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CN105771997A - Preparation method and application of dealkalized red mud - Google Patents

Preparation method and application of dealkalized red mud Download PDF

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Publication number
CN105771997A
CN105771997A CN201610145267.9A CN201610145267A CN105771997A CN 105771997 A CN105771997 A CN 105771997A CN 201610145267 A CN201610145267 A CN 201610145267A CN 105771997 A CN105771997 A CN 105771997A
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red mud
catalyst
dealkalize
dealkalized red
mud
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齐蕾
汤琦
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University of Jinan
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University of Jinan
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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
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/002—Mixed oxides other than spinels, e.g. perovskite
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/86—Catalytic processes
    • B01D53/8621—Removing nitrogen compounds
    • B01D53/8625—Nitrogen oxides
    • B01D53/8628—Processes characterised by a specific catalyst
    • 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
    • B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
    • B01J23/78—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, 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
    • B01J35/40—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
    • B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J35/61—Surface area
    • B01J35/613—10-100 m2/g
    • 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
    • B01J35/615—100-500 m2/g
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2255/00—Catalysts
    • B01D2255/20—Metals or compounds thereof
    • B01D2255/207—Transition metals
    • B01D2255/20738—Iron
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2255/00—Catalysts
    • B01D2255/90—Physical characteristics of catalysts
    • B01D2255/92—Dimensions
    • B01D2255/9202—Linear dimensions
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2255/00—Catalysts
    • B01D2255/90—Physical characteristics of catalysts
    • B01D2255/92—Dimensions
    • B01D2255/9207—Specific surface
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2258/00—Sources of waste gases
    • B01D2258/02—Other waste gases
    • B01D2258/0283—Flue gases
    • 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
    • B01J2523/00—Constitutive chemical elements of heterogeneous catalysts

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Environmental & Geological Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Biomedical Technology (AREA)
  • Analytical Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Catalysts (AREA)
  • Exhaust Gas Treatment By Means Of Catalyst (AREA)

Abstract

The invention relates to a dealkalized red mud catalyst. The dealkalized red mud catalyst comprises the main component of hematite type ferric oxide, the contents of sodium and potassium are low, and the specific surface area of the dealkalized red mud catalyst is 80-160 m<2>.g<-1>, the particle size is 1-10(mu)m, and particles are not clumped. The dealkalized red mud catalyst disclosed by the invention has the characteristics of being large in specific surface area, small in particle size, high in heat stability and the like. In a reaction that NH3 selectively performs catalytic reduction on NO, and in the temperature range of 150-400 DEG C, compared with non-dealkalized red mud, the dealkalized red mud catalyst has the advantages that the denitration performance of the dealkalized red mud catalyst is greatly improved, and the dealkalized red mud catalyst has a potential application value in the field of denitration. The invention discloses a preparation method of the dealkalized red mud catalyst.

Description

A kind of preparation method and its usage of dealkalize red mud
Technical field
The present invention relates to the dealkalize red mud catalyst and preparation method thereof for denitrating flue gas.
Background technology
In recent years, along with being widely used and a large amount of discharges of motor-vehicle tail-gas of fossil fuel, the harm of nitrogen oxides (NOx) is increasingly serious.The nitrogen oxides total amount entering air the most every year is up to 50,000,000 tons, and discharge capacity is also in sustainable growth.Therefore, the emission control of NOx is increasingly paid attention to by countries in the world with governing problem.Ammine selectivity catalytic reduction technology (NH3-SCR) owing to having the advantages such as denitration efficiency is high, operating cost is relatively low, the denitration being widely used in Industrial Boiler and power station unit processes.NH3The key core of-SCR technology is NH3-SCR catalyst system, catalyst cost accounts for the 40% of whole set process expense, and therefore R&D costs height low, active, the denitrating catalyst tool of life-span length are of great significance.
Red mud is a kind of strong basicity solid waste discharged during aluminium metallurgy, the most often produces one ton of aluminum oxide and just has the red mud of 0.5 ~ 2 ton and produce, and current China adds up red mud storage and reached several hundred million tons.China processes the method for red mud and mainly uses Red Mud Dam to store up, and water resource and soil around red mud dump are subject to pollution of seriously alkalizing, and the red mud stacked in addition also results in sand and dust harm.Therefore, along with the volume of cargo in storage of red mud is continuously increased, caused environmental pollution is the most serious, and red mud comprehensive utilization has become one urgent need to solve the problem of aluminum smelting industry.Comprehensive utilization about red mud mainly has three directions: using red mud as producing construction material and the raw material of ceramic；The elements such as iron, aluminium, titanium in red mud are carried out recycling；Utilize red mud to make the environmental pollution such as adsorbent, flocculant, catalyst to administer.Based on red mud, wherein prepare catalyst carry out environmental pollution improvement, be a kind of method being effectively increased discarded object effective value.Red mud itself contains Multicomponent, and wherein iron oxide, titanium oxide etc. have denitration activity, and aluminum oxide, silica are conventional denitration catalyst carriers, therefore can prepare denitrating catalyst based on red mud, reach the purpose of the treatment of wastes with processes of wastes against one another.The strong basicity of red mud can be substantially reduced the denitration efficiency of shadow red mud, and therefore the high alkali content of red mud becomes it and is difficult to the extensive bottleneck effectively utilized, and to red mud carries out dealkalize process, is to solve this bottleneck effective means.
We are by the preparation method of a kind of simplicity, with the red mud as a raw material of industrial residue, are successfully prepared a series of dealkalize red mud catalyst with denitration activity.Meanwhile, this catalyst is raw materials used cheap and easy to get, and preparation method is simple and efficient, less energy consumption, and environmental pollution is little, has the effect of the treatment of wastes with processes of wastes against one another, at NH3There is potential application prospect in-SCR catalytic denitration field.
Summary of the invention
It is an object of the invention to provide a kind of dealkalize red mud catalyst and its production and use.As raw material, to use acid nitrification-alkaline precipitation to carry out dealkalize from the two of factory kinds of red muds (original red mud and carry sodium red mud), the red mud specific surface area after dealkalize is greatly increased, and particle size reduces, and has NH3-SCR denitration activity.
The principle of the present invention is as follows: in red mud carries out acid nitrifying process, first salt and the exchangeable ion of absorption dissolve, most of Al3+And other ionizable metal salt removes from lattice structure, form more microcellular structure, thus improve the specific surface area of red mud.During alkali precipitation, the sodium in red mud, calcium compound decompose and are dissolved in solution, and other slaines define hydroxide and precipitate such as Al (OH)3、Fe(OH)3, afterwards through washing, filtration, remove the alkali metal salt component dissolved.Dealkalize red mud self contains Multimetal oxide component, and wherein iron oxide, titanium oxide etc. have denitration activity, and aluminum oxide, silica etc. are good denitration catalyst carriers.
Technical scheme is as follows:
A kind of dealkalize red mud catalyst, is mainly composed of hematite-type di-iron trioxide, and sodium, potassium content are extremely low, and dealkalize red mud specific surface area of catalyst is 80-160 m2·g-1, particle size is 1 μm-10 μm, soilless sticking between particle.
A kind of method preparing above-mentioned dealkalize red mud catalyst, is made up of following steps: red mud and water are mixed into red mud mud, and red mud is 1:15 with the mass ratio of water, and magnetic agitation 1 h is added dropwise over nitric acid in mixed liquor, and the concentration of nitric acid is 10.3 mol L-1, regulation pH value is 0,50oC stirred in water bath 30 min；Being added dropwise over ammoniacal liquor in mixed liquor after acidifying, the concentration of ammoniacal liquor is 13.2 mol L-1, regulation pH value is 10,50oC stirred in water bath 30 min, stands and is cooled to room temperature；Mud suction filtration is washed to neutrality, by filter cake 120oC is dried 12 h, grinds, in Muffle furnace under air atmosphere 550oC roasting 6 h, i.e. obtains dealkalize red mud catalyst.By untreated original red mud with carry sodium red mud and be respectively labeled as RM and TRM in Muffle furnace after 550 ° of C roasting 6 h, dealkalize process after original red mud and carry sodium red mud and be respectively labeled as PRM and PTRM.
The dealkalize red mud sample of the present invention is as NH3The catalyst of-SCR removing nitrogen oxides, has preferable NH3-SCR denitration activity.
The dealkalize red mud sample of the present invention has the feature such as high-specific surface area, preferable denitration catalyst activity.The dealkalize red mud method for preparing catalyst of the present invention, owing to raw material is cheap and easily-available, operating procedure is simple, and equipment requirement is the highest so that it is have good potential application foreground in catalytic denitration field.
The advantage of preparation method of the present invention:
1. method is easy, and equipment is simple, pollutes few, the treatment of wastes with processes of wastes against one another；
2. gained dealkalize red mud specific surface area of catalyst is big, and particle size is little；
3. gained dealkalize red mud catalyst Heat stability is good, denitration catalyst performance is higher.
Accompanying drawing explanation
Fig. 1 is the XRD spectra of the dealkalize red mud catalyst of preparation.
Fig. 2 is the SEM result of the dealkalize red mud catalyst of the present invention.(a) RM, (b) PRM, (c) TRM, (d) PTRM.
Fig. 3 is the NH of the dealkalize red mud catalyst of the present invention3-SCR reactivity worth result.
Detailed description of the invention
Embodiment 1.The preparation of RM catalyst
After untreated original red mud is ground, in Muffle furnace after 550 ° of C roasting 6 h, i.e. obtain original red mud catalyst, be labeled as RM.Its specific surface area and each component content are shown in Table 1, and its XRD determining result is shown in that Fig. 1, SEM result is shown in that Fig. 2, denitration performance measurement result are shown in Fig. 3.
Embodiment 2. The preparation of TRM catalyst
By untreated carry sodium red mud grind after, in Muffle furnace after 550 ° of C roasting 6 h, i.e. obtain carrying sodium red mud catalyst, be labeled as TRM.Its specific surface area and each component content are shown in Table 1, and its XRD determining result is shown in that Fig. 1, SEM result is shown in that Fig. 2, denitration performance measurement result are shown in Fig. 3.
Embodiment 3. The preparation of PRM catalyst
Untreated original red mud and water are mixed into red mud mud, and original red mud is 1:15 with the mass ratio of water, and magnetic agitation 1 h is added dropwise over nitric acid in mixed liquor, and the concentration of nitric acid is 10.3 mol L-1, regulation pH value is 0,50oC stirred in water bath 30 min；Being added dropwise over ammoniacal liquor in mixed liquor after acidifying, the concentration of ammoniacal liquor is 13.2 mol L-1, regulation pH value is 10,50oC stirred in water bath 30 min, stands and is cooled to room temperature；Mud suction filtration is washed to neutrality, by filter cake 120oC is dried 12 h, grinds, in Muffle furnace under air atmosphere 550oC roasting 6 h, i.e. obtains dealkalize original red mud catalyst, is labeled as PRM.Its specific surface area and each component content are shown in Table 1, and its XRD determining result is shown in that Fig. 1, SEM result is shown in that Fig. 2, denitration performance measurement result are shown in Fig. 3.
Embodiment 4. The preparation of PTRM catalyst
With water, the untreated sodium red mud that carries is mixed into red mud mud, and the mass ratio carrying sodium red mud and water is 1:15, and magnetic agitation 1 h is added dropwise over nitric acid in mixed liquor, and the concentration of nitric acid is 10.3 mol L-1, regulation pH value is 0,50oC stirred in water bath 30 min；Being added dropwise over ammoniacal liquor in mixed liquor after acidifying, the concentration of ammoniacal liquor is 13.2 mol L-1, regulation pH value is 10,50oC stirred in water bath 30 min, stands and is cooled to room temperature；Mud suction filtration is washed to neutrality, by filter cake 120oC is dried 12 h, grinds, in Muffle furnace under air atmosphere 550oC roasting 6 h, i.e. obtains dealkalize and carries sodium red mud catalyst, be labeled as PTRM.Its specific surface area and each component content are shown in Table 1, and its XRD determining result is shown in that Fig. 1, SEM result is shown in that Fig. 2, denitration performance measurement result are shown in Fig. 3.
Embodiment 5. The NH of the dealkalize red mud catalyst of the present invention3The performance test of-SCR denitration
This reaction is carried out on micro-catalytic reaction device, and catalyst amount is 0.1 g, in 200 C He atmosphere, catalyst is pre-processed 30 min, is cooled to room temperature, is passed through reaction gas, and reaction gas consists of 500 ppm NO, 500 ppm NH3、5% O2, residual air is helium, and under condition of normal pressure, gas overall flow rate is 100 mL min-1, the temperature of catalytic reaction is 200-500oC.NH with infrared spectrometer detection outlet3And N2O concentration, with NO, NO of nitrogen-oxide analyzer, detection outlet2And NOx concentration, the denitration performance measurement result of catalyst is shown in Fig. 3.

Claims (5)

1. for a dealkalize red mud catalyst for ammine selectivity catalytic reduction nitrous oxides, it is characterized in that: being mainly composed of hematite-type di-iron trioxide, sodium, potassium content are extremely low, dealkalize red mud specific surface area of catalyst is 80-160 m2·g-1, particle size is 1 μm-10 μm, soilless sticking between particle.
2. the method preparing dealkalize red mud catalyst described in claim 1, is characterized in that: untreated red mud and water are mixed into red mud mud, and red mud is 1:15 with the mass ratio of water, magnetic agitation 1 h, being added dropwise over nitric acid in mixed liquor, regulation pH value is 0,50oC stirred in water bath 30 min；Being added dropwise over ammoniacal liquor in mixed liquor after acidifying, regulation pH value is 10,50oC stirred in water bath 30 min, stands and is cooled to room temperature；Mud suction filtration is washed to neutrality, by filter cake 120oC is dried 12 h, grinds, in Muffle furnace under air atmosphere 550oC roasting 6 h, i.e. obtains dealkalize red mud.
3. according to the preparation method described in claim 2, it is characterized in that: the concentration of described nitric acid is 10.3 mol L-1。
4. according to the preparation method described in claim 2, it is characterized in that: the concentration of described ammoniacal liquor is 13.2 mol L-1。
5. the dealkalize red mud catalyst described in claim 1 is as denitrating catalyst application in smoke catalytic denitration.
CN201610145267.9A 2016-03-15 2016-03-15 Preparation method and application of dealkalized red mud Pending CN105771997A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107537492A (en) * 2017-10-24 2018-01-05 中国科学院过程工程研究所 A kind of method that iron system denitrating catalyst is directly prepared by the activation of red mud soda acid
CN108043404A (en) * 2017-12-20 2018-05-18 中国科学院过程工程研究所 Catalyst of removing volatile organic compounds prepared by a kind of red mud and preparation method thereof
CN110479247A (en) * 2019-07-20 2019-11-22 北京化工大学 A kind of red mud based denitration catalyst and its preparation method and application
CN111013589A (en) * 2019-12-23 2020-04-17 山东大学 Red mud catalyst, and forming method and application thereof
CN112316947A (en) * 2020-11-26 2021-02-05 上海应用技术大学 Method for preparing denitration catalyst by red mud in-situ modification
CN116809602A (en) * 2023-06-20 2023-09-29 贵州师范大学 Method for improving specific surface area of red mud by combining food fermentation waste liquid with agriculture and forestry biomass

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107537492A (en) * 2017-10-24 2018-01-05 中国科学院过程工程研究所 A kind of method that iron system denitrating catalyst is directly prepared by the activation of red mud soda acid
CN108043404A (en) * 2017-12-20 2018-05-18 中国科学院过程工程研究所 Catalyst of removing volatile organic compounds prepared by a kind of red mud and preparation method thereof
CN108043404B (en) * 2017-12-20 2021-06-15 中国科学院过程工程研究所 A kind of catalyst for removing volatile organic compounds prepared from red mud and preparation method thereof
CN110479247A (en) * 2019-07-20 2019-11-22 北京化工大学 A kind of red mud based denitration catalyst and its preparation method and application
CN110479247B (en) * 2019-07-20 2021-01-19 北京化工大学 A kind of red mud-based denitration catalyst and its preparation method and application
CN111013589A (en) * 2019-12-23 2020-04-17 山东大学 Red mud catalyst, and forming method and application thereof
CN112316947A (en) * 2020-11-26 2021-02-05 上海应用技术大学 Method for preparing denitration catalyst by red mud in-situ modification
CN116809602A (en) * 2023-06-20 2023-09-29 贵州师范大学 Method for improving specific surface area of red mud by combining food fermentation waste liquid with agriculture and forestry biomass
CN116809602B (en) * 2023-06-20 2025-11-04 贵州师范大学 A method for increasing the specific surface area of red mud by combining food fermentation waste liquid with agricultural and forestry biomass

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Application publication date: 20160720