CN106179528A - A kind of renovation process of alkali metal poisoning denitrating catalyst - Google Patents

A kind of renovation process of alkali metal poisoning denitrating catalyst Download PDF

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Publication number
CN106179528A
CN106179528A CN201610496335.6A CN201610496335A CN106179528A CN 106179528 A CN106179528 A CN 106179528A CN 201610496335 A CN201610496335 A CN 201610496335A CN 106179528 A CN106179528 A CN 106179528A
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denitrating catalyst
alkali metal
ammonium
renovation process
catalyst
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Inventor
黄力
王虎
李倩
王晓伟
纵宇浩
陈志平
董晓真
张捷
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Datang Nanjing Environmental Protection Technology Co Ltd
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Datang Nanjing Environmental Protection Technology Co Ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J38/00—Regeneration or reactivation of catalysts, in general
    • B01J38/48—Liquid treating or treating in liquid phase, e.g. dissolved or suspended
    • B01J38/485—Impregnating or reimpregnating with, or deposition of metal compounds or catalytically active elements
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • 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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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Exhaust Gas Treatment By Means Of Catalyst (AREA)
  • Catalysts (AREA)

Abstract

The invention discloses the renovation process of a kind of alkali metal poisoning denitrating catalyst, after the denitrating catalyst ash disposal that alkali metal is poisoned, impregnated in ammonium salt aqueous solution；Then mixed solution is transferred in microwave reactor, carries out microwave treatment, then the denitrating catalyst after being regenerated through filtering, drying, after roasting.The renovation process of the alkali metal poisoning denitrating catalyst of the present invention is simple to operate, it is short to process the time, the alkali metal on inactivation denitrating catalyst surface is had preferable removal effect, can also remove most calcium compounds on catalyst simultaneously.Further, in regenerative process, the active component of denitrating catalyst will not run off in a large number.

Description

A kind of renovation process of alkali metal poisoning denitrating catalyst
Technical field
The present invention relates to selective catalytic reduction catalysts technical field, be specifically related to a kind of alkali metal poisoning denitration catalyst The renovation process of agent.
Background technology
The advantages such as SCR (SCR) technology is high with its denitration efficiency, floor space is little, reliable, are should Use most commonly used NOxEmission control technique.As the core of SCR denitration technology, the general of denitrating catalyst is running Will inactivate after 24000h, when the time comes for meeting NOxDischarge index, needs to change fresh catalyst.And catalyst cost is higher, become Originally the 40% of denitration total investment of engineering is accounted for.Therefore, use effective means that decaying catalyst is carried out Regeneration Treatment so that it is denitration Efficiency is recovered to fresh sample level, saves energy and reduce the cost coal-burning power plant significant.
Alkali metal (K, Na) is one of major reason of causing denitrating catalyst to inactivate.Cardinal principle is alkali metal Being remarkably decreased of acid function of denitrating catalyst can be caused, affect NH3Absorption on denitrating catalyst surface.Existing research Showing, the aqueous sulfuric acid of 0.5 mol/L cleans has preferable alkali metal removal effect, but, denitration can be caused to urge Agent active component V2O5Loss.Thus it is necessary to develop the renovation process of novel alkali metal poisoning denitrating catalyst.In recent years Coming, on existing multiple removal denitrating catalyst, alkali-metal method is open, such as CN 104226380A, CN in this area 105080622A, CN 105057008A, US2007032373, US7723251 etc..But still there is operation complexity, scavenging period The problems such as long, loss of active component rate is high.
Summary of the invention
The present invention provides the renovation process of a kind of alkali metal poisoning denitrating catalyst, by using the regeneration side of the present invention Method, can effectively remove the alkali metal on inactivation denitrating catalyst, also can remove major part deposition simultaneously in the short period of time Calcium compounds on a catalyst.And, it is most important that, can effectively prevent active component in denitrating catalyst regenerative process Loss.
To achieve these goals, the technological means that the present invention uses is:
The renovation process of described alkali metal poisoning denitrating catalyst, comprises the steps of
1) compound concentration is the ammonium salt aqueous solution of 1 ~ 40 wt%, be impregnated in ammonium salt aqueous solution by the denitrating catalyst after ash disposal；
2) by step 1) in mixed solution be transferred in microwave reactor, at 25 ~ 100 DEG C, microwave treatment 1 ~ 60min, so Rear filtration, drying, under 400 ~ 700 DEG C of air atmospheres after roasting 1 ~ 8h, obtain the denitrating catalyst after regeneration.
Step 1) described in ammonium salt be ammonium fluoride, ammonium chloride, ammonium bromide, ammonium iodide, ammonium sulfate, ammonium hydrogen sulfate, nitric acid One in ammonium, ammonium carbonate, ammonium hydrogen carbonate.
Step 1) described in the liquid-solid ratio (mL/g) of ammonium salt aqueous solution and denitrating catalyst be 1:1 ~ 50:1.
Step 1) described in ash disposal soot blowing technology well known in the art can be used to remove catalyst surface and duct Interior dust stratification, includes but not limited to the conventional meanses such as compressed air purging, high pressure water washing, the aspiration of negative pressure.
Step 2) described in the output of microwave reactor be 100 ~ 1000 W.
The renovation process of described a kind of alkali metal poisoning denitrating catalyst, preferred scheme is:
1) compound concentration is the ammonium salt aqueous solution of 5 ~ 20 wt%, be impregnated in ammonium salt aqueous solution by the denitrating catalyst after ash disposal；
2) by step 1) in mixed solution be transferred in microwave reactor, at 60 ~ 90 DEG C, stirring, backflow, microwave treatment 5 ~ 20min, then filters, dries, and under 500 ~ 600 DEG C of air atmospheres after roasting 1.5 ~ 4h, obtains the denitrating catalyst after regeneration.
Step 1) described in the liquid-solid ratio (mL/g) of ammonium salt aqueous solution and denitrating catalyst be preferably 4:1 ~ 25:1.
Step 2) described in the output of microwave reactor be preferably 300 ~ 900 W.
Beneficial effect
(1) regeneration methods of the invention uses microwave treatment, and in strengthening ammonium salt, ammonium radical ion is handed over the ion of alkali metal ion Changing, simple to operate, the recovery time is short, can effectively remove the alkali metal on inactivation denitrating catalyst.
(2) regeneration methods of the invention, for CaO, CaSO of deposition on inactivation denitrating catalyst4、CaCO3Close Deng calcification Thing also has preferable removal effect.
(3) regeneration methods of the invention, use ammonium salt aqueous solution as cleanout fluid, it is not necessary to surfactant, penetrating agent, The organic interpolation such as chelating agen, chemical composition is simple, decreases the recycling difficulty of regenerated effluent.
(4) use the present invention renovation process, after regeneration, the turnover rate of the active component of denitrating catalyst is low, permissible Reduce follow-up active component and supplement pickup, or directly omission active component supplements impregnation steps, reduces regeneration cost.
Detailed description of the invention
Following example are by further illustrating that the present invention is given by the selective catalytic denitrification process reaction, rather than to this Bright restriction.
Embodiment 1
Inactivation denitrating catalyst selects the V after certain coal-burning power plant domestic operation 24000h2O5-WO3/TiO2Honeycomb fashion denitration catalyst Agent, removes the dust stratification in catalyst surface and duct with compressed air purging.
Compound concentration is the aqueous ammonium chloride solution of 10 wt%, be impregnated in wherein by the denitrating catalyst after ash disposal.Then will Mixed solution is transferred in microwave reactor, at 90 DEG C, microwave treatment 15 min, then filters, dries, at 550 DEG C of air Under atmosphere after roasting 2h, obtain the denitrating catalyst after regeneration.Wherein, aqueous ammonium chloride solution and the liquid-solid ratio (mL/ of denitrating catalyst G) being 20:1, the output of microwave reactor is 500W.
Regenerated outcome: after regeneration, the K element on denitrating catalyst reduces 99.5%, Na element reduces 99.1%, and Ca element subtracts Few 78%, V2O5Turnover rate 2.5%.
Embodiment 2
Inactivation denitrating catalyst selects the V after certain coal-burning power plant domestic operation 18000h2O5-WO3/TiO2Corrugated plate dst denitration is urged Agent, first purges by compressed air, then the dust stratification in the aspiration of negative pressure removes catalyst surface and duct.
Compound concentration is the ammonium fluoride aqueous solution of 5 wt%, be impregnated in wherein by the denitrating catalyst after ash disposal.Then will be mixed Close solution to be transferred in microwave reactor, at 80 DEG C, microwave treatment 20 min, then filters, dries, at 500 DEG C of air gas Under atmosphere after roasting 4h, obtain the denitrating catalyst after regeneration.Wherein, ammonium fluoride aqueous solution and the liquid-solid ratio (mL/g) of denitrating catalyst For 25:1, the output of microwave reactor is 900W.
Regenerated outcome: after regeneration, the K element on denitrating catalyst reduces 98.6%, Na element reduces 99.7%, and Ca element subtracts Few 72.8%, V2O5Turnover rate 4.3%.
Embodiment 3
Inactivation denitrating catalyst selects the V after certain coal-burning power plant domestic operation 22000h2O5-MoO3/TiO2Board-like denitration catalyst Agent, removes the dust stratification in catalyst surface and duct with high pressure water washing.Again the board-like catalyst after ash disposal is carried out creme with Steel mesh lock out operation.
Compound concentration is the ammonium sulfate solution of 20 wt%, be impregnated in wherein by the denitrating catalyst creme after ash disposal.So After mixed solution is transferred in microwave reactor, at 60 DEG C, microwave treatment 5 min, then filter, dry, at 600 DEG C of skies Under gas atmosphere after roasting 1.5h, obtain the denitrating catalyst after regeneration.Wherein, ammonium sulfate solution and the liquid-solid ratio of denitrating catalyst (mL/g) being 4:1, the output of microwave reactor is 300W.
Regenerated outcome: after regeneration, the K element on denitrating catalyst reduces 99.1%, Na element reduces 99.0%, and Ca element subtracts Few 65.9%, V2O5Turnover rate 4.9%.
Embodiment 4
Inactivation denitrating catalyst selects the V after certain coal-burning power plant domestic operation 21000h2O5-MoO3/TiO2Board-like denitration catalyst Agent, first removes the dust stratification in catalyst surface and duct with compressed air purging.Again the board-like catalyst after ash disposal is carried out cream Material and steel mesh lock out operation.
Compound concentration is the ammonium sulfate solution of 15 wt%, be impregnated in wherein by the denitrating catalyst creme after ash disposal.So After mixed solution is transferred in microwave reactor, at 70 DEG C, microwave treatment 10 min, then filter, dry, at 500 DEG C Under air atmosphere after roasting 3h, obtain the denitrating catalyst after regeneration.Wherein, ammonium sulfate solution and the liquid-solid ratio of denitrating catalyst (mL/g) being 10:1, the output of microwave reactor is 400W.
Regenerated outcome: after regeneration, the K element on denitrating catalyst reduces 97.2%, Na element reduces 98.0%, and Ca element subtracts Few 71.1%, V2O5Turnover rate 3.7%.
Embodiment 5
Inactivation denitrating catalyst selects the V after certain coal-burning power plant domestic operation 21000h2O5-WO3/TiO2Honeycomb fashion denitration catalyst Agent, coordinates crooked chisel dredging with compressed air purging, removes the dust stratification in catalyst surface and duct.
Compound concentration is the ammonium bicarbonate aqueous solution of 12.5 wt%, be impregnated in wherein by the denitrating catalyst after ash disposal.So After mixed solution is transferred in microwave reactor, at 85 DEG C, microwave treatment 15 min, then filter, dry, at 560 DEG C Under air atmosphere after roasting 2.5h, obtain the denitrating catalyst after regeneration.Wherein, ammonium bicarbonate aqueous solution and the liquid of denitrating catalyst Gu be 15:1 than (mL/g), the output of microwave reactor is 700W.
Regenerated outcome: after regeneration, the K element on denitrating catalyst reduces 98.7%, Na element reduces 99.4%, and Ca element subtracts Few 85.0%, V2O5Turnover rate 6.1%.
Comparative example 1
The denitrating catalyst used, and ash disposal step is with embodiment 1.
Prepare the aqueous sulfuric acid of 0.5 mol/L, the catalyst after ash disposal be impregnated in wherein.Again at 60 DEG C, ultrasonic place Reason 1h, then filters, dries, obtain the denitrating catalyst after regeneration.Wherein, aqueous sulfuric acid and the liquid-solid ratio of denitrating catalyst (mL/g) it is 20:1, ultrasonic power 50kHz.
Regenerated outcome: after regeneration, the K element on denitrating catalyst reduces 92.2%, Na element reduces 89.4%, and Ca element subtracts Few 33.3%, V2O5Turnover rate 52.7%.

Claims (8)

1. the renovation process of an alkali metal poisoning denitrating catalyst, it is characterised in that comprise the steps of
1) compound concentration is the ammonium salt aqueous solution of 1 ~ 40 wt%, be impregnated in ammonium salt aqueous solution by the denitrating catalyst after ash disposal；
2) by step 1) in mixed solution be transferred in microwave reactor, at 25 ~ 100 DEG C, microwave treatment 1 ~ 60min, so Rear filtration, drying, under 400 ~ 700 DEG C of air atmospheres after roasting 1 ~ 8h, obtain the denitrating catalyst after regeneration.
The renovation process of a kind of alkali metal the most according to claim 1 poisoning denitrating catalyst, it is characterised in that step 1) In ammonium salt be ammonium fluoride, ammonium chloride, ammonium bromide, ammonium iodide, ammonium sulfate, ammonium hydrogen sulfate, ammonium nitrate, ammonium carbonate, ammonium hydrogen carbonate In one.
The renovation process of a kind of alkali metal the most according to claim 1 poisoning denitrating catalyst, it is characterised in that step 1) In the liquid-solid ratio (mL/g) of ammonium salt aqueous solution and denitrating catalyst be 1:1 ~ 50:1.
The renovation process of a kind of alkali metal the most according to claim 1 poisoning denitrating catalyst, it is characterised in that step 2) The output of middle microwave reactor is 100 ~ 1000 W.
The renovation process of a kind of alkali metal the most according to claim 1 poisoning denitrating catalyst, it is characterised in that step 1) In the concentration of ammonium salt aqueous solution be 5 ~ 20 wt%.
The renovation process of a kind of alkali metal the most according to claim 1 poisoning denitrating catalyst, it is characterised in that step 2) Middle mixed solution is transferred in microwave reactor, at 60 ~ 90 DEG C, and stirring, backflow, microwave treatment 5 ~ 20min, then filter, Dry, under 500 ~ 600 DEG C of air atmospheres after roasting 1.5 ~ 4h, obtain the denitrating catalyst after regeneration.
The renovation process of a kind of alkali metal the most according to claim 3 poisoning denitrating catalyst, it is characterised in that step 1) In the liquid-solid ratio (mL/g) of ammonium salt aqueous solution and denitrating catalyst be 4:1 ~ 25:1.
The renovation process of a kind of alkali metal the most according to claim 4 poisoning denitrating catalyst, it is characterised in that step 2) The output of middle microwave reactor is 300 ~ 900 W.
CN201610496335.6A 2016-06-30 2016-06-30 A kind of renovation process of alkali metal poisoning denitrating catalyst Pending CN106179528A (en)

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Cited By (8)

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Publication number Priority date Publication date Assignee Title
CN107469874A (en) * 2017-09-11 2017-12-15 华中科技大学 A kind of catalyst regeneration device and method based on microwave decoking
CN108144656A (en) * 2017-11-23 2018-06-12 浙江天蓝环保技术股份有限公司 A kind of regenerated liquid and regeneration method for denitrating catalyst of being poisoned
CN108722436A (en) * 2018-06-04 2018-11-02 浙江大学 A kind of solution low temperature SCR denitration catalyst SO2The method of poisoning
CN110769933A (en) * 2017-06-30 2020-02-07 三菱日立电力系统株式会社 Regeneration method and regeneration system of denitration catalyst
CN111036310A (en) * 2019-12-25 2020-04-21 中节能万润股份有限公司 Regenerated monolithic molecular sieve-based denitration catalyst, and regeneration method and application thereof
CN111111772A (en) * 2019-12-25 2020-05-08 中节能万润股份有限公司 Regeneration method of molecular sieve denitration catalyst
CN114308140A (en) * 2021-12-07 2022-04-12 苏州西热节能环保技术有限公司 Catalyst regeneration method based on ammonium bisulfate poisoning
CN114870907A (en) * 2022-06-13 2022-08-09 苏州西热节能环保技术有限公司 Regeneration method of alkali/alkaline earth metal poisoned denitration catalyst

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Cited By (9)

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Publication number Priority date Publication date Assignee Title
CN110769933A (en) * 2017-06-30 2020-02-07 三菱日立电力系统株式会社 Regeneration method and regeneration system of denitration catalyst
CN107469874A (en) * 2017-09-11 2017-12-15 华中科技大学 A kind of catalyst regeneration device and method based on microwave decoking
CN108144656A (en) * 2017-11-23 2018-06-12 浙江天蓝环保技术股份有限公司 A kind of regenerated liquid and regeneration method for denitrating catalyst of being poisoned
CN108722436A (en) * 2018-06-04 2018-11-02 浙江大学 A kind of solution low temperature SCR denitration catalyst SO2The method of poisoning
CN111036310A (en) * 2019-12-25 2020-04-21 中节能万润股份有限公司 Regenerated monolithic molecular sieve-based denitration catalyst, and regeneration method and application thereof
CN111111772A (en) * 2019-12-25 2020-05-08 中节能万润股份有限公司 Regeneration method of molecular sieve denitration catalyst
CN114308140A (en) * 2021-12-07 2022-04-12 苏州西热节能环保技术有限公司 Catalyst regeneration method based on ammonium bisulfate poisoning
CN114870907A (en) * 2022-06-13 2022-08-09 苏州西热节能环保技术有限公司 Regeneration method of alkali/alkaline earth metal poisoned denitration catalyst
CN114870907B (en) * 2022-06-13 2023-10-20 苏州西热节能环保技术有限公司 Regeneration method of denitration catalyst for alkali/alkaline earth metal poisoning

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