CN110639540A - Preparation method of low-temperature low-pressure-drop denitration catalyst - Google Patents

Preparation method of low-temperature low-pressure-drop denitration catalyst Download PDF

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Publication number
CN110639540A
CN110639540A CN201910833907.9A CN201910833907A CN110639540A CN 110639540 A CN110639540 A CN 110639540A CN 201910833907 A CN201910833907 A CN 201910833907A CN 110639540 A CN110639540 A CN 110639540A
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catalyst
low
drop
preparing
pressure
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谢宗丽
Ng·俊谦
李玉亮
李文霞
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Hebei Wei Wo Environmental Project Science And Technology Ltd
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Hebei Wei Wo Environmental Project Science And Technology Ltd
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Priority to CN201910833907.9A priority Critical patent/CN110639540A/en
Publication of CN110639540A publication Critical patent/CN110639540A/en
Priority claimed from EP20861813.2A external-priority patent/EP4025342A1/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/76Catalysts 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
    • B01J23/84Catalysts 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 arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • B01J23/889Manganese, technetium or rhenium
    • B01J23/8892Manganese
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation 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
    • B01D53/34Chemical or biological purification of waste gases
    • B01D53/74General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/86Catalytic processes
    • B01D53/8621Removing nitrogen compounds
    • B01D53/8625Nitrogen oxides
    • B01D53/8628Processes characterised by a specific catalyst
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/002Mixed oxides other than spinels, e.g. perovskite
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00Catalysts, in general, characterised by their form or physical properties
    • B01J35/02Solids
    • B01J35/026Form of the solid particles

Abstract

The invention provides a preparation method of a low-temperature low-pressure-drop denitration catalyst, which comprises the following steps: preparing a raw material, namely a metal nitrate solution and an alkali solution, wherein the metal nitrate solution contains equal amount of iron and manganese, and the alkali solution consists of an ammonia solution, an ammonia mixture and a mixed solution of ammonium bicarbonate or only an ammonium bicarbonate solution; step two, the preparation of the powder catalyst comprises the following steps: pumping the prepared precursor into a high-power ultrasonic reactor at a high-to-low flow rate, and enabling the liquid to form a slurry state; washing the collected slurry in a centrifuge or a rotary dryer for three times with water or once with acetone to form a precipitate; the precipitate formed was further dried at room temperature for more than 24 hours and then coarsely ground into broken pieces; placing the semi-finished product which is coarsely ground into broken blocks in a roasting furnace for roasting; grinding the particle size of the calcined catalyst by a ring mill to finally form a powdery catalyst; and step three, coating a catalyst.

Description

Preparation method of low-temperature low-pressure-drop denitration catalyst
Technical Field
The invention relates to the technical field of catalyst preparation, in particular to a preparation method of a low-temperature low-pressure-drop denitration catalyst.
Background
Nitrogen oxides (NOx, x ═ 1,2) as major atmospheric pollutants are causing a range of environmental problems such as photochemical smog, acid rain, ozone depletion, and particulate contamination. It is well known that 90% of the nox emissions are from combustion, both stationary and mobile sources. In stationary source fuel combustion, nitrogen oxides are mainly derived from power stations, industrial heaters and thermal power plants.
NH3SCR denitration technology is considered to be the most effective and widely used technology for reducing nitrogen oxide emissions from stationary sources. The catalyst is the key of denitration by an ammonia method or a urea method. Currently, it is used industrially for NH3Industrial catalysts for SCR, mainly V on titanium dioxide2O5Catalyst, in WO3(MoO3)/TiO2As the catalyst, the vanadium-tungsten-titanium has higher temperature requirement, the optimal operation temperature is 350-400 ℃, and V can be obtained only in the temperature range2O5-WO3/TiO2High conversion of (b). Although vanadium catalysts have entered the power plant and diesel vehicle markets, they are SO-rich2Oxidation to SO3The activity is high, the activity and the selectivity are rapidly reduced above 550 ℃, and vanadium has toxicity to the ecological environment, so that the application of the vanadium catalyst still has some problems. Furthermore, the commercial V2O 5-WO 3/TiO2 catalyst must be installed upstream of the particle collector and flue gas desulfurization to meet the optimum operating temperature of 350 ℃ and 420 ℃. Therefore, researchers in academia and industry continue to develop new low temperature catalysts to facilitate catalysts capable of temperatures around and below 200 ℃. Therefore, the SCR device can effectively remove the nitrogen oxide in a wider temperature range after being arranged in an electric dust removal desulfurizer of a power plant, thereby realizing the control of the nitrogen oxide. Because the desulfurization and dust removal device is arranged behind the denitration device, substances such as sulfur dioxide, smoke dust and the like in the flue greatly reduce the denitration efficiency and stability of the vanadium-tungsten-titanium catalyst in the denitration process, if the denitration device is arranged behind the desulfurization and dust removal device, the problem can be solved,however, the temperature of the flue gas after desulfurization and dust removal is about 150 ℃, and the working temperature of the vanadium-tungsten-titanium catalyst cannot be reached, so that the flue gas needs to be reheated, the energy consumption is increased, and the operation cost is increased.
Considering the flue gas composition and the ambient temperature to the (NH) in the flue gas4)2SO4、NH4NO3And N2Because of the influence of O generation, it is necessary to develop a low-temperature SCR catalyst having good activity, high selectivity, high stability, and a wide operating temperature range by using a novel carrier. Such a catalyst may be placed downstream of the electrostatic precipitator and even downstream of the desulfurizer, at temperatures below 200 degrees celsius. However, such low temperature catalysts have rarely been demonstrated for removing nitrogen oxides from power plant flue gases. Manganese oxide (MnO)2) Is the main active ingredient for the denitration of the ammonium nitrate-SCR method at low temperature. The techniques for preparing low temperature catalysts reported at present are extrusion (extrusion), hydrothermal and thermal decomposition, simple precipitation and coprecipitation, wet impregnation, ion exchange of support precursors and sol-gel. In most cases, V2O5 and a noble metal are used as key active ingredients of the denitration catalyst, thereby reducing cost effectiveness. Other problems with the above preparation techniques are due to the complexity of the scale-up process, some techniques can only be used for batch reactions (e.g. hydrothermal reactions), some can produce hazardous and unfavorable by-products (e.g. thermal decomposition using citric acid to produce harmful nitrogen oxide fumes, sol-gel methods require the use of hazardous and expensive solvents).
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a method for preparing a low-temperature low-pressure-drop denitration catalyst of a manganese and iron blended oxide MnOx/FeOx-based catalyst, which is non-toxic and low in cost, so that the obtained catalyst can show excellent catalytic activity in the temperature range of 100-200 ℃.
The invention aims to provide a method for preparing a low-temperature low-pressure-drop denitration catalyst, which comprises the following steps of:
preparing a raw material, wherein the raw material is a catalyst precursor and consists of two components, namely a metal nitrate solution and an alkali solution, the metal nitrate solution contains equal amount of iron and manganese, and the alkali solution consists of a mixed solution of an ammonia solution, an ammonia mixture and ammonium bicarbonate or only consists of an ammonium bicarbonate solution;
and step two, preparing the powder catalyst.
Preferably, the metal nitrate solution further contains an additive, and in this embodiment, the additive is deionized water.
Preferably, the second step includes:
step 21, pumping the prepared precursor into a high-power ultrasonic reactor at a high-to-low flow rate, wherein when the precursor is applied to the precursor in a continuous-flow stainless steel shell reaction tank, liquid forms a slurry state;
step 22, washing the collected slurry in a centrifuge or a rotary dryer for three times by using water or once by using acetone to form precipitates, and discharging waste liquid after washing in the washing process;
step 23, further drying the formed precipitate at room temperature for more than 24 hours, and then coarsely grinding into broken blocks;
step 24, placing the semi-finished product which is coarsely ground into crushed blocks in a roasting furnace for roasting;
and 25, grinding the particle size of the calcined catalyst by a ring mill to finally form a powdery catalyst.
Preferably, the flow rate of step 21 is from 50ml/s to 200ml/s, the power of the high power ultrasonic reactor is 500 watts, and the frequency is 20 kilohertz.
Preferably, said washing of said step 22 is preceded by a rest time of 5 hours.
Preferably, said step 24 comprises calcining the semi-finished catalyst in a programmable furnace at a ramp rate of 10 ℃/min at 500 ℃ for 3 h.
Preferably, the milling time of step 25 is about 10 minutes, milling to submicron <2 μm.
Preferably, the method further comprises a third step of coating the catalyst, wherein the third step comprises the following steps:
step 31, grinding the catalyst powder obtained in the step two;
step 32, wet grinding the ground catalyst powder, and adding an additive in the wet grinding process;
step 33, coating on the catalyst carrier;
step 34, drying the catalyst carrier coated with the catalyst at room temperature;
and step 35, placing the dried catalyst carrier in a roasting furnace for roasting to obtain the low-pressure-drop supported catalyst.
Preferably, the additive of step 32 is PTFE.
Preferably, the catalyst support of step 33 is a honeycomb ceramic.
The invention has the beneficial effects that:
(1) iron oxide and manganese oxide based, non-toxic, relatively inexpensive because they can be supplied in large quantities.
(2) Since the manufacturing process can be semi-continuous to fully continuous, it is easy to mass produce.
(3) In the production process of the catalyst, more effective low-temperature denitration catalyst performances can be obtained due to the enhanced reactant dispersibility and the shearing action of high-power ultrasound on catalyst particles.
(4) The catalyst is loaded on the honeycomb ceramic carrier, has the advantage of low pressure drop, and has no influence on the upstream and downstream processes.
Drawings
FIG. 1 is a flow diagram of a method of making a catalyst according to an embodiment of the invention.
Detailed Description
The following detailed description of the embodiments of the present invention is provided with reference to the accompanying drawings, but the present invention is not limited thereto.
The metal oxide catalyst has high low-temperature denitration spark and low price, and transition metal oxides such as MnOx, CuOx, FeOx, CeOx, ZrOx and the like have good low-temperature denitration performance. Metal oxide catalysts are subdivided into monometallic oxide catalysts and corresponding metal oxide catalysts. The low-temperature denitration performance of the single metal oxide catalyst is general and is unstable at high temperature, and the composite oxide has a determined composition and structure, and various metal ions in the structure can be adjusted. The oxides of Fe and Mn show better catalytic performance under the condition of low temperature, and the ammonia selective denitration reaction mechanism is as follows: the surface of the metal oxide catalyst is provided with a plurality of active sites, NO is firstly adsorbed on the active sites and then decomposed into nitrogen and oxygen atoms, and finally nitrogen and oxygen are formed and desorbed to release the active sites.
Example 1:
referring to fig. 1, the method for manufacturing the low-temperature low-pressure-drop denitration catalyst of the embodiment only comprises the first two steps, namely:
preparing a raw material, wherein the raw material is a catalyst precursor and consists of a metal nitrate solution and an alkali solution, the metal nitrate solution can contain equal amount of iron and manganese, and the alkali solution consists of an ammonia solution, an ammonia mixture and an ammonium bicarbonate mixed solution or only consists of an ammonium bicarbonate solution; in this example, the ammonia solution is ammonia water. The metal nitrate solution also contains an additive, and in this embodiment, the additive is deionized water.
Step two, preparing a powder catalyst, wherein the step two comprises the following steps:
step 21, pumping the prepared precursor into a high-power ultrasonic reactor with the power of 500 watts and 20 kilohertz at the flow rate of 50ml/s to 200ml/s, wherein when the high-power ultrasonic reactor is applied to the precursor in a continuous flow reaction tank (stainless steel shell), the low-frequency and high-power ultrasonic waves can generate strong cavitation, the cavitation effect can greatly enhance the dispersion and uniform reaction and remove liquid, so that the processing consistency is improved, and the slurry state is formed, and the current setting can process the precursor with the power of 250 plus 2000 ml/min;
step 22, washing the collected slurry in a centrifuge or a rotary dryer for three times by using water or once by using acetone to form a precipitate, standing for 5 hours before washing, and discharging waste liquid after washing in the washing process;
step 23, further drying the formed precipitate at room temperature for more than 24 hours, and then coarsely grinding into broken blocks;
step 24, placing the semi-finished product which is coarsely ground into the crushed blocks in a roasting furnace for roasting, and roasting the semi-finished product catalyst in a programmable furnace at the temperature rise rate of 10 ℃/min for 3 hours at 500 ℃;
and step 25, grinding the particle size of the calcined catalyst by a ring mill for about 10 minutes to obtain a particle size with the particle size of submicron <2 μm, and finally forming the powdery catalyst.
Example 2:
referring to fig. 1, a method of making a low temperature, low pressure drop, denitration catalyst includes the complete three steps of the process of fig. 1:
preparing a raw material, wherein the raw material is a catalyst precursor and consists of a metal nitrate solution and an alkali solution, the metal nitrate solution can contain equal amount of iron and manganese, and the alkali solution consists of an ammonia solution, an ammonia mixture and an ammonium bicarbonate mixed solution or only consists of an ammonium bicarbonate solution; in this example, the ammonia solution is ammonia water. The metal nitrate solution also contains an additive, and in this embodiment, the additive is deionized water.
Step two, preparing the powder catalyst, comprising:
step 21, pumping the prepared precursor into a high-power ultrasonic reactor with the power of 500 watts and 20 kilohertz at the flow rate of 50ml/s to 200ml/s, wherein when the high-power ultrasonic reactor is applied to the precursor in a continuous flow reaction tank (stainless steel shell), the low-frequency and high-power ultrasonic waves can generate strong cavitation, the cavitation effect can greatly enhance the dispersion and uniform reaction and remove liquid, so that the processing consistency is improved, and the slurry state is formed, and the current setting can process the precursor with the power of 250 plus 2000 ml/min;
step 22, washing the collected slurry in a centrifuge or a rotary dryer for three times by using water or once by using acetone to form a precipitate, standing for 5 hours before washing, and discharging waste liquid after washing in the washing process;
step 23, further drying the formed precipitate at room temperature for more than 24 hours, and then coarsely grinding into broken blocks;
step 24, placing the semi-finished product which is coarsely ground into the crushed blocks in a roasting furnace for roasting, and roasting the semi-finished product catalyst in a programmable furnace at the temperature rise rate of 10 ℃/min for 3 hours at 500 ℃;
and step 25, grinding the particle size of the calcined catalyst by a ring mill for about 10 minutes to obtain a particle size with the particle size of submicron <2 μm, and finally forming the powdery catalyst.
Step three, coating a catalyst, comprising:
step 31, grinding the catalyst powder obtained in the step two;
step 32, wet-grinding the ground catalyst powder, adding an additive in the wet-grinding process, wherein the additive is PTFE in this embodiment, and certainly, other additives which are helpful for wet-grinding and improving the performance of the catalyst can be added by those skilled in the art according to the needs;
step 33, coating is performed on the catalyst carrier, which is honeycomb ceramic, although other carriers can be selected by those skilled in the art as needed. Other vectors include:
1. molecular sieve catalyst: the molecular sieve is used as a catalyst carrier due to the unique pore channel structure, the large specific surface area and the abundant surface acid sites, the large specific surface agent can enable active components to be more uniformly distributed on the carrier, NH3 adsorption and activation are promoted, and the molecular sieve is applied to the aspect of denitration catalysts due to the characteristics of high stability, wide temperature window and the like. The denitration efficiency of the molecular sieve catalyst loading bimetallic Fe and Mn on the SBA-15 type molecular sieve is superior to that of single metal, the dispersion of Mn element on the surface of the molecular sieve is promoted due to the introduction of Fe element, and the Mn element increases acid sites on the surface of the molecular sieve.
2. Activated carbon: the activated carbon is widely used as a denitration catalyst carrier due to its huge specific surface area, strong adsorption performance and chemical stability. The nitric acid is used for pretreating the activated carbon to increase the acid sites of the activated carbon, so that the catalytic performance of the catalyst is further improved.
3. Titanium dioxide: the titanium dioxide of the titanium removal ore type is higher than a surface agent, sulfate generated in the presence of sulfur dioxide is not easy to deposit on the surface of the titanium dioxide, so that active ingredients of the catalyst are protected from being covered, the sulfur resistance of the catalyst is enhanced, and the transition metal oxide is loaded on a sulfur dioxide carrier to research the catalytic activity of the catalyst, so that the manganese oxide-loaded catalyst has the best low-temperature denitration effect, and Mn is loaded on the titanium dioxide carrier through an impregnation method.
Step 34, drying the catalyst carrier coated with the catalyst at room temperature;
and step 35, placing the dried catalyst carrier in a roasting furnace for roasting to obtain the low-pressure-drop supported catalyst.
The technical solutions provided by the embodiments of the present invention are described in detail above, and the principles and embodiments of the present invention are explained herein by using specific examples, and the descriptions of the embodiments are only used to help understanding the principles of the embodiments of the present invention; meanwhile, the detailed description and the application scope of the embodiments according to the present invention may be changed by those skilled in the art, and in summary, the present disclosure should not be construed as limiting the present invention.

Claims (10)

1. A method for preparing a low-temperature low-pressure-drop denitration catalyst is characterized by comprising the following steps of:
preparing a raw material, wherein the raw material is a catalyst precursor and consists of two components, namely a metal nitrate solution and an alkali solution, the metal nitrate solution contains equal amount of iron and manganese, and the alkali solution consists of a mixed solution of an ammonia solution, an ammonia mixture and ammonium bicarbonate or only consists of an ammonium bicarbonate solution;
and step two, preparing the powder catalyst.
2. The method for preparing the low-temperature low-pressure-drop denitration catalyst as claimed in claim 1, wherein the method comprises the following steps: deionized water is also added to the metal nitrate solution as an additive.
3. The method for preparing the low-temperature low-pressure-drop denitration catalyst as claimed in claim 1, wherein the second step comprises:
step 21, pumping the prepared precursor into a high-power ultrasonic reactor at a high-to-low flow rate, wherein when the precursor is applied to the precursor in a continuous-flow stainless steel shell reaction tank, liquid forms a slurry state;
step 22, washing the collected slurry in a centrifuge or a rotary dryer for three times by using water or once by using acetone to form precipitates, and discharging waste liquid after washing in the washing process;
step 23, further drying the formed precipitate at room temperature for more than 24 hours, and then coarsely grinding into broken blocks;
step 24, placing the semi-finished product which is coarsely ground into crushed blocks in a roasting furnace for roasting;
and 25, grinding the particle size of the calcined catalyst by a ring mill to finally form a powdery catalyst.
4. The method for preparing the low-temperature low-pressure-drop denitration catalyst as claimed in claim 3, wherein the method comprises the following steps: the flow rate of step 21 is from 50ml/s to 200ml/s, the power of the high power ultrasonic reactor is 500 watts, and the frequency is 20 kilohertz.
5. The method for preparing the low-temperature low-pressure-drop denitration catalyst as claimed in claim 3, wherein the method comprises the following steps: the washing of the step 22 requires a standing time of 5 hours.
6. The method for preparing the low-temperature low-pressure-drop denitration catalyst as claimed in claim 3, wherein the method comprises the following steps: said step 24 comprises calcining the semi-finished catalyst in a programmable furnace at a ramp rate of 10 ℃/min for 3 hours at 500 ℃.
7. The method for preparing the low-temperature low-pressure-drop denitration catalyst as claimed in claim 3, wherein the method comprises the following steps: the milling time of step 25 is about 10 minutes, milling to submicron <2 μm.
8. The method for preparing the low-temperature low-pressure-drop denitration catalyst as claimed in claim 1, wherein the method comprises the following steps: the method also comprises a third step of coating a catalyst, wherein the third step comprises the following steps:
step 31, grinding the catalyst powder obtained in the step two;
step 32, wet grinding the ground catalyst powder, and adding an additive in the wet grinding process;
step 33, coating on the catalyst carrier;
step 34, drying the catalyst carrier coated with the catalyst at room temperature;
and step 35, placing the dried catalyst carrier in a roasting furnace for roasting to obtain the low-pressure-drop supported catalyst.
9. The method for preparing the low-temperature low-pressure-drop denitration catalyst as claimed in claim 8, wherein the method comprises the following steps: the additive of step 32 is PTFE.
10. The method for preparing the low-temperature low-pressure-drop denitration catalyst as claimed in claim 8, wherein the method comprises the following steps: the catalyst support of step 33 is a honeycomb ceramic.
CN201910833907.9A 2019-09-04 2019-09-04 Preparation method of low-temperature low-pressure-drop denitration catalyst Pending CN110639540A (en)

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CN201910833907.9A CN110639540A (en) 2019-09-04 2019-09-04 Preparation method of low-temperature low-pressure-drop denitration catalyst
EP20861813.2A EP4025342A1 (en) 2019-09-04 2020-09-04 Low-temperature denitration catalyst
US17/640,581 US20220323904A1 (en) 2019-09-04 2020-09-04 Low-temperature denitration catalyst
PCT/CN2020/113505 WO2021043267A1 (en) 2019-09-04 2020-09-04 Low-temperature denitration catalyst
AU2020343826A AU2020343826A1 (en) 2019-09-04 2020-09-04 Low-temperature denitration catalyst

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Application publication date: 20200103