CN104841489A - Rare-earth-based composite multi-component denitration and dioxin-removing catalyst and preparation method thereof - Google Patents
Rare-earth-based composite multi-component denitration and dioxin-removing catalyst and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a rare-earth-based composite multi-component denitration and dioxin-removing catalyst and a preparation method thereof. The rare-earth-based composite multi-component denitration and dioxin-removing catalyst takes titanium dioxide and silicon powder as carriers, and takes tungsten compounds, vanadium compounds, cerium compounds and lanthanum compounds as active components; and under the accompanying of auxiliary materials, all the raw materials are mixed, granulated, kneaded, molded, dried and roasted to prepare the catalyst, wherein the auxiliary materials comprise monoethanolamine, ammonia water, lactic acid, stearic acid, glass fibers, citric acid, PP (Propene Polymer) fibers, cellulose ether, polyoxyethylene and water. The preparation method of the rare-earth-based composite multi-component denitration and dioxin-removing catalyst has a simple process and is safe to operate, and the catalyst has a plurality of functions of denitration, dioxin removal and mercury removal; by adopting a catalytic decomposition technology, the dioxin pollution problem is solved; compared with that of active carbon, the adsorption is relatively complete; and the activity of the catalyst is extremely improved and the temperature use range is expanded.
Description
Technical field
The present invention relates to a kind of catalyst, be specifically related to the denitration of a kind of rare earth based complex multi-component, Tuo bioxin Catalysts and its preparation method.
Background technology
Nitrogen oxide and mercury cause one of atmosphere pollution and heavy metal pollution main component, and it not only can be harmful, but also pollute the environment.
According to the requirement of " thermal power plant's discharged nitrous oxides standard " (secondary exposure draft), new unit or the old Transformation of Unit 100mg/Nm in key area be reached
3emission request must install SCR denitration additional, non-key area meets 200mg/Nm
3emission request.Denitration technology the most ripe in the world is at present SCR method denitration technology.SCR denitration technology refers under the effect of denitrating catalyst, makees reducing agent with ammonia, and the NOx in flue gas is decomposed, and generates N
2and H
2o.
Denitration reaction equation:
4NH
3+4NO+O
2→4N
2+6H
2O
4NH
3+2NO
2+O
2→3N
2+6H
2O
Current SCR denitration technology active component is vanadic anhydride, and carrier is titanium dioxide titanium dioxide.Denitrating catalyst 2-3 in service life, it is very easily water-soluble that vanadic anhydride belongs to noxious material, and like this in order to preventing pollution underground water and soil etc., discarded catalyst just can not at will landfill or air storage.Just cause the problem of catalyst treatment difficulty, bring huge environmental protection pressure to owner.Vanadic anhydride has higher oxygenation efficiency simultaneously, makes sulfur dioxide to sulphur trioxide conversion, and so just make sulfur trioxide and ammonia combine raw sulphur ammonium salt and can cause Corrosion blockage to equipment, cause overhaul of the equipments frequent, impact is produced.The carrier that such denitrating catalyst uses in addition does carrier with titanium dioxide titanium dioxide, easily cracking and wearing and tearing in production and application process, falls apart and collapses.
For flue gas Tuo bioxin technology, refer under the effect of Tuo bioxin catalyst, resolve into HCl, H2O, CO2 by bioxin is oxidized in flue gas, its technological core is also denitration, Tuo bioxin catalyst.And the domestic improvement for Yan gas Zhong bioxin at present, what mainly adopt is charcoal absorption and flue gas quench technique.Bioxin is just transferred in active carbon by charcoal absorption from flue gas, can not fundamentally administer.Flue gas quench technique refers to and flue-gas temperature is plummeted to less than 200 DEG C from 800 DEG C, avoids the generation of bioxin, but causes the waste of mass energy.
In addition, another reaction also can be brought to be that Partial Elements Hg in flue gas is oxidized to divalence Hg while SCR denitration reaction, thus contribute to Hg and washed in desulfuration absorbing tower, thus reduce Hg to the discharge in air, realize the object of Hg reduction of discharging.
Demercuration reaction equation:
Hg
0→Hg
2+
But for flue gas demercuration, gaseous elemental Hg
0removal be the difficult point of mercury in flue gas Environmental capacity all the time.
Existing demercuration technology technology as many in active carbon adsorption, chemical precipitation method etc. can realize the object of demercuration, but demercuration technical matters more complicated, and cost compare is high, even also can produce the accessory substance that other are harmful.
Summary of the invention
The object of the invention is for prior art Problems existing, the denitration of a kind of rare earth based complex multi-component, Tuo bioxin Catalysts and its preparation method are provided, technique is simple, operation security of operation, have denitration, Tuo bioxin and the rare earth based complex multi-component denitration of demercuration multi-efficiency, the preparation method of Tuo bioxin catalyst concurrently, solve bioxin pollution problem, improve the activity of catalyst greatly, widen the temperature scope of application.
A kind of rare earth based complex multi-component of the present invention denitration, Tuo bioxin catalyst, with titanium dioxide, silica flour for carrier, with the compound of the compound of the compound of the compound of tungsten, vanadium, cerium and lanthanum for active component, auxiliary material with under, make through mixing, granulation, kneading, shaping, dry, roasting;
Wherein, auxiliary material is MEA, ammoniacal liquor, lactic acid, stearic acid, glass fibre, citric acid, polypropylene fibre PP, cellulose ether, polyethylene glycol oxide and water.
Raw material is composed as follows: compound 8-12 part of compound 5-45 part of titanium dioxide 500-700 part, silica flour 5-50 part, tungsten, compound 5-15 part of vanadium, cerium, compound 8-12 part of lanthanum, MEA 5-15 part, ammoniacal liquor 39-66 liter, lactic acid 2-7 part, stearic acid 1-5 part, glass fibre 30-40 part, citric acid 5-25 part, polypropylene fibre PP3.0-3.5 part, cellulose ether 2-6 part, polyethylene glycol oxide 2-10 part and water 530-980 liter; Wherein, the unit of ammoniacal liquor and water to rise, the unit of other raw material in kilogram.
The compound of tungsten be ammonium metatungstate and or ammonium paratungstate.
The compound of vanadium is one or more in ammonium metavanadate, vanadium oxide or vanadium oxalate.
The compound of cerium is one or more in cerous nitrate, cerium oxalate, cerous sulfate or cerium oxide.
The compound of lanthanum is one or more in lanthanum nitrate, lanthanum oxalate, lanthanum sulfate or lanthana.
The preparation method of the denitration of rare earth based complex multi-component, Tuo bioxin catalyst, comprises the steps:
(1) active component preparation: the water of 30-80 part is joined mixed dissolution in MEA, when temperature arrives 80-100 DEG C, add the compound uniform stirring of the compound of vanadium, tungsten, the obtained compound of vanadium, the compound activity solution of tungsten after all dissolving;
The water that 40-60 rises is added citric acid stir, then add the compound of cerium, until completely dissolved, then add the compound of lanthanum, until completely dissolved obtained the compound of cerium, the compound activity solution of lanthanum;
(2) carrier impregnation liquid preparation: 300-500 premium on currency is added in dipping filling, then the compound of the compound of the vanadium prepared, the compound of tungsten and cerium, the compound activity solution of lanthanum are joined in impregnating autoclave respectively, be warmed up to 35-45 DEG C;
(3) support-activated: titanium dioxide is added impregnating autoclave, after stirring, the titanium dioxide flooded is carried out pneumatic conveying drying, obtained reactive silica titanium carrier;
(4) mixing process:
Once mixing: reactive silica titanium carrier and silica flour to be added in batch mixer and is dry mixed evenly, then by stearic acid, lactic acid, 100-250 premium on currency and 30-50 rise ammoniacal liquor and add successively in batch mixer and carry out Homogeneous phase mixing;
Secondary is mixing: by reactive silica titanium carrier and 10-20 premium on currency add in batch mixer and carry out Homogeneous phase mixing;
Three times are mixing: by reactive silica titanium carrier and 5-10 rise ammoniacal liquor and add in batch mixer and carry out Homogeneous phase mixing, temperature 85-95 DEG C in batch mixer;
Four times are mixing: by polypropylene fibre PP, glass fibre and 45-55 premium on currency add successively in batch mixer and carry out Homogeneous phase mixing;
Five times are mixing: when temperature in batch mixer being down to below 70 DEG C, by cellulose ether and polyethylene glycol oxide add in batch mixer and carry out Homogeneous phase mixing;
Six times are mixing: again by cellulose ether and polyethylene glycol oxide and 4-6 rise ammoniacal liquor and add batch mixer and carry out Homogeneous phase mixing;
(5) raw material after mixing carries out old, the raw material after old carry out filtration and fully mediate, shaping, dry;
(6) roasting is carried out after drying.
Six times mixing after, pH value is between 7.0-8.0, and moisture control is at 28.0-30.0%, if pH value is not in scope, adds ammoniacal liquor and regulate in mixing at the 6th time.
Mix raw material sealing is placed on temperature 20-30 DEG C, humidity carries out old in 50.0-70.0% environment, the time is at 12-24 hour.
Drying is divided into primary drying and redrying, and primary drying environment temperature is 20-60 DEG C, and dry environment humidity is 85-10%, 10 days drying times; Redrying environment temperature is 57-60 DEG C, drying time 24-48 hour.
The initial product that drying completes enters roasting, and roasting kiln is continuous mesh belt type kiln, and roasting heating curve is parabola, roasting by room temperature, maximum temperature is 530-550 DEG C, and then temperature can reduce gradually, product kiln discharge temperature is 60-80 DEG C, and roasting time controls at 25-30 hour.
After third time mixing end, raw material moisture control is at 26.0-28.50%.
The preparation method of the denitration of rare earth based complex multi-component, Tuo bioxin catalyst, preferred steps is as follows:
(1) active component preparation: the water that 40-60 rises is added dissolving tank, the monoethanolamine of 10-15 ㎏ is joined in dissolving tank, when temperature arrives 85-95 DEG C, the ammonium metatungstate of the ammonium metavanadate of 10-15 ㎏, 35-45 ㎏ is joined in dissolving tank, uniform stirring 30-50 minute, until all dissolve obtained ammonium metavanadate, ammonium metatungstate living solution;
Separately the water that 40-50 rises is added dissolving tank, again 15-25 ㎏ citric acid is joined in dissolving tank after stirring 4-6 minute, the cerous nitrate of 8-12 ㎏ to be added in dissolving tank until completely dissolved, again the lanthanum nitrate of 8-12 ㎏ is added in dissolving tank, until completely dissolved obtained cerous nitrate, lanthanum nitrate living solution;
(2) carrier impregnation liquid preparation: 300-500 premium on currency is added in batch mixing filling, then the ammonium metavanadate prepared, ammonium metatungstate and cerous nitrate, lanthanum nitrate living solution are joined in batch mixing filling, be warmed up to 35-45 DEG C;
(3) support-activated: the titanium dioxide of 500-700 ㎏ is added mixing tank at twice, after stirring, the titanium dioxide flooded is carried out pneumatic conveying drying, obtained reactive silica titanium carrier;
(4) mixing process:
Once mixing: the silica flour of 300-400 ㎏ reactive silica titanium carrier and 10-40 ㎏ to be added in batch mixer and is dry mixed 5-15 minute, then the lactic acid of the stearic acid of 1-3 ㎏, 3-7 ㎏, 200-300 premium on currency and 20-50 are risen ammoniacal liquor and add successively in batch mixer and carry out Homogeneous phase mixing 15-25 minute;
Secondary is mixing: the reactive silica titanium carrier of 80-150 ㎏ and 15-20 premium on currency are added in batch mixer and carry out Homogeneous phase mixing 15-25 minute;
Three times mixing: the reactive silica titanium carrier of 80-150kg and 7-10 are risen ammoniacal liquor and add in batch mixer and carry out Homogeneous phase mixing, until when temperature arrives 85-95 DEG C in batch mixer, discharges the gas that raw material produces;
Four times mixing: the glass fibre of polypropylene fibre PP, 30-50 ㎏ of 1.0-4 ㎏ and 40-60 premium on currency are added successively in batch mixer and carry out Homogeneous phase mixing 15-25 minute;
Five times mixing: when temperature in batch mixer being down to below 70 DEG C, the cellulose ether of 1-3kg and the polyethylene glycol oxide of 1-5kg added in batch mixer and carry out Homogeneous phase mixing 7-15 minute;
Six times mixing: the cellulose ether of 1-3kg and the polyethylene glycol oxide of 1-5kg and 4-6 are risen ammoniacal liquor again and add batch mixer and carry out Homogeneous phase mixing 7-15 minute;
(5) raw material fully mix after pH value between 7.0-8.0, moisture control is at 28.0-30.0%, if pH value is not in scope, adds ammoniacal liquor and regulate in so mixing at the 6th time;
(6) mix raw material sealing is placed on temperature 20-30 DEG C, humidity carries out once old in 50.0-70.0% environment, the time is at 12-24 hours;
(7) raw material after once old, carries out filtration through filter and pre-extruded machine to raw material and fully mediates;
(8) raw material is after filter and pre-extruded machined, and again carry out old, the old time is at 12-24 hour;
(9) secondary old after raw material, through Powerful extruder extrusion molding, after packaging, enter drying;
(10) drying is divided into primary drying and redrying, and primary drying environment temperature is 20-60 DEG C, and dry environment humidity is 85-10%, starts by high humidity low temperature to low humidity high temperature, 10 days drying times; Redrying environment temperature is 57-60 DEG C, drying time 24-48 hour;
(11) initial product that drying completes enters roasting, roasting kiln is continuous mesh belt type kiln, roasting heating curve is parabola, product is entered by room temperature, maximum temperature is 530-550 DEG C, temperature can reduce gradually backward, and product kiln discharge temperature is 60-80 DEG C, and roasting time controls at 25-30 hour.
The preparation method of the denitration of rare earth based complex multi-component, Tuo bioxin catalyst, more preferably step is as follows:
(1) preparation of active component:
The water of 50 liters is added active dissolution tank; Again the monoethanolamine of 13 ㎏ is joined in dissolving tank, when temperature arrives 90 DEG C, the ammonium metatungstate of the ammonium metavanadate of 12 ㎏, 40 ㎏ is joined in dissolving tank, uniform stirring 40 minutes, until all dissolve obtained ammonium metavanadate, ammonium metatungstate living solution;
The water of 50 liters is added active dissolution tank, again 20 ㎏ citric acids are joined in dissolving tank, stir after 5 minutes, the cerous nitrate of 10 ㎏ to be added in dissolving tank until completely dissolved, again the lanthanum nitrate of 10 ㎏ is added in dissolving tank, until completely dissolved obtained cerous nitrate, lanthanum nitrate living solution;
(2) preparation of carrier impregnation liquid: 400 premium on currency are added in batch mixing filling, then the ammonium metavanadate prepared, ammonium metatungstate living solution and cerous nitrate, lanthanum nitrate living solution are joined in mixing tank, be warmed up to 40 DEG C;
(3) support-activated: the titanium dioxide average mark of 609.5 ㎏ is added mixing tank twice, after stirring, the titanium dioxide flooded is dried, then split is sieved, obtained reactive silica titanium carrier split, and be divided into three parts;
(4) mixing process:
Once mixing: the silica flour of 369.5 ㎏ reactive silica titanium carriers and 35 ㎏ to be added in batch mixer and is dry mixed 10 minutes; Again the lactic acid of the stearic acid of 2.6 ㎏, 6.5 ㎏, 230 premium on currency and 45 liters of ammoniacal liquor are added in batch mixer successively and carry out Homogeneous phase mixing 20 minutes;
Secondary is mixing: the reactive silica titanium carrier of 105 ㎏ and 18 premium on currency are added in batch mixer and carry out Homogeneous phase mixing 20 minutes;
Three times are mixing: the reactive silica titanium carrier of 135 ㎏ and 8 liters of ammoniacal liquor are added in batch mixer and carry out Homogeneous phase mixing, until when temperature arrives 90 DEG C in batch mixer, discharge the gas that raw material produces,
Four times mixing: the polypropylene fibre PP of 3.25 ㎏, the glass fibre of 36 ㎏ and 50 premium on currency are added successively in batch mixer and carry out Homogeneous phase mixing 20 minutes;
Five times mixing: when temperature in batch mixer being down to below 70 DEG C, the cellulose ether of 2.44kg and the polyethylene glycol oxide of 2.14kg added in batch mixer and carry out Homogeneous phase mixing 10 minutes;
Six times mixing: again the cellulose ether of 2.44, the polyethylene glycol oxide of 2.14 and 5 liters of ammoniacal liquor are added batch mixer and carry out Homogeneous phase mixing 10 minutes, and raw material mixing is complete;
(5) raw material fully mix after moisture control at 28.0-30.0%, pH value is between 7.0-8.0, if pH value is not in scope, adds ammoniacal liquor and regulate in so mixing at the 6th time;
(6) mix raw material sealing is placed on temperature 20-30 DEG C, humidity carries out old in 50.0-70.0% environment, the time is at 12-24 hours;
(7) raw material after old, through filter and pre-extruded machine, carries out filtration to raw material and fully mediates;
(8) raw material is after filter and pre-extruded machined, again carries out 12-24 hour old;
(9) secondary old after raw material, through Powerful extruder extrusion molding, after packaging, enter drying;
(10) drying is divided into primary drying and redrying, and primary drying environment temperature is 20-60 DEG C, and dry environment humidity is 85-10%, starts by high humidity low temperature to low humidity high temperature, 10 days drying times; Redrying environment temperature is 57-60 DEG C, drying time 24-48 hour;
(11) initial product that drying completes enters roasting, and roasting kiln is continuous mesh belt type kiln, is provided with 12 temperature control points and 13 Temperature displaying points, altogether 25 Temperature displaying points; Roasting heating curve is parabola, by room temperature, enter product, and maximum temperature is 530-550 DEG C, and temperature can reduce gradually backward, and product kiln discharge temperature is 60-80 DEG C, and roasting time controlled at 28 hours.
Catalyst of the present invention is ceramic honeycomb catalyst.
Compared with prior art, the present invention has following beneficial effect:
Rare earth based complex multi-component of the present invention denitration, Tuo bioxin Catalysts and its preparation method, technique is simple, operation security of operation, has denitration, Tuo bioxin and the rare earth based complex multi-component denitration of demercuration multi-efficiency, the preparation method of Tuo bioxin catalyst concurrently; Adopt the technology of catalytic decomposition to solve bioxin pollution problem, compare active carbon adsorption more thorough; Compared with similar Tuo bioxin catalyst technology, adopt integrated forming technique, and add active rare-earth component, greatly improve the activity of catalyst, widened the temperature scope of application, product is applicable to the field clarifying smokes such as thermal power plant, glass factory, chemical plant.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described further.
Embodiment 1
The preparation method of the denitration of rare earth based complex multi-component, Tuo bioxin catalyst, step is as follows:
(1) preparation of active component:
The water of 50 liters is added active dissolution tank; Again the monoethanolamine of 13 ㎏ is joined in dissolving tank, when temperature arrives 90 DEG C, the ammonium metatungstate of the ammonium metavanadate of 12 ㎏, 40 ㎏ is joined in dissolving tank, uniform stirring 40 minutes, until all dissolve obtained ammonium metavanadate, ammonium metatungstate living solution;
The water of 50 liters is added active dissolution tank, again 20 ㎏ citric acids are joined in dissolving tank, stir after 5 minutes, the cerous nitrate of 10 ㎏ to be added in dissolving tank until completely dissolved, again the lanthanum nitrate of 10 ㎏ is added in dissolving tank, until completely dissolved obtained cerous nitrate, lanthanum nitrate living solution;
(2) preparation of carrier impregnation liquid: 400 premium on currency are added in batch mixing filling, then the ammonium metavanadate prepared, ammonium metatungstate living solution and cerous nitrate, lanthanum nitrate living solution are joined in mixing tank, be warmed up to 40 DEG C;
(3) support-activated: the titanium dioxide average mark of 609.5 ㎏ is added mixing tank twice, after stirring, the titanium dioxide flooded is dried, then split is sieved, obtained reactive silica titanium carrier split, and be divided into three parts;
(4) mixing process:
Once mixing: the silica flour of 369.5 ㎏ reactive silica titanium carriers and 35 ㎏ to be added in batch mixer and is dry mixed 10 minutes; Again the lactic acid of the stearic acid of 2.6 ㎏, 6.5 ㎏, 230 premium on currency and 45 liters of ammoniacal liquor are added in batch mixer successively and carry out Homogeneous phase mixing 20 minutes;
Secondary is mixing: the reactive silica titanium carrier of 105 ㎏ and 18 premium on currency are added in batch mixer and carry out Homogeneous phase mixing 20 minutes;
Three times are mixing: the reactive silica titanium carrier of 135 ㎏ and 8 liters of ammoniacal liquor are added in batch mixer and carry out Homogeneous phase mixing, until when temperature arrives 90 DEG C in batch mixer, discharge the gas that raw material produces,
Four times mixing: the polypropylene fibre PP of 3.25 ㎏, the glass fibre of 36 ㎏ and 50 premium on currency are added successively in batch mixer and carry out Homogeneous phase mixing 20 minutes;
Five times mixing: when temperature in batch mixer being down to below 70 DEG C, the cellulose ether of 2.44kg and the polyethylene glycol oxide of 2.14kg added in batch mixer and carry out Homogeneous phase mixing 10 minutes;
Six times mixing: again the cellulose ether of 2.44, the polyethylene glycol oxide of 2.14 and 5 liters of ammoniacal liquor are added batch mixer and carry out Homogeneous phase mixing 10 minutes, and raw material mixing is complete;
(5) raw material fully mix after moisture control at 28.0-30.0%, pH value is between 7.0-8.0, if pH value is not in scope, adds ammoniacal liquor and regulate in so mixing at the 6th time;
(6) mix raw material sealing is placed on temperature 20-30 DEG C, humidity carries out old in 50.0-70.0% environment, the time was at 24 hours;
(7) raw material after old, through filter and pre-extruded machine, carries out filtration to raw material and fully mediates;
(8) raw material is after filter and pre-extruded machined, again carries out 24 hours old;
(9) secondary old after raw material, through Powerful extruder extrusion molding, after packaging, enter drying;
(10) drying is divided into primary drying and redrying, and primary drying environment temperature is 20 DEG C, and dry environment humidity is 10%, starts by high humidity low temperature to low humidity high temperature, 10 days drying times; Redrying environment temperature is 60 DEG C, 48 hours drying times;
(11) initial product that drying completes enters roasting, and roasting kiln is continuous mesh belt type kiln, is provided with 12 temperature control points and 13 Temperature displaying points, altogether 25 Temperature displaying points; Roasting heating curve is parabola, by room temperature, enter product, and maximum temperature is 550 DEG C, and temperature can reduce gradually backward, and product kiln discharge temperature is 80 DEG C, and roasting time controlled at 28 hours.
Embodiment 2
The preparation method of the denitration of rare earth based complex multi-component, Tuo bioxin catalyst, step is as follows:
(1) preparation of active component:
The water of 30 liters is added active dissolution tank; Again the monoethanolamine of 10 ㎏ is joined in dissolving tank, when temperature arrives 85 DEG C, the ammonium metatungstate of the ammonium metavanadate of 10 ㎏, 35 ㎏ is joined in dissolving tank, uniform stirring 30 minutes, until all dissolve obtained ammonium metavanadate, ammonium metatungstate living solution;
The water of 40 liters is added active dissolution tank, again 15 ㎏ citric acids are joined in dissolving tank, stir after 4 minutes, the cerous nitrate of 8 ㎏ to be added in dissolving tank until completely dissolved, again the lanthanum nitrate of 8 ㎏ is added in dissolving tank, until completely dissolved obtained cerous nitrate, lanthanum nitrate living solution;
(2) preparation of carrier impregnation liquid: 300 premium on currency are added in batch mixing filling, then the ammonium metavanadate prepared, ammonium metatungstate living solution and cerous nitrate, lanthanum nitrate living solution are joined in mixing tank, be warmed up to 40 DEG C;
(3) support-activated: the titanium dioxide average mark of 502 ㎏ is added mixing tank twice, after stirring, the titanium dioxide flooded is dried, then split is sieved, obtained reactive silica titanium carrier split, and be divided into three parts;
(4) mixing process:
Once mixing: the silica flour of 308 ㎏ reactive silica titanium carriers and 12 ㎏ to be added in batch mixer and is dry mixed 5 minutes; Again the lactic acid of the stearic acid of 1.1 ㎏, 4 ㎏, 200 premium on currency and 25 liters of ammoniacal liquor are added in batch mixer successively and carry out Homogeneous phase mixing 15 minutes;
Secondary is mixing: the reactive silica titanium carrier of 85 ㎏ and 8 premium on currency are added in batch mixer and carry out Homogeneous phase mixing 20 minutes;
Three times are mixing: the reactive silica titanium carrier of 85 ㎏ and 10 liters of ammoniacal liquor are added in batch mixer and carry out Homogeneous phase mixing, until when temperature arrives 85 DEG C in batch mixer, discharge the gas that raw material produces,
Four times mixing: the polypropylene fibre PP of 1 ㎏, the glass fibre of 30 ㎏ and 40 premium on currency are added successively in batch mixer and carry out Homogeneous phase mixing 25 minutes;
Five times mixing: when temperature in batch mixer being down to below 70 DEG C, the cellulose ether of 1kg and the polyethylene glycol oxide of 2kg added in batch mixer and carry out Homogeneous phase mixing 7 minutes;
Six times mixing: again the cellulose ether of 1, the polyethylene glycol oxide of 1 and 4 liters of ammoniacal liquor are added batch mixer and carry out Homogeneous phase mixing 15 minutes, and raw material mixing is complete;
(5) raw material fully mix after moisture control at 28.0-30.0%, pH value is between 7.0-8.0, if pH value is not in scope, adds ammoniacal liquor and regulate in so mixing at the 6th time;
(6) the raw material sealing mixed is placed on temperature 20 DEG C, humidity is carried out old in 70.0% environment, and the time was at 12 hours;
(7) raw material after old, through filter and pre-extruded machine, carries out filtration to raw material and fully mediates;
(8) raw material is after filter and pre-extruded machined, again carries out 24 hours old;
(9) secondary old after raw material, through Powerful extruder extrusion molding, after packaging, enter drying;
(10) drying is divided into primary drying and redrying, and primary drying environment temperature is 40 DEG C, and dry environment humidity is 10%, starts by high humidity low temperature to low humidity high temperature, 10 days drying times; Redrying environment temperature is 60 DEG C, 24 hours drying times;
(11) initial product that drying completes enters roasting, and roasting kiln is continuous mesh belt type kiln, is provided with 12 temperature control points and 13 Temperature displaying points, altogether 25 Temperature displaying points; Roasting heating curve is parabola, by room temperature, enter product, and maximum temperature is 530 DEG C, and temperature can reduce gradually backward, and product kiln discharge temperature is 80 DEG C, and roasting time controlled at 28 hours.
Embodiment 3
The preparation method of the denitration of rare earth based complex multi-component, Tuo bioxin catalyst, step is as follows:
(1) preparation of active component:
The water of 60 liters is added active dissolution tank; Again the monoethanolamine of 15 ㎏ is joined in dissolving tank, when temperature arrives 95 DEG C, the ammonium metatungstate of the ammonium metavanadate of 15 ㎏, 45 ㎏ is joined in dissolving tank, uniform stirring 50 minutes, until all dissolve obtained ammonium metavanadate, ammonium metatungstate living solution;
The water of 50 liters is added active dissolution tank, again 25 ㎏ citric acids are joined in dissolving tank, stir after 6 minutes, the cerous nitrate of 12 ㎏ to be added in dissolving tank until completely dissolved, again the lanthanum nitrate of 12 ㎏ is added in dissolving tank, until completely dissolved obtained cerous nitrate, lanthanum nitrate living solution;
(2) preparation of carrier impregnation liquid: 500 premium on currency are added in batch mixing filling, then the ammonium metavanadate prepared, ammonium metatungstate living solution and cerous nitrate, lanthanum nitrate living solution are joined in mixing tank, be warmed up to 45 DEG C;
(3) support-activated: the titanium dioxide average mark of 700 ㎏ is added mixing tank twice, after stirring, the titanium dioxide flooded is dried, then split is sieved, obtained reactive silica titanium carrier split, and be divided into three parts;
(4) mixing process:
Once mixing: the silica flour of 400 ㎏ reactive silica titanium carriers and 40 ㎏ to be added in batch mixer and is dry mixed 15 minutes; Again the lactic acid of the stearic acid of 3 ㎏, 7 ㎏, 300 premium on currency and 50 liters of ammoniacal liquor are added in batch mixer successively and carry out Homogeneous phase mixing 25 minutes;
Secondary is mixing: the reactive silica titanium carrier of 100 ㎏ and 20 premium on currency are added in batch mixer and carry out Homogeneous phase mixing 25 minutes;
Three times are mixing: the reactive silica titanium carrier of 150 ㎏ and 10 liters of ammoniacal liquor are added in batch mixer and carry out Homogeneous phase mixing, until when temperature arrives 95 DEG C in batch mixer, discharge the gas that raw material produces,
Four times mixing: the polypropylene fibre PP of 3 ㎏, the glass fibre of 36 ㎏ and 60 premium on currency are added successively in batch mixer and carry out Homogeneous phase mixing 25 minutes;
Five times mixing: when temperature in batch mixer being down to below 70 DEG C, the cellulose ether of 3kg and the polyethylene glycol oxide of 5kg added in batch mixer and carry out Homogeneous phase mixing 15 minutes;
Six times mixing: again the cellulose ether of 3, the polyethylene glycol oxide of 5 and 6 liters of ammoniacal liquor are added batch mixer and carry out Homogeneous phase mixing 15 minutes, and raw material mixing is complete;
(5) raw material fully mix after moisture control at 28.0-30.0%, pH value is between 7.0-8.0, if pH value is not in scope, adds ammoniacal liquor and regulate in so mixing at the 6th time;
(6) the raw material sealing mixed is placed on temperature 30 DEG C, humidity is carried out old in 50.0% environment, and the time was at 20 hours;
(7) raw material after old, through filter and pre-extruded machine, carries out filtration to raw material and fully mediates;
(8) raw material is after filter and pre-extruded machined, again carries out 24 hours old;
(9) secondary old after raw material, through Powerful extruder extrusion molding, after packaging, enter drying;
(10) drying is divided into primary drying and redrying, and primary drying environment temperature is 20 DEG C, and dry environment humidity is 10%, starts by high humidity low temperature to low humidity high temperature, 10 days drying times; Redrying environment temperature is 60 DEG C, 48 hours drying times;
(11) initial product that drying completes enters roasting, and roasting kiln is continuous mesh belt type kiln, is provided with 12 temperature control points and 13 Temperature displaying points, altogether 25 Temperature displaying points; Roasting heating curve is parabola, by room temperature, enter product, and maximum temperature is 550 DEG C, and temperature can reduce gradually backward, and product kiln discharge temperature is 80 DEG C, and roasting time controlled at 28 hours.
Claims (10)
1. rare earth based complex multi-component denitration, de-bioxin catalyst, it is characterized in that: with titanium dioxide, silica flour for carrier, with the compound of the compound of the compound of the compound of tungsten, vanadium, cerium and lanthanum for active component, auxiliary material with under, make through mixing, granulation, kneading, shaping, dry, roasting;
Wherein, auxiliary material is MEA, ammoniacal liquor, lactic acid, stearic acid, glass fibre, citric acid, polypropylene fibre PP, cellulose ether, polyethylene glycol oxide and water.
2. rare earth based complex multi-component according to claim 1 denitration, Tuo bioxin catalyst, is characterized in that: compound 8-12 part of compound 5-45 part of titanium dioxide 500-700 part, silica flour 5-50 part, tungsten, compound 5-15 part of vanadium, cerium, compound 8-12 part of lanthanum, MEA 5-15 part, ammoniacal liquor 39-66 liter, lactic acid 2-7 part, stearic acid 1-5 part, glass fibre 30-40 part, citric acid 5-25 part, polypropylene fibre PP 3.0-3.5 part, cellulose ether 2-6 part, polyethylene glycol oxide 2-10 part and water 530-980 liter; Wherein, the unit of ammoniacal liquor and water to rise, the unit of other raw material in kilogram.
3. rare earth based complex multi-component according to claim 1 denitration, Tuo bioxin catalyst, is characterized in that: the compound of tungsten be ammonium metatungstate and or ammonium paratungstate; The compound of vanadium is one or more in ammonium metavanadate, vanadium oxide or vanadium oxalate; The compound of cerium is one or more in cerous nitrate, cerium oxalate, cerous sulfate or cerium oxide.
4. rare earth based complex multi-component according to claim 1 denitration, Tuo bioxin catalyst, is characterized in that: the compound of lanthanum is one or more in lanthanum nitrate, lanthanum oxalate, lanthanum sulfate or lanthana.
5. a preparation method for rare earth based complex multi-component according to claim 1 denitration, de-bioxin catalyst, is characterized in that: comprise the steps:
(1) active component preparation: the water of 30-80 part is joined mixed dissolution in MEA, when temperature arrives 80-100 DEG C, add the compound uniform stirring of the compound of vanadium, tungsten, the obtained compound of vanadium, the compound activity solution of tungsten after all dissolving;
The water that 40-60 rises is added citric acid stir, then add the compound of cerium, until completely dissolved, then add the compound of lanthanum, until completely dissolved obtained the compound of cerium, the compound activity solution of lanthanum;
(2) carrier impregnation liquid preparation: 300-500 premium on currency is added in dipping filling, then the compound of the compound of the vanadium prepared, the compound of tungsten and cerium, the compound activity solution of lanthanum are joined in impregnating autoclave respectively, be warmed up to 35-45 DEG C;
(3) support-activated: titanium dioxide is added impregnating autoclave, after stirring, the titanium dioxide flooded is carried out pneumatic conveying drying, obtained reactive silica titanium carrier;
(4) mixing process:
Once mixing: reactive silica titanium carrier and silica flour to be added in batch mixer and is dry mixed evenly, then by stearic acid, lactic acid, 100-250 premium on currency and 30-50 rise ammoniacal liquor and add successively in batch mixer and carry out Homogeneous phase mixing;
Secondary is mixing: by reactive silica titanium carrier and 10-20 premium on currency add in batch mixer and carry out Homogeneous phase mixing;
Three times are mixing: by reactive silica titanium carrier and 5-10 rise ammoniacal liquor and add in batch mixer and carry out Homogeneous phase mixing, temperature 85-95 DEG C in batch mixer;
Four times are mixing: by polypropylene fibre PP, glass fibre and 45-55 premium on currency add successively in batch mixer and carry out Homogeneous phase mixing;
Five times are mixing: when temperature in batch mixer being down to below 70 DEG C, by cellulose ether and polyethylene glycol oxide add in batch mixer and carry out Homogeneous phase mixing;
Six times are mixing: again by cellulose ether and polyethylene glycol oxide and 4-6 rise ammoniacal liquor and add batch mixer and carry out Homogeneous phase mixing;
(5) raw material after mixing carries out old, the raw material after old carry out filtration and fully mediate, shaping, dry;
(6) roasting is carried out after drying.
6. the preparation method of rare earth based complex multi-component according to claim 5 denitration, Tuo bioxin catalyst, it is characterized in that, six times mixing after, pH value is between 7.0-8.0, moisture control is at 28.0-30.0%, if pH value is not in scope, adds ammoniacal liquor in mixing at the 6th time and regulate.
7. the preparation method of rare earth based complex multi-component according to claim 5 denitration, Tuo bioxin catalyst, it is characterized in that, mix raw material sealing is placed on temperature 20-30 DEG C, humidity carries out old in 50.0-70.0% environment, the time is at 12-24 hour.
8. the preparation method of rare earth based complex multi-component according to claim 5 denitration, Tuo bioxin catalyst, it is characterized in that, drying is divided into primary drying and redrying, and primary drying environment temperature is 20-60 DEG C, dry environment humidity is 85-10%, 10 days drying times; Redrying environment temperature is 57-60 DEG C, drying time 24-48 hour.
9. the preparation method of rare earth based complex multi-component according to claim 5 denitration, Tuo bioxin catalyst, it is characterized in that, roasting kiln is continuous mesh belt type kiln, roasting heating curve is parabola, roasting by room temperature, and maximum temperature is 530-550 DEG C, then temperature reduces gradually, when being reduced to 60-80 DEG C, product kiln discharge, roasting time controls at 25-30 hour.
10. the preparation method of rare earth based complex multi-component according to claim 5 denitration, de-bioxin catalyst, is characterized in that comprising: after third time mixing end, raw material moisture control is at 26.0-28.50%.
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