Preparation of magnetic porous graphene and rapid detection method of low-concentration triclosan in water by employing magnetic porous graphene

A technology of porous graphene and detection method, which can be used in measurement devices, instruments, scientific instruments, etc., can solve the problems of long liquid chromatography analysis time, high maintenance cost, low detection limit, etc.

Pending Publication Date: 2019-06-25
NORTHEAST NORMAL UNIVERSITY
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Problems solved by technology

Spectrophotometry is the most classic quantitative analysis method, but the accuracy is not high; ultra-high performance liquid chromatography is the most commonly used quantitative detection method, but liquid chromatography has the disadvantages of long analysis time, high detection limit, and large amount of organic solvents used. Disadvantages: High performance liquid chromatography-mass spectrometry has the advantages of low detection limit and short analysis time, but mass spectrometer is expensive and maintenance cost is high

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  • Preparation of magnetic porous graphene and rapid detection method of low-concentration triclosan in water by employing magnetic porous graphene
  • Preparation of magnetic porous graphene and rapid detection method of low-concentration triclosan in water by employing magnetic porous graphene
  • Preparation of magnetic porous graphene and rapid detection method of low-concentration triclosan in water by employing magnetic porous graphene

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preparation example Construction

[0037] The invention provides a kind of preparation method of magnetic porous graphene, comprises the following steps:

[0038] (1) Graphene oxide and potassium hydroxide are mixed and activated to obtain porous graphene oxide;

[0039] (2) The porous graphene oxide, ferric chloride, sodium acetate and ethylene glycol are mixed for hydrothermal reaction to obtain magnetic porous graphene.

[0040] Graphene oxide and potassium hydroxide are mixed for activation treatment to obtain porous graphene oxide. In the present invention, the graphene oxide is preferably prepared by exfoliating flake graphite by a closed oxidation method, and the closed oxidation method preferably includes the following steps:

[0041] After mixing flake graphite, potassium permanganate and concentrated sulfuric acid, the low-temperature airtight oxidation reaction and high-temperature airtight oxidation reaction are carried out successively to obtain an oxidation reaction solution;

[0042] After dilu...

Embodiment 1

[0078] Graphene oxide (GO) is synthesized by using a closed oxidation method to prepare GO by chemical oxidation and exfoliation of flake graphite. The specific steps are as follows:

[0079] (1) Before the start of the experiment, put the used medicine and the inner tank of the reaction kettle into the refrigerator, and store them in cold storage at 4°C to ensure that the inner tank of the reaction kettle is dry.

[0080] (2) Weigh 1g flake graphite and 5g potassium permanganate respectively, mix them uniformly and pour them into a 100mL reactor liner, and then put the reactor liner into a stainless steel reactor jacket. Quickly add 50mL of concentrated sulfuric acid to the inner tank, quickly cover the inner tank cover and rotate the stainless steel reaction kettle cover tightly.

[0081] (3) Put the reaction kettle into the refrigerator, and store it in cold storage at 4°C for 14 hours. After the low-temperature reaction, put the reaction kettle into a 100°C oven to heat qu...

Embodiment 2

[0086] (1) Weigh 2g of GO prepared in Example 1 and 8g of potassium hydroxide, mix them into a tubular resistance furnace filled with nitrogen protection, and the resistance furnace is heated to 800°C at a rate of 5°C / min, and kept 1h. During this process, nitrogen gas has been fed in at a flow rate of 500 mL / min.

[0087] (2) After natural cooling, wash repeatedly 3 times with 0.1M hydrochloric acid solution and deionized water respectively, put into drying box and dry for 12h, take out, the powder at this moment is porous graphene oxide.

[0088] (3) Weigh 0.3 g of porous graphene oxide and dissolve it in 80 mL of ethylene glycol, and disperse it ultrasonically for 30 min. Weigh 0.3g of ferric chloride and 3.6g of sodium acetate and dissolve in 60mL of ethylene glycol, and ultrasonically disperse for 30min.

[0089] (4) After ultrasonication, the above two solutions were mixed and vigorously stirred for 1 hour, then poured into a 200 mL reactor, put the reactor into an ove...

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Abstract

The present invention relates to the field of water quality detection, and provides a preparation method of magnetic porous graphene. The oxidized graphene and potassium hydroxide are mixed for activating treatment, and the obtained porous oxidized graphene, ferric trichloride, sodium acetate and ethylene glycol are mixed for hydrothermal reaction to obtain magnetic porous grapheme. The magnetic porous grapheme has huge superficial area, can absorb a lot of triclosan, has magnetism and is convenient for recycle. The present invention further provides a rapid detection method of low-concentration triclosan in water. The method takes the magnetic porous grapheme as an adsorption substrate to absorb triclosan in water, achieves separation through a magnet, and detects the content of the triclosan through steps of elution, derivatization and extraction. The method is simple in operation, is low in detection limit, does not need to use a mass spectrometer, only uses a gas chromatograph fordetection, is good in repeatability, high in recovery rate, and mature and reliable, and can be applied to detection of the content of the triclosan in the actual waste water.

Description

technical field [0001] The invention relates to the technical field of water quality detection, in particular to a preparation of magnetic porous graphene and a rapid detection method applied to low-concentration triclosan in water. Background technique [0002] Dichlorophenoxychlorophene, also known as triclosan (TCS), as a synthetic broad-spectrum antibacterial agent, is widely used in personal care products such as toothpaste, mouthwash, soap, laundry detergent, body wash and shampoo . TCS has been frequently detected in wastewater and natural reservoirs due to the inefficiency of conventional treatment processes in wastewater treatment plants (WWTPs) for organic micropollutants such as TCS. It has been reported that TCS can undergo photodegradation in water and generate more toxic intermediate by-products, such as dibenzodichlorodioxin, etc. In addition, free chlorine added during drinking water treatment can react with TCS to generate some carcinogenic chlorinated dis...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
Inventor 杨武李烨刘仲谋霍明昕范伟朱遂一王宪泽
Owner NORTHEAST NORMAL UNIVERSITY
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