CN105688936A - In-situ regeneration method of ammonium sulfate poisoning denitration catalyst - Google Patents
In-situ regeneration method of ammonium sulfate poisoning denitration catalyst Download PDFInfo
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- CN105688936A CN105688936A CN201610036036.4A CN201610036036A CN105688936A CN 105688936 A CN105688936 A CN 105688936A CN 201610036036 A CN201610036036 A CN 201610036036A CN 105688936 A CN105688936 A CN 105688936A
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- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
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- B01J23/90—Regeneration or reactivation
- B01J23/92—Regeneration or reactivation of catalysts comprising metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
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Abstract
The invention relates to an in-situ regeneration method of an ammonium sulfate poisoning denitration catalyst and belongs to the technical field of an industrial denitration catalyst. The in-situ regeneration method comprises the following steps: (1) when the concentration of nitrogen oxide in outlet flue gas of an SCR (Semiconductor Control Rectifier) main reactor is close to an emission limit value, switching the flue gas to an SCR reserved reactor; (2) introducing hot gas flow into the SCR main reactor and decomposing an ammonium sulfate layer deposited on the surface of the catalyst under the action of the hot gas flow; continuously introducing the hot gas flow for 1 hour to 8 hours to finish regeneration of the denitration catalyst; (3) switching the flue gas back to the SCR main reactor and continually carrying out a denitration reaction. Under the action of the hot gas flow, ammonium sulfate is decomposed into ammonia gas, sulfur trioxide and water steam and is removed along the flowing of the hot gas flow, so that the denitration performance of the catalyst can be recovered. The in-situ regeneration method of the ammonium sulfate poisoning denitration catalyst has the advantages of simplicity in operation, short regeneration time, low regeneration cost, safety and environmental friendliness, high denitration efficiency of the regenerated catalyst, and no changes of the strength and pore structure of the catalyst.
Description
Technical field
The invention belongs to industry denitrating catalyst technical field, be specially the in situ regeneration method of a kind of poisoning denitrating catalyst of sulfur ammonium。
Background technology
In recent years, China's NOx discharge raises rapidly, if without suitably controlling, nitrogen oxide emission is up to 30,000,000 tons at the year two thousand twenty, brings huge threat to China's atmospheric environment。In view of the severe situation that adverse effect and the discharged nitrous oxides of atmospheric environment are controlled by nitrogen oxides, Chinese Ministry of Environmental Protection has issued the discharged nitrous oxides standard that the industries such as power plant, boiler, coking, cement, glass, iron and steel, petroleum refining are new in succession。The enforcement successively of new standard has pulled Denitration Industry greatly, including the regeneration of relevant device manufacture, catalyst manufacture and dead catalyst。
At present, the denitration technology that countries in the world adopt is mainly SCR technology (being called for short SCR), adopts vanadium Titanium series catalyst。Reducing agent (NH is utilized under catalyst action3) (it is mainly NO and NO with the NOx in flue gas selectively2) there is chemical reaction, it is N by NOx conversion2And H2O, thus reducing the discharge of NOx in flue gas。In SCR denitration system, catalyst activity component vanadium reduction NOx while, the SO that also can will contain in flue gas2It is oxidized to SO3, with reducing agent NH3Reaction generates sulfur ammonium (ammonium sulfate and ammonium hydrogen sulfate) and is deposited on the surface of catalyst。Concrete reaction equation is as follows:
2SO2+O2→2SO3(1)
SO3+NH3+H2O→NH4HSO4(2)
SO3+2NH3+H2O→(NH4)2SO4(3)
Hydrogen sulfate ammonia is the material that a kind of viscosity is very strong, fusing point 147 DEG C, decomposition temperature about 300 DEG C。When flue-gas temperature is lower than 300 DEG C, hydrogen sulfate ammonia mucus can cover catalyst surface, causes that catalyst activity reduces, so SCR technology requires that the temperature of flue gas is 300～450 DEG C at present。Owing to sulfur ammonium poisoning and deactivation can occur catalyst in cold operation process (≤300 DEG C), limit SCR technology application in industrial smoke denitration, such as coke oven flue gas, catalytic cracked regenerated gas etc.。
Summary of the invention
Present invention aims to above technical problem, there is provided a kind of simple to operate, economical and practical, catalyst regeneration rate is high, do not affect catalyst working strength, after regeneration, the denitration efficiency of denitrating catalyst can recover to initial value, has the in situ regeneration method of the poisoning denitrating catalyst of sulfur ammonium of applications well prospect in middle low temperature (≤300 DEG C) denitrating flue gas field。The object of the invention is realized by following technical proposals:
The in situ regeneration method of a kind of poisoning denitrating catalyst of sulfur ammonium, comprises the following steps:
1), when nitrous oxides concentration is close to emission limit in SCR main reactor exiting flue gas, flue gas is switched to SCR standby reactor；
2), by thermal current passing into SCR main reactor, make the sulfur ammonium layer that denitrating catalyst surface deposits decompose under the effect of thermal current, persistently logical thermal current 1～8h, namely completes the regeneration of denitrating catalyst；
3), flue gas is switched back to SCR main reactor and continues denitration reaction。
When present invention process flue gas in SCR main reactor is close to discharge standard, flue gas is switched to SCR standby reactor and continues reaction and discharged by standby reactor；Then sulfur ammonium denitrating catalyst surface deposited higher than the thermal current of sulfur ammonium decomposition temperature is utilized to purge, sulfur ammonium is made to be decomposed into ammonia, sulfur trioxide and water vapour under the environment higher than decomposition temperature, and take away along with thermal current and remove, so that the denitration performance of catalyst is recovered, then flue gas is switched back to SCR main reactor again and continues denitration reaction。Now, sulfur ammonium has been decomposed removing, and denitrating catalyst has also recovered original denitration efficiency, it is ensured that being smoothed out of denitrating flue gas reaction。
One as the present invention is preferred, step 1) in, described nitrous oxides concentration emission limit is 100mg/m3。
One as the present invention is preferred, and described flue gas is middle low-temperature industrial flue gas。
One as the present invention is preferred, and described middle low-temperature industrial flue gas is one or more in coke oven flue gas, the catalytic cracked regenerated gas of petroleum refining, boiler smoke。
One as the present invention is preferred, and described flue-gas temperature is lower than 300 DEG C。The flue-gas temperature of existing industry discharge is below 300 DEG C mostly, and under this temperature conditions, sulfur ammonium poisoning and deactivation can occur catalyst。For this feature, the present invention proposes a kind of in-situ regeneration technique inactivating rear catalyst。
One as the present invention is preferred, and described thermal current is one or more in air, nitrogen, argon。
One as the present invention is preferred, and the temperature of described thermal current is 300～500 DEG C, and air speed is 300～10000h-1。The temperature of thermal current is set to 300～500 DEG C, the decomposition temperature being because sulfur ammonium is about 300 DEG C, only the temperature of thermal current is arranged and the sulfur ammonium of denitrating catalyst surface deposition in SCR reactor could be decomposed higher than 300 DEG C, thus reaching the purpose removed, it is denitrating catalyst regeneration, recovers the denitration performance of catalyst；And temperature is too high, easily cause again the inactivation of catalyst, so the temperature of thermal current of the present invention is 300～500 DEG C。
One as the present invention is preferred, described denitrating catalyst vanadium Titanium series catalyst。
One as the present invention is preferred, and described denitrating catalyst is alveolate texture。
One as the present invention is preferred, and described denitrating catalyst includes the component of following mass parts: V2O5: 1～6 part, WO3: 4～8 parts, TiO2: 75～90 parts, glass fibre: 3～10 parts。
Compared with prior art, the method have the advantages that
1, in situ regeneration method provided by the invention is simple to operate, the recovery time is short, regeneration expense is low, and equipment requirements is low, has effectively saved regeneration cost。
2, the thermal current that the present invention adopts is air, nitrogen and argon, and environmentally safe meets environmental safety。
3, adopt the denitrating catalyst denitration efficiency after the inventive method regeneration to recover to initial value, do not affect the performance of catalyst, and catalyst strength, pore structure all do not change, catalyst renewable repeated use。
Accompanying drawing explanation
Fig. 1 is the in-situ regeneration process flow diagram of the poisoning denitrating catalyst of sulfur ammonium of the present invention。
Detailed description of the invention
In order to make the purpose of the present invention, technical scheme and advantage clearly understand, below in conjunction with drawings and Examples, the present invention is further elaborated。Should be appreciated that specific embodiment described herein is only in order to explain the present invention, is not intended to limit the present invention。
Embodiment 1:
In SCR main reactor, fresh catalyst is 200 DEG C, SO in normal pressure, temperature2Concentration is 2000mg/m3, NO concentration is 800mg/m3, ammonia nitrogen ratio is 1.0, and air speed is 5000h-1Flue gas condition under run 1000h, catalyst denitration efficiency is down to 50% by 90.5%。
Present invention process flow process as it is shown in figure 1, when nitrogen oxides in effluent concentration is close to emission limit, switches to SCR standby reactor, and hot-air pass into SCR main reactor by flue gas, and wherein, the air speed of air is 1000h-1, temperature is 350 DEG C；After warm air blowoff 4h, stop passing into, namely complete the regeneration of denitrating catalyst of the present invention。
Flue gas switches back to SCR main reactor, and detection reactor outlet nitrous oxides concentration reaches discharge standard, and recording denitration efficiency is 89.3%。
Embodiment 2:
In SCR main reactor, fresh catalyst is 200 DEG C in normal pressure, temperature, SO2Concentration is 2000mg/m3, NO concentration is 800mg/m3, ammonia nitrogen ratio is 1.0, and air speed is 5000h-1Flue gas condition under run 1000h, catalyst denitration efficiency is down to 50% by 90.5%。
Present invention process flow process as it is shown in figure 1, when nitrogen oxides in effluent concentration is close to emission limit, switches to SCR standby reactor, and hot-air pass into SCR main reactor by flue gas, and wherein, the air speed of air is 2000h-1, temperature is 400 DEG C；After warm air blowoff 2.0h, stop passing into, namely complete the regeneration of denitrating catalyst of the present invention。
Flue gas switches back to SCR main reactor, and detection reactor outlet nitrous oxides concentration reaches discharge standard, and recording denitration efficiency is 90.7%。
Embodiment 3:
In SCR main reactor, fresh catalyst is 200 DEG C in normal pressure, temperature, SO2Concentration is 2000mg/m3, NO concentration is 800mg/m3, ammonia nitrogen ratio is 1.0, and air speed is 5000h-1Flue gas condition under run 1000h, catalyst denitration efficiency is down to 50% by 90.5%。
Present invention process flow process as it is shown in figure 1, when nitrogen oxides in effluent concentration is close to emission limit, switches to SCR standby reactor, and hot nitrogen pass into SCR main reactor by flue gas, and wherein, the air speed of nitrogen is 1000h-1, temperature is 350 DEG C；Hot nitrogen stops passing into, namely completes the regeneration of denitrating catalyst of the present invention after purging 4.0h。
Flue gas switches back to SCR main reactor, and detection reactor outlet nitrous oxides concentration reaches discharge standard, and recording denitration efficiency is 90.0%。
Embodiment 4:
In SCR main reactor, fresh catalyst is 200 DEG C in normal pressure, temperature, SO2Concentration is 2000mg/m3, NO concentration is 800mg/m3, ammonia nitrogen ratio is 1.0, and air speed is 5000h-1Flue gas condition under run 1000h, catalyst denitration efficiency is down to 50% by 90.5%。
Present invention process flow process as it is shown in figure 1, when nitrogen oxides in effluent concentration is close to emission limit, switches to SCR standby reactor, and hot nitrogen pass into SCR main reactor by flue gas, and wherein, the air speed of nitrogen is 2000h-1, temperature is 400 DEG C；Hot nitrogen stops passing into, namely completes the regeneration of denitrating catalyst of the present invention after purging 1.5h。
Flue gas switches back to SCR main reactor, and detection reactor outlet nitrous oxides concentration reaches discharge standard, and recording denitration efficiency is 90.2%。
In above-described embodiment 1 to 4, after the poisoning denitrating catalyst of sulfur ammonium being carried out in-situ regeneration by present invention process method, the denitration efficiency of catalyst recovers from 50% respectively to 89.3%, 90.7%, 90.0% and 90.2%, and the catalytic efficiency 90.5% initial with denitrating catalyst is almost consistent。Illustrate to adopt the inventive method effectively denitrating catalyst can be carried out in-situ regeneration, the denitration efficiency making catalyst recovers to initial value, it is achieved catalyst repeat regeneration purpose, the performance of catalyst is restored, effectively reuse catalyst, save production cost。
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all any amendment, equivalent replacement and improvement etc. made within the spirit and principles in the present invention, should be included within protection scope of the present invention。
Claims (10)
1. the in situ regeneration method of the poisoning denitrating catalyst of sulfur ammonium, it is characterised in that comprise the following steps:
1) when nitrous oxides concentration is close to emission limit in SCR main reactor exiting flue gas, flue gas is switched to SCR standby reactor；
2) thermal current passing into SCR main reactor, make the sulfur ammonium layer that denitrating catalyst surface deposits decompose under the effect of thermal current, persistently logical thermal current 1～8h, namely completes the regeneration of denitrating catalyst；
3) flue gas is switched back to SCR main reactor and continues denitration reaction。
2. the in situ regeneration method of a kind of poisoning denitrating catalyst of sulfur ammonium as claimed in claim 1, it is characterised in that described nitrous oxides concentration emission limit is 100mg/m3。
3. the in situ regeneration method of a kind of poisoning denitrating catalyst of sulfur ammonium as claimed in claim 1, it is characterised in that described flue gas is middle low-temperature industrial flue gas。
4. the in situ regeneration method of a kind of poisoning denitrating catalyst of sulfur ammonium as claimed in claim 2, it is characterised in that described middle low-temperature industrial flue gas is one or more in coke oven flue gas, the catalytic cracked regenerated gas of petroleum refining, boiler smoke。
5. the in situ regeneration method of a kind of poisoning denitrating catalyst of sulfur ammonium as described in any one of Claims 1-4, it is characterised in that described flue-gas temperature is lower than 300 DEG C。
6. the in situ regeneration method of a kind of poisoning denitrating catalyst of sulfur ammonium as claimed in claim 1, it is characterised in that described thermal current is one or more in air, nitrogen, argon。
7. the in situ regeneration method of a kind of poisoning denitrating catalyst of sulfur ammonium as described in claim 1 or 6, it is characterised in that the temperature of described thermal current is 300～500 DEG C, and air speed is 300～10000h-1。
8. the in situ regeneration method of a kind of poisoning denitrating catalyst of sulfur ammonium as claimed in claim 1, it is characterised in that described denitrating catalyst vanadium Titanium series catalyst。
9. the in situ regeneration method of a kind of poisoning denitrating catalyst of sulfur ammonium as claimed in claim 1, it is characterised in that described denitrating catalyst is alveolate texture。
10. the in situ regeneration method of a kind of poisoning denitrating catalyst of sulfur ammonium as described in any one of claim 1,8,9, it is characterised in that described denitrating catalyst includes the component of following mass parts: V2O5: 1～6 part, WO3: 4～8 parts, TiO2: 75～90 parts, glass fibre: 3～10 parts。
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106731565A (en) * | 2016-11-23 | 2017-05-31 | 无锡市国松环保机械有限公司 | Novel SCR low-temperature denitration device |
| CN107088365A (en) * | 2017-05-15 | 2017-08-25 | 大唐环境产业集团股份有限公司 | A kind of Y types SCR system catalyst on-line continuous regenerating unit |
| WO2018055162A1 (en) * | 2016-09-26 | 2018-03-29 | Shell Internationale Research Maatschappij B.V. | A method of reducing nitrogen oxide compounds |
| CN107876506A (en) * | 2017-12-12 | 2018-04-06 | 杭州凯明催化剂股份有限公司 | A kind of VOCs purifications irregular honeycomb ceramic carrier catalyst blow device and its application method |
| CN109589965A (en) * | 2018-12-23 | 2019-04-09 | 中国科学院山西煤炭化学研究所 | Desulphurization denitration vanadium carbon base catalyst and its preparation method and application |
| WO2019233035A1 (en) * | 2018-06-04 | 2019-12-12 | 浙江大学 | Method for solving problem of so2 poisoning of low-temperature scr denitration catalyst |
| WO2020041140A1 (en) * | 2018-08-22 | 2020-02-27 | Shell Oil Company | A selective catalytic reduction process and method of regenerating deactivated scr catalyst of a parallel flue gas treating system |
| US10814278B2 (en) | 2018-08-22 | 2020-10-27 | Shell Oil Company | Selective catalytic reduction process and off-line regeneration of deactivated catalyst of the process |
| US10814277B2 (en) | 2018-08-22 | 2020-10-27 | Shell Oil Company | Selective catalytic reduction process and off-line regeneration of deactivated catalyst of the process |
| US11097264B2 (en) * | 2016-03-29 | 2021-08-24 | Basf Corporation | Desulfation method for SCR catalyst |
| US11471831B2 (en) | 2016-09-26 | 2022-10-18 | Shell Usa, Inc. | Method of regenerating a deNOx catalyst |
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| US11097264B2 (en) * | 2016-03-29 | 2021-08-24 | Basf Corporation | Desulfation method for SCR catalyst |
| US10843132B2 (en) * | 2016-09-26 | 2020-11-24 | Shell Oil Company | Method of reducing nitrogen oxide compounds |
| WO2018055162A1 (en) * | 2016-09-26 | 2018-03-29 | Shell Internationale Research Maatschappij B.V. | A method of reducing nitrogen oxide compounds |
| CN109789372A (en) * | 2016-09-26 | 2019-05-21 | 国际壳牌研究有限公司 | The method for reducing nitrogen oxide compound |
| US11471831B2 (en) | 2016-09-26 | 2022-10-18 | Shell Usa, Inc. | Method of regenerating a deNOx catalyst |
| CN106731565A (en) * | 2016-11-23 | 2017-05-31 | 无锡市国松环保机械有限公司 | Novel SCR low-temperature denitration device |
| CN107088365A (en) * | 2017-05-15 | 2017-08-25 | 大唐环境产业集团股份有限公司 | A kind of Y types SCR system catalyst on-line continuous regenerating unit |
| CN107876506A (en) * | 2017-12-12 | 2018-04-06 | 杭州凯明催化剂股份有限公司 | A kind of VOCs purifications irregular honeycomb ceramic carrier catalyst blow device and its application method |
| CN107876506B (en) * | 2017-12-12 | 2023-09-05 | 杭州凯明催化剂股份有限公司 | Irregular honeycomb ceramic carrier catalyst purging device for purifying VOCs and application method thereof |
| WO2019233035A1 (en) * | 2018-06-04 | 2019-12-12 | 浙江大学 | Method for solving problem of so2 poisoning of low-temperature scr denitration catalyst |
| CN112638505A (en) * | 2018-08-22 | 2021-04-09 | 国际壳牌研究有限公司 | Selective catalytic reduction process and method for regenerating deactivated SCR catalyst of parallel flue gas treatment system |
| US10814277B2 (en) | 2018-08-22 | 2020-10-27 | Shell Oil Company | Selective catalytic reduction process and off-line regeneration of deactivated catalyst of the process |
| US10814278B2 (en) | 2018-08-22 | 2020-10-27 | Shell Oil Company | Selective catalytic reduction process and off-line regeneration of deactivated catalyst of the process |
| US10722844B2 (en) | 2018-08-22 | 2020-07-28 | Shell Oil Company | Selective catalytic reduction process and method of regenerating deactivated SCR catalyst of a parallel flue gas treating system |
| WO2020041140A1 (en) * | 2018-08-22 | 2020-02-27 | Shell Oil Company | A selective catalytic reduction process and method of regenerating deactivated scr catalyst of a parallel flue gas treating system |
| CN109589965B (en) * | 2018-12-23 | 2021-11-05 | 中国科学院山西煤炭化学研究所 | Vanadium-carbon-based catalyst for desulfurization and denitrification and preparation method and application thereof |
| CN109589965A (en) * | 2018-12-23 | 2019-04-09 | 中国科学院山西煤炭化学研究所 | Desulphurization denitration vanadium carbon base catalyst and its preparation method and application |
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