CN114042466A - Material for degrading organic pollutants in soil - Google Patents
Material for degrading organic pollutants in soil Download PDFInfo
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- CN114042466A CN114042466A CN202111347036.3A CN202111347036A CN114042466A CN 114042466 A CN114042466 A CN 114042466A CN 202111347036 A CN202111347036 A CN 202111347036A CN 114042466 A CN114042466 A CN 114042466A
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- 239000000463 material Substances 0.000 title claims abstract description 18
- 239000002689 soil Substances 0.000 title claims abstract description 18
- 239000002957 persistent organic pollutant Substances 0.000 title claims abstract description 15
- 230000000593 degrading effect Effects 0.000 title claims abstract description 11
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 12
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 150000001868 cobalt Chemical class 0.000 claims abstract description 9
- 239000008367 deionised water Substances 0.000 claims abstract description 9
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 9
- 150000002751 molybdenum Chemical class 0.000 claims abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000004327 boric acid Substances 0.000 claims abstract description 8
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 claims abstract description 8
- 239000011259 mixed solution Substances 0.000 claims abstract description 8
- 239000002245 particle Substances 0.000 claims abstract description 8
- 229910003145 α-Fe2O3 Inorganic materials 0.000 claims abstract description 8
- CDVAIHNNWWJFJW-UHFFFAOYSA-N 3,5-diethoxycarbonyl-1,4-dihydrocollidine Chemical compound CCOC(=O)C1=C(C)NC(C)=C(C(=O)OCC)C1C CDVAIHNNWWJFJW-UHFFFAOYSA-N 0.000 claims abstract description 7
- USFZMSVCRYTOJT-UHFFFAOYSA-N Ammonium acetate Chemical compound N.CC(O)=O USFZMSVCRYTOJT-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000005695 Ammonium acetate Substances 0.000 claims abstract description 7
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 7
- 235000019257 ammonium acetate Nutrition 0.000 claims abstract description 7
- 229940043376 ammonium acetate Drugs 0.000 claims abstract description 7
- 239000004202 carbamide Substances 0.000 claims abstract description 7
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 7
- 238000004729 solvothermal method Methods 0.000 claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims abstract description 6
- 229910018864 CoMoO4 Inorganic materials 0.000 claims abstract description 4
- 230000008569 process Effects 0.000 claims abstract description 4
- 238000005406 washing Methods 0.000 claims abstract description 4
- 238000006731 degradation reaction Methods 0.000 claims description 7
- 230000015556 catabolic process Effects 0.000 claims description 6
- 239000002131 composite material Substances 0.000 claims description 4
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 2
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 2
- WFLYOQCSIHENTM-UHFFFAOYSA-N molybdenum(4+) tetranitrate Chemical compound [N+](=O)([O-])[O-].[Mo+4].[N+](=O)([O-])[O-].[N+](=O)([O-])[O-].[N+](=O)([O-])[O-] WFLYOQCSIHENTM-UHFFFAOYSA-N 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 229910000859 α-Fe Inorganic materials 0.000 claims description 2
- 230000001699 photocatalysis Effects 0.000 abstract description 9
- 230000000694 effects Effects 0.000 abstract description 3
- 230000007547 defect Effects 0.000 abstract description 2
- 238000005516 engineering process Methods 0.000 description 6
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 4
- 238000005067 remediation Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000012855 volatile organic compound Substances 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 239000000575 pesticide Substances 0.000 description 2
- 239000011941 photocatalyst Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 230000004913 activation Effects 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 229940088710 antibiotic agent Drugs 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 230000004298 light response Effects 0.000 description 1
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 150000003071 polychlorinated biphenyls Chemical group 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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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
- B01J27/188—Phosphorus; Compounds thereof with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium with chromium, molybdenum, tungsten or polonium
- B01J27/19—Molybdenum
-
- 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
- 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
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/40—Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
- B01J35/51—Spheres
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09C—RECLAMATION OF CONTAMINATED SOIL
- B09C1/00—Reclamation of contaminated soil
- B09C1/08—Reclamation of contaminated soil chemically
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Soil Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Catalysts (AREA)
Abstract
The invention relates to a material for degrading soil organic pollutants, which is characterized by being prepared by the following process: dissolving cobalt salt, molybdenum salt, disodium hydrogen phosphate and boric acid in a certain proportion in a mixed solution of isopropanol and glycerol, transferring the mixed solution into a high-pressure reaction kettle, and carrying out solvothermal reaction at 180 ℃ and 200 ℃ to obtain spherical P, B co-doped CoMoO with the particle size of 300-4(ii) a CoMoO doping B, P4Washing with deionized water and ethanol alternately, dissolving in deionized water, sequentially adding ferric acetylacetonate, ammonium acetate and urea, and performing hydrothermal reaction at 180 ℃ and 200 ℃ to obtain spherical B, P co-doped CoMoO4Surface loading nano alpha-Fe2O3GranulesThe photocatalytic material has large specific surface area and high activity, and overcomes the defect of a single photocatalytic material.
Description
Technical Field
The application relates to the field of soil remediation, in particular to a composite material for degrading organic pollutants in soil.
Background
The soil photocatalytic degradation technology is a novel deep soil chemical remediation technology and is mainly used for the remediation process of soil with organic pollutants such as pesticides, antibiotics and the like. The photocatalytic degradation technology degrades Volatile Organic Compounds (VOCs) into carbon dioxide, water and inorganic substances at normal temperature and normal pressure, and the reaction process is quick and efficient, easy to operate and low in priceThe method is low in cost and free from secondary pollution, so that the method has great potential application value and becomes an important research direction in the VOCs treatment technology. In addition, photocatalysis is widely applied to degradation of pesticides such as polychlorinated biphenyl and petroleum pollutants in soil. The degradation rate of organic pollutants under natural illumination conditions is very slow, the core of the photocatalytic degradation technology lies in the selection of photocatalytic materials, and the current commonly used photocatalytic materials mainly comprise TiO2、Fe2O3The single photocatalytic material has the defects of poor visible light response performance, unsatisfied chemical adsorption performance of adsorption and activation of certain reactants and the like, so that the composite photocatalytic material is more and more applied in environmental pollution treatment, and the development of more and more efficient composite photocatalytic active materials is the key point of the research of the photocatalytic degradation technology at present.
Disclosure of Invention
The invention aims to provide B, P co-doped CoMoO4-α-Fe2O3A photocatalyst, a preparation method thereof and application thereof in degrading soil organic pollutants.
A material for degrading soil organic pollutants is characterized by being prepared by the following process: dissolving cobalt salt, molybdenum salt, disodium hydrogen phosphate and boric acid in a certain proportion in a mixed solution of isopropanol and glycerol, transferring the mixed solution into a high-pressure reaction kettle, and carrying out solvothermal reaction at 180 ℃ and 200 ℃ to obtain spherical P, B co-doped CoMoO with the particle size of 300-4；
CoMoO doping B, P4Washing with deionized water and ethanol alternately, dissolving in deionized water, sequentially adding ferric acetylacetonate, ammonium acetate and urea, and performing hydrothermal reaction at 180 ℃ and 200 ℃ to obtain B, P codoped CoMoO4-α-Fe2O3。
Preferably, the cobalt salt and the molybdenum salt are cobalt nitrate and molybdenum nitrate;
preferably, the molar ratio of the cobalt salt to the molybdenum salt to the disodium hydrogen phosphate to the boric acid is 1: 1: (0.01-0.1): (0.01-0.1);
preferably, the solvothermal reaction time is 10-18 h;
preferably, the molar ratio of ferric acetylacetonate to ammonium acetate to urea is 1: (1-2): (1-2);
preferably, alpha-Fe2O3The particle size of the (B) is 5-10 nm;
the technical effects are as follows: nanometer spherical P, B-codoped CoMoO is prepared by taking isopropanol and glycerol as solvents4The catalyst has extremely large specific surface area, and is beneficial to improving the catalytic contact area; by pairing CoMoO4P, B co-doping is carried out, disodium hydrogen phosphate and boric acid have crucial influence on regulation and control of material structure morphology on the one hand, and P, B doping is adopted to inhibit photo-generated electron-hole recombination and improve CoMoO4Degradation activity on organic pollutants under visible light conditions; further loading nano-particle alpha-Fe on the surface by hydrothermal process2O3And a heterojunction is easily formed between the two in the hydrothermal process, so that the photocatalytic efficiency is synergistically improved.
Drawings
FIG. 1 is an B, P co-doped CoMoO of core-shell structure prepared in the present application4-α-Fe2O3The lower right corner of the SEM image is an enlarged view.
Detailed Description
Example 1
20mmol of cobalt salt, 20mmol of molybdenum salt, 1mmol of disodium hydrogen phosphate and 1mmol of boric acid are dissolved in 100ml of a solution with a volume ratio of 1: 1, transferring the mixed solution into a high-pressure reaction kettle, and carrying out solvothermal reaction for 10 hours at 180 ℃ to obtain spherical P, B co-doped CoMoO with the particle size of 300-500nm4；
CoMoO doping B, P4Washing with deionized water and ethanol alternately, dissolving in 50ml deionized water, sequentially adding 5mmol of ferric acetylacetonate, 3mmol of ammonium acetate and 3mmol of urea, and carrying out hydrothermal reaction at 180 ℃ for 12h to obtain B, P co-doped CoMoO4-α-Fe2O3。
Comparative example 1
20mmol of cobalt salt, 20mmol of molybdenum salt, 1mmol of disodium hydrogen phosphate and 1mmol of boric acid are dissolved in 100ml of a solution with a volume ratio of 1: 1 isopropyl alcohol, 1,Transferring the mixed solution into a high-pressure reaction kettle, carrying out solvothermal reaction for 10 hours at 180 ℃ to obtain spherical P, B co-doped CoMoO with the particle size of 300-4。
Comparative example 2
Adding 5mmol of ferric acetylacetonate, 3mmol of ammonium acetate and 3mmol of urea into 50ml of deionized water in sequence, and carrying out hydrothermal reaction at 180 ℃ for 12h to obtain alpha-Fe2O3
20mg of the photocatalyst of example 1 and comparative examples 1 to 2 was added to 50g of soil containing 50mg/Kg of bisphenol A, mixed uniformly, and irradiated under visible light for 1 hour to measure the degradation rate of the material to bisphenol A.
| Degradation rate of bisphenol A after 1h | Degradation rate after 20 cycles | |
| Example 1 | 98.3％ | 95.8％ |
| Comparative example 1 | 87.1％ | 79.1％ |
| Comparative example 2 | 80.3％ | 82.4％ |
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims.
Claims (6)
1. A material for degrading soil organic pollutants is characterized by being prepared by the following process: dissolving cobalt salt, molybdenum salt, disodium hydrogen phosphate and boric acid in a certain proportion in a mixed solution of isopropanol and glycerol, transferring the mixed solution into a high-pressure reaction kettle, and carrying out solvothermal reaction at 180 ℃ and 200 ℃ to obtain spherical P, B co-doped CoMoO with the particle size of 300-4；
CoMoO doping B, P4Washing with deionized water and ethanol alternately, dissolving in deionized water, sequentially adding ferric acetylacetonate, ammonium acetate and urea, and performing hydrothermal reaction at 180 ℃ and 200 ℃ to obtain spherical B, P co-doped CoMoO4Surface loading nano alpha-Fe2O3A composite of particles.
2. The material for degrading soil organic pollutants as claimed in claim 1, wherein the cobalt salt and the molybdenum salt are cobalt nitrate and molybdenum nitrate.
3. A material for degrading soil organic pollutants as claimed in claim 1, wherein the molar ratio of cobalt salt, molybdenum salt, disodium hydrogen phosphate and boric acid is 1: 1: (0.01-0.1): (0.01-0.1).
4. A material for the degradation of organic pollutants in soil as claimed in claim 1, wherein the solvothermal reaction time is 10-18 h.
5. A material for degrading soil organic pollutants according to claim 1, wherein the molar ratio of ferric acetylacetonate, ammonium acetate and urea is 1: (1-2): (1-2).
6. According to the claimsThe material for degrading organic pollutants of soil, alpha-Fe, according to claim 12O3The particle size of (A) is 5-10 nm.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111347036.3A CN114042466B (en) | 2021-11-15 | 2021-11-15 | Material for degrading organic pollutants in soil |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202111347036.3A CN114042466B (en) | 2021-11-15 | 2021-11-15 | Material for degrading organic pollutants in soil |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115463663A (en) * | 2022-08-01 | 2022-12-13 | 广西大学 | Magnetic reduction graphene oxide/cobalt molybdate composite catalyst and preparation method and application thereof |
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| CN111330649A (en) * | 2020-05-07 | 2020-06-26 | 俞春亚 | Composite nano material for degrading VOC gas and preparation method thereof |
| US20210276084A1 (en) * | 2020-03-06 | 2021-09-09 | Florida Atlantic University Board Of Trustees | Nanoparticle self-assembling method for forming core-shell nanohybrids |
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2021
- 2021-11-15 CN CN202111347036.3A patent/CN114042466B/en active Active
Patent Citations (6)
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| CN106637290A (en) * | 2016-12-20 | 2017-05-10 | 华南理工大学 | Porous efficient electrochemical catalyst prepared by in-situ pore-forming method and preparation method and application of porous efficient electrochemical catalyst |
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| CN115463663A (en) * | 2022-08-01 | 2022-12-13 | 广西大学 | Magnetic reduction graphene oxide/cobalt molybdate composite catalyst and preparation method and application thereof |
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