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Nano-SiO2 adsorption material and preparation method and application thereof

An adsorption material and nanotechnology, applied in chemical instruments and methods, preparation of test samples, and other chemical processes, etc., can solve the problems of low efficiency, low adsorption capacity, low exchange capacity of precipitation method, etc. mild conditions

Inactive Publication Date: 2010-11-24
JIAXING UNIV
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

The efficiency of the precipitation method is low, and other impurities will be introduced while precipitating metal ions; the selectivity of the ion exchange method is poor and the exchange capacity is low; the liquid-liquid extraction method will use different solvents, which will cause secondary pollution to the environment, and also involves Solvent recovery problem; solid phase extraction is the main method for separating / enriching metal ions developed in recent years, and the research and development of adsorption materials is a key technology. Although there are many types of adsorption materials currently developed, they all have their own shortcomings. In summary, there are mainly the following defects: 1) The adsorption capacity is low, 2) The price of the adsorption material is high

Method used

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  • Nano-SiO2 adsorption material and preparation method and application thereof
  • Nano-SiO2 adsorption material and preparation method and application thereof
  • Nano-SiO2 adsorption material and preparation method and application thereof

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Experimental program
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Effect test

Embodiment 1

[0031] The synthesis of embodiment 1 nano silicon dioxide material

[0032] Accurately weigh 1.00 g (0.017 mol) of nano-silica that has been thermally pretreated at 110°C for 4 hours in a 150 mL three-necked flask, add 50 mL of toluene, degas it ultrasonically for 30 minutes, add 0.0425 aminopropyltriethoxysilane ( KH-550), ultrasonic degassing for 10 minutes. In pass N 2 Under the conditions, the reaction temperature is controlled at 80° C., and the reaction is stirred for 9 hours to obtain nano-silica aminopropylsilane.

[0033] p-Bromomethylbenzoic acid (1.70g, 7.9mmol), triphenylphosphine (2.10g, 8.0mmol) and tetrahydrofuran (30mL) reacted at 80°C for 8 hours, cooled to room temperature, added 10mL of diethyl ether, precipitated and filtered , heating, when the temperature rose to 80 ° C, began to drop thionyl chloride (7mL), dropped after 20 minutes, continued to keep warm for 3 hours, until no more gas escaped, distilled, and dried to obtain a reddish-brown solid ClOC- ...

Embodiment 2

[0036] Structural characterization of the synthesized nano-silica bonded organic functional reagent adsorbent and raw nano-silica-infrared spectra.

[0037] Raw materialNano-SiO 2 There are a lot of hydroxyl groups on the surface, so at 3435.68cm -1 There are large absorption peaks nearby. 1625.95cm -1 The absorption peak at is from adsorbed water, 1107.03cm -1 The strong absorption at is from the asymmetric stretching vibration of the Si-O-Si bond, 789.19cm -1 and 464.86cm -1 The absorption peak at is from the bending vibration of the Si-O-Si bond. exist figure 2 Medium 1684.32cm -1 A strong absorption peak at is from the carbonyl stretching vibration, 3435.68cm -1 A strong absorption peak at is from the stretching vibration of the associated amino group, 3052.97cm -1 The absorption peak at is from the stretching vibration of C-H in the benzene ring, 1113.51cm -1 The strong absorption at is from the asymmetric stretching vibration of the Si-O-Si bond, 776.22cm -1 ...

Embodiment 3

[0039] The determination of embodiment 3 solution pH value

[0040] 0.1g of prepared nano-silica material (Si|(CH 2 ) 3 -NH-CO-Ph-CH 2 -P-(C 6 h 5 ) 3 -Br), add 2.00 mL of Cr with a concentration of 50 μg / mL 2 o 7 2- Solution, adjust the pH, shake for 30 minutes, let stand for 1h, transfer the supernatant and centrifuge for 10 minutes, dilute the concentration to the optimal linear range, and detect the residual Cr by flame atomic absorption spectrometry 2 o 7 2- Ion residual amount, calculate its adsorption rate A%, in order to compare its adsorption effect, use the same amount of nano silicon dioxide to carry out comparative experiment. Experimental results such as image 3 As shown, it can be seen from the figure that the adsorption efficiency of the synthesized adsorbent reaches a maximum of 97.79% at pH=1. With the increase of pH, the adsorption efficiency decreased continuously. And nano-silica is to Cr at pH=1 2 o 7 2- The maximum ion adsorption efficien...

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Abstract

The invention relates to a nano-SiO2 adsorption material. The preparation method comprises the following step: using nano-SiO2, aminopropyl alkyl and -CO-C6H4-CH2P+(C6H5)3Br- to perform a chemical reaction and prepare the nano-SiO2 adsorption material through covalent linkage. The preparation method is simple, the conditions are mild, and product can be used to separate / concentrate trace Cr2O7<2-> in the environment. The nano-SiO2 adsorption material of the invention has the advantages of high adsorption efficiency, easy operation, no secondary pollution and the like.

Description

technical field [0001] The invention relates to a modified material, in particular to a nano-SiO modified with an organic functional reagent 2 Adsorption material and the preparation method of the material, the prepared adsorption material can be used for trace Cr in the environment 2 o 7 2- Separation / enrichment. Background technique [0002] In recent years, industries using chromium compounds, such as electroplating, chemical industry, leather industry, etc., have achieved remarkable economic benefits, thus greatly promoting the scale production of chromium salt factories. The high-concentration hexavalent chromium ions in the chromium-containing waste residue and wastewater generated during the production of chromium salts are toxic to the human body, crops, and livestock. Hexavalent chromium enters the human blood to form chromium oxide, causing hemoglobin to become methemoglobin , The function of red blood cells to carry oxygen is impaired, leading to cell suffocat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/22B01J20/30G01N1/40
Inventor 张祖磊李蕾
Owner JIAXING UNIV
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