Method for preparing iron ion imprinted silica gel

A technology of iron ion and silica gel, which is applied in the field of preparation of iron ion imprinted silica gel, can solve the problems of low iron, inability to achieve selective enrichment of iron ion, interference with iron ion determination, etc., and achieve simple preparation process, easy operation and high adsorption The effect of capacity

Inactive Publication Date: 2010-05-26
XIAMEN UNIV
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  • Abstract
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Problems solved by technology

However, the content of iron in general water samples is extremely low, such as the general concentration in seawater is 0.05 ~ 2.0nmol / L ([4] Wu J.F., Boyle E.A., Analytica ChimicaActa, 1998, 367: 18.), which is beyond the detection range of general instruments At the same time, the complex substrate in the sample will seriously interfere with the determination of iron ions, so before the instrumental measurement, the water sample must be pretreated by appropriate means to achieve the purpose of removing interference and enriching
[0003] At present, the commonly used pretreatment method for the determination of iron ions in water is the ion exchange method ([5] Zheng Jian, Wei Junfu, Zhao Kongyin, etc., Journal of Tianjin University of Technology, 2009, 28 (2): 5; [6] Lu Ming, Tang Lu, Metallurgical Analysis, 2008, 28(3): 75; [7] Ju Hongfang, Physical and Chemical Testing-Chemical Volume, 2004, 40(11): 660), this method utilizes cation exchange resins to achieve iron ions through ion exchange Separation and enrichment, but it also enriches other ions, and cannot achieve selective enrichment of iron ions

Method used

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  • Method for preparing iron ion imprinted silica gel
  • Method for preparing iron ion imprinted silica gel
  • Method for preparing iron ion imprinted silica gel

Examples

Experimental program
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Effect test

Embodiment 1

[0022] Example 1: 1) Activation of silica gel: Take 1.0 g of silica gel with a particle size of 30 mesh, soak it in 5.0 mL of sulfuric acid solution with a concentration of 1.0 mol / L for 0.5 h, then wash it with ultrapure water until neutral, and dry it at 40 ° C. stand-by. 2) Preparation of iron ion-imprinted silica gel: Weigh 0.38 g of ferric sulfate into 7.6 mL of ethanol solution, heat and stir until the solid dissolves. Add 0.26 g of mercaptopropyltriethoxysilane to the above mixture, and heat, stir and reflux at 60° C. for 0.5 h, then add 0.26 g of activated silica gel, and continue heating, stirring, and reflux for 6 h. 3) Post-treatment of iron ion-imprinted silica gel: filter the above-mentioned iron ion-imprinted silica gel, wash with ethanol until no impurities are detected, and then soak in 0.5 mol / L nitric acid until no iron ions are detected. Finally, the iron ion-imprinted silica gel was washed with ultrapure water to neutrality, and dried at 60° C. for 1.0 h t...

Embodiment 2

[0023] Example 2: Activation of silica gel: take 50 g of silica gel with a particle size of 200 mesh, soak it in 500 mL of hydrochloric acid solution with a concentration of 5.0 mol / L for 5.0 h, then wash it with ultrapure water until neutral, and dry it at 80°C for use. Preparation of iron ion imprinted silica gel: weigh 3.41g FeCl 3 ·6H 2 O was placed in 120mL of methanol solution, heated and stirred until the solid dissolved. Add 6.81 g of mercaptopropyltrimethoxysilane to the above mixture, and heat, stir and reflux at 70° C. for 2.0 h, then add 9 g of activated silica gel, and continue heating, stirring, and reflux for 24 h. Post-treatment of iron ion-imprinted silica gel: filter the above-mentioned imprinted silica gel, wash with methanol until no impurities are detected, and then soak in 5.0mol / L hydrochloric acid until no iron ions are detected. Finally, wash the IIP with ultrapure water to neutrality, and dry it at 70°C for 6.0 hours to obtain the final product. fi...

Embodiment 3

[0024] Example 3: Activation of silica gel: take 100 g of silica gel with a particle size of 300 mesh, soak it in 2000 mL of nitric acid solution with a concentration of 10.0 mol / L for 10 h, then wash it with ultrapure water until it becomes neutral, and dry it at 120°C for use. Preparation of iron ion-imprinted silica gel: Weigh 8.0 g of ferric acetate into 400 mL of methanol solution, heat and stir until the solid dissolves. Add 29.1 g of mercaptopropyltrimethoxysilane to the above mixture, and heat, stir and reflux at 80° C. for 5.0 h, then add 58.2 g of activated silica gel, and continue heating, stirring, and reflux for 48 h. Post-treatment of iron ion-imprinted silica gel: filter the above-mentioned iron ion-imprinted silica gel, wash with ethanol until no impurities are detected, and then soak in 2.0mol / L acetic acid solution until no iron ions are detected. Finally, the iron ion-imprinted silica gel was washed with ultrapure water to neutrality, and dried at 80° C. for...

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Abstract

The invention discloses a method for preparing an iron ion imprinted silica gel, which relates to an imprinted silica gel. The method for preparing the iron ion imprinted silica gel comprises the following steps of: soaking a silica gel in acid solution, washing the silica gel until the silica gel is neutral, and drying the silica gel to obtain an activated silica gel; putting a salt containing iron ions into a solvent, heating and stirring the salt and the solvent until the solid is dissolved to obtain a mixture; adding mercapto-propyl silane into the mixture, and heating, stirring and refluxing the mixture; adding the activated silica gel into the mixture, and heating, stirring and refluxing the mixture continuously to obtain a crude product of the iron ion imprinted silica gel; filtering the crude product, washing the crude product with a solvent until no impurity is detected, then soaking the crude product with an acid until no iron ion imprinted silica gel is detected, and finally washing the iron ion imprinted silica gel until the iron ion imprinted silica gel is neutral; and drying the iron ion imprinted silica gel to obtain a final product. In the method, the mercapto-propyl silane is used as a functional monomer, and a synthesis technique of molecular engram is utilized. The preparation process is simple and convenient, and is easy to operate, the obtained iron ion imprinted silica gel has high adsorption capacity and certain adsorption selection performance of the iron ions, and the synthesized iron ion imprinted silica gel can be filled to form a small solid phase extraction column which is used for the selective extraction of the iron ions in a water sample.

Description

technical field [0001] The invention relates to an imprinted silica gel, in particular to a method for preparing iron ion imprinted silica gel with certain selective adsorption performance for iron ions by using iron ions as templates on the surface of the silica gel. Background technique [0002] Iron is a common substance in water and an essential trace element for the human body. The general content has no effect on human health. But for the groundwater containing higher iron, it can produce special color, peculiar smell and turbidity, making it difficult to drink ([1] Li Yuan, Chen Qizhou, Ou Guorong, etc., PLA Journal of Preventive Medicine, 2003, 21 (1): 30). In addition, iron in the ocean has a very important impact on the growth of phytoplankton and the level of primary productivity and even becomes a "limiting factor" ([2] Martin J.H., Fitzwater S.E., Gordon M., Global Biogeochem.Cycl., 1990, 4:5), the latest research results show that iron in coastal seawater may ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/286B01J20/30
Inventor 黄晓佳林建斌袁东星
Owner XIAMEN UNIV
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