CN112619701B - Method for preparing dye-boron nitride composite photocatalytic material and application - Google Patents
Method for preparing dye-boron nitride composite photocatalytic material and application Download PDFInfo
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- 229910052582 BN Inorganic materials 0.000 title claims abstract description 103
- 239000000463 material Substances 0.000 title claims abstract description 53
- 239000002131 composite material Substances 0.000 title claims abstract description 50
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 50
- 238000000034 method Methods 0.000 title claims abstract description 18
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000002351 wastewater Substances 0.000 claims abstract description 35
- 239000002957 persistent organic pollutant Substances 0.000 claims abstract description 6
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical group [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 claims description 40
- 239000004098 Tetracycline Substances 0.000 claims description 30
- 229960002180 tetracycline Drugs 0.000 claims description 30
- 229930101283 tetracycline Natural products 0.000 claims description 30
- 235000019364 tetracycline Nutrition 0.000 claims description 30
- 150000003522 tetracyclines Chemical class 0.000 claims description 30
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 claims description 28
- 238000001035 drying Methods 0.000 claims description 17
- 238000005406 washing Methods 0.000 claims description 14
- 229940043267 rhodamine b Drugs 0.000 claims description 13
- 229960000907 methylthioninium chloride Drugs 0.000 claims description 11
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 10
- 239000004202 carbamide Substances 0.000 claims description 10
- 238000000227 grinding Methods 0.000 claims description 10
- 238000005303 weighing Methods 0.000 claims description 10
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 claims description 9
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 claims description 9
- 239000000843 powder Substances 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
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- 239000000975 dye Substances 0.000 description 44
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- 230000000593 degrading effect Effects 0.000 description 12
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- 238000001782 photodegradation Methods 0.000 description 6
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- 238000001816 cooling Methods 0.000 description 4
- 230000007547 defect Effects 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
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- 238000006731 degradation reaction Methods 0.000 description 3
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- 238000004064 recycling Methods 0.000 description 3
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- 238000002360 preparation method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000004065 wastewater treatment Methods 0.000 description 2
- 239000003463 adsorbent Substances 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000004042 decolorization Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 239000010919 dye waste Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
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- 238000001914 filtration Methods 0.000 description 1
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- 231100000719 pollutant Toxicity 0.000 description 1
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- 238000011084 recovery Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/0234—Nitrogen-, phosphorus-, arsenic- or antimony-containing compounds
- B01J31/0271—Nitrogen-, phosphorus-, arsenic- or antimony-containing compounds also containing elements or functional groups covered by B01J31/0201 - B01J31/0231
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- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
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- B01J31/0234—Nitrogen-, phosphorus-, arsenic- or antimony-containing compounds
- B01J31/0235—Nitrogen containing compounds
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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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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
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- 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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
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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
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Abstract
The invention discloses a method for preparing a dye-boron nitride composite photocatalytic material and application thereof, which prepares dye wastewater and boron nitride, and finally prepares a dye-boron nitride compound by adsorbing the dye wastewater with the boron nitride; the prepared dye-boron nitride composite photocatalytic material can adsorb and reduce visible light to remove other organic pollutants except dye, save the treatment cost of dye wastewater and realize the resource utilization of the dye wastewater.
Description
Technical Field
The invention relates to a method for preparing a dye-boron nitride composite photocatalytic material and application thereof, belonging to the technical field of wastewater treatment.
Background
With the rapid development of economy, the discharge amount of industrial wastewater increases year by year. Statistically, about 160 million tons of dye are produced worldwide each year, with about 1/8 being used in the commercial dye industry. China is a large dye producing country, and the total dye yield exceeds 100 million tons in 2018. The dye wastewater is an important component of industrial wastewater and accounts for about 10 percent of the total amount of industrial wastewater.
The commonly used dye wastewater treatment methods mainly include adsorption, chemical oxidation and biological methods. The adsorption method has the characteristics of simple operation, obvious decolorization effect and small occupied area, and also has the defects of difficult adsorption regeneration, serious membrane pollution and high cost. The chemical method has the advantages of good treatment effect and high decoloring efficiency, but also has the defects of high energy consumption, high cost, high operating cost and the like. The biological method has the advantages of low operation cost, high efficiency, simple operation of process equipment, no secondary pollution and the like, but also has the defects of more limiting factors, low decoloring efficiency, inhibition of microbial growth by dye and the like. In summary, the conventional treatment methods for dye wastewater all have the problems of high cost, high operation cost and the like. But the dye is also a resource, and is necessary to carry out resource treatment on the dye wastewater.
At present, the recovery method of dye wastewater mainly comprises adsorbent desorption and membrane treatment. For example, chinese patent application No. cn201810288666.x discloses a method for recovering residual dye by filtering dye wastewater and recycling the residual dye by a recycling process. At present, the key point of dye wastewater resource is to recycle dyes, but the subsequent reuse of the dyes is lacked.
Through search, relevant patents and published documents for realizing the recycling of dye wastewater in the form of a dye-boron nitride composite photocatalytic material are not found.
Disclosure of Invention
The invention aims to overcome the defects in the prior art, provides a method for preparing a dye-boron nitride composite photocatalytic material and application thereof, and realizes resource utilization of dye wastewater.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the invention provides a method for preparing a dye-boron nitride composite photocatalytic material, which comprises the following steps:
preparing dye wastewater: adding a dye into water to prepare dye wastewater with the concentration of 20-100 mg/L;
preparing boron nitride: according to the mass ratio of 2: 1, weighing urea and diboron trioxide, uniformly mixing, reacting at the constant temperature of 1100 ℃ for 3-5 h to prepare a boron nitride powder material, washing, drying and grinding to obtain a powder boron nitride sample;
preparation of dye-boron nitride compound: weighing and mixing dye wastewater and a powder boron nitride sample; stirring at normal temperature and in the dark for at least 360 min, standing for at least 30 min, centrifuging, taking out the solid, and drying at 60-100 ℃ for 6-10 h to obtain the dye-boron nitride composite photocatalytic material.
Further, in the step of preparing the dye-boron nitride compound, the mass ratio of the dye to the boron nitride is 1: 1.5 weighing the dye wastewater and the powder boron nitride sample.
Further, the dye is rhodamine B and/or methylene blue.
Further, the dye-boron nitride composite photocatalytic material is rhodamine B-boron nitride, methylene blue-boron nitride or a rhodamine B-methylene blue-boron nitride compound.
The invention also provides an application of the dye-boron nitride composite photocatalytic material, and the prepared dye-boron nitride composite photocatalytic material can adsorb dye wastewater and degrade pollutants under visible light.
Further, the contaminant includes tetracycline.
Compared with the prior art, the invention has the following beneficial effects:
the method for preparing the dye-boron nitride composite photocatalytic material and the application thereof realize resource utilization of dye wastewater, and the process for preparing the dye-boron nitride composite photocatalytic material only needs stirring and adsorption at normal temperature, is easy to implement, simple to operate and easy to industrialize; the prepared dye-boron nitride composite photocatalytic material can adsorb organic pollutants, can degrade the organic pollutants under visible light, and saves the treatment cost of dye wastewater.
Drawings
FIG. 1 is a diffraction pattern of a boron nitride crystal in example 1 of the present invention;
FIG. 2 is a Fourier infrared spectrum of boron nitride in example 1 of the present invention;
FIG. 3 is a schematic diagram of the results of degrading tetracycline by the boron nitride and rhodamine B-boron nitride composite photocatalytic material in example 1 of the present invention under visible light;
FIG. 4 is a schematic diagram showing the results of degrading tetracycline by using the boron nitride and methylene blue-boron nitride composite photocatalytic material in example 2 of the present invention under visible light;
FIG. 5 is a schematic diagram of the results of degrading tetracycline by the boron nitride and rhodamine B-methylene blue-boron nitride composite photocatalytic material in example 3 of the present invention under visible light;
FIG. 6 is a schematic diagram of the result of cyclic degradation of tetracycline by the rhodamine B-boron nitride composite photocatalytic material in embodiment 4 of the present invention under visible light.
Detailed Description
The invention is further described below with reference to the accompanying drawings. The following examples are only for illustrating the technical solutions of the present invention more clearly, and the protection scope of the present invention is not limited thereby.
The following examples used dye waste water from a laboratory simulation setup.
Example 1:
a rhodamine B-boron nitride composite photocatalytic material is prepared by the following steps:
firstly, weighing 24 g of urea and 12 g of boron trioxide, wherein the mass ratio of the urea to the boron trioxide is 2: 1, grinding for half an hour to uniformly mix; putting the mixture into a muffle furnace, heating to 1100 ℃ at the speed of 10 ℃/min, reacting at constant temperature for 4 hours, and naturally cooling to room temperature; taking out and washing with hydrochloric acid for 5 times, and washing off unreacted diboron trioxide completely; putting the processed sample into a drying oven at 105 ℃ for drying for 12h, taking out, and grinding to be powdery to obtain a white powdery sample;
the crystal diffraction of the above sample was carried out, and the result is shown in fig. 1, which is a crystal diffraction pattern of boron nitride in example 1 of the present invention, and it can be seen that there are two peaks at 26.7oC and 42.5oC, which are characteristic peaks of boron nitride, which supports that the synthesized product is boron nitride.
As shown in FIG. 2, which is a Fourier infrared spectrum of boron nitride in example 1 of the present invention, the infrared peak at 779 cm-1 and the broad peak at 1377 cm-1 are attributed to bending vibration of B-N-B bond and tensile vibration of B-N bond, and the broad peak at 3195 cm-1 is assigned to tensile vibration of surface O-H bond, supporting that the synthesized product is surface hydroxylated boron nitride.
And (2) taking 20 mg of rhodamine B dye to prepare 20 mg/L rhodamine B solution, taking 30 mg of boron nitride prepared in the steps, taking 100 mL of rhodamine B dye wastewater, placing 30 mg of rhodamine B dye wastewater in the solution to be adsorbed for 6h to reach adsorption saturation to form a rhodamine B-boron nitride compound, standing for 30 min after adsorption is finished, performing centrifugal washing, and drying at 80 ℃ for 6h to obtain the rhodamine B-boron nitride composite photocatalytic material.
As shown in fig. 3, a schematic diagram of the result of degrading tetracycline by the boron nitride and rhodamine B-boron nitride composite photocatalytic material in example 1 of the present invention under visible light is shown. Degrading 20 mg/L tetracycline under visible light by using the rhodamine B-boron nitride composite photocatalytic material obtained by drying, wherein after 4 hours, 72.91% of tetracycline is degraded, and compared with the single boron nitride, the removing efficiency of the single boron nitride to the tetracycline under the visible light is 25.81%, and the degrading efficiency of the rhodamine B-boron nitride composite photocatalytic material to the tetracycline under the visible light is improved by 47.1%.
Example 2:
a methylene blue-boron nitride composite photocatalytic material is prepared by the following steps:
weighing 24 g of urea and 12 g of boron trioxide, wherein the mass ratio of the urea to the boron trioxide is 2: 1, grinding for half an hour to uniformly mix; putting the mixture into a muffle furnace, heating to 1100 ℃ at the speed of 10 ℃/min, reacting at constant temperature for 4 hours, and naturally cooling to room temperature; taking out and washing with hydrochloric acid for 5 times, and washing off unreacted diboron trioxide completely; putting the processed sample into a drying oven at 105 ℃ for drying for 12h, taking out, and grinding to be powdery to obtain a white powdery sample;
and (2) preparing 20 mg of methylene blue dye into 20 mg/L methylene blue solution, preparing 30 mg of boron nitride prepared in the step, preparing 100 mL of methylene blue dye wastewater, placing 30 mg of methylene blue dye wastewater in the solution to adsorb for 6 hours to reach adsorption saturation to form a methylene blue-boron nitride compound, standing for 30 minutes after adsorption is finished, washing by centrifugation, and drying at 80 ℃ for 10 hours to obtain the methylene blue-boron nitride compound photocatalytic material.
FIG. 4 is a schematic diagram showing the results of degrading tetracycline by the boron nitride and methylene blue-boron nitride composite photocatalytic material in example 2 of the present invention under visible light. The methylene blue-boron nitride composite photocatalytic material is degraded by 20 mg/L tetracycline under visible light, after 4 hours, 79.56% of tetracycline is degraded, and compared with the light degradation removal efficiency (25.81%) of single boron nitride to tetracycline under visible light, the light degradation efficiency of the methylene blue-boron nitride composite photocatalytic material to tetracycline under visible light is improved by 53.75%.
Example 3:
a rhodamine B-methylene blue-boron nitride composite photocatalytic material is prepared by the following steps:
weighing 24 g of urea and 12 g of boron trioxide, wherein the mass ratio of the urea to the boron trioxide is 2: 1, grinding for half an hour to uniformly mix; putting the mixture into a muffle furnace, heating to 1100 ℃ at the speed of 10 ℃/min, reacting at constant temperature for 4 hours, and naturally cooling to room temperature; taking out and washing with hydrochloric acid for 5 times, and washing off unreacted diboron trioxide completely; putting the processed sample into a drying oven at 105 ℃ for drying for 12h, taking out, and grinding to be powdery to obtain a white powdery sample;
and respectively taking 20 mg of rhodamine B dye as a 20 mg/L rhodamine B solution and 20 mg of methylene blue dye as a 20 mg/L methylene blue solution, taking 30 mg of boron nitride prepared in the steps, mixing 50 mL of rhodamine B and 50 mL of methylene blue dye wastewater respectively to form a rhodamine B-methylene blue mixed solution, placing 30 mg of rhodamine B-methylene blue mixed solution in the solution to adsorb for 6 hours to reach adsorption saturation to form a rhodamine B-methylene blue-boron nitride compound, standing for 30 minutes after adsorption is finished, washing by centrifugation, and drying for 6 hours at 100 ℃ to obtain the rhodamine B-methylene blue-boron nitride composite photocatalytic material.
As shown in fig. 5, a schematic diagram of the result of degrading tetracycline by the boron nitride and rhodamine B-methylene blue-boron nitride composite photocatalytic material in embodiment 3 of the present invention under visible light is shown. Degrading 20 mg/L tetracycline by the rhodamine B-methylene blue-boron nitride composite photocatalytic material under visible light, wherein 85.01% of tetracycline is degraded after 4 hours, and compared with the single boron nitride, the efficiency of removing the tetracycline by photodegradation under the visible light is 25.81%, and the efficiency of degrading the tetracycline by the rhodamine B-methylene blue-boron nitride composite photocatalytic material under the visible light is improved by 59.2%.
Example 4:
a rhodamine B-boron nitride composite photocatalytic material degrades tetracycline by circulating light under visible light:
weighing 24 g of urea and 12 g of boron trioxide, wherein the mass ratio of the urea to the boron trioxide is 2: 1, grinding for half an hour to uniformly mix; putting the mixture into a muffle furnace, heating to 1100 ℃ at the speed of 10 ℃/min, reacting at constant temperature for 4 hours, and naturally cooling to room temperature; taking out and washing with hydrochloric acid for 5 times, and washing off unreacted diboron trioxide completely; putting the processed sample into a drying oven at 105 ℃ for drying for 12h, taking out, and grinding to be powdery to obtain a white powdery sample;
respectively taking 20 mg of rhodamine B dye to prepare 20 mg/L rhodamine B solution, taking 30 mg of boron nitride prepared in the steps, taking 100 mL of rhodamine B dye wastewater, placing 30 mg of rhodamine B dye wastewater in the solution to be adsorbed for 6 hours to reach adsorption saturation to form a rhodamine B-boron nitride compound, standing for 30 minutes after adsorption is finished, carrying out centrifugal washing, and drying for 6 hours at 60 ℃ to obtain the rhodamine B-boron nitride compound photocatalytic material.
As shown in fig. 6, which is a schematic diagram of a result of degrading tetracycline cyclically by using rhodamine B-boron nitride composite photocatalytic material under visible light in embodiment 4 of the present invention, 35 mg of the rhodamine B-boron nitride composite photocatalytic material is used to degrade tetracycline under visible light, a photodegradation removal rate of tetracycline for the first time reaches 89%, a photodegradation removal rate of tetracycline for the second time reaches 87%, a photodegradation removal rate of tetracycline for the third time reaches 84%, and a photodegradation removal rate of tetracycline for the fourth time reaches 83%.
According to the invention, boron nitride is a good adsorption material, and the dye in the dye wastewater can be well adsorbed at normal temperature, so that the dye in the wastewater is adsorbed to the surface of the boron nitride, the dye wastewater is used as a precursor for the first time, the dye-boron nitride composite photocatalytic material is prepared, and the resource utilization of the dye wastewater is realized.
The preparation process of the dye-boron nitride compound only needs stirring and adsorption at normal temperature, and has simple operation flow and easy industrialization; the photodegradation efficiency of the prepared dye-boron nitride composite photocatalytic material to tetracycline under visible light is improved by about 50 percent relative to boron nitride without dye adsorption; the rhodamine B-boron nitride composite photocatalytic material can still keep 80% of removal efficiency after degrading tetracycline by circulating light for four times, and compared with boron nitride without adsorbing dye, the composite dye-boron nitride composite material can adsorb other organic pollutants, can degrade other organic pollutants under visible light, and effectively saves the treatment cost of dye wastewater.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, several modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.
Claims (5)
1. A method for preparing a dye-boron nitride composite photocatalytic material is characterized by comprising the following steps:
preparing dye wastewater: adding a dye into water to prepare dye wastewater with the concentration of 20-100 mg/L, wherein the dye is rhodamine B and/or methylene blue;
preparing boron nitride: according to the mass ratio of 2: 1, weighing urea and diboron trioxide, uniformly mixing, reacting at the constant temperature of 1100 ℃ for 3-5 h to prepare a boron nitride powder material, washing, drying and grinding to obtain a powder boron nitride sample;
preparing a dye-boron nitride composite photocatalytic material: weighing and mixing dye wastewater and a powder boron nitride sample; stirring under normal temperature and dark conditions, standing, centrifuging, taking out the solid, and drying at 60-100 ℃ for 6-10 h to obtain the dye-boron nitride composite photocatalytic material, wherein the dye-boron nitride composite photocatalytic material is rhodamine B-boron nitride, methylene blue-boron nitride or rhodamine B-methylene blue-boron nitride.
2. The method for preparing the dye-boron nitride composite photocatalytic material as claimed in claim 1, wherein the stirring is carried out for at least 360 min, and the standing is not less than 30 min.
3. The method for preparing the dye-boron nitride composite photocatalytic material according to claim 1, wherein in the step of preparing the dye-boron nitride composite photocatalytic material, the ratio of the dye to the boron nitride is 1: 1.5 weighing the dye wastewater and the powder boron nitride sample.
4. Use of the dye-boron nitride composite photocatalytic material prepared by the method according to any one of claims 1 to 3, wherein the dye-boron nitride composite photocatalytic material degrades organic pollutants under visible light.
5. The use of claim 4, wherein the organic contaminant comprises tetracycline.
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| US20150174567A1 (en) * | 2013-12-20 | 2015-06-25 | Massachusetts Institute Of Technology | Hybrid photocatalyst for wastewater remediation |
| CN104056590A (en) * | 2014-07-14 | 2014-09-24 | 江苏大学 | Few-layer boron nitride as well as preparation method and application thereof |
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