CN115672330A - Preparation method of bean dreg biochar loaded hydroxyl iron and hydroxyl cobalt catalyst - Google Patents
Preparation method of bean dreg biochar loaded hydroxyl iron and hydroxyl cobalt catalyst Download PDFInfo
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- CN115672330A CN115672330A CN202211398856.XA CN202211398856A CN115672330A CN 115672330 A CN115672330 A CN 115672330A CN 202211398856 A CN202211398856 A CN 202211398856A CN 115672330 A CN115672330 A CN 115672330A
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- SAXCKUIOAKKRAS-UHFFFAOYSA-N cobalt;hydrate Chemical compound O.[Co] SAXCKUIOAKKRAS-UHFFFAOYSA-N 0.000 title claims abstract description 28
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- HFZWRUODUSTPEG-UHFFFAOYSA-N 2,4-dichlorophenol Chemical compound OC1=CC=C(Cl)C=C1Cl HFZWRUODUSTPEG-UHFFFAOYSA-N 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- FHHJDRFHHWUPDG-UHFFFAOYSA-L peroxysulfate(2-) Chemical compound [O-]OS([O-])(=O)=O FHHJDRFHHWUPDG-UHFFFAOYSA-L 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 12
- 239000002351 wastewater Substances 0.000 claims description 10
- 230000000694 effects Effects 0.000 claims description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 9
- 239000010941 cobalt Substances 0.000 claims description 7
- 229910017052 cobalt Inorganic materials 0.000 claims description 7
- GFHNAMRJFCEERV-UHFFFAOYSA-L cobalt chloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Co+2] GFHNAMRJFCEERV-UHFFFAOYSA-L 0.000 claims description 7
- 229940044631 ferric chloride hexahydrate Drugs 0.000 claims description 7
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 229920000858 Cyclodextrin Polymers 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- HFHDHCJBZVLPGP-UHFFFAOYSA-N schardinger α-dextrin Chemical compound O1C(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(O)C2O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC2C(O)C(O)C1OC2CO HFHDHCJBZVLPGP-UHFFFAOYSA-N 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
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- 239000000843 powder Substances 0.000 claims description 5
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- 238000005406 washing Methods 0.000 claims description 5
- 230000032683 aging Effects 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- 239000003610 charcoal Substances 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 239000002244 precipitate Substances 0.000 claims description 3
- 230000001376 precipitating effect Effects 0.000 claims description 3
- 150000003254 radicals Chemical class 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 2
- 229940087654 iron carbonyl Drugs 0.000 claims 3
- 238000009777 vacuum freeze-drying Methods 0.000 claims 1
- 239000012425 OXONE® Substances 0.000 abstract description 5
- 238000002474 experimental method Methods 0.000 abstract description 3
- HJKYXKSLRZKNSI-UHFFFAOYSA-I pentapotassium;hydrogen sulfate;oxido sulfate;sulfuric acid Chemical compound [K+].[K+].[K+].[K+].[K+].OS([O-])(=O)=O.[O-]S([O-])(=O)=O.OS(=O)(=O)O[O-].OS(=O)(=O)O[O-] HJKYXKSLRZKNSI-UHFFFAOYSA-I 0.000 abstract description 3
- 239000007788 liquid Substances 0.000 abstract description 2
- OKBMCNHOEMXPTM-UHFFFAOYSA-M potassium peroxymonosulfate Chemical compound [K+].OOS([O-])(=O)=O OKBMCNHOEMXPTM-UHFFFAOYSA-M 0.000 abstract description 2
- 239000010865 sewage Substances 0.000 abstract description 2
- 238000006243 chemical reaction Methods 0.000 description 5
- 239000003344 environmental pollutant Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 231100000719 pollutant Toxicity 0.000 description 5
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 3
- VGVRPFIJEJYOFN-UHFFFAOYSA-N 2,3,4,6-tetrachlorophenol Chemical class OC1=C(Cl)C=C(Cl)C(Cl)=C1Cl VGVRPFIJEJYOFN-UHFFFAOYSA-N 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
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- 229910017061 Fe Co Inorganic materials 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention discloses a preparation method of a bean dreg biochar loaded hydroxyl iron and hydroxyl cobalt catalyst, belonging to the technical field of sewage treatment. The invention provides specific preparation steps of a preparation method of a bean dreg biochar-loaded hydroxyl iron and hydroxyl cobalt catalyst, and compared with the prior art, the preparation method can effectively catalyze potassium peroxymonosulfate to degrade 2, 4-dichlorophen in water. In experiments, the Co/Fe @ BC-2 catalyst has the most use value, and when the concentration of 2, 4-dichlorophen is 40mg/L, the solid-to-liquid ratio is 0.2g/L, the pH is =9, and the concentration of potassium monopersulfate is 200mg/L, the degradation rate of the 2, 4-dichlorophen in 20min is more than 94%.
Description
Technical Field
The invention belongs to the technical field of sewage treatment, and particularly relates to a preparation method of a bean dreg biochar loaded hydroxyl iron and hydroxyl cobalt catalyst.
Background
2, 4-dichlorophenol (2, 4-DCP) is one of typical chlorophenols, and has been widely used as an insecticide, herbicide, fungicide and preservative, and also as an intermediate for synthesizing pesticides, medicines and the like. 2,4-DCP has been identified as an endocrine disrupter, which can lead to tumors, birth defects and various developmental disorders. The chlorophenols pollutants in the water are difficult to remove from the environment, are easy to be enriched in organisms, and have strong carcinogenic, teratogenic and cytotoxic effects on aquatic organisms, crops and other organisms. 2,4-DCP is not easy to biodegrade in the environment, and can cause huge damage to organisms and the environment in extremely low concentration, and can also deteriorate the water body and easily cause serious threat to an ecological system.
The treatment method of the 2,4-DCP pollutants mainly comprises a biological method, an adsorption method, a chemical method and the like. The biological method is widely applied to the wastewater treatment process at present, but the CPs pollutants have biological toxicity and have an inhibiting effect on the growth and metabolism of microorganisms, so the removal effect of trace CPs in the water body is poor. The adsorption method mainly fixes the 2,4-DCP on the surface of the material, can not realize the degradation and complete mineralization of pollutants and is easy to cause secondary pollution.
The traditional chemical method is a main method for degrading CPs pollutants, but has strict requirements on reaction equipment. In addition, new methods for modifying catalysts have been sought in order to overcome the above disadvantages.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation method of a bean dreg biochar loaded hydroxyl iron and hydroxyl cobalt catalyst.
The purpose of the invention can be realized by the following technical scheme:
the preparation method of the bean dreg biochar loaded hydroxyl iron and hydroxyl cobalt catalyst comprises the following steps
Preparing bean dreg biochar;
(1) Heating bean dregs to 700-900 ℃ at a speed of 5-10 ℃/min, keeping for 1 hour under nitrogen flow, cooling, washing the obtained solid sample with ethanol for three times, centrifuging for 8000 rpm, rotating for 10 minutes, drying at 60 ℃, grinding into powder, sieving with a 100-mesh sieve to obtain bean dregs biochar with a particle size of 2-20 mu m, and collecting to obtain bean dregs biochar;
preparing a charcoal-loaded hydroxyl iron and hydroxyl cobalt catalyst;
(2) And adding deionized water into the biochar and the cyclodextrin in a mass ratio of 3 3+ And Co 2+ (ii) a Stirring for 10min, ultrasonically dispersing for 20min, adjusting pH to 8, stirring for 10min, ultrasonically dispersing for 10min, standing for 12-24h, aging and precipitating;
the precipitate was collected by centrifugation, washed three times with ethanol, then freeze-dried, ground into a powder, and passed through a 100 mesh sieve to collect the resulting catalyst.
The material dosage in the step (2) is preferably in the following proportion: 1g of biochar, 50mL of deionized water, 0.6g of cyclodextrin and Fe 3+ And Co 2+ Preferably 4;
fe described in step (2) 3+ And Co 2+ Preferably ferric chloride hexahydrate (FeCl) 3 ·6H 2 O) and cobalt chloride hexahydrate (CoCl) 2 ·6H 2 O)；
Adjusting the pH value, preferably selecting ammonia water in the step (2);
the hydroxyl iron and hydroxyl cobalt catalyst is obtained by adopting the preparation method of the bean dreg biochar loaded hydroxyl iron and hydroxyl cobalt catalyst.
The application of the bean dreg biochar-loaded hydroxyl iron and hydroxyl cobalt catalyst prepared by the method in the degradation treatment of 2, 4-dichlorophen in wastewater.
The application comprises the following steps: adding Co/Fe @ BC catalyst and Peroxymonosulfate (PMS) into 2, 4-dichlorophen wastewater, reacting to generate free radical molecules with an attack effect, and completing degradation treatment of 2, 4-dichlorophen in the wastewater.
The invention has the beneficial effects that:
the invention synthesizes an efficient catalyst which can effectively catalyze potassium peroxymonosulfate to degrade 2, 4-dichlorophen in water. In experiments, the Co/Fe @ BC-2 catalyst has the most use value, and when the concentration of 2, 4-dichlorophen is 40mg/L, the solid-to-liquid ratio is 0.2g/L, the pH is =9, and the concentration of potassium monopersulfate is 200mg/L, the degradation rate of 2, 4-dichlorophen in 20min reaches more than 94%.
Drawings
The invention will be further described with reference to the accompanying drawings.
FIG. 1 shows the effect of different Fe-Co ratio catalysts on PMS catalytic degradation of 2, 4-dichlorophen
FIG. 2 shows the effect of different PMS concentrations on Co/Fe @ BC-2 catalytic degradation of 2,4-dichlorophen
FIG. 3 is a graph showing the effect of different pH on the catalytic degradation of 2,4-dichlorophenol by Co/Fe @ BC-2
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a preparation method and application of a catalyst for loading hydroxyl iron and hydroxyl cobalt by using bean dreg biochar.
The preparation method of the bean dreg biochar loaded hydroxyl iron and hydroxyl cobalt catalyst comprises the following steps:
(1) Preparation of bean dreg biochar
Transferring a certain amount of bean dregs into a tubular furnace, heating to 700-900 ℃ at the speed of 5-10 ℃/min, and keeping for 1 hour under nitrogen flow;
cooling, washing the obtained solid sample with ethanol for three times, centrifuging (8000 rpm/min, 10 min), oven drying at 60 deg.C, grinding into powder, and sieving with 100 mesh sieve;
collecting the obtained bean dreg biochar, and storing the bean dreg biochar in a brown glass bottle for later use;
(2) Preparation of charcoal-loaded hydroxyl iron and hydroxyl cobalt catalyst
Adding 50mL of deionized water into 1g of biochar, adding 0.6g of cyclodextrin, and then adding Fe 3+ And Co 2+ ；
Stirring vigorously for 10min, ultrasonically dispersing for 20min, adjusting pH to 8, stirring vigorously for 10min, ultrasonically dispersing for 10min, standing for 12-24h, aging, and precipitating;
the precipitate was collected by centrifugation, washed three times with ethanol, then freeze-dried, ground in an agate mortar, and sieved through a 100 mesh screen.
Collecting the obtained oxidant, and storing the oxidant in a brown glass bottle until use;
the synthesized catalysts are named as Co/Fe @ BC, co/Fe @ BC-1, co/Fe @ BC-2, co/Fe @ BC-4 and Co/Fe @ BC-8 respectively.
The heating speed of the step (1) is preferably 5 ℃/min, and the temperature is heated to 800 ℃;
the washing in the step (1) is preferably carried out for 3 times by ethanol; the drying conditions are preferably 60 ℃; the grinding is preferably carried out by sieving with a 100-mesh sieve;
the material dosage in the step (2) is preferably in the following proportion: 1g of biochar, 50mL of deionized water, 0.6g of cyclodextrin and Fe 3+ And Co 2+ Preferably 4;
fe described in step (2) 3+ And Co 2+ Ferric chloride hexahydrate (FeCl) is preferred 3 ·6H 2 O) and cobalt chloride hexahydrate (CoCl) 2 ·6H 2 O)；
Adjusting the pH value, preferably selecting ammonia water in the step (2); the aging time is preferably 12h;
the hydroxyl iron and hydroxyl cobalt catalyst is obtained by adopting the preparation method of the bean dreg biochar loaded hydroxyl iron and hydroxyl cobalt catalyst.
The application of the bean dreg biochar-loaded hydroxyl iron and hydroxyl cobalt catalyst prepared by the method in the degradation treatment of 2, 4-dichlorophen in wastewater.
The application comprises the following steps: adding Co/Fe @ BC catalyst and Peroxymonosulfate (PMS) into 2, 4-dichlorophenol wastewater, reacting to generate free radical molecules with an attack effect, and completing degradation treatment of 2, 4-dichlorophenol in the wastewater.
The following experiment was carried out on the catalyst obtained in this example for the degradation of 2, 4-dichlorophenol by potassium monopersulfate:
1. degradation of 2, 4-dichlorophenol by different catalysts
According to the preparation method of Co/Fe @ BC, 1g of biochar is added with 50mL of deionized water, 0.6g of cyclodextrin is added, and ferric chloride hexahydrate (FeCl) with different molar ratios is added 3 ·6H 2 O) and cobalt chloride hexahydrate (CoCl) 2 ·6H 2 O) to carry different contents of Fe 3+ And Co 2+ . As can be seen from FIG. 1, within 20min, the degradation rates of Co/Fe @ BC, co/Fe @ BC-1, co/Fe @ BC-2 and Co/Fe @ BC-4 to 2, 4-dichlorophen were 1.79%, 64.78%, 75.90% and 76.99%, respectively, and the degradation rate of 2, 4-dichlorophen appeared to increase first and then to approach equilibrium with the increase of cobalt content. This indicates that as the cobalt concentration is increased to 2mmol/L, the iron and cobalt loading on the biochar surface has already become saturated, and increasing the cobalt concentration has not allowed it to be loaded onto the hydrated iron oxide, and thus the degradation rate of 2, 4-dichlorophen is no longer increased. The most preferred catalyst of the present invention is Co/Fe @ BC-2.
2. Effect of Permonosulfate (PMS) addition on degradation of 2, 4-dichlorophenol
As can be seen from FIG. 2, the degradation rate of 2, 4-dichlorophen was increased as the concentration of PMS was increased from 0mg/L to 250mg/L, showing a good positive correlation with the concentration of PMS. As the concentration of PMS in the reaction system was increased from 0mg/L to 200mg/L, the degradation rate of 2, 4-dichlorophenol was increased from 7.68% to 85.57%, but when the concentration of PMS was further increased to 250mg/L, the degradation rate of 2, 4-dichlorophenol was increased only to 88.09%, and the reaction rate was increased only slightly. Therefore, the concentration of PMS in the present invention is preferably 200mg/L.
3. Effect of initial pH on TC degradation
The initial pH of the solution plays an important role in the decomposition of PMS to produce sulfate radicals. As can be seen from FIG. 3, when the pH value is in the range of 3.0 to 9.0, the degradation rate of TC increases as the pH value of the solution increases. The degradation rate of 2, 4-dichlorophen increased from 80.64% to 94.22% as the pH in the reaction system increased from 3 to 9,2, 4-dichlorophen, but the reaction rate decreased greatly as the pH concentration was further increased to 11, the degradation rate of 2, 4-dichlorophen was 54.13%. This indicates that the present invention can provide better degradation of 2, 4-dichlorophenol over a wide pH range (5-9).
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing shows and describes the general principles, principal features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are given by way of illustration of the principles of the present invention, but that various changes and modifications may be made without departing from the spirit and scope of the invention, and such changes and modifications are within the scope of the invention as claimed.
Claims (7)
1. The preparation method of the bean dreg biochar loaded hydroxyl iron and hydroxyl cobalt catalyst is characterized by comprising the following steps of:
preparing bean dreg biochar:
heating bean dregs to 700-900 ℃ at a speed of 5-10 ℃/min, keeping for 1 hour under nitrogen flow, cooling, washing the obtained solid sample with ethanol for three times, centrifuging for 8000 rpm, rotating for 10 minutes, drying at 60 ℃, grinding into powder, sieving with a 100-mesh sieve to obtain bean dregs biochar with a particle size of 2-20 μm, and collecting to obtain bean dregs biochar;
preparing a charcoal-loaded hydroxyl iron and hydroxyl cobalt catalyst:
adding deionized water into the biochar and the cyclodextrin in a mass ratio of 3,then adding Fe 3+ And Co 2+ (ii) a Stirring for 10min, ultrasonic dispersing for 20min, adjusting the frequency to 40KHZ, adjusting pH to 8, stirring for 10min, ultrasonic dispersing for 10min, standing for 12-24h, aging, and precipitating;
centrifuging at 8000 rpm for 10min, collecting precipitate, washing with ethanol for three times, vacuum freeze drying at 0.01MPa and cold trap temperature of-60 deg.C, grinding into powder, sieving with 100 mesh sieve, and collecting the catalyst.
2. The preparation method of the bean dreg biochar-supported hydroxyl iron and hydroxyl cobalt catalyst as claimed in claim 1, wherein Fe in the preparation of the biochar-supported hydroxyl iron and hydroxyl cobalt catalyst 3+ And Co 2+ In a molar ratio of 4.
3. The method for preparing the bean dreg biochar-loaded hydroxyl iron and hydroxyl cobalt catalyst as claimed in claim 1, wherein ammonia water is selected for adjusting the pH in the preparation of the biochar-loaded hydroxyl iron and hydroxyl cobalt catalyst.
4. The method for preparing the bean dreg biological carbon-supported hydroxyl iron and hydroxyl cobalt catalyst as claimed in claim 1, wherein the Fe in the preparation of the biological carbon-supported hydroxyl iron and hydroxyl cobalt catalyst 3+ And Co 2+ Ferric chloride hexahydrate and cobalt chloride hexahydrate are used.
5. An iron carbonyl and cobalt carbonyl catalyst loaded on bean dregs biochar, which is characterized in that the iron carbonyl and cobalt carbonyl catalyst is prepared by the preparation method of the iron carbonyl and cobalt carbonyl catalyst loaded on bean dregs biochar according to any one of claims 1 to 4.
6. The application of the bean dreg biochar-supported hydroxyl iron and hydroxyl cobalt catalyst as claimed in claim 5 in degradation treatment of 2, 4-dichlorophen in wastewater.
7. The bean dreg biochar-supported hydroxyl iron and hydroxyl cobalt catalyst as claimed in claim 6, wherein the application in the degradation treatment of 2, 4-dichlorophenol in wastewater specifically comprises the following steps: adding the bean dreg biochar loaded hydroxyl iron and hydroxyl cobalt catalyst and peroxymonosulfate into the 2, 4-dichlorophen wastewater to react to generate free radical molecules with an attacking effect, and finishing degradation treatment of the 2, 4-dichlorophen in the wastewater.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107537566A (en) * | 2017-09-21 | 2018-01-05 | 山东大学 | Metal-doped cyclodextrin modified FeOOH material and its one-step method for synthesizing |
| US20190099743A1 (en) * | 2017-10-04 | 2019-04-04 | Board Of Supervisors Of Louisiana State University And Agricultural And Mechanical College | Catalyst Composition Including a Biochar, and Related Methods |
| CN113877558A (en) * | 2021-09-29 | 2022-01-04 | 湖南大学 | Ni-Fe hydrotalcite biochar composite catalyst and preparation method and application thereof |
| CN114425340A (en) * | 2021-12-15 | 2022-05-03 | 兰州理工大学 | Preparation of charcoal-modified cobalt-iron bimetallic composite catalyst and application of charcoal-modified cobalt-iron bimetallic composite catalyst in catalytic degradation of tetracycline |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107537566A (en) * | 2017-09-21 | 2018-01-05 | 山东大学 | Metal-doped cyclodextrin modified FeOOH material and its one-step method for synthesizing |
| US20190099743A1 (en) * | 2017-10-04 | 2019-04-04 | Board Of Supervisors Of Louisiana State University And Agricultural And Mechanical College | Catalyst Composition Including a Biochar, and Related Methods |
| CN113877558A (en) * | 2021-09-29 | 2022-01-04 | 湖南大学 | Ni-Fe hydrotalcite biochar composite catalyst and preparation method and application thereof |
| CN114425340A (en) * | 2021-12-15 | 2022-05-03 | 兰州理工大学 | Preparation of charcoal-modified cobalt-iron bimetallic composite catalyst and application of charcoal-modified cobalt-iron bimetallic composite catalyst in catalytic degradation of tetracycline |
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