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Dilute sulfuric acid and graphene oxide co-doped modified titanium dioxide composite material and preparation method and application thereof

A composite material and titanium dioxide technology, applied in catalyst activation/preparation, alkali metal oxides/hydroxides, chemical instruments and methods, etc., can solve problems such as high ecological risk, water pollution, and insignificant antibiotic effect, and achieve high efficiency Photocatalytic removal, high-efficiency adsorption removal, and high-efficiency impurity removal

Inactive Publication Date: 2020-06-19
WUHAN UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

Luo Fangyuan and others tested tetracycline and oxytetracycline in the sediments of Hongze Lake. These two antibiotics were detected in the sediment of the lake area, and the content range of the two antibiotics was 1.35-25.43 μg kg -1 ; Fang Longfei et al. investigated 6 typical antibiotics in the upper reaches of the Huangpu River in Shanghai, and found that the concentration of tetracycline antibiotics (the average value totaled 34.25-211.82ng·L -1 ) gradually increased from the wet season to the dry season in the upper reaches of the Huangpu River, and it was the main polluting antibiotic in the upper reaches of the Huangpu River; a total of 15 antibiotics in 5 categories were detected in water samples such as Wei Hong, and the average concentration of oxytetracycline in the downstream was the highest; Yanan et al. studied the pollution distribution of five major antibiotics in a typical small watershed of a town in the Yangtze River Delta. Among them, the detection rate of tetracyclic antibiotics (TCs) was 96.9%, and the concentration range was 27.10-133.0ng L -1 , concentrated in agricultural and industrial areas, with high ecological risk
[0004] Tetracycline antibiotics are excreted through feces and urine, causing serious water pollution
However, the effect of conventional water treatment processes on removing antibiotics is not significant. At present, the methods for removing antibiotic pollution in the water environment mainly include biodegradation, chemical oxidation and adsorption.

Method used

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  • Dilute sulfuric acid and graphene oxide co-doped modified titanium dioxide composite material and preparation method and application thereof
  • Dilute sulfuric acid and graphene oxide co-doped modified titanium dioxide composite material and preparation method and application thereof
  • Dilute sulfuric acid and graphene oxide co-doped modified titanium dioxide composite material and preparation method and application thereof

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preparation example Construction

[0040] A preparation method of dilute sulfuric acid and graphene oxide co-doped modified titanium dioxide composite material, comprising the following steps:

[0041] (1) adding tetrabutyl titanate to ethanol to form liquid A;

[0042] (2) Prepare ethanol-sulfuric acid solution, which is added dropwise to liquid A and stirred to obtain a mixed solution;

[0043] (3) The mixed solution is reacted at a constant temperature, and cooled to obtain a slurry after the reaction is complete;

[0044] (4) centrifuging the slurry to obtain a precipitate, washing, drying, and grinding to obtain a powder;

[0045] (5) Obtain sulfuric acid-titanium dioxide composite material after the powder is calcined;

[0046] (6) prepare graphene oxide dispersion liquid;

[0047] (7) adding the sulfuric acid-titanium dioxide composite material to the graphene dispersion and stirring to react to form a suspension;

[0048] (8) After the suspension is reacted at a constant temperature, a crude product...

Embodiment 1

[0060] This embodiment is the preparation of a dilute sulfuric acid modified titanium dioxide composite material and pure titanium dioxide, as follows:

[0061] 1. Preparation of SO 4 2- TiO 2 :

[0062] (1) Take 10mL of tetrabutyl titanate and add 20mL of absolute ethanol to form A liquid (note the order of addition, if tetrabutyl titanate is poured into absolute ethanol, a large amount of white precipitate will be produced);

[0063] (2) Measure 10 mL of absolute ethanol and 10 mL of distilled water to form liquid B; drop liquid B into the stirred liquid A, and stir for 0.5 h to obtain a mixed liquid;

[0064] (3) Transfer the mixed solution to a reaction kettle, keep it in a constant temperature oven at 180°C for 5 hours, and cool naturally to obtain a slurry;

[0065] (4) The slurry is centrifugally cleaned with a high-speed centrifuge, washed 2-3 times with alcohol, and washed with distilled water until neutral, then the precipitate is dried in an oven at 60° C., and ...

Embodiment 2

[0079] Determination of test conditions

[0080] 1. Determination of initial concentration of tetracycline hydrochloride

[0081] This embodiment is the SO prepared in Example 1 4 2- / TiO 2 The test of the effect of the powder on the initial concentration of tetracycline hydrochloride on the adsorption performance, the specific steps are as follows:

[0082] Weigh 50mg of tetracycline hydrochloride and configure it into 1L solution, dilute to 10mg / L, 15mg / L, 20mg / L, 25mg / L, 30mg / L, 35mg / L, 40mg / L in proportion, add 50mg of material (pure TiO 2 , SO 4 2- / TiO 2 ), then carry out the light-dark reaction in a vibrating shaker with a constant temperature T=30°C and a shaking rate V=150rpm in the dark, and shake the adsorption to equilibrium. Take the supernatant, centrifuge, and measure the absorbance value of the solution.

[0083] Test results such as Figure 4 shown. The results show that under the action of different catalysts, the removal rate of tetracycline hydroc...

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Abstract

The invention discloses a dilute sulfuric acid and graphene oxide co-doped modified titanium dioxide composite material and a preparation method and application thereof. The preparation method comprises the following steps: (1) adding tetrabutyl titanate into ethanol to form a solution A, (2) preparing an ethanol-sulfuric acid solution to form a solution B, dropwise adding the solution B into thesolution A, and uniformly stirring to obtain a mixed solution, (3) reacting at constant temperature to obtain slurry, (4) centrifugally separating the slurry, and washing, drying and grinding to obtain powder, (5) calcining to obtain sulfuric acid-titanium dioxide, (6) preparing a graphene oxide dispersion liquid, (7) adding sulfuric acid-titanium dioxide into the graphene oxide dispersion liquidfor a reaction to form a suspension liquid, (8) carrying out constant-temperature reaction on the suspension to obtain a crude product, and (9) washing and drying the crude product to obtain the composite material. The preparation method is simple, low in cost and suitable for large-scale production. The prepared composite material is high in purity, can efficiently degrade tetracycline hydrochloride, and has good application value in the aspect of environmental pollution remediation.

Description

technical field [0001] The invention belongs to the field of titanium dioxide composite materials and water body treatment, and in particular relates to a modified titanium dioxide composite material co-doped with dilute sulfuric acid and graphene oxide for degrading tetracycline hydrochloride wastewater. Background technique [0002] Antibiotics can prevent diseases and promote growth, so they are widely used in disease treatment and animal husbandry production. my country is a big country in the production and use of antibiotics, but in fact, the antibiotics taken cannot be completely absorbed by the body, and most (about 30% to 90%) will be excreted in urine and feces in the form of mothers or metabolite daughters , and then pollute the environment, destroy ecological stability, and ultimately endanger human health. [0003] It has been reported that antibiotics are frequently detected in the waters of the Yangtze River, Taihu Lake, Pearl River, and the upper reaches of t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/20B01J20/28B01J20/30B01J27/053B01J35/10B01J37/08C02F9/04C02F101/38C02F101/36C02F101/34
CPCB01J20/20B01J20/28059B01J27/053B01J37/08B01J37/082C02F1/281C02F1/30C02F1/725C02F2101/38C02F2101/34C02F2101/36B01J35/61B01J35/39
Inventor 王姗汪恂张龙
Owner WUHAN UNIV OF SCI & TECH
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