahydrofuran solvent The molar ratio of base silane is 0.5:2, and then reacted at 50°C for 50h, and after the solvent was evaporated to dryness by rotary evaporation, it was separated and purified by silica gel chromatography to obtain a viscous oil;

[0030] (2) Mix and stir the porogen P123, NaCl, water and HCl until completely dissolved, as a template stock solution;

[0031] (3) Take the product of step (1) and the template stock solution of step (2) and tetraethyl orthosilicate for 20 h at room temperature, the product of step (1) and the template stock solution of step (2) and orthosilicate The weight ratio of ethyl silicate is 0.1:30:1, and then dried at 70°C for 30 hours to obtain mesoporous organic silica gel, and then use methanol as solvent to remove P123 in mesoporous silica gel through Soxhl...

Embodiment 2

[0035] (1) Under the protection of nitrogen, add hexafluorobisphenol A and 3-propylisocyanotriethoxysilane, hexafluorobisphenol A and 3-propylisocyanotriethoxy to anhydrous tetrahydrofuran solvent The molar ratio of base silane is 2:2, and then reacted at 80°C for 30h, and after the solvent was evaporated to dryness by rotary evaporation, it was separated and purified by silica gel chromatography to obtain a viscous oil;

[0036] (2) Mix and stir the porogen P123, NaCl, water and HCl until completely dissolved, as a template stock solution;

[0037] (3) Take the product of step (1) and the template stock solution of step (2) and tetraethyl orthosilicate at room temperature for 30 hours of mixed reaction condensation, the product of step (1) and the template stock solution of step (2) and orthosilicate The weight ratio of ethyl silicate is 1:60:3, and then dried at 90°C for 20 hours to obtain mesoporous organic silica gel, and then use methanol as solvent to remove P123 in meso...

Embodiment 3

[0041] 3.1 Preparation of new intermediates of BPAF-Si

[0042] Under nitrogen protection, BPAF (4.0 g, 12 mmol) and ICPTES (6.0 mL, 24 mmol) were reacted at 65° C. for 40 h in anhydrous tetrahydrofuran (THF). After the solvent was evaporated by rotary evaporation, it was separated and purified by silica gel chromatography to obtain a viscous oil, which was confirmed to be the target product BPAF-Si by infrared spectroscopy. The reaction yield was 80%. The reaction scheme is as follows:

[0043]

[0044] figure 1 is the infrared spectrum of the intermediate BPAF-Si, from figure 1 It can be seen that in the infrared spectrum of ICPTES at 2270cm -1 There is a strong -NCO absorption peak at figure 1 There is no obvious absorption peak at the corresponding position in , indicating that there is no -NCO group in the product, that is, the ICPTES reaction is complete; in addition figure 1 at 1720cm -1 There is a strong absorption peak at , which is caused by the stretching vi...

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Abstract

The invention discloses a preparation method of a bisphenol A solid phase extractant based on dummy template covalently imprinted silica gel. The preparation method comprises the following steps: taking bisphenol-AF (BPAF) as the dummy template molecule and (3-isocyanatopropyl)-triethoxysilane (ICPTES) as the functional monomer to synthesize a novel monomer/template composite substance BPAF-Si; taking P-123 as the pore forming agent, carrying out condensation reactions between BPAF-Si and tetraethoxysilane (TEOS) to obtain silica gel containing a template, and heating to remove the template molecules which are covalently combined so as to obtain the covalently imprinted mesoporous silica gel namely the bisphenol A solid phase extractant. The bisphenol solid phase extractant has a very high selectivity recognizing performance on the template molecule BPAF, also has a similar selectivity recognizing performance on structural analogue such as BPA, is capable of nearly completely absorb trace BPA in a water solution, has a high enrichment factor, and can be repeatedly used. So the mesoporous imprinted silica gel is advantageously used as a novel solid phase extractant for the high selective enrichment and separation of trace BPA in an environmental sample.

Description

technical field [0001] The invention relates to the technical field of chemistry and chemical engineering, in particular to a method for preparing a bisphenol A solid-phase extractant based on pseudo-template covalently imprinted silica gel. Background technique [0002] In recent years, the threat of environmental estrogen to human health and survival has attracted widespread attention from all walks of life. Bisphenol A (BPA) is a typical environmental hormone with the following chemical structure: [0003] Bisphenol A generally exists in the environment in trace and ultra-trace amounts. At present, the detection of bisphenol A in the environment requires tedious and time-consuming enrichment, separation and pretreatment processes, such as liquid-liquid extraction. Solid-phase extraction technology has the advantages of less solvent usage, high processing efficiency, simple operation, easy automation, and can handle a large number of samples, and has been widely used in...

Claims

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Application Information

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IPC IPC(8): C08G77/26C08J9/26B01J20/26B01J20/30
Inventor 何池洋余丹魏守台
Owner WUHAN TEXTILE UNIV
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