CN106492821A - A kind of efficient cryogenic sulfur resistive water resistant cooperates with the preparation method of denitration demercuration catalyst - Google Patents
A kind of efficient cryogenic sulfur resistive water resistant cooperates with the preparation method of denitration demercuration catalyst Download PDFInfo
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- CN106492821A CN106492821A CN201610857931.2A CN201610857931A CN106492821A CN 106492821 A CN106492821 A CN 106492821A CN 201610857931 A CN201610857931 A CN 201610857931A CN 106492821 A CN106492821 A CN 106492821A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8621—Removing nitrogen compounds
- B01D53/8625—Nitrogen oxides
- B01D53/8628—Processes characterised by a specific catalyst
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8665—Removing heavy metals or compounds thereof, e.g. mercury
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/889—Manganese, technetium or rhenium
- B01J23/8892—Manganese
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
Abstract
The present invention provides the preparation method that a kind of efficient cryogenic sulfur resistive water resistant cooperates with denitration demercuration catalyst, belongs to environmental protection technical field.The method loads various metals salt by catalyst support surface directed modification, with equi-volume impregnating optimization, then obtains high efficient cryogenic denitration demercuration catalyst through fumed pyrogenic.The catalyst is under cryogenic to NOxAnd Hg0Up to 98% and 92% catalytic purification efficiency is respectively provided with, while there is stronger tolerance to water and sulfur dioxide, and with longer catalytic life.This method process conditions are simple, and raw material is cheap, workable, are suitable for large-scale production, with very high practical value, are particularly well-suited to the efficient removal of the industry nitrogen oxides such as power plant, iron and steel.
Description
Technical field
The present invention relates to environmental protection technical field, particularly relates to a kind of efficient cryogenic sulfur resistive water resistant collaboration denitration demercuration and urges
The preparation method of agent.
Background technology
In technical field of air pollution control, due to the sulfur dioxide of chemical plant combustion of fossil fuel discharge（SO2）Nitrogen
Oxide（NOx）With heavy metal element mercury（Hg）Ecological environment and human health, wherein, NO have been had a strong impact onxHarm with Hg
Receive more and more attention, obtain the efficient process technology of both pollutants more urgent.
In NOxIn the control method of pollution, based on NH3SCR for reducing agent（SCR）Due to its efficiently,
Convenient wait good characteristic and in NOxIt is widely adopted in control.But, it is water-fast that SCR denitration catalyst generally there are resistant to sulfur（Steam
Vapour）Performance is strong, not high low temperature active and the problems such as interval narrow active temperature.Wide variety of SCR catalyst has been obtained
In, V2O5Base catalyst is used in denitration field for a long time because of its high efficiency, but the toxicity of V element and V2O5To reaction
The high request of temperature causes which to be difficult to meet at present for the requirement of low-carbon environment-friendly.In recent years, research finds the catalysis of low temperature manganese base
Agent is in NH3NO for reducing agentxThere is in SCR higher activity, but at low temperature, mixed gas are deposited on a small quantity
SO2The activity of destruction catalyst can be had a strong impact on.SO2By with NH3Reaction generates the difficult NH for decomposing under low temperature4HSO4Blocking
The avtive spot of catalyst, or react with catalytically-active materials and generate stable sulphate cpd and cause catalyst to lose work
The modes such as property cause catalyst to be difficult to play preferable clean-up effect.The humidity problem of catalysis system also can be to numerous SCR simultaneously
The performance of catalyst activity produces impact.Simultaneously, the narrow catalyst activity that also limit of catalyst activity temperature window
Stable performance.
At the same time, above-mentioned SCR methods are little to the removing effect of heavy metal Hg present in flue gas, and this is primarily due to unit
Nonvalent mercury in plain Hg（Hg0）Compared with Hg2+Plasma state mercury is more difficult to remove, and the Hg in flue gas is more with Hg0Exist.At present, waste gas
The purification of middle gaseous mercury, mainly passes through activated carbon injection technique（activated carbon injection
technologies）, this method can effectively remove gaseous mercury, but the technical operation cost is very big, nor
NO in waste gas can effectively be removed simultaneouslyx.Therefore develop
With removing NOxAnd Hg0Catalyst significant.
Content of the invention
The technical problem to be solved in the present invention is to provide a kind of low temperature（160-360℃）Efficiently sulfur resistive water resistant collaboration denitration takes off
The preparation method of mercury catalyst.By commercial γ-Al2O3The directed modification of carrier surface group, with certain proportioning by various metals
Oxide optimizes uniform load in the adorned catalyst carrier in surface, is obtained there is the low of excellent properties after fumed pyrogenic
Warm sulfur resistive water resistant denitration demercuration catalyst.
The method is comprised the following steps that：
（1）By commercializationγ-Al2O3Carrier surface group is oriented modification, obtains the carrier for being catalyzed sample；
（2）By step（1）Obtained carrier impregnation impregnates low temperature after certain time in the metal salt solution of certain mass concentration
Dry；
（3）By step（2）The sample obtained after middle drying carries out high-temperature calcination pyrolysis, and catalyst is obtained.
Wherein：Step（1）Middle commercial γ-Al2O3The specific surface area of carrier is 100-400m2/ g, directed modification method of modifying
Modified by the combination of different order for sour modified, alkali modification or both.
Sour modified acid solution used is following at least one：Sulfuric acid, nitric acid, hydrochloric acid, acetic acid；Used by alkali modification, alkalescence is molten
Liquid is following at least one：NaOH, ammoniacal liquor, sodium carbonate, sodium acid carbonate；The concentration of bronsted lowry acids and bases bronsted lowry used by modified is 0.1-10
M, preferably 0.5-4 M, more preferably 1-2 M, modification time are 0.5-72 h.
Step（2）Middle metal salt solution is following at least one：Manganese acetate, nickel acetate, cerous nitrate, copper nitrate, cobalt nitrate,
Ferric nitrate；Metal salt solution mass concentration scope is 1-40%, and preferably 5-30%, more preferably 5-20%, dip time are 0.5-
48 h.
Step（3）Described in fumed pyrogenic temperature be 200-750 DEG C, calcination time be 2-12 h；In calcination process, rise
Warm speed and cooling rate are 1-30 DEG C/min.
The above-mentioned technical proposal of the present invention has the beneficial effect that：
In such scheme, raw material sources are wide, and preparation process is simple, catalyst low cost are easy to prepare and are promoted；Meanwhile, low temperature
The catalyst of lower preparation is to NOxPurification efficiency high, to SO2And H2O has a good resistance, and can long circulating stable.
Specific embodiment
For making the technical problem to be solved in the present invention, technical scheme and advantage clearer, below in conjunction with being embodied as
Example is described in detail.
The present invention provides the preparation method that a kind of efficient cryogenic sulfur resistive water resistant cooperates with denitration demercuration catalyst.
Embodiment 1：
By commercial γ-Al2O3Carrier is placed in the sulfuric acid of 1 M and soaks 24 h, after 80 DEG C of dryings.By dried γ-
Al2O3Carrier impregnation be respectively in mass fraction 6.7%, 6.7%, 6.7% and 1% cerous nitrate, manganese acetate, copper nitrate, ferric nitrate
In mixed solution.After impregnating 24 h, it is vacuum dried in 80 DEG C, is placed in Muffle furnace after drying, is risen to the speed of 5 DEG C/min
450 DEG C, after 8 h of constant temperature, naturally cool to room temperature.
By the catalysis sample obtained in embodiment 1,0.500 g is taken for experimental subjects, with nitrogen as Balance Air, in 160-
360 DEG C of temperature range is interior, 10000/h of air speed, CNO=1000 ppm、CNH3=1000 ppm、CHg0 concentration=50 μ g/m3, oxygen
NO under the conditions of concentration=10%xConversion ratio at 240 DEG C for 92%, Hg0Conversion ratio be 90%.
Embodiment 2：
Other conditions are same as Example 1, and difference is that the mass fraction of transition metal salt solution is 10%, 10% and 20%
Cerous nitrate, manganese acetate, in copper nitrate mixed solution, other conditions and test condition are identical with 1, the catalysis sample NO's
Conversion ratio highest at 280 DEG C, about 76%, Hg0Conversion ratio be 75%, poor compared with Example 1.
Embodiment 3：
Other conditions are same as Example 1, and difference is the nitre that the mass fraction of transition metal salt solution is 2%, 3% and 5%
In the mixed solution of sour cerium, manganese acetate and copper nitrate, other conditions and test condition are identical with 1, the catalysis sample NO's
Conversion ratio is 240oHighest during C, about 80%, Hg0Conversion ratio be 76%, poor compared with Example 1.
Embodiment 4：
Other conditions are same as Example 1, and difference is that the mass fraction of transition metal salt solution is 8.3%, 8.3% and
In the mixed solution of 8.3% cerous nitrate, manganese acetate and copper nitrate, other conditions and test condition are identical with 1, the catalysis
Sample NOxConversion ratio 240oHighest during C, about 90%, Hg0Conversion ratio be 85%, poor compared with Example 1.
Embodiment 5：
Other conditions are same as Example 1, difference be transition metal salt solution for manganese acetate that mass fraction is 8%, 8%
Cerous nitrate and 4% copper nitrate mixed solution, other conditions and test condition identical with 1, the catalysis sample NOx's
Conversion ratio is 240oIt is 78%, Hg during C0Conversion ratio be 71%, poor compared with Example 1.
Embodiment 6：
Other conditions are same as Example 1, and difference is commercial γ-Al2O3The method of modifying of carrier surface group, will
γ-Al2O3Carrier is successively respectively placed in the hydrochloric acid and sodium hydroxide solution of 0.5 M, other conditions and test condition and 1 phase
With the catalysis sample NOxConversion ratio when being not less than 240 DEG C for 98%, Hg0Conversion ratio be 92%, compared with Example 1
Slightly higher.
Embodiment 7：
Other conditions are same as Example 6, and difference is commercial γ-Al2O3The method of modifying of carrier surface group, will
γ-Al2O3Carrier is successively respectively placed in the hydrochloric acid and sodium hydroxide solution of 10 M, other conditions and test condition and 6 phases
With the catalysis sample NOxConversion ratio when being not less than 240 DEG C for 95%, Hg0Conversion ratio be 93%, compared with Example 6
Lower slightly.
Embodiment 8：
The catalyst that will be obtained in embodiment 6, takes 0.500g for experimental subjects, with nitrogen as Balance Air, 240oThe temperature of C
Under, 10000/h of air speed, CNO=1000 ppm、CNH3=1000 ppm、CHg0 concentration=50 μ g/m3, oxygen concentration=10%, reaction
After 26 h, NOxRemoval efficiency maintain more than 90%, Hg0Conversion ratio be not less than 90%.
Embodiment 9：
By the catalysis sample obtained in embodiment 6,0.500 g is taken for experimental subjects, with nitrogen as Balance Air, 240oThe temperature of C
Under degree, 10000/h of air speed, CNO=1000 ppm、CNH3=1000 ppm、CHg0 concentration=50 μ g/m3, oxygen concentration=10%, reaction
After 10 minutes, steam, NO is pumped into toward reaction systemxRemoval efficiency progressively drop to 80% by 95% and maintain stable, Hg0Conversion
Rate is then reduced to 78%, after stopping pumping into steam toward system, NOxAnd Hg0Removal efficiency be gradually restored to 93% and 90% or so respectively.
Embodiment 10：
The catalyst that will be obtained in embodiment 6, takes 0.500 g for experimental subjects, with nitrogen as Balance Air, in 240 DEG C of temperature
Under, 10000/h of air speed, CNO=1000 ppm、CNH3=1000 ppm、CHg0 concentration=50 μ g/m3, oxygen concentration=10%, reaction 10
After minute, 200 ppm SO are pumped into toward reaction system2, NOxRemoval efficiency rise to 98% by 95%, be passed through 200 after stopping
ppm SO2NO afterwardsxRemoval efficiency fall back to 95%, Hg0Efficiency substantially uninfluenced.When continuation pumps into 600 toward reaction system
ppm SO2Afterwards, NOx、Hg0Removal efficiency drop to 70% or so, stop pumping into SO toward system2Afterwards, NOx、Hg0Removal efficiency do not have
There is recovery.
Embodiment 11：
The catalyst that will be obtained in embodiment 6, takes 0.500g for experimental subjects, with nitrogen as Balance Air, in 240 DEG C of temperature
Under, 10000/h of air speed, CNO=1000 ppm、CNH3=1000 ppm、CHg0 concentration=50 μ g/m3, oxygen concentration=10%, reaction 10
After minute, toward reaction system, pump into steam and 200 ppm SO simultaneously2, NOxRemoval efficiency progressively drop to 70%, when stop past
System pumps into steam and SO2Afterwards, NOxAnd Hg0Removal efficiency then go up for 75% or so.
Can by the comparison of embodiment 1, embodiment 2, embodiment 3, embodiment 4, embodiment 5, embodiment 6 and embodiment 7
See, when carrier is with soda acid alkali lye combined modification, the cerous nitrate that metal salt solution is 6.7%, 6.7%, 6.7% and 1%, manganese acetate, nitre
During the mixed solution of sour copper and ferric nitrate, denitration performance is optimal.Can by embodiment 8, embodiment 9, embodiment 10 and embodiment 11
See, the catalyst that the method is prepared has good cycle performance, to H2O and SO2There is preferable resistance.
In sum, the catalyst in the present invention has excellent denitration demercuration performance at low temperature, while water resistant sulfur resistive
Ability is projected.Sample preparation is simple, and raw material is cheap, with good application prospect.
The above is the preferred embodiment of the present invention, it is noted that for those skilled in the art
For, on the premise of without departing from principle of the present invention, some improvements and modifications can also be made, these improvements and modifications
Should be regarded as protection scope of the present invention.
Claims (9)
1. a kind of efficient cryogenic sulfur resistive water resistant cooperates with the preparation method of denitration demercuration catalyst, it is characterised in that：Including following step
Suddenly：
（1）By commercializationγ-Al2O3Carrier surface group is oriented modification, obtains the carrier for being catalyzed sample；
（2）By step（1）Obtained carrier impregnation impregnates low temperature after certain time in the metal salt solution of certain mass concentration
Dry；
（3）By step（2）The sample obtained after middle drying carries out high-temperature calcination pyrolysis, and catalyst is obtained.
2. efficient cryogenic sulfur resistive water resistant according to claim 1 cooperates with the preparation method of denitration demercuration catalyst, its feature
It is：The step（1）Middle commercial γ-Al2O3The specific surface area of carrier is 100-400m2/ g, the directed modification method of modifying
Modified by the combination of different order for sour modified, alkali modification or both.
3. efficient cryogenic sulfur resistive water resistant according to claim 2 cooperates with the preparation method of denitration demercuration catalyst, its feature
It is：Acid solution used by the acid is modified is following at least one：Sulfuric acid, nitric acid, hydrochloric acid, acetic acid；Alkalescence used by alkali modification
Solution is following at least one：NaOH, ammoniacal liquor, sodium carbonate, sodium acid carbonate；The concentration of bronsted lowry acids and bases bronsted lowry used by modified is 0.1-10
M, modification time are 0.5-72 h.
4. efficient cryogenic sulfur resistive water resistant according to claim 3 cooperates with the preparation method of denitration demercuration catalyst, its feature
It is：The concentration of the modification bronsted lowry acids and bases bronsted lowry is 0.5-4 M.
5. efficient cryogenic sulfur resistive water resistant according to claim 3 cooperates with the preparation method of denitration demercuration catalyst, its feature
It is：The concentration of the modification bronsted lowry acids and bases bronsted lowry is 1-2 M.
6. efficient cryogenic sulfur resistive water resistant according to claim 1 cooperates with the preparation method of denitration demercuration catalyst, its feature
It is：The step（2）Middle metal salt solution is following at least one：Manganese acetate, nickel acetate, cerous nitrate, copper nitrate, nitric acid
Cobalt, ferric nitrate；Metal salt solution mass concentration scope is 1-40%, and dip time is 0.5-48 h.
7. efficient cryogenic sulfur resistive water resistant according to claim 6 cooperates with the preparation method of denitration demercuration catalyst, its feature
It is：The metal salt solution mass concentration scope is 5-30%.
8. efficient cryogenic sulfur resistive water resistant according to claim 6 cooperates with the preparation method of denitration demercuration catalyst, its feature
It is：The metal salt solution mass concentration scope is 5-20%.
9. efficient cryogenic sulfur resistive water resistant according to claim 1 cooperates with the preparation method of denitration demercuration catalyst, its feature
It is：The step（3）Described in fumed pyrogenic temperature be 200-750 DEG C, calcination time be 2-12 h；In calcination process, rise
Warm speed and cooling rate are 1-30 DEG C/min.
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| CN107469812A (en) * | 2017-10-10 | 2017-12-15 | 北京科技大学 | NO in low temperature removing coal combustion exhaustxWith VOCs method for preparing catalyst |
| CN107715867A (en) * | 2017-10-10 | 2018-02-23 | 北京科技大学 | NO in low temperature removing coal combustion exhaustxAnd Hg0Method for preparing catalyst |
| CN108686651A (en) * | 2018-05-30 | 2018-10-23 | 临沂大学 | A kind of catalyst and its preparation method and application of flue gas denitration demercuration simultaneously |
| CN113750953A (en) * | 2021-09-27 | 2021-12-07 | 山东大学 | SO in pyrolysis flue gas2、H2S and Hg0Synergistic desorption adsorbent and preparation method thereof |
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| CN113750953A (en) * | 2021-09-27 | 2021-12-07 | 山东大学 | SO in pyrolysis flue gas2、H2S and Hg0Synergistic desorption adsorbent and preparation method thereof |
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