CN102974368A - Deactivated SCR denitration catalyst regeneration method - Google Patents

Deactivated SCR denitration catalyst regeneration method Download PDF

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CN102974368A
CN102974368A CN2012104425213A CN201210442521A CN102974368A CN 102974368 A CN102974368 A CN 102974368A CN 2012104425213 A CN2012104425213 A CN 2012104425213A CN 201210442521 A CN201210442521 A CN 201210442521A CN 102974368 A CN102974368 A CN 102974368A
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catalyst
liquid
30min
regenerated
modification
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CN2012104425213A
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CN102974368B (en
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盘思伟
汤龙华
韦正乐
李丽
赵宁
黄碧纯
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广东电网公司电力科学研究院
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Abstract

A deactivated SCR denitration catalyst regeneration method includes: (1) preparing a reproduction solution including a cleaning liquid and an activity replenisher; (2) preparing an antitoxic modified liquid; (3) purging the catalyst with oil-free compressed air for 30-60 min; (4) immersing the catalyst processed by (3) in a regenerated liquid for 3-5 h accompanied with ultrasonic oscillation, and then drying at 80-110 DEG C for 2h; (5) immersing in an antitoxic modified liquid for 3-5 h accompanied by the ultrasonic oscillation, and then drying at 80-110 DEG C for 2h; (6) conducting oxygen plasma modification in a dielectric barrier reactor to get the regenerated catalyst, wherein the discharge voltage is 5-10kV, and the processing time is 15-30min. The method can remove the poison and replenish active ingredients, and the regenerated addition components are environmental-friendly, low in price, and good in anti-drug performance. The addition of oxygen plasma greatly improves activity and stability of the catalyst.

Description

A kind of renovation process of deactivation SCR denitrating catalyst

Technical field

The present invention relates to a kind of renovation process of catalyst deactivation, particularly be applicable to the renovation process of the SCR of coal-burning power plant denitrating catalyst deactivation.

Background technology

Nitrogen oxide has caused people's extensive concern as one of Air Pollutants owing to can cause acid rain, light pollution, global warming and reduction ozone layer etc.The coal-burning power plant is China NO XThe topmost source of discharge capacity, whole nation generating total installation of generating capacity surpassed 8.18 hundred million kilowatts in 2010, expected the year two thousand twenty and will reach 11.86 hundred million kilowatts.Although the setting of Future in China energy resource structure will be tried one's best the shared specific gravity control of coal in certain scope, so that the speed of thermal power generation future development eases up, but within the quite a while, can't change the ascendancy of coal-fired unit in China's power supply architecture, along with expanding economy, the environmental protection demand grows to even greater heights, China carries out another emphasis behave that emission control is state control thermal power plant pollutant emission after flue gas desulfurization to the continuous reinforcement of coal-burning power plant's discharged nitrous oxides concentration limit to the nitrogen oxide in the coal steam-electric plant smoke.Therefore as a kind of efficient gas denitrifying technology--SCR (Selective catalytic reduction, SCR) technique is widely used, and it mainly is to use ammonia (or other reducing agents) optionally with NO under the effect of catalyst xBe reduced to N 2And H 2The method of O.

As the core of SCR technique, the performance quality of catalyst directly has influence on the whole denitration effect of SCR system.The SCR catalyst of generation current factory assembling is mainly V 2O 5-WO 3/ TiO 2/ cordierite, reaction temperature is 300-500 ℃, is arranged in air preheater and electric cleaner upstream (high grey side), so catalyst is easy to be subject to, and ash content, alkali metal, alkaline-earth metal, arsenic, sulfur dioxide etc. stop up and the impact of poisoning and inactivation.The price of considering denitrating catalyst is higher, if realize efficiently the regeneration of catalyst, will greatly save the denitration cost.

Catalyst recovery process in the patent generally is to purge and wet dip two step pre-treatments through dry type at present, and load and the drying of carrying out active component wait processing again.Patent No. CN101574671A discloses a kind of SCR denitrating catalyst regenerated liquid, this regenerated liquid replenishes liquid, nonionic surface active agent (penetration enhancer JFC+ Surfactant OP-10+ peregal), acid and deionized water by host and forms, adopt infusion process that catalyst is realized cleaning and regeneration synchronously, regeneration rear catalyst activation recovering reaches 90-105%; The patent No. is that the European patent of EP06019991.6 has provided the SCR catalyst that the anti-alkali and alkaline earth metal ions of metal oxide-superpower acidic group is poisoned, and the regeneration of the denitrating catalyst that alkalies and alkaline earth is poisoned has certain inspiration meaning.These methods have all obtained certain SCR catalyst regeneration effect, but still therefore the problem of the aspects such as the easy again inactivation of active and antitoxin poor performance of the catalyst after the existence regeneration, processing complexity needs further developmental research related art method.

Plasma is as a kind of efficient technological means, more and more tightr with contacting of catalyst field, a large amount of studies show that, thereby the catalyst through Cement Composite Treated by Plasma has the raising that the advantages such as specific area is large, rate of reduction fast, catalyst component lattice defect promote catalytic activity, simultaneously its roasting with respect to routine, processing time is short, is very beneficial for industrial production.

Summary of the invention

Technical problem to be solved by this invention, just provide a kind of renovation process of SCR catalyst for denitrating flue gas deactivation, the method not only can make the very high active and antitoxin performance of catalyst recovery stronger, active component environmental protection, the relative low price of adding simultaneously, save the catalyst regeneration cost, used simultaneously plasma to substitute calcination process, large through the specific surface area of catalyst of Cement Composite Treated by Plasma, active dispersion is high, has greatly promoted the stability of the activity of catalyst.

Solve the problems of the technologies described above, the present invention realizes by the following technical solutions:

A kind of renovation process of deactivation SCR denitrating catalyst may further comprise the steps:

(2) comprise cleaning fluid and the active regenerated liquid preparation that replenishes liquid

The cleaning fluid component consists of: sulfuric acid 0.1-0.8mol/L, one or both 0-0.01mol/L of oxalic acid or citric acid; The active fluid component that replenishes consists of: one or more in copper nitrate, ferric nitrate, the cerous nitrate, content are 0.1-1mol/L, bleeding agent (OE-35) 0-0.001mol/L;

Cleaning fluid and the active liquid that replenishes are mixed concussion 20-30min, make it mix to get regenerated liquid;

(2) preparation of antitoxin modification liquid: contain zinc nitrate, antimony acetate, niobium oxalate, methyl alcohol in the antitoxin modification liquid, a small amount of diffusant, zinc nitrate 0.1-1mol/L, antimony acetate 0.5-1mol/L, niobium oxalate 0.5-1mol/L, methyl alcohol 0-0.1mol/L, concussion 20-30min mixes;

The catalyst that (3) will need to regenerate purges 10-30min with oil-free compressed air (0.6MPa);

(4) catalyst soakage of processing through (3) is flooded 3-5h in regenerated liquid, and follow sonic oscillation, again at 80-110 ℃ of dry 2h, repeat at least 2 times;

(5) catalyst soakage of processing through (4) floods 3-5h in antitoxin modification liquid, and follows sonic oscillation, again at 80-110 ℃ of dry 2h;

(6) catalyst of processing through (5) carries out the oxygen plasma modification in the dielectric impedance reactor, discharge voltage is 5-10Kv, processes 15min-30min, the catalyst that obtains regenerating.

Used supersonic frequency is 20-30KHz, time 20-30min.

Used modification plasma is oxygen plasma, and modification voltage is 5-10Kv, time 15-30min.

Beneficial effect:

Again it is carried out replenishing of active component when 1, the present invention cleans the SCR denitrating catalyst of deactivation, and substitute roasting with oxygen plasma it is carried out surface modification, promoted greatly the activity of catalyst, the catalyst activity after the regeneration reaches 90-100%, good stability.

2, the present invention has avoided hypertoxic vanadium to the additional employing of active component comparatively copper nitrate, the ferric nitrate isoreactivity predecessor of environmental protection.

3, the present invention carries out the load of antitoxin component to catalyst, has prolonged the service life of regeneration rear catalyst.

The specific embodiment:

Below by embodiment the present invention is carried out exemplary description, but the following example can not be interpreted as it is limiting the scope of the invention.

Embodiment 1:

(1) preparation of regenerated liquid: preparation regenerated liquid sulfur acid 0.1mol/L, ferric nitrate and cerous nitrate respectively are 0.1mol/L, other adds a small amount of oxalic acid, citric acid and diffusant.With ultrasonic concussion 20min, be made into uniform mixed liquor.

(2) preparation of antitoxin modification liquid: preparation contains zinc nitrate 0.1mol/L, antimony acetate 0.5mol/L, niobium oxalate 0.5mol/L, and other adds a small amount of methyl alcohol and diffusant, with ultrasonic concussion 20min, makes its even mixing.

(3) catalyst of getting certain coal-burning power plant's deactivation is cut into 2.1 * 2.1 * 20(cm) one, with oil-free compressed air (0.6MPa) it is purged 30min.

(4) with above-mentioned catalyst soakage 3h in regenerated liquid, and use ultrasonic concussion, put into again 110 ℃ of dry 2h of drying box.

(5) above-mentioned dry catalyst be impregnated in 3h in the antitoxin modification liquid again, use ultrasonic concussion, again 110 ℃ of dry 2h.

(6) calcined catalyst is put into the dielectric impedance reactor, with discharge process 15min under the 5Kv voltage, reaction atmosphere is O 2, get regenerated catalyst.

Embodiment 2:

(1) preparation of regenerated liquid: preparation regenerated liquid sulfur acid 0.1mol/L, ferric nitrate and cerous nitrate respectively are 0.5mol/L, other adds a small amount of oxalic acid, citric acid and diffusant.With ultrasonic concussion 20min, be made into uniform mixed liquor.

(2) preparation of antitoxin modification liquid: preparation contains zinc nitrate 0.1mol/L, antimony acetate 0.5mol/L, niobium oxalate 0.5mol/L, and other adds a small amount of methyl alcohol and diffusant, with ultrasonic concussion 20min, makes its even mixing.

(3) catalyst of getting certain coal-burning power plant's deactivation is cut into 2.1 * 2.1 * 20(cm) one, with oil-free compressed air (0.6MPa) it is purged 30min.

(4) with above-mentioned catalyst soakage 3h in regenerated liquid, and use ultrasonic concussion, put into again 110 ℃ of dry 2h of drying box.

(5) above-mentioned dry catalyst be impregnated in 3h in the antitoxin modification liquid again, use ultrasonic concussion, again 110 ℃ of dry 2h.

(6) roasting is crossed catalyst and put into the dielectric impedance reactor, with discharge process 15min under the 5Kv voltage, reaction atmosphere is O 2, get regenerated catalyst.

Embodiment 3:

(1) preparation of regenerated liquid: preparation regenerated liquid sulfur acid 0.1mol/L, ferric nitrate and cerous nitrate respectively are 1mol/L, other adds a small amount of oxalic acid, citric acid and diffusant.With ultrasonic concussion 20min, be made into uniform mixed liquor.

(2) preparation of antitoxin modification liquid: preparation contains zinc nitrate 0.1mol/L, antimony acetate 0.5mol/L, niobium oxalate 0.5mol/L, and other adds a small amount of methyl alcohol and diffusant, with ultrasonic concussion 20min, makes its even mixing.

(3) catalyst of getting certain coal-burning power plant's deactivation is cut into 2.1 * 2.1 * 20(cm) one, with oil-free compressed air (0.6MPa) it is purged 30min.

(4) with above-mentioned catalyst soakage 3h in regenerated liquid, and use ultrasonic concussion, put into again 110 ℃ of dry 2h of drying box.

(5) above-mentioned dry catalyst be impregnated in 3h in the antitoxin modification liquid again, use ultrasonic concussion, again 110 ℃ of dry 2h.

(6) baked catalyst is put into the dielectric impedance reactor, with discharge process 15min under the 5Kv voltage, reaction atmosphere is O 2, get regenerated catalyst.

Embodiment 4:

(1) preparation of regenerated liquid: preparation regenerated liquid sulfur acid 0.1mol/L, ferric nitrate and cerous nitrate respectively are 0.1mol/L, other adds a small amount of oxalic acid, citric acid and diffusant.With ultrasonic concussion 20min, be made into uniform mixed liquor.

(2) preparation of antitoxin modification liquid: preparation contains zinc nitrate 0.1mol/L, antimony acetate 0.5mol/L, niobium oxalate 1mol/L, and other adds a small amount of methyl alcohol and diffusant, with ultrasonic concussion 20min, makes its even mixing.

(3) catalyst of getting certain coal-burning power plant's deactivation is cut into 2.1 * 2.1 * 20(cm) one, with oil-free compressed air (0.6MPa) it is purged 30min.

(4) with above-mentioned catalyst soakage 3h in regenerated liquid, and use ultrasonic concussion, put into again 110 ℃ of dry 2h of drying box.

(5) the above-mentioned dry catalyst of crossing be impregnated in 3h in the antitoxin modification liquid again, use ultrasonic concussion, again 110 ℃ of dry 2h.

(6) baked catalyst is put into the dielectric impedance reactor, with discharge process 15min under the 5Kv voltage, reaction atmosphere is O 2, get regenerated catalyst.

Claims (3)

1. the renovation process of a deactivation SCR denitrating catalyst may further comprise the steps:
(1) comprises cleaning fluid and the active regenerated liquid preparation that replenishes liquid
The cleaning fluid component consists of: sulfuric acid 0.1-0.8mol/L, one or both 0-0.01mol/L of oxalic acid or citric acid; The active fluid component that replenishes consists of: one or more in copper nitrate, ferric nitrate, the cerous nitrate, content are 0.1-1mol/L, bleeding agent OE-350-0.001mol/L;
Cleaning fluid and the active liquid that replenishes are mixed, and concussion 20-30min makes its even regenerated liquid that gets;
(2) preparation of antitoxin modification liquid
Zinc nitrate 0.1-1mol/L, antimony acetate 0.5-1mol/L, niobium oxalate 0.5-1mol/L, methyl alcohol 0-0.1mol/L, concussion 20-30min mixes;
The catalyst that (3) will need to regenerate purges 10-30min with the 0.6MPa oil-free compressed air;
(4) catalyst soakage of processing through (3) is flooded 3-5h in regenerated liquid, and follow sonic oscillation, dry 2h in 80-110 ℃ repeats 2 times at least again;
(5) catalyst soakage of processing through (4) floods 3-5h in antitoxin modification liquid, and follows sonic oscillation, drier 2h in 80-110 ℃;
(6) catalyst of processing through (5) places the dielectric impedance reactor to carry out plasma modification, the catalyst that obtains regenerating.
2. the renovation process of deactivation SCR denitrating catalyst according to claim 1, it is characterized in that: the frequency of the sonic oscillation in described step (4) and (5) is 20-30KHz, time 20-30min.
3. the renovation process of deactivation SCR denitrating catalyst according to claim 1, it is characterized in that: the modification plasma in the described step (6) is oxygen plasma, modification voltage is 5-10Kv, time 15-30min.
CN201210442521.3A 2012-11-07 2012-11-07 Deactivated SCR denitration catalyst regeneration method CN102974368B (en)

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103364422A (en) * 2013-07-04 2013-10-23 武汉大学 Method for diagnosing regenerability of inactivating denitration catalyst
CN103433081A (en) * 2013-08-08 2013-12-11 涿州西热环保催化剂有限公司 Regeneration method for honeycomb type SCR (Selective Catalytic Reduction) denitration catalyst
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
CN103949291A (en) * 2014-04-23 2014-07-30 江苏万德环保科技有限公司 Denitration catalyst regeneration solution and preparation method thereof as well as catalyst regeneration method
CN105032501A (en) * 2015-07-15 2015-11-11 浙江浙能催化剂技术有限公司 Method for dredging pore channels of honeycomb SCR (selective catalytic reduction) catalyst
CN105536883A (en) * 2015-12-17 2016-05-04 福建紫荆环境工程技术有限公司 Dry reclamation method for treating failure SCR denitration catalyst by adopting plasma
CN105709861A (en) * 2014-12-05 2016-06-29 中国石油化工股份有限公司 Regeneration method of SCR denitration catalyst
CN105921015A (en) * 2016-07-04 2016-09-07 青岛双瑞海洋环境工程股份有限公司 Soot blowing system of denitrification reactor
CN106179531A (en) * 2016-07-13 2016-12-07 安徽元琛环保科技股份有限公司 A kind of preparation method of the regeneration denitrification catalyst module for power plant's worst cold case

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WO2012106195A2 (en) * 2011-02-03 2012-08-09 Steag Energy Services Llc Method for treating scr catalysts having accumulated iron compounds
CN102658215A (en) * 2012-04-09 2012-09-12 南京工业大学 SCR (selective catalytic reduction) flue gas denitration catalyst regeneration method
CN102658170A (en) * 2012-04-11 2012-09-12 西安交通大学 Regeneration technology of V-Ti-based honeycomb SCR denitration catalyst, and apparatus thereof

Patent Citations (3)

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Publication number Priority date Publication date Assignee Title
WO2012106195A2 (en) * 2011-02-03 2012-08-09 Steag Energy Services Llc Method for treating scr catalysts having accumulated iron compounds
CN102658215A (en) * 2012-04-09 2012-09-12 南京工业大学 SCR (selective catalytic reduction) flue gas denitration catalyst regeneration method
CN102658170A (en) * 2012-04-11 2012-09-12 西安交通大学 Regeneration technology of V-Ti-based honeycomb SCR denitration catalyst, and apparatus thereof

Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103364422A (en) * 2013-07-04 2013-10-23 武汉大学 Method for diagnosing regenerability of inactivating denitration catalyst
CN103433081B (en) * 2013-08-08 2015-07-15 涿州西热环保催化剂有限公司 Regeneration method for honeycomb type SCR (Selective Catalytic Reduction) denitration catalyst
CN103433081A (en) * 2013-08-08 2013-12-11 涿州西热环保催化剂有限公司 Regeneration method for honeycomb type SCR (Selective Catalytic Reduction) denitration catalyst
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
CN103551209B (en) * 2013-10-23 2016-02-24 广东电网公司电力科学研究院 For the activating and regenerating liquid and preparation method thereof of SCR catalyst for denitrating flue gas
CN103949291B (en) * 2014-04-23 2016-01-13 江苏万德环保科技有限公司 Denitrating catalyst regenerated liquid, regenerated liquid preparation method and catalyst recovery process
CN103949291A (en) * 2014-04-23 2014-07-30 江苏万德环保科技有限公司 Denitration catalyst regeneration solution and preparation method thereof as well as catalyst regeneration method
CN105709861A (en) * 2014-12-05 2016-06-29 中国石油化工股份有限公司 Regeneration method of SCR denitration catalyst
CN105709861B (en) * 2014-12-05 2018-07-03 中国石油化工股份有限公司 A kind of regeneration method of SCR denitration
CN105032501A (en) * 2015-07-15 2015-11-11 浙江浙能催化剂技术有限公司 Method for dredging pore channels of honeycomb SCR (selective catalytic reduction) catalyst
CN105536883A (en) * 2015-12-17 2016-05-04 福建紫荆环境工程技术有限公司 Dry reclamation method for treating failure SCR denitration catalyst by adopting plasma
CN105921015A (en) * 2016-07-04 2016-09-07 青岛双瑞海洋环境工程股份有限公司 Soot blowing system of denitrification reactor
CN105921015B (en) * 2016-07-04 2019-08-09 青岛双瑞海洋环境工程股份有限公司 The soot blower system of Benitration reactor
CN106179531A (en) * 2016-07-13 2016-12-07 安徽元琛环保科技股份有限公司 A kind of preparation method of the regeneration denitrification catalyst module for power plant's worst cold case

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