CN103111280A - Transition metal doped cerium-zirconium solid solution high-air-speed denitrification catalyst and preparation method thereof - Google Patents
Transition metal doped cerium-zirconium solid solution high-air-speed denitrification catalyst and preparation method thereof Download PDFInfo
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Abstract
The invention provides a transition metal doped cerium-zirconium solid solution high-air-speed denitrification catalyst and a preparation method thereof. The catalyst is prepared through a sol-gel method, and raw materials used in the method are soluble salt of transition metals (vanadium, chromium, manganese, iron, cobalt and copper), soluble salt of cerium, soluble salt of zirconium, deionized water, ethanol and citric acid, wherein the total metal ion mol concentration is (0.1-0.3) mol/L, the citric acid mol concentration is (0.1-0.3) mol/L, the volume ratio of the deionized water to the ethanol is (5-10):1, and the mol ratio of the transition metals (vanadium, chromium, manganese, iron, cobalt and copper) to the cerium to the zirconium is (0.1-2):(0.1-1):(0.1-1). The catalyst prepared by the invention can be used for SCR (selective catalytic reduction) denitrification reaction, and has favorable denitrification activity.
Description
One, technical field:
The present invention relates to a kind of contain elemental cerium, zirconium and other transition metal element doped solid solution catalyst, its preparation method and the application in the denitration field thereof.
Two, background technology:
Nitrogen oxide (NO
x) be one of main atmosphere pollution, human body there is very big harm.Nitrogen oxide in atmosphere has two large main sources, automotive emission (mobile pollution source) and thermal power plant and industrial furnace fume emission (stationary source).To utilize CO and CH in tail gas for automobile and light diesel fuel car owner
x, under the effect of three-way catalyst, the NOx in tail gas is reduced into nitrogen and removes, and the Medium or severe type diesel vehicle needs to pass through NH
3-SCR technology, namely under catalyst action with NH
3For reducing agent with the NO in tail gas
xBe reduced into nitrogen and remove.Fixed-contamination source tail-gas denitration technology take thermal power plant as representative is mainly with TiO
2V for carrier
2O
5-WO
3/ TiO
2And V
2O
5-MoO
3/ TiO
2Catalyst is with NH
3Be reducing agent.Technique was widely used in developed country before this, and technique is also mostly adopted at present domestic newly-built thermal power plant and the transformation of old thermal power plant.During SCR technological design now, because the operation air speed of catalyst can not be too high, designed air speed is limited in 10000h usually
-1Below.For the transformation of old thermal power plant, due to air preheater and electric cleaner last as larger headspace not, particularly catalyst operation air speed is not high, required catalytic amount strengthens, and need to lay catalyst so the rebuilding construction difficulty is large than large space.
The catalyst of Chinese patent CN101590404 is take anatase titanium dioxide as carrier, and vanadic anhydride is main active component, and tungstic acid and cerium oxide are the inferior active component of performance cooperative effect; And adopt co-impregnation to prepare.Be characterized in reducing the consumption with highly toxic vanadium, reduced cost, simultaneously had NO higher than 90% 200～450 ℃ of scopes
xConversion ratio.But air speed is controlled at 28000h
-1, total gas flow rate is 300ml/min, air speed is lower.
Chinese patent CN1724149A utilize carrying method take the oxide of manganese as active component titanium dioxide as carrier has prepared a series of catalyst.At 10000h
-1Under air speed, catalyst remains on more than 95% the conversion ratio of NO; When reaction temperature rose to 120 ℃, NO removed efficient near 100%, but air speed is also lower.
Chinese patent CN1817448A discloses and has a kind ofly utilized sol-gel technique to prepare and adopt the alkyl oxide of titanium and the soluble-salt of manganese is the low temperature SCR denitration catalyst of raw material.And the impact on activity of adding of some transition metals has been described.In literary composition, catalyst is at 30000h
-1Conversion ratio to NO under air speed reaches 90%, and air speed is also lower.
As previously discussed, existing denitrating catalyst ubiquity the not high shortcoming of air speed, and the meaning of exploitation high-speed catalyst is to improve unit catalyst service efficiency, reduces catalyst amount, thereby reduces the denitrification apparatus volume, is beneficial to rebuilding construction.
Three, summary of the invention:
The present invention has prepared a kind of highly active doping transition elements (vanadium, chromium, manganese, iron, cobalt, copper) cerium zirconium sosoloid denitrating catalyst that can use under the high-speed condition, the cerium zirconium sosoloid catalyst of the containing transition metal element of gained is in 100-400 ℃ of temperature range according to the present invention, 150000h
-1The high-speed condition under, have SCR denitration activity preferably.。
The preparation needed raw material of indication catalyst of the present invention comprises soluble-salt, the soluble-salt of cerium, the soluble-salt of zirconium, deionized water, ethanol, the citric acid of transition metal (vanadium, chromium, manganese, iron, cobalt, copper).Total metal ion molar concentration is (0.1～0.3) mol/L, and the citric acid molar concentration is (0.1～0.3) mol/L, the deionized water volume: the ethanol volume is (5～10): 1.Wherein transition metal (vanadium, chromium, manganese, iron, cobalt, copper) is (0.1～2) with the mol ratio of cerium and zirconium: (0.1～1): (0.1～1).
Catalyst preparation process of the present invention is as follows:
1. the ethanol, deionized water, the citric acid that accurately measure certain volume mix rear 80 ℃ and are stirred into A solution.
2. the soluble-salt that takes the soluble-salt of a certain amount of cerium and zirconium adds A solution to be heated to 80 ℃ to be stirred into B solution.
3. the soluble-salt dissolve complete that slowly splashes into transition elements (V, Cr, Mn, Fe, Co, Cu) under continue stirring in the B solution forms solution C.
4. C is placed in evaporation under 110 ℃ of conditions, gel, foaming, the dry D of formation.
5. D being placed in the baking oven pre-burning under 200 ℃ of conditions grinds after 4 hours and obtains E.
6. E is placed in Muffle furnace calcine under (400-800 ℃) condition roasting (4-8) hour catalyst.
The activity rating method of catalyst is: get the catalyst fines after roasting, pulverize and sieve through compressing tablet, get the catalyst granules between 20 orders～40 orders, fill in the quartz ampoule that internal diameter is 6mm.Evaluating apparatus adopts homemade fixed bed reactors.Reaction bed temperature is controlled at respectively 100-400 ℃.Reaction gas is mixed by steel cylinder gas, and flow-control is at 200ml/min.Catalyst quality is got respectively 0.1g, and air speed is 150000h
-1Reaction atmosphere consists of (volume fraction): NO:1000ppm; NH
3: 1100ppm; O
2: 4%; All the other are nitrogen (balanced gas).In atmosphere, ammonia is as reducing agent, and all the other composition simulation industrial smokes form.
NO conversion ratio computing formula:
Four, the specific embodiment:
Following examples only are used for the present invention is specifically described.But should be appreciated that protection scope of the present invention is not limited in following examples.
Embodiment 1:
Be raw material with ammonium metavanadate, cerous nitrate, zirconium nitrate, ethanol, deionized water.Measure deionized water 140ml, ethanol 20ml adds the dissolving of citric acid 8.4g and vigorous stirring after mixing, then add cerous nitrate 8.69g, and zirconium nitrate 8.59g is in 80 ℃ of uniform stirrings.Slowly add ammonium metavanadate 4.68g, evaporation under 110 ℃ after dissolving is completed, gel, foaming.The foaming complete after 200 ℃ of lower pre-burnings 4 hours.Pre-burning is ground to powder after finishing, and 500 ℃ of roastings 6 hours, obtains catalyst.
Under following reaction condition: 150000h
-1Air speed, 0.1Mpa, 1000ppm NO, 1100ppm NH
3, N
2Be Balance Air, the denitration activity characterization result sees attached list middle example 1
Embodiment 2:
Be raw material with ferric nitrate, cerous nitrate, zirconium nitrate, ethanol, deionized water.Measure deionized water 140ml, ethanol 20ml adds the dissolving of citric acid 8.4g and vigorous stirring after mixing, then add cerous nitrate 8.69g, and zirconium nitrate 8.59g is in 80 ℃ of uniform stirrings.Slowly add ferric nitrate 16g, evaporation under 110 ℃ after dissolving is completed, gel, foaming.The foaming complete after 200 ℃ of lower pre-burnings 4 hours.Pre-burning is ground to powder after finishing, and 500 ℃ of roastings 6 hours, obtains catalyst.
Under following reaction condition: 150000h
-1Air speed, 0.1Mpa, 1000ppm NO, 1100ppm NH
3, N
2Be Balance Air, the denitration activity characterization result sees attached list middle example 2.
Embodiment 3:
Be raw material with chromic nitrate, cerous nitrate, zirconium nitrate, ethanol, deionized water.Measure deionized water 140ml, ethanol 20ml adds the dissolving of citric acid 8.4g and vigorous stirring after mixing, then add cerous nitrate 8.69g, and zirconium nitrate 8.59g is in 80 ℃ of uniform stirrings.Slowly add chromic nitrate 16g, evaporation under 110 ℃ after dissolving is completed, gel, foaming.The foaming complete after 200 ℃ of lower pre-burnings 4 hours.Pre-burning is ground to powder after finishing, and 500 ℃ of roastings 6 hours, obtains catalyst.
Under following reaction condition: 150000h
-1Air speed, 0.1Mpa, 1000ppm NO, 1100ppm NH
3, N
2Be Balance Air, the denitration activity characterization result sees attached list middle example 3.
Embodiment 4:
Be raw material with cobalt nitrate, cerous nitrate, zirconium nitrate, ethanol, deionized water.Measure deionized water 140ml, ethanol 20ml adds the dissolving of citric acid 8.4g and vigorous stirring after mixing, then add cerous nitrate 8.69g, and zirconium nitrate 8.59g is in 80 ℃ of uniform stirrings.Slowly add cobalt nitrate 11.6g, evaporation under 110 ℃ after dissolving is completed, gel, foaming.The foaming complete after 200 ℃ of lower pre-burnings 4 hours.Pre-burning is ground to powder after finishing, and 500 ℃ of roastings 6 hours, obtains catalyst.Under following reaction condition: 150000h
-1Air speed, 0.1Mpa, 1000ppm NO, 1100ppm NH
3, N
2Be Balance Air, the denitration activity characterization result sees attached list middle example 4.
Embodiment 5:
Be raw material with manganese nitrate, cerous nitrate, zirconium nitrate, ethanol, deionized water.Measure deionized water 140ml, ethanol 20ml adds the dissolving of citric acid 8.4g and vigorous stirring after mixing, then add cerous nitrate 8.69g, and zirconium nitrate 8.59g is in 80 ℃ of uniform stirrings.Slowly add 50% manganese nitrate solution 9ml, evaporation under 110 ℃ after dissolving is completed, gel, foaming.The foaming complete after 200 ℃ of lower pre-burnings 4 hours.Pre-burning is ground to powder after finishing, and 500 ℃ of roastings 6 hours, obtains catalyst.
Under following reaction condition: 150000h
-1Air speed, 0.1Mpa, 1000ppm NO, 1100ppmNH
3, N
2Be Balance Air, the denitration activity characterization result sees attached list middle example 5.
Embodiment 6:
Be raw material with manganese nitrate, cerous nitrate, zirconium nitrate, ethanol, deionized water.Measure deionized water 160ml, ethanol 20ml adds the dissolving of citric acid 8.4g and vigorous stirring after mixing, then add cerous nitrate 8.69g, and zirconium nitrate 8.59g is in 80 ℃ of uniform stirrings.Slowly add 50% manganese nitrate solution 9ml, evaporation under 110 ℃ after dissolving is completed, gel, foaming.The foaming complete after 200 ℃ of lower pre-burnings 4 hours.Pre-burning is ground to powder after finishing, and 550 ℃ of roastings 6 hours, obtains catalyst.
Under following reaction condition: 150000h
-1Air speed, 0.1Mpa, 1000ppm NO, 1100ppmNH
3, N
2Be Balance Air, the denitration activity characterization result sees attached list middle example 6.
Embodiment 7:
Be raw material with manganese nitrate, cerous nitrate, zirconium nitrate, ethanol, deionized water.Measure deionized water 100ml, ethanol 20ml adds the dissolving of citric acid 8.4g and vigorous stirring after mixing, then add cerous nitrate 8.69g, and zirconium nitrate 8.59g is in 80 ℃ of uniform stirrings.Slowly add 50% manganese nitrate solution 9ml, evaporation under 110 ℃ after dissolving is completed, gel, foaming.The foaming complete after 200 ℃ of lower pre-burnings 4 hours.Pre-burning is ground to powder after finishing, and 600 ℃ of roastings 6 hours, obtains catalyst.
Under following reaction condition: 150000h
-1Air speed, 0.1Mpa, 1000ppm NO, 1100ppmNH
3, N
2Be Balance Air, the denitration activity characterization result sees attached list middle example 7.
Embodiment 8:
Be raw material with copper nitrate, cerous nitrate, zirconium nitrate, ethanol, deionized water.Measure deionized water 140ml, ethanol 20ml adds the dissolving of citric acid 8.4g and vigorous stirring after mixing, then add cerous nitrate 8.69g, and zirconium nitrate 8.59g is in 80 ℃ of uniform stirrings.Slowly add copper nitrate 9.6g, evaporation under 110 ℃ after dissolving is completed, gel, foaming.The foaming complete after 200 ℃ of lower pre-burnings 4 hours.Pre-burning is ground to powder after finishing, and 500 ℃ of roastings 6 hours, obtains catalyst.
Under following reaction condition: 150000h
-1Air speed, 0.1Mpa, 1000ppmNO, 1100ppmNH
3, N
2Be Balance Air, the denitration activity characterization result sees attached list middle example 8.
Embodiment 9 (Comparative Examples):
Be raw material with cerous nitrate, zirconium nitrate, ethanol, deionized water.Measure deionized water 140ml, ethanol 20ml adds the dissolving of citric acid 8.4g and vigorous stirring after mixing, then add cerous nitrate 8.69g, and zirconium nitrate 8.59g is in 80 ℃ of uniform stirrings.Evaporation under 110 ℃ after dissolving is completed, gel, foaming.The foaming complete after 200 ℃ of lower pre-burnings 4 hours.Pre-burning is ground to powder after finishing, and 550 ℃ of roastings 6 hours, obtains catalyst.
Under following reaction condition: 150000h
-1Air speed, 0.1Mpa, 1000ppm NO, 1100ppmNH
3, N
2Be Balance Air, the denitration activity characterization result sees attached list middle example 9.
Implement 10:
Be raw material with manganese sulfate, cerous nitrate, zirconium nitrate, ethanol, deionized water.Measure deionized water 140ml, ethanol 20ml adds the dissolving of citric acid 8.4g and vigorous stirring after mixing, then add cerous nitrate 8.69g, and zirconium nitrate 8.59g is in 80 ℃ of uniform stirrings.Slowly add manganese sulfate 3.38g, evaporation under 110 ℃ after dissolving is completed, gel, foaming.The foaming complete after 200 ℃ of lower pre-burnings 4 hours.Pre-burning is ground to powder after finishing, and 500 ℃ of roastings 6 hours, obtains catalyst.
Under following reaction condition: 150000h
-1Air speed, 0.1Mpa, 1000ppmNO, 1100ppmNH
3, N
2Be Balance Air, the denitration activity characterization result sees attached list middle example 10.
Embodiment 11:
Be raw material with manganese chloride, cerous nitrate, zirconium nitrate, ethanol, deionized water.Measure deionized water 140ml, ethanol 20ml adds the dissolving of citric acid 8.4g and vigorous stirring after mixing, then add cerous nitrate 8.69g, and zirconium nitrate 8.59g is in 80 ℃ of uniform stirrings.Slowly add manganese chloride 3.94g, evaporation under 110 ℃ after dissolving is completed, gel, foaming.The foaming complete after 200 ℃ of lower pre-burnings 4 hours.Pre-burning is ground to powder after finishing, and 500 ℃ of roastings 6 hours, obtains catalyst.
Under following reaction condition: 150000h
-1Air speed, 0.1Mpa, 1000ppm NO, 1100ppm NH
3, N
2Be Balance Air, the denitration activity characterization result sees attached list middle example 11.
Embodiment 12:
Be raw material with manganese nitrate, cerous nitrate, zirconium sulfate, ethanol, deionized water.Measure deionized water 140ml, ethanol 20ml adds the dissolving of citric acid 8.4g and vigorous stirring after mixing, then add cerous nitrate 8.69g, and zirconium sulfate 7.1g is in 80 ℃ of uniform stirrings.Slowly add manganese nitrate 4.5ml, evaporation under 110 ℃ after dissolving is completed, gel, foaming.The foaming complete after 200 ℃ of lower pre-burnings 4 hours.Pre-burning is ground to powder after finishing, and 500 ℃ of roastings 6 hours, obtains catalyst.Under following reaction condition: 150000h
-1Air speed, 0.1Mpa, 1000ppm NO, 1100ppmNH
3, N
2Be Balance Air, the denitration activity characterization result sees attached list middle example 12.
Embodiment 13:
Be raw material with manganese nitrate, cerous nitrate, zirconium chloride, ethanol, deionized water.Measure deionized water 140ml, ethanol 20ml adds the dissolving of citric acid 8.4g and vigorous stirring after mixing, then add cerous nitrate 8.69g, and zirconium chloride 4.7g is in 80 ℃ of uniform stirrings.Slowly add manganese nitrate 4.5ml, evaporation under 110 ℃ after dissolving is completed, gel, foaming.The foaming complete after 200 ℃ of lower pre-burnings 4 hours.Pre-burning is ground to powder after finishing, and 500 ℃ of roastings 6 hours, obtains catalyst.Under following reaction condition: 150000h
-1Air speed, 0.1Mpa, 1000ppm NO, 1100ppmNH
3, N
2Be Balance Air, the denitration activity characterization result sees attached list middle example 13.
Embodiment 14:
Be raw material with manganese nitrate, cerous nitrate, zirconium nitrate, ferric nitrate, ethanol, deionized water.Measure deionized water 140ml, ethanol 20ml adds the dissolving of citric acid 8.4g and vigorous stirring after mixing, then add cerous nitrate 8.69g, and zirconium nitrate 8.59g is in 80 ℃ of uniform stirrings.Slowly add 50% manganese nitrate solution 9ml, ferric nitrate 16g, evaporation under 110 ℃ after dissolving is completed, gel, foaming.The foaming complete after 200 ℃ of lower pre-burnings 4 hours.Pre-burning is ground to powder after finishing, and 550 ℃ of roastings 6 hours, obtains catalyst.
Under following reaction condition: 150000h
-1Air speed, 0.1Mpa, 1000ppm NO, 1100ppmNH
3, N
2Be Balance Air, the denitration activity characterization result sees attached list middle example 14.
Subordinate list. each catalyst denitration activity (150000h
-1Air speed, 0.1Mpa, 1000ppm NO, 1100ppmNH
3, N
2Be Balance Air)
Subordinate list:
Claims (4)
1. transition metal element doped cerium zirconium sosoloid high-speed denitrating catalyst, it is characterized in that this solid solution catalyst is to use cerium, the soluble-salt of zirconium and transition metal, citric acid, ethanol, deionized water is raw material, through refluxing, foaming, drying and roasting prepare and get, and material molar ratio is the soluble-salt of transition metal: the soluble-salt of cerium: the soluble-salt of zirconium=(0.1～2): (0.1～1): (0.1-1), the slaine total mol concentration is (0.1-0.3) mol/L, the citric acid molar concentration is (0.1～0.3) mol/L, the deionized water volume: the volume ratio of ethanol is (5～10): 1.
2. high-speed denitrating catalyst according to claim 1, is characterized in that described transition metal is vanadium, chromium, manganese, iron, cobalt, copper.
3. high-speed denitrating catalyst according to claim 1 and 2, it is characterized in that the preparation method is: with the mixed evenly rear backflow under 80 ℃ of soluble-salt, citric acid, ethanol, the deionized water of the soluble-salt of the soluble-salt of described transition metal, described cerium, described zirconium, form gel under 110 ℃, foaming, 200 ℃ of lower pre-burnings, cooling rear grinding at 400-800 ℃ of lower roasting 4-8 hour, gets described high-speed denitrating catalyst.
4. the application of the described high-speed denitrating catalyst of any one in denitration reaction according to claim 1 to 3.
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Application publication date: 20130522 |