CN106732530B - For sintering machine, the Ti-base catalyst of pellet denitrating flue gas and preparation method thereof - Google Patents
For sintering machine, the Ti-base catalyst of pellet denitrating flue gas and preparation method thereof Download PDFInfo
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- CN106732530B CN106732530B CN201611130075.7A CN201611130075A CN106732530B CN 106732530 B CN106732530 B CN 106732530B CN 201611130075 A CN201611130075 A CN 201611130075A CN 106732530 B CN106732530 B CN 106732530B
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- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
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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
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- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/24—Chromium, molybdenum or tungsten
- B01J23/30—Tungsten
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2258/00—Sources of waste gases
- B01D2258/02—Other waste gases
- B01D2258/0283—Flue gases
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- 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
- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
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Abstract
The present invention is directed to sintering machine, pellet smoke characteristic, it provides a kind of for sintering machine, the Ti-base catalyst of pellet denitrating flue gas, the catalyst is using titanium dioxide and sieve and silica-sesquioxide mixture as carrier, using the tungsten oxide and complex rare-earth oxidate containing valuable metal being supported on carrier as active constituent.The invention further relates to the preparation methods of above-mentioned catalyst.Catalyst prepared by the present invention effectively reduces SO2/SO3Between conversion ratio, reduce catalyst activity range of reaction temperature, all have higher denitration efficiency between 120 DEG C -420 DEG C using temperature, and also there is certain anti-metal ion energy, the denitration reaction for sintering, pelletizing flue gas provides suitable catalyst.
Description
Technical field
The invention belongs to catalyst technologies and environmental protection technical field, are related to a kind of technology of preparing of denitrating catalyst,
More particularly to it is a kind of for sintering machine, the Ti-base catalyst of pellet denitrating flue gas and preparation method thereof.
Background technique
Steel and iron industry as key pillars of the national economy industry, while be also the main pollutant emission industry of China it
One.Nitrogen oxides is to be strictly limited discharge in China as one of Air Pollutants.Investigation statistics steel as the result is shown
The NO of sintering, the discharge of pelletizing process in enterpriseXAccount for iron and steel enterprise master operation NOXThe half of total emission volumn.Therefore it controls and reduces and burn
Knot, pelletizing process NOXDischarge be entire steel industry NOXThe key of emission reduction." steel sintering, pelletizing industrial air pollution object row
Put standard " (GB28622-2012) regulation: from January 1st, 2015, existing and newly-built steel enterprise sintering, pelletizing equipment were held
The tightened up discharged nitrous oxides concentration limit value 300mg/m of row3.Though although to have built up flue gas substantially de- for existing iron and steel enterprise in China
Sulphur facility, but be sintered (pelletizing) denitrating flue gas in terms of basic research and engineer application obviously lag.
Currently, the main method of removal of nitrogen oxide is selective catalytic reduction (SCR) gas denitrifying technology, it is extensive
Applied to electric power, Industrial Stoves etc..Denitrating catalyst is the core of SCR denitration technology, special for different flue gases
Point needs the catalyst of different performance, and high performance catalyst is SCR denitrating flue gas high efficiency and stable operation reliability
It is crucial.It is external mainly to utilize activated carbon adsorption, domestic Taiyuan Iron and Steel Co. for the processing of sintering machine, pellet nitrogen oxides in effluent
The technique that group also uses, but since its investment and operating cost are high, it is not widely popularized.And exist at present both at home and abroad
The field is primarily due to the denitrating catalyst not being suitble to there are no especially mature SCR engineering example.
The characteristics of sintering and pelletizing flue gas is: exhaust gas volumn is big, and dust concentration height (predominantly miberal powder), flue-gas temperature generally exists
110~150 DEG C, contain certain density SO2With nitrogen oxides, high oxygen content, water capacity are big, and also containing a large amount of in flue gas
The foreign ions such as chlorine, fluorine and metal ion.It is not mature enough both at home and abroad for the denitrating flue gas processing technique of the feature,
Therefore suitable SCR catalyst is developed for being sintered the application with pelletizing Flue Gas Denitrification Engineering with great practical significance.
So far, studying more mature SCR denitration is vanadium tungsten titanium system, but because catalytic reaction temperature reaches
300 DEG C~400 DEG C, so not applicable for sintering, pelletizing low-temperature denitration of flue gas.And the denitrating catalyst of low temperature there are the problem of
It is that catalyst denitration efficiency is low under cryogenic conditions and SO easily occurs2It is poisoned and causes to inactivate.Therefore to low temperature sulfur resistive, anti-
The preparation of water, anti-metal ionic catalyst is the emphasis of sintering, pelletizing denitrating flue gas.
Summary of the invention
The present invention is directed to sintering machine, pellet smoke characteristic, provides a kind of for sintering machine, pellet denitrating flue gas
Ti-base catalyst, the catalyst is using titanium dioxide and sieve and silica-sesquioxide mixture as carrier, to be supported on the WO on carrier3、
La2O3And CeO2For active constituent.Catalyst prepared by the present invention effectively reduces SO2/SO3Between conversion ratio, reduce catalysis
Agent active reaction temperature range all has higher denitration efficiency using temperature between 120 DEG C~420 DEG C, and wear-resisting property is good, simultaneously
And blocked up with certain sulfur resistive, anti-ash, the ability of anti-metal ion poisoning, it is adapted to the denitration reaction item of sintering, pelletizing flue gas
Part.
Specifically, one aspect of the present invention provides one kind for sintering machine, pellet denitrating flue gas Ti-base catalyst, spy
Sign is that using titanium dioxide and a kind of sieve and silica-sesquioxide mixture as carrier, wherein content of titanium dioxide accounts for urges the catalyst
The 42-84wt% of agent total amount, sieve and silica-sesquioxide content account for the 5-20wt% of catalyst total amount；With WO3、La2O3And CeO2For work
Property ingredient, wherein WO3Account for the 1-8wt% of catalyst total amount, La2O3Account for the 5-15wt% of catalyst total amount, CeO2It is total to account for catalyst
The 5-15wt% of amount；Each ingredient is obtained into La by certain process combining together2O3-CeO2-WO3/TiO2Denitration titanium-based is urged
Agent.
Preferably, wherein content of titanium dioxide accounts for the 70-80wt% of catalyst total amount.
Preferably, sieve and silica-sesquioxide content accounts for the 10-15wt% of catalyst total amount.
Preferably, La2O3Account for the 10wt% of catalyst total amount, CeO2Account for the 10wt% of catalyst total amount.
Another aspect of the present invention a kind of specific preparation method of catalyst is provided characterized by the following steps:
(1) solution of ammonium metatungstate is prepared；
(2) titanium dioxide stirs abundant mashing in deionized water, under stirring, it is resulting partially that step (1) is added
Ammonium tungstate solution；
(3) adding ammonium hydroxide to adjust pH value in the mixture in step (2) is 8~10, is then filtered, deionized water
It washes, drying for standby；
(4) product obtained in step (3) is sequentially added into sieve and silica-sesquioxide, expanding agent, lubricant, reinforcing agent and plastic
Agent is kneaded, and honeycomb is then squeezed into, through drying, calcination process, for use；
(5) mixed solution of lanthanum nitrate and cerous nitrate is prepared；
(6) product that step (4) obtains is sufficiently impregnated in the mixed solution of lanthanum nitrate and cerous nitrate, dipping temperature is
20~60 DEG C, dip time 8~12 hours；
(7) the product utilization ammonium hydroxide that step (6) obtains is handled, and adjusting pH value is 7~9, is carried out at 80~120 DEG C
Dry, drying time is 8~18 hours；Calcination activation is carried out at 300~550 DEG C, calcining time is 3~10 hours, thus
The Ti-base catalyst out of stock for sintering machine, pellet flue gas is just obtained.
Preferably, step (1) are as follows: be configured to oxalic acid solution with oxalic acid and deionized water, ammonium metatungstate be added a certain amount of
Oxalic acid solution in, be stirred until be completely dissolved to obtain ammonium metatungstate solution.
Preferably, step (5) are as follows: weigh the desired amount of lanthanum nitrate and cerous nitrate respectively in dissolving tank, be added a certain amount of
Oxalic acid solution in, dissolution obtain lanthanum nitrate and cerous nitrate mixed solution.
Preferably, drying is to be gradually warmed up the melikaria in step (4), 60-120 hours dry；More preferably
Ground, described be gradually warmed up is gradually warmed up from 45 DEG C to 100 DEG C.
Roasting is in being gradually warmed up roasting 10-20 hours in Muffle furnace in step (4)；It is highly preferred that described be gradually warmed up
It is to be gradually warmed up from 100 DEG C to 500 DEG C.
Preferably, expanding agent described in step (4) and lubricant are sesbania powder.
Preferably, reinforcing agent described in step (4) is glass fibre；The plasticizer is hydroxypropyl methyl fiber
The mixture of one or more of element, polyvinyl alcohol, polyethylene glycol oxide.
Preferably, plasticizer is the mixture of hydroxypropyl cellulose and polyvinyl alcohol, and the proportion of the two is 1:1.
A kind of Ti-base catalyst and preparation method thereof for pellet denitrating flue gas provided by the invention, the skill having
Art advantage is embodied in:
Catalyst use temperature range prepared by 1 be 120~420 DEG C, even if under 200 DEG C of cryogenic conditions below its
Denitration efficiency still can reach 85%, and intensity is big, anti-metal poisoning capability and oxidation resistance are strong, SO2/SO3Between conversion
Shuai≤1%；
2 catalyst use active constituent of the lanthanum cerium mischmetal element as catalyst, reduce traditional toxic active at
Divide V2O5Application, be conducive to environmentally protectiveization of catalyst preparation；It is shared, is improved using two kinds of rare earth elements of cerium and lanthanum simultaneously
Denitration efficiency.
3 present invention use the mixture of titanium dioxide and sieve and silica-sesquioxide for carrier, and prepared catalyst carrier compares table
Area is big, high mechanical strength, and carrier is uniformly mixed with active constituent, so that the catalyst active and excellent is urged with high
Change performance.Meanwhile the present invention uses the mixture of hydroxypropyl cellulose and polyvinyl alcohol that can significantly improve and urge as plasticizer
The uniformity of agent component, and then enhance the catalytic performance of catalyst.
Specific embodiment
It is further specifically described the present invention by the following examples, these embodiments are only used for the purpose illustrated, and
It does not limit the scope of the invention.
Embodiment 1
The oxalic acid solution that a certain amount of oxalic acid is configured to 5% is measured, 46g ammonium metatungstate is added and is dissolved by heating,
Until being completely dissolved；
500g titanium dioxide is weighed, deionized water is added and is stirred；And the inclined tungsten dissolved is added in whipping process
The oxalic acid solution of sour ammonium, stirring and ammonium hydroxide adjusting pH is added dropwise after being sufficiently mixed is 8.8~9.0, after filtering, wash, being dry at 60 DEG C
Obtain the titania support of load tungsten；
Once be added in the titania support for the load tungsten for taking step to obtain 63g sieve and silica-sesquioxide, 6g sesbania powder,
The mixture of 20g glass fibre, 5g hydroxypropyl cellulose and polyvinyl alcohol is kneaded, removes bubble, is then squeezed into
The melikaria is gradually warmed up (45~100 DEG C) dryings 90 hours, then in horse by the honeycomb of 50 × 50 × 200mm
(100~500 DEG C) are not gradually warmed up in furnace to roast 15 hours；
66g lanthanum nitrate hexahydrate and 126g cerium nitrate hexahydrate are weighed respectively, and deionized water is added, adds a certain amount of 5%
Oxalic acid solution, obtain the active mixed solution of lanthanum nitrate and cerous nitrate after completely dissolution；
Roasting catalyst precarsor is placed in above active mixed solution and is impregnated 8 hours, until active element is complete
On section load to carrier；
By impregnation product AMMONIA TREATMENT, so that being placed in roasting in Muffle furnace after pH value is 15 hours dry at 8,100 DEG C
It burns, is roasted 3 hours at 500 DEG C, finally obtain Ti-base catalyst.
Embodiment 2
The oxalic acid solution that a certain amount of oxalic acid is configured to 5% is measured, 37g ammonium metatungstate is added and is dissolved by heating,
Until being completely dissolved；
500g titanium dioxide is weighed, deionized water is added and is stirred；And the inclined tungsten dissolved is added in whipping process
The oxalic acid solution of sour ammonium, stirring and ammonium hydroxide adjusting pH is added dropwise after being sufficiently mixed is 8.8~9.0, after filtering, wash, being dry at 60 DEG C
Obtain the titania support of load tungsten；
Once be added in the titania support for the load tungsten for taking step to obtain 94g sieve and silica-sesquioxide, 8g sesbania powder,
The mixture of 30g glass fibre, 9g hydroxypropyl cellulose and polyvinyl alcohol is kneaded, removes bubble, is then squeezed into
The melikaria is gradually warmed up (45~100 DEG C) dryings 90 hours, then in horse by the honeycomb of 50 × 50 × 200mm
(100~500 DEG C) are not gradually warmed up in furnace to roast 15 hours；
84g lanthanum nitrate hexahydrate and 159g cerium nitrate hexahydrate are weighed respectively, and deionized water is added, adds a certain amount of 5%
Oxalic acid solution, obtain the active mixed solution of lanthanum nitrate and cerous nitrate after completely dissolution；
Roasting catalyst precarsor is placed in above active mixed solution and is impregnated 10 hours, until active element is complete
On section load to carrier；
By impregnation product AMMONIA TREATMENT, so that being placed in roasting in Muffle furnace after pH value is 15 hours dry at 8,100 DEG C
It burns, is roasted 5 hours at 500 DEG C, finally obtain Ti-base catalyst.
Embodiment 3
The oxalic acid solution that a certain amount of oxalic acid is configured to 5% is measured, 23g ammonium metatungstate is added and is dissolved by heating,
Until being completely dissolved；
500g titanium dioxide is weighed, deionized water is added and is stirred；And the inclined tungsten dissolved is added in whipping process
The oxalic acid solution of sour ammonium, stirring and ammonium hydroxide adjusting pH is added dropwise after being sufficiently mixed is 8.8~9.0, after filtering, wash, being dry at 60 DEG C
Obtain the titania support of load tungsten；
Once be added in the titania support for the load tungsten for taking step to obtain 113g sieve and silica-sesquioxide, 10g sesbania powder,
The mixture of 35g glass fibre, 15g hydroxypropyl cellulose and polyvinyl alcohol is kneaded, removes bubble, then squeezed
At the honeycomb of 50 × 50 × 200mm, which is gradually warmed up (45~100 DEG C) dryings 90 hours, then in
(100~500 DEG C) are gradually warmed up in Muffle furnace to roast 15 hours；
100g lanthanum nitrate hexahydrate and 189g cerium nitrate hexahydrate are weighed respectively, and deionized water is added, adds a certain amount of 5%
Oxalic acid solution, obtain the active mixed solution of lanthanum nitrate and cerous nitrate after completely dissolution；
Roasting catalyst precarsor is placed in above active mixed solution and is impregnated 12 hours, until active element is complete
On section load to carrier；
By impregnation product AMMONIA TREATMENT, so that being placed in roasting in Muffle furnace after pH value is 15 hours dry at 8,100 DEG C
It burns, is roasted 10 hours at 500 DEG C, finally obtain Ti-base catalyst.
Embodiment 4
The denitrating flue gas Ti-base catalyst that embodiment 1-3 is prepared carries out catalytic activity test, test temperature 140
DEG C, test its denitration efficiency and SO2/SO3Between conversion ratio, it is as a result as follows:
The activity rating of the prepared catalyst of the present invention of table 1
| Group | Denitrification rate (%) | SO2/SO3Between conversion ratio (%) |
| Embodiment 1 | 80.7 | 0.80 |
| Embodiment 2 | 83.5 | 0.76 |
| Embodiment 3 | 84.6 | 0.73 |
Claims (8)
1. one kind is used for sintering machine, pellet denitrating flue gas Ti-base catalyst, which is characterized in that the catalyst is with titanium dioxide
It is carrier with sieve and silica-sesquioxide mixture, wherein content of titanium dioxide accounts for the 42-84wt% of catalyst total amount, and sieve and silica-sesquioxide contains
Amount accounts for the 5-20wt% of catalyst total amount；With WO3、La2O3And CeO2For active constituent, wherein WO3Account for the 1- of catalyst total amount
8wt%, La2O3Account for the 5-15wt% of catalyst total amount, CeO2Account for the 5-15wt% of catalyst total amount；
It is described for sintering machine, pellet denitrating flue gas Ti-base catalyst preparation method the following steps are included:
(1) solution of ammonium metatungstate is prepared；
(2) titanium dioxide stirs abundant mashing in deionized water, under stirring, step (1) resulting metatungstic acid is added
Ammonium salt solution；
(3) adding ammonium hydroxide to adjust pH value in the mixture in step (2) is 8~10, is then filtered, deionization washing, does
It is dry spare；
(4) product obtained in step (3) is sequentially added into sieve and silica-sesquioxide, expanding agent, lubricant, reinforcing agent and plasticizer,
It is kneaded, is then squeezed into honeycomb, through drying, calcination process, for use；
(5) mixed solution of lanthanum nitrate and cerous nitrate is prepared；
(6) product that step (4) obtains is sufficiently impregnated in the mixed solution of lanthanum nitrate and cerous nitrate, dipping temperature be 20~
60 DEG C, dip time 8~12 hours；
(7) the product utilization ammonium hydroxide that step (6) obtains is handled, and adjusting pH value is 7~9, is done at 80~120 DEG C
Dry, drying time is 8~18 hours；Calcination activation is carried out at 300~550 DEG C, calcining time is 3~10 hours, thus
The Ti-base catalyst for sintering machine, pellet denitrating flue gas is obtained.
2. being used for sintering machine, pellet denitrating flue gas Ti-base catalyst as described in claim 1, wherein content of titanium dioxide is accounted for
The 70-80wt% of catalyst total amount.
3. being used for sintering machine, pellet denitrating flue gas Ti-base catalyst as described in claim 1, wherein sieve and silica-sesquioxide content
Account for the 10-15wt% of catalyst total amount.
4. being used for sintering machine, pellet denitrating flue gas Ti-base catalyst as described in claim 1, wherein La2O3It is total to account for catalyst
The 10wt% of amount, CeO2Account for the 10wt% of catalyst total amount.
5. being used for sintering machine, pellet denitrating flue gas Ti-base catalyst as described in claim 1, wherein step (1) are as follows: with grass
Acid is configured to oxalic acid solution with deionized water, and ammonium metatungstate is added in a certain amount of oxalic acid solution, is stirred until completely
Dissolution obtains ammonium metatungstate solution.
6. being used for sintering machine, pellet denitrating flue gas Ti-base catalyst as described in claim 1, wherein step (5) are as follows: respectively
The desired amount of lanthanum nitrate and cerous nitrate are weighed in dissolving tank, is added in a certain amount of oxalic acid solution, dissolution obtain lanthanum nitrate with
Cerous nitrate mixed solution.
7. being used for sintering machine, pellet denitrating flue gas Ti-base catalyst, expansion described in step (4) as described in claim 1
Hole agent and lubricant are sesbania powder.
8. being used for sintering machine, pellet denitrating flue gas Ti-base catalyst, increasing described in step (4) as described in claim 1
Strong agent is glass fibre；The plasticizer is one of hydroxypropyl methyl cellulose, polyvinyl alcohol, polyethylene glycol oxide or several
The mixture of kind.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105148904A (en) * | 2015-08-28 | 2015-12-16 | 武汉京运通环保工程有限公司 | Flue gas denitration catalyst applied at a low temperature and preparation method thereof |
| CN105618029A (en) * | 2015-12-30 | 2016-06-01 | 华电青岛环保技术有限公司 | SCR (Selective Catalytic Reduction) denitration catalyst coated with rare earth and preparation method thereof |
| CN106140144A (en) * | 2016-06-28 | 2016-11-23 | 攀枝花学院 | SCR denitration and preparation method thereof |
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| JP2005246341A (en) * | 2004-03-08 | 2005-09-15 | Babcock Hitachi Kk | Catalyst for removing nitrogen oxides, its production method, and method of removing nitrogen oxides using the catalyst |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105148904A (en) * | 2015-08-28 | 2015-12-16 | 武汉京运通环保工程有限公司 | Flue gas denitration catalyst applied at a low temperature and preparation method thereof |
| CN105618029A (en) * | 2015-12-30 | 2016-06-01 | 华电青岛环保技术有限公司 | SCR (Selective Catalytic Reduction) denitration catalyst coated with rare earth and preparation method thereof |
| CN106140144A (en) * | 2016-06-28 | 2016-11-23 | 攀枝花学院 | SCR denitration and preparation method thereof |
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Granted publication date: 20190913 Termination date: 20191209 |