CN106732653A - A kind of preparation method of low-temperature denitration catalyst - Google Patents
A kind of preparation method of low-temperature denitration catalyst Download PDFInfo
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Abstract
The present invention relates to a kind of preparation method of low-temperature denitration catalyst, belong to catalyst preparation technical field.Present invention walnut shell charcoal is used as template,Titanium deposition colloidal sol,Calcining is obtained catalyst carrier,Citric acid pretreated carrier is used again,Make to adhere to citric acid on carrier,Can be with the characteristic of chelated metal ions using citric acid,Make metal ion-chelant in carrier surface and hole,Increase its adhesion-tight degree,Again citric acid is decomposed by the nitrobacteria in nitrifying sludge,Consume citric acid,The metal ion of attachment is set to expose again,Metal oxide is formed after calcining closely to adsorb in carrier surface,Catalyst is finally obtained,The present invention is with titanium dioxide as carrier,Iron oxide is active component,The introducing of titanium produces induction to iron atom electron outside nucleus cloud,During the physicochemical change that occurs change the internal structure of catalyst and surface chemistry,The active temperature windows of catalyst are promoted to be offset to low temperature direction,Low temperature active is improved,Have a extensive future.
Description
Technical field
The present invention relates to a kind of preparation method of low-temperature denitration catalyst, belong to catalyst preparation technical field.
Background technology
With it is economical develop rapidly, the raising of industrial production and environmental requirement, atmosphere pollution extremely pays close attention into people
Problem.Due to the NO in airXThere are serious damaging effect, therefore NO to health and ecological environmentXDischarge and control
One of gradually cause the great attention of people, and the important process as current control atmosphere pollution.For a long time, China NOX
The increasingly serious basic reason of pollution is the energy consumption structure based on coal, is NO in airXWith the main source of flue dust.
Therefore, coal-fired boiler in power plant NOXEmission reduction and control be one of key task of efforts at environmental protection from now on.
Denitrating flue gas belong to burning post-processing technology, although relatively costly, but denitration efficiency is high, easily match somebody with somebody with burner
Set, is limited small by fuel type.Current gas denitrifying technology can be divided into the major class of dry and wet two.Dry denitration is urged including selection
Change reducing process (SCR), SNCR method (SNCR), catalytic decomposition, absorption method and low-temperature plasma method；Wet method takes off
Nitre is including sour absorption, Alkali absorption, chemical oxidation absorption and biological reducing method etc..Catalyst is the most crucial part of denitration technology,
And metal oxide-type catalyst the most frequently used at present is mainly with V2O5、Fe2O3、CuO、NiO、Co2O3Make Deng metal oxide
It is active component, compared to noble metal catalyst, the cost of metal oxide catalyst is cheaper, and anti-poisoning capability is stronger, and
And its de- really activity is very high, is a kind of cost performance catalyst very high, is current most study, most deep catalyst.But this
Mostly in class catalyst preparation process be obtained using dipping calcination method, and heavy metal ion attachment is insecure in dipping process, causes
Finished product catalysis activity is low, and engineering practice shows that the catalyst is interval interior in 300~400 DEG C of high temperature, just with very high
Denitration efficiency, therefore, invent a kind of has weight with low-temperature denitration ability and catalysis activity catalyst high to denitration field
The meaning wanted.
The content of the invention
Present invention mainly solves technical problem, be mostly to use for common metal oxide-type denitrating catalyst at present
Dipping calcination method is obtained, and heavy metal ion attachment is insecure in dipping process, causes finished product catalysis activity low, and in high temperature bar
Under part, just with the problem of denitration efficiency high.There is provided one kind with walnut shell charcoal as template, in template surface titanium deposition colloidal sol,
Calcining removes after removing template to obtain high specific surface area titanic oxide carrier, then with being put into heavy metallic salt solution after lemon acid soak carrier
Middle reaction, last and nitrifying sludge mixed fermentation is obtained the method for catalyst after calcining.The present invention has huge using walnut shell charcoal
Big specific surface area, with it as template, titanium deposition colloidal sol, calcining is obtained catalyst carrier, catalyst is had greatly ratio
Surface area, improves catalysis activity, then uses citric acid pretreated carrier, makes to adhere to citric acid on carrier, can be with chela using citric acid
The characteristic of metal ion, makes metal ion-chelant in carrier surface and hole, increases its adhesion-tight degree, then dirty by nitrification
Nitrobacteria in mud makes full use of citric acid to participate in tricarboxylic acid cycle, citric acid is consumed so as to reach solution chelate effect, attached
The metal ion on carrier is exposed again, metal oxide is formed after calcining and is closely adsorbed in carrier surface,
Finally prepared catalyst, of the invention with titanium dioxide as carrier, and iron oxide is active component, and the introducing of titanium is understood outside to iron atom core
Electron cloud produces induction, and the physicochemical change for occurring in the process can make the internal structure and surface chemistry of catalyst
Change, promote the active temperature windows of catalyst to be offset to low temperature direction, low temperature active is improved, preceding with wide application
Scape.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is：
（1）Weigh during 400~500g walnut shells are put into ball mill and crush 400 mesh sieves excessively after 20~30min, obtain walnut shell powder
End, walnut shell powder is put into retort, and carbonizing 1~2h with 500~600 DEG C of temperatures under nitrogen protection obtains walnut
Shell carbon powder；
（2）Measure 400~500mL butyl titanates and 200~250mL acetylacetone,2,4-pentanediones are fitted into beaker, with magnetic stirrer with 300
~400r/min rotating speeds stir 15~20min after again in beaker add 80~100g walnut shell carbon powders obtained above and
Be transferred to beaker in water-bath after finishing by 300~500mL absolute ethyl alcohols, addition, is warming up to 60~70 DEG C, insulated and stirred reaction 3
~5h；
（3）Filtered after above-mentioned reaction terminates, obtain filter residue, filter residue is first put into baking oven, 1~2h is dried at 105~110 DEG C
After be transferred to Muffle furnace, with 500~600 DEG C of 3~4h of high-temperature calcination, obtain porous silica titanium carrier；
（4）The above-mentioned porous silica titanium carrier immersion mass fractions of 40~50g are weighed in 30% citric acid solution, shaking table vibrates
20~24h of dipping, is filtrated to get filter residue, and pretreated carrier is after drying, weigh 20~25g ferric nitrates, 5~10g nickel nitrates,
10~12g cobalt nitrates and 3~5g palladium nitrates are dissolved in 900~1000mL absolute ethyl alcohols, obtain mixture-metal ethanol solution；
（5）The above-mentioned pretreated carriers of 40~45g are poured into mixture-metal ethanol solution, the stirring reaction 15 at 40~50 DEG C
~20min, is filtrated to get filter cake, and filter cake is fitted into gauze bag, seals sack, then the gauze bag after sealing is loaded into fermentation tank
In, to the nitrifying sludge added in tank in sewage treatment plant's nitrification tank, until gauze bag is completely covered nitrifying sludge, hermetically sealed can
Fermented 3~5 days at 30~40 DEG C after mouthful；
（6）After fermentation ends, be put into the filter cake after treatment in Muffle furnace by the filter cake after being processed in taking-up gauze bag, rises high temperature
Degree to 400~450 DEG C, after 5~7h of insulation calcining, after taking out product after in-furnace temperature clear-cutting forestland room temperature, after 1~2h of grinding,
Obtain final product low-temperature denitration catalyst.
Application process of the invention：The obtained low-temperature denitration catalyst of 300~500g present invention is loaded into SCR reactors
In, then SCR reactors are arranged between boiler economizer and air preheater, then with the speed of 40~50mL/min to SCR
Ammonia is passed through in reactor, in the presence of catalyst, containing NOXThe reaction of waste gas and ammonia be degraded to innocuous gas discharge,
Catalyst of the invention obtained at 170~200 DEG C denitration efficiency more than 90%, low-temperature denitration efficiency improves 10~30 hundred
Branch, in 100~150 DEG C of intervals, its NO is to NO2Conversion ratio by traditional catalyst be almost 0 bring up to after 4~
10%, with splendid denitration effect.
The beneficial effects of the invention are as follows：
（1）Obtained low-temperature denitration catalyst preparation process of the invention is simple to operation, with low cost；
（2）The low-temperature catalyzed performance of obtained low-temperature denitration catalyst of the invention is splendid, and at 170~200 DEG C, denitration efficiency exceedes
90%, low-temperature denitration efficiency improves 10~30 percentage points；
（3）Metal ion adhesion-tight in obtained low-temperature denitration catalyst preparation process of the invention, final obtained catalyst
High catalytic efficiency.
Specific embodiment
Weigh during 400~500g walnut shells are put into ball mill and crush 400 mesh sieves excessively after 20~30min, obtain walnut shell powder
End, walnut shell powder is put into retort, and carbonizing 1~2h with 500~600 DEG C of temperatures under nitrogen protection obtains walnut
Shell carbon powder；Measure 400~500mL butyl titanates and 200~250mL acetylacetone,2,4-pentanediones be fitted into beaker, with magnetic stirrer with
Again to addition 80~100g walnut shell carbon powders obtained above in beaker after 300~400r/min rotating speeds stirring, 15~20min
With 300~500mL absolute ethyl alcohols, add beaker is transferred in water-bath after finishing, be warming up to 60~70 DEG C, insulated and stirred reaction
3~5h；Filtered after above-mentioned reaction terminates, obtain filter residue, filter residue is first put into baking oven, 1~2h is dried at 105~110 DEG C
After be transferred to Muffle furnace, with 500~600 DEG C of 3~4h of high-temperature calcination, obtain porous silica titanium carrier；Weigh 40~50g above-mentioned
Porous silica titanium carrier immersion mass fraction is in 30% citric acid solution, shaking table vibration 20~24h of dipping is filtrated to get filter
Slag, pretreated carrier is after drying, and weighs 20~25g ferric nitrates, 5~10g nickel nitrates, 10~12g cobalt nitrates and 3~5g nitre
Sour palladium is dissolved in 900~1000mL absolute ethyl alcohols, obtains mixture-metal ethanol solution；By the above-mentioned pretreated carriers of 40~45g
Pour into mixture-metal ethanol solution, 15~20min of stirring reaction, is filtrated to get filter cake at 40~50 DEG C, and filter cake is filled
Enter in gauze bag, seal sack, then the gauze bag after sealing is fitted into fermentation tank, to addition sewage treatment plant nitrification tank in tank
In nitrifying sludge, until gauze bag is completely covered nitrifying sludge, fermented 3~5 days at 30~40 DEG C after sealing tank mouth；Hair
After ferment terminates, be put into the filter cake after treatment in Muffle furnace by the filter cake after being processed in taking-up gauze bag, and liter high-temperature to 400~
450 DEG C, after 5~7h of insulation calcining, after product is taken out after in-furnace temperature clear-cutting forestland room temperature, after 1~2h of grinding, obtain final product low temperature and take off
Denox catalyst.
Example 1
Weigh during 400g walnut shells are put into ball mill and crush 400 mesh sieves excessively after 20min, walnut shell powder is obtained, by walnut shell powder
End is put into retort, and carbonizing 1h with 500 DEG C of temperatures under nitrogen protection obtains walnut shell carbon powder；Measure 400mL titaniums
Acid butyl ester and 200mL acetylacetone,2,4-pentanediones are fitted into beaker, with magnetic stirrer with 300r/min rotating speeds stir 15min after again to beaker
Be transferred to beaker in water-bath after finishing by middle addition 80g walnut shell carbon powders obtained above and 300mL absolute ethyl alcohols, addition,
It is warming up to 60 DEG C, insulated and stirred reaction 3h；Filtered after above-mentioned reaction terminates, obtain filter residue, filter residue is first put into baking oven,
Muffle furnace is transferred to after 1h is dried at 105 DEG C, with 500 DEG C of high-temperature calcination 3h, porous silica titanium carrier is obtained；Weigh on 40g
Porous silica titanium carrier immersion mass fraction is stated in 30% citric acid solution, shaking table vibration dipping 20h is filtrated to get filter residue,
Pretreated carrier is after drying, weighing 20g ferric nitrates, 5g nickel nitrates, 10g cobalt nitrates and 3g palladium nitrates, to be dissolved in 900mL anhydrous
In ethanol, mixture-metal ethanol solution is obtained；The above-mentioned pretreated carriers of 40g are poured into mixture-metal ethanol solution,
Stirring reaction 15min, is filtrated to get filter cake at 40 DEG C, and filter cake is fitted into gauze bag, seals sack, then by the gauze after sealing
It is packed enter fermentation tank in, to the nitrifying sludge added in tank in sewage treatment plant nitrification tank, until nitrifying sludge is complete by gauze bag
All standing, ferments 3 days after sealing tank mouth at 30 DEG C；After fermentation ends, the filter cake after being processed in taking-up gauze bag, after treatment
Filter cake be put into Muffle furnace, rise high-temperature to 400 DEG C, insulation calcining 5h after, after after in-furnace temperature clear-cutting forestland room temperature take out
Product, after grinding 1h, obtains final product low-temperature denitration catalyst.
Application process of the invention：The obtained low-temperature denitration catalyst of the 300g present invention is fitted into SCR reactors, then will
SCR reactors are arranged between boiler economizer and air preheater, then with the speed of 40mL/min to being passed through in SCR reactors
Ammonia, in the presence of catalyst, containing NOXThe reaction of waste gas and ammonia be degraded to innocuous gas discharge, the present invention is obtained
Catalyst denitration efficiency at 170 DEG C is 93%, and low-temperature denitration efficiency improves 10 percentage points, in 100 DEG C of intervals, its NO
To NO2Conversion ratio by traditional catalyst be almost 0 bring up to after 4%, with splendid denitration effect.
Example 2
Weigh during 450g walnut shells are put into ball mill and crush 400 mesh sieves excessively after 25min, walnut shell powder is obtained, by walnut shell powder
End is put into retort, and carbonizing 1h with 550 DEG C of temperatures under nitrogen protection obtains walnut shell carbon powder；Measure 450mL titaniums
Acid butyl ester and 230mL acetylacetone,2,4-pentanediones are fitted into beaker, with magnetic stirrer with 350r/min rotating speeds stir 18min after again to beaker
Be transferred to beaker in water-bath after finishing by middle addition 90g walnut shell carbon powders obtained above and 400mL absolute ethyl alcohols, addition,
It is warming up to 65 DEG C, insulated and stirred reaction 4h；Filtered after above-mentioned reaction terminates, obtain filter residue, filter residue is first put into baking oven,
Muffle furnace is transferred to after 1h is dried at 108 DEG C, with 550 DEG C of high-temperature calcination 3h, porous silica titanium carrier is obtained；Weigh on 45g
Porous silica titanium carrier immersion mass fraction is stated in 30% citric acid solution, shaking table vibration dipping 22h is filtrated to get filter residue,
Pretreated carrier is after drying, weighing 23g ferric nitrates, 8g nickel nitrates, 11g cobalt nitrates and 4g palladium nitrates, to be dissolved in 950mL anhydrous
In ethanol, mixture-metal ethanol solution is obtained；The above-mentioned pretreated carriers of 43g are poured into mixture-metal ethanol solution,
Stirring reaction 18min, is filtrated to get filter cake at 45 DEG C, and filter cake is fitted into gauze bag, seals sack, then by the gauze after sealing
It is packed enter fermentation tank in, to the nitrifying sludge added in tank in sewage treatment plant nitrification tank, until nitrifying sludge is complete by gauze bag
All standing, ferments 4 days after sealing tank mouth at 35 DEG C；After fermentation ends, the filter cake after being processed in taking-up gauze bag, after treatment
Filter cake be put into Muffle furnace, rise high-temperature to 430 DEG C, insulation calcining 6h after, after after in-furnace temperature clear-cutting forestland room temperature take out
Product, after grinding 2h, obtains final product low-temperature denitration catalyst.
Application process of the invention：The obtained low-temperature denitration catalyst of the 400g present invention is fitted into SCR reactors, then will
SCR reactors are arranged between boiler economizer and air preheater, then with the speed of 45mL/min to being passed through in SCR reactors
Ammonia, in the presence of catalyst, containing NOXThe reaction of waste gas and ammonia be degraded to innocuous gas discharge, the present invention is obtained
Catalyst denitration efficiency at 185 DEG C is 95%, and low-temperature denitration efficiency improves 12 percentage points, in 130 DEG C of intervals, its NO
To NO2Conversion ratio by traditional catalyst be almost 0 bring up to after 6%, with splendid denitration effect.
Example 3
Weigh during 500g walnut shells are put into ball mill and crush 400 mesh sieves excessively after 30min, walnut shell powder is obtained, by walnut shell powder
End is put into retort, and carbonizing 2h with 600 DEG C of temperatures under nitrogen protection obtains walnut shell carbon powder；Measure 500mL titaniums
Acid butyl ester and 250mL acetylacetone,2,4-pentanediones are fitted into beaker, with magnetic stirrer with 400r/min rotating speeds stir 20min after again to beaker
Be transferred to beaker in water-bath after finishing by middle addition 100g walnut shell carbon powders obtained above and 500mL absolute ethyl alcohols, addition,
It is warming up to 70 DEG C, insulated and stirred reaction 5h；Filtered after above-mentioned reaction terminates, obtain filter residue, filter residue is first put into baking oven,
Muffle furnace is transferred to after 2h is dried at 110 DEG C, with 600 DEG C of high-temperature calcination 4h, porous silica titanium carrier is obtained；Weigh on 50g
Porous silica titanium carrier immersion mass fraction is stated in 30% citric acid solution, shaking table vibration dipping 24h is filtrated to get filter residue,
After drying be pretreated carrier, weigh 25g ferric nitrates, 10g nickel nitrates, 12g cobalt nitrates and 5g palladium nitrates be dissolved in 1000mL without
In water-ethanol, mixture-metal ethanol solution is obtained；The above-mentioned pretreated carriers of 45g are poured into mixture-metal ethanol solution,
Stirring reaction 20min, is filtrated to get filter cake at 50 DEG C, and filter cake is fitted into gauze bag, seals sack, then by the yarn after sealing
Cloth bag is fitted into fermentation tank, to the nitrifying sludge added in tank in sewage treatment plant nitrification tank, until nitrifying sludge is by gauze bag
It is completely covered, is fermented 5 days at 40 DEG C after sealing tank mouth；After fermentation ends, the filter cake after being processed in taking-up gauze bag will be processed
Filter cake afterwards is put into Muffle furnace, rises high-temperature to 450 DEG C, after insulation calcining 7h, is taken after after in-furnace temperature clear-cutting forestland room temperature
Go out product, after grinding 2h, obtain final product low-temperature denitration catalyst.
Application process of the invention：The obtained low-temperature denitration catalyst of the 500g present invention is fitted into SCR reactors, then will
SCR reactors are arranged between boiler economizer and air preheater, then with the speed of 50mL/min to being passed through in SCR reactors
Ammonia, in the presence of catalyst, containing NOXThe reaction of waste gas and ammonia be degraded to innocuous gas discharge, the present invention is obtained
Catalyst denitration efficiency at 200 DEG C is 96%, and low-temperature denitration efficiency improves 13 percentage points, in 150 DEG C of intervals, its NO
To NO2Conversion ratio by traditional catalyst be almost 0 bring up to after 10%, with splendid denitration effect.
Claims (1)
1. a kind of preparation method of low-temperature denitration catalyst, it is characterised in that specific preparation process is：
（1）Weigh during 400~500g walnut shells are put into ball mill and crush 400 mesh sieves excessively after 20~30min, obtain walnut shell powder
End, walnut shell powder is put into retort, and carbonizing 1~2h with 500~600 DEG C of temperatures under nitrogen protection obtains walnut
Shell carbon powder；
（2）Measure 400~500mL butyl titanates and 200~250mL acetylacetone,2,4-pentanediones are fitted into beaker, with magnetic stirrer with 300
~400r/min rotating speeds stir 15~20min after again in beaker add 80~100g walnut shell carbon powders obtained above and
Be transferred to beaker in water-bath after finishing by 300~500mL absolute ethyl alcohols, addition, is warming up to 60~70 DEG C, insulated and stirred reaction 3
~5h；
（3）Filtered after above-mentioned reaction terminates, obtain filter residue, filter residue is first put into baking oven, 1~2h is dried at 105~110 DEG C
After be transferred to Muffle furnace, with 500~600 DEG C of 3~4h of high-temperature calcination, obtain porous silica titanium carrier；
（4）The above-mentioned porous silica titanium carrier immersion mass fractions of 40~50g are weighed in 30% citric acid solution, shaking table vibrates
20~24h of dipping, is filtrated to get filter residue, and pretreated carrier is after drying, weigh 20~25g ferric nitrates, 5~10g nickel nitrates,
10~12g cobalt nitrates and 3~5g palladium nitrates are dissolved in 900~1000mL absolute ethyl alcohols, obtain mixture-metal ethanol solution；
（5）The above-mentioned pretreated carriers of 40~45g are poured into mixture-metal ethanol solution, the stirring reaction 15 at 40~50 DEG C
~20min, is filtrated to get filter cake, and filter cake is fitted into gauze bag, seals sack, then the gauze bag after sealing is loaded into fermentation tank
In, to the nitrifying sludge added in tank in sewage treatment plant's nitrification tank, until gauze bag is completely covered nitrifying sludge, hermetically sealed can
Fermented 3~5 days at 30~40 DEG C after mouthful；
（6）After fermentation ends, be put into the filter cake after treatment in Muffle furnace by the filter cake after being processed in taking-up gauze bag, rises high temperature
Degree to 400~450 DEG C, after 5~7h of insulation calcining, after taking out product after in-furnace temperature clear-cutting forestland room temperature, after 1~2h of grinding,
Obtain final product low-temperature denitration catalyst.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107519945A (en) * | 2017-06-08 | 2017-12-29 | 河北威达蓝海环保科技有限公司 | A kind of handling process of wide temperature range denitrating catalyst raw material |
| CN112156771A (en) * | 2020-10-30 | 2021-01-01 | 东北电力大学 | Preparation method and application of catalyst loaded by biological thallus |
| CN117865811A (en) * | 2024-03-11 | 2024-04-12 | 山东道可化学有限公司 | Method for preparing nitrobenzotrifluoride by continuously nitrifying benzotrifluoride |
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| CN112156771A (en) * | 2020-10-30 | 2021-01-01 | 东北电力大学 | Preparation method and application of catalyst loaded by biological thallus |
| CN117865811A (en) * | 2024-03-11 | 2024-04-12 | 山东道可化学有限公司 | Method for preparing nitrobenzotrifluoride by continuously nitrifying benzotrifluoride |
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