CN107376898A - A kind of SCR denitration and preparation method thereof - Google Patents

A kind of SCR denitration and preparation method thereof Download PDF

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Publication number
CN107376898A
CN107376898A CN201710499492.7A CN201710499492A CN107376898A CN 107376898 A CN107376898 A CN 107376898A CN 201710499492 A CN201710499492 A CN 201710499492A CN 107376898 A CN107376898 A CN 107376898A
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titanium
soluble
tungsten
salt
cerium
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熊志波
刘晶
涂艳武
金晶
孙成喜
项博超
忻逸飞
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University of Shanghai for Science and Technology
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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
    • B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • B01J23/24—Chromium, molybdenum or tungsten
    • B01J23/30—Tungsten
    • 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
    • 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
    • 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
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/02—Impregnation, coating or precipitation
    • B01J37/03—Precipitation; Co-precipitation
    • B01J37/031—Precipitation
    • 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
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/08—Heat treatment
    • B01J37/082—Decomposition and pyrolysis
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2258/00—Sources of waste gases
    • B01D2258/02—Other waste gases
    • B01D2258/0283—Flue gases
    • 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

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
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Abstract

The invention provides a kind of SCR denitration, and using cerium, tungsten, titanium as catalyst activity element, and described Ce elements, wolfram element and titanium elements mol ratio are 5~30:1~20:100.According to the mol ratio of cerium, tungsten, titanium elements it is 5~30 soluble cerium salt, soluble tungsten salt and soluble titanium salt present invention also offers the preparation method of above-mentioned SCR denitration:1~20:After 100 ratio dissolving, H is added2O2Solution obtains mixed solution；Excess urea is selected hydro-thermal certain time, to promote cerium, tungsten, titanium ion precipitation complete as precipitating reagent, by the filtering of obtained precipitated product, washing, dry, roasting, you can obtain SCR denitration.H2O2Complexing modification can improve the middle low temperature NH of cerium tungsten titanium compound oxide catalyst3SCR denitration activity, and preparation method is simple and easy, suitable for NO x Selective-catalytic-reduction denitrified process.

Description

A kind of SCR denitration and preparation method thereof
Technical field
The invention belongs to chemical field, is related to a kind of catalyst, specifically a kind of SCR denitration and its preparation Method.
Background technology
Nitrogen oxides (NO x ) it is one of Air Pollutant Discharge, photochemical pollution can be caused, causes acid rain etc. to endanger.I Usually said nitrogen oxides mainly include NO and NO2, wherein NO can be combined with the hemoglobin in blood, transport blood The ability of oxygen therapy declines, so as to cause anoxic；In addition, NO also has carcinogenic harm.NO in air can be slowly oxidized to NO2, NO2It is the presoma of nitric acid and nitrous acid, acid rain can be formed, acid rain and photochemical fog can causes crops and forest big Area is withered, corrodes building；NO2Lung and bronchial disease are also resulted in into respiratory tract or even are caused death.In view of such as This harm, effectively removes NOxBecome the important topic for nowadays environmental protection.
With NH3It is widely used in after removing is burnt NO in flue gas for the selective-catalytic-reduction denitrified method of reducing agent x It is de- Remove.Due to the catalytic component based on vanadium applied at present, in low temperature, denitration efficiency is very low, and its active component V in high temperature2O5With poison Property, easily causes secondary pollution, and therefore, it is higher to develop a kind of low temperature active, and environment amenable SCR denitration into For a kind of unavoidable trend.
The content of the invention
For above-mentioned technical problem of the prior art, the invention provides a kind of SCR denitration and its preparation side Method, described this SCR denitration and preparation method thereof will solve business vanadium tungsten titanium SCR denitration catalysis of the prior art The technical problem that agent active temperature windows are narrow, low temperature active is poor.
The invention provides a kind of SCR denitration, using cerium, tungsten, titanium as catalyst activity element, described cerium member Element, wolfram element and titanium elements mol ratio are 5~30:1~20:100.
Present invention also offers a kind of preparation method of above-mentioned SCR denitration, comprise the following steps：
1) by soluble cerium salt, soluble tungsten salt and soluble titanium salt according to Ce elements, wolfram element and titanium elements mol ratio be 5~ 30:1~20:100 are made into the aqueous solution, and H is added into the aqueous solution2O2Solution, control H2O2Solution is 1 with titanium ion mol ratio ~100:100；It is eventually adding excessive urea；
2) by step 1）The mixed solution of gained is placed in water bath containers, and bath temperature is 80 ~ 99 DEG C, the h of water bath time 8 ~ 12, Hydrothermal deposition thing is obtained after cerium, tungsten, titanium ion precipitation are complete；
3) by step 2）The hydrothermal deposition thing of gained is filtered, is washed, dried, is calcined, and a kind of SCR denitration catalysis is prepared Agent.
1. further, the soluble cerium salt be the soluble ceriums such as cerous nitrate, cerous nitrate/cerous sulfate, cerous sulfate/ Any one in sub- cerium salt.
Further, the soluble tungsten salt is any one in ammonium tungstate, ammonium metatungstate.
Further, the soluble titanium salt is any one in titanium sulfate, titanyl sulfate and titanium tetrachloride.
Further, the mol ratio of described urea and soluble cerium salt+soluble tungsten salt+soluble titanium salt is 3~10: 1。
Further, described H2O2The concentration of solution is 0.5 ~ 2 mol/L.
The invention provides a kind of H2O2The new cerium tungsten titanium composite oxide for being complexed modification is selective-catalytic-reduction denitrified (Selective Catalytic Reduction, SCR) catalyst, H2O2As complexing dressing agent, soluble cerium salt, can Dissolubility tungsten salt and soluble titanium salt are 5~30 according to the mol ratio of cerium, tungsten, titanium elements:1~20:After 100 ratio dissolving, add Add a certain amount of certain density H2O2Solution obtains mixed solution；Excess urea is selected as precipitating reagent, under certain bath temperature Hydro-thermal certain time, promote cerium, tungsten, titanium ion precipitation complete, obtain powders from precipitated precursor, by the filtering of obtained precipitated product, wash Wash, dry, be calcined, you can obtain the cerium tungsten titanium composite oxide SCR denitration.H2O2Complexing modification can improve cerium tungsten The middle low temperature NH of titanium compound oxide catalyst3- SCR denitration activity, and preparation method is simple and easy, suitable for NO x Selectivity Catalytic-reduction denitrified process.
The present invention compares with prior art, and its technological progress is significant.The present invention is prepared with conventional hydrothermal co-precipitation Cerium tungsten titanium compound oxide catalyst is compared, H2O2Cerium tungsten titanium composite oxide after complexing modification prepared by hydrothermal co-precipitation exists 250 DEG C ~ 400 DEG C have higher NH3- SCR denitration activity.The catalyst of the present invention is mainly used in selective catalytic reduction Remove the nitrogen oxides in coal-fired plant flue gas.The catalyst of the present invention uses nontoxic component, will not be to health and ecology Environmental pollution, catalyst have wide denitration temperature window under the conditions of superelevation air speed ratio, and good middle low-temperature denitration is lived Property.
Embodiment
In order that the technical means, the inventive features, the objects and the advantages of the present invention are easy to understand, it is real below Apply example H a kind of to the present invention2O2It is complexed the preparation method of the new cerium tungsten titanium composite oxide SCR denitration of modification and urges Agent is specifically addressed；But these examples do not have any restrictions to the scope of the present invention.
Embodiment 1
Step 1, by soluble cerium salt, soluble tungsten salt and soluble titanium salt according to Ce elements, wolfram element and titanium elements mol ratio For 20:10:100 are made into the aqueous solution, and add urea, and it is 5.0 to control urea/(Ce+W+Ti) mol ratio.
Step 2, the mixed solution obtained by step 1 is placed in water bath, in certain 90 DEG C of bath temperature hydro-thermal process 10 H, promote cerium, tungsten, titanium ion precipitation complete.
Step 3, the hydrothermal deposition thing obtained by step 2 filtered, washed, 105 DEG C of 30 min of drying and then in sky Under gas atmospheric condition, 550 DEG C of 5 h of roasting, reach catalyst A in Muffle furnace.
Embodiment 2
Step 1, by soluble cerium salt, soluble tungsten salt and soluble titanium salt according to Ce elements, wolfram element and titanium elements mol ratio For 20:10:100 are made into the aqueous solution, and 1ml H are added into the aqueous solution2O2Solution (1 mol/L), control H2O2With solution titanium from Sub- mol ratio is 10:100；Urea is eventually adding, it is 5.0 to control urea/(Ce+W+Ti) mol ratio.
Step 2, the mixed solution obtained by step 1 is placed in water bath, in certain 90 DEG C of bath temperature hydro-thermal process 10 H, promote cerium, tungsten, titanium ion precipitation complete.
Step 3, the hydrothermal deposition thing obtained by step 2 filtered, washed, 105 DEG C of dry 30min and then in air Under atmospheric condition, 550 DEG C of 5 h of roasting, reach catalyst B in Muffle furnace.
Embodiment 3
Step 1, by soluble cerium salt, soluble tungsten salt and soluble titanium salt according to Ce elements, wolfram element and titanium elements mol ratio For 20:10:100 are made into the aqueous solution, and 2 ml H are added into the aqueous solution2O2Solution (1 mol/L), control H2O2With solution titanium Ion mol ratio is 20:100；Urea is eventually adding, it is 5.0 to control urea/(Ce+W+Ti) mol ratio.
Step 2, the mixed solution obtained by step 1 is placed in water bath, in certain 90 DEG C of bath temperature hydro-thermal process 10 H, promote cerium, tungsten, titanium ion precipitation complete.
Step 3, the hydrothermal deposition thing obtained by step 2 filtered, washed, 105 DEG C of 30 min of drying and then in sky Under gas atmospheric condition, 550 DEG C of 5 h of roasting, reach catalyst C in Muffle furnace.
Embodiment 4
Step 1, by soluble cerium salt, soluble tungsten salt and soluble titanium salt according to Ce elements, wolfram element and titanium elements mol ratio For 20:10:100 are made into the aqueous solution, and 3 ml H are added into the aqueous solution2O2Solution (1 mol/L), control H2O2With solution titanium Ion mol ratio is 30:100；Urea is eventually adding, it is 5.0 to control urea/(Ce+W+Ti) mol ratio.
Step 2, the mixed solution obtained by step 1 is placed in water bath, in certain 90 DEG C of bath temperature hydro-thermal process 10 H, promote cerium, tungsten, titanium ion precipitation complete.
Step 3, the hydrothermal deposition thing obtained by step 2 filtered, washed, 105 DEG C of 30 min of drying and then in sky Under gas atmospheric condition, 550 DEG C of 5 h of roasting, reach catalyst D in Muffle furnace.
Embodiment 5
Step 1, by soluble cerium salt, soluble tungsten salt and soluble titanium salt according to Ce elements, wolfram element and titanium elements mol ratio For 20:10:100 are made into the aqueous solution, and 4 ml H are added into the aqueous solution2O2Solution (1 mol/L), control H2O2With solution titanium Ion mol ratio is 40:100；Urea is eventually adding, it is 5.0 to control urea/(Ce+W+Ti) mol ratio.
Step 2, the mixed solution obtained by step 1 is placed in water bath, in certain 90 DEG C of bath temperature hydro-thermal process 10 H, promote cerium, tungsten, titanium ion precipitation complete.
Step 3, the hydrothermal deposition thing obtained by step 2 filtered, washed, 105 DEG C of 30 min of drying and then in sky Under gas atmospheric condition, 550 DEG C of 5 h of roasting, reach catalyst E in Muffle furnace.
Embodiment 6
Catalyst A~the E prepared according to the method for case study on implementation 1~5, superelevation air speed than 1,200,000 ml/ (gh) and [NO]=[NH3Under the conditions of the ppm of]=1000, using investigating their NH on homemade micro fixed-bed reactor3Selective catalysis Reduce NO x Reactivity.Compared with A catalyst, H is utilized2O2Low temperature during B~D catalyst after complexing modification has preferably NH3- SCR denitration performance.
The each group catalyst of table 1 is in NH3Reactivity test result in-SCR
As seen from the above table, by H2O2It is complexed the catalytic activity of especially 250 ~ 400 DEG C of the catalyst wherein cryogenic property of modification It is significantly improved, highest can bring up to 89.4%.
Above example is only the basic explanation under present inventive concept, is not limited the invention.And according to the present invention Any equivalent transformation for being made of technical scheme, belong to protection scope of the present invention.

Claims (7)

  1. A kind of 1. SCR denitration, it is characterised in that：Using cerium, tungsten, titanium as catalyst activity element, described Ce elements, tungsten Element and titanium elements mol ratio are 5~30:1~20:100.
  2. 2. the preparation method of a kind of SCR denitration described in claim 1, it is characterised in that comprise the following steps：
    1）By soluble cerium salt, soluble tungsten salt and soluble titanium salt according to Ce elements, wolfram element and titanium elements mol ratio be 5~ 30:1~20:100 are made into the aqueous solution, and H is added into the aqueous solution2O2Solution, control H2O2Solution is 1 with titanium ion mol ratio ~100:100；It is eventually adding excessive urea；
    2）By step 1）The mixed solution of gained is placed in water bath containers, and bath temperature is 80 ~ 99 DEG C, the h of water bath time 8 ~ 12, Hydrothermal deposition thing is obtained after cerium, tungsten, titanium ion precipitation are complete；
    3）By step 2）The hydrothermal deposition thing of gained is filtered, is washed, dried, is calcined, and a kind of SCR denitration catalysis is prepared Agent.
  3. A kind of 3. preparation method of SCR denitration according to claim 2, it is characterised in that：The soluble cerium Salt is any one in the soluble cerium/sub- cerium salt such as cerous nitrate, cerous nitrate/cerous sulfate, cerous sulfate.
  4. A kind of 4. preparation method of SCR denitration according to claim 2, it is characterised in that：The soluble tungsten Salt is any one in ammonium tungstate, ammonium metatungstate.
  5. A kind of 5. preparation method of SCR denitration according to claim 2, it is characterised in that：The soluble titanium Salt is any one in titanium sulfate, titanyl sulfate and titanium tetrachloride.
  6. A kind of 6. preparation method of SCR denitration according to claim 2, it is characterised in that：Described urea with The mol ratio of soluble cerium salt+soluble tungsten salt+soluble titanium salt is 3~10:1.
  7. A kind of 7. preparation method of SCR denitration according to claim 2, it is characterised in that：Described H2O2For work Any one in industry or medical hydrogen peroxide.
CN201710499492.7A 2017-06-27 2017-06-27 A kind of SCR denitration and preparation method thereof Pending CN107376898A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109876795A (en) * 2019-04-04 2019-06-14 上海理工大学 A kind of cerium tungsten titanium composite oxide SCR denitration and preparation method thereof

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101327427A (en) * 2008-08-03 2008-12-24 吴进明 High-efficient selective catalytic reduction denitration catalyst and preparation method thereof
CN102302930A (en) * 2011-07-05 2012-01-04 中国科学院生态环境研究中心 Transition metal doped cerium and titanium compound oxide catalyst for selective catalytic reduction of nitric oxide by ammonia
CN103846083A (en) * 2014-03-24 2014-06-11 南京理工大学 Tungsten titanium composite oxide supported cerium oxide catalyst, preparation method as well as application of catalyst
CN103894185A (en) * 2014-04-01 2014-07-02 北京工业大学 Method for preparing selective catalytic reduction (SCR) denitration catalyst by taking TiO2-ZnO as composite carrier
CN104785246A (en) * 2015-04-13 2015-07-22 国电环境保护研究院 Manganese-cerium supported low-temperature SCR catalyst preparation method based on metatitanic acid material
CN105582908A (en) * 2016-02-26 2016-05-18 凯龙蓝烽新材料科技有限公司 Preparation method of V-W-TiO2 based selective reduction catalyst

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101327427A (en) * 2008-08-03 2008-12-24 吴进明 High-efficient selective catalytic reduction denitration catalyst and preparation method thereof
CN102302930A (en) * 2011-07-05 2012-01-04 中国科学院生态环境研究中心 Transition metal doped cerium and titanium compound oxide catalyst for selective catalytic reduction of nitric oxide by ammonia
CN103846083A (en) * 2014-03-24 2014-06-11 南京理工大学 Tungsten titanium composite oxide supported cerium oxide catalyst, preparation method as well as application of catalyst
CN103894185A (en) * 2014-04-01 2014-07-02 北京工业大学 Method for preparing selective catalytic reduction (SCR) denitration catalyst by taking TiO2-ZnO as composite carrier
CN104785246A (en) * 2015-04-13 2015-07-22 国电环境保护研究院 Manganese-cerium supported low-temperature SCR catalyst preparation method based on metatitanic acid material
CN105582908A (en) * 2016-02-26 2016-05-18 凯龙蓝烽新材料科技有限公司 Preparation method of V-W-TiO2 based selective reduction catalyst

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109876795A (en) * 2019-04-04 2019-06-14 上海理工大学 A kind of cerium tungsten titanium composite oxide SCR denitration and preparation method thereof

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