CN104014376A - Preparation method for honeycomb-shaped low-temperature denitration catalytic material taking TiO2-Mg2Al4SiO18 as carrier - Google Patents
Preparation method for honeycomb-shaped low-temperature denitration catalytic material taking TiO2-Mg2Al4SiO18 as carrier Download PDFInfo
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Abstract
The invention provides a preparation method for a honeycomb-shaped low-temperature denitration catalytic material taking TiO2-Mg2Al4SiO18 as a carrier and belongs to an environment material and a catalysis technology. According to the preparation method, the mass percent of cordierite in a composite carrier is 40%-60%; the carrier, manganese acetate, cerous nitrate, ferric nitrate, nickel nitrate, glass fibers and methylcellulose are weighed according to a mass ratio of 100 to (50-70) to (10-20) to (5-10) to (3-8) to (10-15) to (5-10) and then are mixed; 30-40 parts of silica sol, 1-2 parts of triethanolamine, 0.3-0.9 part of polyether polyol, 3-6 parts of soya-bean oil and 1-5 parts of water are added and agitated; then a mixture is agitated and extruded, aged, dried and roasted. According to the preparation method, after the cordierite is added into the carrier, the mechanical strength of the honeycomb-shaped catalytic material is improved and the cost is reduced; a strict drying roasting system is adopted so that a cracking phenomenon is reduced and the yield of the honeycomb-shaped catalytic material is more than 80%; the preparation method is applicable to industrial production and has good denitration effect.
Description
Technical field
The invention belongs to catalyst technical field, relate generally to a kind of cement kiln in order to TiO
2-Mg
2al
4si
5o
18preparation method for the cellular low-temperature denitration of flue gas catalysis material of carrier.
Background technology
Nitrogen oxide (NOx) is a kind of pollutant of atmosphere, can cause the generation of acid rain.Fuel combustion and industrial production etc. all can produce NOx, and NOx pollutes oneself becomes a serious global problem.During " 12 ", NOx has been put into the binding indicator system, and total emission volumn need to cut down 10%.Within 2013, China's cement output is 24.1 hundred million tons, produces cement and produces a large amount of NOx, and concentration of emission is about 300mg/Nm
3～2200mg/Nm
3within 2013, national cement discharge nitrogen oxide is approximately 2,200,000 tons, account for 10% of national nitrogen oxide total release, according to < < cement industry atmosphere pollutants emission standards (GB4915-2013) > > regulation, the NO of new type nonaqueous cement production line
2limitation standard is 450mg/Nm
3.The limitation standard of Beijing is that cement kiln NOx allows concentration of emission to be no more than 200mg/Nm
3.And national Pollutant source investigation result shows that the current discharged nitrous oxides of China is 1100mg/Nm for the first time
3so the discharge present situation of China's cement kiln nitrogen oxide is compared with relevant criterion and is thrown away the larger gap of existence, therefore, very urgent to the reduction of discharging of cement kiln nitrogen oxide.
Cement kiln NOx control technology mainly comprises combustion control NOx draining technology, SNCR method (SNCR) and selective catalytic reduction (SCR) at present.First two denitration technology, because emission reduction efficiency is lower, can not become the main flow measure of denitration.SCR is at NH
3under the effect of catalyst, by NO and NO
2change into N
2, SCR can reach higher NOx reduction rate (85-95%), and flue gas NOx discharge can be reduced to 100-200mg/Nm
3.SCR is because huge reduction potential has been considered to NOx emission-reduction technology the most thoroughly.At present, research the catalyst more ripe and application of putting into production is mainly vanadium tungsten titanium system (V
2o
5-WO
3/ TiO
2), but due to its catalytic reaction temperature higher (300-500 ℃), be not suitable for being applied to the denitration of the low-temperature flue gas environment after cement kiln dedusting, cogeneration.And manganese cerium titanium system (MnO
x-CeO
2/ TiO
2) catalyst is because its low-temperature catalytic activity becomes suitable selection compared with high.
At present, the patent of the SCR denitration catalyst material of having applied for is more, from disclosed patent, SCR denitrating catalyst is mainly divided into honeycomb fashion structure type, flat and corrugated, wherein honeycomb fashion generally accounts for 80% the market share at present, it is the main flow of application, wherein honeycomb fashion is roughly divided into again two kinds, the first is for first using cordierite, the materials such as metal are made cellular framework, then titanium dioxide, above manganese salt isoreactivity material is immersed in, this kind of method, catalysis material mechanical strength is high, but due to air scour, the active material on honeycomb surface easily comes off, the second is for being directly shaped to cellular catalysis material material monolithics such as titanium dioxide, manganese salt, this kind of catalysis material activity keeping is good, but its mechanical strength is not as the former, titanium dioxide is wherein as the abundant carrying active substance of carrier, and cordierite is not generally used as carrier because specific area is little in this kind of catalyst, and the common fault of cellular catalysis material for cracking, one-tenth rate product are low, cause manganese cerium titanium system so far also not carry out suitability for industrialized production, so development erosion resistibility is strong, mechanical strength is high, and catalytic capability honeycombed catalyst strong and cracking resistance is very urgent.
Summary of the invention
For above problem, the present invention utilizes titanium dioxide and cordierite as complex carrier, although the little carrying active substance that is not suitable for of cordierite specific area, but due to titanium dioxide compound use, titanium dioxide surface amasss the load effect of greatly mainly having played, and the ferrimanganic magazine containing in cordierite itself is the metallic element of low-temperature catalyzed needs, so can not reduce the activity of catalysis material during cordierite addition in complex carrier no more than 60%, and the processability of cordierite is good, when the cordierite addition in complex carrier is no less than 40%, can make catalysis material there is higher mechanical strength, and the cost of cordierite is only 1/10th of titanium dioxide, significantly reduced cost, because the congenital low temperature active of manganese cerium titanium system is good, the present invention further adds again a certain amount of ferric nitrate and nickel nitrate on its basis, has further improved its low temperature active again, on drying and roasting, adopted strict temperature control system, reduced cracking, improved yield rate, reached more than 80%, thereby prepare, cost is low, low temperature active good, mechanical strength is high, the high cellular catalysis material that is applicable to suitability for industrialized production of yield rate.
A kind of with TiO
2-Mg
2al
4si
5o
18for cellular low-temperature denitration catalysis material of carrier and preparation method thereof, it is characterized in that comprising the following steps:
(1) adopt complex carrier, wherein to account for the mass ratio of complex carrier be 40%-60% to cordierite:
(2) carrier, manganese acetate, cerous nitrate, ferric nitrate, nickel nitrate, glass fibre, methylcellulose are weighed up for 100:50～70:10～20:5～10:3～8:10～15:5～10 in mass ratio, then put into mixer and be dry mixed 15～30 minutes.
(3) with respect to mass fraction, be the carrier of 100 parts, 30～40 parts of Ludox, 1～2 part of triethanolamine, 0.3～0.9 part of PPG, 3～6 parts of soya-bean oil, 1～5 part of water are added in the mixer in step (2) and stirred 15～30 minutes, become wet feed group, the taking-up of wet feed group is put into vacuum deairing machine mud refining and after 15～30 minutes, extrude cylindrical closely knit degassed material base, old 1～3 day.
(4) pug step (3) being obtained is extruded aperture 3～10 in vacuum material extruder, the cellular catalysis material base substrate of wall thickness 0.8～1.5.
(5) pug obtaining in step (4) is dried, drying system adopts 40 ℃ of constant temperature 4～10 hours, 40 ℃ through 2 hours to 60 ℃, 60 ℃ of constant temperature 6～12 hours, 60 ℃ through 2 hours to 80 ℃, 80 ℃ of constant temperature 8～14 hours, 80 ℃ through 2 hours to 105 ℃, 105 ℃ of constant temperature 10～16 hours.
(6) base substrate step (5) being obtained carries out roasting, and roasting system adopts 30 ℃ through 4～10 hours to 200 ℃; 200 ℃ through 14～20 hours to 350 ℃; 350 ℃ through 8～14 hours to 450 ℃; 450 ℃ are incubated 6～12 hours; 450 ℃ through 4～10 hours to 30 ℃, obtains cellular catalysis material.
Described titanium dioxide is nanoscale Detitanium-ore-type TiO
2play carrier function, because specific area can make greatly above active material fully loads on, be conducive to improve the activity of catalysis material.
Described cordierite is carrier, can improve catalysis material mechanical strength, can reduce the cost of catalysis material.
Described manganese acetate is active material; Cerous nitrate, ferric nitrate, nickel nitrate is auxiliary agent, has reduced denitration reaction activation energy, and denitration reaction is carried out at low temperature.
Described glass fibre is that length is 1-2mm, for further improving mechanical strength and the cracking resistance ability of catalysis material.
The binding agent of described methylcellulose during as catalyst extrusion molding, has played again reaming effect while being burnt when after baking, and the pore structure that has increased catalysis material surface has the carrying out of the catalytic reaction utilized.
The mass concentration of described Ludox is 20%～40%, plays the binding agent of cementation during as after baking.
Described triethanolamine Main Function is plasticizer, improves the plasticity of material, is convenient to extrude.
Described PPG is dispersant, can make glass fibre be uniformly dispersed in wet feed, there is no agglomeration.
Described soya-bean oil is lubricant, reduces owing to adding methylcellulose to cause the viscosity of material too high, is conducive to the extrusion molding of catalyst.
Compared with prior art, the invention has the beneficial effects as follows:
In complex carrier, add cordierite, improved the mechanical strength of catalyst, reduced cost
Adopt strict drying and roasting system, reduced cracking, improved yield rate, reach more than 80%, make suitability for industrialized production become possibility.
The low temperature active of formula is good, and cellular catalysis material prepared by the present invention, at 150～300 ℃ of temperature, air speed 10000～30000h
-1, NO
xin the atmosphere of concentration 800～1500ppm, denitration efficiency is all greater than 80%
The specific embodiment
Embodiment mono-
(1) take titanium dioxide 1.2kg, cordierite 0.8kg, manganese acetate 1.35kg, cerous nitrate 0.35kg, ferric nitrate 0.18kg, nickel nitrate 0.14kg, glass fibre 0.2kg, methylcellulose 0.18kg, puts into mixer and is dry mixed 15min; Take mass concentration and be 20% Ludox 0.8kg, triethanolamine 0.035kg, PPG 0.016kg, soya-bean oil 0.12kg, water 0.02kg joins in the dry powder after stirring and continues to stir 15 minutes.
(2) take out wet feed and carry out vacuum mud refining 15 minutes, old 3 days, then with vacuum material extruder, extrude aperture 3mm, the green honeycomb body of wall thickness 0.9mm.
(3) base substrate is dried, drying system adopts 40 ℃ of constant temperature 4 hours, and 40 ℃ through 2 hours to 60 ℃, 60 ℃ of constant temperature 6 hours, and 60 ℃ through 2 hours to 80 ℃, 80 ℃ of constant temperature 8 hours, 80 ℃ through 2 hours to 105 ℃, 105 ℃ of constant temperature 10 hours; After dry, carry out roasting, roasting system adopts 30 ℃ through 4 hours to 200 ℃; 200 ℃ through 14 hours to 350 ℃; 350 ℃ through 8 hours to 450 ℃; 450 ℃ are incubated 6 hours; 450 ℃ through 4 hours to 30 ℃, obtains cellular catalysis material.
The forward compression strength of this cellular catalysis material is 5.2MPa.At air speed 30000h
-1, NO
xconcentration is under 1500ppm condition, and this honeycomb catalysis material denitration rate in the time of 150 ℃ is 86.7%.
Embodiment bis-
(1) take titanium dioxide 1kg, cordierite 1kg, manganese acetate 1.25kg, cerous nitrate 0.3kg, ferric nitrate 0.16kg, nickel nitrate 0.12kg, glass fibre 0.23kg, methylcellulose 0.16kg, puts into mixer and is dry mixed 20min; Take mass concentration and be 30% Ludox 0.7kg, triethanolamine 0.03kg, PPG 0.012kg, soya-bean oil 0.1kg, continues to stir 20 minutes in the dry powder after after water 0.04kg joins and stirs.
(2) take out wet feed and carry out vacuum mud refining 20 minutes, within old 2 days, then with vacuum material extruder, extrude aperture 3.7mm, the green honeycomb body of wall thickness 1mm.
(3) base substrate is dried, drying system adopts 40 ℃ of constant temperature 6 hours, and 40 ℃ through 2 hours to 60 ℃, 60 ℃ of constant temperature 8 hours, and 60 ℃ through 2 hours to 80 ℃, 80 ℃ of constant temperature 10 hours, 80 ℃ through 2 hours to 105 ℃, 105 ℃ of constant temperature 12 hours; After dry, carry out roasting, roasting system adopts 30 ℃ through 6 hours to 200 ℃; 200 ℃ through 16 hours to 350 ℃; 350 ℃ through 10 hours to 450 ℃; 450 ℃ are incubated 8 hours; 450 ℃ through 6 hours to 30 ℃, obtains cellular catalysis material.
The forward compression strength of this cellular catalysis material is 6.6MPa.At air speed 22000h
-1, NO
xconcentration is under 1300ppm condition, and this honeycomb catalysis material denitration rate in the time of 150 ℃ is 84.2%.
Embodiment tri-
(1) take titanium dioxide 0.9kg, cordierite 1.1kg, manganese acetate 1.15kg, cerous nitrate 0.25kg, ferric nitrate 0.14kg, nickel nitrate 0.1kg, glass fibre 0.26kg, methylcellulose 0.14kg, puts into mixer and is dry mixed 25min; Take the Ludox 0.7kg of mass concentration 30%, triethanolamine 0.025kg, PPG 0.01kg, soya-bean oil 0.08kg, water 0.06kg joins to stir in rear dry powder and continues to stir 25 minutes.
(2) take out wet feed and carry out vacuum mud refining 25 minutes, old 2 days, then with vacuum material extruder, extrude aperture 5mm, the green honeycomb body of wall thickness 1.2mm.
(3) base substrate is dried, drying system adopts 40 ℃ of constant temperature 8 hours, and 40 ℃ through 2 hours to 60 ℃, 60 ℃ of constant temperature 10 hours, and 60 ℃ through 2 hours to 80 ℃, 80 ℃ of constant temperature 12 hours, 80 ℃ through 2 hours to 105 ℃, 105 ℃ of constant temperature 14 hours; After dry, carry out roasting, roasting system adopts 30 ℃ through 8 hours to 200 ℃; 200 ℃ through 18 hours to 350 ℃; 350 ℃ through 12 hours to 450 ℃; 450 ℃ are incubated 10 hours; 450 ℃ through 8 hours to 30 ℃, obtains cellular catalysis material.
The forward compression strength of this cellular catalysis material is 7.4MPa.At air speed 18000h
-1, NO
xconcentration is under 1000ppm condition, and this honeycomb catalysis material denitration rate in the time of 150 ℃ is 82.4%.
Embodiment tetra-
(1) take titanium dioxide 0.8kg, cordierite 1.2kg, manganese acetate 1.05kg, cerous nitrate 0.2kg, ferric nitrate 0.12kg, nickel nitrate 0.08kg, glass fibre 0.3kg, methylcellulose 0.12kg, puts into mixer and is dry mixed 30min; Take mass concentration and be 40% Ludox 0.6kg, triethanolamine 0.02kg, PPG 0.006kg, soya-bean oil 0.06kg, continues to stir 30 minutes in the dry powder after after water 0.08kg joins and stirs.
(2) take out wet feed and carry out vacuum mud refining 30 minutes, within old 1 day, then with vacuum material extruder, extrude aperture 7.4mm, the green honeycomb body of wall thickness 1.5mm.
(3) base substrate is dried, drying system adopts 40 ℃ of constant temperature 10 hours, and 40 ℃ through 2 hours to 60 ℃, 60 ℃ of constant temperature 12 hours, and 60 ℃ through 2 hours to 80 ℃, 80 ℃ of constant temperature 14 hours, 80 ℃ through 2 hours to 105 ℃, 105 ℃ of constant temperature 16 hours; After dry, carry out roasting, roasting system adopts 30 ℃ through 10 hours to 200 ℃; 200 ℃ through 20 hours to 350 ℃; 350 ℃ through 14 hours to 450 ℃; 450 ℃ are incubated 12 hours; 450 ℃ through 10 hours to 30 ℃, obtains cellular catalysis material.
The forward compression strength of this cellular catalysis material is 8.5MPa.At air speed 10000h
-1, NO
xconcentration is under 800ppm condition, and this honeycomb catalysis material denitration rate in the time of 150 ℃ is 80.8%.
Table one is denitration rate and the intensity under every group of example different temperatures under corresponding conditions.
Claims (4)
1. one kind with TiO
2-Mg
2al
4si
5o
18preparation method for the cellular low-temperature denitration catalysis material of carrier, is characterized in that comprising the following steps:
(1) adopt complex carrier, wherein to account for the mass ratio of complex carrier be 40%-60% to cordierite;
(2) carrier, manganese acetate, cerous nitrate, ferric nitrate, nickel nitrate, glass fibre, methylcellulose are weighed up for 100:50～70:10～20:5～10:3～8:10～15:5～10 in mass ratio, then put into mixer and be dry mixed 15～30 minutes;
(3) with respect to mass fraction, be the carrier of 100 parts, 30～40 parts of Ludox, 1～2 part of triethanolamine, 0.3～0.9 part of PPG, 3～6 parts of soya-bean oil, 1～5 part of water are added in the mixer in step (2) and stirred 15～30 minutes, become wet feed group, the taking-up of wet feed group is put into vacuum deairing machine mud refining and after 15～30 minutes, extrude cylindrical closely knit degassed material base, old 1～3 day;
(4) pug step (3) being obtained is extruded aperture 3～10 in vacuum material extruder, the cellular catalysis material base substrate of wall thickness 0.8～1.5;
(5) pug obtaining in step (4) is dried, drying system adopts 40 ℃ of constant temperature 4～10 hours, 40 ℃ through 2 hours to 60 ℃, 60 ℃ of constant temperature 6～12 hours, 60 ℃ through 2 hours to 80 ℃, 80 ℃ of constant temperature 8～14 hours, 80 ℃ through 2 hours to 105 ℃, 105 ℃ of constant temperature 10～16 hours;
(6) base substrate step (5) being obtained carries out roasting, and roasting system adopts 30 ℃ through 4～10 hours to 200 ℃; 200 ℃ through 14～20 hours to 350 ℃; 350 ℃ through 8～14 hours to 450 ℃; 450 ℃ are incubated 6～12 hours; 450 ℃ through 4～10 hours to 30 ℃, obtains cellular catalysis material.
2. according to claim 1 a kind of with TiO
2-Mg
2a
l4si
5o
18for the preparation method of the cellular low-temperature denitration catalysis material of carrier, wherein said titanium dioxide is nanoscale Detitanium-ore-type TiO
2.
3. according to claim 1 a kind of with TiO
2-Mg
2a
l4si
5o
18for the preparation method of the cellular low-temperature denitration catalysis material of carrier, wherein said glass fibre length is 1-2mm.
4. according to claim 1 a kind of with TiO
2-Mg
2a
l4si
5o
18for the preparation method of the cellular low-temperature denitration catalysis material of carrier, the mass concentration of Ludox is wherein 20%～40%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104525187A (en) * | 2014-12-27 | 2015-04-22 | 北京工业大学 | Preparation method of honeycomb-like Mn-Ce/TiO2-Mg2Al4Si5O18 low-temperature denitrating catalytic material |
| CN110898832A (en) * | 2019-12-20 | 2020-03-24 | 江苏芳杜若环境技术有限公司 | Preparation method of photocatalytic active carbon particles for purifying air |
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| CN103263914A (en) * | 2013-05-03 | 2013-08-28 | 北京工业大学 | Honeycomb-shaped SCR denitration catalysis material for cement kiln and preparation method thereof |
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2014
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| CN103263914A (en) * | 2013-05-03 | 2013-08-28 | 北京工业大学 | Honeycomb-shaped SCR denitration catalysis material for cement kiln and preparation method thereof |
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Cited By (2)
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| CN104525187A (en) * | 2014-12-27 | 2015-04-22 | 北京工业大学 | Preparation method of honeycomb-like Mn-Ce/TiO2-Mg2Al4Si5O18 low-temperature denitrating catalytic material |
| CN110898832A (en) * | 2019-12-20 | 2020-03-24 | 江苏芳杜若环境技术有限公司 | Preparation method of photocatalytic active carbon particles for purifying air |
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