CN105435765A - Preparation method of denitration catalyst - Google Patents
Preparation method of denitration catalyst Download PDFInfo
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- CN105435765A CN105435765A CN201510813972.7A CN201510813972A CN105435765A CN 105435765 A CN105435765 A CN 105435765A CN 201510813972 A CN201510813972 A CN 201510813972A CN 105435765 A CN105435765 A CN 105435765A
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- denitrating catalyst
- tio
- catalyst according
- nitric acid
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- 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
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8621—Removing nitrogen compounds
- B01D53/8625—Nitrogen oxides
- B01D53/8628—Processes characterised by a specific catalyst
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/14—Silica and magnesia
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2255/00—Catalysts
- B01D2255/20—Metals or compounds thereof
- B01D2255/207—Transition metals
- B01D2255/20707—Titanium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2255/00—Catalysts
- B01D2255/20—Metals or compounds thereof
- B01D2255/209—Other metals
- B01D2255/2092—Aluminium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/40—Nitrogen compounds
- B01D2257/404—Nitrogen oxides other than dinitrogen oxide
Abstract
The invention relates to a preparation method of a denitration catalyst and belongs to the technical field of petrochemical industry. The preparation process comprises preparation of alumina sol, preparation of a TiO2 coating and representation of a TiO2 coating. The preparation method comprises the following steps: firstly performing magnetic stirring on alumina sol, urea and nitric acid at room temperature until the alumina sol, urea and nitric acid are uniformly dispersed, thereby obtaining milk white transparent alumina sol; and adding TiO2 nitric acid and an additive into a beaker in proportion, performing magnetic stirring, then adding the alumina sol, stirring uniformly so as to obtain needed TiO2 slurry, soaking a cordierite honeycomb ceramic matrix with the TiO2 slurry, then taking out the cordierite honeycomb ceramic matrix, blowing away redundant raffinate in pores by use of compressed air, drying at a temperature of 110-150 DEG C in a drying oven for 5-7 hours, and roasting in a muffle furnace for 4-7 hours, thereby obtaining a honeycomb ceramic matrix loaded with the TiO2 coating. The denitration catalyst provided by the method has the characteristics of bed pressure reduction, high catalysis efficiency and less change of amplification reaction, and is high in firmness, high in charge capacity and simple in preparation process.
Description
Technical field
The present invention relates to a kind of preparation method of denitrating catalyst, belong to technical field of petrochemical industry.
Background technology
Along with the increasingly stringent of environmental regulation, the requirement of country to the restriction of oil refining enterprise's Air Pollutant Emission is also stricter.The emission limit of current country to most area existing enterprise nitrogen oxide is 240mg/m3, and July 1 in 2014, the emission limit of Qi existing enterprise nitrogen oxide reduced to 100mg/m3, and some area is even lower.Reaching this standard, there is certain difficulty in existing exhaust gas denitration technology.Exhaust gas denitration technology conventional both at home and abroad has dry method exhaust gas denitration and wet method exhaust gas denitration.The dry method exhaust gas denitration technology that present commercial plant adopts mainly comprises selective catalytic reduction (SCR) and SNCR method (SNSR), but these two kinds of technology also exist the shortcomings such as cost of investment is high, denitration rate is low.And wet method exhaust gas denitration technology industrially Application comparison many have sour absorption process, aqueous slkali absorption process, oxidative absorption method, liquid-phase reduction absorption process etc., wet method exhaust gas denitration technology has the advantages such as process equipment is relatively simple, operating temperature is lower, energy consumption is low, disposal cost is lower, has research and industrial application value.
SCR technology (SCR) is the gas denitrifying technology be most widely used at present, plays an important role to the discharge controlling nitrogen oxide.SCR catalyst can be divided into board-like, corrugated and honeycomb fashion by structure difference.Bed pressure drop is low, catalytic efficiency is high because having for honeycomb fashion integer catalyzer, the iodine change advantage such as little and obtain commercial Application widely, is wherein one of integral catalyzer study hotspot becoming this field of matrix with cordierite.
Cordierite monolithic catalyst by cordierite substrates, coating and active component three part form, cordierite substrates is an indirect supporter of integral catalyzer, and coating is only the true carrier of active component.At present the research of cordierite coating is focused mostly in Al
2o
3coating, as Chen Chunbo etc. with boehmite powder for raw material, adopt Alumina gel method, active A l respectively
2o
3slurry method and mixed slurry method, carry out coating load to cordierite honeycomb matrix, prepared the Al with higher firmness and bigger serface
2o
3coating.TiO
2the SiO that continues
2and Al
2o
3third generation carrier afterwards, with TiO
2denitrating catalyst for carrier has showed excellent catalytic activity, as V
2o
5/ TiO
2, MnO
x/ TiO
2, CeO
2/ TiO
2deng, but current research focuses mostly on powder or pellet type catalyst, for the TiO of cordierite monolith formula denitrating catalyst
2coating research is less, and existing TiO
2preparation method's many employings sol-gal process of coating, preparation time is grown and the comparatively complicated mouth of preparation method, is not suitable for commercial Application.Therefore, exploitation firmness is high, load capacity is high and the simple TiO of preparation technology
2the industrialization development of coating to cordierite monolith formula denitrating catalyst is significant.
201110374711.1 disclose a kind of denitrating catalyst, relate to catalyst technical field.This catalyst is made up of each component of following parts by weight: titanium dioxide 75-85 part; Tungstic acid 10-12 part; Silica 3-6 part; Vanadic anhydride 2-3 part; Kapok slurry 3-6 part; Glass fibre 2-7 part; Stearic acid 2-3 part; Mix after each component by weight proportioning, stir, then after, extrusion molding old through old, pre-extruded, secondary successively, primary drying, redrying, high-temperature calcination, finished product finishing, finished catalyst can be packed to obtain.Denitrating catalyst of the present invention, in horizontal mechanical strength, longitudinal mechanical strength, rate of wear etc., performance improves a lot, thus improves the range of application of product, and the service life of product and efficiency.
201310588022.X discloses a kind of denitrating catalyst, it is characterized in that: described catalyst is prepared from by each component of following weight fraction: molybdenum trioxide 25-35 part; Tungstic acid 10-18 part; Titanium dioxide 55-80 part; Vanadic anhydride 2-5 part; Lime stone 6-17 part; Stearic acid 2.5-6 part; Glass dust 2.5-3 part; Inorganic silica gel 3.5-5 part; Polyethylene 2.5-3.5 part; Paraffin 0.5-1.5 part.Denitrating catalyst compressive resistance of the present invention is high, and catalyst not easily efflorescence thus extend service life of catalyst, the porosity of denitrating catalyst increases, thus improves catalytic efficiency, decreases catalyst amount.
201410419979.6 disclose a kind of denitrating catalyst, and its production process comprises the following steps successively: (1) uses glass-ceramic procedure of fibre production catalyst substrate; (2) catalyst substrate using mixture solution soaking step (1) to produce; (3) catalyst substrate that step (2) was soaked is carried out drying; (4) calcine.Wherein, step (1) uses the cogged calender production catalyst substrate of band; Mixture solution in step (2) contains the SiO220-30% of mixture solution gross mass, glass fibre 10-20%, V2O
5~ 10-20%, WO
35-10%, TiO
220-30%.Specific surface area of catalyst of the present invention is large, and intensity is high, and under the prerequisite ensureing denitration effect, resistance to corrosion, anti-smoke-shock ability etc. are all better than traditional cellular catalyst.
Summary of the invention
The object of this invention is to provide a kind of preparation method of denitrating catalyst, this technology can realize the denitrification process in petroleum refining process.
A preparation method for denitrating catalyst, method is as follows:
(1) a certain amount of boehmite, urea and certain density nitric acid are stirred to dispersed in room temperature lower magnetic force, obtain milky Alumina gel;
(2) by TiO
2, certain density nitric acid and additive add in beaker by a certain percentage;
(3) add Alumina gel after magnetic agitation certain hour, be stirred to evenly and obtain required TiO
2slurries;
(4) cordierite honeycomb ceramic matrix is immersed in TiO
2a period of time in slurries;
(5) raffinate unnecessary in duct is blown away with compressed air after taking out, dry in baking oven, and roasting in Muffle furnace, namely obtain load TiO
2the ceramic honey comb matrix of coating;
The consumption of the boehmite described in step (1) is 100 ~ 200g; The amount of the urea described in step (1) is 3 ~ 6g; Step (1) and the concentration of nitric acid described in step (2) are 0.01 ~ 0.1mol/L; TiO described in step (2)
2consumption be 200 ~ 400g; Additive amount described in step (2) is 0.02 ~ 0.08% of total inventory; Magnetic agitation time 0.5 ~ 2h described in step (3); Cordierite honeycomb ceramic matrix described in step (4) is immersed in TiO
2the slurries time is 3 ~ 6min; Oven temperature described in step (5) is 110 ~ 150 DEG C, and drying time is 5 ~ 7h; Muffle furnace described in step (5) is at 400 ~ 600 DEG C, and roasting time is 4 ~ 7h.
Tool of the present invention has the following advantages:
(1) denitrating catalyst that the method obtains has that bed pressure drop is low, catalytic efficiency is high, iodine changes little feature;
(2) firmness of denitrating catalyst that obtains of the method is high, load capacity is high and preparation technology is simple.
Detailed description of the invention
Be described in further details the present invention below by embodiment, these embodiments are only used for the present invention is described, do not limit the scope of the invention.
embodiment 1
A preparation method for denitrating catalyst, method is as follows:
(1) nitric acid of the boehmite of 100g, 3g urea and 0.01mol/L concentration is stirred to dispersed in room temperature lower magnetic force, obtains milky Alumina gel;
(2) by 200gTiO
2, the nitric acid of 0.01mol/L concentration and additive 0.2 add in beaker in proportion;
(3) add Alumina gel after magnetic agitation 0.5h, be stirred to evenly and obtain required TiO
2slurries;
(4) cordierite honeycomb ceramic matrix is immersed in TiO
23min in slurries;
(5) blow away raffinate unnecessary in duct with compressed air, 110 DEG C of dry 5h in baking oven after taking out, and in Muffle furnace roasting 4h at 400 DEG C, namely obtain load TiO
2the ceramic honey comb matrix of coating.
embodiment 2
A preparation method for denitrating catalyst, method is as follows:
(1) nitric acid of the boehmite of 150g, 5g urea and 0.05mol/L concentration is stirred to dispersed in room temperature lower magnetic force, obtains milky Alumina gel;
(2) by 300gTiO
2, the nitric acid of 0.05mol/L concentration and additive 0.5 add in beaker in proportion;
(3) add Alumina gel after magnetic agitation 1.5h, be stirred to evenly and obtain required TiO
2slurries;
(4) cordierite honeycomb ceramic matrix is immersed in TiO
25min in slurries;
(5) blow away raffinate unnecessary in duct with compressed air, 130 DEG C of dry 6h in baking oven after taking out, and in Muffle furnace roasting 5h at 500 DEG C, namely obtain load TiO
2the ceramic honey comb matrix of coating.
embodiment 3
A preparation method for denitrating catalyst, method is as follows:
(1) nitric acid of the boehmite of 200g, 6g urea and 0.1mol/L concentration is stirred to dispersed in room temperature lower magnetic force, obtains milky Alumina gel;
(2) by 400gTiO
2, the nitric acid of 0.1mol/L concentration and additive 0.8 add in beaker in proportion;
(3) add Alumina gel after magnetic agitation 2h, be stirred to evenly and obtain required TiO
2slurries;
(4) cordierite honeycomb ceramic matrix is immersed in TiO
26min in slurries;
(5) blow away raffinate unnecessary in duct with compressed air, 150 DEG C of dry 7h in baking oven after taking out, and in Muffle furnace roasting 7h at 600 DEG C, namely obtain load TiO
2the ceramic honey comb matrix of coating.
embodiment 4
A preparation method for denitrating catalyst, method is as follows:
(1) nitric acid of the boehmite of 150g, 3g urea and 0.01mol/L concentration is stirred to dispersed in room temperature lower magnetic force, obtains milky Alumina gel;
(2) by 250gTiO
2, the nitric acid of 0.01mol/L concentration and additive 0.2 add in beaker in proportion;
(3) add Alumina gel after magnetic agitation 0.5h, be stirred to evenly and obtain required TiO
2slurries;
(4) cordierite honeycomb ceramic matrix is immersed in TiO
26min in slurries;
(5) blow away raffinate unnecessary in duct with compressed air, 110 DEG C of dry 6h in baking oven after taking out, and in Muffle furnace roasting 4h at 400 DEG C, namely obtain the ceramic honey comb matrix of load TiO2 coating.
embodiment 5
A preparation method for denitrating catalyst, method is as follows:
(1) nitric acid of the boehmite of 100g, 3g urea and 0.01mol/L concentration is stirred to dispersed in room temperature lower magnetic force, obtains milky Alumina gel;
(2) by 300gTiO
2, the nitric acid of 0.1mol/L concentration and additive 0.2 add in beaker in proportion;
(3) add Alumina gel after magnetic agitation 0.5h, be stirred to evenly and obtain required TiO
2slurries;
(4) cordierite honeycomb ceramic matrix is immersed in TiO
25min in slurries;
(5) blow away raffinate unnecessary in duct with compressed air, 130 DEG C of dry 5h in baking oven after taking out, and in Muffle furnace roasting 6h at 400 DEG C, namely obtain load TiO
2the ceramic honey comb matrix of coating.
Claims (10)
1. a preparation method for denitrating catalyst, is characterized in that: comprise the steps:
(1) a certain amount of boehmite, urea and certain density nitric acid are stirred to dispersed in room temperature lower magnetic force, obtain milky Alumina gel;
(2) by TiO
2, certain density nitric acid and additive add in beaker by a certain percentage;
(3) add Alumina gel after magnetic agitation certain hour, be stirred to evenly and obtain required TiO
2slurries;
(4) cordierite honeycomb ceramic matrix is immersed in TiO
2a period of time in slurries;
(5) raffinate unnecessary in duct is blown away with compressed air after taking out, dry in baking oven, and roasting in Muffle furnace, namely obtain load TiO
2the ceramic honey comb matrix of coating.
2. the preparation method of a kind of denitrating catalyst according to claim 1, is characterized in that:
The consumption of the boehmite described in step (1) is 100 ~ 200g.
3. the preparation method of a kind of denitrating catalyst according to claim 1, is characterized in that:
The amount of the urea described in step (1) is 3 ~ 6g.
4. the preparation method of a kind of denitrating catalyst according to claim 1, is characterized in that:
Step (1) and the concentration of nitric acid described in step (2) are 0.01 ~ 0.1mol/L.
5. the preparation method of a kind of denitrating catalyst according to claim 1, is characterized in that:
TiO described in step (2)
2consumption be 200 ~ 400g.
6. the preparation method of a kind of denitrating catalyst according to claim 1, is characterized in that:
Additive amount described in step (2) is 0.02 ~ 0.08% of total inventory.
7. the preparation method of a kind of denitrating catalyst according to claim 1, is characterized in that:
Magnetic agitation time 0.5 ~ 2h described in step (3).
8. the preparation method of a kind of denitrating catalyst according to claim 1, is characterized in that:
Cordierite honeycomb ceramic matrix described in step (4) is immersed in TiO
2the slurries time is 3 ~ 6min.
9. the preparation method of a kind of denitrating catalyst according to claim 1, is characterized in that:
Oven temperature described in step (5) is 110 ~ 150 DEG C, and drying time is 5 ~ 7h.
10. the preparation method of a kind of denitrating catalyst according to claim 1, is characterized in that:
Muffle furnace described in step (5) is at 400 ~ 600 DEG C, and roasting time is 4 ~ 7h.
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|---|---|---|---|
| CN201510813972.7A CN105435765A (en) | 2015-11-23 | 2015-11-23 | Preparation method of denitration catalyst |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108067218A (en) * | 2016-11-15 | 2018-05-25 | 中国石油化工股份有限公司 | The preparation method of denitrating catalyst |
| CN108114756A (en) * | 2016-11-29 | 2018-06-05 | 中国石油化工股份有限公司 | A kind of sulfur-containing organic waste gas catalysis oxidation protective agent and its preparation method and application |
| CN110833826A (en) * | 2019-11-19 | 2020-02-25 | 山东中材汽车复合材料有限公司 | Preparation method of composite coating material |
-
2015
- 2015-11-23 CN CN201510813972.7A patent/CN105435765A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108067218A (en) * | 2016-11-15 | 2018-05-25 | 中国石油化工股份有限公司 | The preparation method of denitrating catalyst |
| CN108114756A (en) * | 2016-11-29 | 2018-06-05 | 中国石油化工股份有限公司 | A kind of sulfur-containing organic waste gas catalysis oxidation protective agent and its preparation method and application |
| CN110833826A (en) * | 2019-11-19 | 2020-02-25 | 山东中材汽车复合材料有限公司 | Preparation method of composite coating material |
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Application publication date: 20160330 |