CN102921430B - Process for preparing denitrification catalyst - Google Patents
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- CN102921430B CN102921430B CN201210511327.6A CN201210511327A CN102921430B CN 102921430 B CN102921430 B CN 102921430B CN 201210511327 A CN201210511327 A CN 201210511327A CN 102921430 B CN102921430 B CN 102921430B
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Abstract
The invention relates to a process for preparing a denitrification catalyst. The process is characterized by comprising the following steps of: firstly, selecting and mixing powdered activated carbon or granular activated carbon which has the C content of more than 90 percent and the specific surface area of more than 1000 m<2>/g into an alcohol amine solution to obtain a suspension liquid for later use; secondly, dissolving a mixed solution of ammonium metavanadate, titanium nitrate and aluminium nitrate in the suspension liquid according to the mass ratio of 10-50 percent to form a sizing agent A; thirdly, dissolving a mixed solution of manganese nitrate, ferric nitrate and copper nitrate in the suspension liquid to form a sizing agent B, coating a carrier with the sizing agent A, drying to a constant weight and then heating to 530-570 DEG C under the protective atmosphere, and carrying out heat preservation for 3-5 hours and subsequently cooling to the room temperature at a temperature reduction speed; and finally, the sizing agent B is coated on the surface of the carrier obtained from the last step, the carrier is dried to a constant weight and then heating to 630-670 DEG C under the atmosphere containing 70 percent of N2, 20 percent of CO2 and 10 percent of CO, carrying out heat preservation and then cooling to the room temperature at a temperature reduction speed to achieve the catalyst in which pores and channels are communicated and are in a two-layer structure. The space velocity of the catalyst can be improved by more than 60 percent, and the resistance is reduced by more than 45 percent, so that a small-sized catalyst device is achieved.
Description
Technical field
The present invention relates to a kind of catalyst, especially a kind of gas-fired equipment vent gas treatment catalyst, specifically a kind of preparation method of denitrating catalyst.
Background technology
Gas internal-combustion engine has a wide range of applications in gaseous fuel generating and cogeneration field, be not only applicable to the burning of the conventional gas fuel such as natural gas, at industrial by-product Gas recoveries such as blast furnace gas, coke-stove gas, and aspect the recyclings such as biogas, coal bed gas, all brought into play important using energy source effect.Along with China is to the deepening continuously of energy-saving and emission-reduction work, the application scale of gas internal-combustion engine is by increasing.
The impact of the operation principle of being burnt, the tail gas nitrogen oxide concentration of emission of gas internal-combustion engine is higher, often in 600 ~ 1000mg/Nm
3between, this is mainly because the sky of gas internal-combustion engine is so than large, sufficient combustion, and in batch (-type) combustion process, ignition temperature peak value is high, causes nitrogen oxide burning product to increase.
Gas internal-combustion engine is usually used in power industry, and its discharged nitrous oxides concentration, generally higher than current standard, only, because the positive meaning of its waste utilization generating is larger, has been covered people's strict demand up to standard to its exhaust emissions.From now on, along with China is tight to constantly adding of atmosphere pollution discharged nitrous oxides, carry out the research of gas internal-combustion engine tail gas denitration purification techniques and application, make it to meet the requirement of environmental regulation, become the inevitable demand of gas internal-combustion engine industry development.
The conventional technology of combustion gas denitration is SCR (SCR), adopts urea or ammonia as reducing agent, under catalyst action, by reduction of nitrogen oxide, is nitrogen.The core of SCR technology is catalyst, the catalyst adopting in engineering at present be take the integral catalyzer that titanium dioxide is carrier loaded vanadic anhydride often, the type catalyst is mainly used in boiler of power plant denitrating flue gas, and be not suitable for large to air speed in gas internal-combustion engine, resistance is little, can be high temperature resistant, the requirement of the performance such as anti-gas shock, this just requires to carry out pointed denitrating catalyst R&D work.
According to analysis, we think that reason that conventional denitrating catalyst is difficult to meet gas internal-combustion engine application requirements mainly: one is that the specific area of catalyst is less, and the contact area that makes to participate in catalytic reaction is little, causes catalytic reaction conversion ratio not high; Another is that the mechanical attachment of vanadium pentoxide active component is not strong, easily by airflow scouring, is walked, and causes catalyst attrition large.
Summary of the invention
The object of the invention is can not adapt to gas internal-combustion engine needs for existing denitrfying agent, cause for a long time gas internal-combustion engine because the catalyst without suitable can not reach desirable denitration effect, easily to problems such as environments, design that a kind of internal voids is abundant, the preparation method of double-deck denitrating catalyst.
Technical scheme of the present invention is:
A preparation method for denitrating catalyst, is characterized in that it comprises the following steps:
First, select that C content is greater than 90%, specific area is greater than 1000m
2the Powdered Activated Carbon of/g or granular activated carbon, after oven dry, under dry state, ball milling obtains particle diameter at the Powdered Activated Carbon of 0.1--1 micron, 2% ~ 5% the Powdered Activated Carbon after ball milling is mixed in solution in mass ratio subsequently, described solution is the aqueous alkanolamine of 8% ~ 30% volume ratio, under hygrometric state, ball milling is no less than 10 hours again, after standing 24 hours, standby by getting stable suspension after sediment separation, now in suspension, the diameter of micro activated carbon particle is less than 1 micron;
Secondly, by ammonium metavanadate, Titanium Nitrate, aluminum nitrate (1-5) in mass ratio: (2-8): ratio (5-15) is mixed, get 100 ~ 500 grams, this mixture and add in 1 liter of suspension, adopt ammoniacal liquor or second acid for adjusting pH to 4-4.5, ball milling is not less than 10 hours, forms slurry A;
The 3rd, by manganese nitrate, ferric nitrate, copper nitrate (1-2) in mass ratio: (0.5-1): ratio (0.2-1) is mixed, get 100 ~ 500 grams, this mixture and add in 1 liter of suspension, adopt ammoniacal liquor or second acid for adjusting pH to 4-4.5, ball milling 10 hours, forms slurry B;
The 4th, with slurry A coated carrier, dry to constant weight, subsequently at 70%N
2, 20%CO
2, under 10%CO protective atmosphere, with 4-6 ℃/min heating rate, be warming up to 530-570 ℃, be incubated after 3-5 hour, with 8-12 ℃/min rate of temperature fall, be cooled to room temperature; In this process, form internal layer catalyst active component structure, and carbon particle is in pyrolytic process, forms the abundant hole of inner density; Obtain the carrier with one deck catalyst.
Finally, with slurry B, be coated on the carrier surface with one deck catalyst that previous step prepares, at 110-130 ℃, dry to constant weight, subsequently at 70%N
2, 20%CO
2, under 10%CO atmosphere, with 4-6 ℃/min heating rate, be warming up to 630-670 ℃, be incubated after 3-5 hour, with 8-12 ℃/min rate of temperature fall, be cooled to room temperature; In this process, form outer layer catalyst active component structure, and outer layer catalyst is combined with internal layer catalyst closely, hole duct communicates, and has formed the catalyst with double-layer structure.
Described aqueous alkanolamine is one or more the mixed liquor in monoethanolamine, diethanol amine, triethanolamine or methyl diethanolamine.
Described Powdered Activated Carbon or the bake out temperature of granular activated carbon are 150-170 ℃, and drying time is 4-6 hour, and under dry state, Ball-milling Time is not less than 6 hours.
Described carrier is ceramic honey comb, metal beehive or woven wire, and carrier bake out temperature is 110-130 ℃.
Beneficial effect of the present invention:
(1) the present invention adopts micro activated carbon particle to add catalyst to prepare in slurry, and prepared by traditional catalyst do not have active carbon in slurry.
(2), for micro activated carbon particle is uniformly distributed in slurry, adopt alkanolamine solution as stabilizing agent.
(3) prepared double-deck catalyst, internal layer contains alum, titanium, aluminum oxide active component, and skin contains manganese, iron, Cu oxide active component, and the work object of two-layer catalyst differs.
(4) object at catalyst pulp interpolation active carbon is to have larger gas diffusivity between the two-layer catalyst that makes to prepare, and is convenient to jointly play a role.
(5) it is abundant that the catalyst that prepared by the inventive method has internal voids, by mixing micro activated carbon particle, in roasting process, pyrolytic gasification forms gap structure, double-decker is that catalytic component based on vanadium is placed in internal layer, the frame for movements such as outer employing manganese base, iron-based, copper base are stable, the activated catalyst of tool, improve the performance of catalyst by these two kinds of measures.
(6) air speed that experiment showed, catalyst of the present invention can improve more than 60%, and resistance declines and is greater than 45%, therefore can realize the miniaturization of catalyst-assembly, meets the application requirements in gas engine; In addition, because catalyst structure is firm, wash away loss amount little, catalyst-coated amount can reduce over half, thereby contributes to reduce catalyst cost.
The specific embodiment
Below in conjunction with embodiment, the present invention is further illustrated.
Embodiment mono-.
Get and select that C content is greater than 90%, specific area is greater than 1000m
220 grams of the Powdered Activated Carbon of/g or granular activated carbons, after 150-170 ℃ of oven dry, under dry state, ball milling obtains particle diameter for 6 hours at the Powdered Activated Carbon of 0.1～1 micron of micron, Powdered Activated Carbon after ball milling is mixed in 1000 grams of solution subsequently, described solution is the aqueous alkanolamine of 8%% volume ratio, under hygrometric state, ball milling is no less than 10 hours again, after standing 24 hours, get suspension standby, now in suspension, the diameter of micro activated carbon particle is less than 1 micron; Described aqueous alkanolamine is one or more the mixed liquor in monoethanolamine, diethanol amine, triethanolamine or methyl diethanolamine.
5 grams of 1 gram of ammonium metavanadates, 2 grams of Titanium Nitrates, aluminum nitrate are dissolved in 72 grams of suspension after mixing, adopt ammoniacal liquor or second acid for adjusting pH to 4-4.5, ball milling is not less than 10 hours, forms slurry A;
The 3rd, will after 1 gram of manganese nitrate, 0.5 gram of ferric nitrate, 0.2 gram of mixing of copper nitrate, dissolve in 15.3 grams of suspension, adopt ammoniacal liquor or second acid for adjusting pH to 4-4.5, ball milling 10 hours, forms slurry B;
The 5th, with slurry A coated carrier, at 110-130 ℃, dry to constant weight, subsequently at 70%N
2, 20%CO
2, under 10%CO protective atmosphere, with 4-6 ℃/min heating rate, be warming up to 530-570 ℃, be incubated after 3-5 hour, with 8-12 ℃/min rate of temperature fall, be cooled to room temperature; In this process, form internal layer catalyst active component structure, and carbon particle is in pyrolytic process, forms the abundant hole of inner density; Obtain the carrier with one deck catalyst
Finally, with slurry B, be coated on the carrier surface with one deck catalyst that previous step prepares, at 110-130 ℃, dry to constant weight, subsequently at 70%N
2, 20%CO
2, under 10%CO atmosphere, with 4-6 ℃/min heating rate, be warming up to 630-670 ℃, be incubated after 3-5 hour, with 8-12 ℃/min rate of temperature fall, be cooled to room temperature; In this process, form outer layer catalyst active component structure, and outer layer catalyst is combined with internal layer catalyst closely, hole duct communicates, and has formed the catalyst with double-layer structure.
The catalyst that above method is prepared is tested, and air speed can improve more than 60%, and resistance declines and is greater than 45%, therefore can realize the miniaturization of catalyst-assembly, meets the application requirements in gas engine; In addition, because catalyst structure is firm, wash away loss amount little, catalyst-coated amount can reduce over half, thereby contributes to reduce catalyst cost.
Embodiment bis-.
Get and select that C content is greater than 90%, specific area is greater than 1000m
250 grams of the Powdered Activated Carbon of/g or granular activated carbons, after 150-170 ℃ of oven dry, under dry state, ball milling obtains particle diameter for 6 hours at the Powdered Activated Carbon of 0.1～1 micron of micron, Powdered Activated Carbon after ball milling is mixed in 1000 grams of solution subsequently, described solution is the aqueous alkanolamine of 30% volume ratio, under hygrometric state, ball milling is no less than 10 hours again, after standing 24 hours, get suspension standby, now in suspension, the diameter of micro activated carbon particle is less than 1 micron; Described aqueous alkanolamine is one or more the mixed liquor in monoethanolamine, diethanol amine, triethanolamine or methyl diethanolamine.
15 grams of 5 grams of ammonium metavanadates, 8 grams of Titanium Nitrates, aluminum nitrate are dissolved in 28 grams of suspension after mixing, adopt ammoniacal liquor or second acid for adjusting pH to 4-4.5, ball milling is not less than 10 hours, forms slurry A;
The 3rd, will after 2 grams of manganese nitrates, 1 gram of ferric nitrate, 1 gram of mixing of copper nitrate, dissolve in 4 grams of suspension, adopt ammoniacal liquor or second acid for adjusting pH to 4-4.5, ball milling 10 hours, forms slurry B;
The 6th, with slurry A coated carrier, at 110-130 ℃, dry to constant weight, subsequently at 70%N
2, 20%CO
2, under 10%CO protective atmosphere, with 4-6 ℃/min heating rate, be warming up to 530-570 ℃, be incubated after 3-5 hour, with 8-12 ℃/min rate of temperature fall, be cooled to room temperature; In this process, form internal layer catalyst active component structure, and carbon particle is in pyrolytic process, forms the abundant hole of inner density; Obtain the carrier with one deck catalyst
Finally, with slurry B, be coated on the carrier surface with one deck catalyst that previous step prepares, at 110-130 ℃, dry to constant weight, subsequently at 70%N
2, 20%CO
2, under 10%CO atmosphere, with 4-6 ℃/min heating rate, be warming up to 630-670 ℃, be incubated after 3-5 hour, with 8-12 ℃/min rate of temperature fall, be cooled to room temperature; In this process, form outer layer catalyst active component structure, and outer layer catalyst is combined with internal layer catalyst closely, hole duct communicates, and has formed the catalyst with double-layer structure.
The catalyst that above method is prepared is tested, and air speed can improve more than 60%, and resistance declines and is greater than 45%, therefore can realize the miniaturization of catalyst-assembly, meets the application requirements in gas engine; In addition, because catalyst structure is firm, wash away loss amount little, catalyst-coated amount can reduce over half, thereby contributes to reduce catalyst cost.
Embodiment tri-.
Get and select that C content is greater than 90%, specific area is greater than 1000m
235 grams of the Powdered Activated Carbon of/g or granular activated carbons, after 150-170 ℃ of oven dry, under dry state, ball milling obtains particle diameter for 6 hours at the Powdered Activated Carbon of 0.1～1 micron of micron, Powdered Activated Carbon after ball milling is mixed in 1000 grams of solution subsequently, described solution is the aqueous alkanolamine of 8%% volume ratio, under hygrometric state, ball milling is no less than 10 hours again, after standing 24 hours, get suspension standby, now in suspension, the diameter of micro activated carbon particle is less than 1 micron; Described aqueous alkanolamine is one or more the mixed liquor in monoethanolamine, diethanol amine, triethanolamine or methyl diethanolamine.
10 grams of 3 grams of ammonium metavanadates, 5 grams of Titanium Nitrates, aluminum nitrate are dissolved in 42 grams of suspension after mixing, adopt ammoniacal liquor or second acid for adjusting pH to 4-4.5, ball milling is not less than 10 hours, forms slurry A;
The 3rd, will after 1.5 grams of manganese nitrates, 0.75 gram of ferric nitrate, 0.6 gram of mixing of copper nitrate, dissolve in 6.65 grams of suspension, adopt ammoniacal liquor or second acid for adjusting pH to 4-4.5, ball milling 10 hours, forms slurry B;
The 7th, with slurry A coated carrier, at 110-130 ℃, dry to constant weight, subsequently at 70%N
2, 20%CO
2, under 10%CO protective atmosphere, with 4-6 ℃/min heating rate, be warming up to 530-570 ℃, be incubated after 3-5 hour, with 8-12 ℃/min rate of temperature fall, be cooled to room temperature; In this process, form internal layer catalyst active component structure, and carbon particle is in pyrolytic process, forms the abundant hole of inner density; Obtain the carrier with one deck catalyst
Finally, with slurry B, be coated on the carrier surface with one deck catalyst that previous step prepares, at 110-130 ℃, dry to constant weight, subsequently at 70%N
2, 20%CO
2, under 10%CO atmosphere, with 4-6 ℃/min heating rate, be warming up to 630-670 ℃, be incubated after 3-5 hour, with 8-12 ℃/min rate of temperature fall, be cooled to room temperature; In this process, form outer layer catalyst active component structure, and outer layer catalyst is combined with internal layer catalyst closely, hole duct communicates, and has formed the catalyst with double-layer structure.
The catalyst that above method is prepared is tested, and air speed can improve more than 60%, and resistance declines and is greater than 45%, therefore can realize the miniaturization of catalyst-assembly, meets the application requirements in gas engine; In addition, because catalyst structure is firm, wash away loss amount little, catalyst-coated amount can reduce over half, thereby contributes to reduce catalyst cost.
The part that the present invention does not relate to all prior art that maybe can adopt same as the prior art is realized.
Claims (4)
1. a preparation method for denitrating catalyst, is characterized in that it comprises the following steps:
First, select that C content is greater than 90%, specific area is greater than 1000m
2the Powdered Activated Carbon of/g or granular activated carbon, after oven dry, under dry state, ball milling obtains particle diameter at the Powdered Activated Carbon of 0.1--1 micron, 2% ~ 5% the Powdered Activated Carbon after ball milling is mixed in solution in mass ratio subsequently, described solution is the aqueous alkanolamine of 8% ~ 30% volume ratio, under hygrometric state, ball milling is no less than 10 hours again, after standing 24 hours, standby by getting stable suspension after sediment separation, now in suspension, the diameter of micro activated carbon particle is less than 1 micron;
Secondly, by ammonium metavanadate, Titanium Nitrate, aluminum nitrate (1-5) in mass ratio: (2-8): ratio (5-15) is mixed, get 100 ~ 500 grams, this mixture and add in 1 liter of suspension, adopt ammoniacal liquor or second acid for adjusting pH to 4-4.5, ball milling is not less than 10 hours, forms slurry A;
The 3rd, by manganese nitrate, ferric nitrate, copper nitrate (1-2) in mass ratio: (0.5-1): ratio (0.2-1) is mixed, get 100 ~ 500 grams, this mixture and add in 1 liter of suspension, adopt ammoniacal liquor or second acid for adjusting pH to 4-4.5, ball milling 10 hours, forms slurry B;
With slurry A coated carrier, dry to constant weight, subsequently at 70%N
2, 20%CO
2, under 10%CO protective atmosphere, with 4-6 ℃/min heating rate, be warming up to 530-570 ℃, be incubated after 3-5 hour, with 8-12 ℃/min rate of temperature fall, be cooled to room temperature; In this process, form internal layer catalyst active component structure, and carbon particle is in pyrolytic process, forms the abundant hole of inner density; Obtain the carrier with one deck catalyst;
Finally, with slurry B, be coated on the carrier surface with one deck catalyst that previous step prepares, at 110-130 ℃, dry to constant weight, subsequently at 70%N
2, 20%CO
2, under 10%CO atmosphere, with 4-6 ℃/min heating rate, be warming up to 630-670 ℃, be incubated after 3-5 hour, with 8-12 ℃/min rate of temperature fall, be cooled to room temperature; In this process, form outer layer catalyst active component structure, and outer layer catalyst is combined with internal layer catalyst closely, hole duct communicates, and has formed the catalyst with double-layer structure.
2. method according to claim 1, is characterized in that described aqueous alkanolamine is one or more the mixed liquor in monoethanolamine, diethanol amine, triethanolamine or methyl diethanolamine.
3. method according to claim 1, is characterized in that described Powdered Activated Carbon or the bake out temperature of granular activated carbon are 150-170 ℃, and drying time is 4-6 hour, and under dry state, Ball-milling Time is not less than 6 hours.
4. method according to claim 1, is characterized in that described carrier is ceramic honey comb, metal beehive or woven wire, and carrier bake out temperature is 110-130 ℃.
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| CN201210511327.6A CN102921430B (en) | 2012-12-04 | 2012-12-04 | Process for preparing denitrification catalyst |
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| CN102921430B true CN102921430B (en) | 2014-07-23 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103638921B (en) * | 2013-12-11 | 2015-07-22 | 安徽省元琛环保科技有限公司 | Vanadium-tungsten denitration catalyst and preparation method thereof |
| CN106914245A (en) * | 2017-03-03 | 2017-07-04 | 安徽工业大学 | A kind of activated carbon supported iron-based low temperature SCR denitration catalyst and its preparation method and application method |
| CN107803113A (en) * | 2017-12-15 | 2018-03-16 | 江苏龙净科杰催化剂再生有限公司 | The preparation method of flue gas ash removal denitration Tuo bioxin integrated ceramic filters |
| CN108671750A (en) * | 2018-06-04 | 2018-10-19 | 常州宝电节能环保科技有限公司 | A kind of preparation method of width temperature operating window dedusting denitration double functional ceramics column |
| CN110917833A (en) * | 2019-12-13 | 2020-03-27 | 西安润川环保科技有限公司 | Novel flue gas denitration method |
| CN113499768A (en) * | 2021-07-09 | 2021-10-15 | 安徽元琛环保科技股份有限公司 | Preparation method of coating type high-strength denitration catalyst and prepared denitration catalyst |
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| CN1046473A (en) * | 1989-04-21 | 1990-10-31 | 中国科学院大连化学物理研究所 | Purification catalyst for automobile exhaust |
| JP2004322004A (en) * | 2003-04-25 | 2004-11-18 | Mitsubishi Heavy Ind Ltd | Nitrogen oxide removal catalyst, and denitrification method and denitrification apparatus using the same |
| CN101043944A (en) * | 2004-10-15 | 2007-09-26 | 约翰逊马西日本株式会社 | Catalyst for treating exhaust gas and device for treating exhaust gas using the same |
| CN102008958A (en) * | 2010-11-09 | 2011-04-13 | 上海歌地催化剂有限公司 | Three-way catalyst used for purifying gasoline car tail gas and preparation method thereof |
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2012
- 2012-12-04 CN CN201210511327.6A patent/CN102921430B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1046473A (en) * | 1989-04-21 | 1990-10-31 | 中国科学院大连化学物理研究所 | Purification catalyst for automobile exhaust |
| JP2004322004A (en) * | 2003-04-25 | 2004-11-18 | Mitsubishi Heavy Ind Ltd | Nitrogen oxide removal catalyst, and denitrification method and denitrification apparatus using the same |
| CN101043944A (en) * | 2004-10-15 | 2007-09-26 | 约翰逊马西日本株式会社 | Catalyst for treating exhaust gas and device for treating exhaust gas using the same |
| CN102008958A (en) * | 2010-11-09 | 2011-04-13 | 上海歌地催化剂有限公司 | Three-way catalyst used for purifying gasoline car tail gas and preparation method thereof |
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