CN106622380B - A kind of denitrating catalyst and its preparation method and application - Google Patents

A kind of denitrating catalyst and its preparation method and application Download PDF

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CN106622380B
CN106622380B CN201611227701.4A CN201611227701A CN106622380B CN 106622380 B CN106622380 B CN 106622380B CN 201611227701 A CN201611227701 A CN 201611227701A CN 106622380 B CN106622380 B CN 106622380B
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catalyst
denitrating catalyst
denitrating
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zinc
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CN106622380A (en
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白书立
李换英
刘敏超
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Wuyi University
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    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J31/00Catalysts comprising hydrides, coordination complexes or organic compounds
    • B01J31/26Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
    • B01J31/28Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of the platinum group metals, iron group metals or copper
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34Chemical or biological purification of waste gases
    • B01D53/74General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/86Catalytic processes
    • B01D53/8621Removing nitrogen compounds
    • B01D53/8625Nitrogen oxides
    • B01D53/8628Processes characterised by a specific catalyst
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34Chemical or biological purification of waste gases
    • B01D53/74General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/86Catalytic processes
    • B01D53/90Injecting reactants
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00Catalysts, in general, characterised by their form or physical properties
    • B01J35/60Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J35/61Surface area
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2258/00Sources of waste gases
    • B01D2258/02Other waste gases
    • B01D2258/0283Flue gases

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Abstract

The present invention relates to a kind of denitrating catalysts and its preparation method and application, belong to catalyst technical field.Catalyst of the invention is using ZIFs mesopore molecular sieve as carrier, and active principle includes the oxide of zinc, the oxide of iron, cerium.Denitrating catalyst of the invention is carrier using ZIFs mesopore molecular sieve, and specific surface greatly increases, and is conducive to adsorb and activate more flue gases, improves denitration efficiency;Carrier and active component while one-step synthesis when preparation, can be enhanced the composite attribute of ferro element and Ce elements, improve active component in the dispersion degree and bond strength of carrier surface, the mechanical strength and thermal stability of catalyst;Catalyst granules is thinner, and active component is uniformly dispersed, denitration activity, wider denitration temperature range and anti-SO with higher2Activity;Reduce energy consumption without 100% desulfurization without heating when denitrating catalyst is applied to denitrating flue gas.

Description

A kind of denitrating catalyst and its preparation method and application
Technical field
The present invention relates to denitrating catalysts, and in particular to a kind of denitrating catalyst and its preparation method and application belongs to and urges Agent technical field.
Background technique
Reacting removing atmosphere pollution NO with selective catalytic reduction (SCR) is an effective method.SCR denitrating flue gas The key of technology is the excellent catalyst of selection.SCR catalyst answer it is active it is high, anti-poisoning capability is strong, mechanical strength and resistance to Polishing machine is good, has the characteristics that suitable operation temperature section.Preferably it is with most widely used industrial SCR catalyst at present V2O5/TiO2And V2O5-WO3/TiO2Catalyst, major advantage show high activity and high antisulphuric ability, but such catalyst (> 350 DEG C) applications at a higher temperature are needed, to avoid the SO in flue gas2With NH3React the NH generated4HSO4(NH4)2S2O7The pore structure of blocking catalyst.But high-temperature operation results in the increase of energy consumption and operating cost, low temperature in many cases, SCR device be conducive to China's most of Industrial Boiler matching at present, therefore, the low temperature of SCR catalyst causes generally Attention.Though current many low-temperature denitration catalysts have good denitration efficiency, vulnerable to SO2Poison and be difficult to practical application. And these catalyst mainly use coprecipitation, sol-gel method preparation these preparation methods, are easy to cause the work of catalyst Property component on carrier dispersibility it is poor, temperature window is also relatively narrow, and stability is poor.Therefore, it is necessary to develop others Low temperature sulfur resistive denitrating catalyst.
Summary of the invention
In view of the deficiencies of the prior art, the purpose of the present invention is to provide one kind to have the high sulfur resistive of bigger serface low temperature de- Denox catalyst, the denitrating catalyst can be improved anti-SO2Toxicity and low-temperature catalytic activity expand operation temperature window, thus Be conducive to industrial applications.
Above-mentioned purpose is achieved through the following technical solutions:
A kind of denitrating catalyst, the catalyst are using ZIFs mesopore molecular sieve as carrier, and active principle includes zinc, iron Oxide, cerium oxide, the content of the zinc, ferriferous oxide and cerium oxide are Zn:Fe:Ce with the molar ratio of elemental metal =0.01:0.0001:0.0001~0.01:0.0007:0.0001.
Preferably, the zinc is simple substance zinc, and the ferriferous oxide is Fe2O3, the cerium oxide is CeO2And Ce2O3In It is one or two kinds of;The zinc doping forms carrier into the ZIFs mesopore molecular sieve, to load the iron oxygen as active component Compound and cerium oxide.
Preferably, the surface area of the denitrating catalyst is 800~1200m2/g。
It is a further object to provide the preparation methods of the denitrating catalyst, comprising the following steps:
(1) by the salt solution containing zinc in solvent 1, the first solution is obtained;
(2) methylimidazole is dissolved in solvent 2, is then added in the first solution, stirs evenly, obtains mixed liquor;
(3) by after molysite and cerium salt dissolution, the second solution containing ferriferous oxide and cerium oxide is prepared;
(4) the second solution is added in the mixed liquor of step (2), then magnetic agitation is aged;
(5) material after ageing in step (4) is filtered, washed, dried, ground, then calcined again, oxygen Change, obtains solid powder, i.e. denitrating catalyst.
Preferably, the salting liquid containing zinc described in step (1) includes Zn (NO3)2.5H2O、Zn(CH3COO)2In at least one Kind;The solvent 1 includes at least one of ethyl alcohol, methanol, water, DMF;The concentration of salting liquid containing zinc in first solution For 0.03~0.04mol/L;Solvent 2 described in step (2) includes at least one of ethyl alcohol, methanol, DMF;Step (2) is mixed The concentration for closing methylimidazole described in liquid is 0.26~0.35mol/L;Step (3) described molysite include ferric nitrate, ferric acetate, At least one of ferric sulfate, the cerium salt include at least one of cerous nitrate, cerous acetate, cerium chloride;Second solution The total concentration of middle ferro element and Ce elements is 0.0002~0.0007mol/L.
Preferably, the revolving speed of step (4) described magnetic agitation is 1000~2000r/min, and the time is 2~4h;It is described old The time of change is 8~12h.
Preferably, described be filtered into of step (5) is filtered with the sintered glass filter that filter sizes are 0.22~0.45 μm; The drying is vacuum drying, and drying temperature is 100~140 DEG C, and the time is 4~8h.
Preferably, the temperature of step (5) described calcining is 350~500 DEG C, and the time is 3~5h.
It is also another object of the present invention to provide the applications of the denitrating catalyst, de- to dedusting with the denitrating catalyst Flue gas after sulphur carries out selective catalytic reduction reaction.First to flue-gas dust-removing and desulfurization, it is lower than sulfur dioxide in flue gas concentration 400ppm, then carry out low-temperature denitration, without being reheated to flue gas, energy consumption can be reduced and improving denitration effect when denitration Rate.
Preferably, SO in the flue gas after the dust-removal and desulfurizing2Concentration is 0~400ppm, and the selective catalytic reduction is anti- The temperature answered is 80~300 DEG C.
Compared with prior art, the beneficial effects of the present invention are:
1. denitrating catalyst of the invention is carrier using ZIFs mesopore molecular sieve, compares and use TiO2When for carrier, than Surface greatly increases, and is conducive to Catalyst Adsorption and activates more flue gases, improves denitration efficiency;
2. the preparation method of denitrating catalyst of the invention is carrier and active component one-step synthesis simultaneously, iron can be enhanced The composite attribute of element and Ce elements improves active component in the dispersion degree and bond strength of carrier surface, improves catalyst Mechanical strength and thermal stability;
3. denitrating catalyst of the invention is prepared as one-step synthesis, catalyst granules is thinner, and active component is uniformly dispersed, Denitration activity with higher, wider denitration temperature range and anti-sulfur dioxide activity, at 80~300 DEG C, SO in flue gas2It is dense When degree is 0~400ppm, 85% or more denitration efficiency can be reached;
4. denitrating catalyst of the invention is applied to denitrating flue gas, without heating before denitration, it is not necessarily to 100% desulfurization, is reduced Energy consumption.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph of denitrating catalyst prepared by embodiment 1.
Specific embodiment
Below with reference to specific implementation example, present invention is further described in detail, but not as a limitation of the invention.
Embodiment 1
Weigh 3gZn (NO3)2·5H2O is dissolved into wiring solution-forming in 150mL methanol;8g methylimidazole is dissolved into 150mL After mixing by two kinds of solution 50.1mg Fe (NO is added in wiring solution-forming in ethyl alcohol in the solution3)3·9H2O and 38.2mgCe(NO3)2·9H2O stirs 2h at magnetic stirring apparatus revolving speed 1000r/min, stands 10 minutes, is then aged 8h; It is filtered with 0.22 μm of sintered glass filter of filter membrane diameter, then the dry 6h in 140 DEG C of vacuum constant temperature drying boxes, grinds after taking-up It is powdered to wear into 40-60 mesh, the ZIFs mesopore molecular sieve denitration catalyst of iron cerium load is made in 500 DEG C of calcining 5h in Muffle furnace Agent, the specific surface of the catalyst are 1000m2/g。
Denitrating catalyst denitrating flue gas reaction condition obtained above are as follows: catalyst grain size is 40-60 mesh, and dosage is 200mg, reaction gas composition are as follows: NO 500ppm, NH3500ppm, 3% (percent by volume) O2、SO2400ppm uses N2 For Balance Air, the gas space velocity in reaction is 30000mL/ (gh), and 80 DEG C of reaction temperature, catalyst denitration efficiency is 86%. Catalytic perfomance data are tested in fixed-bed quartz reactor.
Embodiment 2
Weigh 2.5gZn (NO3)2·5H2O is dissolved into wiring solution-forming in 150mL ethyl alcohol;6.5g methylimidazole is dissolved into After mixing by two kinds of solution 100.2mg Fe (NO is added in wiring solution-forming in 150mLDMF in the solution3)3·9H2O and 38.2mgCe(NO3)2·9H2O stirs 2h at magnetic stirring apparatus revolving speed 1500r/min, stands 10 minutes, is aged 10h;With filter The sintered glass filter that 0.22 μm of film diameter filters, and then dry 6h, taking-up are ground into 140 DEG C of vacuum constant temperature drying boxes 40-60 mesh is powdered, 400 DEG C of calcining 4h in Muffle furnace, and the ZIFs mesopore molecular sieve denitrating catalyst of iron cerium load is made, should The specific surface of catalyst is 900m2/g。
Denitrating catalyst denitrating flue gas reaction condition obtained above are as follows: catalyst grain size is 40-60 mesh, and dosage is 200mg, reaction gas composition are as follows: NO 500ppm, NH3500ppm, 3% (percent by volume) O2、SO2400ppm uses N2 For Balance Air, the gas space velocity in reaction is 30000mL/ (gh), and 100 DEG C of reaction temperature, catalyst denitration efficiency is 88%. Catalytic perfomance data are tested in fixed-bed quartz reactor.
Embodiment 3
Weigh 3gZn (NO3)2·5H2O is dissolved into wiring solution-forming in 150mL DMF;8g methylimidazole is dissolved into After mixing by two kinds of solution 125.3mg Fe (NO is added in wiring solution-forming in 150mLDMF in the solution3)3·9H2O and 38.2mgCe(NO3)2·9H2O stirs 2h at magnetic stirring apparatus revolving speed 2000r/min, stands 10 minutes, is aged 12h;With filter 0.22 μm of sintered glass filter of film diameter filters, and then in 8h dry in 140 DEG C of vacuum constant temperature drying boxes, taking-up is ground into 40-60 mesh is powdered, 450 DEG C of calcining 4h in Muffle furnace, and the ZIFs mesopore molecular sieve denitrating catalyst of iron cerium load is made, should The specific surface of catalyst is 1200m2/g。
Denitrating catalyst denitrating flue gas reaction condition obtained above are as follows: catalyst grain size is 40-60 mesh, and dosage is 200mg, reaction gas composition are as follows: NO 500ppm, NH3500ppm, 3% (percent by volume) O2, SO2 400ppm, use N2 For Balance Air, the gas space velocity in reaction is 30000mL/ (gh), and 150 DEG C of reaction temperature, catalyst denitration efficiency is 95%. Catalytic perfomance data are tested in fixed-bed quartz reactor.
Embodiment 4
Weigh 3.5gZn (NO3)2·5H2O is dissolved into wiring solution-forming in 150mL distilled water;7.5g methylimidazole is dissolved into After mixing by two kinds of solution 150.3mg Fe (NO is added in wiring solution-forming in 150mL ethyl alcohol in the solution3)3·9H2O and 38.2mg Ce(NO3)2·9H2O stirs 2h at magnetic stirring apparatus revolving speed 2000r/min, stands 10 minutes, is aged 12h;With The sintered glass filter that 0.40 μm of filter membrane diameter filters, and then in 6h dry in 140 DEG C of vacuum constant temperature drying boxes, takes out grinding Powdered at 40-60 mesh, the ZIFs mesopore molecular sieve denitrating catalyst of iron cerium load is made in 350 DEG C of calcining 5h in Muffle furnace, The specific surface of the catalyst is 1100m2/g。
Denitrating catalyst denitrating flue gas reaction condition obtained above are as follows: catalyst grain size is 40-60 mesh, and dosage is 200mg, reaction gas composition are as follows: NO 500ppm, NH3500ppm, 3% (percent by volume) O2、SO2400ppm uses N2 For Balance Air, the gas space velocity in reaction is 30000mL/ (gh), and 200 DEG C of reaction temperature, catalyst denitration efficiency is 92%. Catalytic perfomance data are tested in fixed-bed quartz reactor.
Embodiment 5
Weigh 3gZn (NO3)2·5H2O is dissolved into wiring solution-forming in 150mL DMF;8g methylimidazole is dissolved into 150mL After mixing by two kinds of solution 250.5mg Fe (NO is added in wiring solution-forming in methanol in the solution3)3·9H2O and 38.2mgCe(NO3)2·9H2O stirs 2h at magnetic stirring apparatus revolving speed 1500r/min, stands 10 minutes, is aged 10h;With filter The sintered glass filter that 0.45 μm of film diameter filters, and then in 6h dry in 140 DEG C of vacuum constant temperature drying boxes, taking-up is ground into 40-60 mesh is powdered, 350 DEG C of calcining 3h in Muffle furnace, and the ZIFs mesopore molecular sieve denitrating catalyst of iron cerium load is made, should The specific surface of catalyst is 800m2/g。
Denitrating catalyst denitrating flue gas reaction condition obtained above are as follows: catalyst grain size is 40-60 mesh, and dosage is 200mg, reaction gas composition are as follows: NO 500ppm, NH3500ppm, 3% (percent by volume) O2、SO2400ppm uses N2 For Balance Air, the gas space velocity in reaction is 30000mL/ (gh), and 300 DEG C of reaction temperature, catalyst denitration efficiency is 85%. Catalytic perfomance data are tested in fixed-bed quartz reactor.

Claims (8)

1. a kind of denitrating catalyst, which is characterized in that the catalyst is the active principle using ZIFs mesopore molecular sieve as carrier Including zinc, ferriferous oxide, cerium oxide, the content of the zinc, ferriferous oxide and cerium oxide is with the molar ratio of elemental metal For Zn:Fe:Ce=0.01:0.0001:0.0001~0.01:0.0007:0.0001;
Wherein the zinc is simple substance zinc, and the ferriferous oxide is Fe2O3, the cerium oxide is CeO2And Ce2O3One of or Two kinds;
The denitrating catalyst is prepared by the following method:
(1) by the salt solution containing zinc in solvent 1, the first solution is obtained;
(2) methylimidazole is dissolved in solvent 2, is then added in the first solution, stirs evenly, obtains mixed liquor;
(3) by after molysite and cerium salt dissolution, the second solution containing molysite and cerium salt is prepared;
(4) the second solution is added in the mixed liquor of step (2), then magnetic agitation is aged;
(5) material after ageing in step (4) is filtered, washed, dried, ground, then calcined again, aoxidized, obtain To solid powder, i.e. denitrating catalyst.
2. denitrating catalyst according to claim 1, which is characterized in that the specific surface area of the denitrating catalyst is 800 ~1200m2/g。
3. denitrating catalyst according to claim 1, which is characterized in that the salting liquid containing zinc described in step (1) includes Zn (NO3)2·5H2O、Zn(CH3COO)2At least one of;The solvent 1 includes at least one of ethyl alcohol, methanol, water, DMF; The concentration of the salting liquid containing zinc is 0.03~0.04mol/L in first solution;Step (2) solvent 2 includes ethyl alcohol, first At least one of alcohol, DMF;The concentration of methylimidazole is 0.26~0.35mol/L in the mixed liquor of step (2);Step (3) The molysite includes at least one of ferric nitrate, ferric acetate, ferric sulfate, and the cerium salt includes cerous nitrate, cerous acetate, cerium chloride At least one of;The total concentration of ferro element and Ce elements is 0.0002~0.0007mol/L in second solution.
4. denitrating catalyst according to claim 1, which is characterized in that the revolving speed of step (4) described magnetic agitation is 1000~2000r/min, time are 2~4h;The time of the ageing is 8~12h.
5. denitrating catalyst according to claim 1, which is characterized in that described be filtered into of step (5) be with filter sizes 0.22~0.45 μm of sintered glass filter filtering;The drying is vacuum drying, and drying temperature is 100~140 DEG C, the time For 4~8h.
6. denitrating catalyst according to claim 1, which is characterized in that the temperature of step (5) described calcining be 350~ 500 DEG C, the time is 3~5h.
7. application of the denitrating catalyst described in claim 1 in denitrating flue gas, which is characterized in that with the denitrating catalyst Selective catalytic reduction reaction is carried out to the flue gas after dust-removal and desulfurizing.
8. application according to claim 7, which is characterized in that SO in the flue gas after the dust-removal and desulfurizing2Concentration be 0~ 400ppm, the temperature of the selective catalytic reduction reaction are 80~300 DEG C.
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CN109395710B (en) * 2018-08-20 2021-05-25 浙江师范大学 Preparation method of cerium and carbon co-doped zinc oxide
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