CN102008967A - Ferric sulfate catalyst and preparation method thereof - Google Patents
Ferric sulfate catalyst and preparation method thereof Download PDFInfo
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- CN102008967A CN102008967A CN 201010529669 CN201010529669A CN102008967A CN 102008967 A CN102008967 A CN 102008967A CN 201010529669 CN201010529669 CN 201010529669 CN 201010529669 A CN201010529669 A CN 201010529669A CN 102008967 A CN102008967 A CN 102008967A
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- ferric sulfate
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Abstract
The invention discloses a ferric sulfate catalyst and a preparation method thereof. The method comprises the following steps: firstly, preparing a ferric sulfate or ferric nitrate solution; then adding a TiO2 carrier into the solution, and stirring to evaporate moisture; and finally vulcanizing to obtain the ferric sulfate catalyst, wherein the chemical formula of the ferric sulfate catalyst is Fe2(SO4)3/TiO2. The ferric sulfate catalyst comprises the following components in percentage by weight: 6.7-22.2% of ferric sulfate and 77.8-93.3% of TiO2. Compared with the prior art, the invention has the following advantages and obvious effects: toxicant active component V2O5 is not adopted, thus environmental pollution is lightened and the performance of the catalyst is effectively improved; at the temperature of 300-500 DEG C, the metallic oxide catalyst prepared by the method has nitric oxide purification efficiency up to 70-100%; and the ferric sulfate catalyst can efficiently catalyze and reduce nitric oxide in the presence of water and sulfur dioxide.
Description
Technical field
The present invention relates to a kind of environmentally friendly denitrating catalyst in environmental protection, environmentally conscious materials and the environmental catalysis technical field, particularly a kind of Ferric Sulfate Hydrafe agent and preparation method thereof.
Background technology
Along with China's rapid economy development, the sustainable growth of energy-consuming consumes a large amount of fossil fuels in the energy-consuming mode of fire coal, fuel oil, combustion gas, is discharged into the constantly aggravation of harm such as nitrogen oxide (NOx) in the atmosphere.At present, some metropolitan atmosphere pollution of China have presented region composite type characteristics, and the discharging of effectively controlling NOx has become the important means of alleviating compound pollution situation.NOx discharging in city stationary source and the moving source is one of main source of municipal pollution, and therefore effectively the discharging of these type of pollution sources of control NOx is to carry out the pith that the region composite type pollutes control.
At present, the SCR technology is the gas denitrifying technology that is most widely used in the world.Difference according to reducing agent can be divided into the ammonia Selective Catalytic Reduction of NO
x(NH
3-SCR) and hydrocarbon Selective Catalytic Reduction of NO x (HC-SCR) technology; Wherein, NH
3(Selective Catalytic Reduction, SCR) technology is the mainstream technology of stationary source denitrating flue gas to-SCR, is used widely abroad.Its principle is by adding NH
3Is harmless N as reducing agent with the NOx selective reduction
2And discharge.The key of SCR technology is the catalyst of exploitation efficient stable, is the applied environment of principal character to be applicable to high-sulfur, high dirt.Good sulfur tolerance has become the bottleneck that can the decision catalyst engineering practicability.At present, the NH of industrial applications
3How-SCR catalyst is with TiO
2Be carrier, more a certain amount of V in the load
2O
5, WO
3Or MoO
3Etc. component, such catalyst possesses good sulfur resistance in efficient purification NOx.
But, traditional denitration V
2O
5-WO
3/ TiO
2Catalyst still exists some problems, the one, active component V in actual use
2O
5The presoma general toxicity very big, easily human body and environment are produced secondary pollution; The 2nd, V
2O
5NOx is reduced to N in flue gas
2And H
2In the time of O also with SO in the flue gas
2Be oxidized to SO
3, SO
3Meeting and NH
3React generation ammonium sulfate and ammonium hydrogen sulfate and influence catalyst activity and obstruction catalytic reactor passage; The 3rd, WO
3And MoO
3N during high temperature
2Selectivity is relatively poor, can promote N
2The generation of O, and N
2O can cause environmental problems such as greenhouse effects, depletion of the ozone layer.Therefore, how to adopt domestic catalyst, reduce the catalyst cost, realize high activity, the high sulfidation resistance energy of catalyst, and can improve the security in Preparation of Catalyst and the use, determining this technology can be widely used in the denitration of China's stationary source and moving source.At present, research and development non-vanadium SCR catalyst with low cost, the eco-friendly hot subject that is domestic and international academia and industrial circle.In fact, under not sulfur-bearing, dustless, anhydrous condition, a lot of catalyst have all presented excellent NOx detergent power, but their great majority do not possess the ability of the anti-sulphur of long-time anti-water.
Summary of the invention
In order to overcome the defective of above-mentioned prior art, the object of the present invention is to provide a kind of Ferric Sulfate Hydrafe agent and preparation method thereof, be used for fixing source and moving source denitration, be implemented in high-sulfur, high dirt, high humidity and be that efficient catalytic purifies NOx in the applied environment of principal character, this catalyst at 300 ℃~450 ℃ to NH
3-SCR reaction is very efficient, and has good stable, adapts to stricter emission regulation demands, and reaches the purpose that reduces cost and improve safety in utilization.
In order to achieve the above object, technical scheme of the present invention is achieved in that
A kind of preparation method of Ferric Sulfate Hydrafe agent may further comprise the steps:
Step 1, preparation ferrum sulfuricum oxydatum solutum, ferric sulfate accounts for 0.1~0.3% of whole solution quality;
Step 3, the white thick material in the step 2 is placed in the baking oven in 110~120 ℃ of drying 12~24h, puts into Muffle furnace again in 300~500 ℃ of roastings 2~6 hours, sieving in 8~15Mpa pressure compressing tablet, 40~60 orders then just obtains Fe
2(SO
4)
3/ TiO
2Catalyst, the Ferric Sulfate Hydrafe agent that promptly will prepare.
The preparation method of Ferric Sulfate Hydrafe agent, can also be according to the following steps:
Step 1, preparation iron nitrate solution, ferric nitrate accounts for 0.1~0.3% of whole solution quality;
Step 3, with gained Fe in the step 2
2O
3/ TiO
2Catalyst is placed in the tubular react furnace, passes through 500~1000ppm SO in 300~500 ℃
2Make its sulfuration 24~36 hours, obtain Fe
2(SO
4)
3/ TiO
2Catalyst, the Ferric Sulfate Hydrafe agent that promptly will prepare.
More than the Ferric Sulfate Hydrafe agent chemical formula that obtains of two kinds of methods be Fe
2(SO
4)
3/ TiO
2, its each several part component is: ferric sulfate accounts for the 6.7-22.2% of total catalyst weight, TiO
2Account for the 77.8-93.3% of total catalyst weight.
The present invention is an active component with ferric sulfate or ferric nitrate, and anatase titania is a carrier, prepares denitrating catalyst with infusion process or coprecipitation, thus reach do not adopt vanadium be active component and can be under the high-sulfur high humidity environment the effective purpose of catalytic reduction of NOx.
Technical characterictic of the present invention also is: the present invention relates to a kind of denitrating catalyst under high-sulfur, high dirt, super-humid conditions, major technique is that with ferric sulfate or ferric nitrate be active component, anatase titania is a carrier, preparing catalyst with infusion process or coprecipitation, is that reducing agent effectively will be reduced into N as the NOx in steam power plant, smeltery, oil plant and the exhaust gas from diesel vehicle in the industrial production with the ammonia
2
The present invention compared with prior art has the following advantages and the high-lighting effect: do not adopt virose active component V
2O
5Thereby, alleviated pollution to environment, effectively improved the performance of catalyst.Metal oxide catalyst of the present invention is in 300~500 ℃ of scopes, and the purification efficiency of nitrogen oxide reaches 70-100%.Ferric Sulfate Hydrafe agent among the present invention still can the efficient catalytic nitrogen oxides reduction in the presence of water and sulfur dioxide.
Description of drawings
Fig. 1 is the influence figures of different preparation methods to Ferric Sulfate Hydrafe agent activity, and wherein abscissa is a reaction temperature; Ordinate is the NOx conversion ratio.
Fig. 2 is different Fe
2(SO
4)
3Load capacity is to Fe
2(SO
4)
3/ TiO
2Catalyst activity influence figure, wherein abscissa is a reaction temperature; Ordinate is the NOx conversion ratio.
Fig. 3 is H
2O and SO
2To the figure that influences of Ferric Sulfate Hydrafe agent activity, wherein abscissa is the reaction time; Ordinate is the NOx conversion ratio.
The specific embodiment
Embodiment one
Present embodiment may further comprise the steps:
Step 1, preparation ferrum sulfuricum oxydatum solutum, ferric sulfate accounts for 0.3% of whole solution quality;
Step 3, the white thick material in the step 2 is placed in baking oven in 120 ℃ of dry 24h, puts into Muffle furnace again in 500 ℃ of roastings 2 hours, sieving in 15Mpa pressure compressing tablet, 60 orders then just obtains Fe
2(SO
4)
3/ TiO
2Catalyst, the Ferric Sulfate Hydrafe agent that promptly will prepare.
The Ferric Sulfate Hydrafe agent chemical formula that present embodiment obtains is Fe
2(SO
4)
3/ TiO
2, its each several part component is: ferric sulfate accounts for 22.2% of total catalyst weight, TiO
2Account for 77.8% of total catalyst weight.
At 500ppm NH
3, 500ppm NO, 3%O
2, N
2Under the reaction condition for balance gas, test Fe
2(SO
4)
3/ TiO
2Activity of such catalysts.Gained result black triangle curve map as shown in Figure 1, Fe
2(SO
4)
3/ TiO
2Catalyst catalytic performance the best can obviously transform NOx under 300~450 ℃, conversion ratio reaches more than 99%.
Embodiment two
Present embodiment may further comprise the steps:
Step 1, preparation ferrum sulfuricum oxydatum solutum, ferric sulfate accounts for 0.1% of whole solution quality;
Step 3, the white thick material in the step 2 is placed in baking oven in 110 ℃ of dry 12h, puts into Muffle furnace again in 300 ℃ of roastings 6 hours, sieving in 8Mpa pressure compressing tablet, 40 orders then just obtains Fe
2(SO
4)
3/ TiO
2Catalyst, the Ferric Sulfate Hydrafe agent that promptly will prepare.
The Ferric Sulfate Hydrafe agent chemical formula that present embodiment obtains is Fe
2(SO
4)
3/ TiO
2, its each several part component is: ferric sulfate accounts for 6.7% of total catalyst weight, TiO
2Account for 93.3% of total catalyst weight.
Embodiment three
Present embodiment may further comprise the steps:
Step, preparation ferrum sulfuricum oxydatum solutum, ferric sulfate accounts for 0.2% of whole solution quality;
Step 3, the white thick material in the step 2 is placed in baking oven in 115 ℃ of dry 18h, puts into Muffle furnace again in 400 ℃ of roastings 4 hours, sieving in 12Mpa pressure compressing tablet, 50 orders then just obtains Fe
2(SO
4)
3/ TiO
2Catalyst, the Ferric Sulfate Hydrafe agent that promptly will prepare.
The Ferric Sulfate Hydrafe agent chemical formula that present embodiment obtains is Fe
2(SO
4)
3/ TiO
2, its each several part component is: ferric sulfate accounts for 15.2% of total catalyst weight, TiO
2Account for 84.8% of total catalyst weight.
At 500ppm NH
3, 500ppm NO, 3%O
2, N
2The reaction atmosphere of balance gas is the Fe of the above-mentioned different iron contents of test down
2(SO
4)
3/ TiO
2Activity of such catalysts, result are as shown in Figure 2.The Fe of mass content 8%
2(SO
4)
3The Fe that obtains as active constituent loading
2(SO
4)
3/ TiO
2Catalyst has best catalytic activity, the broadest active temperature windows.This shows that this catalyst is suitable for 8% mass content Fe
2(SO
4)
3Prepare under the condition.
At 500ppm NH
3, 500ppm NO, 3%O
2, 10%H
2O, 100ppm SO
2, N
2Be balance gas, be stabilized under 350 ℃ the reaction condition, test Fe
2(SO
4)
3/ TiO
2Activity of such catalysts, result are as shown in Figure 3.This catalyst exists at water and sulfur dioxide still can keep about 99% NOx conversion ratio under the situation, show that this catalyst has very strong anti-water sulfur resistance.
Embodiment four
Present embodiment may further comprise the steps:
Step 1, preparation iron nitrate solution, ferric nitrate accounts for 0.3% of whole solution quality;
Step 3, with gained Fe in the step 2
2O
3/ TiO
2Catalyst is placed in the tubular react furnace, passes through 1000ppm SO in 300 ℃
2Make its sulfuration 24 hours, obtain Fe
2(SO
4)
3/ TiO
2Catalyst, the Ferric Sulfate Hydrafe agent that promptly will prepare.
The Ferric Sulfate Hydrafe agent chemical formula that present embodiment obtains is Fe
2(SO
4)
3/ TiO
2, its each several part component is: ferric sulfate accounts for 22.2% of total catalyst weight, TiO
2Account for 77.8% of total catalyst weight.
At 500ppm NH
3, 500ppm NO, 3%O
2, N
2Under the reaction condition for balance gas, test Fe
2(SO
4)
3/ TiO
2Activity of such catalysts.Gained result hollow triangle curve map as shown in Figure 1, have with embodiment one in Fe
2(SO
4)
3/ TiO
2Similar activity, its temperature range is at 300~450 ℃.
Embodiment five
Present embodiment may further comprise the steps:
Step 1, preparation iron nitrate solution, ferric nitrate accounts for 0.1% of whole solution quality;
Step 3, with gained Fe in the step 2
2O
3/ TiO
2Catalyst is placed in the tubular react furnace, passes through 500ppm SO in 500 ℃
2Make its sulfuration 36 hours, obtain Fe
2(SO
4)
3/ TiO
2Catalyst, the Ferric Sulfate Hydrafe agent that promptly will prepare.
The Ferric Sulfate Hydrafe agent chemical formula that present embodiment obtains is Fe
2(SO
4)
3/ TiO
2, its each several part component is: ferric sulfate accounts for 6.7% of total catalyst weight, TiO
2Account for 93.3% of total catalyst weight.
Embodiment six
Present embodiment may further comprise the steps:
Step 1, preparation iron nitrate solution, ferric nitrate accounts for 0.2% of whole solution quality;
Step 3, with gained Fe in the step 2
2O
3/ TiO
2Catalyst is placed in the tubular react furnace, passes through 800ppm SO in 400 ℃
2Make its sulfuration 30 hours, obtain Fe
2(SO
4)
3/ TiO
2Catalyst, the Ferric Sulfate Hydrafe agent that promptly will prepare.
The Ferric Sulfate Hydrafe agent chemical formula that present embodiment obtains is Fe
2(SO
4)
3/ TiO
2, its each several part component is: ferric sulfate accounts for 15.2% of total catalyst weight, TiO
2Account for 84.8% of total catalyst weight.
Claims (8)
1. the preparation method of a Ferric Sulfate Hydrafe agent is characterized in that, may further comprise the steps:
Step 1, preparation ferrum sulfuricum oxydatum solutum, ferric sulfate accounts for 0.1~0.3% of whole solution quality;
Step 2, in above-mentioned ferrum sulfuricum oxydatum solutum, add TiO
2Carrier is with magneton electric mixer stirring reaction 4~6h under 70~90 ℃ of temperature conditions, wherein iron and TiO in the ferrum sulfuricum oxydatum solutum
2The mass ratio of carrier is 2~8%, obtains white thick material after the moisture of gained solution evaporates fully;
Step 3, the white thick material in the step 2 is placed in baking oven in 110~120 ℃ of drying 12~24h, puts into Muffle furnace again in 300~500 ℃ of roastings 2~6 hours, sieving in 8~15Mpa pressure compressing tablet, 40~60 orders then just obtains Fe
2(SO
4)
3/ TiO
2Catalyst, the Ferric Sulfate Hydrafe agent that promptly will prepare.
2. the preparation method of a kind of Ferric Sulfate Hydrafe agent according to claim 1 is characterized in that, may further comprise the steps:
Step 1, preparation ferrum sulfuricum oxydatum solutum, ferric sulfate accounts for 0.3% of whole solution quality;
Step 2, in above-mentioned ferrum sulfuricum oxydatum solutum, add TiO
2Carrier is with magneton electric mixer stirring reaction 6h under 90 ℃ of temperature conditions, wherein iron and TiO in the ferrum sulfuricum oxydatum solutum
2The mass ratio of carrier is 8%, obtains white thick material after the moisture of gained solution evaporates fully;
Step 3, the white thick material in the step 2 is placed in baking oven in 120 ℃ of dry 24h, puts into Muffle furnace again in 500 ℃ of roastings 2 hours, sieving in 15Mpa pressure compressing tablet, 60 orders then just obtains Fe
2(SO
4)
3/ TiO
2Catalyst, the Ferric Sulfate Hydrafe agent that promptly will prepare.
3. the preparation method of a Ferric Sulfate Hydrafe agent is characterized in that, may further comprise the steps:
Step 1, preparation iron nitrate solution, ferric nitrate accounts for 0.1~0.3% of whole solution quality;
Step 2, in above-mentioned iron nitrate solution, add TiO
2Carrier is with magneton electric mixer stirring reaction 4~6h under 70~90 ℃ of temperature conditions, wherein iron and TiO in the iron nitrate solution
2The mass ratio of carrier is 2~8%, and the moisture of gained solution obtains Fe after evaporating fully
2O
3/ TiO
2Catalyst;
Step 3, with gained Fe in the step 2
2O
3/ TiO
2Catalyst is placed in the tubular react furnace, passes through 500~1000ppm SO in 300~500 ℃
2Make its sulfuration 24~36 hours, obtain Fe
2(SO
4)
3/ TiO
2Catalyst, the Ferric Sulfate Hydrafe agent that promptly will prepare.
4. the preparation method of a kind of Ferric Sulfate Hydrafe agent according to claim 3 is characterized in that, may further comprise the steps:
Step 1, preparation iron nitrate solution, ferric nitrate accounts for 0.3% of whole solution quality;
Step 2, in above-mentioned iron nitrate solution, add TiO
2Carrier is with magneton electric mixer stirring reaction 6h under 90 ℃ of temperature conditions, wherein iron and TiO in the iron nitrate solution
2The mass ratio of carrier is 8%, and the moisture of gained solution obtains Fe after evaporating fully
2O
3/ TiO
2Catalyst;
Step 3, with gained Fe in the step 2
2O
3/ TiO
2Catalyst is placed in the tubular react furnace, passes through 1000ppm SO in 300 ℃
2Make its sulfuration 24 hours, obtain Fe
2(SO
4)
3/ TiO
2Catalyst, the Ferric Sulfate Hydrafe agent that promptly will prepare.
5. a Ferric Sulfate Hydrafe agent is characterized in that, Ferric Sulfate Hydrafe agent chemical formula is Fe
2(SO
4)
3/ TiO
2, its each several part component is: ferric sulfate accounts for the 6.7-22.2% of total catalyst weight, TiO
2Account for the 77.8-93.3% of total catalyst weight.
6. a kind of Ferric Sulfate Hydrafe agent according to claim 5 is characterized in that Ferric Sulfate Hydrafe agent chemical formula is Fe
2(SO
4)
3/ TiO
2, its each several part component is: ferric sulfate accounts for 22.2% of total catalyst weight, TiO
2Account for 77.8% of total catalyst weight.
7. a kind of Ferric Sulfate Hydrafe agent according to claim 5 is characterized in that Ferric Sulfate Hydrafe agent chemical formula is Fe
2(SO
4)
3/ TiO
2, its each several part component is: ferric sulfate accounts for 6.7% of total catalyst weight, TiO
2Account for 93.3% of total catalyst weight.
8. a kind of Ferric Sulfate Hydrafe agent according to claim 5 is characterized in that Ferric Sulfate Hydrafe agent chemical formula is Fe
2(SO
4)
3/ TiO
2, its each several part component is: ferric sulfate accounts for 15.2% of total catalyst weight, TiO
2Account for 84.8% of total catalyst weight.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102701315A (en) * | 2012-06-28 | 2012-10-03 | 厦门大学 | Method for processing dye wastewater by applying nanocomposite photocatalyst combination-Fenton |
CN111389419A (en) * | 2020-03-31 | 2020-07-10 | 北京化工大学 | Cerium dioxide loaded ferric sulfate catalyst and preparation method and application thereof |
CN113231085A (en) * | 2021-05-25 | 2021-08-10 | 北京化工大学 | Ferric sulfate modified red mud-based denitration catalyst and preparation method and application thereof |
-
2010
- 2010-11-01 CN CN 201010529669 patent/CN102008967A/en active Pending
Non-Patent Citations (1)
Title |
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《清华大学本科生毕业论文》 20071231 毛颖 负载型硫酸盐/氧化物脱硝催化剂研究 21页第3.1.1.1节 1-8 , 2 * |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102701315A (en) * | 2012-06-28 | 2012-10-03 | 厦门大学 | Method for processing dye wastewater by applying nanocomposite photocatalyst combination-Fenton |
CN102701315B (en) * | 2012-06-28 | 2014-04-09 | 厦门大学 | Method for processing dye wastewater by applying nanocomposite photocatalyst combination-Fenton |
CN111389419A (en) * | 2020-03-31 | 2020-07-10 | 北京化工大学 | Cerium dioxide loaded ferric sulfate catalyst and preparation method and application thereof |
CN111389419B (en) * | 2020-03-31 | 2021-07-20 | 北京化工大学 | Cerium dioxide loaded ferric sulfate catalyst and preparation method and application thereof |
CN113231085A (en) * | 2021-05-25 | 2021-08-10 | 北京化工大学 | Ferric sulfate modified red mud-based denitration catalyst and preparation method and application thereof |
CN113231085B (en) * | 2021-05-25 | 2023-06-27 | 北京化工大学 | Ferric sulfate modified red mud-based denitration catalyst and preparation method and application thereof |
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Application publication date: 20110413 |