CN111760578A - SCR denitration catalyst regeneration active liquid and preparation method thereof - Google Patents
SCR denitration catalyst regeneration active liquid and preparation method thereof Download PDFInfo
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- B01J38/00—Regeneration or reactivation of catalysts, in general
- B01J38/48—Liquid treating or treating in liquid phase, e.g. dissolved or suspended
- B01J38/68—Liquid treating or treating in liquid phase, e.g. dissolved or suspended including substantial dissolution or chemical precipitation of a catalyst component in the ultimate reconstitution of the catalyst
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Abstract
The invention relates to an SCR denitration catalyst regeneration active liquid and a preparation method thereof, wherein the SCR denitration catalyst regeneration active liquid comprises 0.4-1.0 wt% of ammonium metavanadate, 0.4-4.0 wt% of oxalic acid and/or formic acid, 0.8-4.0 wt% of ammonium tungstate, 0.6-4.0 wt% of ammonium molybdate and 87-98.8 wt% of tap water and/or desalted water; the sum of the weight percentages of the components is 100 percent.
Description
Technical Field
The invention relates to the technical field of catalyst recovery and regeneration, in particular to an active liquid for SCR denitration catalyst regeneration and a preparation method thereof.
Background
The flue gas denitration transformation of the thermal power plant adopting the SCR technology in large scale in China begins in 2010, and the earliest flue gas denitration system can be traced to 2008. The chemical life of the vanadium-titanium catalyst used for SCR flue gas denitration is 20000-24000 hours, and the mechanical life is 10 years. However, in practical application, due to the influence of product quality and operating environment, the catalyst capable of reaching the theoretical life is few, and generally, after 2-3 years of use, the activity is reduced and cleaning and regeneration are needed, and after 6-7 years, the catalyst needs to be updated, so that tens of thousands of tons of waste denitration catalysts per year are generated in recent years.
The SCR denitration catalyst mostly takes TiO2 as a carrier, and V2O5, V2O5-WO3 or V2O5-MoO3 as an active main component, and the SCR denitration catalyst generally has three types, namely a honeycomb type, a plate type and a corrugated type. Studies have shown that the causes of deactivation of SCR catalysts are mainly: catalyst poisoning (alkali metal poisoning, arsenic poisoning, mercury poisoning, etc.), sulfate plugging, fly ash plugging, etc. In recent years, the domestic catalyst regeneration technology is developed rapidly and forms a domestic autonomous brand, and the regeneration method mainly comprises the following steps: water washing regeneration, acid liquor treatment, SO2 acidification and thermal regeneration, etc. The invention researches an SCR catalyst active supplement (hereinafter referred to as regeneration liquid or active liquid) and a preparation method thereof.
Disclosure of Invention
The first purpose of the invention is to provide an active liquid for regenerating an SCR denitration catalyst, which aims to solve the technical problem of forming a substance for supplementing the activity of a deactivated catalyst.
The second purpose of the invention is to provide a preparation method of the regeneration active liquid of the SCR denitration catalyst, which aims to solve the technical problem of forming a substance for activity supplement of the deactivated catalyst.
The SCR denitration catalyst regeneration active liquid is realized by the following steps:
an SCR denitration catalyst regeneration active liquid, comprising: 0.4-1.0% of ammonium metavanadate, 0.4-4.0% of oxalic acid and/or formic acid, 0.8-4.0% of ammonium tungstate, 0.6-4.0% of ammonium molybdate and 87-98.8% of tap water and/or desalted water in percentage by weight; the sum of the weight percentages of the components is 100 percent.
In a preferred embodiment of the invention, the conductivity of the tap water is not more than 600. mu.S/cm.
The preparation method of the SCR denitration catalyst regeneration active liquid is realized by the following steps:
a preparation method of an SCR denitration catalyst regeneration active liquid is characterized by comprising the following steps:
step S1, preparing desalted water or selecting tap water meeting the requirement according to the catalyst deactivation mechanism to form a solvent;
s2, introducing compressed air into the solvent formed in the step S1, stirring, and heating the solvent at the same time, so that the temperature of the solvent is controlled to be 50-70 ℃;
step S3, adding oxalic acid and/or formic acid into the solvent under the heating environment in the step S2, and fully dissolving the oxalic acid and/or formic acid into the solvent to form a cosolvent acid solution;
step S4, adding an active substance ammonium metavanadate which is insoluble in water and has oxidability into the cosolvent acid solution, stirring, controlling the temperature to be 50-70 ℃, reacting for more than 30min, and stopping heating;
and step S5, adding ammonium tungstate and ammonium molybdate into the cosolvent acid solution added with the ammonium metavanadate, and stirring for reacting for more than 30 min.
In a preferred embodiment of the present invention, the weight percentage of the ammonium metavanadate is 0.4 to 1.0%;
the weight percentage of the oxalic acid and/or the formic acid is 0.4-4.0%;
the weight percentage of the ammonium tungstate is 0.8-4.0%;
the weight percentage of the ammonium molybdate is 0.6-4.0%;
the weight percentage of the tap water and/or the desalted water is 87-98.8%.
In a preferred embodiment of the present invention, in step S3, oxalic acid and/or formic acid is added into the solvent in the heating environment of step S2 at a dosing rate of 100kg/h, so that the oxalic acid and/or formic acid is fully dissolved in the solvent to form a cosolvent solution, the temperature is controlled to be 50-70 ℃, and the reaction is carried out for 45 min.
In a preferred embodiment of the present invention, in step S4, ammonium metavanadate is added into the cosolvent acid solution formed in step S3 at a dosing speed of 60kg/h, and the mixture is stirred and reacted for 60min with the temperature controlled at 50-70 ℃.
In a preferred embodiment of the present invention, in step S5, ammonium tungstate and ammonium molybdate are sequentially added to the cosolvent solution to which ammonium metavanadate has been added at a dosing rate of 120kg/h, and then the mixture is bubbled for 90min after the dosing is completed.
Compared with the prior art, the embodiment of the invention has the following beneficial effects: according to the SCR denitration catalyst regeneration active liquid and the preparation method, the adopted active substance metavanadate has oxidability and is slightly soluble in water at normal temperature, so that the reductive carboxylic acid cosolvent oxalic acid and/or formic acid are introduced into the solvent water, the reaction is converted into a vanadium-containing complex which is easily soluble in water, and the vanadium pentoxide is decomposed into vanadium pentoxide after high-temperature treatment during catalyst activity implantation, namely the catalyst effective activity load.
Furthermore, according to different catalyst deactivation mechanisms, water with different qualities can be selected as an active substance solvent, and when tap water is selected as the solvent, the production cost of the activating solution is greatly saved.
Detailed Description
Example 1:
the embodiment provides an active liquid for regenerating an SCR denitration catalyst, which comprises: 0.4-1.0% of ammonium metavanadate, 0.4-4.0% of oxalic acid and/or formic acid, 0.8-4.0% of ammonium tungstate, 0.6-4.0% of ammonium molybdate and 87-98.8% of tap water and/or desalted water in percentage by weight; the sum of the weight percentages of the components is 100 percent.
It should be noted that the conductivity of the tap water is not more than 600. mu.S/cm.
The solvents in this embodiment may be tap water, desalted water, or a mixture of tap water and desalted water, which is not limited in this embodiment. In particular, in the embodiment, water with different qualities can be selected as an active substance solvent according to different catalyst deactivation mechanisms, and when tap water is selected as the solvent, the production cost of the activating solution is greatly saved.
The oxalic acid and/or formic acid in this embodiment mainly play a role of acting as a co-solvent of the reducing carboxylic acid, and here, the oxalic acid alone or the formic acid alone may be used, or of course, a mixture of the oxalic acid and the formic acid may be used, which is not limited in this embodiment.
Example 2:
the embodiment provides a preparation method of an SCR denitration catalyst regeneration active liquid, which comprises the following steps:
step S1, preparing desalted water or selecting tap water meeting the requirement according to the catalyst deactivation mechanism to form a solvent;
s2, introducing compressed air into the solvent formed in the step S1, stirring, and heating the solvent at the same time, so that the temperature of the solvent is controlled to be 50-70 ℃;
step S3, adding oxalic acid and/or formic acid into the solvent under the heating environment in the step S2, and fully dissolving the oxalic acid and/or formic acid into the solvent to form a cosolvent acid solution;
step S4, adding an active substance ammonium metavanadate which is insoluble in water and has oxidability into the cosolvent acid solution, stirring, controlling the temperature to be 50-70 ℃, reacting for more than 30min, and stopping heating;
and step S5, adding ammonium tungstate and ammonium molybdate into the cosolvent acid solution added with the ammonium metavanadate, and stirring for reacting for more than 30 min.
Specifically, the components in the steps are as follows by weight percent:
the weight percentage of the ammonium metavanadate is 0.4-1.0%; the weight percentage of the oxalic acid and/or the formic acid is 0.4-4.0%; the weight percentage of the ammonium tungstate is 0.8-4.0%; the weight percentage of the ammonium molybdate is 0.6-4.0%; the weight percentage of the tap water and/or the desalted water is 87-98.8%, and the sum of the weight percentages of the above components is 100%.
In a specific optional implementation case, in step S3, adding oxalic acid and/or formic acid into the solvent in the heating environment of step S2 at a dosing speed of 100kg/h, so that the oxalic acid and/or formic acid is sufficiently dissolved in the solvent to form a cosolvent acid solution, controlling the temperature to be 50-70 ℃, and reacting for 45 min.
In a specific optional implementation case, in step S4, adding ammonium metavanadate into the cosolvent acid solution formed in step S3 at a dosing speed of 60kg/h, stirring, controlling the temperature to be 50-70 ℃, and reacting for 60 min.
In a specific alternative implementation case, in step S5, ammonium tungstate and ammonium molybdate are sequentially added to the cosolvent acid solution to which ammonium metavanadate has been added at a dosing rate of 120kg/h, and after the dosing is completed, a bubbling reaction is performed for 90 min.
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (7)
1. An SCR denitration catalyst regeneration active liquid is characterized by comprising: 0.4-1.0% of ammonium metavanadate, 0.4-4.0% of oxalic acid and/or formic acid, 0.8-4.0% of ammonium tungstate, 0.6-4.0% of ammonium molybdate and 87-98.8% of tap water and/or desalted water in percentage by weight; the sum of the weight percentages of the components is 100 percent.
2. The SCR denitration catalyst regeneration active liquid according to claim 1, wherein an electrical conductivity of the tap water is not more than 600 μ S/cm.
3. A preparation method of an SCR denitration catalyst regeneration active liquid is characterized by comprising the following steps:
step S1, preparing desalted water or selecting tap water meeting the requirement according to the catalyst deactivation mechanism to form a solvent;
s2, introducing compressed air into the solvent formed in the step S1, stirring, and heating the solvent at the same time, so that the temperature of the solvent is controlled to be 50-70 ℃;
step S3, adding oxalic acid and/or formic acid into the solvent under the heating environment in the step S2, and fully dissolving the oxalic acid and/or formic acid into the solvent to form a cosolvent acid solution;
step S4, adding an active substance ammonium metavanadate which is insoluble in water and has oxidability into the cosolvent acid solution, stirring, controlling the temperature to be 50-70 ℃, reacting for more than 30min, and stopping heating;
and step S5, adding ammonium tungstate and ammonium molybdate into the cosolvent acid solution added with the ammonium metavanadate, and stirring for reacting for more than 30 min.
4. The method for preparing the regeneration active liquid of the SCR denitration catalyst according to claim 3, wherein the weight percentage of the ammonium metavanadate is 0.4-1.0%;
the weight percentage of the oxalic acid and/or the formic acid is 0.4-4.0%;
the weight percentage of the ammonium tungstate is 0.8-4.0%;
the weight percentage of the ammonium molybdate is 0.6-4.0%;
the weight percentage of the tap water and/or the desalted water is 87-98.8%.
5. The method for preparing the SCR denitration catalyst regeneration active liquid according to any one of claims 3 or 4, wherein in step S3, oxalic acid and/or formic acid is added into the solvent under the heating environment of step S2 at a dosing speed of 100kg/h, and is sufficiently dissolved in the solvent to form a cosolvent acid solution, the temperature is controlled at 50-70 ℃, and the reaction is carried out for 45 min.
6. The method for preparing the SCR denitration catalyst regeneration active liquid according to any one of claims 3 or 4, wherein in step S4, ammonium metavanadate is added into the cosolvent acid solution formed in step S3 at a dosing speed of 60kg/h, and the reaction is carried out for 60min while stirring and controlling the temperature to be 50-70 ℃.
7. The method of preparing an SCR denitration catalyst regeneration active liquid according to any one of claims 3 or 4, wherein in step S5, ammonium tungstate and ammonium molybdate are added to the hydrotropic solution to which ammonium metavanadate has been added in sequence at a dosing rate of 120kg/h, and after the dosing is completed, a bubbling reaction is performed for 90 min.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114713292A (en) * | 2022-05-05 | 2022-07-08 | 安徽工程大学 | End face treating agent, preparation method and application thereof, and end face treatment method after catalyst regeneration |
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| CN103551209A (en) * | 2013-10-23 | 2014-02-05 | 广东电网公司电力科学研究院 | Activated regeneration solution for selective catalyst reduction (SCR) flue gas denitration catalyst and preparation method of activated regeneration solution |
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| JP2020015029A (en) * | 2018-07-27 | 2020-01-30 | 三菱日立パワーシステムズ株式会社 | Regeneration method of used denitration catalyst |
| CN111318316A (en) * | 2020-02-28 | 2020-06-23 | 江苏峰业科技环保集团股份有限公司 | SCR flue gas denitration catalyst regeneration liquid and preparation method thereof |
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- 2020-08-03 CN CN202010767341.7A patent/CN111760578A/en not_active Withdrawn
Patent Citations (5)
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| CN102935388A (en) * | 2012-10-22 | 2013-02-20 | 广东电网公司电力科学研究院 | Antitoxic regeneration solution of deactivated SCR denitration catalyst, and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114713292A (en) * | 2022-05-05 | 2022-07-08 | 安徽工程大学 | End face treating agent, preparation method and application thereof, and end face treatment method after catalyst regeneration |
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