CN103506108B - Waste gas purification catalysts for treating - Google Patents
Waste gas purification catalysts for treating Download PDFInfo
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- CN103506108B CN103506108B CN201210313467.2A CN201210313467A CN103506108B CN 103506108 B CN103506108 B CN 103506108B CN 201210313467 A CN201210313467 A CN 201210313467A CN 103506108 B CN103506108 B CN 103506108B
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Abstract
The invention provides a kind of waste gas purification catalysts for treating, even if this catalyst also can obtain high waste gas purification under the condition reducing reaction temperature, even and if minimizing use amount also can improve durability.Waste gas purification catalysts for treating of the present invention load in the composite oxides of the oxide of titanyl compound and silicon has the oxide of vanadium, the content of the oxide of silicon is 1 ~ 10 quality %, and described composite oxides are higher than 500 DEG C in sintering temperature and make under the condition of less than 520 DEG C.Particularly by sintering temperature being set to higher than 500 DEG C and less than 520 DEG C, catalyst strength improves, and durability improves.
Description
Technical field
The present invention relates to the catalyst used when purified treatment waste gas.
Background technology
In the waste gas of discharging from the various incinerator such as city garbage incinerator, industrial waste incinerator, sludge incinerator, sometimes containing nitrogen oxide, two
the organic chlorides such as English class.Therefore, usually, for the waste gas of discharging from incinerator, the process that removing nitrogen oxide and organic chloride and carrying out purify is implemented.
As the nitrogen oxide in removing waste gas and the method for organic chloride, there will be a known make nitrogen oxide and organic chloride be adsorbed in active carbon method, nitrogen oxide and organic chloride carried out to the method for thermal decomposition, use the method (catalytic decomposition) of catalyst decomposes nitrogen oxide and organic chloride.In these methods, catalytic decomposition is not owing to needing dust process and wastewater treatment, and efficiency is high, therefore extensively popularizes.
Catalytic decomposition is the method making the catalyst exposure of waste gas and decomposing nitrogen oxide and organic chloride to carry out to purify.Catalyst cupport in bag hose, or to be filled in reactor thus to reaction supply.
In the past as the catalyst used in catalytic decomposition, having widely used using the oxide of vanadium, tungsten, molybdenum etc. as active metal, took titanium oxide as the catalyst (patent document 1,2) of carrier.
Existing patent document
Patent document
Patent document 1: Japanese Kohyo 4-503772 publication
Patent document 2: Japan Patent No. 3457917 publication
Summary of the invention
The problem that invention will solve
In the catalyst that patent document 1,2 is recorded, when waste gas purification, in order to improve waste gas purification, reaction temperature is set as higher than 230 DEG C, but, if too improve EGT to improve purification property, the heat recovery rate in the boiler of previous stage then can be caused to decline, uneconomical.On the other hand, if reduce reaction temperature to carry out recuperation of heat, then exhaust-gas purifying performance declines.Therefore, in the past by reaction temperature setting lower than 230 DEG C time, ensure that purification property and durability by increasing the use amount of catalyst, but due to the use amount of catalyst many, therefore cost is high.
The object of the present invention is to provide a kind of exhaust gas purification catalyst, even if this exhaust gas purification catalyst also can obtain high waste gas purification when reaction temperature is low, even and if reduce its use amount and also durability can be improved.In addition, the object of the present invention is to provide a kind of catalyst, even if it in use adheres to poisoning material (by malicious thing Quality) and performance when reducing, also can restorability by regenerate with water.
The method of dealing with problems
For waste gas purification catalysts for treating of the present invention, in the composite oxides of the oxide of titanyl compound and silicon, load has the oxide of vanadium, relative to described composite oxides, the content of the oxide of silicon is 1 ~ 10 quality %, wherein, described composite oxides are more than 500 DEG C in sintering temperature and make under the condition of less than 520 DEG C, and the solid acid amount obtained by pyridine adsorption method is more than 0.30mmol/g and regenerate with water restoring degree is more than 0.70.
The effect of invention
In exhaust gas purification catalyst of the present invention, even if reduce reaction temperature also can obtain high waste gas purification.In addition, in exhaust gas purification catalyst of the present invention, even if do not increase use amount also durability can be improved, in addition, if there is the durability of same degree with product in the past, then use amount can be reduced.In addition, in use, even if when adhering to poisoning material and performance and reducing, also can by regenerate with water restorability.
Accompanying drawing explanation
Fig. 1 represents TiO
2siO
2the curve map of relation between the composition of composite oxides and pyridine adsorption amount and specific area;
Fig. 2 represents to obtain TiO
2siO
2sintering temperature during composite oxides and the curve map of relation between regenerate with water restoring degree.
Detailed description of the invention
Exhaust gas purification catalyst of the present invention is (hreinafter referred to as " catalyst ".) be at titanyl compound (TiO
2) and the oxide (SiO of silicon
2) composite oxides in load have the oxide (V of vanadium
2o
5) catalyst.
Relative to described composite oxides, SiO
2content is 1 ~ 10 quality %, is preferably 2 ~ 8 quality %.
V is had in non-load
2o
5tiO
2siO
2in composite oxides, specific area and pyridine adsorption amount are different according to its composition.That is, as shown in Figure 1, at SiO
2content increase time, specific area increase.In addition, as shown in Figure 1, at SiO
2content when being increased to about 5 quality % by 0 quality %, pyridine adsorption amount increases, and SiO
2content increase further, then pyridine adsorption amount reduce.In addition, pyridine adsorption amount represents solid acid amount, and its amount is more, and initial stage catalytic activity is higher.In addition, catalyst strength also uprises, and durability improves.
In catalyst of the present invention, because load has V
2o
5, the curve map same with Fig. 1 can not be obtained, but demonstrate same trend.Therefore, the SiO of no matter catalyst of the present invention
2content is lower than above-mentioned lower limit still higher than above-mentioned higher limit, and pyridine adsorption amount, all lower than 0.3mmol/g, is insufficient.Therefore, initial stage catalytic activity step-down, in addition, also reduces relative to the patience of poisoning material.In addition, at SiO
2content lower than above-mentioned lower limit time, specific area is lower than 40m
2/ g is insufficient.
Specific area can be obtained by BET absorption method.
Pyridine adsorption amount can be obtained by the following method.
That is, first, after being heated with 450 DEG C under helium-atmosphere by exhaust gas purification catalyst, at 150 DEG C, pyridine is supplied to exhaust gas purification catalyst and makes it adsorb, then vacuum discharge is attached to the pyridine beyond solid acid position (solid acid point).Afterwards, by exhaust gas purification catalyst is heated to 800 DEG C with constant programming rate from 150 DEG C, the pyridine being adsorbed in solid acid position is departed from, then measures the pyridine amount of this disengaging.Using this pyridine amount as being pyridine adsorption amount.
The TiO of catalyst of the present invention
2content is preferably 70 ~ 98 quality %, is more preferably 77 ~ 93 quality %.As long as TiO
2content be more than above-mentioned lower limit and below above-mentioned higher limit, then the in the initial stage of that catalytic activity raises further.In addition, catalyst strength also increases, and durability improves.
The V of catalyst of the present invention
2o
5content is preferably 1 ~ 20 quality %, is more preferably 5 ~ 15 quality %.V
2o
5as long as content is more than above-mentioned lower limit, then just can obtain practical initial stage catalytic activity.But, even if containing the V higher than above-mentioned higher limit
2o
5, the raising of catalytic activity also can culminate, and causes the V wasted
2o
5change is many.
In catalyst of the present invention, regenerate with water restoring degree is more than 0.70, preferably more than 0.75.The value of regenerate with water restoring degree is larger, and durability is more excellent.When regenerate with water restoring degree is lower than above-mentioned lower limit, the performance after regenerate with water is insufficient.
At this, regenerate with water restoring degree is the value obtained by following formula:
(using the catalyst after the use of washing to carry out the rate constant K that purified treatment contains the gas of pollutant component)/(rate constant K using original catalyst to carry out purified treatment to contain the gas of pollutant component
0).
Reaction condition when regenerate with water restoring degree measures is as follows: use cast circulation reaction test device as reaction unit, reaction temperature is set as 190 DEG C, is NO concentration 150ppm, NH by the concentration of catalyst cleaning pollutant component
3concentration 105ppm, space velocity is 10000h
-1.
In addition, when regenerate with water restoring degree measures, actual waste gas can being used, also can being used in carry out the simulated exhaust prepared when regenerate with water restoring degree measures.As the pollutant component contained in simulated exhaust, nitric oxide, two can be enumerated
english substitute materials etc.
The shape of catalyst can be pill shape (pellet), tabular, cylindrical shape, corrugated (corrugate), the arbitrary shape such as cellular.In addition, catalyst also can be carried on bag hose.
For the manufacture method of above-mentioned catalyst, there is no particular limitation, but, usually preparing TiO
2siO
2after composite oxides, supported V
2o
5.
Such as, after being mixed with the slaine (chloride, sulfate, nitrate) of titanium or alkoxide, the slaine (chloride, sulfate, nitrate) of silicon or alkoxide, carry out co-precipitation or hydrolysis, thus, obtain the slurry of complex hydroxide.Then, dewater to the slurry of complex hydroxide, cleaning obtains wet cake (wetcake), then makes it dry, then higher than 500 DEG C and the scope of less than 520 DEG C sinter, obtain composite oxides.Generally speaking, containing TiO
2catalyst in, when sintering more than 550 DEG C, due to TiO
2crystal structure be that rutile structure makes catalytic activity reduce, therefore sintering lower than 500 DEG C.But in the regenerate with water of catalyst, the crushing strength outbalance of catalyst, as shown in Figure 2, when sintering below 500 DEG C, the use because of the intensity reduction of catalyst body after regenerate with water becomes difficulty.When sintering higher than 500 DEG C, crushing strength sharply rises, and durability improves, and is significantly recovered by regenerate with water performance.On the other hand, when higher than 520 DEG C, can not ignore the reduction of catalytic activity, the performance after regenerate with water reduces.
Next, using above-mentioned composite oxides as carrier, add the aqueous solution of the salt of vanadic acid and sinter, manufacturing catalyst thus.
When by catalyst cupport in bag hose, under the existence of bag hose, apply the manufacture method of above-mentioned catalyst.
Above-mentioned catalyst goes for the purification of the waste gas of discharging from the various incinerator such as city garbage incinerator, industrial waste incinerator, sludge incinerator.By catalyst cleaning pollutant component of the present invention, the nitrogen oxide such as nitric oxide, two can be enumerated as what contain in waste gas
the organic chlorides such as English class and PCB class, high condensation degree aromatic hydrocarbon etc.When purifying nitrogen oxide, preferably in waste gas, mix the reducing agents such as ammonia.
When being arbitrary shape by shaping of catalyst, to reactor catalyst filling, import waste gas to this reactor, thus, decomposing pollutant matter and waste gas is purified.In this situation, before waste gas is imported to reactor, bag hose is preferably used to carry out dedusting to waste gas.
When by catalyst cupport in bag hose, make waste gas carry out dedusting by bag hose, and, can catalyst decomposes pollutant component and then purifying exhaust air be passed through.In the method, dedusting and purification can be carried out simultaneously, therefore, it is possible to simplify the device being used for purifying exhaust air, realize low cost.
Different according to the kind of pollutant component contained in waste gas and concentration, the use amount of catalyst, the specification of waste gas purification apparatus etc. by reaction condition during catalyst cleaning waste gas.Even if catalyst of the present invention also can keep high initial stage catalytic activity under lower reaction temperature, therefore, the low reaction temperatures of 200 ~ 230 DEG C of scopes can be set as.
As the method for adjustment of reaction temperature, the method for the temperature of adjustment waste gas can be applied, adjust the method being filled with the temperature of the reactor of catalyst.
In addition, be the waste gas such as municipal refuse or industrial waste at waste gas, and in the offgas containing two
when the organic chlorides such as English, in order to make organic chloride suitably decompose, preferably reaction temperature being set as on the basis of 200 ~ 230 DEG C, space velocity (GHSV) is being set to 1000 ~ 20000h
-1and oxygen concentration is set to 0.1 ~ 21 volume %.
Embodiment
(embodiment 1)
Mixing titanium sulfate (TiSO
4) aqueous solution and the cataloid aqueous solution makes TiO
2be 85 mass parts, SiO
2be 5 mass parts, this mixed aqueous solution is heated to 70 DEG C.In the mixed aqueous solution after heating, drip ammonia spirit until pH=7, form coprecipitate slurry.This slurry is stirred at 70 DEG C also slaking, after 2 hours, to carry out filtering and cleaning, obtain pie.Next, above-mentioned pie is carried out drying at 100 DEG C, then at 520 DEG C, carry out 5 hours sintering, obtain TiO
2siO
2composite oxides.
Relative to this composite oxides 100 mass parts, in methylamine water solution, dissolve ammonium metavanadate make V
2o
5be 10 mass parts, pulverous above-mentioned composite oxides drip solution obtained above and carries out mixing and dry, repeating aforesaid operations, thus load V
2o
5.Then, at 500 DEG C, carry out 5 hours sintering, obtain catalyst 1.
(embodiment 2)
Except interpolation titanium sulfate aqueous solution, the cataloid aqueous solution, ammonium metavanadate make TiO
2be 85 mass parts, SiO
2be 5 mass parts, V
2o
5be outside 10 mass parts, according to mode similarly to Example 1, obtain catalyst 2.
(comparative example 1)
Except will TiO be obtained
2siO
2sintering temperature during composite oxides is set as outside 500 DEG C, according to mode similarly to Example 1, obtains catalyst.
< evaluates >
For the catalyst of each example, determine specific area, pyridine adsorption amount, catalytic activity and regenerate with water restoring degree by following method.These results are as shown in table 1.
[specific area]
By BET1 point absorption method (nitrogen adsorption methods) measurement the specific area.Condition determination is as described below.
Sample size: 0.1g, Pretreatment: under blanket of nitrogen, 200 DEG C, 2 hours, nitrogen adsorption temperature :-196 DEG C, desorption temperature: room temperature, detector: thermal conductivity detector (TCD)
[pyridine adsorption amount]
Pyridine adsorption amount is measured by pyridine adsorption intensification spin off method.Condition determination is as described below.
Sample size: 0.0125g, Pretreatment: under helium-atmosphere, 450 DEG C, 30 minutes, pyridine adsorption temperature: 150 DEG C (repeating pyridine 0.2 μ 1 Pulse adsorption), desorption conditions: 150 DEG C → 800 DEG C (programming rate: 30 DEG C/min), detector: flame ionization ditector (FID)
In addition, pyridine adsorption amount is more, and solid acid amount is more.
[catalytic activity]
Under following reaction condition, determine the catalytic activity (denitrification percent) when purified treatment contains the waste gas of nitric oxide (NO).
Experimental rig: tubular type circulation reaction test device
EGT: 190 DEG C
NO concentration in waste gas: 150ppm
Reducing agent (NH
3) concentration: 105ppm
Space velocity: 10000h
-1
[regenerate with water restoring degree]
By the mensuration of above-mentioned catalytic activity, obtain rate constant K
0.
Then, for the attachment of the hydrosulphate due to ammonium sulfate, acid ammonium sulfate and Na, K and the catalyst sample causing performance to reduce, after cleaning with the pure water relative to catalyst capacity being 10 times, obtain rate constant K by the method same with the mensuration of above-mentioned catalytic activity.And, by K/K
0obtain regenerate with water restoring degree.
Table 1
Even if the catalyst of embodiment 1,2 also has sufficient nitrogen removal performance under reaction temperature is the temperature of 200 DEG C low like this, durability is high, and in addition, regenerate with water restoring degree is high.Think this result be due to catalyst composition within the scope of the invention, thus specific area becomes large and solid acid quantitative change multi-band is come.
In contrast, the catalyst of comparative example 1 is when reaction temperature 200 DEG C, and denitrogenation is slightly low, and regenerate with water restoring degree is also insufficient.Think that this result is because catalyst composition is outside scope of the present invention, thus the little and solid acid amount of specific area causes less.
Claims (7)
1. a waste gas purification catalysts for treating, its load in the composite oxides of the oxide of titanyl compound and silicon has the oxide of vanadium,
Relative to described composite oxides, the content of the oxide of silicon is 1 ~ 10 quality %, wherein,
Described composite oxides are higher than 500 DEG C in sintering temperature and make under the condition of less than 520 DEG C,
The solid acid amount adopting pyridine adsorption method to obtain is more than 0.30mmol/g and regenerate with water restoring degree is more than 0.70.
2. waste gas purification catalysts for treating according to claim 1, wherein, described titanyl compound content is in the catalyst 70 ~ 98 quality %.
3. waste gas purification catalysts for treating according to claim 1, wherein, described titanyl compound content is in the catalyst 77 ~ 93 quality %.
4. waste gas purification catalysts for treating according to claim 1 and 2, wherein, the oxide content in the catalyst of described vanadium is 1 ~ 20 quality %.
5. waste gas purification catalysts for treating according to claim 1 and 2, wherein, the oxide content in the catalyst of described vanadium is 5 ~ 15 quality %.
6. waste gas purification catalysts for treating according to claim 1, wherein, described regenerate with water restoring degree is more than 0.75.
7. the manufacture method of the waste gas purification catalysts for treating according to any one of claim 1 ~ 6, the method comprises:
After the slaine of the slaine of titanium or alkoxide and silicon or alkoxide are mixed, carry out co-precipitation or hydrolysis, obtain the operation of the slurry of complex hydroxide thus;
The slurry of described complex hydroxide is dewatered, cleans the wet cake that obtains, then make it dry, then higher than 500 DEG C and the scope of less than 520 DEG C sinter, obtain the operation of composite oxides; And using described composite oxides as carrier, add the aqueous solution of the salt of vanadic acid and sinter, manufacturing the operation of catalyst thus.
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| JP2012-147765 | 2012-06-29 | ||
| JP2012147765A JP6032974B2 (en) | 2012-06-29 | 2012-06-29 | Method for producing exhaust gas purification catalyst |
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| BR112019012724A2 (en) * | 2016-12-20 | 2019-11-26 | Umicore Ag & Co Kg | scr catalyst device containing vanadium oxide and molecular sieve containing iron |
| CN114950032A (en) * | 2022-06-13 | 2022-08-30 | 湖南奇思环保设备制造有限公司 | Garbage pyrolysis treatment system |
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| CN102523735A (en) * | 2009-07-31 | 2012-06-27 | 美礼联无机化工公司 | Silica-stabilized ultrafine anatase titania, vanadia catalysts, and methods of production thereof |
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| US4929586A (en) * | 1988-06-09 | 1990-05-29 | W. R. Grace & Co.-Conn. | Catalysts for selective catalytic reduction DeNOx technology |
| JPH11300213A (en) * | 1998-04-22 | 1999-11-02 | Mitsubishi Heavy Ind Ltd | Denitration catalyst |
| JP4680748B2 (en) * | 2004-11-08 | 2011-05-11 | 株式会社日本触媒 | Exhaust gas treatment catalyst and exhaust gas treatment method |
| JP4999388B2 (en) * | 2006-07-24 | 2012-08-15 | 日揮触媒化成株式会社 | Modified titanium oxide particles, method for producing the same, and exhaust gas treatment catalyst using the modified titanium oxide particles |
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| CN102523735A (en) * | 2009-07-31 | 2012-06-27 | 美礼联无机化工公司 | Silica-stabilized ultrafine anatase titania, vanadia catalysts, and methods of production thereof |
Non-Patent Citations (4)
| Title |
|---|
| Dispersion and thermal stability of vanadium oxide catalysts supported on titania-silica mixed oxide;B. Mahipal Reddy et al.;《Catalysis Letters》;19931231;第20卷;317-327 * |
| Study of Dispersion and Thermal Stability of V2O5/TiO2-SiO2 Catalysts by XPS and Other Techniques;Benjaram M. Reddy et al.;《J. Phys. Chem. B》;19971231;第101卷;1769-1774 * |
| TiO2-SiO2 and V2O5/TiO2-SiO2 catalyst: Physico-chemical characteristics and catalytic behavior in selective catalytic reduction of NO by NH3;Motonobu Kobayashi et al.;《Applied Catalysis B: Environmental》;20050414;第60卷;173–179 * |
| V2O5/TiO2-SiO2表面酸性对选择性催化还原NO及抗碱金属性能的影响;胡石磊等;《无机化学学报》;20080731;第24卷(第7期);1113-1118 * |
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| JP2014008473A (en) | 2014-01-20 |
| JP6032974B2 (en) | 2016-11-30 |
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