CN112316947A - Method for preparing denitration catalyst by red mud in-situ modification - Google Patents

Method for preparing denitration catalyst by red mud in-situ modification Download PDF

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Publication number
CN112316947A
CN112316947A CN202011342808.XA CN202011342808A CN112316947A CN 112316947 A CN112316947 A CN 112316947A CN 202011342808 A CN202011342808 A CN 202011342808A CN 112316947 A CN112316947 A CN 112316947A
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red mud
denitration catalyst
preparing
catalyst
situ modification
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周扬
魏旭东
金双玲
许骥文
王友一
陈永正
杭加旺
李俊强
韩奇
王晓瑞
金鸣林
张睿
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Shanghai Institute of Technology
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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
    • B01J23/70—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
    • 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
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
    • B01J37/0027—Powdering
    • B01J37/0036—Grinding
    • 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
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/02—Impregnation, coating or precipitation
    • B01J37/03—Precipitation; Co-precipitation
    • B01J37/031—Precipitation
    • 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
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/06—Washing
    • 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
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/08—Heat treatment

Abstract

The invention discloses a method for preparing a denitration catalyst by red mud in-situ modification, which is characterized by mixing red mud with a hydrochloric acid solution; adding an ammonia solution into the mixture under the condition of stirring to adjust the pH value; the product is washed to neutrality by deionized water, dried and calcined. The method can remove sodium and calcium elements which generate toxic action on the catalyst in the red mud, and simultaneously remoulds a composition structure system in the red mud in an acid-soluble recrystallization mode, so that the red mud composition is modified in situ, and the red mud can be used as an efficient denitration catalyst to realize resource utilization of the red mud.

Description

Method for preparing denitration catalyst by red mud in-situ modification
Technical Field
The invention relates to the field of comprehensive utilization of solid wastes and a nitrogen oxide control technology, in particular to a method for jointly utilizing red mud and denitration.
Background
In recent years, with the improvement of scientific and technical level and the rapid development of economy, large-scale enterprises at home and abroad are briskly started, and the discharge amount of waste materials brought by industrial production, such as tailings, waste gas and waste residues, fly ash and the like, is increasing while the development is achieved. The red mud is pollution waste slag discharged when aluminum oxide is extracted in the aluminum industry, and generally 1.0-2.0 tons of red mud are additionally produced when 1 ton of aluminum oxide is produced on average. In 2010, the yield of Chinese alumina is 3119 ten thousand tons, and in 2016, the yield is 6000 ten thousand tons, and in 2018, the yield of Chinese alumina reaches 7253.1 ten thousand tons all the year round, and in 2019, the yield of Chinese alumina reaches 7247.42 ten thousand tons in 1-12 months. It follows that a very large increase in alumina production is rapidly accompanied by a large red mud pile. The red mud of the alumina plant in China has the following basic properties: the diameter of the granule is 0.088-0.25mm, the specific gravity is 2.7-2.9, the volume weight is 0.8-1.0, and the melting point is 1200-1250 ℃. XRD analysis results show that the red mud contains hematite, goethite, diaspore, quartz, garnet hydrate, calcite, hydrous sodium aluminosilicate, calcium iron ore, calcite and other phases, wherein the content of the hematite is high. The red mud is residue generated after alumina is dissolved by an alkali dissolution method, and is strongly alkaline solid waste. The red mud has the characteristics of fine granularity, complex composition, radioactivity and strong alkalinity, is very easy to cause a series of environmental problems, and the risk of red mud dam break can be caused by the red mud treatment in a mode of piling up the red mud in a large area. Meanwhile, the red mud contains rich iron, aluminum, titanium, sodium, calcium, silicon and a plurality of rare earth elements, and is a precious secondary resource. Therefore, how to recycle effective resources in the red mud and reduce the red mud stacking amount is a research hotspot in recent years.
In recent years, the total amount of nitrogen oxide emission in China is increasing, which causes environmental and ecological deterioration, so that the problem of controlling the emission is urgently needed to be solved. The harm of nitrogen oxide mainly refers to NO and NO2、N2The substances such as O and the like mainly cause pollution and harm to the environment, particularly the harm of NO. The nitrogen oxides can not only form acid rain to destroy the ecological environment, but also cause the destruction of the atmospheric layer, generate photochemical smog in the reaction of hydrocarbon compounds and pollute the environment. NO combines with hemoglobin in human body to induce insufficient supply of nutrients to human body and make breathing difficult. NO2Can cause respiratory diseases of human body, N2O also destroys the ozone layer. NOxThe emission control technology covers all links of the combustion process, including fuel control, control of the combustion process and control of the exhaust emission. The fuel control technology is mainly used for carrying out secondary processing on the fuel to reduce the generation of nitrogen oxides; the combustion process is controlled mainly by developing an efficient burner according to the combustion process, improving the combustion condition in the furnace and controlling the emission of nitrogen oxides. The control technology has low cost and easy realization of industrial application, but can reduce NO by 50 percent at the highest energyxThe emission needs to be controlled by tail gas if higher environmental requirements are met. The tail gas denitration control technology comprises two types of dry denitration control and wet denitration control technologies, wherein the wet denitration technology mainly comprisesThe method includes a direct tail gas absorption method, an oxidation tail gas absorption method, a reduction tail gas absorption method and the like, and the dry denitration control technology includes an adsorption technology, a catalytic elimination technology, a plasma elimination technology and the like. The dry flue gas removal technology is the most studied elimination technology at present due to low investment cost and high removal efficiency. The technology which is well researched and part of the technologies which are achieved industrially at present are catalytic elimination technologies (including Selective Catalytic Reduction (SCR) technology and selective non-catalytic reduction (SNCR) technology), and other denitration technologies are still researched and are not applied to actual production.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the prior technical problem that the activity of the denitration active ingredients of the red mud is not high.
In order to solve the technical problems, the technical scheme provided by the invention is as follows: a method for preparing a denitration catalyst by red mud in-situ modification is characterized by comprising the following steps:
step 1): mixing the red mud with a hydrochloric acid solution;
step 2): adding an ammonia solution into the mixture obtained in the step 1) under the stirring condition to adjust the pH value;
step 3): washing the product obtained in the step 2) to be neutral by deionized water, drying and calcining.
Preferably, the mass ratio of the red mud to the hydrochloric acid solution in the step 1) is 1: 23-28, wherein the mass ratio of the red mud to HCl in the hydrochloric acid solution is 1: 1-3.
Preferably, the mixing in step 1) is specifically: heating to 80 deg.C, stirring for 60-120min, and cooling to room temperature.
Preferably, the pH value in the step 2) is adjusted to 9-11.
Preferably, the stirring time in the step 2) is 60-120 min.
Preferably, the calcining temperature in the step 3) is 300-800 ℃ and the time is 200-300 min.
Preferably, the product obtained in step 3) is cooled to room temperature and then ground.
More preferably, the product is ground to 40-80 mesh.
The invention has the beneficial effects that: the method can remove sodium and calcium elements which generate toxic action on the catalyst in the red mud, and simultaneously remoulds a composition structure system in the red mud in an acid-soluble recrystallization mode, so that the red mud composition is modified in situ, the activity of the red mud catalyst is improved, the catalyst can be used as an efficient denitration catalyst, and the resource utilization of the solid waste red mud is facilitated.
Drawings
Fig. 1 is a process flow diagram of a method for preparing a denitration catalyst by in-situ modification of red mud provided by the invention;
FIG. 2 is an XRD pattern of red mud catalysts prepared at different acid concentrations for samples 1-5;
FIG. 3 is a graph of the sulfur resistance and water resistance of the catalyst of sample 5;
fig. 4 is a graph of the lifetime of the catalyst of sample 5.
Detailed Description
In order to make the invention more comprehensible, preferred embodiments are described in detail below with reference to the accompanying drawings.
Comparative example 1
Pretreating a red mud raw material: firstly, primary grinding and crushing of original red mud blocks, drying for 600min at 105 ℃ to fully remove water, and then grinding the red mud raw materials to below 200 meshes by using a planetary ball mill for later use.
Preparing a red mud raw material catalyst: directly putting the pretreated red mud raw material into a tubular furnace, heating to 500 ℃ at the heating rate of 10 ℃/min, calcining for 240min, cooling to room temperature, and grinding to 40-80 meshes.
And (3) putting the dried modified red mud into a tubular furnace, heating to 500 ℃ at a heating rate of 10 ℃/min, calcining for 240min, cooling to room temperature, and grinding (40-80 meshes) to obtain a modified red mud catalyst, wherein the label is sample 1.
Example 1
(1) Pickling red mud, namely firstly weighing 3g of pretreated red mud according to a solid-liquid mass ratio of 1: 23, adding a dilute hydrochloric acid solution, wherein the mass ratio of the red mud to the HCl is 1: 1, heating to 80 ℃ and stirring for 90 min. And cooling the acidified red mud to room temperature after the stirring is stopped.
(2) And (3) alkaline precipitation for remodeling the structure, then dropwise adding an ammonia water solution with the mass fraction of 25% into the acidified red mud solution, adjusting the pH value of the solution to 9, and stirring on a magnetic stirring instrument for 90 min.
(3) Removing impurities, washing the red mud solution subjected to alkali precipitation with distilled water, and performing centrifugal treatment for 5-8 times until the modified red mud precipitate is neutral. The precipitate was then placed in an oven at 105 ℃ for 640 min.
(4) And (3) high-temperature calcination, namely putting the dried modified red mud into a tubular furnace, heating to 500 ℃ at the heating rate of 10 ℃/min, calcining for 240min, cooling to room temperature, and grinding (40-80 meshes) to obtain the modified red mud catalyst, wherein the label is sample 2.
Example 2
(1) Pickling red mud, namely firstly weighing 3g of pretreated red mud according to a solid-liquid mass ratio of 1: 24, adding a dilute hydrochloric acid solution, wherein the mass ratio of the red mud to the HCl is 1:2, heating to 80 ℃ and stirring for 90 min. And cooling the acidified red mud to room temperature after the stirring is stopped.
(2) And (3) alkaline precipitation for remodeling the structure, then dropwise adding an ammonia water solution with the mass fraction of 25% into the acidified red mud solution, adjusting the pH value of the solution to 10, and stirring on a magnetic stirring instrument for 90 min.
(3) Removing impurities, washing the red mud solution subjected to alkali precipitation with distilled water, and performing centrifugal treatment for 5-8 times until the modified red mud precipitate is neutral. The precipitate was then placed in an oven at 105 ℃ for 640 min.
(4) And (3) high-temperature calcination, namely putting the dried modified red mud into a tubular furnace, heating to 500 ℃ at the heating rate of 10 ℃/min, calcining for 240min, cooling to room temperature, and grinding (40-80 meshes) to obtain the modified red mud catalyst, wherein the label is sample 3.
Example 3
(1) Pickling red mud, namely firstly weighing 3g of pretreated red mud according to a solid-liquid mass ratio of 1: 25 adding a dilute hydrochloric acid solution, wherein the mass ratio of the red mud to the HCl is 1:2, heating to 80 ℃, and stirring for 90 min. And cooling the acidified red mud to room temperature after the stirring is stopped.
(2) And (3) alkaline precipitation for remodeling the structure, then dropwise adding an ammonia water solution with the mass fraction of 25% into the acidified red mud solution, adjusting the pH value of the solution to 11, and stirring on a magnetic stirring instrument for 90 min.
(3) Removing impurities, washing the red mud solution subjected to alkali precipitation with distilled water, and performing centrifugal treatment for 5-8 times until the modified red mud precipitate is neutral. The precipitate was then placed in an oven at 105 ℃ for 640 min.
(4) And (3) high-temperature calcination, namely putting the dried modified red mud into a tubular furnace, heating to 500 ℃ at the heating rate of 10 ℃/min, calcining for 240min, cooling to room temperature, and grinding (40-80 meshes) to obtain a modified red mud catalyst, wherein the label is sample 4.
Example 4
(1) Pickling red mud, namely firstly weighing 3g of pretreated red mud according to a solid-liquid mass ratio of 1: 28 adding a dilute hydrochloric acid solution, wherein the mass ratio of the red mud to the HCl is 1:3, heating to 80 ℃, and stirring for 90 min. And cooling the acidified red mud to room temperature after the stirring is stopped.
(2) And (3) alkaline precipitation for remodeling the structure, then dropwise adding an ammonia water solution with the mass fraction of 25% into the acidified red mud solution, adjusting the pH value of the solution to 9, and stirring on a magnetic stirring instrument for 90 min.
(3) Removing impurities, washing the red mud solution subjected to alkali precipitation with distilled water, and performing centrifugal treatment for 5-8 times until the modified red mud precipitate is neutral. The precipitate was then placed in an oven at 105 ℃ for 640 min.
(4) And (3) high-temperature calcination, namely putting the dried modified red mud into a tubular furnace, heating to 500 ℃ at the heating rate of 10 ℃/min, calcining for 240min, cooling to room temperature, and grinding (40-80 meshes) to obtain the modified red mud catalyst, wherein the label is sample 5.
The raw red mud was further characterized and analyzed, and the results are shown in table 1.
TABLE 1
Element(s) Fe Al Ti Si Na Ca
Mass content 16.25％ 9.7％ 3.24％ 5.96％ 4.66％ 13.01％
As shown in Table 1, the mutual verification of XRD and ICP chemical content analysis shows that the red mud contains a large amount of Fe element mainly including Fe2O3Exist in the form of (1). FIG. 2 is a diffraction pattern of the catalysts of samples 1-5. The phase of sample 1 is relatively complex, multiple mineral components are in intergrowth with each other, and main phases include hematite, corundum, perovskite, zeolite and calcite. The presence of the sodium calcium compound is a major cause of the extremely poor denitration activity of the catalyst of example 1. The XRD patterns of the catalysts of the samples 2-5 can find that the diffraction peak of the calcium sodium phase disappears, which shows that the sodium calcium element in the red mud can be effectively removed by a proper acid-washing and alkali-precipitation mode. While removing the Na-Ca element, the Fe content in the catalyst of samples 2-5 can be found by continuously increasing the acid washing concentration2O3Diffraction peak intensity becomes lowThis indicates that the relatively high concentration of acid wash and alkali re-precipitation conditions may improve the internal structure of the red mud. From fig. 3, it can be seen that the catalyst of sample 5 has excellent sulfur-resistant and water-resistant properties in practical industrial applications, which is often an important indicator. The sulfur-resistant and water-resistant test research is carried out on the catalyst of the sample 5, and SO is introduced during the test2Concentration of 100ppm, 5 vol.% H2O, the selected SCR reaction temperature is 320 ℃, and other reaction conditions are consistent with the SCR activity test shown above. The catalyst is introduced with SO2And before water, the good and stable denitration activity is maintained; in the presence of SO2And H2After O, the catalyst started to decrease in NO conversion, mainly due to the steam and SO fed in2Will react with adsorbed NH3And NO competitively adsorbs on the surface of the catalyst, so that the SCR reaction is influenced. In the presence of SO2And after 60min of water, the activity of the catalyst obviously has a descending trend, but the catalyst of the sample 5 is introduced with SO2And the NO conversion rate can be kept above 80% after 6h of water. In the cutting off of SO2+H2At 120min after O, the catalyst of sample 5 can be restored from 80% to the original 100% activity. This demonstrates that the red mud catalyst of sample 5 has excellent sulfur and water resistance. Fig. 4 is a stability test of the catalyst of sample 5, and the SCR activity of the catalyst can be maintained at 100% within 40 hours under the SCR test condition of 320 ℃, which shows that the red mud catalyst treated by modification has excellent stability.

Claims (8)

1. A method for preparing a denitration catalyst by red mud in-situ modification is characterized by comprising the following steps:
step 1): mixing the red mud with a hydrochloric acid solution;
step 2): adding an ammonia solution into the mixture obtained in the step 1) under the stirring condition to adjust the pH value;
step 3): washing the product obtained in the step 2) to be neutral by deionized water, drying and calcining.
2. The method for preparing the denitration catalyst through in-situ modification of the red mud of claim 1, wherein the mass ratio of the red mud to the hydrochloric acid solution in the step 1) is 1: 23-28, wherein the mass ratio of the red mud to HCl in the hydrochloric acid solution is 1: 1-3.
3. The method for preparing the denitration catalyst through in-situ modification of the red mud of claim 1, wherein the mixing in the step 1) is specifically as follows: heating to 80 deg.C, stirring for 60-120min, and cooling to room temperature.
4. The method for preparing the denitration catalyst through in-situ modification of the red mud of claim 1, wherein the pH value in the step 2) is adjusted to 9-11.
5. The method for preparing the denitration catalyst through in-situ modification of the red mud as claimed in claim 1, wherein the stirring time in the step 2) is 60-120 min.
6. The method for preparing the denitration catalyst through in-situ modification of the red mud as claimed in claim 1, wherein the calcination temperature in the step 3) is 300-800 ℃ and the calcination time is 200-300 min.
7. The method for preparing the denitration catalyst through in-situ modification of the red mud of claim 1, wherein the product obtained in the step 3) is cooled to room temperature and then ground.
8. The method for preparing the denitration catalyst by in-situ modification of the red mud as claimed in claim 7, wherein the product is ground to 40-80 mesh.
CN202011342808.XA 2020-11-26 2020-11-26 Method for preparing denitration catalyst by red mud in-situ modification Pending CN112316947A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113877591A (en) * 2021-09-30 2022-01-04 山东省科学院能源研究所 Preparation method of acid-treated iron mud denitration catalyst
CN113877621A (en) * 2021-11-01 2022-01-04 武汉工程大学 Red mud modified carbon nitride nano material and preparation method and application thereof

Citations (4)

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Publication number Priority date Publication date Assignee Title
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CN105771997A (en) * 2016-03-15 2016-07-20 济南大学 Preparation method and application of dealkalized red mud
CN106345473A (en) * 2016-08-22 2017-01-25 山东大学 Denitration catalyst material, and preparation method and application thereof
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

Patent Citations (4)

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Publication number Priority date Publication date Assignee Title
GB1398831A (en) * 1972-05-12 1975-06-25 Shin Jen Shiad Activated red mud and its preparing method
CN105771997A (en) * 2016-03-15 2016-07-20 济南大学 Preparation method and application of dealkalized red mud
CN106345473A (en) * 2016-08-22 2017-01-25 山东大学 Denitration catalyst material, and preparation method and application thereof
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

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Title
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113877591A (en) * 2021-09-30 2022-01-04 山东省科学院能源研究所 Preparation method of acid-treated iron mud denitration catalyst
CN113877621A (en) * 2021-11-01 2022-01-04 武汉工程大学 Red mud modified carbon nitride nano material and preparation method and application thereof

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