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Titanic acid nano material absorbent and preparation method thereof

A nanomaterial and titanate nanotube technology is applied in the field of titanate nanomaterial adsorbent and its preparation, which can solve the problems of inconvenient extraction operation, cumbersome operation, low recovery rate and the like, achieve simple reagents and equipment, simple preparation method, The effect of high adsorption capacity

Inactive Publication Date: 2011-07-27
RES CENT FOR ECO ENVIRONMENTAL SCI THE CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The commonly used extraction solvents in ion-to-liquid-liquid extraction are methyl tert-butyl ether (MTBE), acetonitrile and methanol. This method uses a large amount of extraction agents when processing environmental water samples, and the operation is cumbersome, which is not conducive to human health. And environmental protection, low efficiency, poor extraction recovery, sometimes seem powerless to low concentration and complex matrix samples
Commonly used solid phase extraction C 18 and C 8 Silica gel column, a few polymer columns are also used. This method has poor extraction ability for polar and water-soluble perfluoroalkyl sulfonic acids and perfluoroalkyl carboxylic acids, which is not conducive to the enrichment of large volumes of water samples, and the determination sensitivity does not meet the requirements, and C 18 and C 8 The strong hydrophobicity of the silica gel extractant causes them to be in close contact with the water sample solution, resulting in poor extraction effect and low recovery rate, and the extractant must be pretreated before extracting the water sample, which also causes extreme difficulties in the extraction operation. big inconvenience
Low extraction efficiency will lead to a decrease in the accuracy and specificity of the instrument's determination, and it will not be possible to obtain reliable results
In addition, the commonly used broad-spectrum adsorbent is activated carbon, which has a strong adsorption capacity for most organic pollutants in water, especially for organic substances with strong hydrophobicity, but does not have the ability of selective adsorption.

Method used

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  • Titanic acid nano material absorbent and preparation method thereof
  • Titanic acid nano material absorbent and preparation method thereof
  • Titanic acid nano material absorbent and preparation method thereof

Examples

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Embodiment 1

[0032] Example 1 : Invention C 18 -NH 2 - Preparation of TNs adsorbent

[0033] This embodiment is the present invention C 18 -NH 2 -The preparation method of TNs adsorbent. The following combination figure 1 and figure 2 , for C 18 and aminopropyl-modified titanate nanotubes (C 18 -NH 2 -TNs) The preparation method of adsorbent is described in detail as follows:

[0034] First, titanate nanotubes (TNs) were prepared: 3 g of nano-titanium dioxide particles (TP) (purchased from Shanghai Zhuerna High-tech Powder Materials Co., Ltd., particle size 40-50 nm, surface area 15 m 2 / g) was dispersed in 100mL of 10M NaOH solution, electromagnetically stirred for 2 hours to make it fully dispersed, then transferred to a polytetrafluoroethylene autoclave, and heated at 180°C for 10 hours; the obtained titanate nanotubes were washed with deionized water to neutral, and then soaked in 0.5M hydrochloric acid solution for 5 hours, so that the sodium ions in the crystal lattice a...

Embodiment 2

[0041] Example 2 : Invention C 18 -NH 2 -Structural characterization of TNs adsorbent

[0042] This embodiment is to the present invention C 18 -NH 2 - Structural characterization of TNs adsorbents, including the following aspects:

[0043] 1. Morphological observation:

[0044] Use scanning electron microscope S-3000N (SEM, Hitachi) to the present invention C 18 -NH 2 -TNs adsorbent for morphology observation, the results are as follows image 3 shown. At the same time, it is equipped with an energy dispersive X-ray spectrometer EDAX to determine the elemental composition of the adsorbent, according to the element number ratio (C: 30.38%, N: 4.2%, O: 41.65%, Ti: 18.6% and Si: 5.17%) and the two According to the theoretical ratio relationship of Si, C and N in the group, the C prepared by this method is calculated 18 and NH 2 The molar ratio is 1 / 4.

[0045] C obtained using a transmission electron microscope H7500 (TEM, Hitachi, Japan) 18 -NH 2 -TNs adsorbent T...

Embodiment 3

[0052] Example 3 : Invention C 18 -NH 2 -Adsorption capacity test of TNs adsorbent

[0053] This embodiment is to use the present invention C 18 -NH 2 - TNs adsorbent to carry out adsorption experiments on pollutants PFOS and PFOA.

[0054] 1. Adsorption capacity experiment

[0055] The experimental method is as follows: in a 250mL polypropylene container, add 100mL PFOS or PFOA standard solution respectively, and adjust the acidity of the sample to pH 3.0 with 1M HCl and 1M Tris solution. Take 1mg C 18 -NH 2 -TNs adsorbent was added to the solution. In order to investigate the effect of solution acidity on the adsorption of compounds, the pH of the water samples was adjusted in the range of pH 2-10.5, and the concentrations of PFOS and PFOA were both 1 mg / L. The results showed that the adsorption capacity of these two compounds on this adsorbent was the strongest in the pH range of 2-4. Prepare a series of PFOS and PFOA (0.05 ~ 5mg / L) solutions, and examine them at...

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Abstract

The invention provides a titanic acid nano material absorbent for enriching and / or purifying the organic pollutant in the biological and / or environmental samples and a preparation method thereof. The absorbent provided by the invention is a titanic acid nano tube modified by a hydrophobic group and a hydrophilic group simultaneously, preferred a titanic acid nano tube modified by C18 and aminopropyl, which can be uniformly dispersed in the water solution and has high adsorption capacity and better selectivity to the perfluorochemical in virtue of the mixed mechanism of the hydrophobic functionand the electrostatic attraction, and is especially suitable for the enrichment and / or purification of the perfluorooctane sulfonate and the perfluorooctane carboxylic acid in the biological and / or environmental samples. The absorbent provided by the invention is prepared by a hydrothermal method and an sol-gel method. The reagent and device are simple and cheap and the repeatability is good.

Description

technical field [0001] The invention belongs to the field of chemical analysis testing instruments and equipment, and relates to a titanic acid nanomaterial adsorbent for enriching and / or purifying organic pollutants in biological and / or environmental samples and a preparation method thereof. Background technique [0002] Perfluorinated compounds are a class of persistent organic pollutants that widely exist in various environmental media, and are common in the world. The international environmental science community has formed an upsurge in the study of perfluorinated compound pollution, which has become the frontier of environmental science research. Among them, perfluoroalkyl sulfonic acid and perfluoroalkyl carboxylic acid are the two most important types of perfluorinated compounds. Their vapor pressure and volatility are small, and they have strong polarity and high water solubility. For most environmental samples, due to the low concentration of perfluorinated compou...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/30B01J20/06
Inventor 蔡亚岐牛红云
Owner RES CENT FOR ECO ENVIRONMENTAL SCI THE CHINESE ACAD OF SCI
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