CN105126824A - Low-temperature manganese-based composite oxide denitration catalyst and preparation method thereof - Google Patents
Low-temperature manganese-based composite oxide denitration catalyst and preparation method thereof Download PDFInfo
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Abstract
The invention provides a low-temperature manganese-based composite oxide denitration catalyst; the denitration catalyst is used for selective catalytic reduction reaction of oxynitrides in boiler flue gas under a condition of low temperatures, so the denitration catalyst can be arranged after a dust remover and a desulfurization device, and influence of fly ash and sulfur content in the flue gas is effectively reduced. The denitration catalyst is characterized by comprising nanoscale titanium dioxide as a carrier, a manganese cerium vanadium compound oxide loaded on the nanoscale titanium dioxide and used as an active component, and a partial reinforcing agent component, wherein the mass ratio of all the components is titanium dioxide:Mn salt:Ce salt:V salt:reinforcing agent=1:(0.625-1.563):(0.05-2.71):(0.001-0.029):(0.05-0.3). The invention also provides a preparation method of the low-temperature manganese-based composite oxide denitration catalyst.
Description
Technical field
The present invention relates to the technical field of catalyst and manufacture thereof, particularly relate to a kind of low temperature manganese system complex oxide denitrating catalyst and preparation method thereof.
Background technology
Selective catalytic reduction (SCR) gas denitrifying technology is widely used in coal-burning power plant of China as the most effective method of the control coal-burning power plant discharged nitrous oxides of generally acknowledging at present.According to statistics, SCR accounts for 90% of the denitrating flue gas pool-size that puts into operation.
The technological core of SCR flue-gas denitration process is denitrating catalyst, and use maturation, the most widely denitrating catalyst to be the most vanadium tungsten Titanium series catalysts at present, general operation temperature is at about 350 DEG C.In Flue Gas Denitrification Engineering application, in order to meet the requirement of denitrating catalyst to operating temperature, denitrating catalyst be generally be arranged in deduster before, but because in flue gas, fly ash content is higher, easily cause wearing and tearing to catalyst, meanwhile, the impurity such as the alkali metal oxide contained in flying dust can make catalyst poisoning lose efficacy, and sulfureous in flue gas content is higher, denitrating catalyst can by part SO
2be oxidized to SO
3, SO
3with the NH escaped
3easy reaction forms sulphur ammonium, can cause the corrosion of upstream device.For reducing flying dust and sulfur content impact in flue gas, after can considering that denitrating catalyst is arranged in deduster and desulfurizer, this configuration is comparatively rational, flue gas is by after deduster and desulfurizer, temperature can significantly reduce, and after dust-removal and desulfurizing, flue-gas temperature is lower and cause the catalyst of existing routine directly to use.
Summary of the invention
For the problems referred to above, the invention provides a kind of low temperature manganese system complex oxide denitrating catalyst, for the selective catalytic reduction reaction of the nitrogen oxide in boiler smoke under cryogenic conditions, denitrating catalyst make after can be arranged in deduster and desulfurizer, effectively reduce flying dust and sulfur content impact in flue gas, invention also provides a kind of preparation method of low temperature manganese system complex oxide denitrating catalyst.
A kind of low temperature manganese system complex oxide denitrating catalyst, it is characterized in that: take Nano titanium dioxide as carrier, the manganese cerium vanadium oxides composite of load on it is active component, and part reinforcing agent composition, each constituent mass is than being titanium dioxide: Mn salt: Ce salt: V salt: reinforcing agent=1:(0.625 ~ 1.563): (0.05 ~ 2.71): (0.001 ~ 0.029): (0.05 ~ 0.3).
The preparation method of described a kind of low temperature manganese system complex oxide denitrating catalyst is:
(1) mixing action: by Nano titanium dioxide, water, Bronsted acid, emprotid, plasticizer, pore creating material, reinforcing agent, lubricant is according to mass ratio 1:(0.1 ~ 1): (0.02 ~ 0.2): (0.05 ~ 0.5): (0.005 ~ 0.02): (0.005 ~ 0.02): (0.05 ~ 0.3): (0.005 ~ 0.02) is by adding the soluble-salt of manganese after mixing method mixing, the soluble-salt of cerium and the soluble-salt of vanadium form plastic mud material, manganese salt, cerium salt, the addition of vanadic salts is determined according to the mole of titanium dioxide, manganese salt, cerium salt, the addition of vanadic salts is determined according to the quality of titanium dioxide, each constituent mass is than being titanium dioxide: Mn salt: Ce salt: V salt=1:(0.625 ~ 1.563): (0.27 ~ 2.71): (0.001 ~ 0.029),
(2) ageings: the plastic mud material obtained in step (1) moisturizing ageing under 25 DEG C of constant temperature is placed 1 ~ 2 day;
(3) pre-extruded: the plastic mud material pre-extruded equipment of completing steps (2) is carried out pre-extruded operation, forms pug square;
(4) secondary ageing: the pug square obtained in step (3) moisturizing ageing under 25 DEG C of constant temperature is placed 1 ~ 2 day
(5) extrusion molding: the pug square extrusion equipment of completing steps (4) is carried out extruding operation, obtains cellular sample;
(6) primary drying: by the cellular sample temperature programming dry catalyst at 30 ~ 70 DEG C obtained in step (5), drying time is 5 ~ 8 days;
(7) redrying: by the cellular sample of completing steps (6) temperature programming dry catalyst at 100 ~ 300 DEG C, drying time is 3 ~ 5h;
(8) high-temperature roasting: by the cellular sample of completing steps (7) roasting 3 ~ 8h under 400 ~ 600 DEG C of high temperature, can MnO be obtained
x-CeO
2-V
2o
5/ TiO
2catalyst.
Adopt the low temperature manganese system complex oxide denitrating catalyst of the invention described above, the selective catalytic reduction reaction of the nitrogen oxide under cryogenic in boiler smoke, denitrating catalyst make after can be arranged in deduster and desulfurizer, reduce the wearing and tearing to catalyst, effectively reduce flying dust and sulfur content impact in flue gas simultaneously, decrease SO
2be oxidized to SO
3, effectively reduce SO
3with the NH escaped
3form the quantity of sulphur ammonium, effectively avoid the corrosion of upstream device.
Detailed description of the invention
Below in conjunction with specific embodiment, the invention will be further described.
Embodiment one
Catalyst preparing:
(1) mixing action: Nano titanium dioxide, water, lactic acid, ammoniacal liquor, PEO, purified cotton, glass, stearic acid are formed plastic mud material according to mass ratio 1:0.1:0.02:0.05:0.005:0.005:0.05:0.005 by adding manganese acetate, cerous nitrate and ammonium metavanadate after mixing method mixing, the addition of manganese acetate, cerous nitrate and ammonium metavanadate is determined according to the quality of titanium dioxide, and each constituent mass is than being titanium dioxide: manganese acetate: cerous nitrate: ammonium metavanadate=1:0.625:0.27:0.001;
(2) ageings: the plastic mud material obtained in step (1) moisturizing ageing under 25 DEG C of constant temperature is placed 1 day;
(3) pre-extruded: the plastic mud material pre-extruded equipment of completing steps (2) is carried out pre-extruded operation, forms pug square;
(4) secondary ageing: the pug square obtained in step (3) moisturizing ageing under 25 DEG C of constant temperature is placed 1 day;
(5) extrusion molding: the pug square extrusion equipment of completing steps (4) is carried out extruding operation, obtains cellular sample;
(6) primary drying: by the cellular sample temperature programming dry catalyst at 30 ~ 70 DEG C obtained in step (5), namely 30 DEG C 1 day--40 DEG C 1 day--50 DEG C of 1 day--60 DEG C 1 day--70 DEG C 1 day--constant weights, drying time is 5 days;
(7) redrying: by the cellular sample of completing steps (6) temperature programming dry catalyst at 100 ~ 300 DEG C, i.e. 100 DEG C of 1h--300 DEG C of 2h, drying time is 3h;
(8) high-temperature roasting: by the cellular sample of completing steps (7) roasting 8h under 400 DEG C of high temperature, can MnO be obtained
x-CeO
2-V
2o
5/ TiO
2catalyst.
Catalyst activity is tested:
Activity experiment carries out on fixed bed reactors, and loaded catalyst is the catalyst sample of 5 × 5 holes, length 20cm.NH
3/ NO mol ratio=1, O
2concentration=5%, air speed=7500h
-1flue gas condition, when reaction temperature is 160 DEG C, denitration efficiency is 38.13%; When reaction temperature is 220 DEG C, denitration efficiency is 69.35%.
Embodiment two
Catalyst preparing:
(1) mixing action: Nano titanium dioxide, water, acetic acid, monoethanolamine, CMC, purified cotton, glass, stearic acid are formed plastic mud material according to mass ratio 1:0.5:0.1:0.01:0.01:0.01:0.1:0.01 by adding manganese nitrate, cerous nitrate and ammonium metavanadate after mixing method mixing, the addition of manganese nitrate, cerous nitrate and ammonium metavanadate is determined according to the quality of titanium dioxide, and each constituent mass is than being titanium dioxide: manganese nitrate: cerous nitrate: ammonium metavanadate=1:0.938:0.54:0.01;
(2) ageings: the plastic mud material obtained in step (1) moisturizing ageing under 25 DEG C of constant temperature is placed 2 days;
(3) pre-extruded: the plastic mud material pre-extruded equipment of completing steps (2) is carried out pre-extruded operation, forms pug square;
(4) secondary ageing: the pug square obtained in step (3) moisturizing ageing under 25 DEG C of constant temperature is placed 2 days;
(5) extrusion molding: the pug square extrusion equipment of completing steps (4) is carried out extruding operation, obtains cellular sample;
(6) primary drying: by the cellular sample temperature programming dry catalyst at 30 ~ 70 DEG C obtained in step (5), namely 30 DEG C 1 day--40 DEG C 1 day--50 DEG C of 1 day--60 DEG C 1 day--70 DEG C 1 day--constant weights, drying time is 6 days;
(7) redrying: by the cellular sample of completing steps (6) temperature programming dry catalyst at 100 ~ 300 DEG C, i.e. 100 DEG C of 2h--300 DEG C of 3h, drying time is 5h;
(8) high-temperature roasting: by the cellular sample of completing steps (7) roasting 6h under 500 DEG C of high temperature, can MnO be obtained
x-CeO
2-V
2o
5/ TiO
2catalyst.
Catalyst activity is tested:
With embodiment one, when reaction temperature is 160 DEG C, denitration efficiency is 53.62%; When reaction temperature is 220 DEG C, denitration efficiency is 75.66%.
Embodiment three
Catalyst preparing:
(1) mixing action: Nano titanium dioxide, water, lactic acid, ammoniacal liquor, CMC, active carbon, glass, glycerine are formed plastic mud material according to mass ratio 1:0.8:0.15:0.2:0.15:0.15:0.2:0.01 by adding manganese chloride, cerous nitrate and ammonium metavanadate after mixing method mixing, the addition of manganese nitrate, cerous nitrate and ammonium metavanadate is determined according to the quality of titanium dioxide, and each constituent mass is than being titanium dioxide: manganese chloride: cerous nitrate: ammonium metavanadate=1:0.625:1.08:0.015;
(2) ageings: the plastic mud material obtained in step (1) moisturizing ageing under 25 DEG C of constant temperature is placed 1 day;
(3) pre-extruded: the plastic mud material pre-extruded equipment of completing steps (2) is carried out pre-extruded operation, forms pug square;
(4) secondary ageing: the pug square obtained in step (3) moisturizing ageing under 25 DEG C of constant temperature is placed 1 day;
(5) extrusion molding: the pug square extrusion equipment of completing steps (4) is carried out extruding operation, obtains cellular sample;
(6) primary drying: by the cellular sample temperature programming dry catalyst at 30 ~ 70 DEG C obtained in step (5), namely 30 DEG C 1 day--40 DEG C 1 day--50 DEG C of 1 day--60 DEG C 1 day--70 DEG C 1 day--constant weights, drying time is 7 days;
(7) redrying: by the cellular sample of completing steps (6) temperature programming dry catalyst at 100 ~ 300 DEG C, i.e. 100 DEG C of 1h--300 DEG C of 3h, drying time is 4h;
(8) high-temperature roasting: by the cellular sample of completing steps (7) roasting 5h under 600 DEG C of high temperature, can MnO be obtained
x-CeO
2-V
2o
5/ TiO
2catalyst.
Catalyst activity is tested:
With embodiment one, when reaction temperature is 160 DEG C, denitration efficiency is 50.29%; When reaction temperature is 220 DEG C, denitration efficiency is 72.58%.
Embodiment four
Catalyst preparing:
(1) mixing action: by Nano titanium dioxide, water, acetic acid, monoethanolamine, CMC mixing PEO(1:2 in mass ratio), active carbon, glass, stearic acid form plastic mud material according to mass ratio 1:1:0.2:0.5:0.02:0.02:0.3:0.02 by adding manganese chloride, cerous nitrate and ammonium metavanadate after the mixing of mixing method, the addition of manganese acetate, cerous nitrate and ammonium metavanadate is determined according to the quality of titanium dioxide, and each constituent mass is than being titanium dioxide: manganese acetate: cerous nitrate: ammonium metavanadate=1:1.563:2.71:0.002;
(2) ageings: the plastic mud material obtained in step (1) moisturizing ageing under 25 DEG C of constant temperature is placed 2 days;
(3) pre-extruded: the plastic mud material pre-extruded equipment of completing steps (2) is carried out pre-extruded operation, forms pug square;
(4) secondary ageing: the pug square obtained in step (3) moisturizing ageing under 25 DEG C of constant temperature is placed 2 days;
(5) extrusion molding: the pug square extrusion equipment of completing steps (4) is carried out extruding operation, obtains cellular sample;
(6) primary drying: by the cellular sample temperature programming dry catalyst at 30 ~ 70 DEG C obtained in step (5), namely 30 DEG C 1 day--40 DEG C 1 day--50 DEG C of 1 day--60 DEG C 1 day--70 DEG C 1 day--constant weights, drying time is 8 days;
(7) redrying: by the cellular sample of completing steps (6) temperature programming dry catalyst at 100 ~ 300 DEG C, i.e. 100 DEG C of 2h--300 DEG C of 3h, drying time is 5h;
(8) high-temperature roasting: by the cellular sample of completing steps (7) roasting 5h under 500 DEG C of high temperature, can MnO be obtained
x-CeO
2-V
2o
5/ TiO
2catalyst.
Catalyst activity is tested:
With embodiment one, when reaction temperature is 160 DEG C, denitration efficiency is 54.78%; When reaction temperature is 220 DEG C, denitration efficiency is 79.36%.
Embodiment five
Catalyst preparing:
(1) mixing action: by Nano titanium dioxide, water, acetic acid, ammoniacal liquor, CMC mixing PEO(1:4 mixing in mass ratio), purified cotton, glass, stearic acid form plastic mud material according to mass ratio 1:0.75:0.1:0.2:0.01:0.01:0.15:0.01 by adding manganese acetate, cerous nitrate and ammonium metavanadate after the mixing of mixing method, the addition of manganese acetate, cerous nitrate and ammonium metavanadate is determined according to the quality of titanium dioxide, and each constituent mass is than being titanium dioxide: manganese acetate: cerous nitrate: ammonium metavanadate=1:1.25:1.08:0.01;
(2) ageings: the plastic mud material obtained in step (1) moisturizing ageing under 25 DEG C of constant temperature is placed 1 day;
(3) pre-extruded: the plastic mud material pre-extruded equipment of completing steps (2) is carried out pre-extruded operation, forms pug square;
(4) secondary ageing: the pug square obtained in step (3) moisturizing ageing under 25 DEG C of constant temperature is placed 1 day;
(5) extrusion molding: the pug square extrusion equipment of completing steps (4) is carried out extruding operation, obtains cellular sample;
(6) primary drying: by the cellular sample temperature programming dry catalyst at 30 ~ 70 DEG C obtained in step (5), namely 30 DEG C 1 day--40 DEG C 1 day--50 DEG C of 1 day--60 DEG C 1 day--70 DEG C 1 day--constant weights, drying time is 7 days;
(7) redrying: by the cellular sample of completing steps (6) temperature programming dry catalyst at 100 ~ 300 DEG C, i.e. 100 DEG C of 2h--300 DEG C of 3h, drying time is 5h;
(8) high-temperature roasting: by the cellular sample of completing steps (7) roasting 4h under 500 DEG C of high temperature, can MnO be obtained
x-CeO
2-V
2o
5/ TiO
2catalyst.
Catalyst activity is tested:
With embodiment one, when reaction temperature is 160 DEG C, denitration efficiency is 63.22%; When reaction temperature is 220 DEG C, denitration efficiency is 85.39%.
Adopt above-mentioned mixing method preparation technology, be convenient to the suitability for industrialized production realizing low temperature manganese system complex oxide denitrating catalyst.
Catalyst performance aspect, within the scope of said components, carries out the detection of catalyst denitration activity by Catalyst packing on fixed bed reactors, and in the scope of 130 ~ 280 DEG C, the highest denitration efficiency is 85.39%, has possessed good practicality.
Claims (7)
1. a low temperature manganese system complex oxide denitrating catalyst, it is characterized in that: described catalyst take Nano titanium dioxide as carrier, the manganese cerium vanadium oxides composite of load on it is active component, and part reinforcing agent composition, each constituent mass is than being titanium dioxide: Mn salt: Ce salt: V salt: reinforcing agent=1:(0.625 ~ 1.563): (0.05 ~ 2.71): (0.001 ~ 0.029): (0.05 ~ 0.3).
2. a preparation method for low temperature manganese system complex oxide denitrating catalyst, is characterized in that: it is as follows that it comprises step:
(1) mixing action: by Nano titanium dioxide, water, Bronsted acid, emprotid, plasticizer, pore creating material, reinforcing agent, lubricant is according to mass ratio 1:(0.1 ~ 1): (0.02 ~ 0.2): (0.05 ~ 0.5): (0.005 ~ 0.02): (0.005 ~ 0.02): (0.05 ~ 0.3): (0.005 ~ 0.02) is by adding the soluble-salt of manganese after mixing method mixing, the soluble-salt of cerium and the soluble-salt of vanadium form plastic mud material, manganese salt, cerium salt, the addition of vanadic salts is determined according to the quality of titanium dioxide, each constituent mass is than being titanium dioxide: Mn salt: Ce salt: V salt=1:(0.625 ~ 1.563): (0.27 ~ 2.71): (0.001 ~ 0.029),
(2) ageings: the plastic mud material obtained in step (1) moisturizing ageing under 25 DEG C of constant temperature is placed 1 ~ 2 day;
(3) pre-extruded: the plastic mud material pre-extruded equipment of completing steps (2) is carried out pre-extruded operation, forms pug square;
(4) secondary ageing: the pug square obtained in step (3) moisturizing ageing under 25 DEG C of constant temperature is placed 1 ~ 2 day;
(5) extrusion molding: the pug square extrusion equipment of completing steps (4) is carried out extruding operation, obtains cellular sample;
(6) primary drying: by the cellular sample temperature programming dry catalyst at 30 ~ 70 DEG C obtained in step (5), drying time is 5 ~ 8 days;
(7) redrying: by the cellular sample of completing steps (6) temperature programming dry catalyst at 100 ~ 300 DEG C, drying time is 3 ~ 5h;
(8) high-temperature roasting: by the cellular sample of completing steps (7) roasting 3 ~ 8h under 400 ~ 600 DEG C of high temperature, can MnO be obtained
x-CeO
2-V
2o
5/ TiO
2catalyst.
3. the preparation method of a kind of low temperature manganese system complex oxide denitrating catalyst according to claim 2, is characterized in that: described Bronsted acid is acetic acid or lactic acid; Described emprotid is ammoniacal liquor or monoethanolamine; Described plasticizer is CMC or PEO or CMC mixing PEO.
4. the preparation method of a kind of low temperature manganese system complex oxide denitrating catalyst according to claim 5, is characterized in that: described CMC mixing PEO is by CMC, PEO mass ratio 1:(2 ~ 5).
5. the preparation method of a kind of low temperature manganese system complex oxide denitrating catalyst according to claim 2, is characterized in that: described pore creating material is purified cotton or active carbon; Described reinforcing agent is glass or carbon fiber; Described lubricant is stearic acid or glycerine; The soluble-salt of described manganese is manganese nitrate, manganese acetate or manganese chloride; The soluble-salt of described cerium is cerous nitrate or cerium chloride; The soluble-salt of described vanadium is ammonium metavanadate or vanadyl oxalate.
6. the preparation method of a kind of low temperature manganese system complex oxide denitrating catalyst according to claim 2, is characterized in that: the temperature programming dry catalyst at 30 ~ 70 DEG C of the cellular sample in primary drying is 30 DEG C of 1 day--40 DEG C 1 day--50 DEG C of 1 day--60 DEG C 1 day--70 DEG C 1 day--constant weights.
7. the preparation method of a kind of low temperature manganese system complex oxide denitrating catalyst according to claim 2, is characterized in that: the temperature programming dry catalyst at 100 ~ 300 DEG C of the cellular sample in redrying is 100 DEG C of 1 ~ 2h--300 DEG C of 2 ~ 3h.
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| CN107552043A (en) * | 2017-09-06 | 2018-01-09 | 北京科技大学 | A kind of support type low temperature SCR denitration catalyst and preparation method thereof |
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| CN111871068A (en) * | 2019-11-12 | 2020-11-03 | 南京工业大学 | Preparation method of integrated filter material |
| CN115888693A (en) * | 2022-10-25 | 2023-04-04 | 浙江大学 | Supported manganese/cerium low-temperature honeycomb denitration catalyst and preparation method thereof |
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| CN109201042B (en) * | 2018-11-07 | 2021-08-10 | 清华大学盐城环境工程技术研发中心 | Preparation method and application of vanadium-doped umbrella-shaped manganese-cerium composite oxide catalyst |
| CN111871068A (en) * | 2019-11-12 | 2020-11-03 | 南京工业大学 | Preparation method of integrated filter material |
| CN115888693A (en) * | 2022-10-25 | 2023-04-04 | 浙江大学 | Supported manganese/cerium low-temperature honeycomb denitration catalyst and preparation method thereof |
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