CN106111149A - Boats and ships denitrating catalyst and preparation method thereof - Google Patents
Boats and ships denitrating catalyst and preparation method thereof Download PDFInfo
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
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- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/92—Chemical or biological purification of waste gases of engine exhaust gases
- B01D53/94—Chemical or biological purification of waste gases of engine exhaust gases by catalytic processes
- B01D53/9404—Removing only nitrogen compounds
- B01D53/9409—Nitrogen oxides
- B01D53/9413—Processes characterised by a specific catalyst
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
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Abstract
The invention belongs to gas denitrifying technology field, relate to a kind of boats and ships denitrating catalyst and preparation method thereof.It comprises the following steps: prepared by A, catalyst precursor, by metatitanic acid, zirconium oxychloride, cerous nitrate or CeO2, niobium oxalate, ferric nitrate mix homogeneously, add and mediate after attapulgite, extrusion molding, obtain catalyst precursor, B, catalyst precursor activate, and the dried high-temperature roasting of catalyst precursor obtains this catalyst.Denitration efficiency of the present invention is high, is suitable for large-scale production.
Description
Technical field
The invention belongs to gas denitrifying technology field, relate to the preparation method of a kind of boats and ships denitrating catalyst.
Background technology
The prevention and control of air pollution plan enjoying whole nation all circles to attract attention has been started up, and iron and steel, chemical industry, building materials (comprise glass row
Industry) etc. heavy polluted industry also will face, under " world is the tightest " prevention and control of air pollution policy, the severe destiny newly shuffled！This
Under pressure and background, various denitration technologies and corresponding catalyst are also kept up a steady flow of.
In numerous denitration technologies, SCR (SCR) owner's Flow Technique.
It is known that all places having high temperature, harmful nitrogen oxides all can be produced.The improvement of stationary source nitrogen oxides is own
Paid much attention to by people, and the improvement of mobile source nitrogen oxides also oneself causes the attention of countries in the world.Boats and ships shipping produces
Nitrogen oxides be exactly one of them.International Environmental Protection tissue natural resources protection association (NRDC) issue in Beijing " boats and ships and
Harbour air pollution white paper " display: a medium-to-large integrates shipment as used sulfur content as the marine fuel of 35000ppm
Oil, and during with the load of 70% peak power, the PM2.5 of one sky discharge is about as much as 500,000 state four lorries one day
Total emission volumn.In addition, the most a large amount of oxysulfides, nitrogen oxides etc..It is crucial that the foreign-going ship of 70% be thrown into away from
Marine site in 400 kilometers of water front off sea, and marine exhaust can be delivered to hinterland farther out.Analysis is had to point out: about 30%
Municipal pollution is from harbour.
At present in the ten big container hargours of the whole world, there are seven in China.The collection in three one-tenth of the Chinese Port annual coprocessing whole world
Vanning freight volume.But, although each the boats and ships entering harbour and lorry bring goods and expanding economy, but also aggravate
The air pollution at harbour and surrounding area.
To this end, more American-European major ports, formulating detailed harbour waste gas emission inventories, establishment meets harbour feature
" harbour clean air action plan ", wherein promotes ship, freight and the harbour facilities cleaned, significantly alleviates country and edge
Sea emphasis Polluted area, improves air quality.
Summary of the invention
It is an object of the invention to for the problems referred to above, it is provided that the preparation method of a kind of boats and ships denitrating catalyst.
It is a further object of the present invention to provide the boats and ships denitrating catalyst that a kind of denitration rate is high.
For reaching above-mentioned purpose, present invention employs following technical proposal: the preparation side of a kind of boats and ships denitrating catalyst
Method, comprises the following steps:
Prepared by A, catalyst precursor, by metatitanic acid, zirconium oxychloride, cerous nitrate or CeO2, niobium oxalate, ferric nitrate mixing all
Even, mediate after adding attapulgite, extrusion molding, obtain catalyst precursor,
B, catalyst precursor activate, and the dried high-temperature roasting of catalyst precursor obtains this catalyst.
In the preparation method of above-mentioned boats and ships denitrating catalyst, in step, metatitanic acid is with TiO2Meter is containing 35-
40wt%, zirconium oxychloride is with ZrO2Meter containing 30-35wt%, attapulgite in terms of dried object containing 10-20wt%, cerous nitrate or CeO2
With CeO2Meter is containing 5-10wt%, and niobium oxalate is with Nb2O5Meter is containing 0.1-3wt%, and ferric nitrate is with Fe2O3Meter is containing 0-8wt%.
In the preparation method of above-mentioned boats and ships denitrating catalyst, in step, metatitanic acid is with TiO2Meter contains
40wt%, zirconium oxychloride is with ZrO2Meter containing 30wt%, attapulgite in terms of dried object containing 15wt%, cerous nitrate or CeO2With CeO2
Meter is containing 9wt%, and niobium oxalate is with Nb2O5Meter is containing 1wt%, and ferric nitrate is with Fe2O3Meter is containing 5wt%.
In the preparation method of above-mentioned boats and ships denitrating catalyst, in step, when adding CeO2Time, described CeO2
It is carrier gas at 300 DEG C with air, with containing 300-500mg/m3SO2Carry out presulfurization process to prepare for 0.5-2 hour.
In the preparation method of above-mentioned boats and ships denitrating catalyst, in step, it is additionally added after adding attapulgite
There are cotton fibre, poly(ethylene oxide), carboxymethyl cellulose, stearic acid, ethanolamine and sesbania powder.
In the preparation method of above-mentioned boats and ships denitrating catalyst, in catalyst precursor, cotton fibre account for 0.48wt%,
Poly(ethylene oxide) accounts for 0.8wt%, carboxymethyl cellulose accounts for 0.25wt%, stearic acid accounts for 0.2wt%, ethanolamine accounts for 1.5wt%, field
Cyanines powder accounts for 5wt%.
In the preparation method of above-mentioned boats and ships denitrating catalyst, in stepb, catalyst precursor is at 60-120 DEG C
Under be dried 16-288 hour, and roasting 8-24 hour at 350-500 DEG C.
In the preparation method of above-mentioned boats and ships denitrating catalyst, it is little that catalyst precursor is dried 144 at 105 DEG C
Time, and roasting 16 hours at 450 DEG C.
In the preparation method of above-mentioned boats and ships denitrating catalyst, in step, it is extruded in cellular.
The boats and ships denitrating catalyst prepared according to above-mentioned preparation method.
Cerium-rich rare earth is the fine active constituent preparing SCR denitration.Generally CeO2Cheap as one
, nontoxic material, it is possible to as preferably storage oxygen agent, strengthening the Oxygen cycle of catalyst, it is as NH3SCR denitration reaction
It is inactive.But, CeO2There is SO2Exist or after presulfurization, CeO can be promoted2Under the conditions of 300-500 DEG C, SCR denitration is anti-
Should there is the activity of brilliance.This is due to CeO2By SO2Sulfated result.CeO2With sulphation CeO2SCR reaction, it then follows
Fley-Rideal mechanism.
NH3, NO and O2Redox reaction is occurred to generate N under catalyst action2And H2O.NH in this process3Suction
Attached is also most important, and TiO2There is abundant surface acidity.So, select TiO2It is the selection of a kind of wisdom for carrier.In order to
Widen rich cerium SCR denitration low temperature window, also should add metal-oxide (can also be configured the metal-oxide of ferrum) and necessity of niobium
Molding additive, could foot large-scale production demand.
Compared with prior art, it is an advantage of the current invention that: simple and reliable process, prepared denitrfying agent denitration efficiency is high,
It is suitable for large-scale production and popularization and application.
Detailed description of the invention
Reagent used in following embodiment, if no special instructions, can be commercially available from routine biochemistry reagent shop.With
Quantitative data in lower embodiment, is respectively provided with three times and repeats experiment, results averaged.
About the computational methods of material in embodiment:
(1) Ti0 in metatitanic acid2Content 45% calculates
(2) zirconium oxychloride (ZrOCl2*8H2O) molecular weight 322.25, the molecular weight 91 of zirconium, press 91+ by ZrO2 molecular weight
16x2=123 counts, and ZrO2 accounts for the percentage composition of zirconium oxychloride based on 123 ÷ 322.25=38.17%
(3) attapulgite is based on solid content 90%,
(4) cerous nitrate [Ce (NO3)3*6H2O] molecular weight is based on 434.22, and the molecular weight Ce=140.12 of cerium counts, CeO2's
Molecular weight is based on 140.12+16x2=172.13, and CeO2 accounts for the percentage composition of cerous nitrate by 172.13 ÷ 434.22=39.64%
Meter,
(5) niobium oxalate [C12H7NbO24] molecular weight based on 628.07, the molecular weight of antimony based on Nb=92.91, Nb2O molecule
Measure based on 92.91x2+16x5=185.82+80=265.82, Nb2O5Account for the percentage composition of niobium oxalate by 265.82 ÷
628.07x2=21.16% counts,
(6) ferric nitrate [Fe (NO3)3*9H2O] molecular weight is based on 404, and the molecular weight of ferrum is based on 55.8, and Fe2O3 molecular weight is pressed
159.69 meter, Fe2O3Account for the percentage composition of ferric nitrate: 159.69 ÷ 404x2=19.76% count.
Embodiment 1
Take the metatitanic acid 88.89g (counting percentage by weight as 40wt% with TiO2) after cleaning to put in 500ml burning bosom, then
Add a small amount of deionized water making beating, be subsequently adding zirconium oxychloride 78.6g (with ZrO2Meter percentage by weight is 30wt%) so that it is fill
Divide and stir, add cerous nitrate 12.61g (with CeO2Meter percentage by weight is 5wt%), niobium oxalate 0.47g is (with Nb2O5Meter
Percentage by weight is 5wt%), ferric nitrate 25.3g is (with Fe2O3Meter percentage by weight is 5wt%), strong agitation makes above-mentioned material
It is sufficiently mixed uniformly.Being poured into kneader afterwards, (in terms of attapulgite solid content, percentage by weight is to add attapulgite 21.1g
20%w), sesbania powder 5g, cotton fine 0.48g, poly(ethylene oxide) 0.8g, carboxymethyl cellulose 0.25g, stearic acid 0.2g, ethanolamine
1.5g.Fully mediate so that it is after having fixed toughness, take out and be placed on small-sized molding press, be squeezed into the cellular of fritter and urge
Agent presoma.Catalyst precursor is warmed up to 60 DEG C, is dried 288 hours.After being dried thoroughly, in activation furnace roasting, roasting temperature
Spend 500 DEG C, roasting time 24 hours, become the CeO that we need2-Nb2O5-Fe2O3/TiO2-ZrO2Denitrating catalyst.Should
The appreciation condition of catalyst: SO2 2000mg/m3、NO 500mg/m3、H2O content 8%, denitration rate: at 280 DEG C 95%.
Embodiment 2
Take metatitanic acid 88.89g (counting percentage by weight as 40wt% with TiO2) to put in 500ml burning bosom, then add a small amount of
Deionized water is pulled an oar, and is subsequently adding zirconium oxychloride 78.6g (with ZrO2Meter percentage by weight is 30wt%) so that it is it is sufficiently stirred for all
Even, add cerous nitrate 17.66g (with CeO2Meter percentage by weight is 7wt%), niobium oxalate 2.36g is (with Nb2O5Meter weight percent
Than being 0.5wt%), ferric nitrate 25.3g is (with Fe2O3Meter percentage by weight is 5wt%), strong agitation makes above-mentioned material the most mixed
Close uniformly.Being poured into kneader afterwards, (in terms of attapulgite solid content, percentage by weight is 17.5% to add attapulgite 19.4g
W), sesbania powder 5g, cotton fine 0.48g, poly(ethylene oxide) 0.8g, carboxymethyl cellulose 0.25g, stearic acid 0.2g and ethanolamine
1.5g.Fully mediate so that it is after there is toughness, take out and be placed on small-sized molding press, be squeezed into the honeycombed catalyst of fritter
Presoma.Catalyst precursor is warmed up to 120 DEG C, is dried 16 hours.After being dried thoroughly, at activation furnace roasting, sintering temperature 300
DEG C, roasting time 8 hours, become the CeO that we need2-Nb2O5-Fe2O3/TiO2-ZrO2Denitrating catalyst.This catalyst
Appreciation condition: SO22000mg/m3、NO 500mg/m3、H2O content 8%, denitration rate: at 280 DEG C 98%.
Embodiment 3
Take metatitanic acid 88.89g (counting percentage by weight as 40wt% with TiO2) to put in 500ml burning bosom, then add a small amount of
Deionized water is pulled an oar, and is subsequently adding zirconium oxychloride 78.6g (with ZrO2Meter percentage by weight is 30wt%) so that it is it is sufficiently stirred for all
Even, add cerous nitrate 22.7g (with CeO2Meter percentage by weight is 9wt%), niobium oxalate 4.73g is (with Nb2O5Meter weight percent
Than being 1wt%), ferric nitrate 25.3g is (with Fe2O3Meter percentage by weight is 5wt%), strong agitation makes above-mentioned material be sufficiently mixed
Uniformly.Be poured into kneader afterwards, add attapulgite 16.7g (counting percentage by weight as 15wt% with attapulgite solid content),
Sesbania powder 5g, cotton fine 0.48g, poly(ethylene oxide) 0.8g, carboxymethyl cellulose 0.25g, stearic acid 0.2g and ethanolamine 1.5g.Fill
Divide and mediate so that it is after there is toughness, take out and be placed on small-sized molding press, be squeezed into the honeycombed catalyst presoma of fritter.
Catalyst precursor is warmed up to 105 DEG C, is dried 144 hours.After being dried thoroughly, in activation furnace roasting, sintering temperature 450 DEG C, roasting
16 hours burning time, become the CeO that we need2-Nb2O5-Fe2O3/TiO2-ZrO2 denitrating catalyst.Commenting of this catalyst
Valency condition: SO22000mg/m3, NO 500mg/m3, H2O content 8%, denitration rate: at 280 DEG C 100%.
Embodiment 4
Choosing commercially available metatitanic acid is raw material, pulls an oar with deionized water, carries out washing, filtering, and removes the SO not cleaned4Make
SO4Control 3 4% (with TiO2Meter).Take the metatitanic acid 88.89g after cleaning (with TiO2Meter percentage by weight is 40%W) put
Enter 500ml to burn in bosom, then add a small amount of deionized water making beating.It is subsequently adding zirconium oxychloride 78.6g (with ZrO2Meter percentage by weight
For 30%W) so that it is stir.(also can by stir-zirconium mixture put into oven for drying, pulverize standby).
Add and process through presulfurization, and wear into the CeO of 100 mesh fine powders25g is (with CeO2Meter percentage by weight is 5%w), niobium oxalate
0.47g is (with Nb2O5Meter percentage by weight is 0.1%w), ferric nitrate 25.3g (counting percentage by weight as 5%w with Fe2O3), with strong
Strong stirring makes above-mentioned material be sufficiently mixed uniformly.It is poured into kneader afterwards, adds attapulgite 19.9g and (admittedly contain with attapulgite
Gauge percentage by weight is 17.9%w), sesbania powder 5g, cotton fine 0.48g, poly(ethylene oxide) 0.8g, carboxymethyl cellulose 0.25g,
Stearic acid 0.2g, ethanolamine 1.5g, etc. adjuvant.Fully close so that it is after having fixed property, take out and be placed on small-sized molding press
On, it is squeezed into the honeybee catalyst precursor of fritter.Presoma to be progressively warmed up to 80--100 DEG C, is dried 48 hours.It is dried thorough
At at the end, also will be in activation furnace roasting, sintering temperature 450-550 DEG C, roasting time 2 hours, become the CeO that we need2-
Nb2O5-Fe2O3/TiO2-ZrO2Denitrating catalyst.The appreciation condition of this catalyst: SO2 2000mg/m3、NO 500mg/m3、H2O
Content 8%, denitration rate: at 280 DEG C 96%.
CeO2It is carrier gas at 300 DEG C with air, with containing 300-500mg/m3SO2Carry out presulfurization and process 0.5-2 hour system
?.
Embodiment 5
Take TiO250g, ZrO230g puts into 500ml and burns in bosom, then adds a small amount of deionized water making beating so that it is be sufficiently stirred for
Uniformly, CeO is added2 10g、Nb2O5 3g、Fe2O38g, strong agitation makes above-mentioned material be sufficiently mixed uniformly.It is poured into afterwards and pinches
Conjunction machine, adds attapulgite 10g, sesbania powder 5g, cotton fine 0.48g, poly(ethylene oxide) 0.8g, carboxymethyl cellulose 0.25g, tristearin
Acid 0.2g and ethanolamine 1.5g.Fully mediate so that it is after having fixed toughness, take out and be placed on small-sized molding press, be squeezed into
The honeycombed catalyst presoma of fritter.Catalyst precursor is warmed up to 60 DEG C, is dried 288 hours.After being dried thoroughly, in activation
Stove roasting, sintering temperature 500 DEG C, roasting time 24 hours, become the CeO that we need2-Nb2O5-Fe2O3/TiO2-ZrO2
Denitrating catalyst.The appreciation condition of this catalyst: SO2 2000mg/m3、NO 500mg/m3、H2O content 8%, denitration rate: 280
At DEG C 97%.
CeO2It is carrier gas at 300 DEG C with air, with containing 300-500mg/m3SO2Carry out presulfurization and process 0.5-2 hour system
?.
Embodiment 6
The present embodiment is substantially the same manner as Example 5, and difference is to be not added with Fe2O3.The appreciation condition of this catalyst:
SO2 2000mg/m3、NO 500mg/m3、H2O content 8%, denitration rate: at 280 DEG C 90%.
Specific embodiment described herein is only to present invention spirit explanation for example.Technology neck belonging to the present invention
Described specific embodiment can be made various amendment or supplements or use similar mode to replace by the technical staff in territory
Generation, but without departing from the spirit of the present invention or surmount scope defined in appended claims.
Claims (10)
1. the preparation method of a boats and ships denitrating catalyst, it is characterised in that comprise the following steps:
Prepared by A, catalyst precursor, by metatitanic acid, zirconium oxychloride, cerous nitrate or CeO2, niobium oxalate, ferric nitrate mix homogeneously, add
Mediate after entering attapulgite, extrusion molding, obtain catalyst precursor,
B, catalyst precursor activate, and the dried high-temperature roasting of catalyst precursor obtains this catalyst.
The preparation method of boats and ships denitrating catalyst the most according to claim 1, it is characterised in that in step, inclined titanium
Acid is with TiO2Meter is containing 35-40wt%, and zirconium oxychloride is with ZrO2Meter containing 30-35wt%, attapulgite in terms of dried object containing 10-
20wt%, cerous nitrate or CeO2With CeO2Meter is containing 5-10wt%, and niobium oxalate is with Nb2O5Meter is containing 0.1-3wt%, and ferric nitrate is with Fe2O3
Meter is containing 0-8wt%.
The preparation method of boats and ships denitrating catalyst the most according to claim 2, it is characterised in that in step, inclined titanium
Acid is with TiO2Meter is containing 40wt%, and zirconium oxychloride is with ZrO2Meter containing 30wt%, attapulgite in terms of dried object containing 15wt%, cerous nitrate
Or CeO2With CeO2Meter is containing 9wt%, and niobium oxalate is with Nb2O5Meter is containing 1wt%, and ferric nitrate is with Fe2O3Meter is containing 5wt%.
The preparation method of boats and ships denitrating catalyst the most according to claim 1, it is characterised in that in step, when adding
Enter CeO2Time, described CeO2It is carrier gas at 300 DEG C with air, with containing 300-500mg/m3SO2Carry out presulfurization and process 0.5-
Within 2 hours, prepare.
The preparation method of boats and ships denitrating catalyst the most according to claim 1, it is characterised in that in step, is adding
Cotton fibre, poly(ethylene oxide), carboxymethyl cellulose, stearic acid, ethanolamine and sesbania powder it has been additionally added after entering attapulgite.
The preparation method of boats and ships denitrating catalyst the most according to claim 5, it is characterised in that at catalyst precursor
In, cotton fibre accounts for 0.48wt%, poly(ethylene oxide) accounts for 0.8wt%, carboxymethyl cellulose accounts for 0.25wt%, stearic acid accounts for 0.2wt%,
Ethanolamine accounts for 1.5wt%, sesbania powder accounts for 5wt%.
The preparation method of boats and ships denitrating catalyst the most according to claim 1, it is characterised in that in stepb, catalysis
Agent presoma is dried 16-288 hour at 60-120 DEG C, and roasting 8-24 hour at 350-500 DEG C.
The preparation method of boats and ships denitrating catalyst the most according to claim 7, it is characterised in that catalyst precursor exists
It is dried 144 hours at 105 DEG C, and roasting 16 hours at 450 DEG C.
The preparation method of boats and ships denitrating catalyst the most according to claim 1, it is characterised in that in step, extrusion
Become in cellular.
10. the boats and ships denitrating catalyst prepared according to the preparation method described in claim 1-9 any one.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106824212A (en) * | 2017-03-10 | 2017-06-13 | 扬州大学 | A kind of CeO2/Fe2O3The preparation method of the nano environment material on load attapulgite |
| CN106890634A (en) * | 2017-02-15 | 2017-06-27 | 福建帕特纳环境产品有限公司 | A kind of SCR denitration of boat diesel engine vent gas treatment |
| CN109078631A (en) * | 2017-06-13 | 2018-12-25 | 中国科学院福建物质结构研究所 | The Ce base catalyst preparation and NOx of efficient cryogenic eliminate performance study |
| CN109603922A (en) * | 2018-11-29 | 2019-04-12 | 北京国电龙源环保工程有限公司 | A kind of composite titanium dioxide and preparation method thereof for high-ratio surface denitrating catalyst |
| CN111715230A (en) * | 2020-06-11 | 2020-09-29 | 华北电力大学 | Thin-wall flat-plate type low-temperature sulfur-resistant SCR denitration catalyst and preparation method thereof |
| CN112473682A (en) * | 2020-11-24 | 2021-03-12 | 南京大学 | High-performance medium-low temperature NH3-SCR catalyst, preparation method and application thereof |
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| CN111715230A (en) * | 2020-06-11 | 2020-09-29 | 华北电力大学 | Thin-wall flat-plate type low-temperature sulfur-resistant SCR denitration catalyst and preparation method thereof |
| CN111715230B (en) * | 2020-06-11 | 2021-03-19 | 华北电力大学 | Thin-wall flat-plate type low-temperature sulfur-resistant SCR denitration catalyst and preparation method thereof |
| CN112473682A (en) * | 2020-11-24 | 2021-03-12 | 南京大学 | High-performance medium-low temperature NH3-SCR catalyst, preparation method and application thereof |
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