CN105597730A - Honeycomb vanadium series denitration preformed catalyst, and preparation method and use thereof - Google Patents
Honeycomb vanadium series denitration preformed catalyst, and preparation method and use thereof Download PDFInfo
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Abstract
The invention relates to a high-water resistance and high-sulfur resistance honeycomb vanadium series denitration preformed catalyst suitable for FCC flue gas, and a preparation method and a use thereof, and belongs to the technical fields of environment catalysis and environment protection. The preparation method comprises the following steps: preparing catalyst powder through adopting a volume immersion technology with anatase titanium dioxide as a carrier, V2O5 as an active component and WO3 as an active assistant, and adding a forming assistant to prepare the honeycomb preformed catalyst with wide active temperature window, strong water resistance and strong sulfur resistance. The forming assistant mainly comprises a reinforcing agent, an inorganic binder, an organic binder, a pore forming agent and a lubricant. Pilot plant test of the preformed catalyst in a small FCC apparatus shows that the denitration efficiency of the catalyst under an air speed of 4000h<-1>, an NO concentration of 1000ppm, an SO2 concentration of 1500ppm and an H2O content of 5% is 85% or above at 250-450DEG C and reaches 90% or above at 300-450DEG C.
Description
Technical field
The invention belongs to environmental catalysis and environmental protection technical field, being specifically related to a kind of cellular vanadium is denitrationPreformed catalyst, preparation method and its usage, be specifically related to a kind of anti-sulphur of high water resistant of applicable FCC flue gasThe cellular vanadium of energy is denitration preformed catalyst, preparation method and its usage.
Background technology
Nitrogen oxide is that mankind's activity is discharged into the common pollutant in atmospheric environment, wherein proportion maximumBe NO and NO2. The NO of atmosphere middle and high concentrationxPeople's respiratory system is had to strong impulse effect, thisIn outer NO and blood, hemoglobin affinity is stronger, thereby blood oxygen carrying capacity is declined. NO also can pass throughPhotochemical oxidation effect is converted into NO2, then form nitric acid and nitrous acid, be the main contributions person of acid rain alsoCause a series of environmental problem. In addition NO,xUnder effect of sunlight, very easily generate light with hydrocarbon compoundChemical fumes etc. have more supervirulent secondary pollution.
During " 12 ", nitrogen oxides pollution control becomes the emphasis of environmental protection, but current domestic fire coalThe pilot project of gas denitrifying technology is all from external introduction, and catalyst cost is high, domestic catalyst for denitrating flue gasStill immature, so it is extremely urgent to research and develop the denitrating catalyst of novel autonomous property right.
CN104162421A discloses a kind of vanadium tungsten titanyl for ammine selectivity catalytic reduction nitrous oxidesThe preparation method of thing catalyst. Described preparation method is that first to prepare tungsten titanium by sluggish precipitation compoundOxide is as catalyst carrier, then adopts infusion process load barium oxide on tungsten titanium composite oxide, warpAfter crossing roasting, obtain vanadium tungsten titanium oxide catalyst. This prior art adopts tungsten titanium composite oxide as carrier,Barium oxide is as active component. But two steps of the synthetic needs of this catalyst, preparation technology is loaded down with trivial details, increasesAdd the preparation cost of this catalyst.
CN101036884A discloses a kind of Ti-base catalyst and system for coal steam-electric plant smoke SCR denitrationPreparation Method. This catalyst is with 80～99% TiO2With 1～20% sieve and silica-sesquioxide be carrier, extrude as honeybeeNest body, then applies active component V with the method for dipping on honeycomb ceramics surface2O5And WO3, owing to being surfaceApply, so vanadium load capacity is higher, and poor corrosion resistance.
CN1778466A discloses by adding binding agent that nano titanium dioxide powder is made to solid slurry,Extrusion molding, drying and calcining makes the titanium dioxide forming substances with some strength definite shape, but described twoTitanium oxide article shaped is mainly as catalyst carrier, and it does not have catalytic activity, does not therefore also consider bondingThe adverse effect that agent may cause catalytic activity in the application of specific catalytic active substance.
CN101676024A discloses a kind of Faviform ammonia-method selective-catalytic-reduction denitrified catalyst and system thereofPreparation Method, adopts the method for integral extrusion moulding to prepare V-W/TiO2Honeycombed catalyst, this catalystAt small scall coal-fired boiler pilot scale denitration test, air speed 5000h-1, flue-gas temperature in the time of 350 DEG C, denitration efficiencyReach 95%, after long-term operation, denitration effect is still more than 80%. But this catalyst is not investigated catalystThe anti-sulphur of water resistant, stability be not very good, and be only suitable for the environmental condition in coal-burning boiler.
Summary of the invention
For the problem of prior art, the present invention is intended to develop a kind of high water resistant sulfur resistance and applicable FCCThe SCR denitrating catalyst of flue gas, based on this, the invention provides a kind of cellular vanadium is denitration moulding catalysisAgent, preparation method and application thereof. The water resistant excellent in sour resistance of described catalyst, denitration efficiency is high, stableProperty is good, and mechanical strength is high, and the preparation method of this catalyst is simple.
To achieve these goals, the present invention has adopted following technical scheme:
A kind of cellular vanadium is denitration preformed catalyst, and it is mainly by catalyst powder and shaping assistant mouldingObtain, described catalyst powder is taking anatase titania as carrier, V2O5For active component, WO3For workProperty auxiliary agent, its composition is expressed as V2O5-WO3/TiO2。
Described anatase titania is available commercially.
Preferably, in described catalyst powder, active component V2O5Quality be catalyst powder weight0.1～3%, for example 0.2%, 0.5%, 0.8%, 1.1%, 1.4%, 1.7%, 2%, 2.3%, 2.6% or2.9%, preferably 0.1～1.5%.
Preferably, in described catalyst powder, coagent WO3Quality be catalyst powder weight1～10%, for example 1.5%, 2%, 2.5%, 3%, 3.5%, 4%, 4.5%, 5%, 5.5%, 6%,6.5%, 7%, 7.5%, 8%, 8.5%, 9% or 9.5%, preferably 1～5%.
Preferably, described shaping assistant is reinforcing agent, inorganic binder, organic binder bond, pore creating material and profitThe mixture of lubrication prescription. The forming method that the present invention adopts organic binder bond and inorganic binder to combine, increasesThe mechanical strength of honeycombed catalyst, improved the denitration performance of catalyst simultaneously.
Preferably, described reinforcing agent content is 10～30% of catalyst powder weight, for example 12%, 14%,16%, 18%, 20%, 22%, 24%, 26% or 28%, preferably 10～20%.
Preferably, described reinforcing agent is glass fibre.
Preferably, described inorganic binder is that waterglass is or/and Ludox.
Preferably, the content of described inorganic binder is 5～15% of catalyst powder weight, for example 5.5%,6%, 6.5%, 7%, 7.5%, 8%, 8.5%, 9% or 9.5%, preferably 5～8%.
Preferably, described organic binder bond be polyvinyl alcohol, hydroxypropyl methylcellulose, methylcellulose orThe mixture of any one in PEO or at least two kinds.
Preferably, the content of described organic binder bond is 1～5% of catalyst powder weight, for example 1.5%,2%, 2.5%, 3%, 3.5%, 4% or 4.5%, preferably 2～4%.
Preferably, described pore creating material is that active carbon is or/and sesbania powder.
Preferably, the content of described pore creating material is 5～10% of catalyst powder weight, for example 5.5%,6%, 6.5%, 7%, 7.5%, 8%, 8.5%, 9% or 9.5%, preferably 8～10%.
Preferably, described lubricant is glycerine.
Preferably, described lubricant content is 10～15% of catalyst powder weight, for example 10.5%,11%, 11.5%, 12%, 12.5%, 13%, 13.5%, 14% or 14.5%, preferably 10～12%.
In the present invention, exemplary solid forming auxiliary agent is glass fibre, waterglass, active carbon, hydroxypropylYlmethyl cellulose and sesbania powder, exemplary liquid molding auxiliary agents of silicon colloidal sol and glycerine. Preferably, exampleThe solid forming auxiliary agent of property is glass fibre, waterglass, active carbon, hydroxypropyl methylcellulose and sesbaniaPowder, exemplary liquid molding auxiliary agents of silicon colloidal sol and glycerine, each constituent content is respectively: content of glass fiberBe 10%, active carbon content is 5%, and hydroxypropyl methylcellulose content is 5%, and Ludox content is 5%,Glycerol content is 10%.
It is denitration preformed catalyst that two of object of the present invention is to provide a kind of cellular vanadium as abovePreparation method, described method comprises preparation and the forming process of catalyst powder.
Preferably, adopted the method Kaolinite Preparation of Catalyst powder of volume dipping, comprised the following steps:
(1) in oxalic acid solution, add vanadium source, being stirred to solution is navy blue, and now dissolve completely in vanadium source,Then add tungsten source, be stirred to without solid matter, now dissolve completely in tungsten source;
(2) solution step (1) being obtained joins in titania powder, and uniform stirring, is starchedLiquid, dry, grind (object of grinding be mainly make roasting more complete), roasting, then grind, obtain catalysisAgent powder.
Preferably, the concentration of described oxalic acid solution is 5～10wt%.
Preferably, described tungsten source is selected from any one in ammonium metatungstate, ammonium tungstate, potassium tungstate or sodium tungstateOr the mixture of at least two kinds.
Preferably, described vanadium source is ammonium metavanadate.
Preferably, step (1) adds behind vanadium source, and at the temperature of 40～55 DEG C, being stirred to solution is navy blue.
Preferably, the described baking temperature of step (2) is 80～120 DEG C, for example 85 DEG C, 90 DEG C, 95 DEG C,100 DEG C, 105 DEG C, 110 DEG C or 115 DEG C, be 12～24h drying time.
Preferably, the described sintering temperature of step (2) is 400～550 DEG C, and roasting time is 3～8h, preferably 5h,Sintering temperature is too low, and slaine cannot be converted into metal oxide completely, and sintering temperature is too high, titanium dioxideMay change to rutile-type from Detitanium-ore-type.
Preferably, described forming process comprises the following steps:
(a) catalyst powder and solid forming auxiliary agent are dry mixed, then add liquid molding auxiliary agent to carry outWet mixing, then adds deionized water to stir;
(b) material step (a) being obtained is transferred in vacuum deairing machine and is fully mixed, and then allowsIt carries out 6～48h (for example 8h, 12h, 16h, 20h, 24h, 28h, 32h, 36h, 40h or 44h)Old, obtain final moulding idiosome;
(c) moulding idiosome step (b) being obtained is extruded as cellular by extrusion shaping machine;
(d) cellular moulding idiosome step (c) being obtained is dried, and calcining, obtains cellular vanadiumIt is denitration preformed catalyst.
Preferably, in step (a), catalyst powder and solid forming auxiliary agent add and are dry mixed simultaneously.
Preferably, carry out primary drying and redrying two procedures in step (d), primary drying adopts permanentThe method of wet constant temperature, 30～70 DEG C of primary drying temperature, for example 35 DEG C, 40 DEG C, 45 DEG C, 50 DEG C,55 DEG C, 60 DEG C or 65 DEG C, humidity 85～10%, for example 80%, 75%, 70%, 65%, 60%, 55%,50%, 45%, 40%, 35%, 30%, 25%, 20%, 15%, 3～7 days drying times, for example 3.5My god, 4 days, 4.5 days, 5 days, 5.5 days, 6 days or 6.5 days, preferably 5～7 days, redrying adopt drumAir-dry dry method, 70～110 DEG C of redrying temperature, for example 75 DEG C, 80 DEG C, 85 DEG C, 90 DEG C,95 DEG C, 100 DEG C or 105 DEG C, drying time 12～48h, for example 15h, 20h, 25h, 30h, 35h, 40hOr 45h, preferably 24～48h.
In the present invention, primary drying directly affects the yield rate of catalyst prod, will be by honeybee at this procedureMost moisture in nest shape moulding idiosome evaporate, and to ensure that idiosome is indeformable simultaneously, not ftracture, because ofThis must strictly control dry temperature and humidity. Redrying medium is hot-air, will be through primary dryingCellular moulding idiosome carry out redrying, remove remaining moisture in cellular moulding idiosome.
Preferably, 110～600 DEG C of calcining heats in step (d), for example 150 DEG C, 200 DEG C, 250 DEG C,300 DEG C, 350 DEG C, 400 DEG C, 450 DEG C, 500 DEG C or 550 DEG C, preferably 300～500 DEG C, calcination time6～24h, for example 8h, 12h, 16h, 20h or 22h, preferably 6～12h.
It is denitration preformed catalyst that three of object of the present invention is to provide a kind of cellular vanadium as abovePurposes, described catalyst is for the purification of nitrogen oxides of FCC flue gas.
Compared with the prior art, the present invention has following beneficial effect:
The present invention is by adopting the main component of titanium dioxide as catalyst, and this catalyst powder is with businessAnatase titania be carrier, V2O5For active component, WO3For coagent, obtain powder catalysisAgent, and to obtain cellular vanadium by specific shaping assistant and moulding process be denitration preformed catalyst,To preformed catalyst there is excellent anti-SO2With steam poisoning performance, the denitration efficiency of excellence, goodStability and excellent mechanical performance. Described catalyst is at air speed (4000h-1), high-load titanium dioxideIn the flue gas of sulphur (>=1500ppm) and high-load steam (>=5%), NOx conversion ratio is very high, its300～450 DEG C of conversion ratios that can reach more than 90%, at 350 DEG C, after 100h, its conversion ratio can be protectedBe held in more than 90%. In addition, more than the compression strength of described catalyst can reach 4MPa.
Brief description of the drawings
Fig. 1 is the denitration activity change curve of embodiment 3 prepared catalyst, wherein, and air speed 4000h-1，NH3/NOx＝1，NOx1000ppm，O23％，SO21500ppm，H2O5％。
Fig. 2 is the denitration stability change curve of embodiment 3 prepared catalyst, wherein,
Air speed 4000h-1，NH3/NOx＝1，NOx1000ppm，O23％，SO21500ppm，H2O5％。
Detailed description of the invention
Further illustrate technical scheme of the present invention below in conjunction with accompanying drawing and by detailed description of the invention.
Embodiment 1
The oxalic acid solution of configuration 5wt%, then adds ammonium metavanadate, active component V2O5Content accounts for catalyst0.1% of powder quality percentage composition, stirring and dissolving at the temperature of 55 DEG C, becomes navy blue to solution, thenAdd ammonium metatungstate, WO3Content accounts for 10% of catalyst powder weight percentage composition, is stirred to dissolving. SoAfter this solution is joined in titania powder, uniform stirring, obtains slurries. Dry at 110 DEG C12h, grinds, and roasting 5h at 500 DEG C grinds, and obtains catalyst powder.
Take catalyst powder, then add solid forming auxiliary agent glass fibre, active carbon, methylcelluloseStir and be dry mixed, wherein content of glass fiber is 10%, and active carbon content is 10%, and methylcellulose containsAmount is 1%, adds liquid molding auxiliary agents of silicon colloidal sol, glycerine to carry out wet mixing, wherein Ludox after mixingContent is 5%, and glycerol content is 10%, then adds water and mix, until that humidity of materials is transferred to after suitable is trueIn empty pug mill, mix, the time of mixing is 30min, repeatedly mix 3 times, and the material having mixedNeed to carry out oldly, the old time is 12h, then old good idiosome is extruded in extruderType is cellular, need in constant temperature and humidity drying case, carry out once for the cellular molding blank of formingDry, design temperature and humidity program, slowly heat up, and baking temperature scope is 30～70 DEG C, and humidity changesScope is 95～10%, 5～7 days arid cycles, then carries out redrying, temperature is controlled at 70～110 DEG C, be 24～48h arid cycle, finally carries out calcination processing, calcination temperature range is 300～500 DEG C, the calcining cycle is 6～12h, finally obtains cellular preformed catalyst.
The honeycombed catalyst activity test method making is: honeycombed catalyst is put into and is connected with simulation fire coalIn the reactor of power-plant flue gas, measure NO with flue gas analyzerxInitial concentration, then measure each temperatureSection flue gas is by remaining NO after catalystxConcentration, then calculate NOxConversion ratio and SO2OxygenRate, finally obtains the Evaluation results of catalyst.
Embodiment 2
The oxalic acid solution of configuration 5wt%, then adds ammonium metavanadate, active component V2O5Content accounts for catalyst3% of powder quality percentage composition, stirring and dissolving at the temperature of 55 DEG C, becomes navy blue to solution, thenAdd ammonium metatungstate, WO3Content accounts for 1% of catalyst powder weight percentage composition, is stirred to dissolving. SoAfter this solution is joined in titania powder, uniform stirring, obtains slurries. Dry at 110 DEG C12h, grinds, and roasting 5h at 500 DEG C grinds, and obtains catalyst powder.
Take catalyst powder, then add solid forming auxiliary agent glass fibre, sesbania powder, polyvinyl alcohol to enterRow stirs and is dry mixed, and wherein content of glass fiber is 10%, and sesbania powder content is 5%, and polyvinyl alcohol content is1%, after mixing, add liquid molding auxiliary agents of silicon colloidal sol, glycerine to carry out wet mixing, wherein Ludox content is5%, glycerol content is 15%, then adds water and mix, until humidity of materials is transferred to vacuum pugging after suitableIn machine, mix, the time of mixing is 30min, repeatedly mixes 3 times, and the material having mixed need to enterRow is old, and the old time is 12h, and then old good idiosome being carried out to extrusion molding in extruder is honeybeeNest shape need to carry out primary drying for the cellular molding blank of forming in constant temperature and humidity drying case,Design temperature and humidity program, slowly heat up, and baking temperature scope is 30～70 DEG C, and range of humidity variation is95～10%, 3～5 days arid cycles, then carry out redrying, temperature is controlled at 70～110 DEG C, dryCycle is 12～24h, finally carries out calcination processing, and calcination temperature range is 300～500 DEG C, the calcining cycleBe 36～48h, finally obtain cellular preformed catalyst.
The honeycombed catalyst activity test method making is: honeycombed catalyst is put into and is connected with simulation fire coalIn the reactor of power-plant flue gas, measure NO with flue gas analyzerxInitial concentration, then measure each temperatureSection flue gas is by remaining NO after catalystxConcentration, then calculate NOxConversion ratio and SO2OxygenRate, finally obtains the Evaluation results of catalyst.
Embodiment 3
The oxalic acid solution of configuration 5wt%, then adds ammonium metavanadate, active component V2O5Content accounts for catalyst1.5% of powder quality percentage composition, stirring and dissolving at the temperature of 55 DEG C, becomes navy blue to solution, thenAdd ammonium metatungstate, WO3Content accounts for 10% of catalyst powder weight percentage composition, is stirred to dissolving. SoAfter this solution is joined in titania powder, uniform stirring, obtains slurries. Dry at 110 DEG C12h, grinds, and roasting 5h at 500 DEG C grinds, and obtains catalyst powder.
Take catalyst powder, then add solid forming auxiliary agent glass fibre, waterglass, active carbon, hydroxylPropyl methocel, sesbania powder stir and are dry mixed, and wherein content of glass fiber is 10%, and active carbon containsAmount is 5%, and sesbania powder content is 5%, and hydroxypropyl methylcellulose content is 5%, after mixing, adds liquidBody formed auxiliary agents of silicon colloidal sol, glycerine carry out wet mixing, and wherein Ludox content is 5%, and glycerol content is 10%,Add water and mix again, mix until humidity of materials is transferred in vacuum deairing machine after suitable, mix oneThe inferior time is 30min, repeatedly mixes 3 times, and the material having mixed need to carry out old, and the old time is12h, it is cellular then old good idiosome being carried out to extrusion molding in extruder, for formingCellular molding blank need to carry out primary drying, design temperature and humidity journey in constant temperature and humidity drying caseOrder, slowly heats up, and baking temperature scope is 30～70 DEG C, and range of humidity variation is 95～10%, dry week5～7 days phases, then carry out redrying, temperature is controlled at 70～110 DEG C, be 24 arid cycle～48h, finally carries out calcination processing, and calcination temperature range is 110～500 DEG C, and the calcining cycle is 36～48h,Finally obtain cellular preformed catalyst.
The honeycombed catalyst activity test method making is: honeycombed catalyst is put into and is connected with simulation fire coalIn the reactor of power-plant flue gas, measure NO with flue gas analyzerxInitial concentration, then measure each temperatureSection flue gas is by remaining NO after catalystxConcentration, then calculate NOxConversion ratio and SO2OxygenRate, finally obtains the Evaluation results of catalyst.
Embodiment 4
The oxalic acid solution of configuration 5wt%, then adds ammonium metavanadate, active component V2O5Content accounts for catalyst1.5% of powder quality percentage composition, stirring and dissolving at the temperature of 55 DEG C, becomes navy blue to solution, thenAdd ammonium metatungstate, WO3Content accounts for 5% of catalyst powder weight percentage composition, is stirred to dissolving. SoAfter this solution is joined in titania powder, uniform stirring, obtains slurries. Dry at 110 DEG C12h, grinds, and roasting 5h at 500 DEG C grinds, and obtains catalyst powder.
Take catalyst powder, then add solid forming auxiliary agent glass fibre, sesbania powder, PEOStir and be dry mixed, wherein content of glass fiber is 10%, and sesbania powder content is 10%, and PEO containsAmount is 3%, adds liquid molding auxiliary agents of silicon colloidal sol, glycerine to carry out wet mixing, wherein Ludox after mixingContent is 15%, and glycerol content is 10%, then adds water and mix, until humidity of materials is transferred to after suitableIn vacuum deairing machine, mix, the time of mixing is 30min, repeatedly mix 3 times, and the thing having mixedMaterial need to carry out old, and the old time is 12h, then old good idiosome is extruded in extruderBe shaped to cellularly, need in constant temperature and humidity drying case, carry out one for the cellular molding blank of formingInferior dry, design temperature and humidity program, slowly heat up, and baking temperature scope is 30～70 DEG C, and humidity becomesChange scope is 95～10%, 4～6 days arid cycles, then carries out redrying, temperature is controlled at 70～110 DEG C, be 12～24h arid cycle, finally carries out calcination processing, calcination temperature range is 110～500 DEG C, the calcining cycle is 36～48h, finally obtains cellular preformed catalyst.
The honeycombed catalyst activity test method making is: honeycombed catalyst is put into and is connected with simulation fire coalIn the reactor of power-plant flue gas, measure NO with flue gas analyzerxInitial concentration, then measure each temperatureSection flue gas is by remaining NO after catalystxConcentration, then calculate NOxConversion ratio and SO2OxygenRate, finally obtains the Evaluation results of catalyst.
Embodiment 5
The oxalic acid solution of configuration 5wt%, then adds ammonium metavanadate, active component V2O5Content accounts for catalyst1% of powder quality percentage composition, stirring and dissolving at the temperature of 55 DEG C, becomes navy blue to solution, thenAdd ammonium metatungstate, WO3Content accounts for 5% of catalyst powder weight percentage composition, is stirred to dissolving. SoAfter this solution is joined in titania powder, uniform stirring, obtains slurries. Dry at 110 DEG C12h, grinds, and roasting 5h at 500 DEG C grinds, and obtains catalyst powder.
Take catalyst powder, then add solid forming auxiliary agent glass fibre, sesbania powder, polyvinyl alcohol to enterRow stirs and is dry mixed, and wherein content of glass fiber is 10%, and sesbania powder content is 5%, and polyvinyl alcohol content is5%, after mixing, add liquid molding auxiliary agents of silicon colloidal sol, glycerine to carry out wet mixing, wherein Ludox content is5%, glycerol content is 10%, then adds water and mix, until humidity of materials is transferred to vacuum pugging after suitableIn machine, mix, the time of mixing is 30min, repeatedly mixes 3 times, and the material having mixed need to enterRow is old, and the old time is 6h, and then old good idiosome being carried out to extrusion molding in extruder is honeycombShape need to carry out primary drying for the cellular molding blank of forming in constant temperature and humidity drying case, establishesFixed temperature and humidity program, slowly heat up, and baking temperature scope is 30～70 DEG C, and range of humidity variation is95～10%, 5～7 days arid cycles, then carry out redrying, temperature is controlled at 70～110 DEG C, dryCycle is 24～48h, finally carries out calcination processing, and calcination temperature range is 300～500 DEG C, the calcining cycleBe 24～48h, finally obtain cellular preformed catalyst. The honeycombed catalyst activity test method makingFor: honeycombed catalyst is put into the reactor that is connected with simulation coal-fired plant flue gas, surveyed with flue gas analyzerDetermine the initial concentration of NOx, then measure dense by remaining NOx after catalyst of each temperature section flue gasSpend, then calculate conversion ratio and the SO of NOx2Oxygenation efficiency, finally obtain the performance evaluation knot of catalystReally.
The honeycombed catalyst activity test method making is: honeycombed catalyst is put into and is connected with simulation fire coalIn the reactor of power-plant flue gas, measure NO with flue gas analyzerxInitial concentration, then measure each temperatureSection flue gas is by remaining NO after catalystxConcentration, then calculate NOxConversion ratio and SO2OxygenRate, finally obtains the Evaluation results of catalyst.
Embodiment 6
The oxalic acid solution of configuration 5wt%, then adds ammonium metavanadate, active component V2O5Content accounts for catalyst0.8% of powder quality percentage composition, stirring and dissolving at the temperature of 55 DEG C, becomes navy blue to solution, thenAdd ammonium metatungstate, WO3Content accounts for 5% of catalyst powder weight percentage composition, is stirred to dissolving. SoAfter this solution is joined in titania powder, uniform stirring, obtains slurries. Dry at 110 DEG C12h, grinds, and roasting 5h at 500 DEG C grinds, and obtains catalyst powder.
Take catalyst powder, then add solid forming auxiliary agent glass fibre, active carbon, methylcelluloseStir and be dry mixed, wherein content of glass fiber is 10%, and active carbon content is 5%, methylcellulose contentBe 1%, add liquid molding auxiliary agents of silicon colloidal sol, glycerine to carry out wet mixing after mixing, wherein Ludox containsAmount is 5%, and glycerol content is 10%, then adds water and mix, until humidity of materials is transferred to vacuum after suitableIn pug mill, mix, the time of mixing is 30min, repeatedly mixes 3 times, and the material having mixed needsCarry out oldly, the old time is 48h, then old good idiosome is carried out to extrusion molding in extruderFor cellular, need in constant temperature and humidity drying case, once do for the cellular molding blank of formingDry, design temperature and humidity program, slowly heat up, and baking temperature scope is 30～70 DEG C, and humidity changesScope is 95～10%, 5～7 days arid cycles, then carries out redrying, temperature is controlled at 70～110 DEG C, be 24～48h arid cycle, finally carries out calcination processing, calcination temperature range is 300～500 DEG C, the calcining cycle is 6～12h, finally obtains cellular preformed catalyst.
The honeycombed catalyst activity test method making is: honeycombed catalyst is put into and is connected with simulation fire coalIn the reactor of power-plant flue gas, measure NO with flue gas analyzerxInitial concentration, then measure each temperatureSection flue gas is by remaining NO after catalystxConcentration, then calculate NOxConversion ratio and SO2OxygenRate, finally obtains the Evaluation results of catalyst.
Embodiment 7
The oxalic acid solution of configuration 5wt%, then adds ammonium metavanadate, active component V2O5Content accounts for catalyst1% of powder quality percentage composition, stirring and dissolving at the temperature of 55 DEG C, becomes navy blue to solution, thenAdd ammonium metatungstate, WO3Content accounts for 5% of catalyst powder weight percentage composition, is stirred to dissolving. SoAfter this solution is joined in titania powder, uniform stirring, obtains slurries. Dry at 110 DEG C12h, grinds, and roasting 5h at 500 DEG C grinds, and obtains catalyst powder.
Take catalyst powder, then add solid forming auxiliary agent glass fibre, active carbon, methylcelluloseStir and be dry mixed, wherein content of glass fiber is 10%, and active carbon content is 5%, methylcellulose contentBe 1%, add liquid molding auxiliary agents of silicon colloidal sol, glycerine to carry out wet mixing after mixing, wherein Ludox containsAmount is 5%, and glycerol content is 10%,, then add water and mix, until that humidity of materials is transferred to after suitable is trueIn empty pug mill, mix, the time of mixing is 30min, repeatedly mix 3 times, and the material having mixedNeed to carry out oldly, the old time is 48h, then old good idiosome is extruded in extruderType is cellular, need in constant temperature and humidity drying case, carry out once for the cellular molding blank of formingDry, design temperature and humidity program, slowly heat up, and baking temperature scope is 30～70 DEG C, and humidity becomesChange scope is 95～10%, 5～7 days arid cycles, then carries out redrying, temperature is controlled at 70～110 DEG C, be 24～48h arid cycle, finally carries out calcination processing, calcination temperature range is 300～500 DEG C, the calcining cycle is 6～12h, finally obtains cellular preformed catalyst.
The honeycombed catalyst activity test method making is: honeycombed catalyst is put into and is connected with simulation fire coalIn the reactor of power-plant flue gas, measure NO with flue gas analyzerxInitial concentration, then measure each temperatureSection flue gas is by remaining NO after catalystxConcentration, then calculate NOxConversion ratio and SO2OxygenRate, finally obtains the Evaluation results of catalyst.
Embodiment 8
The oxalic acid solution of configuration 5wt%, then adds ammonium metavanadate, active component V2O5Content accounts for catalyst0.5% of powder quality percentage composition, stirring and dissolving at the temperature of 55 DEG C, becomes navy blue to solution, thenAdd ammonium metatungstate, WO3Content accounts for 10% of catalyst powder weight percentage composition, is stirred to dissolving. SoAfter this solution is joined in titania powder, uniform stirring, obtains slurries. Dry at 110 DEG C12h, grinds, and roasting 5h at 500 DEG C grinds, and obtains catalyst powder.
Take catalyst powder, then add solid forming auxiliary agent glass fibre, active carbon, methylcelluloseStir and be dry mixed, wherein content of glass fiber is 15%, and active carbon content is 5%, PEO contentBe 1.5%, add liquid molding auxiliary agents of silicon colloidal sol, glycerine to carry out wet mixing after mixing, wherein Ludox containsAmount is 5%, and glycerol content is 10%, then adds water and mix, until humidity of materials is transferred to vacuum after suitableIn pug mill, mix, the time of mixing is 30min, repeatedly mixes 3 times, and the material having mixed needsCarry out oldly, the old time is 48h, then old good idiosome is carried out to extrusion molding in extruderFor cellular, need in constant temperature and humidity drying case, once do for the cellular molding blank of formingDry, design temperature and humidity program, slowly heat up, and baking temperature scope is 30～70 DEG C, and humidity changesScope is 95～10%, 5～7 days arid cycles, then carries out redrying, temperature is controlled at 70～110 DEG C, be 24～48h arid cycle, finally carries out calcination processing, calcination temperature range is 300～500 DEG C, the calcining cycle is 6～12h, finally obtains cellular preformed catalyst.
The honeycombed catalyst activity test method making is: honeycombed catalyst is put into and is connected with simulation fire coalIn the reactor of power-plant flue gas, measure NO with flue gas analyzerxInitial concentration, then measure each temperatureSection flue gas is by remaining NO after catalystxConcentration, then calculate NOxConversion ratio and SO2OxygenRate, finally obtains the Evaluation results of catalyst.
(specification is that 20cm is long, and the cellular of 37mm*37mm urged to get respectively the catalyst of embodiment 1～10Agent) pack in catalyst performance evaluation reaction unit, carry out activity rating by simulation gas. Simulation gas is pressedAccording to coal-burning power plant or petroleum catalytic cracking tail gas composition, it is composed as follows: NO (1000ppm), O2(3％)，NH3(1000ppm)、SO2(1500ppm), steam (5%), N2For carrier gas, gasTotal flow 14L/min, the volume space velocity of gas is 4000h-1, catalyst 250～350 DEG C of cigarette temperature andAs shown in the table at 350 DEG C of reaction results after 100h:
Catalyst compression strength is at microcomputer controlled electronic anti-folding and anti-pressing testing machine (YDW-03 type, the prosperous high-tech in HangzhouCo., Ltd) on carry out, unit is N. The catalysis of being cut into solid shape is carved to (2.5cmx2.5cmx5cm) putsOn testing machine platform, by continuous pressure, in the time that pressure suddenly disappears, read maximum pressure value, and pass throughRepeatedly test averages to reduce accidental error. Test result is as shown in the table:
Comparative example 1
This catalyst is the enforcement that its disclosed forming method of the disclosed employing of patent CN101676024A obtainsThe V-W/TiO of example 12Catalyst.
Comparative example 2
This catalyst is the disclosed V-W/TiO of patent CN101428215A2Catalyst.
Comparative example 3
This catalyst is the disclosed V-W/TiO of patent CN101711978A2Catalyst.
Comparative example 4
The composition of catalyst powder is with embodiment 3, except adopting the disclosed forming method of CN101676024A to obtainTo preformed catalyst.
Comparative example 5
Catalyst powder consist of the disclosed powder catalyst of CN104162421A embodiment 1, and adoptThe forming method identical in order to embodiment 3 carries out moulding.
(specification is that 20cm is long, and the cellular of 37mm*37mm urged to get respectively the catalyst of comparative example 1～5Agent) pack in catalyst performance evaluation reaction unit, carry out activity rating by simulation gas. Simulation gas is pressedAccording to coal-burning power plant or petroleum catalytic cracking tail gas composition, it is composed as follows: NO (1000ppm), O2(3％)，NH3(1000ppm)、SO2(1500ppm), steam (5%), N2For carrier gas, gasTotal flow 14L/min, the volume space velocity of gas is 4000h-1, catalyst in the time of 250～350 DEG C of cigarette temperature,Reaction result is as shown in the table:
Catalyst compression strength is at microcomputer controlled electronic anti-folding and anti-pressing testing machine (YDW-03 type, the prosperous high-tech in HangzhouCo., Ltd) on carry out, unit is N. The catalysis of being cut into solid shape is carved to (2.5cmx2.5cmx5cm) putsOn testing machine platform, by continuous pressure, in the time that pressure suddenly disappears, read maximum pressure value, and pass throughRepeatedly test averages to reduce accidental error. Test result is as shown in the table:
Comparative example 6
All the other are identical with embodiment 3, are 7% except controlling content of glass fiber.
Comparative example 7
All the other are identical with embodiment 3, are 1% except controlling active carbon content, and sesbania powder content is 2%.
Comparative example 8
All the other are identical with embodiment 3, are 8% except controlling hydroxypropyl methylcellulose content.
Comparative example 9
All the other are identical with embodiment 3, are 3% except controlling Ludox content.
Comparative example 10
All the other are identical with embodiment 3, are 18% except controlling glycerol content.
Comparative example 11
All the other are identical with embodiment 3, except shaping assistant is not for containing Ludox.
Comparative example 12
All the other are identical with embodiment 3, except shaping assistant does not contain hydroxypropyl methylcellulose.
(specification is that 20cm is long, and the cellular of 37mm*37mm urged to get respectively the catalyst of comparative example 6～12Agent) pack in catalyst performance evaluation reaction unit, carry out activity rating by simulation gas. Simulation gas is pressedAccording to coal-burning power plant or petroleum catalytic cracking tail gas composition, it is composed as follows: NO (1000ppm), O2(3％)，NH3(1000ppm)、SO2(1500ppm), steam (5%), N2For carrier gas, gasTotal flow 14L/min, the volume space velocity of gas is 4000h-1, catalyst in the time of 250～350 DEG C of cigarette temperature,Reaction result is as shown in the table:
Catalyst compression strength is at microcomputer controlled electronic anti-folding and anti-pressing testing machine (YDW-03 type, the prosperous high-tech in HangzhouCo., Ltd) on carry out, unit is N. The catalysis of being cut into solid shape is carved to (2.5cmx2.5cmx5cm) putsOn testing machine platform, by continuous pressure, in the time that pressure suddenly disappears, read maximum pressure value, and pass throughRepeatedly test averages to reduce accidental error. Test result is as shown in the table:
Can find with comparative example 6～12 by embodiment 3, organic and inorganic bond be used in conjunction with andThe content of each shaping assistant of certain content is vital for realizing excellent technique effect.
Comparative example 13
All the other are identical with embodiment 3, except after primary drying technique finishes, directly carry out calcination processing, and notCarry out redrying technique.
Comparative example 14
All the other are identical with embodiment 3, except not carrying out primary drying technique, and directly carry out redrying technique,Then calcining.
Comparative example 15
All the other are identical with embodiment 3, except primary drying temperature is 90 DEG C.
Comparative example 16
All the other are identical with embodiment 3, except redrying temperature is 60 DEG C.
(specification is that 20cm is long, and 37mm*37mm's is cellular to get respectively the catalyst of comparative example 13～16Catalyst) pack in catalyst performance evaluation reaction unit, carry out activity rating by simulation gas. Simulation gasAccording to coal-burning power plant or petroleum catalytic cracking tail gas composition, it is composed as follows: NO (1000ppm), O2(3％)，NH3(1000ppm)、SO2(1500ppm), steam (5%), N2For carrier gas, gasTotal flow 14L/min, the volume space velocity of gas is 4000h-1, catalyst in the time of 250～350 DEG C of cigarette temperature,Reaction result is as shown in the table:
Catalyst compression strength is at microcomputer controlled electronic anti-folding and anti-pressing testing machine (YDW-03 type, the prosperous high-tech in HangzhouCo., Ltd) on carry out, unit is N. The catalysis of being cut into solid shape is carved to (2.5cmx2.5cmx5cm) putsOn testing machine platform, by continuous pressure, in the time that pressure suddenly disappears, read maximum pressure value, and pass throughRepeatedly test averages to reduce accidental error. Test result is as shown in the table:
Can find with comparative example 13～16 by embodiment 3, only contain primary drying technique or redryingThe technique effect of technique is all inferior to the technique effect that adopts primary drying and redrying technique and deposit significantly.And specific primary drying technique and redrying technique are also must for realizing excellent technique effectWant.
In sum, catalyst of the present invention has strong anti-SO2With steam ability, there is good stablizingProperty, and excellent mechanical performance, the denitration condition of work of applicable FCC apparatus.
To those skilled in the art, obviously the invention is not restricted to the details of above-mentioned example embodiment,And in the situation that not deviating from spirit of the present invention or essential characteristic, can realize with other concrete formThe present invention. Therefore, no matter from which point, all should regard embodiment as exemplary, and right and wrongRestrictive, scope of the present invention is limited by claims instead of above-mentioned explanation, is therefore intended to fallAll changes in the implication and the scope that are equal to important document of claim are included in the present invention.
In addition although should be appreciated that this description is described according to embodiment, be not each enforcement,Mode only comprises an independently technical scheme, and this narrating mode of description is only for clarity sake,Those skilled in the art should make description as a whole, and the technical scheme in each embodiment also can be throughAppropriately combined, form other embodiments that it will be appreciated by those skilled in the art that.
Applicant's statement, the present invention illustrates method detailed of the present invention by above-described embodiment, but the present inventionBe not limited to above-mentioned method detailed, do not mean that the present invention must rely on above-mentioned method detailed ability realExecute. Person of ordinary skill in the field should understand, any improvement in the present invention, to product of the present inventionThe selections of the equivalence replacement of each raw material and the interpolation of auxiliary element, concrete mode etc., all drop on guarantor of the present inventionWithin protecting scope and open scope.
Claims (10)
1. cellular vanadium is a denitration preformed catalyst, and it is mainly by catalyst powder and shaping assistantMoulding obtains, and described catalyst powder is taking anatase titania as carrier, V2O5For active component, WO3For coagent.
2. preformed catalyst as claimed in claim 1, is characterized in that, at described catalyst powderIn, active component V2O5Quality be 0.1～3% of catalyst powder weight, preferably 0.1～1.5%.
3. preformed catalyst as claimed in claim 1 or 2, is characterized in that, at described catalyst powderIn, coagent WO3Quality be 1～10% of catalyst powder weight, preferably 1～5%.
4. the preformed catalyst as described in one of claim 1-3, is characterized in that, described shaping assistant isThe mixture of reinforcing agent, inorganic binder, organic binder bond, pore creating material and lubricant;
Preferably, described reinforcing agent content is 10～30% of catalyst powder weight, preferably 10～20%;
Preferably, described reinforcing agent is glass fibre;
Preferably, described inorganic binder is that waterglass is or/and Ludox;
Preferably, the content of described inorganic binder is 5～15% of catalyst powder weight, preferably5～8％；
Preferably, described organic binder bond be polyvinyl alcohol, hydroxypropyl methylcellulose, methylcellulose orThe mixture of any one in PEO or at least two kinds;
Preferably, the content of described organic binder bond is 1～5% of catalyst powder weight, preferably 2～4%;
Preferably, described pore creating material is that active carbon is or/and sesbania powder;
Preferably, the content of described pore creating material is 5～10% of catalyst powder weight, preferably 8～10%;
Preferably, described lubricant is glycerine;
Preferably, described lubricant content is 10～15% of catalyst powder weight, preferably 10～12%.
5. the preparation side that the cellular vanadium as described in one of claim 1-4 is denitration preformed catalystMethod, described method comprises preparation and the forming process of catalyst powder.
6. method as claimed in claim 5, is characterized in that, adopts the method preparation of volume dippingCatalyst powder, comprises the following steps:
(1) in oxalic acid solution, add vanadium source, being stirred to solution is navy blue, then adds tungsten source, stirsExtremely without solid matter;
(2) solution step (1) being obtained joins in titania powder, and uniform stirring, is starchedLiquid, dry, grind, roasting, then grind, obtain catalyst powder.
7. method as claimed in claim 6, is characterized in that, the concentration of described oxalic acid solution is5～10wt％；
Preferably, described tungsten source is selected from any one in ammonium metatungstate, ammonium tungstate, potassium tungstate or sodium tungstateOr the mixture of at least two kinds;
Preferably, described vanadium source is ammonium metavanadate;
Preferably, step (1) adds behind vanadium source, and at the temperature of 40～55 DEG C, being stirred to solution is navy blue;
Preferably, the described baking temperature of step (2) is 80～120 DEG C, and be 12～24h drying time;
Preferably, the described sintering temperature of step (2) is 400～550 DEG C, and roasting time is 3～8h, preferably5h。
8. the method as described in one of claim 5-7, is characterized in that, described forming process comprises followingStep:
(a) catalyst powder and solid forming auxiliary agent are dry mixed, then add liquid molding auxiliary agent to carry outWet mixing, then adds deionized water to stir;
(b) material step (a) being obtained is transferred in vacuum deairing machine and is fully mixed, and then allowsIt carries out the old of 6～48h, obtains final moulding idiosome;
(c) moulding idiosome step (b) being obtained is extruded as cellular by extrusion shaping machine;
(d) cellular moulding idiosome step (c) being obtained is dried, and calcining, obtains cellular vanadiumIt is denitration preformed catalyst.
9. method as claimed in claim 8, is characterized in that, in step (a), catalyst powder is with solidBody formed auxiliary agent adds and is dry mixed simultaneously;
Preferably, carry out primary drying and redrying two procedures in step (d), primary drying adopts permanentThe method of wet constant temperature, 30～70 DEG C of primary drying temperature, humidity 85～10%, 3～7 days drying times, preferably5～7 days, redrying adopted the method for forced air drying, 70～110 DEG C of redrying temperature, drying time12～48h, preferably 24～48h;
Preferably, 110～600 DEG C of calcining heats in step (d), preferably 300～500 DEG C, calcination time6～24h, preferably 6～12h.
10. the cellular vanadium as described in one of claim 1-4 is a purposes for denitration preformed catalyst,Described catalyst is for the purification of nitrogen oxides of FCC flue gas.
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