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Graphene oxide aerogel solid-phase extraction column special for perfluoro acid compounds and preparation method thereof

A graphene aerogel, solid-phase extraction column technology, applied in the directions of alkali metal compounds, chemical instruments and methods, separation methods, etc., can solve problems such as environmental pollution, low removal efficiency, etc., to improve enrichment efficiency and improve detection. The effect of the lower limit

Pending Publication Date: 2020-07-10
ANYANG INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because these perfluoroalkyl carboxylic acids are stable and refractory substances, they cause great pollution to the environment. However, the traditional AAO process in existing municipal sewage treatment plants has a low removal efficiency for these pollutants, resulting in their use in water. Accumulate in the environment, and become the difficulty of water pollution control

Method used

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  • Graphene oxide aerogel solid-phase extraction column special for perfluoro acid compounds and preparation method thereof
  • Graphene oxide aerogel solid-phase extraction column special for perfluoro acid compounds and preparation method thereof
  • Graphene oxide aerogel solid-phase extraction column special for perfluoro acid compounds and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0026] The preparation of embodiment 1 solid phase extraction column

[0027] The first step is to prepare graphene oxide:

[0028] Adding stage: Prepare a water bath first, accurately measure 110mL of concentrated sulfuric acid and place it in a 500mL three-necked round-bottomed flask, bathe in ice for 15min, and control the temperature between -5-0°C. Then 5g of natural graphite and 2.5g of sodium nitrate are slowly added to the concentrated sulfuric acid (during this feeding process, a weighing paper can be rolled into a funnel and plugged in the rightmost opening of the there-necked bottle, so that the added graphite can be completely added to the concentrated sulfuric acid In order to prevent the graphite from sticking to the bottle wall and unable to completely react with the concentrated sulfuric acid), after stirring for 30 minutes under ice bath, 15 g of potassium permanganate was added slowly (must be added slowly and evenly).

[0029] Low temperature stage: After a...

Embodiment 2

[0036] Embodiment 2: Adsorption to PFOS

[0037] Configure 600mg / L PFOS solution, weigh 1-10mg of aminated graphene oxide airgel in the third step in Example 1, and adsorb at 25°C and 140r / min for 12h; the maximum adsorption capacity is 3702mg / g, and the maximum removal rate 97%, much higher than the adsorption capacity of traditional activated carbon materials (1208mg / g), the adsorption effect is as attached image 3 shown. The adsorption isotherms of EDA-GO gel to PFOS at different temperatures can be seen that the maximum adsorption capacity of this material is 3500mg / g, which is much higher than the adsorption capacity of activated carbon material of 263mg / g. The adsorption isotherm is shown in the attached Figure 4 shown.

Embodiment 3

[0038] Embodiment 3: to the adsorption of PFOA

[0039] Configure 10, 100, 1000mg / LPFOA solutions, weigh 1mg of the third step of aminated graphene oxide airgel in Example 1, and adsorb at 25°C and 140r / min for 12h; the maximum adsorption capacity is 1560mg / g, and the maximum removal rate 99.95%, much higher than the adsorption capacity of traditional activated carbon materials (277 ~ 434.8mg / g), the adsorption effect is as attached Figure 5 shown.

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Abstract

The invention relates to a graphene oxide aerogel solid-phase extraction column special for perfluoro acid compounds and a preparation method thereof. The solid-phase extraction column adopts grapheneoxide aerogel, and the preparation method comprises the following steps: firstly acquiring graphene oxide, then acquiring aminated graphene oxide hydrogel, then preparing aminated graphene oxide aerogel, and finally preparing the solid-phase extraction column. The graphene oxide aerogel prepared by the method does not need to use other polymer support materials, has excellent adsorption performance, can adsorb a lot of perfluoro acid compounds, has higher adsorption capacity and good adsorption effect, can quickly absorb target substances, and enables detection to be faster and more sensitive.

Description

technical field [0001] The invention relates to the technical field of solid phase extraction, in particular to a special graphene oxide airgel solid phase extraction material for perfluorinated acid compounds and a preparation method thereof. Background technique [0002] Solid phase extraction (SPE for short) is a sample pretreatment technology developed since the mid-1980s. It is based on traditional liquid-liquid extraction, combining the principle of similar miscibility of substance interaction and the widely used HPLC The basic knowledge of stationary phases in / GC has gradually developed. Most of SPE is used to process liquid samples, extract, concentrate and purify semi-volatile and non-volatile compounds. The main purpose is to reduce sample matrix interference and improve detection sensitivity. SPE It can also be applied to solid samples, but it must be processed into a liquid first. [0003] Perfluorinated compounds (PFCs), represented by perfluorooctane carboxyl...

Claims

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Application Information

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IPC IPC(8): B01J20/22B01J20/28B01J20/30B01D15/10G01N30/08C02F1/28C02F101/36
CPCB01J20/22B01J20/28047B01D15/10G01N30/08C02F1/285G01N2030/085C02F2101/36
Inventor 田大勇耿丹王涛张大平赵梦磊杨爽郑勇吕会超
Owner ANYANG INST OF TECH
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