CN105251543A - Method for regenerating arsenic-poisoned denitration catalysts through hydrogen gas reduction - Google Patents
Method for regenerating arsenic-poisoned denitration catalysts through hydrogen gas reduction Download PDFInfo
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Abstract
The invention provides a method for regenerating arsenic-poisoned denitration catalysts through hydrogen gas reduction. Firstly, pores of deactivated catalysts are cleaned through iron wires and a high-pressure water gun, silicon oxide, calcium sulfate and organic residual impurities left on surfaces and in the pores of the catalysts are removed, and the deactivated catalysts are dried at the normal temperature for standby application; the dried and deactivated catalysts are put into a tube furnace and calcined in an atmosphere of H2/He, and the catalysts with arsenic removed are obtained after natural temperature reduction; finally, the catalysts with the arsenic removed are taken out, dried for 2h at the temperature of 110 DEG C and put into an air atmosphere to be calcined, and the regenerated catalyst is obtained. The method can be widely used for various arsenic induced deactivated denitration catalysts, the catalysts can be regenerated and the service life of the catalysts can be prolonged through simple hydrogen gas reduction, and no solvents or activity supplement process are required.
Description
Technical field
The present invention relates to the denitrating catalyst technical field of regeneration in atmospheric environment protection, be specifically related to the hydrogen reducing renovation process of the out of stock catalyst of a kind of arsenic poisoning.
Background technology
Research shows, nitrogen oxide (NOx) is the important as precursors thing causing nitric acid type acid rain, photochemical fog and haze weather, its discharge is mainly from the burning of coal, and thermal power plant NOx generation is the half of national total amount, therefore, thermal power plant's NOx emission controls to be the key that China's NOx emission controls.SCR (SCR), as the most efficient denitration technology, is the first-selection of domestic and international coal fired power plant vent gas treatment always.But denitrating catalyst General Life is 24000 hours; In addition, estimated for the end of the year 2015, in coal-burning power plant, denitrating catalyst use amount will reach 60-80 ten thousand m
3.If by direct for a large amount of waste catalyst landfill, not only cost is high but also cause the significant wastage of resource, and therefore regeneration becomes best dead catalyst processing mode.
Noble metal arsenic As not only has higher physiological-toxicity, and very large for denitrating catalyst activity influence.Research shows, in coal, the mass fraction of arsenic is more than 30ppm, and SCR catalyst chemical lifetime is by reduction about 50%.Although arsenic content exists deviation with coal difference in coal, in general, the poisoned catalyst arsenic oxide arsenoxide content after work in 24000 hours is between 0 to 3wt%.If without the direct landfill of process, to the very large hidden danger of underground water and soil security presence.Traditional sulfuric acid cleaned, not only can not remove and be stored in arsenic species in catalyst pores and surperficial, and loss of active component, equipment corrosion and intensity can be caused to decline.Therefore development of new is efficiently suitable for the renovation process of the poisoning denitrating catalyst of As, and it is very necessary for realizing resource circulation utilization.
Summary of the invention
In order to overcome the shortcoming of above-mentioned prior art, the object of the present invention is to provide the hydrogen reducing renovation process of the out of stock catalyst of a kind of arsenic poisoning, multiple (vanadium base, cerium base etc.) denitrating catalyst that arsenic causes inactivation can be widely used in, and regenerate extending catalyst service life by simple hydrogen reducing and supplement process without the need to solvent and activity.
In order to achieve the above object, the technical solution used in the present invention is:
A hydrogen reducing renovation process for the out of stock catalyst of arsenic poisoning, comprises the steps:
Step one: decaying catalyst duct is utilized iron wire and giant deashing, removes surperficial and that duct is residual silica, calcium sulfate and organic residue impurity, stand-by after air drying;
Step 2: dry decaying catalyst step one obtained is placed in tube furnace, in H
2the roasting of/He atmosphere, actual conditions: hydrogen volume ratio accounts for H
2between the 0-100% of/He atmosphere, H
2between/He gas flow 0-100ml/min, heating rate is 1-30 DEG C/min, rises to 400-650 DEG C from room temperature, and is held in this temperature calcination, and roasting time is between 0-10h, obtains the catalyst removing arsenic after Temperature fall;
Step 3: the catalyst removing arsenic step 2 obtained takes out, after 110 DEG C of dry 2h, be placed in air atmosphere roasting, roasting condition: between gas flow 0-50ml/min, heating rate is 1-50 DEG C/min, sintering temperature is 300-600 DEG C, and roasting time is between 0-10h, obtains regenerated catalyst.
Compared with prior art, tool of the present invention has the following advantages:
1. the present invention is without the need to any regenerated liquid, operates easy, and As clearance is high, is applicable to multiclass denitrating catalyst, re-uses after being particularly suitable for the poisoning denitrating catalyst regeneration of high As.
2. the present invention while a large amount of arsenic is removed, can retain most vanadium oxide, tungsten oxide isoreactivity component, and can omit the active implantation step in the later stage of conventional regeneration technology.
Under the prerequisite of non-activity implantation step, can efficient removal nitrogen oxide (the highest >90% of conversion rate of NOx) and realize efficient oxidation arsenic remove (As
2o
3the highest >90% of clearance).
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in detail.
Embodiment 1
A hydrogen reducing renovation process for the out of stock catalyst of arsenic poisoning, comprises the steps:
Step one: first prepare vanadium tungsten titanium or vanadium molybdenum titanium catalyst by the precipitation method, be then placed on arsenic oxide arsenoxide As
2o
3after solution impregnation drying, obtain arsenic oxide arsenoxide As
2o
3mass concentration is 3%, then by the catalyst of arsenic poisoning after 450 degree of roasting 3h fix arsenic oxide arsenoxide, grinding is sieved, and obtains 40-60 order decaying catalyst;
Step 2: the decaying catalyst of 1g is placed in tube furnace, in H
2the roasting of/He atmosphere, roasting condition: hydrogen volume ratio accounts for H
210%, H of/He atmosphere
2/ He gas flow is 80mL/min, and heating rate is 20 DEG C/min, rises to 500 DEG C from room temperature, and in 500 DEG C of roastings, keeps 2h, obtain the catalyst removing arsenic after Temperature fall;
Step 3: the catalyst removing arsenic step 2 obtained takes out, and after 110 DEG C of dry 2h, is placed in air atmosphere roasting, roasting condition: gas flow 20ml/min, heating rate is 5 DEG C/min, and sintering temperature is 500 DEG C, roasting time is 2 hours, obtains regenerated catalyst.
Embodiment 2
A hydrogen reducing renovation process for the out of stock catalyst of arsenic poisoning, comprises the steps:
Step one: first prepare cerium tungsten titanium catalyst by the precipitation method, be then placed on arsenic oxide arsenoxide As
2o
3after solution impregnation drying, obtain arsenic oxide arsenoxide As
2o
3mass concentration is that after 3%, 450 degree of roasting 3h fix arsenic oxide arsenoxide, grinding is sieved, and obtains 40-60 order decaying catalyst;
Step 2: the decaying catalyst of 1g is placed in tube furnace, in H
2the roasting of/He atmosphere, roasting condition: hydrogen volume ratio accounts for H
25%, H of/He atmosphere
2/ He gas flow is under the atmosphere of 50mL/min, and heating rate is 10 DEG C/min, rises to 600 DEG C from room temperature, and in 600 DEG C of roastings, keeps 20min, obtain the catalyst removing arsenic after Temperature fall;
Step 3: the catalyst removing arsenic step 2 obtained takes out, and after 110 DEG C of dry 2h, is placed in air atmosphere roasting, roasting condition: gas flow 50ml/min, heating rate is 10 DEG C/min, and sintering temperature is 600 DEG C, roasting time is 4 hours, obtains regenerated catalyst.
Embodiment 3
A hydrogen reducing renovation process for the out of stock catalyst of arsenic poisoning, comprises the steps:
Step one: first prepare cerium tungsten titanium catalyst by the precipitation method, be then placed on arsenic oxide arsenoxide As
2o
3after solution impregnation drying, obtain arsenic oxide arsenoxide As
2o
3mass concentration is that after 3%, 450 degree of roasting 3h fix arsenic oxide arsenoxide, grinding is sieved, and obtains 40-60 order decaying catalyst;
Step 2: the decaying catalyst of 1g is placed in tube furnace, in H
2the roasting of/He atmosphere, roasting condition: hydrogen volume ratio accounts for H
240%, H of/He atmosphere
2/ He gas flow is 90mL/min, and heating rate is 30 DEG C/min, rises to 550 DEG C from room temperature, and in 550 DEG C of roastings, keeps 5h, obtain the catalyst removing arsenic after Temperature fall;
Step 3: the catalyst removing arsenic step 2 obtained takes out, and after 110 DEG C of dry 2h, is placed in air atmosphere roasting, roasting condition: gas flow 10ml/min, heating rate is 40 DEG C/min, and sintering temperature is 500 DEG C, roasting time is 2 hours, obtains regenerated catalyst.
Embodiment 4
A hydrogen reducing renovation process for the out of stock catalyst of arsenic poisoning, comprises the steps:
Step one: first prepare vanadium tungsten titanium catalyst by the precipitation method, be then placed on arsenic oxide arsenoxide As
2o
3after solution impregnation drying, obtain arsenic oxide arsenoxide As
2o
3mass concentration is that after 3%, 450 degree of roasting 3h fix arsenic oxide arsenoxide, grinding is sieved, and obtains 40-60 order decaying catalyst;
Step 2: the decaying catalyst of 1g is placed in tube furnace, in H
2the roasting of/He atmosphere, roasting condition: hydrogen volume ratio accounts for H
280%, H of/He atmosphere
2/ He gas flow is 60mL/min, and heating rate is 10 DEG C/min, rises to 500 DEG C from room temperature, and in 500 DEG C of roastings, keeps 20min, obtain the catalyst removing arsenic after Temperature fall;
Step 3: the catalyst removing arsenic step 2 obtained takes out, and after 110 DEG C of dry 2h, is placed in air atmosphere roasting, roasting condition: gas flow 50ml/min, heating rate is 10 DEG C/min, and sintering temperature is 500 DEG C, roasting time is 8 hours, obtains regenerated catalyst.
Embodiment 5
A hydrogen reducing renovation process for the out of stock catalyst of arsenic poisoning, comprises the steps:
Step one: Shen Zhi inactivation enterprise vanadium tungsten titanium catalyst duct is utilized iron wire and giant deashing, remove surperficial and that duct is residual silica, calcium sulfate and organic residue impurity, being cut into hole count is 3 × 3, and length is the small catalyst dried for standby of 100mm;
Step 2: the decaying catalyst that 10g step one obtains is placed in tube furnace, in H
2the roasting of/He atmosphere, roasting condition: hydrogen volume ratio accounts for H
21%, H of/He atmosphere
2/ He gas flow is 10mL/min, and heating rate is 5 DEG C/min, rises to 600 DEG C from room temperature, and in 600 DEG C of roastings, keeps 4h, obtain the catalyst removing arsenic after Temperature fall;
Step 3: the catalyst removing arsenic step 2 obtained takes out, and after 110 DEG C of dry 2h, is placed in air atmosphere roasting, roasting condition: gas flow 30ml/min, heating rate is 5 DEG C/min, and sintering temperature is 500 DEG C, roasting time is 3 hours, obtains regenerated catalyst.
The efficiency recovery rate contrast test of embodiment 1-5 regenerated catalyst:
Use regenerated catalyst 350 DEG C of efficiency recovery rates of embodiment 1-5 to contrast, and utilize XRF to test As clearance, catalyst denitration efficiency, activation recovering rate and As clearance, to be calculated as follows:
Denitration efficiency μ=([NO
xin]-[NO
xout])/[NO
xin] × 100%
Activation recovering rate y=(μ
regenerated-μ
poisoned)/μ
regenerated
As clearance x=([As
2o
3poisoned]-[As
2o
3regenerated])/[As
2o
3poisoned] × 100%
Wherein: [NO
xin] be the NOx concentration (ppm) of Reactor inlet, [NO
xout] for processing the concentration (ppm) of NOx in rear gas.Test condition is: temperature 350 DEG C, normal pressure, reaction velocity 120000h
-1, 0.1g got by catalyst, and flue gas concentration is 500ppmNH
3, 500ppmNO, 3%O
2; [As
2o
3poisoned] for poisoned catalyst arsenic percentage composition is (with As
2o
3), [As
2o
3regenerated] for regenerated catalyst arsenic percentage composition is (with As
2o
3).Table one is the experimental result of above-described embodiment.
Table one
| Embodiment | Denitration efficiency (%) | As clearance (%) | Activation recovering rate (%) |
| 1 | 83 | 84.4 | 82％ |
| 2 | 93 | 92.9 | 69.8％ |
| 3 | 60 | 72.6 | 43.9 |
| 4 | 47 | 33.3 | 34.5 |
| 5 | 50 | 74.2 | 77.9 |
Table one result shows, 600 DEG C, 5%H
2under/He condition, high temperature reduction can the arsenic of effectively clear vanadium base and ceria-based denitration catalyst, and have efficient recovery catalytic activity; Although and 500 DEG C and 550 DEG C of regeneration temperatures can remove portion arsenic, can only recovered part active; For the waste and old poisoned catalyst of enterprise, hydrogen high temperature regeneration also obtains good result.
Claims (6)
1. a hydrogen reducing renovation process for the out of stock catalyst of arsenic poisoning, is characterized in that, comprise the steps:
Step one: decaying catalyst duct is utilized iron wire and giant deashing, removes surperficial and that duct is residual silica, calcium sulfate and organic residue impurity, stand-by after air drying;
Step 2: dry decaying catalyst step one obtained is placed in tube furnace, in H
2the roasting of/He atmosphere, actual conditions: hydrogen volume ratio accounts for H
2between the 0-100% of/He atmosphere, H
2between/He gas flow 0-100ml/min, heating rate is 1-30 DEG C/min, rises to 400-650 DEG C from room temperature, and is held in this temperature calcination, and roasting time is between 0-10h, obtains the catalyst removing arsenic after Temperature fall;
Step 3: the catalyst removing arsenic step 2 obtained takes out, after 110 DEG C of dry 2h, be placed in air atmosphere roasting, roasting condition: between gas flow 0-50ml/min, heating rate is 1-50 DEG C/min, sintering temperature is 300-600 DEG C, and roasting time is between 0-10h, obtains regenerated catalyst.
2. the hydrogen reducing renovation process of the out of stock catalyst of a kind of arsenic poisoning according to claim 1, is characterized in that, comprise the steps:
Step one: first prepare vanadium tungsten titanium or vanadium molybdenum titanium catalyst by the precipitation method, be then placed on arsenic oxide arsenoxide As
2o
3after solution impregnation drying, obtain arsenic oxide arsenoxide As
2o
3mass concentration is 3%, then by the catalyst of arsenic poisoning after 450 degree of roasting 3h fix arsenic oxide arsenoxide, grinding is sieved, and obtains 40-60 order decaying catalyst;
Step 2: the decaying catalyst of 1g is placed in tube furnace, in H
2the roasting of/He atmosphere, roasting condition: hydrogen volume ratio accounts for H
210%, H of/He atmosphere
2/ He gas flow is 80mL/min, and heating rate is 20 DEG C/min, rises to 500 DEG C from room temperature, and in 500 DEG C of roastings, keeps 2h, obtain the catalyst removing arsenic after Temperature fall;
Step 3: the catalyst removing arsenic step 2 obtained takes out, and after 110 DEG C of dry 2h, is placed in air atmosphere roasting, roasting condition: gas flow 20ml/min, heating rate is 5 DEG C/min, and sintering temperature is 500 DEG C, roasting time is 2 hours, obtains regenerated catalyst.
3. the hydrogen reducing renovation process of the out of stock catalyst of a kind of arsenic poisoning according to claim 1, is characterized in that, comprise the steps:
Step one: first prepare cerium tungsten titanium catalyst by the precipitation method, be then placed on arsenic oxide arsenoxide As
2o
3after solution impregnation drying, obtain arsenic oxide arsenoxide As
2o
3mass concentration is that after 3%, 450 degree of roasting 3h fix arsenic oxide arsenoxide, grinding is sieved, and obtains 40-60 order decaying catalyst;
Step 2: the decaying catalyst of 1g is placed in tube furnace, in H
2the roasting of/He atmosphere, roasting condition: hydrogen volume ratio accounts for H
25%, H of/He atmosphere
2/ He gas flow is under the atmosphere of 50mL/min, and heating rate is 10 DEG C/min, rises to 600 DEG C from room temperature, and in 600 DEG C of roastings, keeps 20min, obtain the catalyst removing arsenic after Temperature fall;
Step 3: the catalyst removing arsenic step 2 obtained takes out, and after 110 DEG C of dry 2h, is placed in air atmosphere roasting, roasting condition: gas flow 50ml/min, heating rate is 10 DEG C/min, and sintering temperature is 600 DEG C, roasting time is 4 hours, obtains regenerated catalyst.
4. the hydrogen reducing renovation process of the out of stock catalyst of a kind of arsenic poisoning according to claim 1, is characterized in that, comprise the steps:
Step one: first prepare cerium tungsten titanium catalyst by the precipitation method, be then placed on arsenic oxide arsenoxide As
2o
3after solution impregnation drying, obtain arsenic oxide arsenoxide As
2o
3mass concentration is that after 3%, 450 degree of roasting 3h fix arsenic oxide arsenoxide, grinding is sieved, and obtains 40-60 order decaying catalyst;
Step 2: the decaying catalyst of 1g is placed in tube furnace, in H
2the roasting of/He atmosphere, roasting condition: hydrogen volume ratio accounts for H
240%, H of/He atmosphere
2/ He gas flow is 90mL/min, and heating rate is 30 DEG C/min, rises to 550 DEG C from room temperature, and in 550 DEG C of roastings, keeps 5h, obtain the catalyst removing arsenic after Temperature fall;
Step 3: the catalyst removing arsenic step 2 obtained takes out, and after 110 DEG C of dry 2h, is placed in air atmosphere roasting, roasting condition: gas flow 10ml/min, heating rate is 40 DEG C/min, and sintering temperature is 500 DEG C, roasting time is 2 hours, obtains regenerated catalyst.
5. the hydrogen reducing renovation process of the out of stock catalyst of a kind of arsenic poisoning according to claim 1, is characterized in that, comprise the steps:
Step one: first prepare vanadium tungsten titanium catalyst by the precipitation method, be then placed on arsenic oxide arsenoxide As
2o
3after solution impregnation drying, obtain arsenic oxide arsenoxide As
2o
3mass concentration is that after 3%, 450 degree of roasting 3h fix arsenic oxide arsenoxide, grinding is sieved, and obtains 40-60 order decaying catalyst;
Step 2: the decaying catalyst of 1g is placed in tube furnace, in H
2the roasting of/He atmosphere, roasting condition: hydrogen volume ratio accounts for H
280%, H of/He atmosphere
2/ He gas flow is 60mL/min, and heating rate is 10 DEG C/min, rises to 500 DEG C from room temperature, and in 500 DEG C of roastings, keeps 20min, obtain the catalyst removing arsenic after Temperature fall;
Step 3: the catalyst removing arsenic step 2 obtained takes out, and after 110 DEG C of dry 2h, is placed in air atmosphere roasting, roasting condition: gas flow 50ml/min, heating rate is 10 DEG C/min, and sintering temperature is 500 DEG C, roasting time is 8 hours, obtains regenerated catalyst.
6. the hydrogen reducing renovation process of the out of stock catalyst of a kind of arsenic poisoning according to claim 1, is characterized in that, comprise the steps:
Step one: Shen Zhi inactivation enterprise vanadium tungsten titanium catalyst duct is utilized iron wire and giant deashing, remove surperficial and that duct is residual silica, calcium sulfate and organic residue impurity, being cut into hole count is 3 × 3, and length is the small catalyst dried for standby of 100mm;
Step 2: the decaying catalyst that 10g step one obtains is placed in tube furnace, in H
2the roasting of/He atmosphere, roasting condition: hydrogen volume ratio accounts for H
21%, H of/He atmosphere
2/ He gas flow is 10mL/min, and heating rate is 5 DEG C/min, rises to 600 DEG C from room temperature, and in 600 DEG C of roastings, keeps 4h, obtain the catalyst removing arsenic after Temperature fall;
Step 3: the catalyst removing arsenic step 2 obtained takes out, and after 110 DEG C of dry 2h, is placed in air atmosphere roasting, roasting condition: gas flow 30ml/min, heating rate is 5 DEG C/min, and sintering temperature is 500 DEG C, roasting time is 3 hours, obtains regenerated catalyst.
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Cited By (2)
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| CN105251543B (en) | 2018-08-28 |
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