CN106475128B - A kind of preparation method of industrial waste gas purifying catalyst - Google Patents
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Abstract
The present invention provides a kind of preparation methods of industrial waste gas purifying catalyst, it can be improved the anti-sintering property of catalyst, and improve catalytic activity, the following steps are included: 1) by aluminium isopropoxide, and one or more of alkaline earth precursor, rare earth precursor, transition metal precursor, it is dissolved in solvent；2) activated alumina, silicon nitride, dispersing agent is added, is stirred, forms suspension slurry；3) coating forms catalyst coatings on a catalyst support, dry；4) it is placed in the reducing atmosphere of flowing and roasts；5) noble metal solution impregnated is immersed, dry, roasting, maturing temperature is 400~700 DEG C, forms final products.
Description
[technical field]
The present invention relates to waste gas purification fields more particularly to a kind of industrial waste gas purifying catalyst and preparation method thereof.
[background technique]
It is well known that industrial waste gas (such as volatile organic matter (VOCs)) and vehicle exhaust (such as carbon monoxide, hydrocarbonization
Close object and nitrogen oxides etc.) be atmosphere pollution main source.Motor-vehicle tail-gas due to three-way catalyst development and application
It is substantially purified, VOCs, which becomes, causes one of main factor of atmosphere pollution.From chemical industry, electronics industry, printer
The industrial process such as industry, paint and coating, boiler of power plant tail gas and construction material, finishing material, the binder of furniture, kitchen oil
The daily lifes such as cigarette discharge organic matter (as lower carbon number hydrocarbons, aromatic hydrocarbons, alcohol, ketone, ether, ester, aldehyde, carboxylic acid, amine and containing halogen and sulfur-bearing
Organic matter etc.) it is most there is toxicity, foul smell and inflammable and explosive, VOCs be discharged into after atmosphere be also possible to generate toxicity it is bigger
Photochemical fog.Since VOCs pollutes, wide, harm is big, complex in composition, difficulty of governance is big, studies the control and improvement pair of VOCs
It is of great significance in human social.The purification treatment technology of VOCs have become environmental catalysis field one grinds
Study carefully hot spot.
Currently, catalysis method be acknowledged as it is most effective and have huge applications prospect thorough elimination VOCs means it
One.It burns and is handled in VOCs exhaust gas technology in catalysis, the superiority and inferiority of catalyst has decisive influence to treatment effeciency and energy consumption.Cause
This finds high activity, the catalyst of high thermal stability is always the research hotspot of low-temperature catalytic oxidation VOCs.Traditional catalyst
There are noble metal catalyst and transition-metal catalyst.Carried noble metal (Pd, Pt, Ag etc.) catalyst is living with good low temperature
Property, but it is expensive, and active component is volatile, is sintered and is poisoned.Low in cost, the master of catalyst of transition metal oxide
It is used for medium temperature catalysis oxidation, however its anti-poisoning and sintering character to be poor.Common oxide and perovskite structure composite oxygen
Compound catalyst equally exists the defect of easy-sintering inactivation.
[summary of the invention]
The object of the present invention is to provide a kind of preparation methods of industrial waste gas purifying catalyst, can be improved catalyst
Anti-sintering property, and improve catalytic activity.
The technical scheme is that
A kind of preparation method of industrial waste gas purifying catalyst, which comprises the following steps:
1) by one of aluminium isopropoxide and alkaline earth precursor, rare earth precursor, transition metal precursor
Or it is several, it is dissolved in solvent, obtains metal salt precursor solution；
2) activated alumina, silicon nitride, dispersing agent is added in the metal salt precursor solution that step 1) obtains, stirring is mixed
It closes, forms suspension slurry；
3) the suspension slurry coating that step 2) obtains is formed into catalyst coatings on a catalyst support, it is dry to water content
Less than or equal to 3%, dry presoma is obtained；
4) the drying presoma that step 3) obtains is placed in the reducing atmosphere of flowing and is roasted, roasted at 500~600 DEG C
0.5~2h is burnt, in 1000~1400 DEG C of 2~6h of roasting, obtains pretreatment body；
5) the pretreatment body that step 4) obtains is immersed in the precious metal solution of 0.01~0.3mol/L, dipping 5~
10min, dry, roasting, maturing temperature are 400~700 DEG C, form final products.
Further, above-mentioned steps 1) in alkaline earth precursor be barium nitrate, barium acetate, strontium nitrate, calcium nitrate, vinegar
Sour magnesium or magnesium nitrate；Rare earth precursor is lanthanum nitrate, lanthanum acetate, cerous nitrate, cerous acetate, yttrium nitrate, acetic acid yttrium；Transition gold
Category predecessor is manganese nitrate, manganese acetate, cobalt nitrate, cobalt acetate, ferric nitrate, ferric acetate, iron chloride.
Further, alkaline-earth metal in above-mentioned metal salt precursor solution, rare earth metal, transition metal ions concentration it
With for 0.01~0.1mol/L, the additional amount of aluminium isopropoxide is that alkaline-earth metal, rare earth metal, the molal quantity of transition metal ions are total
With.
Further, above-mentioned steps 2) in silicon nitride be α-siliconnitride or nm amorphous silicon nitride.α-siliconnitride or
The reactivity of nm amorphous silicon nitride is high, is conducive to improve Si-N key to the substitution amount of Al-O key.
Further, above-mentioned steps 2) in the additional amount of silicon nitride be 0.9~1.1 times of aluminium isopropoxide molal quantity, it is living
Property aluminium oxide additional amount be alkaline-earth metal, 9.5~10.5 times of molal quantity summation of rare earth metal, transition metal ions.
Further, above-mentioned steps 2) in dispersing agent be that Sodium Polyacrylate, sodium polycarboxylate or phenylethylene-maleic anhydride are total
The one or more of polymers, naphthalenesulfonate antiprecipitant.Dispersing agent precipitates suspension stabilization not, is conducive to mentioning for uniformity
It is high.
Further, the additional amount of above-mentioned dispersing agent is the 0.1~1% of activated alumina and silicon nitride powder weight.
Further, above-mentioned steps 3) drying be freeze-drying, pressure be 10~40Pa.Freeze-drying is to utilize moisture
Distillation achieve the purpose that it is dry, it is dry after small product size it is constant, loose porous, it is not easy to crack or fall off.
Further, above-mentioned steps 3) in catalyst coatings with a thickness of 0.2~2 μm.
Further, above-mentioned steps 5) precious metal solution in sodium citrate or citric acid containing 0.01~0.3mol/L
Potassium or potassium acetate or sodium oxalate.
The present invention can generate following beneficial technical effect:
(1) catalyst prepared by the present invention is part Al-O key (chemical formula is by hexa-aluminate that Si-N key replaces
AAl12O19, A is metal) and noble metal composite catalyst；Si-N key and Al-O key have similar bond distance and bond energy, therefore Si-
N key can replace the part Al-O key in hexa-aluminate structure and maintain stable structure constant, and still, the introducing of Si-N key can increase
Add the Lacking oxygen defect of hexa-aluminate structure, provides a large amount of active sites for the absorption of gas phase oxygen molecule, it is anti-to increase adsorption
It answers, improves catalytic activity；Meanwhile uniformly existing Lacking oxygen is also beneficial to improve the expansion of atom or ion in lattice in structure
Rate is dissipated, the reactivity of Lattice Oxygen is further increased, greatly improves rate of catalysis reaction, improves catalytic activity.
(2) catalyst Si-N key prepared by the present invention replaces the part Al-O key in hexa-aluminate structure, due to Si-N key
Bond energy be greater than the bond energy of Al-O key, therefore, to carried metal to contain overall stability stronger, can be by carried metal beam
Be tied in certain space, substantially reduce various loaded noble metal catalysts in practical the sintering from carrier itself and lead
The catalyst deactivation of cause improves the anti-sintering property of catalyst.
(3) present invention utilizes isopropyl using activated alumina and aluminium isopropoxide as the silicon source for forming hexa-aluminate structure
Aluminium alcoholates is decomposed to form porous network shape aluminium, it can be made to be dispersed in wherein with other reacted constituents, increases the uniform of structure
Property, the Si-N key substitution that the addition of especially silicon nitride generates, substitution amount is high, product good crystallinity, uses part low cost
Activated alumina appropriate can reduce cost, overall cost and effect.
(4) present invention using freeze-drying and unconventional heat drying, achieved the purpose that using water sublimed it is dry, do
Small product size after dry is constant, loose porous, not easy to crack not adding additives or surface modifier or fall off, Neng Gouti
Uniformity of the high catalyst activity site on atomic level improves catalytic activity, reduces active layer thickness, reduces dosage.
(5) roasting can guarantee that Si-N key is successfully entered six aluminic acids using the reducing atmosphere of flowing to the present invention for the first time
The structure of salt and it is not oxidized, the N/O ratio of product maintains 5% or more, once and Si-N key enter form hexa-aluminate
Crystal structure, then it is sufficiently stable, all will not be oxidized in subsequent after baking and high temperature real-world environment, maintain stablize and
Effective catalysis.
[specific embodiment]
Below in conjunction with specific embodiment, the present invention is described further.
Embodiment provided below is not intended to limit the invention covered range, and described step is also not use
Sequence is executed to limit its.Those skilled in the art combine existing common knowledge to do conspicuous improvement to the present invention, also fall
Enter the present invention claims protection scope within.
Embodiment one
A kind of preparation method of industrial waste gas purifying catalyst, which comprises the following steps:
1) aluminium isopropoxide, strontium nitrate, cerous nitrate is soluble in water, obtaining Al concentration is that 0.02mol/L, Sr concentration are
0.01mol/L, Ce concentration are the metal salt precursor solution of 0.01mol/L；
Activated alumina, silicon nitride, dispersing agent Sodium Polyacrylate is added in the metal salt precursor solution that step 1) obtains,
The additional amount of silicon nitride is 0.9~1.1 times of aluminium isopropoxide molal quantity, and the additional amount of activated alumina is mole of Sr and Ce
9.5~10.5 times of number summation, the additional amount of dispersing agent Sodium Polyacrylate are the 0.1 of activated alumina and silicon nitride powder weight
~1%, it is stirred, forms suspension slurry；
2) the suspension slurry coating obtained step 2) forms the coating of 0.2~2 μ m-thick of catalysis on a catalyst support,
Freeze-drying, pressure is 10~40Pa, until water content is less than or equal to 3%, obtains dry presoma；
3) the drying presoma that step 3) obtains is placed in the nitrogen atmosphere of flowing and is roasted, roasted at 500~600 DEG C
0.5~2h obtains pretreatment body in 1000~1400 DEG C of 2~6h of roasting；
4) the pretreatment body that step 4) obtains is immersed in the precious metal solution of 0.01~0.3mol/L, the precious metal solution
In the sodium citrate containing 0.01~0.3mol/L, impregnate 5~10min, dry, roasting, maturing temperature is 400~700 DEG C, shape
At final products.
Through detecting, the N/O ratio in catalyst is 6.3%, illustrates that Si-N key is stable in the presence of in structure；Extremely by the catalyst
In internal diameter be 6mm reaction tube in, using dimethylbenzene, toluene and phenyl methylcarbamate as organic contamination source, respectively adjusting dimethylbenzene, toluene and
The carrier gas flux of gas circuit, makes its concentration respectively reach 1000mg/m where phenyl methylcarbamate3、3000mg/m3、5000mg/m3, react wet
Degree is 30%RH, and it is that reaction velocity reaches 110000h that air mixed gas flow, which is 300ml/min, in reaction-1.The result shows that urging
Above-mentioned exhaust gas complete catalysts oxidation can be carbon dioxide and water in 600 DEG C by agent；Under identical test environment, pass through
Obviously inactivating do not occur in 300 DEG C, 600h stability test, catalyst.
Embodiment two
A kind of preparation method of industrial waste gas purifying catalyst, which comprises the following steps:
1) aluminium isopropoxide, manganese nitrate, acetic acid yttrium is soluble in water, obtaining Al concentration is that 0.05mol/L, Mn concentration are
0.02mol/L, Y concentration are the metal salt precursor solution of 0.03mol/L；
2) activated alumina, nano-silicon nitride, the poly- carboxylic of dispersing agent is added in the metal salt precursor solution that step 1) obtains
Sour sodium, the additional amount of silicon nitride are 0.9~1.1 times of aluminium isopropoxide molal quantity, and the additional amount of activated alumina is rubbing for Mn and Y
9.5~10.5 times of that number summation, the additional amount of dispersing agent sodium polycarboxylate are activated alumina and Nano powder of silicon nitride quality
0.1~1%, be stirred, formed suspension slurry；
3) the suspension slurry coating obtained step 2) forms the coating of 0.2~2 μ m-thick of catalysis on a catalyst support,
Freeze-drying, pressure is 10~40Pa, until water content is less than or equal to 3%, obtains dry presoma；
4) the drying presoma that step 3) obtains is placed in the nitrogen atmosphere of flowing and is roasted, roasted at 500~600 DEG C
0.5~2h obtains pretreatment body in 1000~1400 DEG C of 2~6h of roasting；
5) the pretreatment body that step 4) obtains is immersed in the precious metal solution of 0.01~0.3mol/L, the precious metal solution
In the potassium citrate containing 0.01~0.3mol/L, impregnate 5~10min, dry, roasting, maturing temperature is 400~700 DEG C, shape
At final products.
Through detecting, the N/O ratio in catalyst is 6.9%, illustrates that Si-N key is stable in the presence of in structure；Extremely by the catalyst
In internal diameter be 6mm reaction tube in, using dimethylbenzene, toluene and phenyl methylcarbamate as organic contamination source, respectively adjusting dimethylbenzene, toluene and
The carrier gas flux of gas circuit, makes its concentration respectively reach 1000mg/m where phenyl methylcarbamate3、3000mg/m3、5000mg/m3, react wet
Degree is 30%RH, and it is that reaction velocity reaches 110000h that air mixed gas flow, which is 300ml/min, in reaction-1.The result shows that urging
Above-mentioned exhaust gas complete catalysts oxidation can be carbon dioxide and water in 600 DEG C by agent；Under identical test environment, pass through
Obviously inactivating do not occur in 300 DEG C, 300h stability test, catalyst.
Embodiment three
A kind of preparation method of industrial waste gas purifying catalyst, which comprises the following steps:
1) aluminium isopropoxide, calcium nitrate, cobalt acetate, lanthanum nitrate is soluble in water, obtaining Al concentration is 0.1mol/L, Ca concentration
It is the metal salt precursor solution that 0.04mol/L, La concentration are 0.04mol/L for 0.02mol/L, Co concentration；
2) activated alumina, α-siliconnitride, dispersing agent naphthalene sulfonic acids is added in the metal salt precursor solution that step 1) obtains
Salt antiprecipitant, the additional amount of silicon nitride are 0.9~1.1 times of aluminium isopropoxide molal quantity, and the additional amount of activated alumina is
9.5~10.5 times of the molal quantity summation of Ca, Co, La, the additional amount of dispersing agent naphthalenesulfonate antiprecipitant are active oxidation
The 0.1~1% of aluminium and silicon nitride powder weight, is stirred, and forms suspension slurry；
3) the suspension slurry coating obtained step 2) forms the coating of 0.2~2 μ m-thick of catalysis on a catalyst support,
Freeze-drying, pressure is 10~40Pa, until water content is less than or equal to 3%, obtains dry presoma；
4) the drying presoma that step 3) obtains is placed in the nitrogen atmosphere of flowing and is roasted, roasted at 500~600 DEG C
0.5~2h obtains pretreatment body in 1000~1400 DEG C of 2~6h of roasting；
5) the pretreatment body that step 4) obtains is immersed in the precious metal solution of 0.01~0.3mol/L, the precious metal solution
In the potassium acetate containing 0.01~0.3mol/L, impregnate 5~10min, dry, roasting, maturing temperature is 400~700 DEG C, is formed
Final products.
Through detecting, the N/O ratio in catalyst is 7.1%, illustrates that Si-N key is stable in the presence of in structure；Extremely by the catalyst
In internal diameter be 6mm reaction tube in, using dimethylbenzene, toluene and phenyl methylcarbamate as organic contamination source, respectively adjusting dimethylbenzene, toluene and
The carrier gas flux of gas circuit, makes its concentration respectively reach 1000mg/m where phenyl methylcarbamate3、3000mg/m3、5000mg/m3, react wet
Degree is 30%RH, and it is that reaction velocity reaches 110000h that air mixed gas flow, which is 300ml/min, in reaction-1.The result shows that urging
Above-mentioned exhaust gas complete catalysts oxidation can be carbon dioxide and water in 600 DEG C by agent；Under identical test environment, pass through
Obviously inactivating do not occur in 300 DEG C, 300h stability test, catalyst.
Example IV
A kind of preparation method of industrial waste gas purifying catalyst, which comprises the following steps:
1) aluminium isopropoxide, barium nitrate, iron chloride is soluble in water, obtaining Al concentration is 0.01~0.1mol/L, Ba concentration
The metal salt precursor solution for being 0.01~0.1mol/L for 0.01~0.1mol/L, Fe concentration；
2) activated alumina, silicon nitride, dispersing agent styrene-horse is added in the metal salt precursor solution that step 1) obtains
Carry out acid anhydride copolymer, the additional amount of silicon nitride is 0.9~1.1 times of aluminium isopropoxide molal quantity, and the additional amount of activated alumina is
9.5~10.5 times of the molal quantity summation of Ba and Fe, the additional amount of dispersing agent styrene-maleic anhydride copolymer are active oxidation
The 0.1~1% of aluminium and silicon nitride powder weight, is stirred, and forms suspension slurry；
3) the suspension slurry coating obtained step 2) forms the coating of 0.2~2 μ m-thick of catalysis on a catalyst support,
Freeze-drying, pressure is 10~40Pa, until water content is less than or equal to 3%, obtains dry presoma；
4) the drying presoma that step 3) obtains is placed in the nitrogen atmosphere of flowing and is roasted, roasted at 500~600 DEG C
0.5~2h obtains pretreatment body in 1000~1400 DEG C of 2~6h of roasting；
5) the pretreatment body that step 4) obtains is immersed in the precious metal solution of 0.01~0.3mol/L, the precious metal solution
In the sodium oxalate containing 0.01~0.3mol/L, impregnate 5~10min, dry, roasting, maturing temperature is 400~700 DEG C, is formed
Final products.
Through detecting, the N/O ratio in catalyst is 6.8%, illustrates that Si-N key is stable in the presence of in structure；Extremely by the catalyst
In internal diameter be 6mm reaction tube in, using dimethylbenzene, toluene and phenyl methylcarbamate as organic contamination source, respectively adjusting dimethylbenzene, toluene and
The carrier gas flux of gas circuit, makes its concentration respectively reach 1000mg/m where phenyl methylcarbamate3、3000mg/m3、5000mg/m3, react wet
Degree is 30%RH, and it is that reaction velocity reaches 110000h that air mixed gas flow, which is 300ml/min, in reaction-1.The result shows that urging
Above-mentioned exhaust gas complete catalysts oxidation can be carbon dioxide and water in 600 DEG C by agent；Under identical test environment, pass through
Obviously inactivating do not occur in 300 DEG C, 300h stability test, catalyst.
Claims (9)
1. a kind of preparation method of industrial waste gas purifying catalyst, which comprises the following steps:
1) by one of aluminium isopropoxide and alkaline earth precursor, rare earth precursor, transition metal precursor or several
Kind, it is dissolved in solvent, obtains metal salt precursor solution；
2) activated alumina, silicon nitride, dispersing agent is added in the metal salt precursor solution that step 1) obtains, is stirred, shape
At suspension slurry；
3) the suspension slurry coating that step 2 obtains is formed into catalyst coatings on a catalyst support, drying to water content is less than
Equal to 3%, dry presoma is obtained；
4) the drying presoma that step 3) obtains is placed in the reducing atmosphere of flowing and is roasted, roast 0.5 at 500 ~ 600 DEG C
~ 2h obtains pretreatment body in 1000 ~ 1400 DEG C of 2 ~ 6h of roasting；
5) the pretreatment body for obtaining step 4) immerses in the precious metal solution of 0.01 ~ 0.3mol/L, impregnates 5 ~ 10min, does
Dry, roasting, maturing temperature is 400 ~ 700 DEG C, forms final products；
Alkaline earth precursor in the step 1) is barium nitrate, barium acetate, strontium nitrate, calcium nitrate, magnesium acetate or magnesium nitrate；
Rare earth precursor is lanthanum nitrate, lanthanum acetate, cerous nitrate, cerous acetate, yttrium nitrate, acetic acid yttrium；Transition metal predecessor is nitre
Sour manganese, manganese acetate, cobalt nitrate, cobalt acetate, ferric nitrate, ferric acetate, iron chloride.
2. the preparation method of the industrial waste gas purifying catalyst according to claim 1, which is characterized in that the metal salt
The sum of concentration of alkaline-earth metal, rare earth metal, transition metal ions is 0.01 ~ 0.1mol/L, aluminium isopropoxide in precursor solution
Additional amount be alkaline-earth metal, rare earth metal, transition metal ions molal quantity summation.
3. the preparation method of the industrial waste gas purifying catalyst according to claim 1, which is characterized in that the step 2
In silicon nitride be α-siliconnitride or nm amorphous silicon nitride.
4. the preparation method of the industrial waste gas purifying catalyst according to claim 1, which is characterized in that the step 2
In the additional amount of silicon nitride be 0.9 ~ 1.1 times of aluminium isopropoxide molal quantity, the additional amount of activated alumina be alkaline-earth metal,
9.5 ~ 10.5 times of the molal quantity summation of rare earth metal, transition metal ions.
5. the preparation method of the industrial waste gas purifying catalyst according to claim 1, which is characterized in that the step 2
In dispersing agent be Sodium Polyacrylate, sodium polycarboxylate or styrene-maleic anhydride copolymer, naphthalenesulfonate antiprecipitant one
Kind is several.
6. the preparation method of the industrial waste gas purifying catalyst according to claim 1, which is characterized in that the dispersing agent
Additional amount be the 0.1 ~ 1% of activated alumina and silicon nitride powder weight.
7. the preparation method of the industrial waste gas purifying catalyst according to claim 1, which is characterized in that the step 3)
Drying be freeze-drying, pressure be 10~40Pa.
8. the preparation method of the industrial waste gas purifying catalyst according to claim 1, which is characterized in that the step 3)
In catalyst coatings with a thickness of 0.2 ~ 2 μm.
9. the preparation method of the industrial waste gas purifying catalyst according to claim 1, which is characterized in that the step 5)
Precious metal solution in the sodium citrate containing 0.01 ~ 0.3mol/L or potassium citrate or potassium acetate or sodium oxalate.
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| CN1346694A (en) * | 2000-09-29 | 2002-05-01 | 株式会社电装 | Ceramic catalyst body and ceramic carrier |
| CN104781004A (en) * | 2012-12-27 | 2015-07-15 | 三井金属矿业株式会社 | Catalyst carrier and exhaust gas purifying catalyst |
| CN105289676A (en) * | 2015-10-27 | 2016-02-03 | 展宗城 | Foam-like low-temperature SCR catalyst and preparation method thereof |
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