CN114797895A - Composite catalyst and preparation method and application thereof - Google Patents
Composite catalyst and preparation method and application thereof Download PDFInfo
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- CN114797895A CN114797895A CN202210572111.4A CN202210572111A CN114797895A CN 114797895 A CN114797895 A CN 114797895A CN 202210572111 A CN202210572111 A CN 202210572111A CN 114797895 A CN114797895 A CN 114797895A
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- 239000003054 catalyst Substances 0.000 title claims abstract description 50
- 239000002131 composite material Substances 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical class O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 12
- 230000003197 catalytic effect Effects 0.000 claims abstract description 10
- MMDJDBSEMBIJBB-UHFFFAOYSA-N [O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[NH6+3] Chemical compound [O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[NH6+3] MMDJDBSEMBIJBB-UHFFFAOYSA-N 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 15
- 239000000243 solution Substances 0.000 claims description 8
- 239000011259 mixed solution Substances 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 5
- 229910052751 metal Inorganic materials 0.000 claims description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- 238000001354 calcination Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 3
- 229910021486 amorphous silicon dioxide Inorganic materials 0.000 claims description 3
- 229910021591 Copper(I) chloride Inorganic materials 0.000 claims description 2
- 101100028920 Neurospora crassa (strain ATCC 24698 / 74-OR23-1A / CBS 708.71 / DSM 1257 / FGSC 987) cfp gene Proteins 0.000 claims description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 2
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical compound [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 claims description 2
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 238000001704 evaporation Methods 0.000 claims description 2
- 239000002243 precursor Substances 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 239000000126 substance Substances 0.000 abstract description 14
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 9
- 239000010865 sewage Substances 0.000 abstract description 9
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 238000001179 sorption measurement Methods 0.000 abstract description 3
- 229910052742 iron Inorganic materials 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract description 2
- 238000002156 mixing Methods 0.000 abstract description 2
- YPJKMVATUPSWOH-UHFFFAOYSA-N nitrooxidanyl Chemical compound [O][N+]([O-])=O YPJKMVATUPSWOH-UHFFFAOYSA-N 0.000 abstract description 2
- 238000012545 processing Methods 0.000 abstract description 2
- 238000006243 chemical reaction Methods 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 229910002668 Pd-Cu Inorganic materials 0.000 description 3
- 238000010531 catalytic reduction reaction Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 238000006722 reduction reaction Methods 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 238000002306 biochemical method Methods 0.000 description 2
- 125000004432 carbon atom Chemical group C* 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 150000007524 organic acids Chemical class 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N Formic acid Chemical compound OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 1
- 241000282414 Homo sapiens Species 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000012851 eutrophication Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000002352 surface water Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
-
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/89—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals
- B01J23/8926—Copper and noble metals
-
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/89—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals
- B01J23/8933—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals also combined with metals, or metal oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/8946—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals also combined with metals, or metal oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with alkali or alkaline earth metals
-
- 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
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
-
- 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
- C02F1/70—Treatment of water, waste water, or sewage by reduction
-
- 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
- C02F2101/10—Inorganic compounds
- C02F2101/16—Nitrogen compounds, e.g. ammonia
- C02F2101/163—Nitrates
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Catalysts (AREA)
Abstract
The invention provides a composite catalyst and a preparation method and application thereof, belonging to the technical field of sewage treatment in environmental engineering. The catalyst is a supported catalyst and consists of a catalytic active component and a carrier. The active component loaded by the catalyst consists of a main catalyst and a cocatalyst. The carrier is prepared by mixing and processing two materials according to a certain proportion, and the carrier is composed of graphene and modified diatomite which are stable in chemical property, good in adsorption performance and large in specific surface area. The catalyst active component in the invention: the main catalyst is Pd and the auxiliary catalyst is Cu, nitrate radical and reducing iron simple substance (Fe) in the water body are catalyzed by the catalyst 0 ) Is reacted and converted into N 2 Thereby to achieveTo achieve the purpose of effective denitrification.
Description
The application is a divisional application with application date of 2019, 03 and 25, application number of 201910228790.1 and invention name of 'a composite catalyst and a preparation method thereof'.
Technical Field
The invention belongs to the technical field of sewage treatment in environmental engineering, and relates to a composite catalyst, and a preparation method and application thereof.
Background
With the development of industry and agriculture, nitrate Nitrogen (NO) in water body 3 - ) Contamination has become an environmental problem that is urgently sought to be solved. The excessive discharge of nitrate nitrogen in sewage can directly cause eutrophication of water body and reduction of water quality, and pollution damages ecological environment, thereby causing great influence on production and life of human beings. In addition, data show that the pollution of nitrate in underground water is more serious to a certain extent due to the discharge of high-nitrogen-content sewage. Therefore, the nitrogen-containing sewage is treated in a municipal sewage plant before being discharged to the surface water body and then discharged. In practice, the treatment process is limited by the quality of the sewage and the treatment process,the denitrification effect is not ideal, and the nitrate nitrogen content of the effluent is often higher, so that the effluent cannot reach the standard and is discharged. Therefore, it is an urgent problem to adopt any technique to effectively reduce the effluent nitrate nitrogen of the sewage plant to reduce the nitrogen pollution.
At present, common technologies for removing nitrate nitrogen in water bodies include: physical chemical, biological and chemical methods. The physical and chemical method is mainly used for removing nitrate nitrogen in the water body through the actions of selective adsorption, selective permeability of a membrane and the like. The method has the disadvantages that nitrate nitrogen in the water body cannot be completely removed, and only the transfer or concentration of pollutants occurs. The biochemical method is a denitrification technology which is applied more at present, and although the removal effect is better, the biochemical method has the defects of low impact load resistance, large influence by water quality, complex process and the like. Chemical methods include active metal reduction methods and catalytic reduction methods. The active metal reduction method utilizes active metal (such as Fe) 0 ) Reducing and removing nitrate nitrogen in the water body. The method has the defect that the by-product of the reaction mainly comprises ammonia nitrogen and needs secondary treatment. The catalytic reduction method mainly uses hydrogen or organic acid (such as HCOOH) as a reducing agent, and removes nitrate nitrogen by catalytic reduction under the action of a catalyst. The method has the disadvantages of high operation conditions (such as hydrogen gas inflow and operation pressure), incomplete decomposition of organic acid, easy secondary pollution and the like.
Disclosure of Invention
The invention aims to provide a composite catalyst, and a preparation method and application thereof. The catalyst is a supported catalyst and consists of a catalytic active component and a carrier. The active component loaded by the catalyst consists of a main catalyst and a cocatalyst. The carrier is prepared by mixing and processing two materials according to a certain proportion, and the carrier is composed of graphene and modified diatomite which are stable in chemical property, good in adsorption performance and large in specific surface area. The catalyst active component in the invention: the main catalyst is Pd and the auxiliary catalyst is Cu, nitrate radical and reducing iron simple substance (Fe) in the water body are catalyzed by the catalyst 0 ) Is reacted and converted into N 2 Thereby achieving the purpose of effective denitrification.
The specific technical scheme is as follows:
a composite catalyst is a supported catalyst and consists of a catalytic active component and a carrier, wherein the carrier consists of modified diatomite and graphene; the mass ratio of the graphene to the modified diatomite is 2: 1 or 3: 1; the active components are as follows: a main catalyst Pd and a cocatalyst Cu;
in the active components of the catalyst, Pd: the Cu mass ratio is 3: 1 or 4: 1;
the mass of the Pd accounts for 5 percent of the composite catalyst;
the mass ratio of the catalyst carrier to the catalyst active components is 24: 1-11.5: 1;
the specific surface area of the modified diatomite is 325m 2 /g；
The modified diatomite is obtained by modifying diatomite in 0.5mol/L hydrochloric acid for 1 hour;
the diatomite is in a round sieve shape and comprises amorphous SiO 2 、Al 2 O 3 、MgO、Fe 2 O 3 CaO and Na 2 O。
The preparation method of the composite catalyst comprises the following steps:
step 1: weighing metal precursor PdC1 to reach target load 2 、CuCl 2 ·2H 2 Dissolving O in water to obtain a mixed solution; the volume of the mixed solution is slightly larger than that of the carrier;
step 2: placing the pretreated composite carrier and the mixed solution in a rotary evaporator, and evaporating until no water exists to obtain a sample;
and step 3: putting the sample into a muffle furnace, calcining for 2 hours at 400 ℃, and introducing N into the muffle furnace during calcination 2 Wrapping the crucible containing the sample by using tin foil paper to obtain a sample to be reduced;
and 4, step 4: after the sample to be reduced is naturally cooled to room temperature, adding excessive 1mol/L NaBH into the sample 4 Fully stirring the solution for 12 hours, repeatedly washing the solution by using deionized water, centrifugally dewatering, drying in vacuum, and then placing the solution in a dryer for drying to obtain the composite catalyst; the stirring intensity is 400 r/min.
In the present inventionThe sample to be reduced is reacted with NaBH 4 The chemical reaction equation for the reaction is as follows:
2PdCl 2 +NaBH 4 +3H 2 O＝2Pd+NaCl+3HCl+B(OH) 3 +2H 2 ；
2CuCl 2 +NaBH 4 +3H 2 O＝2Cu+NaNO 3 +B(OH) 3 +2H 2 +3HNO 3 。
the invention also provides the application of the composite catalyst or the catalyst prepared by the preparation method in the scheme in removing nitrate nitrogen in water.
Compared with the prior art, the invention has the following beneficial effects:
the diatomite used in the composite catalyst of the invention is in a round sieve shape, and the main chemical component is amorphous SiO 2 And also contains a small amount of Al 2 O 3 、MgO、Fe 2 O 3 、CaO、Na 2 O, etc. has high thermal stability and chemical stability, and after modification, the diatomite has large pore size and large specific surface area of 255m 2 The g is changed to 325m 2 (ii)/g; on the other hand, the chemical properties of the diatomite are changed, substances such as CaO, MgO and the like in the diatomite are dissolved by acid, the purity is higher, the surface activity is enhanced along with the substances, and the absorption of nitrate nitrogen is facilitated, so that the occurrence of catalytic denitrification reaction is promoted. Graphene is a novel two-dimensional carbon nanomaterial, and the structure of the graphene is mainly a two-dimensional lattice consisting of carbon atoms with the thickness of a monoatomic layer, wherein the carbon atoms are periodically arranged in a six-membered ring form. The graphene has excellent mechanical and thermal properties, a large specific surface area, high chemical stability and excellent electronic conductivity, and can be used for sewage treatment.
Detailed Description
The technical solution of the present invention will be further described in detail with reference to specific examples.
Under certain reaction conditions, Pd-Cu/modified diatomite-graphene and Pd-Cu/diatomite-graphene catalysts are respectively selected to be used for removing nitrate nitrogen in water, and the nitrate nitrogen can be converted into nitrate nitrogen through catalytic reaction under the catalytic action of the catalystsHarmless N 2 . The test investigates the influence of the mass ratio of Pd to Cu and the mass ratio of graphene to modified diatomite in the catalyst on the catalytic effect, and the test results are as follows:
TABLE 1 comparison of catalytic Effect
From the above experiments, it was found that when the mass ratio of Pd to Cu in the catalyst is 3: 1. the mass ratio of the graphene to the diatomite/modified diatomite is 2: 1, the system can obtain better catalytic effect and has good economical efficiency. In addition, compared with Pd-Cu/graphene-diatomite, the catalytic effect of the modified catalyst is remarkably improved.
The above description is only a preferred embodiment of the present invention, and the scope of the present invention is not limited thereto, and any simple modifications or equivalent substitutions of the technical solutions that can be obviously obtained by those skilled in the art within the technical scope of the present invention are within the scope of the present invention.
Claims (3)
1. The composite catalyst is characterized by being a supported catalyst and comprising a catalytic active component and a carrier, wherein the carrier consists of modified diatomite and graphene; the mass ratio of the graphene to the modified diatomite is 2: 1 or 3: 1; the active components are as follows: a main catalyst Pd and a cocatalyst Cu;
in the active components of the catalyst, Pd: the Cu mass ratio is 3: 1 or 4: 1;
the mass of the Pd accounts for 5 percent of the composite catalyst;
the mass ratio of the catalyst carrier to the catalyst active components is 24: 1-11.5: 1;
the specific surface area of the modified diatomite is 325m 2 /g；
The modified diatomite is obtained by modifying diatomite in 0.5mol/L hydrochloric acid for 1 hour;
the diatomite is in a round sieve shape and comprises amorphous SiO 2 、Al 2 O 3 、MgO、Fe 2 O 3 CaO and Na 2 O。
2. A method for preparing the composite catalyst of claim 1, comprising the steps of:
step 1: weighing metal precursor PdC1 to reach target load 2 、CuCl 2 ·2H 2 Dissolving O in water to obtain a mixed solution; the volume of the mixed solution is slightly larger than that of the carrier;
step 2: placing the pretreated composite carrier and the mixed solution in a rotary evaporator, and evaporating until no water exists to obtain a sample;
and step 3: putting the sample into a muffle furnace, calcining for 2 hours at 400 ℃, and introducing N into the muffle furnace during calcination 2 And wrapping the crucible containing the sample by using tin foil paper;
and 4, step 4: when the sample is naturally cooled to room temperature, adding excessive 1mol/L NaBH 4 Fully stirring the solution for 12 hours, repeatedly washing the solution by using deionized water, centrifugally dewatering, drying in vacuum, and then placing the solution in a dryer for drying to obtain the composite catalyst; the stirring intensity is 400 r/min.
3. Use of the composite catalyst according to claim 1 or the catalyst prepared by the preparation method according to claim 2 for removing nitrate nitrogen in water.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210572111.4A CN114797895A (en) | 2019-03-25 | 2019-03-25 | Composite catalyst and preparation method and application thereof |
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| CN202210572111.4A CN114797895A (en) | 2019-03-25 | 2019-03-25 | Composite catalyst and preparation method and application thereof |
| CN201910228790.1A CN109759076A (en) | 2019-03-25 | 2019-03-25 | A kind of composite catalyst and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001008550A (en) * | 1999-06-30 | 2001-01-16 | Goko Kikaku:Kk | Method for reducing nitrate nitrogen in soil and material used for the method |
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| CN108745373A (en) * | 2018-06-15 | 2018-11-06 | 南京大学 | A kind of preparation method of precious metal alloys/carbon material supported type catalyst |
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2019
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- 2019-03-25 CN CN202210572111.4A patent/CN114797895A/en active Pending
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