CN109158118A - A kind of preparation method and applications for exempting from the tetracycline degradation photochemical catalyst that processing can repeatedly use - Google Patents
A kind of preparation method and applications for exempting from the tetracycline degradation photochemical catalyst that processing can repeatedly use Download PDFInfo
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- CN109158118A CN109158118A CN201810819760.3A CN201810819760A CN109158118A CN 109158118 A CN109158118 A CN 109158118A CN 201810819760 A CN201810819760 A CN 201810819760A CN 109158118 A CN109158118 A CN 109158118A
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- tetracycline
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- photochemical catalyst
- exempting
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- 239000004098 Tetracycline Substances 0.000 title claims abstract description 46
- 229960002180 tetracycline Drugs 0.000 title claims abstract description 46
- 229930101283 tetracycline Natural products 0.000 title claims abstract description 46
- 235000019364 tetracycline Nutrition 0.000 title claims abstract description 46
- 150000003522 tetracyclines Chemical class 0.000 title claims abstract description 46
- 239000003054 catalyst Substances 0.000 title claims abstract description 40
- 230000015556 catabolic process Effects 0.000 title claims abstract description 26
- 238000006731 degradation reaction Methods 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 31
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- 239000000463 material Substances 0.000 claims abstract description 10
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims abstract description 8
- 239000007787 solid Substances 0.000 claims abstract description 6
- 235000019441 ethanol Nutrition 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 18
- 230000003197 catalytic effect Effects 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 14
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 7
- 239000008103 glucose Substances 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000002604 ultrasonography Methods 0.000 claims description 6
- 239000002351 wastewater Substances 0.000 claims description 4
- 238000011282 treatment Methods 0.000 abstract description 15
- 230000008929 regeneration Effects 0.000 abstract description 9
- 238000011069 regeneration method Methods 0.000 abstract description 9
- 238000000926 separation method Methods 0.000 abstract description 6
- 238000004108 freeze drying Methods 0.000 abstract 1
- 238000001027 hydrothermal synthesis Methods 0.000 abstract 1
- 238000002156 mixing Methods 0.000 abstract 1
- 230000000593 degrading effect Effects 0.000 description 8
- 238000011067 equilibration Methods 0.000 description 8
- 230000003115 biocidal effect Effects 0.000 description 7
- 239000011941 photocatalyst Substances 0.000 description 7
- 238000006555 catalytic reaction Methods 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 229910021389 graphene Inorganic materials 0.000 description 4
- 238000005286 illumination Methods 0.000 description 4
- 239000002131 composite material Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
- 241000894006 Bacteria Species 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 239000003242 anti bacterial agent Substances 0.000 description 2
- 229940088710 antibiotic agent Drugs 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 229910002905 Bi4V2O11 Inorganic materials 0.000 description 1
- 206010059866 Drug resistance Diseases 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 210000003608 fece Anatomy 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- 230000037323 metabolic rate Effects 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 229940126572 wide-spectrum antibiotic Drugs 0.000 description 1
Classifications
-
- 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/14—Phosphorus; Compounds thereof
- B01J27/186—Phosphorus; Compounds thereof with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
-
- B01J35/39—
-
- 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
-
- 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
- C02F2101/34—Organic compounds containing oxygen
-
- 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
- C02F2101/38—Organic compounds containing nitrogen
-
- 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
Abstract
The invention discloses a kind of preparation method and applications for exempting from the tetracycline degradation photochemical catalyst that processing can repeatedly use, preparation method is: by GO, Bi (NO3)3, CTAB be dispersed or dissolved in positive six alcohol respectively, after then mixing three solution sufficiently, be transferred to reaction kettle and carry out hydro-thermal reaction.By solid separation, freeze-drying after reaction, product is obtained.Products obtained therefrom shows degradation property rapidly and efficiently to tetracycline, and can be not required to do any regeneration treatment and repeatedly use.The material preparation method is simple, low in cost, there is the potentiality of large-scale promotion application.
Description
Technical field
The present invention relates to it is a kind of exempt from processing can repeatedly use tetracycline degradation photochemical catalyst preparation method and its
Using belonging to pollutant control field.
Background technique
Antibiotic is made that huge tribute as one of greatest discovery of the twentieth century mankind, for clinical medical development
It offers, has saved the life of countless sufferers.However, at present abuse of antibiotics problem also than more prominent or even many antibiotic by with
In the growth (asian treatment dosage) for promoting animal.The metabolic rate of antibiotic in vivo is lower, it was found that there are about the anti-of 30-90%
Raw element is discharged with prototype by excreta.The phenomenon that abuse of antibiotics, results in many antibiotic to be discharged into environment.And
The antibiotic overwhelming majority for being discharged into environment finally can all enter water environment, therefore the influence to water environment is the most serious.Antibiotic
Harm maximum to environment is that bacterium can be caused to generate drug resistance, causes to generate the drug-fast bacteria to past medical help.Therefore, it reduces anti-
Raw element pollution is significant.
Photocatalysis technology is as a kind of green catalysis technology, and the application in terms of environmental contaminants improvement is increasingly by weight
Depending on.It has many advantages, such as that green, pollution-free, energy consumption is few using natural light as the driving force of catalysis.Tetracycline is a kind of wide spectrum
Antibiotic has been widely used for the disease treatment of people, animal, and annual usage amount is huge, residual in the environment also compared with
It is more, have become a threat for influencing Environmental security.There is researcher to start using photocatalyst for degrading tetracycline.But mesh
That when degrading tetracycline, there is also degradation times is long for preceding photochemical catalyst, reduces the lower problem of efficiency.As prepared by Yang Chen et al.
TiO2/ GO composite photo-catalyst, illumination 90min reach a kind of most degradation rate~65% [efficient degradation tetracycline to tetracycline
Composite photo-catalyst and the preparation method and application thereof, grant number ZL201510278124.0];Apply big east et al. preparation
Bi4V2O11/RGO photochemical catalyst, illumination 60min, reaching most degradation rate~70% to tetracycline, [a kind of hetero-junctions for preparing is multiple
The method of light combination catalyst, number of patent application 201711127019.2].In addition, when photochemical catalyst regenerates, it is often necessary to use H2O2
Or other reagents progress regeneration treatments could put into the Catalysis work [201711127019.2] of next round.These deficiencies all influence
Photochemical catalyst on a large scale promotes and applies in processing pollutant field.
Based on background above, this technology has invented a kind of tetracycline degradation photochemical catalyst exempting from processing and can repeatedly using
Preparation method and applications.The catalysis material BiOBr/rGO prepared using the method, the degradable tetracycline of illumination 20min
90% or more, illumination 130min or so basically reach catalytic equilibration, and degradable tetracycline 99% is shown quickly high to tetracycline
The degradation property of effect.In addition, used catalyst need to only be separated from the water body for reached catalytic equilibration, it is not required to be appointed
What regeneration treatment (including not needing to be rinsed with water) can put into the new waste water to be processed containing tetracycline and carry out next round
Catalysis work is at least reused 4 times, and catalytic activity is not substantially reduced.The catalyst, degradation tetracycline speed is fast, efficiency
It is high, to exempt from regeneration treatment, reusability good, can preferably solve some passes that current photocatalyst for degrading tetracycline is encountered
Key problem may advantageously facilitate the development of photocatalyst for degrading antibiotic.This technology correlation technique has not been reported.
Summary of the invention
The purpose of the present invention is to provide a kind of systems for exempting from the tetracycline degradation photochemical catalyst that processing can repeatedly use
Preparation Method and its application.
The present invention uses following means: a kind of preparation for exempting from the tetracycline degradation photochemical catalyst that processing can repeatedly use
Method and its application, it is characterised in that method and steps is as follows:
(1) positive six alcohol of 10mL is dispersed by the GO of 1.4mg-20mg, is solution A;
(2) by 0.6mmol Bi (NO3)3·5H2O is dissolved in positive six alcohol of 20mL, is B solution;
(3) 0.6mmolCTAB (cetyl trimethylammonium bromide) is dissolved in positive six alcohol of 20mL, is C solution;
(4) A, B, C solution are mixed and 0.1g-0.3g glucose and 5mL ethylene glycol is added after ten minutes, and ultrasound 30
Continue stirring 1 hour after minute.It is then transferred in reaction kettle, 180 DEG C are reacted 24 hours.It after reaction, is cooled to room temperature, will consolidate
Body is separated, and is alternately cleaned up with ethyl alcohol and deionized water, material is freeze-dried up to product.
(4) the product BiOBr/rGO composite photocatalyst material prepared by, visible light absorbing quickly and efficiently drop by photocatalysis
Tetracycline is solved, and after product reaches catalytic equilibration for photocatalytic degradation tetracycline, product is separated from processed water body, it can
It is without any processing and put into new need processing water body and carry out next round Catalysis work, it at least can so reuse 4 activity
Nothing is decreased obviously.
The present invention has the advantages that 1. can utilize Visible Light Induced Photocatalytic tetracycline, the time of degradation is short, high-efficient;2. when place
When reason waste water has reached catalytic equilibration, need to only come out the photocatalyst separation can be direct plungeed into the waste water of new need processing
It uses, does not need to do any regeneration treatment;3. the catalyst repeat performance is good, at least reusable 4 times and it is active
Nothing is decreased obviously;4. material preparation method is simple, low in cost, there are the potentiality of large-scale promotion application.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph of 1 product of the embodiment of the present invention.
Fig. 2 is the performance map of 1 product of embodiment of the present invention degradation tetracycline.
Fig. 3 is 1 product repeat performance figure of the embodiment of the present invention.
Specific embodiment
Embodiment 1
Graphene oxide GO is prepared by the improvement Hummers method routinely reported.
Positive six alcohol of 10mL is dispersed by 2mg GO, is set as solution A;By 0.6mmol Bi (NO3)3·5H2O is dissolved in 20mL
Positive six alcohol, is set as B solution;0.6mmolCTAB (cetyl trimethylammonium bromide) is dissolved in positive six alcohol of 20mL, it is molten to be set as C
Liquid;A, B, C solution are mixed, 0.1g glucose and 5mL ethylene glycol are added after ten minutes, and ultrasound continues to stir after 30 minutes
It mixes 1 hour.It is then transferred in reaction kettle, 180 DEG C are reacted 24 hours.It after reaction, is cooled to room temperature, solid is separated,
It is alternately cleaned up with ethyl alcohol and deionized water, material is freeze-dried up to product.
Above-mentioned catalyst prod is added in a clean beaker, 20mg/L tetracycline is then added, catalyst
Concentration is 1g/L, under visible light for tetracycline of degrading.When reaching catalytic equilibration, by catalyst by centrifuge separation, do not do
Any processing direct plunges into new 20mg/L tetracycline, carries out the catalytic degradation tetracycline of next round.Such circular treatment
4 times.
When repeating every time, catalyst direct plunges into the water for needing processing next time after separating in last processed water body
Body operation, catalyst do not do any regeneration treatment.
Embodiment 2
Graphene oxide GO is prepared by the improvement Hummers method routinely reported.
Positive six alcohol of 10mL is dispersed by 1.4mg GO, is set as solution A;By 0.6mmol Bi (NO3)3·5H2O is dissolved in
Positive six alcohol of 20mL, is set as B solution;0.6mmolCTAB (cetyl trimethylammonium bromide) is dissolved in positive six alcohol of 20mL, is set as
C solution;A, B, C solution are mixed, 0.1g glucose and 5mL ethylene glycol are added after ten minutes, and ultrasound continues after 30 minutes
Stirring 1 hour.It is then transferred in reaction kettle, 180 DEG C are reacted 24 hours.It after reaction, is cooled to room temperature, solid is isolated
Come, is alternately cleaned up with ethyl alcohol and deionized water, material is freeze-dried up to product.
Above-mentioned catalyst prod is added in a clean beaker, 20mg/L tetracycline is then added, catalyst
Concentration is 1g/L, under visible light for tetracycline of degrading.When reaching catalytic equilibration, by catalyst by centrifuge separation, do not do
Any processing direct plunges into new 20mg/L tetracycline, carries out the catalytic degradation tetracycline of next round.Such circular treatment
4 times.
When repeating every time, catalyst direct plunges into the water for needing processing next time after separating in last processed water body
Body operation, catalyst do not do any regeneration treatment.
Embodiment 3
Graphene oxide GO is prepared by the improvement Hummers method routinely reported.
Positive six alcohol of 10mL is dispersed by 2mg GO, is set as solution A;By 0.6mmol Bi (NO3)3·5H2O is dissolved in 20mL
Positive six alcohol, is set as B solution;0.6mmolCTAB (cetyl trimethylammonium bromide) is dissolved in positive six alcohol of 20mL, it is molten to be set as C
Liquid;A, B, C solution are mixed, 0.3g glucose and 5mL ethylene glycol are added after ten minutes, and ultrasound continues to stir after 30 minutes
It mixes 1 hour.It is then transferred in reaction kettle, 180 DEG C are reacted 24 hours.It after reaction, is cooled to room temperature, solid is separated,
It is alternately cleaned up with ethyl alcohol and deionized water, material is freeze-dried up to product.
Above-mentioned catalyst prod is added in a clean beaker, 20mg/L tetracycline is then added, catalyst
Concentration is 1g/L, under visible light for tetracycline of degrading.When reaching catalytic equilibration, by catalyst by centrifuge separation, do not do
Any processing direct plunges into new 20mg/L tetracycline, carries out the catalytic degradation tetracycline of next round.Such circular treatment
4 times.
When repeating every time, catalyst direct plunges into the water for needing processing next time after separating in last processed water body
Body operation, catalyst do not do any regeneration treatment.
Embodiment 4
Graphene oxide GO is prepared by the improvement Hummers method routinely reported.
Positive six alcohol of 10mL is dispersed by 20mg GO, is set as solution A;By 0.6mmol Bi (NO3)3·5H2O is dissolved in 20mL
Positive six alcohol, is set as B solution;06mmolCTAB (cetyl trimethylammonium bromide) is dissolved in positive six alcohol of 20mL, it is molten to be set as C
Liquid;A, B, C solution are mixed, 0.3g glucose and 5mL ethylene glycol are added after ten minutes, and ultrasound continues to stir after 30 minutes
It mixes 1 hour.It is then transferred in reaction kettle, 180 DEG C are reacted 24 hours.It after reaction, is cooled to room temperature, solid is separated,
It is alternately cleaned up with ethyl alcohol and deionized water, material is freeze-dried up to product.
Above-mentioned catalyst prod is added in a clean beaker, 20mg/L tetracycline is then added, catalyst
Concentration is 1g/L, under visible light for tetracycline of degrading.When reaching catalytic equilibration, by catalyst by centrifuge separation, do not do
Any processing direct plunges into new 20mg/L tetracycline, carries out the catalytic degradation tetracycline of next round.Such circular treatment
4 times.
When repeating every time, catalyst direct plunges into the water for needing processing next time after separating in last processed water body
Body operation, catalyst do not do any regeneration treatment.
Claims (4)
1. a kind of preparation method and applications for exempting from the tetracycline degradation photochemical catalyst that processing can repeatedly use, feature exist
In:
(1) positive six alcohol of 10mL is dispersed by GO, is set as solution A;
(2) by 0.6mmol Bi (NO3)3·5H2O is dissolved in positive six alcohol of 20mL, is set as B solution;
(3) 06mmol CTAB (cetyl trimethylammonium bromide) is dissolved in positive six alcohol of 20mL, is set as C solution;
(4) A, B, C solution are mixed and glucose and 5mL ethylene glycol is added after ten minutes, and ultrasound continues to stir after 30 minutes
It mixes 1 hour.It is then transferred in reaction kettle, 180 DEG C are reacted 24 hours.It after reaction, is cooled to room temperature, solid is separated,
It is alternately cleaned up with ethyl alcohol and deionized water, material is freeze-dried up to product.
2. a kind of preparation side for exempting from the tetracycline degradation photochemical catalyst that processing can repeatedly use according to claim 1
Method and its application, it is characterised in that: the amount of GO is 1.4mg-20mg in claim 1 step (1).
3. a kind of preparation side for exempting from the tetracycline degradation photochemical catalyst that processing can repeatedly use according to claim 1
Method and its application, it is characterised in that: the amount of claim 1 step (2) middle finger glucose is 0.1g-0.3g.
4. a kind of preparation side for exempting from the tetracycline degradation photochemical catalyst that processing can repeatedly use according to claim 1
Method and its application, it is characterised in that: the application of the tetracycline degradation photochemical catalyst is to carry out light to the waste water containing tetracycline
Catalytic degradation, and at least can so reuse 4 times.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN112642451A (en) * | 2021-01-22 | 2021-04-13 | 河南师范大学 | Photocatalytic material and preparation method and application thereof |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN112642451A (en) * | 2021-01-22 | 2021-04-13 | 河南师范大学 | Photocatalytic material and preparation method and application thereof |
CN112642451B (en) * | 2021-01-22 | 2023-09-15 | 河南师范大学 | Photocatalytic material and preparation method and application thereof |
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