CN110270327A - A kind of catalyst and preparation method of the quick dealuminated USY cataluyst Florfenicol of photoelectrocatalysis - Google Patents
A kind of catalyst and preparation method of the quick dealuminated USY cataluyst Florfenicol of photoelectrocatalysis Download PDFInfo
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- CN110270327A CN110270327A CN201811134948.0A CN201811134948A CN110270327A CN 110270327 A CN110270327 A CN 110270327A CN 201811134948 A CN201811134948 A CN 201811134948A CN 110270327 A CN110270327 A CN 110270327A
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- florfenicol
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
- B01J23/44—Palladium
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/36—Organic compounds containing halogen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Health & Medical Sciences (AREA)
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Abstract
The present invention provides a kind of catalyst of the quick dealuminated USY cataluyst Florfenicol of photoelectrocatalysis: in titanium dioxide nanotube array photocatalyst (TiO2NTS palladium nano-particles, TiO are loaded on)2NTS is photochemical catalyst and has hollow tubular structures, large specific surface area, is the load feasible material of palladium nano-particles.Prepare TiO2NTS is to utilize electrochemical oxidation method, then be placed in Muffle furnace and burn to 400~500 °, and high temperature sintering is anatase TiO after 4h2Then NTS prepares 5mmol PdCl2Aqueous solution uses potential step method electroreduction depositing Pd using electrochemical workstation, to prepare Pd/TiO2NTS.Under the action of sunlight, TiO2NTS generate hydroxyl radical free radical can degrade Florfenicol simultaneously Technique of Nano Pd can H under electro-catalysis environment in activated solution carry out reduction dechlorination, to achieve the purpose that fast degradation pollutant.The catalyst has efficient, non-toxic, environmental protection, the characteristic easily produced in batches, can have the function that protection environment, environment purification with the organic pollutant of removal difficult in fast degradation water.
Description
Technical field
The present invention relates to environmental technology field is belonged to, specially a kind of quick dealuminated USY cataluyst Florfenicol of photoelectrocatalysis is urged
Agent and preparation method.
Background technique
Since nineteen twenty-nine penicillin comes out, antibiotic has become the sharp weapon for improving human and animal's health.One
A little countries, veterinary antibiotic is usually also added into animal feed, to improve the speed of growth and feed efficiency.The mankind and animal doctor
The antibiotic used is mainly to pass through urine and excrement discharge, wherein being greatly with the discharge of unchanged active form
's.Antibiotic is added in the waste water and sludge of sewage treatment plants (WWTPs), hospital and livestock farm, leads to antibiosis
Element is released to surface water and soil etc. and receives in environment.In different environmental regionalizations, such as WWTPs, herding farm, river water
With deposit, soil and groundwater, it has been reported that various antibiotic.Remaining antibiotic may be to non-targeted life in environment
Object generates adverse effect, contaminated food and drinking water supply, and increases resistance.
Florfenicol is to be developed by Sehering-Plough company as one of antibiotic the 1980s
Amides alcohols animal semisynthetic antibiotics of new generation.The wide, nothing with good, safe and efficient, the internal distribution of has a broad antifungal spectrum, absorbability
It is the characteristics of alpastic anemia, significant in efficacy to zoogenetic infection caused by sensitive bacteria.It is widely used to domestic animal, poultry and
Aquaculture.The residual of Florfenicol and its metabolin in animal body can not only endanger safety and the people of animal derived food
Body health, can also be discharged into environment together with animal wastes, endanger natural ecological environment.Currently, the research of Florfenicol has very
Various aspects, including clinical medicine is carried out on domestic animal, metabolism dynamic regime in vivo, and analysis medicament residue are studied in animal sources
The property medium aspect of food.Florfenicol enters in animal body and after being discharged in excrement and urine, influences Florfenicol in environment
There is not been reported for the factor of middle degradation and its degradation rate.China is at present to the usage amount of Florfenicol every year about 10000
Ton or so, this is very big for the natural environment and Human health effects in China, for the workload of Florfenicol degradation removal
It is great.Degrade and remove that such antibiotic is particularly important, for water pollutant removal at present mostly using biology at
Logos, but biological treatment is to the degradation effect very little of antibiotic, so the present invention synthesizes a kind of catalyst of quick dechlorination,
It purifies water, protects environment.
Summary of the invention
The present invention provides the catalyst and preparation method of a kind of quick dealuminated USY cataluyst Florfenicol of photoelectrocatalysis, Yi Zhongwen
Fixed efficient catalyst, can efficiently quickly be degraded in a manner of dechlorination under the conditions of photoelectricity Florfenicol.
A kind of catalyst and preparation method of the quick dealuminated USY cataluyst Florfenicol of photoelectrocatalysis, the catalyst are that load is received
The TiO of rice palladium particle2The composite material of NTS, the preparation method comprises the following steps: choosing business titanium silk, clip 40cm coiled is used respectively
It acetone, ethyl alcohol, deionized water ultrasonic half an hour, is then placed in drying box dry.The titanium silk wound is taken out, as sun
Pole, platinum guaze do cathode, at room temperature constant voltage 30V, aoxidize 8h, electrolyte is by the hydrofluoric acid of mass fraction 2%, and solvent is two
Methyl sulfoxide takes out immediately after the completion of oxidation, dries.What oxidation came out is the titanium dioxide crystal of amorphous state, performance ratio
Poor, the present invention calcines 4h using Muffle furnace under 500 °, prepares TiO2The anatase form titanium dioxide of NTS, to promote it
Performance.In order to further widen the photoelectric respone ability of material, the present invention has further modified titania nanotube, has passed through
Prepare the PdCl of 5mmol/L2Solution, titanium wire material are cathode, and platinum guaze is as anode, more potential step method uniform deposition Technique of Nano Pd
Particle, the reducing power that incident photon-to-electron conversion efficiency, catalysis efficiency, while palladium can be improved in the presence of precious metal palladium is strong, and palladium can be in fluorine
Benzene Buddhist nun is admitted to catalytic hydrodehalogenation, and under photoelectrocatalysis effect, nano titania catalyst is under illumination condition, hole Jiang Shui
In hydroxyl be oxidized to hydroxyl radical free radical, oxidative degradation Florfenicol, new catalyst is to Florfenicol in light in summary
There is fast degradation ability under electro-catalysis.
The present invention it is novel the utility model has the advantages that
(1) it can efficiently use solar energy, electric energy degrades organic pollutant, reach and purify water, protect environment
Purpose;
(2)TiO2NTS has the hollow tubular structures of large area, and large specific surface area can be very equal by palladium nano-particles
Even loads to around nanotube;
(3) catalyst has efficient, non-toxic, environmental protection, the characteristic easily produced in batches.
Detailed description of the invention:
Fig. 1 is the material different multiplying electron microscope that present example 1 obtains.
Fig. 2 is photoelectric catalysis degrading figure of 2 material of present example to Florfenicol.
Specific embodiment
Embodiment 1
Experiment uses the anodic oxidation of constant voltage method, chooses business titanium silk, clip 40cm coiled, respectively with third
It ketone, ethyl alcohol, deionized water ultrasonic half an hour, is then placed in drying box dry.The titanium silk that winds is taken out, as anode,
Platinum guaze does cathode, at room temperature constant voltage 30V, aoxidizes 8~10h, electrolyte is by the hydrofluoric acid of mass fraction 2%, and solvent is
Dimethyl sulfoxide takes out immediately after the completion of oxidation, dries.What oxidation came out is the titanium dioxide crystal of amorphous state, performance
Poor, the present invention calcines 4h using Muffle furnace under 400~500 °, the anatase titanium dioxide in right 1 is prepared, to mention
Rise its performance.In order to further widen the photoelectric respone ability of material, the present invention has further modified titania nanotube,
Configure the Pdcl of 5mmol/l2Solution uses occasion China electrochemical workstation as laboratory apparatus, using more potential step methods by palladium
Evengranular reduction is on titania nanotube.
Embodiment 2
In degradation experiment, the Na of 0.5mol/l is prepared before this2SO4Solution takes 100ml as the fluorine of solvent configuration 20mg/l
Benzene Buddhist nun examines, and using xenon lamp as analog light source, electrochemical workstation is power supply, relies on three-electrode system, composite material as cathode,
Anode is platinum guaze, and Ag/AgCl is reference electrode, fast in 2h with the Florfenicol of photoelectrocatalysis at room temperature under the bias of -1.2V
95% or more prompt drop solution purifies the purpose of water resource to reach degradation of contaminant.
Claims (5)
1. a kind of catalyst of the quick dealuminated USY cataluyst Florfenicol of photoelectrocatalysis, which is characterized in that the catalyst is that load is received
The composite material of the TiO2NTS of rice palladium particle.
2. a kind of preparation method of the catalyst of the quick dealuminated USY cataluyst Florfenicol of photoelectrocatalysis, which is characterized in that use anodic oxygen
The preparation of change method, the specific steps are as follows:
(1) titanium silk is put into anode in electrolytic cell, and platinum guaze is cathode, and additional 30V bias aoxidizes 8h at room temperature, is with titanium silk
Substrate prepares the titanium dioxide of amorphous state;
(2) drying is taken out, 500 ° of high-temperature calcination 4h of Muffle furnace are placed on, is converted by amorphous state titanium dioxide crystal to sharp
Titanium ore;
(3) PdCl of 5mmol/L is prepared2Solution, titanium wire material are cathode, and platinum guaze is uniform using more potential step methods as anode
Nanoparticle palladium is deposited on the titanium dioxide for the anatase form that step (2) obtains.
3. a kind of preparation method of the catalyst of the quick dealuminated USY cataluyst Florfenicol of photoelectrocatalysis according to claim 2,
It is characterized in that, electrolyte is the dimethyl sulphoxide solution of hydrofluoric acid mass fraction 2% in the step (1).
4. a kind of preparation method of the catalyst of the quick dealuminated USY cataluyst Florfenicol of photoelectrocatalysis according to claim 2,
It is characterized in that, the preparatory coiled of titanium silk in the step (1), half small with acetone, ethyl alcohol, deionized water ultrasound respectively
When, it is then placed in drying box dry.
5. a kind of preparation method of the catalyst of the quick dealuminated USY cataluyst Florfenicol of photoelectrocatalysis according to claim 2,
It is characterized in that, the forbidden bandwidth Eg of anatase is 3.2eV in the step (2).
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Citations (6)
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CN101591001A (en) * | 2009-06-29 | 2009-12-02 | 西北有色金属研究院 | A kind of Pd doped Ti O 2The preparation method of nanotube array composite material |
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CN102703942A (en) * | 2012-06-20 | 2012-10-03 | 北京工业大学 | Method for preparing nano-platinum/palladium titanium dioxide nanotube composite electrode by pulse electrodeposition |
CN103165908A (en) * | 2011-12-14 | 2013-06-19 | 中国科学院大连化学物理研究所 | Preparation method of ordered electrode |
CN104492431A (en) * | 2014-12-10 | 2015-04-08 | 青岛农业大学 | Preparation method of Au-Pd/TiO2 NBs photocatalyst |
CN105951154A (en) * | 2016-04-27 | 2016-09-21 | 中国计量大学 | Anodic oxidation preparation method for titanium dioxide nanotube array photocatalyst for degrading rhodamine B |
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2018
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CN101591001A (en) * | 2009-06-29 | 2009-12-02 | 西北有色金属研究院 | A kind of Pd doped Ti O 2The preparation method of nanotube array composite material |
CN103165908A (en) * | 2011-12-14 | 2013-06-19 | 中国科学院大连化学物理研究所 | Preparation method of ordered electrode |
CN102658130A (en) * | 2012-04-20 | 2012-09-12 | 大连理工大学 | Preparation method of Ru-Pd bimetal-supported TiO2 nanotube photocatalyst and application thereof |
CN102703942A (en) * | 2012-06-20 | 2012-10-03 | 北京工业大学 | Method for preparing nano-platinum/palladium titanium dioxide nanotube composite electrode by pulse electrodeposition |
CN104492431A (en) * | 2014-12-10 | 2015-04-08 | 青岛农业大学 | Preparation method of Au-Pd/TiO2 NBs photocatalyst |
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