CN115106128A - Preparation method of nano composite material capable of adsorbing and detecting cadmium ions and simultaneously strengthening photocatalytic degradation of tetracycline - Google Patents

Preparation method of nano composite material capable of adsorbing and detecting cadmium ions and simultaneously strengthening photocatalytic degradation of tetracycline Download PDF

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Publication number
CN115106128A
CN115106128A CN202210804483.5A CN202210804483A CN115106128A CN 115106128 A CN115106128 A CN 115106128A CN 202210804483 A CN202210804483 A CN 202210804483A CN 115106128 A CN115106128 A CN 115106128A
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China
Prior art keywords
tetracycline
adsorbing
cadmium ions
thiocarbazone
photocatalytic degradation
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CN202210804483.5A
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Chinese (zh)
Inventor
蒋华麟
范东东
陈萍华
邓颖
吴光辉
李松原
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Nanchang Hangkong University
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Nanchang Hangkong University
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    • B01J35/39
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/22Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B01J20/223Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material containing metals, e.g. organo-metallic compounds, coordination complexes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J31/00Catalysts comprising hydrides, coordination complexes or organic compounds
    • B01J31/02Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
    • B01J31/04Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing carboxylic acids or their salts
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J31/00Catalysts comprising hydrides, coordination complexes or organic compounds
    • B01J31/16Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes
    • B01J31/22Organic complexes
    • B01J31/2204Organic complexes the ligands containing oxygen or sulfur as complexing atoms
    • B01J31/2208Oxygen, e.g. acetylacetonates
    • B01J31/2226Anionic ligands, i.e. the overall ligand carries at least one formal negative charge
    • B01J31/2243At least one oxygen and one nitrogen atom present as complexing atoms in an at least bidentate or bridging ligand
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • C02F1/285Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/30Treatment of water, waste water, or sewage by irradiation
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2531/00Additional information regarding catalytic systems classified in B01J31/00
    • B01J2531/40Complexes comprising metals of Group IV (IVA or IVB) as the central metal
    • B01J2531/46Titanium
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/10Inorganic compounds
    • C02F2101/20Heavy metals or heavy metal compounds
    • C02F2101/22Chromium or chromium compounds, e.g. chromates
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/38Organic compounds containing nitrogen
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2305/00Use of specific compounds during water treatment
    • C02F2305/10Photocatalysts
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W10/00Technologies for wastewater treatment
    • Y02W10/30Wastewater or sewage treatment systems using renewable energies
    • Y02W10/37Wastewater or sewage treatment systems using renewable energies using solar energy

Abstract

The invention discloses a preparation method of a tetracycline nanocomposite material capable of adsorbing and detecting cadmium ions and simultaneously strengthening photocatalytic degradation, which comprises the following steps: TO 2 And 1, 5-diphenylcarboxylic acidStirring the 3-thiocarbazone in a mixed solution of propanol and water for reaction, and finally cleaning and drying to obtain a final product; the nano composite material prepared by the invention can detect and adsorb to remove cadmium ions, can degrade tetracycline through photocatalysis, is simple to prepare, has low cost, and is suitable for large-area popularization and application.

Description

Preparation method of nano composite material capable of adsorbing and detecting cadmium ions and simultaneously strengthening photocatalytic degradation of tetracycline
Technical Field
The invention relates to the technical field of wastewater treatment, in particular to a preparation method of a tetracycline nanocomposite capable of adsorbing and detecting cadmium ions and simultaneously strengthening photocatalysis degradation.
Background
With the rapid development of human society, the environmental pollution of the earth is increasingly serious, and the environmental pollution becomes a difficult problem to be solved urgently in many countries. Among them, the large-area use of heavy metal ions and antibiotics causes the problem of the residual heavy metal ions and antibiotics in the environment to attract extensive attention of many scholars. After entering the environment, a lot of heavy metals cannot be biodegraded, so that the atmosphere, drinking water and agricultural and sideline products are polluted, and can be ingested into human bodies through breathing and diet, and the heavy metals are accumulated due to the enrichment action of food chains and organisms, so that the heavy metals are finally seriously harmful to human beings; many remain antibiotics and get into the water after, still can stay in the middle of waste water with prototype or metabolite, have serious harm to the existence of the animals and plants in aqueous, very easily destroy the ecological balance in the water, produce the microorganism of drug resistance easily, including it is difficult by the degradation in the water, through the circulation of water, get into the human body through the drinking water, have had very big threat to human health in long-term accumulation. Therefore, the treatment of the residual heavy metal ions and antibiotics is not slow.
For Cd 2+ Removal and detection, and research into tetracycline removal methods have attracted a wide range of interest to researchers, such as songhangong patent application no: 201210568784.9 method for trapping Cd by polyamine adsorbing material 2+ (ii) a Patent application number of Zhuweiqin: 202110321634.7 method for removing Cd by adsorbing with functional earthworm excrement 2+ (ii) a Patent application No. of Dandan: 201610463716.4 detection of Cd by using carbon quantum dot/gold cluster ratiometric fluorescent probe 2+ (ii) a Plum blossom patentApplication No.: detection of Cd by biosensor in 202110807990.X 2+ (ii) a Zhang Zhanghu patent application number: 202011018452.4 patent application No. of Xujing stamen for removing tetracycline in water by using magnetic sludge biochar activated by zinc chloride: 202210058730.1 removing tetracycline and the like in the water body by using an algae-bacteria complex; however, these methods can only treat Cd alone 2+ Or tetracycline, cannot synergistically co-process Cd 2+ And tetracycline.
Based on the technical background, the technology discloses a preparation method of a functional nano composite material, and particularly relates to a preparation method of a nano composite material capable of adsorbing and detecting cadmium ions and simultaneously strengthening photocatalytic degradation of tetracycline.
Disclosure of Invention
The invention aims to solve the technical problems in the prior art and provides a preparation method of a tetracycline nanocomposite capable of adsorbing and detecting cadmium ions and simultaneously strengthening photocatalytic degradation.
In order to achieve the purpose, the technical scheme provided by the invention is as follows: a preparation method of a nano composite material capable of adsorbing and detecting cadmium ions and simultaneously strengthening photocatalytic degradation of tetracycline comprises the following preparation steps:
(1) the method of the prior art is adopted to prepare the nano TiO 2
(2) Preparing 1, 5-diphenylcarboxyl-3-thiocarbazone by adopting the prior art method;
(3) nano TiO prepared in the step (1) 2 Stirring the 1, 5-diphenylcarboxyl-3-thiocarbazone prepared in the step (2) in a mixed solution A of 20mL of acetone and water for reacting for 4h to obtain a reaction product B;
(4) and (3) alternately cleaning the reaction product B with deionized water and ethanol for three times respectively, and drying at 50 ℃ to obtain the product obtained by the method.
Preferably, the volume ratio of acetone to water in the mixed solution a is 1: 1.
Preferably, the nano TiO put into the step (3) 2 The amount of the 1, 5-diphenylcarboxy-3-thiocarbazone to be added is 0.2 to 0.6gIs 1-5 mg.
The invention has the beneficial effects that:
the nano composite material prepared by the invention can detect and adsorb to remove cadmium ions, can degrade tetracycline through photocatalysis, is simple to prepare, has low cost, and is suitable for large-area popularization and application.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention and not to limit the invention.
FIG. 1 is a scanning electron micrograph of the product of example 2;
FIG. 2 is a graph showing the change of the visible light absorption wavelength of a product of example 2 of the present invention after adsorbing Cd2 +;
FIG. 3 is an adsorption isotherm diagram of the product of example 2 of the present invention adsorbing Cd2 +;
FIG. 4 is a diagram of the photocatalytic degradation of tetracycline by the product of example 2 of the present invention.
Detailed Description
Reference will now be made in detail to the present preferred embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like reference numerals refer to like elements throughout.
Referring to fig. 1 to 4, a method for preparing a tetracycline nanocomposite capable of adsorbing and detecting cadmium ions and simultaneously enhancing photocatalytic degradation is disclosed in the preferred embodiment of the present invention, and the method is characterized in that: the method comprises the following preparation steps:
(1) the method for preparing nano TiO by adopting the prior art 2
(2) Preparing 1, 5-diphenylcarboxyl-3-thiocarbazone by adopting the prior art method;
(3) nano TiO prepared in the step (1) 2 Stirring the 1, 5-diphenylcarboxyl-3-thiocarbazone prepared in the step (2) in a mixed solution A of 20mL of acetone and water for reacting for 4h to obtain a reaction productB;
(4) And respectively washing the reaction product B with deionized water and ethanol for three times alternately, and then drying at 50 ℃ to obtain the product obtained by the method.
As a preferred embodiment of the present invention, it may also have the following additional technical features:
in this example, the volume ratio of acetone to water in the mixed solution a was 1: 1.
In this embodiment, the nano TiO charged in the step (3) 2 The amount of the 1, 5-diphenylcarboxy-3-thiocarbazone is 0.2-0.6 g, and the amount of the 1, 5-diphenylcarboxy-3-thiocarbazone added is 1-5 mg.
The technical solution of the present invention will be described in detail with reference to the specific embodiments of the present application. However, the scope of the present invention is not limited to the following specific examples.
Detailed description of the preferred embodiment 1
Synthesizing nano TiO by conventional method 2 And 1, 5-diphenylcarboxy-3-thiocarbazone (DAT);
0.2g of nano TiO 2 And 1mg of DAT are dispersed in 20mL of mixed solution A of acetone and water (the volume ratio of the acetone to the water is 1:1), the mixture is stirred and reacted for 4 hours to obtain a reaction product B, the reaction product B is alternately washed three times by deionized water and ethanol respectively, and then the reaction product B is dried at 50 ℃ to obtain the product obtained by the method.
Specific example 2
Synthesizing nano TiO2 and 1, 5-diphenylcarboxyl-3-thiocarbazone (DAT) by adopting a conventional prior art method;
dispersing 0.3g of nano TiO2 and 2mg of DAT into 20mL of mixed solution A of acetone and water (the volume ratio of acetone to water is 1:1), stirring and reacting for 4h to obtain a reaction product B, alternately cleaning the reaction product B with deionized water and ethanol for three times respectively, and drying at 50 ℃ to obtain the product obtained by the method.
FIG. 1 is a scanning electron microscope image of the product of example 2, from which it can be seen that the material morphology is uniform and regular; FIG. 2 is a graph showing the change of the absorption wavelength of visible light after Cd2+ is adsorbed by the product of embodiment 2; FIG. 3 is an adsorption isotherm diagram of the adsorption of Cd2+ by the product of specific example 2; FIG. 4 is a diagram of the photocatalytic degradation of tetracycline by the product of the embodiment 2.
Specific example 3
Synthesizing nano TiO2 and 1, 5-diphenylcarboxyl-3-thiocarbazone (DAT) by adopting a conventional prior art method;
dispersing 0.5g of nano TiO2 and 3mg of DAT into 20mL of acetone-water mixed solution A (the volume ratio of acetone to water is 1:1), stirring and reacting for 4h to obtain a reaction product B, alternately cleaning the reaction product B with deionized water and ethanol for three times respectively, and drying at 50 ℃ to obtain the product obtained by the method.
Specific example 4
Synthesizing nano TiO2 and 1, 5-diphenylcarboxyl-3-thiocarbazone (DAT) by adopting a conventional prior art method;
dispersing 0.6g of nano TiO2 and 5mg of DAT in 20mL of acetone and water mixed solution A (the volume ratio of acetone to water is 1:1), stirring and reacting for 4h to obtain a reaction product B, alternately cleaning the reaction product B with deionized water and ethanol for three times respectively, and drying at 50 ℃ to obtain the product obtained by the method.
The nano composite material prepared by the invention can detect and adsorb to remove cadmium ions, can degrade tetracycline through photocatalysis, is simple to prepare, has low cost, and is suitable for large-area popularization and application.
The above additional technical features can be freely combined and used in superposition by those skilled in the art without conflict.
The above description is only a preferred embodiment of the present invention, and the technical solutions that achieve the objects of the present invention by basically the same means are all within the protection scope of the present invention.

Claims (3)

1. A preparation method of a nano composite material capable of adsorbing and detecting cadmium ions and simultaneously strengthening photocatalytic degradation of tetracycline is characterized in that: the method comprises the following preparation steps:
(1) the method for preparing nano TiO by adopting the prior art 2
(2) Preparing 1, 5-diphenylcarboxyl-3-thiocarbazone by adopting the prior art method;
(3) nano TiO prepared in the step (1) 2 Stirring the 1, 5-diphenylcarboxyl-3-thiocarbazone prepared in the step (2) in a mixed solution A of 20mL of acetone and water for reacting for 4h to obtain a reaction product B;
(4) and respectively washing the reaction product B with deionized water and ethanol for three times alternately, and then drying at 50 ℃ to obtain the product obtained by the method.
2. The method for preparing the tetracycline nanocomposite capable of adsorbing and detecting cadmium ions and simultaneously enhancing photocatalytic degradation according to claim 1, wherein the method comprises the following steps: the volume ratio of acetone to water in the mixed solution A is 1: 1.
3. The method for preparing the tetracycline nanocomposite capable of adsorbing and detecting cadmium ions and simultaneously strengthening photocatalytic degradation according to claim 1, wherein the method comprises the following steps: the nano TiO put into the step (3) 2 The amount of the 1, 5-diphenylcarboxy-3-thiocarbazone is 0.2-0.6 g, and the amount of the 1, 5-diphenylcarboxy-3-thiocarbazone added is 1-5 mg.
CN202210804483.5A 2022-07-08 2022-07-08 Preparation method of nano composite material capable of adsorbing and detecting cadmium ions and simultaneously strengthening photocatalytic degradation of tetracycline Pending CN115106128A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1970537A (en) * 2005-11-22 2007-05-30 上海三爱思试剂有限公司 Process for manufacturing diphenylthiocarbazone
CN110352256A (en) * 2016-10-19 2019-10-18 不列颠哥伦比亚大学 The technique for leaching metal sulfide with the reagent with thiocarbonyl functionality
CN114377728A (en) * 2021-12-30 2022-04-22 浙江优丽全立消科技有限公司 Preparation method of nano material capable of simultaneously detecting and adsorbing cadmium ions and degrading tetracycline through photocatalysis

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1970537A (en) * 2005-11-22 2007-05-30 上海三爱思试剂有限公司 Process for manufacturing diphenylthiocarbazone
CN110352256A (en) * 2016-10-19 2019-10-18 不列颠哥伦比亚大学 The technique for leaching metal sulfide with the reagent with thiocarbonyl functionality
CN114377728A (en) * 2021-12-30 2022-04-22 浙江优丽全立消科技有限公司 Preparation method of nano material capable of simultaneously detecting and adsorbing cadmium ions and degrading tetracycline through photocatalysis

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
高鸿宾等, 高等教育出版社 *

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