CN102114423B - Denitrifying catalyst and preparation method thereof as well as flue gas denitrifying method - Google Patents
Denitrifying catalyst and preparation method thereof as well as flue gas denitrifying method Download PDFInfo
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- CN102114423B CN102114423B CN2011100052642A CN201110005264A CN102114423B CN 102114423 B CN102114423 B CN 102114423B CN 2011100052642 A CN2011100052642 A CN 2011100052642A CN 201110005264 A CN201110005264 A CN 201110005264A CN 102114423 B CN102114423 B CN 102114423B
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Abstract
The invention relates to a denitrifying catalyst and a preparation method thereof as well as a flue gas denitrifying method. The preparation method of the denitrifying catalyst comprises the following steps: mixing, aging, drying and calcining, wherein in the mixing step, ITAC-14-7A, CTAC-115, stearic acid, deionized water, ammonia, lactic acid, glass fiber, wood pulp, water, an ammonium metavanadate solution, carboxymethyl cellulose and polyoxyethylene are mixed by a mixer. The denitrifying catalyst prepared by the method has high-efficiency denitrifying efficiency.
Description
Technical field
The present invention relates to a kind of Preparation of catalysts method, particularly relate to a kind of catalyst for denitrating flue gas
The preparation method.
Background technology
The coal in China consumption is big, and the environmental pollution that causes thus is particularly serious, wherein flue dust, SO
2With, NOx is major pollutants.The present situation of China coal fired power plant NOx discharged nitrous oxides is, nineteen ninety-five discharge capacity be 2,650,000 tons, 2000 is 4,690,000 tons, 2002 is 5,200,000 tons, expects 2011 and will reach 5,500,000 tons, NOx becomes the main pollutant of thermal power generation discharging.NOx is one of main source of acid rain, or the precursor substance of photochemical fog.To form bigger harm to health and ecological environment simultaneously.
At present, coal fired power plant the most effectively NOx control technology is SCR (SCR) technology, and the crucial high performance catalyst of SCR.But existing denitrating catalyst exists intensity low, is prone to efflorescence, lacks service life, and manufacturing process is difficult for shaping and demoulding, and porosity is undesirable, and catalytic efficiency is low, catalyst amount is big, the high deficiency of cost.Therefore, the denitrating catalyst of developing a kind of cheapness is the problem that Selective Catalytic Reduction of NO x technology presses for solution.
Summary of the invention
Main purpose of the present invention is, overcomes the defective that existing denitrating catalyst exists, and a kind of new denitrating catalyst and preparation method thereof is provided, and technical problem to be solved is to overcome the problems referred to above, further improves denitration efficiency.
The object of the invention and solve its technical problem and adopt following technical scheme to realize.The preparation method of a kind of denitrating catalyst that proposes according to the present invention; Comprise mixing, aging, drying and calcination steps, described mixing step be with ITAC-140-7A, CTAC-115, stearic acid, deionized water, ammoniacal liquor, lactic acid, glass fibre, wood pulp, water and aforesaid ammonium metavanadate solution, carboxymethyl cellulose and polyethylene glycol oxide add carry out in the mixing roll mixing.
Preferably, the preparation method of the denitrating catalyst that the present invention proposes, described ammonium metavanadate solution is that the water by the ammonium metavanadate of the monoethanol ammonium of 80-100 weight portion, 70-80 weight portion and 650-1000 weight portion mixes and obtains.
Preferably, the preparation method of the denitrating catalyst that the present invention proposes, described mixing step comprises following process:
Once mixing: the CTAC-115 of the ITAC-140-7A of 280-350 weight portion and 80-120 weight portion is carried out mixing in mixing roll, 15% the ammoniacal liquor of water and 40-50 weight portion that adds 50% lactic acid, the 200-250 weight portion of stearic acid, the 5.5-7.0 weight portion of 1.0-1.5 weight portion then carries out mixing;
Secondary is mixing: after once mixing, with the water of the ITAC-140-7A of 80-120 weight portion and 15-20 weight portion join once carry out in the mixing batch mixing that obtains mixing;
Three times are mixing: after secondary is mixing, with 15% ammoniacal liquor of the ITAC-140-7A of 100-150 weight portion and 5-10 weight portion join carry out in the mixing batch mixing that obtains of secondary mixing;
Four times are mixing: three times mixing after, with the water of the wood pulp of the glass fibre of 30-40 weight portion, 2.8-3.5 weight portion, 40-60 weight portion and 40-80 weight portion ammonium metavanadate solution join carry out in three mixing batch mixings that obtain mixing;
Five times are mixing: four times mixing after, with the polyethylene glycol oxide of the carboxymethyl cellulose of 1.5-3.0 weight portion and 1.8-3.0 weight portion join carry out in four mixing batch mixings that obtain mixing;
Six times are mixing: five times mixing after, with 15% ammoniacal liquor of the polyethylene glycol oxide of the carboxymethyl cellulose of 1.5-3.0 weight portion and 1.8-3.0 weight portion and 3-8 weight portion join carry out in five mixing batch mixings that obtain mixing.
Preferably, the preparation method of the denitrating catalyst that the present invention proposes, described once mixing mixing time is 5-30 minute, the pH value of the once mixing batch mixing that obtains should if the pH value should be lower than 7.5, then add ammoniacal liquor and regulate greater than 7.5.
Preferably, the preparation method of the denitrating catalyst that the present invention proposes in three mixing process, when temperature of charge reaches 95 ℃, discharges the gas that mixing material produces, and three times the mixing moisture that finishes in the material of back reaches 25.5-27.5wt%.
Preferably, the preparation method of the denitrating catalyst that the present invention proposes, in aging step, the temperature of ageing environment is 20-30 ℃, humidity is greater than 80%.
Preferably, the preparation method of the denitrating catalyst that the present invention proposes, described drying steps comprises:
Primary drying, the temperature of dry environment are 25-65 ℃, and humidity is 15-85%, and be more than 10 days drying time; With
Redrying, the temperature of dry environment are 60-65 ℃.
Preferably, the preparation method of the denitrating catalyst that the present invention proposes, described calcination steps comprises:
One section intensification was elevated to 200 ℃-250 ℃ with 5 hours with temperature;
One section roasting, the constant roasting 4-5 of holding temperature hour;
Two sections intensifications after one section roasting finishes, were elevated to 600 ℃-650 ℃ with 8 hours with temperature;
Two-stage calcination, the constant roasting 4.5-6 of holding temperature hour.
The present invention also proposes a kind of denitrating catalyst, is the catalyst that the preparation method by above-mentioned denitrating catalyst prepares.
The present invention also proposes a kind of denitration method for flue gas, adopts described denitrating catalyst that flue gas is carried out denitration and handles.
By technique scheme, the preparation method of denitrating catalyst of the present invention has advantage at least:
The denitrating catalyst that the present invention provides method for preparing catalyst to prepare has the compressive resistance height, is difficult for efflorescence, long service life, the easy shaping and demoulding of manufacturing process, ideal porosity, advantage such as catalytic efficiency is high, catalyst amount is few, cost is low.
Above-mentioned explanation only is the general introduction of technical scheme of the present invention, understands technological means of the present invention in order can more to know, and can implement according to the content of specification, below with preferred embodiment of the present invention specify as after.
The specific embodiment
Should reach technological means and the effect that predetermined goal of the invention is taked for further setting forth the present invention; Below in conjunction with preferred embodiment; Its specific embodiment of preparation method, structure, characteristic and effect thereof to the denitrating catalyst that proposes according to the present invention specify as follows.
The preparation method of denitrating catalyst of the present invention mainly may further comprise the steps:
The preparation example 1 of ammonium metavanadate solution
In the ammonium metavanadate dissolving tank, add 720 liters of deionized waters and 93.6 kilograms of monoethanol ammoniums (MEA); Through Steam Heating to 80 ℃; Add 75.2 kilograms of ammonium metavanadate powder (AMV) then; Continuation is heated mixing material through steam, is 98 ℃ and the maintenance 30 minutes of under this temperature, wearing out up to ammonium metavanadate dissolving tank temperature.Temperature with mixed material is adjusted into 60 ℃ then.With deionized water adjustment liquor capacity to 900 liter, obtain ammonium metavanadate solution at last.
The preparation example 2 of ammonium metavanadate solution
In the ammonium metavanadate dissolving tank, add 600 liters of deionized waters and double centner monoethanol ammonium (MEA); Through Steam Heating to 70 ℃; Add 80 kilograms of ammonium metavanadate powder (AMV) then; Continuation is heated mixing material through steam, is 95 ℃ and the maintenance 25 minutes of under this temperature, wearing out up to ammonium metavanadate dissolving tank temperature.Temperature with mixed material is adjusted into 55 ℃ then.With deionized water adjustment liquor capacity to 650 liter, obtain ammonium metavanadate solution at last.
The preparation example 3 of ammonium metavanadate solution
In the ammonium metavanadate dissolving tank, add 900 liters of deionized waters and 80 kilograms of monoethanol ammoniums (MEA); Through Steam Heating to 85 ℃; Add 70 kilograms of ammonium metavanadate powder (AMV) then; Continuation is heated mixing material through steam, is 90 ℃ and the maintenance 45 minutes of under this temperature, wearing out up to ammonium metavanadate dissolving tank temperature.Temperature with mixed material is adjusted into 65 ℃ then.With deionized water adjustment liquor capacity to 1000 liter, obtain ammonium metavanadate solution at last.
Preparation of Catalyst embodiment 1
Mixing
Once mixing: a certain amount of 292.7 kilograms ITAC-140-7A (TiO2-WO3) and 100.5 kilograms CTAC-115 (TiO2-WO3-SiO2) are joined in the powerful muller, and through the low speed rotation of rotor, rotating speed is 350rpm, the operation mixing roll.Then, add the ammoniacal liquor of 1.30 kilograms of stearic acid, 6.5 kilogram 50% lactic acid (50%LA), 230 liters of deionized waters and 45 liter 15%, with above material mix, mixing.Mixing process moves mixing roll 7 minutes for the high speed rotation (750rpm) through rotor.
Above-mentioned ITAC-140-7A and CTAC-115 change into the titania powder that Co., Ltd. produces for Japan's day sunshine catalyst, and ITAC-140-7A and CTAC-115 are product grades.Above-mentioned titania powder is from the hydrolysis of titanium sulfate solution, to obtain.Titanium dioxide is anatase titanium dioxide.The representative value of burning vector is 3% in the time of 1000 ℃.
The representative property of titania powder (ITAC-140-7A) is following:
140 ± 10 millimeters of the peak heights of X ray
Specific area 90 ± 10m
2/ g
ITAC-140-7A consists of:
Titanium dioxide 93 ± 0.7%
Tungstic acid 7 ± 0.7%
Sodium oxide molybdena maximum 0.01%
Potassium oxide maximum 0.01%
Di-iron trioxide maximum 0.01%
Four sulfur oxide 1.5-3.5%
The representative property of titania powder (CTAC-115) is following:
110 ± 15 millimeters of the peak heights of X ray
Specific area 110 ± 20m
2/ g
CTAC-115 consists of:
Titanium dioxide 90 ± 1.0%
Tungstic acid 5 ± 0.7%
Silica 7.5 ± 3.5%
Sodium oxide molybdena maximum 0.06%
Potassium oxide maximum 0.03%
Di-iron trioxide maximum 0.01%
Four sulfur oxides maximum 2.8%
Secondary is mixing: after once mixing; A certain amount of 105.0 kilograms ITAC-140-7A powder to mixing roll and 18 liters of deionized waters are joined once further to mix, carry out secondary in the mixing batch mixing that obtains mixing, the operation mixing roll 20 minutes of running up of rotor.
Three times are mixing: after secondary was mixing, the ammoniacal liquor of ITAC-140-7A and 8 liter 15% that adds 135.0 kilograms mixed in the mixing batch mixing that obtains of secondary, carry out three times mixing.When the temperature of mixed material reaches 95 ℃; Open the mixing roll air bleeding valve and discharge the gas that produces in the material; Open (leading to the ammonia stripping tower) exhaust air throttle fully near mixing roll; And regulate opening near the exhaust air throttle of ammonia stripping tower, waste gas can not revealed from hood like this, and continues mixing 35 minutes.Reach 25.5-27.5wt% at moisture, stop three times mixing.In order to obtain raw-material plasticity, the operating sequence of muller, batch mixing moisture must strictly be controlled by regulation in this stage.In three mixing operations,, open NH for the moisture of getting rid of in the batch mixing is convenient to drying
3The exhaust blower of scrubbing tower.
Four times are mixing: three times mixing after; Under rotor low speed, in three mixing batch mixings that obtain, add 36.1 kilograms of ammonium metavanadate solutions of going into preparation example 1 preparation of glass fibre (GF), 3.25 kilograms of wood pulp cottons, 50 liters of deionized waters and 50 liters of aforementioned ammonium metavanadate solutions.The high speed rotating operation mixing roll of rotor continued mixing, mixing in 10 minutes then.
Five times are mixing: four times mixing after, change the rotation direction and the low cruise of rotor, add 2.14 kilograms of carboxymethyl celluloses (CMC) and 2.44 kilograms of polyethylene glycol oxides (PEO) successively.After adding carboxymethyl cellulose and polyethylene glycol oxide, operation mixing roll air-cooler is also regulated the opening near the exhaust air throttle of ammonia stripping tower, and waste gas can not revealed from hood like this, and passes through the high-speed reverse rotating operation mixing roll 5 minutes of rotor.During five mixing end, stop the mixing roll air-cooler simultaneously.
Six times are mixing: five times mixing after, the ammoniacal liquor that adds remaining 2.14 thousand carboxymethyl celluloses (CMC), 2.44 kilograms of polyethylene glycol oxides (PEO) and 5 liter 15% continues to mix, mixing, moves the muller cooling blower simultaneously.When moisture through adding 15% ammoniacal liquor and deionized water adjustment batch mixing and pH value, moisture is 29.7wt%, and bulk density is 2.1g/cm
3, the pH value is 8.0.
With pack into batch mixing cloth bag sealing of the material after mixing.The time of placing then at least one day wears out.
Through the material after mixing, its typical physical data such as table 1
The mixing back of table 1 material physical data
| Index | ? |
| Moisture (%) | 29.7 |
| Bulk density (g/cm 3) | 2.1 |
| The pH value | 8.0 |
| The residue ratio (%) of 200 order mesh oversize material | ＜0.40 |
| Plasticity (plasticity index) | 23.0-25.0 |
| Constriction coefficient (8 millimeters rods, %) | 4.0-5.6 |
| TiO 2Content (wt%) | 87±5.0 |
| WO 3Content (wt%) | 6.0±1.0 |
| V 2O 5Content (wt%) | 0.5±0.2 |
The measuring condition of moisture in the last table: 180 ℃, infrared moisture meter 30 minutes.
Filter
Add the material that blendes together in the batch mixing cloth bag to the filter hopper, the filter discharging opening is equipped with screen cloth.Filter after the filtration becomes material to join preparatory extruder preformed continuously.Preformed raw material is cut into the cylinder stripping and slicing by piano wire extruding in advance on the conveyer.Stripping and slicing is positioned on the pallet, and more than 12 hours, the stripping and slicing after wearing out is filled in the extruder with vinyl drop cloth seal aging.
Extrude
Extruding the stage, extruder will be extruded raw material in advance and be extruded as honeycomb ceramics.
Open the vinyl drop cloth in the preformed stripping and slicing, stripping and slicing is placed send into the extruder charging aperture on the extruder feeding conveyor, outlet of extruder is equipped with mould.
Preforming material is extruded honeycomb ceramics through the extruder mould, and honeycomb ceramics slides on the extruder conveyer through exerting oneself of extruder, isolates with the sponge backing plate between extrusion pin and conveyer, and extrusion pin is cut into the length of regulation with piano wire on the extruder conveyer.Then, smear resinous coat at two tangent planes of extrusion pin with brush, the carton of packing into of the extrusion pin after smearing, and between extrusion pin and carton place mat sponge and paper, get into the ageing step.
When confirming the length of extrusion pin cutting, must consider that the longitudinal length that drying, roasting cause shrinks.When starting extruder, use vavuum pump to get rid of the air of extruder vacuum chamber, need add cooling agent at low side spiral and peripheral cylinder simultaneously.The vacuum pressure of vacuum chamber with extrude raw-material temperature and must maintain below the rated value separately.Resinous coat is the crack to occur for the two ends that prevent extrusion pin.Paint coatings solution is to be that 1: 1 mixed forms by resin and acetone with volume ratio.Described resin main component is a vinyl chloride-vinyl acetate copolymer, is solvent with ethyl acetate, non-volatile residual be 40 ± 1%, stickiness is 4000 ± 1000cps (30 ℃).This resin for example is KBK12 number of KANEBO-NSC company.
When smearing resinous coat, make and paint organic volatile gas poisonous in the exhaust blower deaeration.Extruding the stage, needing the preceding extrusion pressure of control mould is 15-40kg/cm2, and extruded velocity is 600-1000mm/ minute.The physical data of extrusion pin material is as shown in table 2.
The physical data of table 2 extrusion pin material
| Moisture (%) | 29.7 |
| Bulk density (g/cm 3) | 0.67 |
| The pH value | 8.0 |
Aging
In the ageing step, the internal moisture of balance extrusion pin, and discharge extrusion pressure.The carton that extrusion molding article is housed is positioned over respectively on the primary drying shelf, during the course, extrusion pin is weighed, and measures extrusion pin sectional dimension and length, confirms shrinkage factor.Dry shelf left standstill in hothouse more than 24 hours.In the ageing step, the temperature of primary drying chamber must maintain 20-30 ℃, and humidity should be greater than 80%.
Primary drying
In this stage, aging extrusion pin carries out evenly in hothouse, slowly, drying progressively.
Air heater adds hot-air, and primary drying cycling hot blower fan goes into circulation the air of each hothouse.The temperature of primary drying chamber is controlled at by the controller that is installed in the air heater outlet and regulates, and the thermal source of air heater is a steam.On the other hand, the humidity of hothouse is controlled at through controller (executing agency) and regulates.If dry indoor humidity is on the low side, then spray into steam; If humidity is higher, then discharges the high humility circulating air and inject the low humidity air.Two injection line of circulating air are installed on the bottom of hothouse, and circulating air sprays into hothouse through the nozzle on the injection line.Be installed on nozzle exit with sheet metal or other similar installations, avoid hot-air directly to blow dry product.
The primary drying shelf that extrusion pin is housed are put into hothouse, take out after dry 10 days.
The temperature and humidity control data of primary drying process is as shown in table 3.
The temperature and humidity control data table of table 3 primary drying process
In the hothouse temperature-rise period, dry product is weighed and measured sectional dimension and length, confirm shrinkage factor.After accomplishing primary drying, take out the dry product in the carton, put in the redrying shelf, put into then in the redrying case.At the dry initial stage of dry product, need progressively orderly drying so that the even degree of uneven drying minimizes, and realize that the catalyst internal particle arranges (therefore occurring shrinking) again, uneven drying is even possibly to cause that dry product breaks, breakage.
Therefore; In the incipient stage of drying; Baking temperature is maintained low relatively state; And in two sides on cutting surface and near the outer wall application of resin coating (note: the catalyst drying is dry very fast with the cutting corner on the cutting surface) of building stones cut point, thereby avoid uneven drying, and use the carton that to alleviate air-flow and improve the catalyst ambient humidity, light and temperature.The moisture that catalyst inside gives out will be in a state that soaks in carton, and will move to the carton outside gradually through the humidity difference inside and outside the carton.
Redrying
Residue moisture in the catalyst is extremely important with the profile that influences the roasting product that from mesh-belt kiln, comes out for the inner air of control mesh-belt kiln.In this step, the product behind the primary drying is carried out further drying, adopt flue gas to reduce residue moisture through the mode in the hole in its drying box.Product behind the primary drying is installed in the redrying shelf.Suitably insert sealing gasket between the sidewall of every catalyst and the shelf madial wall.The shelf of fully loaded catalyst is moved in the redrying case, under 60-65 ℃ temperature, carries out drying.In dry run, the weight reduction ratio of results of regular determination product less than 25%, then continues dry like the weight reduction ratio of fruit product.
After the redrying step was accomplished, every dry product was drawn out shelf, and is sent to mesh-belt kiln.Be imported into each drying box by redrying air heater heated hot air heated through the redrying blower fan.The thermal source of redrying air heater is a steam.In this step, the hot air temperature of each drying box import must keep below designated value, thereby avoids the MEA burning in the catalyst.
Roasting
(1) scope
In this step, the redrying article carry out the roasting of active and reinforcement aspect through mesh-belt kiln.
Catalyst is placed on the guipure of mesh-belt kiln.In this case, catalyst should be arranged on the parallel direction of guipure operation.The control of sintering temperature is carried out according to following mode,
One section intensification was elevated to 200 ℃-250 ℃ with 5 hours with temperature,
One section roasting, the constant roasting 4-5 of holding temperature hour;
Two sections intensifications after one section roasting finishes, were elevated to 600 ℃-650 ℃ with 8 hours with temperature;
Two-stage calcination, the constant roasting 4.5-6 of holding temperature hour;
Cooling, the baked catalyst that exports out from mesh-belt kiln is deposited on the tray, with 8-10 hour, with the product cool to room temperature.
Take every caution against error and handle baked catalyst, because they lack flexibility, and also more frangible than dry product.
Mesh-belt kiln has a lot of curtain walls at the top, the end in inside has the spacer of fragment of brick, and this space with catalyst top on the guipure has been divided into several sections, thereby lets fresh air circulate through catalyst pores.Use sack cleaner to handle all waste gas.After roasting was accomplished, every catalyst was moved to cutting step.The physical data of the catalyst that obtains after the process roasting is as shown in table 4.
The physical data of the catalyst that obtains after table 4 roasting
Cutting
In this step, the catalyst of each roasting all is cut the machine cutting, makes it meet the length of appointment, blows off with the dust of hand-held blower fan with catalyst cut surface and perforate.
Each baked catalyst is placed on the cutting support of cutting machine, slides into a band saw then, by the two ends that predetermined operation is cut baked catalyst, makes product meet designated length.
The waste product that cuts from each catalyst is collected in sealing preservation in the drum.When cutting, the dust around the cutting machine is discharged by the dust cleaning case blower fan.
After cutting was accomplished, each product all was deposited on the shelf, is placed into the dedusting area ash disposal then, and the hand-held exhaust blower of dust cleaning case is used for this purposes.The dust cleaning case blower fan is used to discharge the waste gas of dust cleaning case.
Packing
In packaging process, product should closely be placed and arrange in packing, and product just can not damage in transportation like this.
Denitration effect test 1
The 1m that the foregoing description is made
3Denitrating catalyst is inserted in the reactor, feeds typical boiler smoke, and concrete composition is the NO of 500ppm, the SO of 400ppm
2, 15% CO
2, 7% H
2O, all the other are N
2, 380 ℃ of flue-gas temperatures, air speed are 30000h
-1, NOx/NH
3Be 1.1, detecting its denitration rate behind the reaction 200h is 95%.
Filtration among the above embodiment and extrusion step be used to prepare have given shape preformed catalyst, do not have above-mentioned steps not influence the denitration catalyst performance of catalyst.
Preparation of Catalyst embodiment 2
Mixing
Once mixing: a certain amount of 280 kilograms ITAC-140-7A (TiO2-WO3) and 120 kilograms CTAC-115 (TiO2-WO3-SiO2) are joined in the powerful muller, and through the low speed rotation of rotor, rotating speed is 350rpm, the operation mixing roll.Then, add the ammoniacal liquor of 1.0 kilograms of stearic acid, 5.0 kilogram 50% lactic acid (50%LA), 200 liters of deionized waters and 40 liter 15%, with above material mix, mixing.Mixing process moves mixing roll 7 minutes for the high speed rotation (750rpm) through rotor.
Secondary is mixing: after once mixing; A certain amount of 120 kilograms ITAC-140-7A powder to mixing roll and 15 liters of deionized waters are joined once further to mix, carry out secondary in the mixing batch mixing that obtains mixing, the operation mixing roll 20 minutes of running up of rotor.
Three times are mixing: after secondary was mixing, the ammoniacal liquor of ITAC-140-7A and 10 liter 5% that adds double centner mixed in the mixing batch mixing that obtains of secondary, carry out three times mixing.When the temperature of mixed material reaches 95 ℃; Open the mixing roll air bleeding valve and discharge the gas that produces in the material; Open (leading to the ammonia stripping tower) exhaust air throttle fully near mixing roll; And regulate opening near the exhaust air throttle of ammonia stripping tower, waste gas can not revealed from hood like this, and continues mixing 35 minutes.Reach 25.5wt% at moisture, stop three times mixing.In order to obtain raw-material plasticity, the operating sequence of muller, batch mixing moisture must strictly be controlled by regulation in this stage.In three mixing operations,, open NH for the moisture of getting rid of in the batch mixing is convenient to drying
3The exhaust blower of scrubbing tower.
Four times are mixing: three times mixing after, under rotor low speed, in three mixing batch mixings that obtain, add the ammonium metavanadate solutions of 30 kilograms of preparation example 2 preparations of going into glass fibre (GF), 2.8 kilograms of wood pulp cottons, 40 liters of deionized waters and 40 liters of aforementioned ammonium metavanadate solutions.The high speed rotating operation mixing roll of rotor continued mixing, mixing in 10 minutes then.
Five times are mixing: four times mixing after, change the rotation direction and the low cruise of rotor, add 1.5 kilograms of carboxymethyl celluloses (CMC) and 1.8 kilograms of polyethylene glycol oxides (PEO) successively.After adding carboxymethyl cellulose and polyethylene glycol oxide, operation mixing roll air-cooler is also regulated the opening near the exhaust air throttle of ammonia stripping tower, and waste gas can not revealed from hood like this, and passes through the high-speed reverse rotating operation mixing roll 5 minutes of rotor.During five mixing end, stop the mixing roll air-cooler simultaneously.
Six times are mixing: five times mixing after, the ammoniacal liquor that adds remaining 1.5 thousand carboxymethyl celluloses (CMC), 1.8 kilograms of polyethylene glycol oxides (PEO) and 3 liter 15% continues to mix, mixing, moves the muller cooling blower simultaneously.When moisture through adding 15% ammoniacal liquor and deionized water adjustment batch mixing and pH value, moisture is 29.7wt%, and bulk density is 2.1g/cm
3, the pH value is 8.0.
With pack into batch mixing cloth bag sealing of the material after mixing.The time of placing then at least one day wears out.
Filter
Add the material that blendes together in the batch mixing cloth bag to the filter hopper, the filter discharging opening is equipped with screen cloth.Filter after the filtration becomes material to join preparatory extruder preformed continuously.Preformed raw material is cut into the cylinder stripping and slicing by piano wire extruding in advance on the conveyer.Stripping and slicing is positioned on the pallet, and more than 12 hours, the stripping and slicing after wearing out is filled in the extruder with vinyl drop cloth seal aging.
Extrude
Extruding the stage, extruder will be extruded raw material in advance and be extruded as honeycomb ceramics.
Open the vinyl drop cloth in the preformed stripping and slicing, stripping and slicing is placed send into the extruder charging aperture on the extruder feeding conveyor, outlet of extruder is equipped with mould.
Preforming material is extruded honeycomb ceramics through the extruder mould, and honeycomb ceramics slides on the extruder conveyer through exerting oneself of extruder, isolates with the sponge backing plate between extrusion pin and conveyer, and extrusion pin is cut into the length of regulation with piano wire on the extruder conveyer.Then, smear resinous coat at two tangent planes of extrusion pin with brush, the carton of packing into of the extrusion pin after smearing, and between extrusion pin and carton place mat sponge and paper, get into the ageing step.
When confirming the length of extrusion pin cutting, must consider that the longitudinal length that drying, roasting cause shrinks.When starting extruder, use vavuum pump to get rid of the air of extruder vacuum chamber, need add cooling agent at low side spiral and peripheral cylinder simultaneously.The vacuum pressure of vacuum chamber with extrude raw-material temperature and must maintain below the rated value separately.Resinous coat is the crack to occur for the two ends that prevent extrusion pin.Paint coatings solution is to be that 1: 1 mixed forms by resin and acetone with volume ratio.Described resin main component is a vinyl chloride-vinyl acetate copolymer, is solvent with ethyl acetate, non-volatile residual be 40 ± 1%, stickiness is 4000 ± 1000cps (30 ℃).This resin for example is KBK12 number of KANEBO-NSC company.
When smearing resinous coat, make and paint organic volatile gas poisonous in the exhaust blower deaeration.Extruding the stage, needing the preceding extrusion pressure of control mould is 15-40kg/cm
2, extruded velocity is 600-1000mm/ minute.
Aging
In the ageing step, the internal moisture of balance extrusion pin, and discharge extrusion pressure.The carton that extrusion molding article is housed is positioned over respectively on the primary drying shelf, during the course, extrusion pin is weighed, and measures extrusion pin sectional dimension and length, confirms shrinkage factor.Dry shelf left standstill in hothouse more than 24 hours.In the ageing step, the temperature of primary drying chamber must maintain 30 ℃, and humidity should be greater than 80%.
Primary drying
The primary drying shelf that extrusion pin is housed are put into hothouse, take out after dry 10 days.
The temperature and humidity control data of primary drying process is as shown in table 3.
In the incipient stage of drying; Baking temperature is maintained low relatively state; And in two sides on cutting surface and near the outer wall application of resin coating (note: the catalyst drying is dry very fast with the cutting corner on the cutting surface) of building stones cut point; Thereby avoid uneven drying, and use the carton that to alleviate air-flow and improve the catalyst ambient humidity, light and temperature.
Redrying
The shelf of fully loaded catalyst is moved in the redrying case, under 60-65 ℃ temperature, carries out drying.In dry run, the weight reduction ratio of results of regular determination product less than 25%, then continues dry like the weight reduction ratio of fruit product.
Roasting
The control of sintering temperature is carried out according to following mode,
One section intensification was elevated to 200 ℃-250 ℃ with 5 hours with temperature,
One section roasting, the constant roasting 4-5 of holding temperature hour;
Two sections intensifications after one section roasting finishes, were elevated to 600 ℃-650 ℃ with 8 hours with temperature;
Two-stage calcination, the constant roasting 4.5-6 of holding temperature hour;
Cooling, the baked catalyst that exports out from mesh-belt kiln is deposited on the tray, with 8-10 hour, with the product cool to room temperature.
Take every caution against error and handle baked catalyst, because they lack flexibility, and also more frangible than dry product.
Mesh-belt kiln has a lot of curtain walls at the top, the end in inside has the spacer of fragment of brick, and this space with catalyst top on the guipure has been divided into several sections, thereby lets fresh air circulate through catalyst pores.Use sack cleaner to handle all waste gas.After roasting was accomplished, every catalyst was moved to cutting step.The physical data of the catalyst that obtains after the process roasting is as shown in table 5.
The physical data of the catalyst that obtains after table 5 roasting
Denitration effect test 2
The 1m that the foregoing description is made
3Denitrating catalyst is inserted in the reactor, feeds typical boiler smoke, and concrete composition is 500ml/m
3NO, 400ml/m
3SO
2, 15% CO
2, 7% H
2O, all the other are N
2, 380 ℃ of flue-gas temperatures, air speed are 30000h
-1, NOx/NH
3Be 1.1, detecting its denitration rate behind the reaction 200h is 94%.
Preparation of Catalyst embodiment 3
Mixing
Once mixing: a certain amount of 350 kilograms ITAC-140-7A (TiO2-WO3) and 80 kilograms CTAC-115 (TiO2-WO3-SiO2) are joined in the powerful muller, and through the low speed rotation of rotor, rotating speed is 350rpm, the operation mixing roll.Then, add the ammoniacal liquor of 1.5 kilograms of stearic acid, 8.0 kilogram 50% lactic acid (50%LA), 250 liters of deionized waters and 50 liter 5%, with above material mix, mixing.Mixing process moves mixing roll 7 minutes for the high speed rotation (750rpm) through rotor.
Secondary is mixing: after once mixing, a certain amount of 80 kilograms ITAC-140-7A powder to mixing roll and 20 liters of deionized waters are joined once further to mix, carry out secondary in the mixing batch mixing that obtains mixing, the operation mixing roll 40 minutes of running up of rotor.
Three times are mixing: after secondary was mixing, the ammoniacal liquor of ITAC-140-7A and 5 liter 15% that adds 150 kilograms mixed in the mixing batch mixing that obtains of secondary, carry out three times mixing.When the temperature of mixed material reaches 96 ℃, open the mixing roll air bleeding valve and discharge the gas that produces in the material, and continued mixing 35 minutes.Reach 27.5wt% at moisture, stop three times mixing.
Four times are mixing: three times mixing after, under rotor low speed, in three mixing batch mixings that obtain, add the ammonium metavanadate solutions of 40 kilograms of preparation example 3 preparations of going into glass fibre (GF), 3.5 kilograms of wood pulp cottons, 60 liters of deionized waters and 80 liters of aforementioned ammonium metavanadate solutions.The high speed rotating operation mixing roll of rotor continued mixing, mixing in 10 minutes then.
Five times are mixing: four times mixing after, change the rotation direction and the low cruise of rotor, add 3.0 kilograms of polyethylene glycol oxides of 3.0 kilograms of carboxymethyl celluloses (CMC) (PEO) successively.After adding carboxymethyl cellulose and polyethylene glycol oxide, operation mixing roll air-cooler is also regulated the opening near the exhaust air throttle of ammonia stripping tower, and waste gas can not revealed from hood like this, and passes through the high-speed reverse rotating operation mixing roll 5 minutes of rotor.During five mixing end, stop the mixing roll air-cooler simultaneously.
Six times are mixing: five times mixing after, the ammoniacal liquor that adds remaining 3.0 thousand carboxymethyl celluloses (CMC), 3.0 kilograms of polyethylene glycol oxides (PEO) and 8 liter 15% continues to mix, mixing, moves the muller cooling blower simultaneously.When moisture through adding 15% ammoniacal liquor and deionized water adjustment batch mixing and pH value, moisture is 30wt%, and bulk density is 2.2g/cm
3, the pH value is 7.6.
With pack into batch mixing cloth bag sealing of the material after mixing.The time of placing then at least one day wears out.
Filter
Add the material that blendes together in the batch mixing cloth bag to the filter hopper, the filter discharging opening is equipped with screen cloth.Filter after the filtration becomes material to join preparatory extruder preformed continuously.Preformed raw material is cut into the cylinder stripping and slicing by piano wire extruding in advance on the conveyer.Stripping and slicing is positioned on the pallet, and more than 12 hours, the stripping and slicing after wearing out is filled in the extruder with vinyl drop cloth seal aging.
Extrude
Extruding the stage, extruder will be extruded raw material in advance and be extruded as honeycomb ceramics.
Open the vinyl drop cloth in the preformed stripping and slicing, stripping and slicing is placed send into the extruder charging aperture on the extruder feeding conveyor, outlet of extruder is equipped with mould.
Preforming material is extruded honeycomb ceramics through the extruder mould, and honeycomb ceramics slides on the extruder conveyer through exerting oneself of extruder, isolates with the sponge backing plate between extrusion pin and conveyer, and extrusion pin is cut into the length of regulation with piano wire on the extruder conveyer.Then, smear resinous coat at two tangent planes of extrusion pin with brush, the carton of packing into of the extrusion pin after smearing, and between extrusion pin and carton place mat sponge and paper, get into the ageing step.
When confirming the length of extrusion pin cutting, must consider that the longitudinal length that drying, roasting cause shrinks.When starting extruder, use vavuum pump to get rid of the air of extruder vacuum chamber, need add cooling agent at low side spiral and peripheral cylinder simultaneously.The vacuum pressure of vacuum chamber with extrude raw-material temperature and must maintain below the rated value separately.Resinous coat is the crack to occur for the two ends that prevent extrusion pin.Paint coatings solution is to be that 1: 1 mixed forms by resin and acetone with volume ratio.Described resin main component is a vinyl chloride-vinyl acetate copolymer, is solvent with ethyl acetate, non-volatile residual be 40 ± 1%, stickiness is 4000 ± 1000cps (30 ℃).This resin for example is KBK12 number of KANEBO-NSC company.
When smearing resinous coat, make and paint organic volatile gas poisonous in the exhaust blower deaeration.Extruding the stage, needing the preceding extrusion pressure of control mould is 15-40kg/cm2, and extruded velocity is 600-1000mm/ minute.
Aging
In the ageing step, the internal moisture of balance extrusion pin, and discharge extrusion pressure.The carton that extrusion molding article is housed is positioned over respectively on the primary drying shelf, during the course, extrusion pin is weighed, and measures extrusion pin sectional dimension and length, confirms shrinkage factor.Dry shelf left standstill in hothouse more than 24 hours.In the ageing step, the temperature of primary drying chamber must maintain 20 ℃, and humidity should be greater than 80%.
Primary drying
The primary drying shelf that extrusion pin is housed are put into hothouse, and the temperature of dry environment is 65 ℃, and humidity is 15%, take out after dry 13 days.
Redrying
The shelf of fully loaded catalyst is moved in the redrying case, under 65 ℃ temperature, carries out drying.In dry run, the weight reduction ratio of results of regular determination product less than 25%, then continues dry like the weight reduction ratio of fruit product.
Roasting
The control of sintering temperature is carried out according to following mode,
One section intensification was elevated to 200 ℃-250 ℃ with 5 hours with temperature,
One section roasting, the constant roasting 4-5 of holding temperature hour;
Two sections intensifications after one section roasting finishes, were elevated to 600 ℃-650 ℃ with 8 hours with temperature;
Two-stage calcination, the constant roasting 4.5-6 of holding temperature hour;
Cooling, the baked catalyst that exports out from mesh-belt kiln is deposited on the tray, with 8-10 hour, with the product cool to room temperature.
Take every caution against error and handle baked catalyst, because they lack flexibility, and also more frangible than dry product.
Mesh-belt kiln has a lot of curtain walls at the top, the end in inside has the spacer of fragment of brick, and this space with catalyst top on the guipure has been divided into several sections, thereby lets fresh air circulate through catalyst pores.Use sack cleaner to handle all waste gas.After roasting was accomplished, every catalyst was moved to cutting step.The physical data of the catalyst that obtains after the process roasting is as shown in table 6.
The physical data of the catalyst that obtains after table 6 roasting
Denitration effect test 3
The 1m that the foregoing description 3 is made
3Denitrating catalyst is inserted in the reactor, feeds typical boiler smoke, and concrete composition is 500ml/m
3NO, 400ml/m
3SO
2, 15% CO
2, 7% H
2O, all the other are N
2, 380 ℃ of flue-gas temperatures, air speed are 30000h
-1, NOx/NH
3Be 1.1, detecting its denitration rate behind the reaction 200h is 96%.
The various raw material properties that adopted in the above-described embodiments are following.
Ammonium metavanadate is equivalent to the ammonium metavanadate of SHINCO chemistry Co., Ltd.Carboxymethyl cellulose is equivalent to the NH of NICHIRIN chemical industry Co., Ltd
4-CMC NA-L, representative property is: dry loss: 10-20% (105 ℃ time drying), stickiness: 100-300mPa.s (1.0wt dry% solution), pH value 5-8.Polyethylene glycol oxide is equivalent to the ALKOX E-160 type of MEISEI chemical industry Co., Ltd, and stickiness is 150-170mPa.s (a 0.5wt% solution), ash: maximum 2.5%, apparent bulk density 0.2-0.45g/ml, molecular wt are 3.6-4 1,000,000.MEA is equivalent to the MEA of Japanese CHEMTECH Co., Ltd, proportion: 1.017-1.019 (20 ℃), and molecular wt: 61-62.5, the amine value: 910-920mg KOH/g, moisture: maximum 0.3%, H2N-CH2CH2OH minimum 99%.Lactic acid is equivalent to the lactic acid of MISASHINO chemical laboratory Co., Ltd, proportion (d20/20): 1.12-1.13, lactic acid: 50-52wt%.Glass fibre is equivalent to the short chopping of glass of FUJI glass fibre Co., Ltd, size: diameter (um) 11 ± 1.5um, and length (mm) 6 ± 1.5mm, this glass fibre all is the E-glass mould.Cotton pulp is equivalent to the LDP-R08 of FUJIGAWA SENKA Co., Ltd, granularity: 100% through the 8mm screen cloth.Stearic acid is equivalent to the stearic acid Cica-level solvent of KANTO chemical industry Co., Ltd, dissolves point: 64-71 ℃, acid number: 192-202, iodine number; Maximum 3%. binders are equivalent to the MARINE BOND-M of Japanese ASBESTOS Co., Ltd.Ceramic fibre is equivalent to the ceramic fibre ceramic wool of ORIBEST Co., Ltd, is equivalent to the SC BLANKET 1260 of Japanese SYEEL chemistry Co., Ltd.
The above only is preferred embodiment of the present invention, is not the present invention is done any pro forma restriction; Though the present invention discloses as above with preferred embodiment; Yet be not in order to limiting the present invention, anyly be familiar with the professional and technical personnel, in not breaking away from technical scheme scope of the present invention; When the technology contents of above-mentioned announcement capable of using is made a little change or is modified to the equivalent embodiment of equivalent variations; In every case be the content that does not break away from technical scheme of the present invention, to any simple modification, equivalent variations and modification that above embodiment did, all still belong in the scope of technical scheme of the present invention according to technical spirit of the present invention.
Claims (8)
1. the preparation method of a denitrating catalyst comprises mixing, aging, drying and calcination steps, and it is characterized in that: described mixing step comprises following process:
Once mixing: 280-350 parts by weight of titanium oxide powder ITAC-140-7A and 80-120 parts by weight of titanium oxide powder CTAC-115 are carried out mixing in mixing roll, the ammoniacal liquor of 5-15% of water and 40-50 weight portion that adds lactic acid, the 200-250 weight portion of stearic acid, the 2.5-4.0 weight portion of 1.0-1.5 weight portion then carries out mixing;
Secondary is mixing: after once mixing, with the water of 80-120 parts by weight of titanium oxide powder ITAC-140-7A and 15-20 weight portion join once carry out in the mixing batch mixing that obtains mixing;
Three times are mixing: after secondary is mixing, with the ammoniacal liquor of the 5-15% of 100-150 parts by weight of titanium oxide powder ITAC-140-7A and 5-10 weight portion join carry out in the mixing batch mixing that obtains of secondary mixing;
Four times are mixing: three times mixing after, with the ammonium metavanadate solution of the water of the wood pulp of the glass fibre of 30-40 weight portion, 2.8-3.5 weight portion, 40-60 weight portion and 40-80 weight portion join carry out in three mixing batch mixings that obtain mixing;
Five times are mixing: four times mixing after, with the polyethylene glycol oxide of the carboxymethyl cellulose of 1.5-3.0 weight portion and 1.8-3.0 weight portion join carry out in four mixing batch mixings that obtain mixing;
Six times are mixing: five times mixing after, with the ammoniacal liquor of the 5-15% of the polyethylene glycol oxide of the carboxymethyl cellulose of 1.5-3.0 weight portion and 1.8-3.0 weight portion and 3-8 weight portion join carry out in five mixing batch mixings that obtain mixing;
Above-mentioned titania powder ITAC-140-7A consists of:
Above-mentioned titania powder CTAC-115 consists of:
2. the preparation method of denitrating catalyst according to claim 1; It is characterized in that described once mixing mixing time is 5-30 minute, the pH value of the once mixing batch mixing that obtains should be greater than 7.5; If the pH value should be lower than 7.5, then add ammoniacal liquor and regulate.
3. the preparation method of denitrating catalyst according to claim 1 is characterized in that, in three mixing process, when temperature of charge reaches 95 ℃, discharges the gas that mixing material produces, and three times the mixing moisture that finishes in the material of back reaches 25.5-27.5wt%.
4. the preparation method of denitrating catalyst according to claim 1 is characterized in that, in aging step, the temperature of ageing environment is 20-30 ℃, and humidity is greater than 80%.
5. the preparation method of denitrating catalyst according to claim 1 is characterized in that, described drying steps comprises:
Primary drying, the temperature of dry environment are 25-65 ℃, and humidity is 15-85%, and be more than 10 days drying time;
Redrying, the temperature of dry environment are 60-65 ℃.
6. the preparation method of denitrating catalyst according to claim 1 is characterized in that, described calcination steps comprises:
One section intensification was elevated to 200 ℃-250 ℃ with 5 hours with temperature;
One section roasting, the constant roasting 4-5 of holding temperature hour;
Two sections intensifications after one section roasting finishes, were elevated to 600 ℃-650 ℃ with 8 hours with temperature;
Two-stage calcination, the constant roasting 4.5-6 of holding temperature hour.
7. a denitrating catalyst is characterized in that the catalyst that it is prepared by the preparation method of each described denitrating catalyst of claim 1-6.
8. a denitration method for flue gas is characterized in that adopting the described denitrating catalyst of claim 7 that flue gas is carried out denitration and handles.
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| CN102614866B (en) * | 2012-03-01 | 2013-08-28 | 浙江大学 | Honeycomb SCR smoke denitration catalyst embryoid body and preparation method thereof |
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| CN103638980A (en) * | 2013-11-21 | 2014-03-19 | 张亚丽 | Denitrification catalyst |
| CN103673590A (en) * | 2013-12-06 | 2014-03-26 | 湖北大清捷能环保窑炉有限公司 | Honeycomb type SCR denitration catalyst calcining furnace and method for drying SCR denitration catalyst |
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| CN106622214A (en) * | 2016-12-16 | 2017-05-10 | 内蒙古华元科技有限公司 | Flue gas denitrification titanium-based catalyst for ceramic and preparation method of catalyst |
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| CN106693953A (en) * | 2016-12-27 | 2017-05-24 | 内蒙古华元科技有限公司 | Ti-based catalyst for coking flue gas denitrification and preparation method thereof |
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| CN101347722B (en) * | 2008-09-05 | 2011-08-31 | 江苏科行环境工程技术有限公司 | Catalyst for denitration by SCR method with low cost and preparation method thereof |
| CN101676024A (en) * | 2008-09-17 | 2010-03-24 | 晶锐瓷业（北京）有限公司 | Faviform ammonia-method selective-catalytic-reduction denitrified catalyst and preparation method thereof |
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