CN113481517A - Preparation method of bifunctional catalyst for degrading environmental pollutant hydrazine - Google Patents
Preparation method of bifunctional catalyst for degrading environmental pollutant hydrazine Download PDFInfo
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- CN113481517A CN113481517A CN202110923754.4A CN202110923754A CN113481517A CN 113481517 A CN113481517 A CN 113481517A CN 202110923754 A CN202110923754 A CN 202110923754A CN 113481517 A CN113481517 A CN 113481517A
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- hydrazine
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- porous
- nanoneedle
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- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 239000003054 catalyst Substances 0.000 title claims abstract description 29
- 239000003344 environmental pollutant Substances 0.000 title claims abstract description 18
- 230000001588 bifunctional effect Effects 0.000 title claims abstract description 7
- 238000002360 preparation method Methods 0.000 title claims description 14
- 230000000593 degrading effect Effects 0.000 title claims description 6
- 230000015556 catabolic process Effects 0.000 claims abstract description 14
- 238000006731 degradation reaction Methods 0.000 claims abstract description 14
- 230000003197 catalytic effect Effects 0.000 claims abstract description 13
- 239000007788 liquid Substances 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 8
- 231100000719 pollutant Toxicity 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- 239000000243 solution Substances 0.000 claims description 12
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims description 8
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 8
- 239000003153 chemical reaction reagent Substances 0.000 claims description 8
- 229910052750 molybdenum Inorganic materials 0.000 claims description 8
- 239000011733 molybdenum Substances 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- 239000012018 catalyst precursor Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 229910003178 Mo2C Inorganic materials 0.000 claims description 5
- IMQLKJBTEOYOSI-GPIVLXJGSA-N Inositol-hexakisphosphate Chemical compound OP(O)(=O)O[C@H]1[C@H](OP(O)(O)=O)[C@@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@@H]1OP(O)(O)=O IMQLKJBTEOYOSI-GPIVLXJGSA-N 0.000 claims description 4
- IMQLKJBTEOYOSI-UHFFFAOYSA-N Phytic acid Natural products OP(O)(=O)OC1C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C1OP(O)(O)=O IMQLKJBTEOYOSI-UHFFFAOYSA-N 0.000 claims description 4
- 235000018660 ammonium molybdate Nutrition 0.000 claims description 4
- 239000011609 ammonium molybdate Substances 0.000 claims description 4
- 229940010552 ammonium molybdate Drugs 0.000 claims description 4
- 229940068041 phytic acid Drugs 0.000 claims description 4
- 235000002949 phytic acid Nutrition 0.000 claims description 4
- 239000000467 phytic acid Substances 0.000 claims description 4
- 239000012265 solid product Substances 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 3
- 229910021607 Silver chloride Inorganic materials 0.000 claims description 3
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 3
- 238000004458 analytical method Methods 0.000 claims description 3
- 238000000137 annealing Methods 0.000 claims description 3
- 239000007853 buffer solution Substances 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 229910021397 glassy carbon Inorganic materials 0.000 claims description 3
- 229910052698 phosphorus Inorganic materials 0.000 claims description 3
- 239000011574 phosphorus Substances 0.000 claims description 3
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims description 2
- -1 ammonium molybdate heptahydrate Chemical class 0.000 claims description 2
- ZKKLPDLKUGTPME-UHFFFAOYSA-N diazanium;bis(sulfanylidene)molybdenum;sulfanide Chemical compound [NH4+].[NH4+].[SH-].[SH-].S=[Mo]=S ZKKLPDLKUGTPME-UHFFFAOYSA-N 0.000 claims description 2
- 229910000476 molybdenum oxide Inorganic materials 0.000 claims description 2
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 claims description 2
- 235000015393 sodium molybdate Nutrition 0.000 claims description 2
- 239000011684 sodium molybdate Substances 0.000 claims description 2
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 2
- QIJNJJZPYXGIQM-UHFFFAOYSA-N 1lambda4,2lambda4-dimolybdacyclopropa-1,2,3-triene Chemical compound [Mo]=C=[Mo] QIJNJJZPYXGIQM-UHFFFAOYSA-N 0.000 claims 1
- 229910039444 MoC Inorganic materials 0.000 claims 1
- 239000001257 hydrogen Substances 0.000 abstract description 13
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 13
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 11
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 7
- 230000007613 environmental effect Effects 0.000 abstract description 5
- 230000002829 reductive effect Effects 0.000 abstract 1
- 239000002243 precursor Substances 0.000 description 4
- 239000002803 fossil fuel Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 239000010411 electrocatalyst Substances 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 229910052755 nonmetal Inorganic materials 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 150000002843 nonmetals Chemical class 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/02—Hydrogen or oxygen
-
- 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
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/46104—Devices therefor; Their operating or servicing
- C02F1/46109—Electrodes
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
- C25B11/091—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds
-
- 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
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/46104—Devices therefor; Their operating or servicing
- C02F1/46109—Electrodes
- C02F2001/46133—Electrodes characterised by the material
-
- 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
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/46104—Devices therefor; Their operating or servicing
- C02F1/46109—Electrodes
- C02F2001/46152—Electrodes characterised by the shape or form
-
- 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
Abstract
Hydrazine, an environmental pollutant, is colorless oily liquid which is fuming, corrosive and highly reductive. The catalytic degradation of hydrazine pollutants is a hotspot problem in the field of environmental catalytic chemistry and is also a hotspot for researching bifunctional catalysts. The electrocatalysis degradation of hydrazine pollutants and the generation of hydrogen have important scientific and practical significance for evaluating the environmental ecology. The pollution of hydrazine organic pollutants in water seriously harms the ecological environment and the life safety of people. By developing a novel bifunctional catalyst, the cathode is used for generating hydrogen in the electrocatalysis process, and the anode is used for electrocatalysis degradation of hydrazine organic pollutants, so that not only is zero-pollution degradation of hydrazine realized, but also a new thought is provided for constructing a resource-saving society.
Description
Technical Field
The invention relates to the field of preparation methods and applications of catalysts doped with various non-metals, in particular to a method for preparing N, P-Mo2C, a method for preparing the porous nanoneedle catalyst and application of the porous nanoneedle catalyst in the field of electrocatalytic degradation of hydrazine environmental pollutants and hydrogen production; the method adopts an electrochemical method, so that the process is pollution-free, organic pollutants are degraded, and hydrogen, a novel energy source, is generated, and the two aims are achieved; meanwhile, the preparation of the electrocatalyst is of a porous structure, so that the electrocatalyst is more beneficial to exposing more active sites, degrading pollutants and producing more hydrogen.
Background
The energy is the guarantee of human development and is an important support for social progress. The main energy sources of the current society are fossil fuels such as coal, petroleum and shale gas, but the fossil fuels face the problems of low reserves, difficult exploitation, non-regeneration and the like, and simultaneously cause environmental pollution and threaten human health. Hydrogen energy has received attention from researchers as a clean, efficient renewable energy source. The combustion product of hydrogen is water, which not only has zero pollution, but also has high heat and wide source, and is the most ideal alternative energy of the traditional fossil fuel. The catalytic hydrogen production by water electrolysis is considered to be an effective hydrogen production method.
The catalytic degradation of hydrazine pollutants is a hot problem in the field of environmental catalytic chemistry, and the electrocatalytic degradation of the hydrazine pollutants and the generation of hydrogen have important scientific and practical significance for evaluating environmental ecology. The pollution of hydrazine organic pollutants in water seriously harms the ecological environment and the life safety of people. The cathode of the electrocatalysis process is used for generating hydrogen, and the anode is used for electrocatalysis degradation of hydrazine organic pollutants, so that zero-pollution degradation of hydrazine is realized, and a new idea is provided for constructing a resource-saving society.
The research and development of the multifunctional catalyst have important significance in the fields of nano materials, environmental catalysis and the like. The traditional single catalyst has the problems of low catalytic efficiency, poor catalytic effect and the like, so that the development of the high-efficiency doped catalyst has important guiding significance in the field of catalysis.
Disclosure of Invention
One of the objects of the present invention is an N, P-Mo2A novel preparation method of a C porous nanometer needle bifunctional catalyst.
The other purpose of the invention is to apply the synthesized nanoneedle catalyst to the electrocatalytic degradation of hydrazine organic pollutants.
The third purpose of the invention is to apply the synthesized nanoneedle catalyst to a system for producing hydrogen while degrading organic pollutants by electrocatalysis.
The fourth purpose of the invention is to provide a preparation method for synthesizing a doped porous precursor at room temperature.
The technical scheme of the invention is as follows:
1.N，P-Mo2c, preparation of a porous nanoneedle catalyst: adding a molybdenum source reagent, 0-50 g of phytic acid and 0-50 g of aniline into 100 mL of deionized water, adding 0-50 mL of 1M hydrochloric acid, and strongly stirring uniformly to control the pH value of the solution to be 1.5-8.5 to obtain a preparation solution of the catalyst; controlling the temperature of the prepared liquid to be 40-80 ℃, strongly stirring for 3-10 h, then carrying out centrifugal analysis on the prepared liquid, washing the obtained solid product with ethanol, and drying to obtain a nitrogen and phosphorus double-doped catalyst precursor; annealing the obtained nitrogen, phosphorus-double doped catalyst precursor at 650-1200 ℃ for 3-20 h to obtain N, P-Mo2C porous nanoneedle catalyst.
2. The N, P-Mo of the scheme2The C porous nanometer needle catalyst is synthesized for the first time, and the precursor doping at a lower temperature is realized by skillfully using the non-metal elements in the phytic acid, the aniline and the molybdenum source reagent, so that compared with the traditional direct high-temperature doping, a large amount of energy is saved, and a very good doping effect is achieved.
3. N，P-Mo2In the preparation method of the C porous nanoneedle catalyst, the molybdenum source reagent is one or a combination of more of ammonium molybdate heptahydrate, ammonium molybdate, sodium molybdate, ammonium thiomolybdate and molybdenum oxide, and the content of the molybdenum source reagent is 0.01-100 mol.
4. Hydrogen is produced during the process of electro-catalytic degradation of the hydrazine environmental pollutants, a three-electrode system is adopted for testing, and the performance of electro-catalytic degradation of the hydrazine environmental pollutants is tested on an electrochemical workstation; adding a certain concentration of pollutant liquid into the catalytic base liquid to be coated with N, P-Mo2And the glassy carbon electrode of the C porous nanoneedle catalyst is used as a working electrode, a carbon rod is used as a counter electrode, an Ag/AgCl electrode is used as a reference electrode, and 0.1-10 mol/L sulfate buffer solution is used as a catalytic base solution.
5. The doping mode applied in the scheme is low-temperature precursor doping, so that the defect of energy waste of the traditional high-temperature precursor doping is overcome, and a new idea for synthesizing the porous material at low temperature is provided.
Detailed description of the preferred embodiments
For a further understanding of the invention, reference will now be made to the preferred embodiments of the invention by way of example, and to the accompanying drawings, which are included to further illustrate features and advantages of the invention, and not to limit the scope of the invention as claimed.
Example 1
Adding a molybdenum source reagent, 25 g of phytic acid and 0-50 g of aniline into 100 mL of deionized water, adding 0-50 mL of 1M hydrochloric acid, and strongly stirring uniformly to control the pH value of the solution to be about 5.5 to obtain a preparation solution of the catalyst.
Example 2
Controlling the temperature of the prepared solution at 60 ℃, stirring the solution vigorously for 3 hours, then carrying out centrifugal analysis on the solution, washing the obtained solid product with ethanol, and drying the solid product to obtain the nitrogen and phosphorus double-doped catalyst precursor.
Example 3
Annealing the obtained nitrogen, phosphorus-double doped catalyst precursor at 850 ℃ for 10 h to obtain N, P-Mo2C porous nanoneedle catalyst.
Example 4
A three-electrode system is adopted for testing, and the performance of electrocatalytic degradation of hydrazine environmental pollutants is tested on an electrochemical workstation; adding a certain concentration of pollutant liquid into the catalytic base liquid to be coated with N, P-Mo2The glassy carbon electrode of the C porous nanoneedle catalyst is used as a working electrode, a carbon rod is used as a counter electrode, an Ag/AgCl electrode is used as a reference electrode, and 0.5 mol/L sulfate buffer solution is used as a catalytic base solution.
Claims (3)
1. A method for preparing a bifunctional catalyst for degrading environmental pollutant hydrazine, relating to nitrogen and phosphorus-double-doped molybdenum carbide N, P-Mo2The C porous nanoneedle catalyst is characterized by comprising the following preparation steps:
(1) adding a molybdenum source reagent, 0-50 g of phytic acid and 0-50 g of aniline into 100 mL of deionized water, adding 0-50 mL of 1M hydrochloric acid, and strongly stirring uniformly to control the pH value of the solution to be 1.5-8.5 to obtain a preparation solution of the catalyst;
(2) controlling the temperature of the prepared liquid to be 40-80 ℃, strongly stirring for 3-10 h, then carrying out centrifugal analysis on the prepared liquid, washing the obtained solid product with ethanol, and drying to obtain a nitrogen and phosphorus double-doped catalyst precursor;
(3) annealing the obtained nitrogen, phosphorus-double doped catalyst precursor at 650-1200 ℃ for 3-20 h to obtain N, P-Mo2C porous nanoneedle catalyst.
2. The N, P-Mo of claim 12The preparation method of the C porous nanoneedle catalyst is characterized in that in the step (1), the molybdenum source reagent is one or a combination of more of ammonium molybdate heptahydrate, ammonium molybdate, sodium molybdate, ammonium thiomolybdate and molybdenum oxide, and the content of the molybdenum source reagent is 0.01-100 mol.
3. A preparation method of a bifunctional catalyst for degrading environmental pollutant hydrazine is characterized by comprising the following steps of: a three-electrode system is adopted for testing, and the performance of electrocatalytic degradation of hydrazine environmental pollutants is tested on an electrochemical workstation; adding a certain concentration of pollutant liquid into the catalytic base liquid to be coated with N, P-Mo2C porous nanoneedle catalysisThe glassy carbon electrode of the catalyst is a working electrode, a carbon rod is used as a counter electrode, an Ag/AgCl electrode is used as a reference electrode, and 0.1-10 mol/L sulfate buffer solution is used as a catalytic base solution.
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| CN202110923754.4A CN113481517A (en) | 2021-08-12 | 2021-08-12 | Preparation method of bifunctional catalyst for degrading environmental pollutant hydrazine |
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| CN113481517A true CN113481517A (en) | 2021-10-08 |
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Citations (1)
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| CN111644195A (en) * | 2020-07-01 | 2020-09-11 | 济南大学 | Preparation method of catalyst for electrocatalytic degradation of hydrazine environmental pollutants and hydrogen production |
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| CN111644195A (en) * | 2020-07-01 | 2020-09-11 | 济南大学 | Preparation method of catalyst for electrocatalytic degradation of hydrazine environmental pollutants and hydrogen production |
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Application publication date: 20211008 |