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Preparation method of chitosan-grafted beta-cyclodextrin bonded silica gel absorbent

A technology of bonding silica gel and cyclodextrin, which is applied in chemical instruments and methods, adsorption water/sewage treatment, water/sludge/sewage treatment, etc., to achieve large enrichment multiples, good reproducibility, and good reproducibility Effect

Inactive Publication Date: 2013-05-22
FUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, there is no relevant report on the use of chitosan grafted β-cyclodextrin bonded silica gel as an adsorbent for solid phase extraction

Method used

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  • Preparation method of chitosan-grafted beta-cyclodextrin bonded silica gel absorbent
  • Preparation method of chitosan-grafted beta-cyclodextrin bonded silica gel absorbent
  • Preparation method of chitosan-grafted beta-cyclodextrin bonded silica gel absorbent

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Effect test

Embodiment 1

[0019] Preparation of chitosan grafted β-cyclodextrin bonded silica gel adsorbent

[0020] (1) Activation of silica gel: soak the silica gel with concentrated nitric acid and deionized water (volume ratio 1:1) for 12 hours, then use deionized water to filter until neutral, and then use concentrated hydrochloric acid and deionized water (volume ratio 1:1 ) magnetically stirred for 12 h, washed with deionized water and filtered until neutral. Dry at 60 °C for 24 h and cool in a drying oven;

[0021] (2) γ-aminopropyl bonded silica gel: Take 10 g of the activated silica gel in step (1) in a 250 mL three-neck flask, then measure 50 mL of toluene and 20 mL of γ-aminopropyltriethoxysilane ( YDH-550), in an oil bath at 110 °C, stirred and refluxed for 16 h, after cooling, the product was washed with toluene, ethanol, and acetone in turn and suction filtered until no gel was present. Dry at 60 °C for 24 h and cool in a drying oven;

[0022] (3) Silica gel aldehyde group modificatio...

Embodiment 2

[0026] Effect of pH on Adsorption Properties of Chitosan Grafted β-Cyclodextrin Bonded Silica Gel Adsorbent

[0027] The absorption rate was measured by flame atomic absorption method (FAAS) through the static test of solutions with different pH values. figure 1 For the effect of pH on the adsorption performance of chitosan-grafted β-cyclodextrin-bonded silica gel and chitosan-bonded silica gel for Cd(II), figure 2 The effect of pH on the adsorption of Cd(II) on chitosan-grafted β-cyclodextrin-bonded silica gel. The initial Cu(II) ion concentration: 2.0 mg / L; adsorbent dosage: 0.15g; shaking time: 30 min; sample volume: 50 mL; 25°C. Initial Cd(II) ion concentration: 1.0 μg / ml; adsorbent dosage: 0.15g; shaking time: 30 min; temperature: 25°C; sample volume: 50ml.

Embodiment 3

[0029] Determination of maximum enrichment fold

[0030] The enrichment performance of adsorbent for Cu(II) under different sample volume conditions was investigated by dynamic experiment method. In the experiment, 100, 200, 400, 600, 800, 1000, 1200, 1400, 1600 and 1800 mL sample solutions containing 10 μg Cu(II) were enriched by column extraction under optimal extraction and elution conditions, and then The maximum enrichment factor was studied by measuring the recovery rate of Cu(II). The results are shown in Table 1. When the sample volume increased to 1600 mL, the recovery rate of Cu(II) dropped to 82.5%, and when the sample volume increased to 1800 mL, the recovery rate of Cu(II) decreased even more. to 69.2%. This shows that the adsorbent has a good extraction and enrichment ability for Cu(II). Since 4 mL of hydrochloric acid solution can achieve quantitative recovery of Cu(II), the maximum enrichment factor is 350, which is expected to achieve ppb level Cu in the sam...

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Abstract

The invention discloses a chitosan-grafted beta-cyclodextrin bonded silica gel absorbent as well as a preparation method and application of the chitosan-grafted beta-cyclodextrin bonded silica gel absorbent, and belongs to the technical field of the absorbent material preparation. The preparation method of the chitosan-grafted beta-cyclodextrin bonded silica gel absorbent comprises the steps of (1) activating silica gel, (2) bonding the silica gel with gamma-aminopropyl, (3) carrying out silica gel formyl group modification reaction, and (4) bonding chitosan with glutaraldehyde and grafting beta-cyclodextrin with the chitosan. According to the chitosan-grafted beta-cyclodextrin bonded silica gel absorbent provided by the invention, the activated silica gel surface is chemically modified by gamma aminopropyl triethoxy silane, and then, cyclodextrin-grafted chitosan is taken as a functional monomer to compound a solid-phase extraction material. By combining cyclodextrin recognition performance and a chitosan absorbing function, the chitosan-grafted beta-cyclodextrin bonded silica gel absorbent has the advantages of firmness in bonding, stable property, favorable reproducibility and selection, and large enrichment multiple, and the chitosan-grafted beta-cyclodextrin bonded silica gel absorbent can be used in a wide pH scope. The absorbent can be used in the enrichment pretreatment of trace Cu (I) and Cd (II) in an environmental water sample.

Description

technical field [0001] The invention belongs to the field of adsorption material preparation technology, and in particular relates to a chitosan grafted β-cyclodextrin bonded silica gel adsorbent and a preparation method and application thereof. Background technique [0002] The pollution of heavy metal ions to water bodies will seriously endanger human life and safety due to their different types, contents and forms, and their characteristics of not easy to degrade and high toxicity, such as Cr(II), Cd(II), etc. Heavy metal elements have risks such as carcinogenicity, teratogenicity, and gene mutation, so it is particularly important to determine the concentration of metal ions in water. At present, there are many methods for the detection of trace heavy metal ions in environmental water samples, and flame atomic absorption (FAAS) is more commonly used. The ion concentration of the actual water sample is extremely low (for example, the Cd(II) of the first-class water quali...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/26B01J20/30C02F1/28C02F1/62C08B37/08C08B37/16
Inventor 吕海霞王晓明安洪涛易娇娇谢增鸿
Owner FUZHOU UNIV
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