JPS58247A - Regenerating method for denitrating catalyst - Google Patents
Regenerating method for denitrating catalystInfo
- Publication number
- JPS58247A JPS58247A JP56098361A JP9836181A JPS58247A JP S58247 A JPS58247 A JP S58247A JP 56098361 A JP56098361 A JP 56098361A JP 9836181 A JP9836181 A JP 9836181A JP S58247 A JPS58247 A JP S58247A
- Authority
- JP
- Japan
- Prior art keywords
- catalyst
- denitrification
- tungsten
- poisoned
- catalysts
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Landscapes
- Exhaust Gas Treatment By Means Of Catalyst (AREA)
- Catalysts (AREA)
Abstract
Description
【発明の詳細な説明】
本発明は各極燃焼装置より排出される排ガス中の窒素酸
化物を、アンモニアの存在下で接触還元除去するために
用いられた少なくともバナジウム、チタニアを含む被毒
脱硝触媒の再生法に関するものである。DETAILED DESCRIPTION OF THE INVENTION The present invention provides a poisoned denitrification catalyst containing at least vanadium and titania, which is used for catalytic reduction removal of nitrogen oxides in the exhaust gas discharged from each pole combustion device in the presence of ammonia. It concerns the regeneration method.
各稙燃焼装置より排出される腓ガス中に含まれる窒素酸
化物は大気汚染の原因物質の一つであ・るのでその除去
法が種々提案されているが、その中でも特に還元剤とし
てのアンモニアの存在下で排ガスを触媒と接触させて、
窒素酸化物を窒素と水に分解する接触還元法が多く実用
化されている。Nitrogen oxides contained in the gas emitted from various combustion devices are one of the causes of air pollution, and various methods have been proposed to remove them. by contacting the exhaust gas with a catalyst in the presence of
Many catalytic reduction methods for decomposing nitrogen oxides into nitrogen and water have been put into practical use.
そして、この接触還元法に用いられる脱硝触媒はバナジ
ウムおよびチタニアを含む触媒が優れた活性と長い寿命
を有するので最も多く用いられている。しかしながら、
これらのバナジウムおよびチタニアを含む脱硝触媒も長
時間の使用により排ガス中に含まれるダストの付着堆積
や排ガス中に含まれるＳＯ□ガスの脱硝触媒によるＳ０
３への転化にもとづくアンモニアガスとの反応により硫
酸アンモニウムを生成し、そのｉｌ！ｌＩｌ！アンモニ
ウムが脱硝触媒にｍｔ１１＆ζ付層堆積する等のいわゆ
る触媒被毒により、脱硝特性が大巾に低下することが避
けられないものであった。そして、従来、このような被
毒脱硝触媒の再生法としては、例えば水洗後α〜ＳＯＯ
℃で焼成する方法（特開昭５ｔ−ｔｏぶり６号）、水又
は補熱ｔｓ酸溶液で洗浄するか又は蒸気を吹きつける方
法（特開昭５コーλり０９Ｆ／号）、蓚酸水溶液を接触
させバナジウム成分の一部を抽出後バナジウム化合物な
含浸担持し焼成する方法（特開＠３９−１０２９１１号
）勢が提案され実施されている。これらの洗浄処理法に
より、触媒に付着したダストや水溶性の触媒劣化の原因
物質がある一度まで除去されるため触媒性能の回復効果
はかなり認められる。As the denitrification catalyst used in this catalytic reduction method, catalysts containing vanadium and titania are most often used because they have excellent activity and long life. however,
These denitrification catalysts containing vanadium and titania also cause the accumulation of dust contained in exhaust gas and the SO□ gas contained in exhaust gas due to the denitration catalyst due to long-term use.
The reaction with ammonia gas based on the conversion to 3 produces ammonium sulfate, and its il! lIl! Due to so-called catalyst poisoning, such as ammonium depositing mt11 and ζ layers on the denitrification catalyst, it was inevitable that the denitrification properties would be greatly reduced. Conventionally, as a method for regenerating such a poisoned denitrification catalyst, for example, after washing with water α~SOO
℃ firing method (Japanese Patent Application Laid-open No. 5 T-Toburi No. 6), method of washing with water or reheating TS acid solution or spraying with steam (Japanese Patent Application Laid-open No. 5 Co., Ltd. A method (Japanese Patent Application Laid-open No. 39-102911) has been proposed and implemented, in which a part of the vanadium component is extracted by contacting the material, and then impregnated and supported with a vanadium compound and fired. With these cleaning treatment methods, dust adhering to the catalyst and water-soluble substances that cause catalyst deterioration can be removed to a certain extent, so the effect of restoring the catalyst performance can be recognized to a considerable extent.
しかしながら、触媒被毒にともなって増加したＳ０２転
化率を十分低下回復することができず、必ずしも満足で
きる脱硝触媒の再生法ではなかった。However, it was not possible to sufficiently reduce and recover the S02 conversion rate that increased due to catalyst poisoning, and this method was not necessarily a satisfactory method for regenerating the denitrification catalyst.
本発明の脱硝触媒の再生法は、従来のこのような欠点を
解決するためになされたものであり、特に触媒性能およ
びＳＯ２転化率の特性回復に優れた触媒の再生法であり
、排ガス中の菫素酸化物をアンモニアの存在下で接触還
元除去する少なくとも。The denitrification catalyst regeneration method of the present invention has been developed to solve these conventional drawbacks, and is a catalyst regeneration method that is particularly excellent in recovering the characteristics of catalyst performance and SO2 conversion rate. At least phosphorus oxide is removed by catalytic reduction in the presence of ammonia.
バナジウム、チタニアを含む脱硝触媒の再生法において
、被毒触媒を水又は無４ｉＩ１１１！溶液で洗浄した後
、タングステンを含有する溶液に浸漬し、触媒の見掛は
体＠ｉｍ３当りＷＯ３に換算して０．０／ ７９〜１０
ｋｇのタングステン化合物を触媒に含浸担持し、次いで
乾燥後ダ００−≦ＳＯ″Ｃで焼成する脱硝触媒の再生法
である。In a method for regenerating a denitrification catalyst containing vanadium and titania, the poisoned catalyst is treated with water or without 4iI111! After washing with a solution, it is immersed in a solution containing tungsten, and the apparent appearance of the catalyst is 0.0/79-10 in terms of WO3 per body@im3.
This is a method for regenerating a denitrification catalyst, in which kg of a tungsten compound is impregnated and supported on the catalyst, and then dried and then calcined at a temperature of 00-≦SO''C.
以下、本発明を更に詳しく説明する。The present invention will be explained in more detail below.
バナジウム−チタニア糸触媒、バナジウム成分、ングス
テンーチ貞ニア系触媒あるいはこれらの成分の中にモリ
ブデン、鉄、＃ｌ、クロム、ニッケル。Vanadium-titania thread catalyst, vanadium component, stainless steel catalyst, or molybdenum, iron, #l, chromium, nickel among these components.
コバルト、セリウム等の触媒活性物質のｌ種以上を含有
する少なくともバナジウム、チタニアを含む脱硝触媒よ
りなり、長時間の使用により脱硝性能の低下したいわゆ
る被毒脱硝触媒を常温〜ｔｏ℃の水又は温水、あるいは
１０ ％以下の濃度の塩酸、硫！！等の無機酸溶液中で
例えば超音波洗浄等で洗浄する。この洗浄により触媒表
面および内部に入り込んだダストとともにアルカリ金属
化合物や触媒成分と反応した水溶性の被毒物質等がＶ７
Ｉ４＊される。この場合、洗浄に要する時間はダスＦや
被毒物質の付着状況や洗浄液の温度、無機酸の濃度、攪
拌等の条件に上り員なるが通常１０分〜３時間程度でよ
い。この洗浄によりダストや被毒物質を除去した触媒を
乾燥し、その触媒をタングステンを含む溶液中に浸漬し
、触媒の見掛は体積ｔ ｍ３当りＷＯ，に換算してｏ、
ｏｌＪ１９〜ｌｏｋｇ、好ましくは０．／に９〜３Ｉ１
９のタングステン化合物を触媒に含浸担持させた後、ｗ
ｏｏ℃〜ｔｓｏ ’ｃ、好ましくはｊｏｏ℃〜１００℃
で焼成する触媒の再生法である。なお、含浸に用いるタ
ングステン、を含む溶液としては、パラタングステン酸
アンモニウムをモノエタノールアミンやメタノールアミ
ン等のｉｍ溶剤に溶解したものや、市販のタングステン
酸水溶液を用いるとよい。The so-called poisoned denitrification catalyst, which is made of a denitrification catalyst containing at least vanadium and titania and contains l or more of catalytically active substances such as cobalt and cerium, and whose denitrification performance has deteriorated due to long-term use, is washed with water at room temperature to up to ℃ or hot water. , or hydrochloric acid or sulfuric acid at a concentration of 10% or less! ! for example, by ultrasonic cleaning or the like in an inorganic acid solution such as This cleaning removes the dust that has entered the catalyst surface and inside, as well as water-soluble poisonous substances that have reacted with alkali metal compounds and catalyst components.
I4* will be done. In this case, the time required for cleaning depends on conditions such as the adhesion status of dust F and poisonous substances, the temperature of the cleaning liquid, the concentration of inorganic acid, and stirring, but it is usually about 10 minutes to 3 hours. The catalyst from which dust and poisonous substances have been removed by this washing is dried, and the catalyst is immersed in a solution containing tungsten.
olJ19~lokg, preferably 0. / to 9~3I1
After impregnating and supporting the tungsten compound of No. 9 on the catalyst, w
oo℃~tso'c, preferably joo℃~100℃
This is a catalyst regeneration method that involves firing the catalyst. As the solution containing tungsten used for impregnation, it is preferable to use a solution obtained by dissolving ammonium paratungstate in an im solvent such as monoethanolamine or methanolamine, or a commercially available aqueous tungstic acid solution.
また、ＷＯ３の含浸担持の方法としては、目標とする担
持蓋に合わせてＷＯ３の濃度を＃１壊し一度で含浸させ
てもよいし、畑い１１１度の液を用いて繰り返し含浸し
担持させてもよいが、ＷＯ３の担持量が０．０／ ｌｅ
ｇ／ｍ３以下では脱硝率と８０２転化率の回復効果が小
さいため好ましくなく、また１０ Ｖｍ３以上相持して
も脱硝率およびＳＯ２転化率のいずれも効果の向上があ
まり期待できず、経済的に意味がないためである。In addition, as a method for impregnating and supporting WO3, the concentration of WO3 may be reduced to #1 and impregnated at once depending on the target support lid, or it may be repeatedly impregnated and supported using a 111 degree solution. However, the supported amount of WO3 is 0.0/le
If it is less than 10 Vm3, the recovery effect on the denitrification rate and 802 conversion rate is unfavorable, and if it is more than 10 Vm3, neither the denitrification rate nor the SO2 conversion rate can be expected to improve much, so it is not economically meaningful. This is because there is no.
さらに、担持後の焼成温度を１００″Ｃ〜ｔｓｏ”ｃに
するのは、ｔｉｏｏ”ｃ以下では相持したタングステン
化合物が完全にＷＯ３になりきらないためであり６ｊＯ
℃以上では元の触媒に含有されているバナジウム成分が
溶融を起こし、触媒比表面積の低下を招き、脱硝率の低
下とＳｏ、転化率の増加を生ずるためである。なお、本
発明で再生処理ができる少なくともバナジウム、チタニ
アを含む脱硝触媒としては、ムライト、コージェライト
略の基材上に活性物質を担持したいわゆる被覆触媒でも
あるいは活性物質で触媒を形成したいわゆるソリッド触
媒でもよく、また触媒の形状はハニカム状、ペレット状
、パイプ状等のいずれもよいものである。Furthermore, the reason why the firing temperature after supporting is set to 100"C to tso"c is because the supported tungsten compound cannot completely become WO3 below tioo"c, and 6jO
This is because when the temperature exceeds .degree. C., the vanadium component contained in the original catalyst melts, leading to a decrease in the specific surface area of the catalyst, resulting in a decrease in the denitrification rate and an increase in the So and conversion rate. The denitrification catalyst containing at least vanadium and titania that can be regenerated in the present invention may be a so-called coated catalyst in which an active substance is supported on a base material such as mullite or cordierite, or a so-called solid catalyst in which an active substance is formed as a catalyst. The shape of the catalyst may be honeycomb, pellet, pipe, etc.
次に、本発明を実施例により具体的に説明する。Next, the present invention will be specifically explained using examples.
触媒成分としテｖ２ｏ、 ｚ、ｏ％、ＴｉＯ，９７Ｓ
ｔｐ ラ’ｊ ルハニカム触媒（以下触媒ムという）お
よびＶＱＯ。Catalyst component: Tiv2o, z, o%, TiO, 97S
tp la'j honeycomb catalyst (hereinafter referred to as catalyst) and VQO.
／、０％、ｗｏ、７．０％、Ｔｉｅ、 ｖｘ％からな６
ハニカＡ触媒（以下触媒Ｂという） ％ Ｖ、Ｏ，／
、０ ％、１００３５４％、Ｔ１０□りＪ、１％、から
なるへ二カム触媒（以下触媒０という）、ｖ、ｏ、 Ｊ
、ｏ％、Ｆｅ、Ｏ，３，０％、ＯｕＯコ、ｊｌＴｉＯ□
デλ、５％からなる八ニカ、ム触媒（以下触媒りという
）、Ｖ２Ｏ５／、０ ％、Ｗｏｏ３Ｊ、０憾、ｗｏ、
ｚ、ｏ囁、ＴｉＯ□ｑｉ、ｏ％からなるノ為二カム触媒
（以下触媒Ｅという）を用い第１表に示した条件でボイ
ラー排ガス中で１２０００時間使用したところ３１０℃
におする脱硝率とＳ０２転化率は第２表に示すように初
期に比べ触媒性能の低下が起こった。/, 0%, wo, 7.0%, Tie, vx%6
Honeycomb A catalyst (hereinafter referred to as catalyst B) % V, O, /
, 0%, 100354%, T10□riJ, 1%, Henicam catalyst (hereinafter referred to as catalyst 0), v, o, J
,o%,Fe,O,3,0%,OuOko,jlTiO□
deλ, 5%, mu catalyst (hereinafter referred to as catalyst), V2O5/, 0%, Woo3J, 0 regret, wo,
When used for 12,000 hours in boiler exhaust gas under the conditions shown in Table 1 using a non-taming catalyst (hereinafter referred to as catalyst E) consisting of z, o, TiO□qi, and o%, the temperature reached 310°C.
As shown in Table 2, the denitrification rate and S02 conversion rate decreased compared to the initial stage.
第１表
第２表
この性能の低下したｊつの被毒触媒を第３表に′示した
条件で、触媒の見掛は体積の３倍の水又は無機酸の水溶
液中で超音波洗浄装置を用い洗浄した後、ハラタングス
テン酸アンモニウムのモノエタノールアミン溶解溶液中
に触媒を浸漬しＷＯ２に換算して第３表に記−する蓋含
浸拒持し、ついで乾燥、第３表中に記載する条件で焼成
して再生触媒轟／ −Ａ ｎを得た。そして、これらの
再生した触媒を第１表に示した排ガス条件下で脱硝率お
よび８０２転化率を比較測定した。結未は第３表に記載
するとおりである。なお、比較のために本発明の範囲外
の、ものを比較例として、又、従来法のものを従来例と
して第３表に併せ記載した。Table 1 Table 2 These poisoned catalysts with degraded performance are shown in Table 3. Under the conditions shown in Table 3, the apparent appearance of the catalysts is reduced by ultrasonic cleaning in three times the volume of water or an aqueous solution of inorganic acid. After washing, the catalyst was immersed in a solution of ammonium halatungstate in monoethanolamine, impregnated with a cap as shown in Table 3 in terms of WO2, and then dried under the conditions listed in Table 3. A regenerated catalyst Todoroki/-An was obtained. Then, the denitrification rate and 802 conversion rate of these regenerated catalysts were comparatively measured under the exhaust gas conditions shown in Table 1. The results are as shown in Table 3. For comparison, those outside the scope of the present invention are listed as comparative examples, and those made using conventional methods are listed as conventional examples in Table 3.
第３表の結果より明らかなとおり、本発明の触媒の再生
法によれば、脱硝率および８０２転化率とも初期特性ま
で完全に回復することができるが、本発明範囲外のもの
および従来法のものは脱硝率およびＳＯ□転化率とも初
期値まで回復することはできないものであった。As is clear from the results in Table 3, according to the catalyst regeneration method of the present invention, both the denitrification rate and the 802 conversion rate can be completely restored to their initial characteristics. Both the denitrification rate and the SO□ conversion rate could not be recovered to their initial values.
以上、述べたとおり本発明は、バナジウム、チタニアを
含む被毒脱硝触媒を洗浄した後、タングステンの所定量
を含浸担持する簡単な操作により、脱硝率および８０２
転化率とも初期値まで完−全に回復することができる再
生法であり、現在火力発電所尋のボイラー排ガス中の窒
素酸化＠除去に大意に用いられているバナジウム、チタ
ニアを含む脱硝触媒の再生法として極めて有用であり、
産業上ｌｚ＆な被毒脱硝触媒の再生法である。As described above, the present invention improves the denitrification rate by impregnating and supporting a predetermined amount of tungsten after cleaning the poisoned denitrification catalyst containing vanadium and titania.
This is a regeneration method that can completely restore the conversion rate to its initial value, and is currently used to regenerate denitrification catalysts containing vanadium and titania, which are widely used for removing nitrogen oxidation from boiler exhaust gas at thermal power plants. extremely useful as a law;
This is an industrially useful method for regenerating poisoned denitrification catalysts.
Claims (1)
触還元除去する少なくともバナジウム。 チタニアを含む脱硝触媒の再生法において、被毒触媒を
水又は無機酸溶液で洗浄した後タングステンを含有する
溶液に渋漬し触媒の見掛は体積ｔ ｍ３当りＷＯ２に換
算して０．０／に９〜１０ｋｇのタングステン化合物を
触媒に含＊坦持し、次いで乾燥後４１００Ｎ≦ＳＯ℃で
焼成することを特徴とする脱硝触媒の再生法。[Claims] Li1 - At least vanadium for removing nitrogen oxides in gas by catalytic reduction in the presence of ammonia. In a method for regenerating a denitrification catalyst containing titania, the poisoned catalyst is washed with water or an inorganic acid solution and then soaked in a solution containing tungsten, so that the apparent appearance of the catalyst is 0.0/m3 in terms of WO2/volume tm3. A method for regenerating a denitrification catalyst, which comprises supporting 9 to 10 kg of a tungsten compound on the catalyst, drying it, and then firing it at 4100N≦SO°C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP56098361A JPS58247A (en) | 1981-06-26 | 1981-06-26 | Regenerating method for denitrating catalyst |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP56098361A JPS58247A (en) | 1981-06-26 | 1981-06-26 | Regenerating method for denitrating catalyst |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS58247A true JPS58247A (en) | 1983-01-05 |
| JPS6248537B2 JPS6248537B2 (en) | 1987-10-14 |
Family
ID=14217734
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP56098361A Granted JPS58247A (en) | 1981-06-26 | 1981-06-26 | Regenerating method for denitrating catalyst |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS58247A (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6034743A (en) * | 1983-08-08 | 1985-02-22 | Babcock Hitachi Kk | Regeneration of used denitration catalyst |
| JPS60209252A (en) * | 1984-04-03 | 1985-10-21 | Mitsubishi Heavy Ind Ltd | Regeneration method of denitration catalyst |
| JPS60212238A (en) * | 1984-04-05 | 1985-10-24 | Mitsubishi Heavy Ind Ltd | Regeneration of ammonia catalytic reducing and denitration catalyst |
| JPS6470144A (en) * | 1987-06-05 | 1989-03-15 | Babcock Hitachi Kk | Denitration catalyst utilizing catalytic-reduction of ammonia and its production |
| EP0974397A2 (en) * | 1998-07-24 | 2000-01-26 | Mitsubishi Heavy Industries, Ltd. | Methods for the regeneration of a denitration catalyst |
| WO2000012211A1 (en) * | 1998-08-26 | 2000-03-09 | Integral Umwelt- Und Anlagentechnik Gesellschaft Mbh | METHOD FOR REGENERATING USED DeNOx OR DeDIOXIN CATALYTIC CONVERTERS |
| CN106944138A (en) * | 2016-01-07 | 2017-07-14 | 中国石油化工股份有限公司 | A kind of Application way of useless hydrogenation catalyst |
| CN106944114A (en) * | 2016-01-07 | 2017-07-14 | 中国石油化工股份有限公司 | A kind of Application way of useless hydrotreating catalyst |
-
1981
- 1981-06-26 JP JP56098361A patent/JPS58247A/en active Granted
Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6034743A (en) * | 1983-08-08 | 1985-02-22 | Babcock Hitachi Kk | Regeneration of used denitration catalyst |
| JPH0446621B2 (en) * | 1983-08-08 | 1992-07-30 | Babcock Hitachi Kk | |
| JPS60209252A (en) * | 1984-04-03 | 1985-10-21 | Mitsubishi Heavy Ind Ltd | Regeneration method of denitration catalyst |
| JPH0534057B2 (en) * | 1984-04-03 | 1993-05-21 | Mitsubishi Heavy Ind Ltd | |
| JPS60212238A (en) * | 1984-04-05 | 1985-10-24 | Mitsubishi Heavy Ind Ltd | Regeneration of ammonia catalytic reducing and denitration catalyst |
| JPH0417701B2 (en) * | 1984-04-05 | 1992-03-26 | Mitsubishi Heavy Ind Ltd | |
| JPS6470144A (en) * | 1987-06-05 | 1989-03-15 | Babcock Hitachi Kk | Denitration catalyst utilizing catalytic-reduction of ammonia and its production |
| JP2991431B2 (en) * | 1987-06-05 | 1999-12-20 | バブコツク日立株式会社 | Catalyst for catalytic reduction and denitration of ammonia and its production method |
| EP0974397A2 (en) * | 1998-07-24 | 2000-01-26 | Mitsubishi Heavy Industries, Ltd. | Methods for the regeneration of a denitration catalyst |
| EP0974397A3 (en) * | 1998-07-24 | 2000-05-03 | Mitsubishi Heavy Industries, Ltd. | Methods for the regeneration of a denitration catalyst |
| US6395665B2 (en) | 1998-07-24 | 2002-05-28 | Mitsubishi Heavy Industries, Ltd. | Methods for the regeneration of a denitration catalyst |
| EP1325779A1 (en) * | 1998-07-24 | 2003-07-09 | Mitsubishi Heavy Industries, Ltd. | Methods for the regeneration of a denitration catalyst |
| WO2000012211A1 (en) * | 1998-08-26 | 2000-03-09 | Integral Umwelt- Und Anlagentechnik Gesellschaft Mbh | METHOD FOR REGENERATING USED DeNOx OR DeDIOXIN CATALYTIC CONVERTERS |
| EP1107824B1 (en) * | 1998-08-26 | 2001-12-05 | INTEGRAL UMWELT- UND ANLAGENTECHNIK GESSELLSCHAFT m.b.H. | METHOD FOR REGENERATING USED DeNOx OR DeDIOXIN CATALYTIC CONVERTERS |
| CN106944138A (en) * | 2016-01-07 | 2017-07-14 | 中国石油化工股份有限公司 | A kind of Application way of useless hydrogenation catalyst |
| CN106944114A (en) * | 2016-01-07 | 2017-07-14 | 中国石油化工股份有限公司 | A kind of Application way of useless hydrotreating catalyst |
| CN106944138B (en) * | 2016-01-07 | 2019-07-12 | 中国石油化工股份有限公司 | A kind of utilization method of useless hydrogenation catalyst |
| CN106944114B (en) * | 2016-01-07 | 2019-08-06 | 中国石油化工股份有限公司 | A kind of utilization method of useless hydrotreating catalyst |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS6248537B2 (en) | 1987-10-14 |
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