CN109158118B - Preparation method of treatment-free tetracycline degradation photocatalyst capable of being repeatedly used - Google Patents
Preparation method of treatment-free tetracycline degradation photocatalyst capable of being repeatedly used Download PDFInfo
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- CN109158118B CN109158118B CN201810819760.3A CN201810819760A CN109158118B CN 109158118 B CN109158118 B CN 109158118B CN 201810819760 A CN201810819760 A CN 201810819760A CN 109158118 B CN109158118 B CN 109158118B
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- 239000004098 Tetracycline Substances 0.000 title claims abstract description 47
- 229960002180 tetracycline Drugs 0.000 title claims abstract description 47
- 229930101283 tetracycline Natural products 0.000 title claims abstract description 47
- 235000019364 tetracycline Nutrition 0.000 title claims abstract description 47
- 150000003522 tetracyclines Chemical class 0.000 title claims abstract description 47
- 230000015556 catabolic process Effects 0.000 title claims abstract description 28
- 238000006731 degradation reaction Methods 0.000 title claims abstract description 28
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims abstract description 13
- 239000000463 material Substances 0.000 claims abstract description 10
- 238000004108 freeze drying Methods 0.000 claims abstract description 7
- 239000007787 solid Substances 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract 2
- 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 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 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
- 238000003756 stirring Methods 0.000 claims description 7
- 238000004140 cleaning Methods 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 239000002351 wastewater Substances 0.000 claims description 4
- 238000013033 photocatalytic degradation reaction Methods 0.000 claims description 3
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 238000009210 therapy by ultrasound Methods 0.000 claims 1
- 230000008929 regeneration Effects 0.000 abstract description 9
- 238000011069 regeneration method Methods 0.000 abstract description 9
- IRHTZOCLLONTOC-UHFFFAOYSA-N hexacosan-1-ol Chemical compound CCCCCCCCCCCCCCCCCCCCCCCCCCO IRHTZOCLLONTOC-UHFFFAOYSA-N 0.000 abstract 2
- 238000001027 hydrothermal synthesis Methods 0.000 abstract 1
- 239000003054 catalyst Substances 0.000 description 24
- 230000003197 catalytic effect Effects 0.000 description 16
- 238000000034 method Methods 0.000 description 12
- 239000003242 anti bacterial agent Substances 0.000 description 8
- 229940088710 antibiotic agent Drugs 0.000 description 8
- 238000000527 sonication Methods 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 230000003115 biocidal effect Effects 0.000 description 4
- 239000002131 composite material Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 229910021389 graphene Inorganic materials 0.000 description 4
- ZSIAUFGUXNUGDI-UHFFFAOYSA-N hexan-1-ol Chemical compound CCCCCCO ZSIAUFGUXNUGDI-UHFFFAOYSA-N 0.000 description 4
- 239000003814 drug Substances 0.000 description 3
- 239000003344 environmental pollutant Substances 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
- 241000894006 Bacteria Species 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 230000000593 degrading effect Effects 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005286 illumination 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
- 241001465754 Metazoa Species 0.000 description 1
- 238000013475 authorization Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 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
- 230000007613 environmental effect Effects 0.000 description 1
- 210000003608 fece Anatomy 0.000 description 1
- 244000144972 livestock Species 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000011287 therapeutic dose Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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Classifications
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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
- 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 preparation method of a treatment-free tetracycline degradation photocatalyst capable of being repeatedly used, which comprises the following steps: mixing GO and Bi (NO)3)3And CTAB is respectively dispersed or dissolved in the hexacosanol, and then the three solutions are fully mixed and transferred into a reaction kettle for hydrothermal reaction. And (4) separating the solid after the reaction is finished, and freeze-drying to obtain the product. The obtained product shows rapid and efficient degradation performance to tetracycline, and can be repeatedly used for many times without any regeneration treatment. The material has the advantages of simple preparation method, low cost and large-scale popularization and application potential.
Description
Technical Field
The invention relates to a preparation method of a treatment-free tetracycline degradation photocatalyst capable of being repeatedly used, belonging to the field of pollutant treatment.
Background
As one of the greatest discoveries of the human in the twentieth century, the antibiotics make a great contribution to the development of clinical medicine and save lives of countless patients. However, the problem of abuse of antibiotics is now prominent, and even many antibiotics are used to promote growth in animals (sub-therapeutic doses). The metabolism rate of antibiotics in the body is low, and it has been studied that about 30-90% of antibiotics are excreted through excreta in the prototype. The phenomenon of antibiotic abuse has led to the discharge of a large number of antibiotics into the environment. Most of the antibiotics discharged into the environment finally enter the water environment, so the influence on the water environment is the most serious. The biggest harm of antibiotics to the environment is that bacteria can generate drug resistance, so that drug-resistant bacteria which can not be cured by drugs are generated. Therefore, the method has great significance for reducing antibiotic pollution.
The application of the photocatalysis technology in the aspect of environmental pollutant treatment is more and more emphasized as a green catalysis technology. It uses natural light as the driving force of catalysis, and has the advantages of green, no pollution, less energy consumption, etc. Tetracycline is a broad-spectrum antibiotic, has been widely used for treating diseases of human and livestock, is used in huge amount every year, has more residues in the environment, and has become a threat influencing the environmental safety. Researchers have begun to use photocatalysts to degrade tetracycline. However, the existing photocatalyst has the problems of long degradation time and low degradation efficiency when degrading tetracycline. TiO made by Yanhen et al2The light irradiation of the/GO composite photocatalyst is 90min, and the maximum degradation rate of tetracycline is 65% [ a composite photocatalyst for efficiently degrading tetracycline, and a preparation method and application thereof, wherein the authorization number is ZL 201510278124.0](ii) a The Bi4V2O11/RGO photocatalyst prepared by Shiweidong et al is irradiated by light for 60min, and the maximum degradation rate of tetracycline is up to 70% [ a method for preparing a heterojunction composite photocatalyst, and patent application No. 201711127019.2 ]]. In addition, when the photocatalyst is regenerated, H is often used2O2Or other reagents for regeneration before the next round of catalytic operation [ 201711127019.2]. These shortcomings all affect the large-scale popularization and application of the photocatalyst in the field of pollutant treatment.
Based on the background, the technology discloses a preparation method of a tetracycline degradation photocatalyst which is free of treatment and can be repeatedly used. The photocatalytic material BiOBr/rGO prepared by the method can degrade tetracycline by more than 90% in 20min under illumination, basically achieve catalytic balance in about 130min under illumination, can degrade tetracycline by 99%, and shows rapid and efficient degradation performance to tetracycline. In addition, the used catalyst only needs to be separated from the water body which achieves catalytic equilibrium, and does not need any regeneration treatment (including no need of washing with water), and new tetracycline-containing wastewater to be treated can be put into the next round of catalytic operation, and the catalyst can be reused for at least 4 times without obviously reducing the catalytic activity. The catalyst has the advantages of high tetracycline degradation speed, high efficiency, no regeneration treatment and good reusability, can better solve some key problems encountered by the prior photocatalyst in tetracycline degradation, and is beneficial to promoting the development of photocatalyst in antibiotic degradation. The related method of the technology is not reported.
Disclosure of Invention
The invention aims to provide a preparation method of a tetracycline degradation photocatalyst which is free from treatment and can be repeatedly used.
The invention adopts the following means: a preparation method of a tetracycline degradation photocatalyst which is free of treatment and can be repeatedly used is characterized by comprising the following steps:
(1) dispersing 1.4-20 mg of GO in 10mL of n-hexaol to obtain a solution A;
(2) 0.6mmol of Bi (NO)3)3·5H2Dissolving O in 20mL of n-hexaol to obtain a solution B;
(3) dissolving 0.6mmol CTAB (cetyl trimethyl ammonium bromide) in 20mL of n-hexaol to obtain a C solution;
(4) the A, B, C solution was mixed and stirred for 10 minutes, then 0.1 g-0.3 g glucose and 5mL ethylene glycol were added, and stirring was continued for 1 hour after 30 minutes of sonication. Then transferred to a reaction kettle and reacted at 180 ℃ for 24 hours. After reaction, cooling to room temperature, separating out solids, alternately cleaning with ethanol and deionized water, and freeze-drying the material to obtain the product.
(4) The prepared BiOBr/rGO composite photocatalytic material can absorb visible light to carry out photocatalytic degradation on tetracycline rapidly and efficiently, and after the product is used for carrying out photocatalytic degradation on tetracycline to reach catalytic balance, the product is separated from treated water, and can be put into new water needing to be treated to carry out next round of catalytic operation without any treatment, and the product can be reused at least for 4 times without obvious reduction of activity.
The invention has the advantages that: 1. the tetracycline can be degraded by visible light, the degradation time is short, and the efficiency is high; 2. when the treated wastewater reaches catalytic equilibrium, the photocatalyst is separated out and can be directly put into new wastewater to be treated without any regeneration treatment; 3. the catalyst has good reusability, can be reused for at least 4 times without obvious reduction of activity; 4. the material preparation method is simple, the cost is low, and the potential of large-scale popularization and application is realized.
Drawings
FIG. 1 is a scanning electron micrograph of a product of example 1 of the present invention.
FIG. 2 is a graph showing the tetracycline degradation performance of the product of example 1 of the present invention.
FIG. 3 is a graph of the reuse performance of the product of example 1 of the present invention.
Detailed Description
Example 1
Graphene oxide GO was prepared by a conventionally reported modified Hummers method.
Dispersing 2 mg GO in 10mL of n-hexaol to obtain solution A; 0.6mmol of Bi (NO)3)3·5H2Dissolving O in 20mL of n-hexaol to obtain a solution B; dissolving 0.6mmol CTAB (cetyl trimethyl ammonium bromide) in 20mL of n-hexanol to obtain solution C; the A, B, C solution was mixed and stirred for 10 minutes, then 0.1 g glucose and 5mL ethylene glycol were added, and stirring was continued for 1 hour after 30 minutes of sonication. Then transferred to a reaction kettle and reacted at 180 ℃ for 24 hours. After reaction, cooling to room temperature, separating out solids, alternately cleaning with ethanol and deionized water, and freeze-drying the material to obtain the product.
The catalyst product was added to a clean beaker, followed by 20 mg/L tetracycline solution, 1g/L catalyst concentration, and used to degrade tetracycline in visible light. When the catalytic equilibrium is reached, the catalyst is centrifugally separated without any treatment, and a new 20 mg/L tetracycline solution is directly added for the next round of catalytic degradation of tetracycline. The treatment is circulated for 4 times.
When the process is repeated every time, the catalyst is separated from the water body treated last time and then directly put into the water body to be treated next time, and the catalyst is not subjected to any regeneration treatment.
Example 2
Graphene oxide GO was prepared by a conventionally reported modified Hummers method.
Dispersing 1.4 mg GO in 10mL of n-hexaol to obtain solution A; 0.6mmol of Bi (NO)3)3·5H2Dissolving O in 20mL of n-hexaol to obtain a solution B; dissolving 0.6mmol CTAB (cetyl trimethyl ammonium bromide) in 20mL of n-hexanol to obtain solution C; the A, B, C solution was mixed and stirred for 10 minutes, then 0.1 g glucose and 5mL ethylene glycol were added, and stirring was continued for 1 hour after 30 minutes of sonication. Then transferred to a reaction kettle and reacted at 180 ℃ for 24 hours. After reaction, cooling to room temperature, separating out solids, alternately cleaning with ethanol and deionized water, and freeze-drying the material to obtain the product.
The catalyst product was added to a clean beaker, followed by 20 mg/L tetracycline solution, 1g/L catalyst concentration, and used to degrade tetracycline in visible light. When the catalytic equilibrium is reached, the catalyst is centrifugally separated without any treatment, and a new 20 mg/L tetracycline solution is directly added for the next round of catalytic degradation of tetracycline. The treatment is circulated for 4 times.
When the process is repeated every time, the catalyst is separated from the water body treated last time and then directly put into the water body to be treated next time, and the catalyst is not subjected to any regeneration treatment.
Example 3
Graphene oxide GO was prepared by a conventionally reported modified Hummers method.
Dispersing 2 mg GO in 10mL of n-hexaol to obtain solution A; 0.6mmol of Bi (NO)3)3·5H2Dissolving O in 20mL of n-hexaol to obtain a solution B; dissolving 0.6mmol CTAB (hexadecyl trimethyl ammonium bromide)Dissolving in 20mL of n-hexaol to obtain a solution C; the A, B, C solution was mixed and stirred for 10 minutes, then 0.3 g glucose and 5mL ethylene glycol were added, and stirring was continued for 1 hour after 30 minutes of sonication. Then transferred to a reaction kettle and reacted at 180 ℃ for 24 hours. After reaction, cooling to room temperature, separating out solids, alternately cleaning with ethanol and deionized water, and freeze-drying the material to obtain the product.
The catalyst product was added to a clean beaker, followed by 20 mg/L tetracycline solution, 1g/L catalyst concentration, and used to degrade tetracycline in visible light. When the catalytic equilibrium is reached, the catalyst is centrifugally separated without any treatment, and a new 20 mg/L tetracycline solution is directly added for the next round of catalytic degradation of tetracycline. The treatment is circulated for 4 times.
When the process is repeated every time, the catalyst is separated from the water body treated last time and then directly put into the water body to be treated next time, and the catalyst is not subjected to any regeneration treatment.
Example 4
Graphene oxide GO was prepared by a conventionally reported modified Hummers method.
Dispersing 20 mg GO in 10mL of n-hexaol to obtain solution A; 0.6mmol of Bi (NO)3)3·5H2Dissolving O in 20mL of n-hexaol to obtain a solution B; dissolving 06mmol CTAB (cetyl trimethyl ammonium bromide) in 20mL of n-hexaol to obtain solution C; the A, B, C solution was mixed and stirred for 10 minutes, then 0.3 g glucose and 5mL ethylene glycol were added, and stirring was continued for 1 hour after 30 minutes of sonication. Then transferred to a reaction kettle and reacted at 180 ℃ for 24 hours. After reaction, cooling to room temperature, separating out solids, alternately cleaning with ethanol and deionized water, and freeze-drying the material to obtain the product.
The catalyst product was added to a clean beaker, followed by 20 mg/L tetracycline solution, 1g/L catalyst concentration, and used to degrade tetracycline in visible light. When the catalytic equilibrium is reached, the catalyst is centrifugally separated without any treatment, and a new 20 mg/L tetracycline solution is directly added for the next round of catalytic degradation of tetracycline. The treatment is circulated for 4 times.
When the process is repeated every time, the catalyst is separated from the water body treated last time and then directly put into the water body to be treated next time, and the catalyst is not subjected to any regeneration treatment.
Claims (4)
1. A preparation method of a tetracycline degradation photocatalyst which is free of treatment and can be repeatedly used is characterized in that:
(1) dispersing GO in 10mL of orthohexaol to obtain solution A;
(2) 0.6mmol of Bi (NO)3)3·5H2Dissolving O in 20mL of n-hexaol to obtain a solution B;
(3) dissolving 06mmol CTAB (hexadecyl trimethyl ammonium bromide) in 20mL of n-hexaol to obtain a solution C;
(4) mixing and stirring the A, B, C solution for 10 minutes, adding glucose and 5mL of glycol, performing ultrasonic treatment for 30 minutes, and continuing stirring for 1 hour; then transferring the mixture into a reaction kettle, and reacting for 24 hours at 180 ℃; after reaction, cooling to room temperature, separating out solids, alternately cleaning with ethanol and deionized water, and freeze-drying the material to obtain the product.
2. The preparation method of the tetracycline degradation photocatalyst which is disposable and can be repeatedly used according to claim 1, wherein the preparation method comprises the following steps: the amount of GO in the step (1) is 1.4-20 mg.
3. The preparation method of the tetracycline degradation photocatalyst which is disposable and can be repeatedly used according to claim 1, wherein the preparation method comprises the following steps: in the step (2), the amount of the glucose is 0.1 g-0.3 g.
4. The preparation method of the tetracycline degradation photocatalyst which is disposable and can be repeatedly used according to claim 1, wherein the preparation method comprises the following steps: the application of the tetracycline degradation photocatalyst is to carry out rapid and efficient photocatalytic degradation on the tetracycline-containing wastewater, and the tetracycline degradation photocatalyst can be repeatedly used for at least 4 times.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102698775A (en) * | 2012-06-13 | 2012-10-03 | 上海大学 | BiOI-graphene visible light catalyst and preparation method thereof |
| CN104353472A (en) * | 2014-11-26 | 2015-02-18 | 安徽工业大学 | Preparation method of BiOBr/RGO nanometer composite and application thereof in reaction of degrading rhodamine |
| CN105562040A (en) * | 2016-01-11 | 2016-05-11 | 安徽工业大学 | Preparation and application of BiOCl-(001)/GO nano-composite photocatalyst |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104841461A (en) * | 2015-05-25 | 2015-08-19 | 中南民族大学 | Preparation method and application of novel hexagonal-prism BiOCl nanometer photocatalytic materials |
| CN107159274A (en) * | 2017-04-27 | 2017-09-15 | 武汉纺织大学 | The preparation method and obtained photochemical catalyst of a kind of BiOCl photochemical catalysts and its application |
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|---|---|---|---|---|
| CN102698775A (en) * | 2012-06-13 | 2012-10-03 | 上海大学 | BiOI-graphene visible light catalyst and preparation method thereof |
| CN104353472A (en) * | 2014-11-26 | 2015-02-18 | 安徽工业大学 | Preparation method of BiOBr/RGO nanometer composite and application thereof in reaction of degrading rhodamine |
| CN105562040A (en) * | 2016-01-11 | 2016-05-11 | 安徽工业大学 | Preparation and application of BiOCl-(001)/GO nano-composite photocatalyst |
Non-Patent Citations (2)
| Title |
|---|
| BiOBr/BiOI-FACs光催化降解四环素的动力学研究;林立等;《硅酸盐通报》;20160531;第35卷(第5期);第1551页第2段 * |
| Reduced graphene oxide as co-catalyst for enhanced visible light photocatalytic activity of BiOBr;Tingting Jiang et al.;《Ceramics International》;20160614;第42卷;摘要、第2.1部分、第16466页右栏倒数第1段 * |
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