CN106582615A - Preparation method for low-temperature V-W-TiO2 based selective reduction catalyst - Google Patents
Preparation method for low-temperature V-W-TiO2 based selective reduction catalyst Download PDFInfo
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- CN106582615A CN106582615A CN201611069102.4A CN201611069102A CN106582615A CN 106582615 A CN106582615 A CN 106582615A CN 201611069102 A CN201611069102 A CN 201611069102A CN 106582615 A CN106582615 A CN 106582615A
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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
- B01D53/92—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
- B01D53/9418—Processes characterised by a specific catalyst for removing nitrogen oxides by selective catalytic reduction [SCR] using a reducing agent in a lean exhaust gas
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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
- B01D2258/01—Engine exhaust 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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02T—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO TRANSPORTATION
- Y02T10/00—Road transport of goods or passengers
- Y02T10/10—Internal combustion engine [ICE] based vehicles
- Y02T10/12—Improving ICE efficiencies
Abstract
The invention discloses a preparation method for a low-temperature V-W-TiO2 based selective reduction catalyst. The method comprises the following steps of weighing ammonium metatungstate, ammonium metavanadate, cerous nitrate, oxalic acid powder, zirconium acetate and de-ionized water; performing kneading, drying, grinding and roasting to obtain V-Ce-Zr-W-TiO2 powder; mixing the V-Ce-Zr-W-TiO2 powder, silica sol and the de-ionized water; performing ball-milling, dipping and drying; and finally performing roasting to obtain the catalyst. According to the method, the addition of the cerous nitrate facilitates the dispersion of WO3 and improves the oxygen storage capacity of the catalyst; the addition of the zirconium acetate improves the effect of CeO2; and the synergistic effect of CeO2-ZrO2 and WO3 can facilitate the dispersity of V2O5 on the surface of TiO2, so that the prepared V-W-TiO2 based selective reduction catalyst has the advantages that the low-temperature activity is good, the initiation temperature is lower than 190 DEG C, and the like, and is especially suitable for purification of NOx in diesel exhaust gas.
Description
Technical field
The present invention relates to the technical field of diesel car tail gas refining, more particularly to a kind of low form V-W-TiO2Base is selected
The preparation method of property reducing catalyst.
Background technology
Along with the continuous progress of society, the paces of economic and technical sustainable development, the motor vehicles industry of China is in recent years
Constantly develop and grow to be also able to, the volume of production of its motor vehicles, the growth all continuously and healthily of sales volume and recoverable amount, diesel oil
, with dynamic property is strong, the significant advantage such as fuel economy is good, the thermal efficiency is high compared with gasoline engine, its distribution market is from friendship for machine
Logical field expands to other industry, and proportion is increasing.But diesel engine ratio be significantly increased also give environment band
Many negative impacts are carried out, serious pollution problem have been caused to atmospheric environment.NOx and PM are that the primary discharge of diesel engine is dirty
Dye thing, wherein NOx is one of major pollutants of air, and forms the main matter of photochemical fog；And PM particulate matters, it is special
It is not fine particle such as PM2.5, has become the focus paid close attention in recent years, it is that the chief-criminal for causing each city haze weather brings disaster upon
It is first.In recent years, the pollution problem for solving oxynitride generation in exhaust gas from diesel vehicle is paid much attention to by each side, tail gas
Catalytic purification method has been obtained for being widely applied as a kind of effective means for reducing exhaust pollution.For China's actual conditions and
Oil product situation, vanadio NH3- SCR catalyst has been obtained for most commonly used application.But state more than four is met on the market at present
The vanadia-based SCR catalysts of discharge standard have the shortcomings that low temperature active is undesirable.
The content of the invention
The purpose of the present invention is in view of the shortcomings of the prior art, there is provided a kind of low form V-W-TiO2Based selective is also
The preparation method of raw catalyst (SCR), with the shortcoming for overcoming catalyst low-temperature activity in prior art poor.
For achieving the above object, the technical solution used in the present invention is as follows：
A kind of low form V-W-TiO2The preparation method of based selective reducing catalyst, it is characterised in that including following step
Suddenly：
1) according to TiO2Solution weight needed for incipient impregnation is calculated, and is weighed ammonium metatungstate, cerous nitrate and acetic acid zirconium and is added
Enter in deionized water, after being completely dissolved, form ammonium metatungstate solution and cerium zirconium aqueous solution；
2) according to W-TiO2Solution weight needed for incipient impregnation is calculated, and is weighed ammonium metavanadate and is added to deionized water
In, add the oxalic acid powder of 98% mass fraction, stirring reaction to form ammonium metavanadate solution for a period of time afterwards after heating for dissolving；
3) in kneader, by above-mentioned steps, 1) the middle ammonium metatungstate aqueous solution for preparing is slowly added to TiO2It is middle to mediate
It is even；
4) by above-mentioned steps, 1) the middle cerium zirconium aqueous solution for preparing is slowly added to the TiO after step (3) dipping2In, mediate equal
It is even；
5) wet mash for 4) obtaining above-mentioned steps is dried, crushing and roasting obtain Ce-Zr-W-TiO2Powder；
6) in kneader, by above-mentioned steps, 2) the middle ammonium metavanadate solution for preparing is slowly added to above-mentioned Ce-Zr-W-TiO2
Mediate in powder powder uniform；
7) by above-mentioned steps 6) in the wet mash that obtains be dried, crush and roasting obtains V-Ce-Zr-W-TiO2Powder；
8) weigh above-mentioned V-Ce-Zr-W-TiO2The mixing of powder, Ludox and deionized water, ball milling obtain coating paste；
9) ceramic honey comb is impregnated into into step 8) in prepare coating paste in, remaining slurry in duct is blown after taking-up,
Repeated impregnations and drying, last roasting obtain final product monoblock type selective reduction (SCR) catalyst.
Wherein, step 1) described in ammonium metatungstate with WO3Weight is calculated, 8-12% of the addition for titanium dioxide weight；
Cerous nitrate is with CeO2Weight is calculated, 1-3% of the addition for titanium dioxide weight, and acetic acid zirconium is with ZrO2Weight is calculated, CeO2With ZrO2
Mol ratio is 1:3-1:6.
Step 2) described in ammonium metavanadate with V2O5Weight is calculated, addition for titanium dioxide weight 3%, ammonium metavanadate
Weight ratio with oxalic acid is 1:1.5-2.0.
Step 3) described in kneading time be 60-75min.
Step 4) described in kneading time be 60-75min.
Step 5) described in baking temperature be 70-100 DEG C, drying time is 20-24h；Sintering temperature is 500-550
DEG C, roasting time is 2-3h.
Step 6) described in kneading time be 60-75min.
Step 7) described in baking temperature be 70-100 DEG C, drying time is 20-24h；Sintering temperature is 500-550
DEG C, roasting time is 2-3h.
Step 8) described in Ludox with SiO2Calculate, addition is V-W-TiO2The 8-12% of grain weight amount, Ball-milling Time
For 2-4h.
Step 9) described in baking temperature be 70-100 DEG C, drying time is 20-24h；500-550 DEG C of sintering temperature,
Roasting time is 2-3h.
The present invention obtains the modified V-W- of cerium zirconium using the mode of uploading of the active component for mediating batch mixing incipient impregnation
TiO2Powder.Being added with for cerous nitrate is beneficial to promote WO3Dispersion, improve the oxygen storage capacity of catalyst, the addition of acetic acid zirconium is favourable
In enhancing CeO2Effect；CeO2-ZrO2With WO3Synergism can promote TiO2Surface V2O5Dispersibility, therefore be obtained
V-W-TiO2Base SCR catalyst has good low temperature active.
Specific embodiment
For the clearer explanation present invention, following 8 groups of embodiments are enumerated：
A kind of low form V-W-TiO2The preparation method of based selective reducing catalyst, comprises the following steps：
1) according to TiO2Solution weight needed for incipient impregnation is calculated, and is weighed ammonium metatungstate, cerous nitrate and acetic acid zirconium and is added
Enter in deionized water, after being completely dissolved, form ammonium metatungstate solution and cerium zirconium aqueous solution；
2) according to W-TiO2Solution weight needed for incipient impregnation is calculated, and is weighed ammonium metavanadate and is added to deionized water
In, add the oxalic acid powder of 98% mass fraction, stirring reaction to form ammonium metavanadate solution for a period of time afterwards after heating for dissolving；
In kneader, by above-mentioned steps, 1) the middle ammonium metatungstate aqueous solution for preparing is slowly added to TiO2It is middle to mediate uniformly；
4) by above-mentioned steps, 1) the middle cerium zirconium aqueous solution for preparing is slowly added to the TiO after above-mentioned incipient impregnation2Middle kneading
Uniformly；
5) wet mash for 4) obtaining above-mentioned steps is dried, crushing and roasting obtain Ce-Zr-W-TiO2Powder；
6) in kneader, by above-mentioned steps, 2) the middle ammonium metavanadate solution for preparing is slowly added to above-mentioned Ce-Zr-W-TiO2
Mediate in powder powder uniform；
7) by above-mentioned steps 6) in the wet mash that obtains be dried, crush and roasting obtains V-Ce-Zr-W-TiO2Powder；
8) weigh above-mentioned V-Ce-Zr-W-TiO2The mixing of powder, Ludox and deionized water, ball milling obtain coating paste；
9) ceramic honey comb is impregnated into into step 8) in prepare coating paste in, remaining slurry in duct is blown after taking-up,
Repeated impregnations and drying, last roasting obtain final product monoblock type selective reduction (SCR) catalyst.
Wherein, the various process parameters of embodiment 1-8 are as shown in table 1.
Table 1：
Wherein embodiment 7, the Ludox adopted in 8 are the Ludox of improvement, are particularly well-suited to the preparation of catalyst.
Described in embodiment 7, the preparation method of Ludox is：
1. prepared by active silicic acid：The industrial metasilicate that modulus is 2.2 is added water and is configured to the silicon of dioxide-containing silica 6wt%
Acid sodium aqueous solution, is added in retort, is stirred with 120 revs/min of speed；Industrial sulphuric acid is added water and is configured to 10wt%
Sulfuric acid solution, be added in above-mentioned sodium silicate aqueous solution with the speed of 450ml/min, until pH be 9.2, heat up 95 DEG C insulation
Obtain within 1 hour Ludox bottom liquid；The industrial metasilicate that modulus is 3.2 is added water and is configured to the sodium silicate water of silicon dioxide 7wt%
Solution, carries out ion exchange using storng-acid cation exchange resin, and the pH value after controlling to exchange is 2.5, and silicic acid is obtained；
2. micelle increases：By the silicic acid of above-mentioned preparation, the Ludox bottom liquid of above-mentioned preparation is added with the speed of 200ml/min
In, period is slowly added to the sodium silicate adjustment pH value of concentration 4wt% and keeps final pH to be 9.2, and at 90 DEG C, insulation 1 is little
When, and room temperature is cooled to, obtain Ludox；The Ludox of above-mentioned preparation is carried out into ion by storng-acid cation exchange resin
Exchange, the pH after keeping exchanging is 1.5, and dioxide-containing silica is 42wt%, added containing NH while stirring330% ammonia is to PH
It is worth for 9.2, obtains alkaline silica sol.
3. dilute concentrating silica：Polyethylene glycol 6000 and penetrating agent AEP are added in alkaline silica sol obtained above, wherein
The weight ratio of polyethylene glycol 6000 and penetrating agent AEP is 1:1,1.2wt% of the addition for Ludox bottom liquid silicon dioxide；
Ludox, Ludox mean diameter 20nm, sodium ions content 0.039%, concentration 41%, viscosity is obtained using being concentrated by ultrafiltration
14cps, dioxide-containing silica are 29.7%, and pH value is 9.2.
Above-mentioned Ludox impurity content is low, average particle size distribution is narrow, viscosity is less, stable in higher concentrations, particularly suitable
In the production of catalyst.
Described in embodiment 8, the preparation method of Ludox is：
1. the activation of silica flour：The silica flour for weighing 50 parts of 200 mesh is added to 1000 parts of deionized water hot-water soak 30min and makes
Activation, obtain the solution of dilute cream shape.
2. hydration reaction：The solution of above-mentioned dilute cream shape is added to into the ammonia containing 5 part 25%, 50 part of 2.5 modulus points for 3 times
In the retort of the aqueous solution of industrial metasilicate, it is stirred and heats with 120 revs/min of speed, 90 DEG C of reaction 8h.
3. sucking filtration：Unreacted silica flour is removed by the method for sucking filtration, Ludox is obtained；
4. surface is modified：Add 5 parts of aminopropyl trimethoxysilanes to carry out surface to be modified in Ludox obtained above,
And the pH value for adjusting the Ludox with ammonia is adjusted to 9.5.Ludox mean diameter 23nm, concentration 40%, viscosity 15cps,
Dioxide-containing silica is 28%, and pH value is 9.5.
The addition of industrial metasilicate in the present embodiment can improve the content of Ludox, and the addition of ammonia can then be accelerated
The carrying out of reaction.SiO in Ludox internal system obtained in this method2Content it is higher, while the uniform component of Ludox, point
Cloth is uniform, and long-term stablizing can be kept during preservation.
Initiation temperature test result of the table 2 for catalyst obtained in the inventive method
Table 2
From table 2 it can be seen that a kind of low form V-W-TiO of the present invention2Based selective reduces the preparation of (SCR) catalyst
Method, in the case where the consumption of vanadium is relatively low, initiation temperature is less than 190 DEG C to the integral catalyzer which is prepared, with good
Low temperature active；
Above presently preferred embodiments of the present invention is described.It is to be appreciated that the invention is not limited in above-mentioned
Particular implementation, wherein the equipment and structure that do not describe in detail to the greatest extent are construed as giving reality with the common mode in this area
Apply；Any those of ordinary skill in the art, under without departing from technical solution of the present invention ambit, all using the disclosure above
Methods and techniques content make many possible variations and modification to technical solution of the present invention, or be revised as equivalent variations etc.
Effect embodiment, this has no effect on the flesh and blood of the present invention.Therefore, every content without departing from technical solution of the present invention, foundation
The technical spirit of the present invention still falls within the present invention to any simple modification made for any of the above embodiments, equivalent variations and modification
In the range of technical scheme protection.
Claims (10)
1. a kind of low form V-W-TiO2The preparation method of based selective reducing catalyst, it is characterised in that comprise the following steps：
1) according to TiO2Solution weight needed for incipient impregnation is calculated, and is weighed ammonium metatungstate, cerous nitrate and acetic acid zirconium and is added to
In ionized water, ammonium metatungstate solution and cerium zirconium aqueous solution after being completely dissolved, are formed；
2) according to W-TiO2Solution weight needed for incipient impregnation is calculated, and is weighed ammonium metavanadate and is added in deionized water, is heated
The oxalic acid powder of 98% mass fraction is added after dissolving, ammonium metavanadate solution after stirring reaction, is formed；
3) in kneader, by above-mentioned steps, 1) the middle ammonium metatungstate aqueous solution for preparing is slowly added to TiO2It is middle to mediate uniformly；
4) by above-mentioned steps, 1) the middle cerium zirconium aqueous solution for preparing is slowly added to the TiO after above-mentioned incipient impregnation2It is middle to mediate uniformly；
5) wet mash for 4) obtaining above-mentioned steps is dried, crushing and roasting obtain Ce-Zr-W-TiO2Powder；
6) in kneader, by above-mentioned steps, 2) the middle ammonium metavanadate solution for preparing is slowly added to above-mentioned Ce-Zr-W-TiO2In powder
Mediate uniform；
7) by above-mentioned steps 6) in the wet mash that obtains be dried, crush and roasting obtains V-Ce-Zr-W-TiO2Powder；
8) weigh above-mentioned V-Ce-Zr-W-TiO2The mixing of powder, Ludox and deionized water, ball milling obtain coating paste；
9) ceramic honey comb is impregnated into into step 8) in prepare coating paste in, remaining slurry in duct is blown after taking-up, repeat
Impregnate and be dried, last roasting obtains final product monoblock type selective reduction (SCR) catalyst.
2. a kind of low form V-W-TiO according to claim 12The preparation method of based selective reducing catalyst, its feature
It is：Step 1) described in ammonium metatungstate with WO3Weight is calculated, 8-12% of the addition for titanium dioxide weight；Cerous nitrate with
CeO2Weight is calculated, 1-3% of the addition for titanium dioxide weight, and acetic acid zirconium is with ZrO2Weight is calculated, CeO2With ZrO2Mol ratio is
1:3-1:6。
3. a kind of low form V-W-TiO according to claim 12The preparation method of based selective reducing catalyst, its feature
It is：Step 2) described in ammonium metavanadate with V2O5Weight is calculated, and addition is the 3% of titanium dioxide weight, ammonium metavanadate and grass
The weight ratio of acid is 1:1.5-1:2.0.
4. a kind of low form V-W-TiO according to claim 12The preparation method of based selective reducing catalyst, its feature
It is：Step 3) described in kneading time be 60-75min.
5. a kind of low form V-W-TiO according to claim 12The preparation method of based selective reducing catalyst, its feature
It is：Step 4) described in kneading time be 60-75min.
6. a kind of low form V-W-TiO according to claim 12The preparation method of based selective reducing catalyst, its feature
It is：Step 5) described in baking temperature be 70-100 DEG C, drying time is 20-24h；Sintering temperature is 500-550 DEG C, roasting
The burning time is 2-3h.
7. a kind of low form V-W-TiO according to claim 12The preparation method of based selective reducing catalyst, its feature
It is：Step 6) described in kneading time be 60-75min.
8. a kind of low form V-W-TiO according to claim 12The preparation method of based selective reducing catalyst, its feature
It is：Step 7) described in baking temperature be 70-100 DEG C, drying time is 20-24h；Sintering temperature is 500-550 DEG C, roasting
The burning time is 2-3h.
9. a kind of V-W-TiO according to claim 12The preparation method of base selecting property reducing catalyst, it is characterised in that：Step
It is rapid 8) described in Ludox with SiO2Calculate, addition is V-W-TiO2The 8-12% of grain weight amount, Ball-milling Time are 2-4h.
10. a kind of low form V-W-TiO according to claim 12The preparation method of based selective reducing catalyst, which is special
Levy and be：Step 9) described in baking temperature be 70-100 DEG C, drying time is 20-24h；500-550 DEG C of sintering temperature, roasting
The burning time is 2-3h.
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Cited By (5)
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| CN107930659A (en) * | 2017-12-01 | 2018-04-20 | 延海港 | A kind of mesoporous F, Ce codope SCR catalyst |
| CN111036229A (en) * | 2019-11-15 | 2020-04-21 | 十堰汇铂环境科技有限公司 | Low-temperature V2O5-WO3/TiO2NH3Selective reduction catalytic NO catalyst and preparation method thereof |
| CN111097442A (en) * | 2019-12-11 | 2020-05-05 | 西南化工研究设计院有限公司 | Flue gas synergistic denitration and demercuration catalyst and preparation method thereof |
| CN112403485A (en) * | 2020-11-19 | 2021-02-26 | 高化学（江苏）化工新材料有限责任公司 | V/Cu/B/W-TiO2-ZrO2Production method of composite low-temperature denitration catalyst |
| CN112403486A (en) * | 2020-11-19 | 2021-02-26 | 高化学（江苏）化工新材料有限责任公司 | V/Cu/B/W-TiO2-ZrO2Composite low-temperature denitration catalyst and preparation method thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107930659A (en) * | 2017-12-01 | 2018-04-20 | 延海港 | A kind of mesoporous F, Ce codope SCR catalyst |
| CN107930659B (en) * | 2017-12-01 | 2020-12-01 | 合肥中亚环保科技有限公司 | Mesoporous F, Ce co-doped SCR catalyst |
| CN111036229A (en) * | 2019-11-15 | 2020-04-21 | 十堰汇铂环境科技有限公司 | Low-temperature V2O5-WO3/TiO2NH3Selective reduction catalytic NO catalyst and preparation method thereof |
| CN111097442A (en) * | 2019-12-11 | 2020-05-05 | 西南化工研究设计院有限公司 | Flue gas synergistic denitration and demercuration catalyst and preparation method thereof |
| CN111097442B (en) * | 2019-12-11 | 2021-06-15 | 西南化工研究设计院有限公司 | Flue gas synergistic denitration and demercuration catalyst and preparation method thereof |
| CN112403485A (en) * | 2020-11-19 | 2021-02-26 | 高化学（江苏）化工新材料有限责任公司 | V/Cu/B/W-TiO2-ZrO2Production method of composite low-temperature denitration catalyst |
| CN112403486A (en) * | 2020-11-19 | 2021-02-26 | 高化学（江苏）化工新材料有限责任公司 | V/Cu/B/W-TiO2-ZrO2Composite low-temperature denitration catalyst and preparation method thereof |
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