Method for removing tetracycline hydrochloride in water by catalytically activating sodium persulfate under visible light by using CeO2 composite BiOI material

A technology of tetracycline hydrochloride and sodium persulfate, applied in the environmental field, can solve problems such as high cost, poor efficiency, and difficult antibiotic degradation, and achieve the effects of high use efficiency, reduced energy cost, and short removal time

Inactive Publication Date: 2020-06-09

POWERCHINA CHENGDU ENG

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AI-Extracted Technical Summary

Problems solved by technology

[0004] The technical problem to be solved by the present invention is that the commonly used method for removing antibiotics in the water environment at home and abroad is not only difficult to completely...

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Abstract

The invention discloses a method for removing tetracycline hydrochloride in water by catalytically activating sodium persulfate under visible light by using a CeO2 composite BiOI material. The methodcomprises the following steps: preparing a rare earth oxide CeO2 composite BiOI material; adding a certain amount of rare earth oxide CeO2 composite BiOI material into a tetracycline hydrochloride aqueous solution, uniformly mixing, and carrying out ultrasonic treatment at room temperature at the frequency of 20khz for 20-45min so that the nano powder of the rare earth oxide composite BiOI material is uniformly dispersed into the tetracycline hydrochloride aqueous solution; adding a certain mass of sodium persulfate into the mixed solution of the rare earth oxide CeO2 composite BiOI material and tetracycline hydrochloride, quickly and uniformly stirring with a glass rod, and carrying out a catalytic reaction under visible light illumination; the method is high in removal rate, short in removal time and simple in process operation, and degradation byproducts are non-toxic and harmless; meanwhile, the selected rare earth oxide is small in dosage, low in price and controllable in cost.

Application Domain

Physical/chemical process catalystsWater/sewage treatment by irradiation +2

Technology Topic

Tetracycline HydrochlorideEnvironmental chemistry +9

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Examples

Experimental program(4)

Example Embodiment

[0038] Example 1

[0039] The present invention utilizes CeO Composite BiOI material Catalytic activation sodium persulfate removes the method for tetracycline hydrochloride in water under visible light, wherein the degradation process of tetracycline hydrochloride is as follows figure 1 As shown, the specific implementation includes the following steps:

[0040] (1) 0.3mmol of CeO 2 The nano powder was ultrasonically dispersed at a frequency of 20khz for 30min in ultrapure water with a volume of 40mL to form a uniform solution A; 3.0mmol of Bi(NO 3 )3·5H 2 O was uniformly magnetically stirred at 160r/min for 45min to dissolve in 30Ml of ethylene glycol solution to form a uniform solution B; 3.0mmol of KI was dissolved in 30mL of ultrapure water, and ultrasonicated at 20khz for 30min to form a uniform solution C;

[0041] (2) Solution B is added dropwise to solution A under magnetic stirring conditions to form mixed solution D, and solution D is magnetically stirred and mixed for a period of time; solution C is added dropwise to solution D under magnetic stirring conditions A mixed solution E is formed, and the mixed solution E is magnetically stirred and mixed for a period of time; wherein, the magnetic stirring speed is 160r/min; the mixed solution D and the mixed solution E are magnetically stirred and mixed for 30min;

[0042] (3) Put solution E in a water bath at 80°C for 2 hours, and magnetically stir at a speed of 160r/min to obtain a mixed solution with a brick-red precipitate. Centrifuge at a centrifugal speed of 4000r/min and a centrifugation time of 10min. The brick-red precipitate was collected by the method, and the precipitate was repeatedly washed with ultrapure water and absolute ethanol. After washing, the precipitate was dried in a vacuum drying oven at 60 ° C and a pressure of 0.06 MPa for 12 hours. Grinding in a bowl to obtain rare earth oxide CeO 2 Composite nanopowder of BiOI material;

[0043] (4) Add the obtained nano-powder into the pretreated water containing tetracycline hydrochloride and mix evenly, and ultrasonically disperse the nano-powder into the tetracycline hydrochloride aqueous solution at room temperature for 20min to 45min at a frequency of 20khz to obtain solution F; The concentration of tetracycline hydrochloride is 100mg/L; the rare earth oxide CeO 2 The mass ratio of the dosing mass of the composite BiOI material to the tetracycline hydrochloride solution is 1:1000;

[0044] (5) Sodium persulfate is added to solution F, and quickly stirred evenly with a glass rod to obtain solution G; the mass ratio of sodium persulfate to pretreated water is 1:1000;

[0045] (6) Add 0.1mol/L~100mol/L perchloric acid and 0.1mol/L~100mol/L sodium hydroxide solution to solution G under the condition of magnetic stirring speed of 150r/min~200r/min In, adjust the pH value to 3.0 to obtain the mixed solution H after adjusting the pH value;

[0046] (7) Solution H is irradiated with visible light to realize the degradation of tetracycline hydrochloride. Among them, the wavelength of visible light is 420-700 nm; the power of the visible light source is 500W; the irradiation time is 30min; while stirring, the stirring speed is 150 r/min.

[0047] (8) Use centrifugation to separate the rare earth oxide CeO2 composite BiOI material, centrifuge at 4000r/min for 10min, collect the rare earth oxide CeO2 composite BiOI material and use a glass fiber membrane with a pore size of 0.45 μm to recover the rare earth oxide CeO 2 The composite BiOI material is filtered, and the filtered rare earth oxide CeO is filtered using ultrapure water and absolute ethanol. 2 The composite BiOI materials were washed 5 to 10 times respectively, and then dried in vacuum at a temperature of 60°C and a pressure of 0.06MPa for 12h to 48h to obtain pure rare earth oxide CeO 2 Composite BiOI materials, and again for the removal of tetracycline hydrochloride in water.

[0048] Wherein there are three possible degradation pathways of tetracycline hydrochloride (TC), as figure 1 As shown, due to the oxidation of OH, the TC structure is destroyed to produce P1 (m/z 477), and then the benzene ring is further attacked by OH, resulting in ketone and carboxyl structures. Due to the low binding energy of N-C bonds, N-dealkylation reaction occurs, and then the carbon ring is further destroyed by SO4·-, and the hydroxyl group is lost to produce P2 (m/z 333). Due to the oxidation of OH, C=O is converted into C-OH, and then attacked by SO4·-, demethylation occurs, and the carbocycle is also destroyed at the same time, forming P3 (m/z 293). And P3 is further oxidized by SO4·-, loses the hydroxyl group, and forms P4 (m/z 261), and further destroys the C-C single bond by OH, and generates demethylation by SO4·-oxidation, forming P5 (m/z 201) . P5 is oxidized by SO4·- to form P6 (m/z 165), and then demethylated to form P7 (m/z 109). Then continue to be mineralized by oxygen vacancies on the surface of BiOI to CO 2 and H 2 O.

[0049] This embodiment is easy to operate, and the degradation by-products are non-toxic and harmless; at the same time, the reaction is carried out at normal temperature and pressure, and the visible light is used to save energy. Compared with other methods for removing antibiotics in water, the cost is reduced by more than 50%;

[0050] In this embodiment, the removal rate of antibiotics in water can reach 99%.

Example Embodiment

[0051] Example 2

[0052] The comparative test of using visible light to remove tetracycline hydrochloride in water is specifically completed according to the following steps:

[0053] 100 mL of tetracycline hydrochloride solution with a concentration of 100 mg/L was magnetically stirred at a speed of 150 r/min under visible light irradiation, and reacted for 30 min to obtain water from which residual antibiotics were removed;

[0054] In embodiment 2, the visible light adopts a xenon lamp light source, and uses a visible light filter to filter out other illuminations other than visible light, and the visible light power is 500W

[0055] In Example 2, the removal rate of antibiotics in pretreated water using sodium persulfate was 0%.

Example Embodiment

[0056] Example 3

[0057] Use sodium persulfate to remove the comparative test of tetracycline hydrochloride in water, specifically complete according to the following steps:

[0058] Add 0.1 g of sodium persulfate to 100 mL of tetracycline hydrochloride solution with a concentration of 100 mg/L, and stir magnetically in the dark at a speed of 150 r/min, and react for 30 min to obtain water that removes residual antibiotics in the water;

[0059] In Example 3, sodium persulfate was used to remove antibiotics in pretreated water with a removal rate of 5%.

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PUM

Property	Measurement	Unit
Wavelength	420.0 ~ 700.0	nm
tensile		MPa
Particle size		Pa
strength	10

Description & Claims & Application Information

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Classification and recommendation of technical efficacy words

High removal rate
Short removal time

Method for removing tetracycline hydrochloride in water by catalytically activating sodium persulfate under visible light by using CeO2 composite BiOI material

A technology of tetracycline hydrochloride and sodium persulfate, applied in the environmental field, can solve problems such as high cost, poor efficiency, and difficult antibiotic degradation, and achieve the effects of high use efficiency, reduced energy cost, and short removal time

AI-Extracted Technical Summary

Problems solved by technology

Abstract

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Examples

Example Embodiment

Example Embodiment

Example Embodiment

PUM

Description & Claims & Application Information

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