CN105126818A - Wear-resistant anti-poisoning honeycomb SCR denitration catalyst and preparation method thereof - Google Patents
Wear-resistant anti-poisoning honeycomb SCR denitration catalyst and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a wear-resistant anti-poisoning honeycomb SCR denitration catalyst and a preparation method thereof. The method includes the steps of mixing, primary ageing, filtration and pre-extrusion, secondary ageing, extrusion forming, first-stage drying, second-stage drying, roasting, cutting and end face hardening. The denitration catalyst has the advantages of being high in wear resistance, compressive strength and anti-poisoning capacity, easy to form in an extrusion mode, good in denitration activity, long in service life and the like. By adding montmorillonite clay for replacing part of titanium tungsten powder, the raw material cost is lowered, meanwhile, the pore size and pore size distribution of the catalyst are improved, dispersion of active substances is facilitated, the surface acidity of the catalyst can be improved, and the denitration performance can be improved; by adding a catalyst recovering material for effectively recovering production waste, solid waste treatment of the production waste is omitted, and meanwhile the cost is lowered. The denitration catalyst can be widely applied to nitric oxide removal treatment under complex smoke working conditions of thermal power boilers, glass kilns, cement kilns, chemical engineering, steelworks and the like.
Description
Technical field
The present invention relates to catalyst field, particularly a kind of preparation method of wear-resisting anti-poisoning honeycomb fashion SCR denitration.
Background technology
The nitrogen oxide of the burning generation of fossil fuel is almost NO and NO entirely
2and estimate in 30 ~ 50 years in the future, the energy general layout of China's energy-consuming based on coal can not change, this primary energy production and consumption structure based on coal brings serious problem of environmental pollution, within 2010, China's NOx emission has reached 2,273 ten thousand tons, by this development trend, NOx discharge will reach 3,540 ten thousand tons in the year two thousand thirty, and the discharge of control NOx has become pollution control major tasks.Along with the development of power industry and increasing of automobile quantity, NOx discharge is increasing, NOx can not only form acid rain, and photochemical fog can be generated with hydrocarbon, also participate in the destruction of ozone layer, also be one of major reason producing the fine particles pollutions such as PM2.5 and gray haze, huge threat is formed to health and ecological environment.
China " 12 " increases the control dynamics of NOx emission period, simple low-NO_x combustion technology cannot meet the discharge standard of NOx, flue gas SCR technology (SCR) is the method for the most effective NO_x removal, high performance catalyst is the key in SCR denitration, and existing most of denitrating catalyst in use exists easy to wear, blocking, poisoning, the problems such as efflorescence cause the lost of life, and specific area, the low catalytic efficiency that causes of porosity is low, also there is catalyst amount large, the defects such as production cost is higher, therefore, develop a kind of anti-wear performance good, anti-poisoning capability is strong, denitration efficiency is high and cost is low denitrating catalyst is problem demanding prompt solution in SCR denitration.
Summary of the invention
The object of the invention is to provide a kind of preparation method of wear-resisting anti-poisoning SCR denitration, can improve wear-resisting, the anti-poisoning performance of denitrating catalyst, improve its denitration efficiency and service life.
The object of the invention to solve the technical problems is achieved through the following technical solutions.A preparation method for wear-resisting anti-poisoning SCR denitration, comprise mixing, once old, filter that pre-extruded, secondary are old, extrusion molding, one-level drying, secondary drying, roasting, cutting and end face cure step.
1) mixing process described in comprises following six stages:
(1) first stage: mixing roll under stopped status, by the titanium tungsten silica flour of the titanium tungsten powder of 300 ~ 400 weight portions, 70 ~ 150 weight portions, the catalyst recovery material of 30 ~ 80 weight portions, the ammonium paramolybdate of 5 ~ 30 weight portions; The stearic acid of 0.8 ~ 2.0 weight portion is added under rotor forward stirring at low speed, the lactic acid of 5 ~ 10 weight portions, 280 ~ 350 parts by weight of deionized water and 25 ~ 40 weight portion concentration are 18% ~ 25%(mass percent) ammoniacal liquor in mixing roll, forward at a high speed lower strong stirring is even;
(2) second stage: the titanium tungsten powder of 70 ~ 150 weight portions, the montmorillonitic clay of 40 ~ 60 weight portions, under stopped status, add in mixing roll by mixing roll.The deionized water and 3 ~ 15 weight portion concentration that add 10 ~ 30 weight portions under in forward stirring at low speed are 18% ~ 25%(mass percent) ammoniacal liquor in mixing roll, under forward high-speed stirred, material is warming up to 90 DEG C ~ 98 DEG C, then open intake valve and air bleeding valve carries out dehumidifier, during dehumidifier, open intake valve and drain tap;
(3) phase III: under mixing roll forward lower-speed state, add in batch mixer by the deionized water of the kapok of the ammonium metavanadate solution of 40 ~ 60 weight portions, 2.5 ~ 4.0 weight portions, the glass fibre of 25 ~ 40 weight portions and 10 ~ 25 weight portions, then forward high-speed stirred is even;
(4) fourth stage: under the reverse low speed of mixing roll (350rpm) state, CMC(carboxymethyl cellulose by 0.8 ~ 2.0 weight portion), the PEO(PEO of 1.5 ~ 4.5 weight portions) and the deionized water of 8 ~ 15 weight portions add in mixing roll, oppositely (750rpm) stirs at a high speed;
(5) five-stages: under the reverse lower-speed state of mixing roll, add in mixing roll by the PEO of the carboxymethyl cellulose of 0.8 ~ 2.0 weight portion and 1.5 ~ 4.5 weight portions, and then oppositely high-speed stirred is even;
(6) the 6th stages: according to the Testing index of mixing material, the ammoniacal liquor of the deionized water and 1 ~ 10 weight portion that add 1 ~ 10 weight portion in mixing roll carries out modified, unloads the material mixed after making the moisture of material, pH value, shrinkage factor and plasticity reach standard-required bottom mixing roll.
After the above-mentioned mixing first stage terminates, the moisture of mixed material is 40% ~ 42%, and pH value is 9.0 ~ 10.0; After mixing second stage terminates, the moisture of mixed material is 24% ~ 26%, and pH value is 8.0 ~ 9.0; After the mixing phase III terminates, the moisture of mixed material is 27% ~ 29%, and pH value is 8.3 ~ 9.2; After mixing five-stage terminates, mixed material moisture is 27 ~ 30%, and pH value is 7.8 ~ 8.6; After mixing 6th stage terminates, mixed material moisture 28 ~ 30%, pH value 8.0 ~ 8.6, with extrude power replace plasticity of slurry value for 1600 ~ 2200N.
Described mixing first to the 6th stage carried out in same mixing roll, and mixing roll inside is provided with high-energy rotator and star rake, and the first to phase III is forward running, the 4th to the 6th stage antiport.
Described titanium tungsten powder crystal formation is Detitanium-ore-type, and its main component is TiO
2: 93% ~ 96%, WO
3: 4.5% ~ 5.5%, specific area is 80 ~ 100m
2/ g, average grain diameter 1.0 ~ 3.5um; Titanium tungsten silica flour crystal formation is Detitanium-ore-type, and its main component is TiO
2: 85% ~ 90%, WO
3: 4.5% ~ 5.5%, SiO
2: 4.0% ~ 6.0%, specific area is 95 ~ 115m
2/ g, average grain diameter 1.0 ~ 3.5um; Montmorillonitic clay main component is SiO
2: 58% ~ 65%, Al
2o
3%:18% ~ 24%, Fe
2o
3: 2% ~ 6%, MgO:2% ~ 6%; The average grain diameter of catalyst recovery material is at 5 ~ 20um.
Described ammonium metavanadate solution is the ammonium metavanadate of 50 ~ 200 weight portions, the deionized water of the MEA of 60 ~ 220 weight portions and 500 ~ 700 weight portions temperature be 55 ~ 95 DEG C, preparing tank motor speed prepares under being 35r/min, ammonium metavanadate solution density is 1.0 ~ 1.5g/ml, and the concentration l ferrous ammonium sulfate solution of ammonium metavanadate carries out titration.
2), in the once old step described in, after material is packed with plastic bag sealing, be positioned over that temperature is 10 ~ 30 DEG C, humidity is greater than in the ageing silo of 60%, once old 10 ~ 48h.
3), in the filtration preliminary extrusion step described in, after being filtered on filtration pre-extruded machine by the material after once old, pre-extruded squarely is block, and its extrusion temperature is not higher than 45 DEG C, and filtration stainless (steel) wire mesh size is 1 × 3mm,
4), in the old step of the secondary described in, filter after pre-extruded and lump material be sealed in plastic box, temperature be 10 ~ 30 DEG C, humidity is greater than in the ageing silo of 60%, the old 10 ~ 36h of secondary.
5) in the extrusion molding step described in, extruded velocity is 1 ~ 1.5m/min, and pressure is 2.5 ~ 5.5MPa, and temperature is less than 30 DEG C, and vacuum is less than-0.096MPa, and extrusioning catalyst cross section is wide is 155.5 ~ 157.5mm, and length is 400 ~ 1300mm.
6) in the one-level drying steps described in, preformed catalyst is wrapped in the carton of band sponge liner, to be placed on dry dolly and to push in hothouse, dry indoor temperature from 25 ± 5 DEG C rise to 60 ± 5 DEG C gradually, humidity drops to 20 ± 5% gradually from 90 ± 5%, arid cycle is 7 ~ 12 days.
7) in the secondary drying step described in, being taken out in carton by dried for one-level catalyst overlays secondary drying car, in feeding tunnel cave, temperature be 60 ± 5 DEG C, humidity carries out F.D drying 20 ± 5% times, drying time is 12 ~ 24h, and dry rear catalyst moisture is 0.5% ~ 3.0%.
8) in the calcination steps described in, the catalyst after secondary drying is arranged side by side on mesh-belt kiln, passes through intensification section I, constant temperature zone I, intensification section II, constant temperature zone II, cooling section five sections successively; Each zone temperatures is respectively: intensification section I: from inlet temperature rise to 170 ~ 200 DEG C, heating-up time 5h; Constant temperature zone I: constant temperature 4h at 170 ~ 200 DEG C; Intensification section II: be warmed up to 600 ~ 625 DEG C from 170 ~ 200 DEG C, heating-up time 9h; Constant temperature zone II: constant temperature 5.5h at 600 ~ 625 DEG C; Cooling section: be cooled to 50 ~ 80 DEG C from 600 ~ 625 DEG C, cool time 9h; Exhaust static pressure is-80Pa ~-30Pa.
9) in the cutting described in and end face cure step, calcined catalyst both ends of the surface cut, the dip time of cutting rear catalyst one end in hardening bath is 20 ~ 50s, and dipping is highly 10 ~ 30mm; Hardening bath is phosphate dihydrogen aluminum solution or aluminum sulfate solution, and phosphate dihydrogen aluminum solution is 1.4 ~ 1.6g/ml 25 DEG C of lower densities, and aluminum sulfate solution is 1.0 ~ 1.4g/ml 25 DEG C of lower densities.
Compared to existing technology, the present invention has following beneficial effect:
The invention provides a kind of wear-resisting anti-poisoning honeycomb fashion SCR denitration, overcome existing most of denitrating catalyst and in use there is the problems such as easy to wear, blocking, poisoning, efflorescence, cause shortening in its service life, specific surface area and porosity reduction, catalytic efficiency is caused to decline, also there is catalyst amount large, the defects such as production cost is higher.This catalyst has that wearability is strong, compression strength is high, anti-poisoning capability is strong, be easy to the advantages such as extrusion molding, denitration activity is good, the life-span is long; Replacing partial-titanium tungsten powder by adding montmorillonitic clay, reducing cost of material, improving aperture and the pore-size distribution of catalyst simultaneously, be beneficial to the dispersion of active material, catalyst surface acidity can also be increased, improving denitration performance; Also add catalyst recovery material and carry out waste material in effective remanufacture, the fixed-end forces avoiding production waste provides cost savings simultaneously; In addition, the honeycomb fashion SCR denitration prepared by above-mentioned steps, according to different operating condition designs, can be widely used in the denitrifying oxide process under the complicated flue gas operating modes such as apparatus of thermo-electric power boiler, glass furnace, cement kiln, chemical industry and steel plant.
Detailed description of the invention
Below in conjunction with embodiment the present invention done and illustrate further, but embodiments of the present invention are not limited to this.
embodiment 1
Detailed description of the invention prepared by wear-resisting anti-poisoning honeycomb fashion SCR denitration of the present invention is as follows:
One, preparation method
1) preparation of catalyst recovery material: by the fragmentation at the beginning of crushing material system of the catalyst waste material after cutting, dry method is levigate under 900r/min again, detects its average grain diameter is 7.6um with laser fineness gage.
2) ammonium metavanadate solution preparation: add 500L deionized water in ammonium metavanadate solution preparing tank, start stirring motor, be steam heated to 30 DEG C, then add 73kg MEA, under 30r/min stirs, be heated to 75 DEG C, add 61kg ammonium metavanadate powder, be heated with stirring to 95 DEG C and be incubated 1h, adding deionized water again to volume is 730L, after being cooled to 60 DEG C, detects ammonium metavanadate solution concentration is 0.091kg/L by titration.
3) mixing: be divided into six stages, specific embodiments is as follows:
(1) first stage: the titanium tungsten silica flour of the titanium tungsten powder of 320kg, 80kg, the catalyst recovery material of 50kg, the ammonium paramolybdate of 15kg, under stopped status, add in mixing roll by mixing roll.Add under forward low speed (350rpm) rotates the stearic acid of 1.5kg, the lactic acid of 7.5kg, 320L deionized water, 32L ammoniacal liquor in mixing roll, under forward high speed (750rpm), strong stirring is even, detect mixing rear material moisture be 41.2%, pH is 9.5;
(2) second stage: mixing roll is under stopped status, the titanium tungsten powder of 80kg, the montmorillonitic clay of 40kg are added in mixing roll, the ammoniacal liquor of the deionized water and 7L that add 15L under in forward stirring at low speed is in mixing roll, under forward high-speed stirred, material is warming up to 92 DEG C, then intake valve is opened and air bleeding valve carries out dehumidifier, detect material moisture be 24.6%, pH is 8.6 after dehumidifier;
(3) phase III: under mixing roll forward lower-speed state, the kapok of the ammonium metavanadate solution of 55L, 3.5kg slurry, the glass fibre of 32kg and the deionized water of 15L are added in batch mixer, then forward high-speed stirred is even, and to record material moisture after stirring be 27.6%, pH is 8.9;
(4) fourth stage: under the reverse low speed of mixing roll (350rpm) state, the deionized water of PEO and 10L of CMC, 3.0kg of 1.4kg is added in mixing roll, oppositely (750rpm) stirs at a high speed;
(5) five-stages: under the reverse lower-speed state of mixing roll, then the PEO of CMC and 2.0kg of 0.8kg is added in mixing roll, then oppositely high-speed stirred is even, and the moisture recording material after stirring is 27.2%, pH is 7.9;
(6) the 6th stages: according to the Testing index of mixing material, the ammoniacal liquor of the deionized water and 5L that add 10L in mixing roll carries out modified, unloads the material mixed after making the moisture of material, pH value, shrinkage factor and plasticity reach standard-required bottom mixing roll.Material Testing index result after mixing end is as shown in table 1
Table 1 mixing material Testing index result
| Testing index | Moisture (180 DEG C, %) | pH | Shrinkage factor (6mm rod, %) | Plasticity (in force value, N) |
| Testing result | 28.4 | 8.4 | 2.9 | 1850 |
4) once old: the material after mixing to be loaded good seal in polybag, puts into the ageing silo 18h of temperature 20 DEG C, humidity 75%, to reduce the residual stress of pug and to make internal moisture more even.
5) pre-extruded is filtered: the pug after old is filtered out bulky grain on the filter that stainless steel mesh is housed, then on pre-extruded machine, is extruded into lump material.
6) secondary is old: be loaded in sealed plastic box by the cake mass of pre-extruded, at 20 DEG C, the old 15h of ageing silo's secondary of humidity 75%.
7) shapingly to extrude: the pug extrusion molding in vacuum-extruder after extruding will be filtered, extruding hole count is 18 × 18, extruded velocity is 1.1m/min, pressure is 3.5MPa, temperature is 16.8 DEG C, vacuum is-0.096MPa, and extrusioning catalyst cross section is wide is 155.6mm, cuts into automatic gas cutting machine the moist catalysis honeycomb type semi-finished product that length is 820mm.
8) one-level is dry: pack extruding the carton of aftershaping catalyst manipulator folder to packaging table top band sponge, be placed on drying cart, push drying room, slowly dry under uniform temperature and humidity, in dry run, every day detects weight-loss ratio and shrinkage factor, stops one-level dry when loss of weight reaches 20 ± 2%.The parameter such as baking temperature, humidity is as shown in table 2.
Table 2 one-level drying parameter
| Time/h | 24 | 48 | 72 | 96 | 120 | 144 | 168 | 192 | 216 |
| Temperature/DEG C | 25±5 | 30±5 | 30±5 | 40±5 | 45±5 | 50±5 | 55±5 | 60±5 | 60±5 |
| Humidity/% | 90±5 | 85±5 | 80±5 | 75±5 | 70±5 | 60±5 | 45±5 | 30±5 | 20±5 |
9) secondary drying: dry for one-level rear catalyst is taken out in carton, is placed on secondary drying car and sends in tunnel cave, temperature be 60 ± 5 DEG C, humidity is carry out forced air drying 15h 20 ± 5% times, dry rear catalyst moisture is 2.3%.
10) roasting: the catalyst after secondary drying is placed on mesh-belt kiln, laterally longitudinally maintain a certain distance, in order to avoid mutually collide, catalyst passes through intensification section I successively: from inlet's temperature rise to 185 DEG C, heating-up time 5h; Constant temperature zone I: constant temperature 4h at 185 DEG C; Intensification section II: be warmed up to 610 DEG C from 185 DEG C, heating-up time 9h; Constant temperature zone II: constant temperature 5.5h at 610 DEG C; Cooling section: be cooled to 60 DEG C from 610 DEG C, cool time 9h; Discharge duct static pressure is-80Pa ~-30Pa.
11) cut: the catalyst after roasting directly delivers to cutting machine by automation equipment, 800mm is automatically cut into by design, cutting residue garbage collection, in ash can, cuts dust and blows grey dust cloth dust collector and collect, and waste material and recovery dust are all recycled.
12) end face sclerosis: cutting is blown the catalyst one end after ash and immerse 25s in phosphate dihydrogen aluminum solution, dipping is highly 20cm, piles up in disk stripping air-dry after taking-up.
Two, Performance Detection
The main component of catalyst and Performance Detection are detected.Tear strength is 10 × 10 holes at sample size, and height of specimen is 10cm, air velocity: 15 ± 2m/s, quartz sand concentration: 50 ± 5%, and quartz sand average grain diameter is 40 ~ 50 orders, and test sample is tested 2h with comparative sample and measured under the condition of connecting; Denitration performance is flue-gas temperature 370 DEG C, and air speed is 2.3m/s, and ammonia nitrogen mol ratio is 0.85, NO is 220ppm, SO
2for 950ppm, O
2be 3.5%, H
2o is 9.6%, and all the other are N
2, result is as shown in table 3.
Table 3 catalyst component and properties testing result
embodiment 2
Detailed description of the invention prepared by wear-resisting anti-poisoning honeycomb fashion SCR denitration of the present invention is as follows:
One, preparation method
1) preparation of catalyst recovery material: by the fragmentation at the beginning of crushing material system of the catalyst waste material after cutting, dry method is levigate under 900r/min again, detects its average grain diameter is 8.1um with laser fineness gage.
2) ammonium metavanadate solution preparation: add 500L deionized water in ammonium metavanadate solution preparing tank, start mixer, be steam heated to 30 DEG C, then add 180kg MEA, under 30r/min stirs, be heated to 75 DEG C, add 157kg ammonium metavanadate powder, be heated with stirring to 95 DEG C and be incubated 1h, in tank, add deionized water to volume is again 730L, and after solution is cooled to 60 DEG C, detecting ammonium metavanadate solution concentration by titration is 0.2154kg/L.
3) mixing: be divided into six stages to complete, specific embodiments is as follows:
(1) first stage: the titanium tungsten silica flour of the titanium tungsten powder of 350kg, 95kg, the catalyst recovery material of 30kg, the ammonium paramolybdate of 20kg, under stopped status, add in mixing roll by mixing roll.Add under forward low speed (350rpm) rotates the stearic acid of 1.8kg, the lactic acid of 10kg, 290L deionized water, 35L ammoniacal liquor in mixing roll, under forward high speed (750rpm), strong stirring is even, detect mixing rear material moisture be 40.7%, pH is 9.8 respectively with Moisture Meter and pH meter;
(2) second stage: mixing roll is under stopped status, the titanium tungsten powder of 95kg, the montmorillonitic clay of 50kg are added in mixing roll, the ammoniacal liquor of the deionized water and 10L that add 20L under in forward stirring at low speed is in mixing roll, under forward high-speed stirred, material is warming up to 94 DEG C, then intake valve is opened and air bleeding valve carries out dehumidifier, detect material moisture be 25.2%, pH is 8.8 after dehumidifier;
(3) phase III: under mixing roll forward lower-speed state, the kapok of the ammonium metavanadate solution of 55L, 3.8kg slurry, the glass fibre of 35kg and the deionized water of 18L are added in batch mixer, then forward high-speed stirred is even, and to record material moisture after stirring be 28.2%, pH is 9.0;
(4) fourth stage: under the reverse low speed of mixing roll (350rpm) state, adds in mixing roll by PEO and the 15L deionized water of CMC, 2.6kg of 1.0kg, and oppositely (750rpm) stirs at a high speed;
(5) five-stages: under the reverse lower-speed state of mixing roll, then the PEO of CMC and 2.5kg of 1.2kg is added in mixing roll, then oppositely high-speed stirred is even, and the moisture recording material after stirring is 27.9%, pH is 8.4;
In (6) the 6th stages: according to the Testing index of mixing material, in mixing roll, add 10L deionized water carry out modified, after making the moisture of material, pH value, shrinkage factor and plasticity reach standard-required, bottom mixing roll, unload the material mixed.Material Testing index result after mixing is as shown in table 4
Table 4 mixing material Testing index result
| Testing index | Moisture (180 DEG C, %) | pH | Shrinkage factor (6mm rod, %) | Plasticity (in force value, N) |
| Testing result | 29.5 | 8.3 | 3.0 | 1920 |
4) once old: the material after mixing to be loaded good seal in polybag, puts into the ageing silo once old 20h of temperature 25 DEG C, humidity 80%, to reduce pug residual stress and even moisture.
5) pre-extruded is filtered: the pug after old is filtered out bulky grain on the filter that stainless steel mesh is housed, then on pre-extruded machine, is extruded into lump material.
6) secondary is old: be loaded in sealed plastic box by the cake mass of pre-extruded, at 25 DEG C, the old 10h of ageing silo's secondary of humidity 80%.
7) shapingly to extrude: the pug extrusion molding in vacuum-extruder after extruding will be filtered, extruding hole count is 20 × 20, extruded velocity is 1.2m/min, pressure is 3.8MPa, temperature is 17.2 DEG C, vacuum is-0.096MPa, and extrusioning catalyst cross section is wide is 155.4mm, cuts into automatic gas cutting machine the moist catalysis honeycomb type semi-finished product that length is 1020mm.
8) one-level is dry: pack extruding the carton of aftershaping catalyst manipulator folder to packaging table top band sponge, be placed on drying cart, push drying room, slowly dry under uniform temperature and humidity, in dry run, every day detects weight-loss ratio and shrinkage factor, stops one-level dry when loss of weight reaches 20 ± 2%.The parameter such as baking temperature, humidity is as shown in table 5.
Table 5 one-level drying parameter
| Time/h | 24 | 48 | 72 | 96 | 120 | 144 | 168 | 192 | 216 |
| Temperature/DEG C | 25±5 | 30±5 | 35±5 | 40±5 | 45±5 | 50±5 | 55±5 | 60±5 | 60±5 |
| Humidity/% | 90±5 | 85±5 | 80±5 | 70±5 | 65±5 | 50±5 | 45±5 | 30±5 | 20±5 |
9) secondary drying: dry for one-level rear catalyst is taken out in carton, is placed on secondary drying car and sends in tunnel cave, temperature be 60 ± 5 DEG C, humidity is carry out forced air drying 16h 20 ± 5% times, dry rear catalyst moisture is 2.1%.
10) roasting: the catalyst after secondary drying is placed on mesh-belt kiln, laterally longitudinally maintain a certain distance, in order to avoid mutually collide, catalyst passes through intensification section I successively: from inlet's temperature rise to 195 DEG C, heating-up time 5.5h; Constant temperature zone I: constant temperature 4h at 195 DEG C; Intensification section II: be warmed up to 618 DEG C from 195 DEG C, heating-up time 9h; Constant temperature zone II: constant temperature 5.5h at 618 DEG C; Cooling section: be cooled to 70 DEG C from 618 DEG C, cool time 9h; Discharge duct static pressure is-80Pa ~-30Pa.
11) cut: the catalyst after roasting directly delivers to cutting machine by automation equipment, 1000mm is automatically cut into by design length, cutting residue garbage collection, in ash can, cuts dust and blows grey dust cloth dust collector and collect, and waste material and recovery dust are all recycled.
12) end face sclerosis: cutting is blown the catalyst one end after ash and immerse 25s in aluminum sulfate solution, dipping is highly 20cm, piles up in disk stripping air-dry after taking-up.
Two, Performance Detection
The main component of catalyst and Performance Detection are detected.Tear strength is 10 × 10 holes at sample size, and height of specimen is 10cm, air velocity: 15 ± 2m/s, quartz sand concentration: 50 ± 5%, and quartz sand average grain diameter is 40 ~ 50 orders, and test sample is tested 2h with comparative sample and measured under the condition of connecting; Denitration performance is flue-gas temperature 370 DEG C, and air speed is 2.3m/s, and ammonia nitrogen mol ratio is 0.85, NO is 220ppm, SO
2for 950ppm, O
2be 3.5%, H
2o is 9.6%, and all the other are N
2, result is as shown in table 6.
Table 6 catalyst component and properties testing result
Finally should be noted that; above preferred embodiment is only in order to illustrate technical scheme of the present invention but not limiting the scope of the invention; although content of the present invention is made complete with regard to detailed description of the invention disclosed in it and described clearly, it is not limited only to this.Those of ordinary skill in the art should be appreciated that and do not departing within the scope of technical solution of the present invention, can be modified or equivalent replacement, and do not depart from essence and the scope of technical solution of the present invention by the guidance of these statements to technical scheme of the present invention.
Claims (8)
1. a wear-resisting anti-poisoning honeycomb fashion SCR denitration preparation method, is characterized in that, comprise mixing, once old, filter that pre-extruded, secondary are old, extrusion molding, one-level drying, secondary drying, roasting, cutting and end face cure step.
2. wear-resisting anti-poisoning honeycomb fashion SCR denitration preparation method according to claim 1, is characterized in that, described mixing point following six stages:
(1) first stage: the titanium tungsten silica flour of the titanium tungsten powder of 300 ~ 400 weight portions, 70 ~ 150 weight portions, the catalyst recovery material of 30 ~ 80 weight portions, the ammonium paramolybdate of 5 ~ 30 weight portions, under stopped status, add in mixing roll by mixing roll; Under forward stirring at low speed, add the stearic acid of 0.8 ~ 2.0 weight portion, the lactic acid of 5 ~ 10 weight portions, the deionized water of 280 ~ 350 weight portions, 25 ~ 40 weight portion concentration be the ammoniacal liquor of 18wt% ~ 25wt% in mixing roll, forward at a high speed lower strong stirring is even;
(2) second stage: mixing roll is under stopped status, the titanium tungsten powder of 70 ~ 150 weight portions, the montmorillonitic clay of 40 ~ 60 weight portions are added in mixing roll, the deionized water and 3 ~ 15 weight portion concentration that add 10 ~ 30 weight portions under forward stirring at low speed are that the ammoniacal liquor of 18wt% ~ 25wt% is in mixing roll, under forward high-speed stirred, material is warming up to 90 DEG C ~ 98 DEG C, then opens intake valve and air bleeding valve carries out dehumidifier;
(3) phase III: under mixing roll forward lower-speed state, add in batch mixer by the glass fibre of the kapok of the ammonium metavanadate solution of 40 ~ 60 weight portions, 2.5 ~ 4.0 weight portions slurry, 25 ~ 40 weight portions and 10 ~ 25 parts by weight of deionized water, then forward high-speed stirred is even;
(4) fourth stage: under the reverse lower-speed state of mixing roll, add in mixing roll by the PEO of the carboxymethyl cellulose of 0.8 ~ 2.0 weight portion, 1.5 ~ 4.5 weight portions and the deionized water of 8 ~ 15 weight portions, reverse high-speed stirred is even;
(5) five-stages: under the reverse lower-speed state of mixing roll, then the PEO of the carboxymethyl cellulose of 0.8 ~ 2.0 weight portion and 1.5 ~ 4.5 weight portions is added in mixing roll, then oppositely high-speed stirred is even;
In (6) the 6th stages: according to the Testing index of mixing material, the ammoniacal liquor of the deionized water and 1 ~ 10 weight portion that add 1 ~ 10 weight portion in mixing roll carries out modified, unloads the material mixed after modified bottom mixing roll;
Described once old be by after the material plastic bag sealing packaging that mixes, be positioned over that temperature is 10 ~ 30 DEG C, humidity is greater than in the ageing silo of 60%, once old 10 ~ 48h;
Described filtration pre-extruded is that after being filtered on filtration pre-extruded machine by the material after once old, pre-extruded squarely is block, and its extrusion temperature is not higher than 45 DEG C, and filtration stainless steel mesh mesh size is 1 × 3mm;
Described secondary is old is filter after pre-extruded lump material to be sealed in plastic box, temperature be 10 ~ 30 DEG C, humidity is greater than in the ageing silo of 60%, the old 10 ~ 36h of secondary;
Described extrusion molding be secondary is old after lump material drop into extrusion molding in vacuum-extruder, extruded velocity is 1 ~ 1.5m/min, pressure is 2.5 ~ 5.5MPa, temperature is 10 ~ 30 DEG C, vacuum is less than-0.096MPa, extrusioning catalyst cross section is wide is 155.5 ~ 157.5mm, and length is 400 ~ 1300mm;
Described one-level drying is wrapped into by preformed catalyst in the carton of band sponge liner, and being placed on dry dolly and pushing in hothouse, dry indoor temperature through periodically at the uniform velocity heating up and thermostatic process, finally rises to 60 ± 5 DEG C from 25 ± 5 DEG C; Humidity through periodicity at the uniform velocity wet down and constant humidity process, is finally down to 20 ± 5% from 90 ± 5%; Whole arid cycle is 7 ~ 12 days;
Described secondary drying is taken out by dried for one-level catalyst to overlay secondary drying car in carton, in feeding tunnel cave, temperature be 60 ± 5 DEG C, humidity carries out F.D drying 20 ± 5% times, drying time is 12 ~ 24h, and dry rear catalyst moisture is 0.5% ~ 3.0%;
Described roasting be by secondary drying after catalyst pass through intensification section I, constant temperature zone I, intensification section II, constant temperature zone II, cooling section five roasting sections successively; Each zone temperatures is respectively: intensification section I: from inlet temperature rise to 170 ~ 200 DEG C, heating-up time 5h; Constant temperature zone I: constant temperature 4h at 170 ~ 200 DEG C; Intensification section II: be warmed up to 600 ~ 625 DEG C from 170 ~ 200 DEG C, heating-up time 9h; Constant temperature zone II: constant temperature 5.5h at 600 ~ 625 DEG C; Cooling section: be cooled to 50 ~ 80 DEG C from 600 ~ 625 DEG C, cool time 9h; Exhaust static pressure is-80Pa ~-30Pa;
Described cutting and section sclerosis are cut at calcined catalyst both ends of the surface, and the dip time of cutting rear catalyst one end in hardening bath is 20 ~ 50s, and dipping is highly 10 ~ 30mm; Hardening bath is phosphate dihydrogen aluminum solution or aluminum sulfate solution, and the density of its phosphate dihydrogen aluminum solution at 25 DEG C is 1.4 ~ 1.6g/ml, and the density of aluminum sulfate solution at 25 DEG C is 1.0 ~ 1.4g/ml.
3. wear-resisting anti-poisoning honeycomb fashion SCR denitration preparation method according to claim 2, it is characterized in that, after the mixing first stage terminates, the moisture of mixed material is 40% ~ 42%, and pH value is 9.0 ~ 10.0; After mixing second stage terminates, the moisture after mixed material dehumidifier is 24% ~ 26%, and pH value is 8.0 ~ 9.0; After the mixing phase III terminates, the moisture of mixed material is 27% ~ 29%, and pH value is 8.3 ~ 9.2; After mixing five-stage terminates, mixed material moisture is 27 ~ 30%, and pH value is 7.8 ~ 8.6; After mixing 6th stage modified end, mixed material moisture 28 ~ 30%, pH value 8.0 ~ 8.6, with extrude power replace plasticity of slurry value for 1600 ~ 2200N.
4. wear-resisting anti-poisoning honeycomb fashion SCR denitration preparation method according to claim 2, it is characterized in that, mixing first to the 6th stage carried out in same mixing roll, mixing roll inside is provided with high-energy rotator and star rake, the first to phase III is forward running, the 4th to the 6th stage antiport.
5. wear-resisting anti-poisoning honeycomb fashion SCR denitration preparation method according to claim 2, it is characterized in that, described titanium tungsten powder crystal formation is Detitanium-ore-type, and its main component is TiO
2: 93% ~ 96%, WO
3: 4.5% ~ 5.5%, specific area is 80 ~ 100m
2/ g, average grain diameter 1.0 ~ 3.5um; Described titanium tungsten silica flour crystal formation is Detitanium-ore-type, and its main component is TiO
2: 85% ~ 90%, WO
3: 4.5% ~ 5.5%, SiO
2: 4.0% ~ 6.0%, specific area is 95 ~ 115m
2/ g, average grain diameter 1.0 ~ 3.5um; Described montmorillonitic clay main component is SiO
2: 58% ~ 65%, Al
2o
3%:18% ~ 24%, Fe
2o
3: 2% ~ 6%, MgO:2% ~ 6%; The average grain diameter of described catalyst recovery material is at 5 ~ 20um.
6. wear-resisting anti-poisoning honeycomb fashion SCR denitration preparation method according to claim 2, it is characterized in that, ammonium metavanadate solution used is the ammonium metavanadate of 50 ~ 200 weight portions, the deionized water of the MEA of 60 ~ 220 weight portions and 500 ~ 700 weight portions temperature be 55 ~ 95 DEG C, preparing tank motor speed prepares under being 35r/min, ammonium metavanadate solution density is 1.0 ~ 1.5g/ml, solution concentration l ferrous ammonium sulfate solution titration.
7. wear-resisting anti-poisoning honeycomb fashion SCR denitration preparation method according to claim 2, it is characterized in that, it is 350rpm that described forward low speed refers to that mixing roll rotates forward rotating speed, it is 750rpm that forward refers to that at a high speed mixing roll rotates forward rotating speed, described reverse low speed refers to that mixing roll reverse is 350rpm, oppositely refers to that mixing roll reverse is 750rpm at a high speed.
8. a wear-resisting anti-poisoning honeycomb fashion SCR denitration, is characterized in that its catalyst prepared by the preparation method of the denitrating catalyst described in any one of claim 1 ~ 7.
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