CN103599796B - A kind of renovation process of alloyed powder catalyst - Google Patents
A kind of renovation process of alloyed powder catalyst Download PDFInfo
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Abstract
The invention provides the renovation process of a kind of alloyed powder catalyst, after it carries out sifting sort to pretreated inactivation alloyed powder catalyst, dual pathways route is used to carry out Regeneration Treatment sorted high value catalyst and low value catalyst, wherein the regeneration of high value catalyst includes accompanying burning and two processes of Acid leaching through vulcanizing treatment, burning carbon, reduction, acidization, the regeneration of low value catalyst.The present invention uses dual channel mode to process the alloyed powder catalyst of inactivation, optimizes the efficiency of alloyed powder regeneration so that the alloyed powder catalyst of inactivation is recycled to greatest extent, has saved energy consumption, has promoted environmental conservation；Stage of making charcoal adds a certain amount of sulfur, reduces the agglomeration of noble metal in alloyed powder catalyst；For the inactivation alloyed powder catalyst of low value, abandon traditional accompanying and burn and the mode of melting, but the method taking Acid leaching, substantially increase the organic efficiency of noble metal, make the response rate of metal reach 95～99%.
Description
Technical field
The present invention relates to the renovation process of a kind of catalyst, be specifically related to the renovation process of a kind of alloyed powder catalyst, belong to
In industrial catalyst regeneration field.
Background technology
Catalyst has been widely used in chemical industry, thus also produces substantial amounts of dead catalyst, and dead catalyst belongs to
Heavy metal dangerous materials are useless solid, process and need to spend financial resources, and cause serious pollution environment.Therefore, one is the most usually taked
Fixed method carries out existing regeneration to dead catalyst, is so possible not only to reduce the pollution of environment, can also save energy simultaneously
The utilization in source, increase economic efficiency.
Processing mode two kinds of thinkings nothing more than of the existing alloyed powder catalyst for having inactivated: a kind of is urging inactivation
Agent carries out roasting simply and melting as waste metal.This mode operates the simplest, but in alloyed powder catalyst
Metal, especially noble metal organic efficiency is the lowest, and a large amount of highly purified metals are run off, deficiency in economic performance.Meanwhile, roasting is with molten
Refining process can produce more environmental contaminants, poses a big pressure local environmental conservation.
Another kind is to be catalyzed alloyed powder by complicated making charcoal, burning sulfur and a series of process such as acidifying, hydrogen reducing
Agent carries out ex-situ regeneration.Although this method can promote the service efficiency of alloyed powder catalyst in theory so that inactivation
Catalyst obtains resurrection largely, again puts into production.But, in practice, because the alloyed powder of inactivation is urged
In agent, some is because the change of metal crystalline state on catalyst and assembles, collapsing etc. of catalyst and pore structure thereof causes
Permanent inactivation, the step for regeneration of row complexity more above-mentioned for this partial catalyst is invalid, so causing regrowth
Material, the waste of the energy, because of the existence of this demi-permanent decaying catalyst, overall resurrection rate is not yet for the catalyst after regeneration
High.
In the existing alloyed powder catalyst regeneration method to inactivation, stress tamper in catalyst backbone structure
Remove, dredge duct, recover the surface area of catalyst, and the removal of the inert metal to surface deposition, recover skeleton surface
Effective active center on Ji.But, existing method often have ignored catalytic metal and the rendezvous problem of co-catalysis metal, lives
The situation of property accumulation of metal causes the active center distribution of alloyed powder catalyst the most uneven, has upset the reasonable of active center
Distribution.
Summary of the invention
Goal of the invention: the purpose of the present invention is aiming at the deficiency in current alloyed powder dead catalyst renovation process, it is provided that
A kind of renovation process of alloyed powder catalyst.
Technical scheme: for achieving the above object, this invention takes following technical scheme:
A kind of renovation process of alloyed powder catalyst, it is characterised in that: pretreated inactivation alloyed powder catalyst is entered
After row filter classification, then dual pathways route is used to carry out at regeneration sorted high value catalyst and low value catalyst
Reason, specifically comprises the following steps that
(1) pretreatment: to inactivation alloyed powder catalyst be first washed with deionized, then priority diluted sodium hydroxide solution with
Strong caustic carries out gradient type washing, then is washed with deionized, last dry for standby；
(2) screening: separating screen device poured into by the inactivation alloyed powder catalyst after drying, is divided into by catalyst according to screening criteria
2～4 kinds, and distinguish the inactivation alloyed powder catalyst of high value and low value；
(3) dual pathways route carries out Regeneration Treatment to inactivation alloyed powder catalyst: high value catalyst after differentiation and low
Be worth catalyst uses different routes to process, wherein simultaneously:
A: high value catalyst regeneration route: the inactivation alloyed powder catalyst of high value is successively through vulcanizing treatment, burning
Carbon, reduce, be acidified regenerative process, particularly as follows:
A: vulcanizing treatment: inactivation alloyed powder catalyst enters vulcanization plant, is vulcanizing with vulcanizing agent in vulcanization plant
The catalyst inactivated；
B: burn carbon: cured catalyst burns carbon under oxygen；
C: reduction: after burning carbon terminates, with hydrogen reduction catalyst 1～10h；
D: acidifying regeneration: the catalyst after over cure, burning carbon, reduction enters acidizing device and carries out acidification, finally
Obtain the catalyst after regeneration.
B: low value catalyst regeneration route: the inactivation alloyed powder catalyst of low value is introduced into calciner, adds
Na2CO3Roasting 2～5h, then Acid leaching groove poured into by the catalyst after roasting, reclaims metal by Acid leaching.
Preferably, described step 1 is particularly as follows: by uneven slimy inactivation alloyed powder catalyst, with going after heating
Ionized water washs, and the temperature of hot water is 30 DEG C～100 DEG C；Then with the diluted sodium hydroxide solution washing that concentration is 2%～10%,
Control temperature at 3 DEG C～50 DEG C, then with the washing of strong caustic that concentration is 20%～50%, control temperature be 30 DEG C～
100 DEG C, keep 1～10h, during a steady state value being maintained between 0.1～0.5MPa of pressure；Then going by room temperature
Ionized water washs to pH=6～8；Finally drying, the catalyst after drying is available for next step screening and uses.
Preferably, the separating screen device used in described step 2 is: separating screen device or discontinuous semi-automatic sub-sieve automatically
Device；The screening criteria used is: large granular catalyst more than some value in 10～200 mesh is defined as high regeneration and is worth
Catalyst, the catalyst particle below some value in 10～300 mesh is defined as low regeneration be worth catalyst.
Preferably, vulcanizing agent employed in sulfidation processes described in described step 3 route A include sulfur dioxide,
One or both in lightweight mercaptan, hydrogen sulfide, temperature during sulfuration is 50 DEG C～250 DEG C, and pressure is normal pressure to 3.6MPa.
Preferably, the sulfur dioxide of 100ppm ~ 2%, institute can also be added during burning carbon described in described step 3 route A
Stating temperature when burning carbon is 200 DEG C～500 DEG C, and oxygen concentration is 0.5% ~ 20%.
Preferably, temperature when reducing in reduction process described in described step 3 route A is 300 DEG C～500 DEG C, pressure
Power is normal pressure～2.9MPa.
Preferably, addition active metal component in regenerative process it is acidified described in described step 3 route A.
Preferably, described active metal component is at least one in Co, Ni, Mo, W, adding of described active metal component
Enter the 2.5% ~ 5.5% of the weight that amount is the alloyed powder catalyst needing regeneration.
Preferably, in described step 3 route B, Na2CO3The temperature used during roasting is 200 DEG C～600 DEG C.
Preferably, in described step 3 route B, Acid leaching reclaims in metal process, and acid used is sulphuric acid, nitric acid, salt
One or more in acid, oxalic acid, citric acid, gluconic acid, tartaric acid.
Beneficial effect: use the invention have the advantages that of technique scheme
1, the dual channel mode used processes the alloyed powder catalyst of inactivation, optimizes the efficiency of alloyed powder regeneration so that
The alloyed powder catalyst of inactivation is recycled to greatest extent, has saved energy consumption, has promoted environmental conservation.
2, inactivation alloyed powder catalyst is carried out pretreatment, be possible not only to the raw material magazine tentatively removing in catalyst, and
And create condition for follow-up screening link.
3, the special screening plant that the present invention uses first, and screening criteria, is divided into height by inactivation alloyed powder catalyst
It is worth and low value two class, carries out following process and process by different processing routines respectively, make decaying catalyst Maximum Value
Change, more rationally, sufficiently utilize the energy.
4, the present invention adds a certain amount of sulfur in the stage of making charcoal, and greatly reduces the agglomeration of noble metal in alloyed powder catalyst
Effect, the inactivation alloyed powder catalyst energy activity recovery processed through the present invention causes the 80～90% of fresh catalyst.
5, for the inactivation alloyed powder catalyst of low value, abandon the mode of traditional roasting and melting, but take acid
The method of leaching, substantially increases the organic efficiency of noble metal so that the response rate of metal reaches 95～99%.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in detail, but protection scope of the present invention is described also simultaneously
Being not limited to the concrete scope of the present embodiment, based on the embodiment in the present invention, those of ordinary skill in the art are not making
The every other embodiment obtained under creative work premise, broadly falls into the scope of protection of the invention.
Embodiment 1: the renovation process of the alloyed powder catalyst of the present embodiment is specific as follows:
(1) deionized water is heated to about 45 DEG C, then chooses slimy inactivation alloyed powder catalyst, with 45 DEG C of left sides
Right deionized water wash；Inactivation alloyed powder catalyst after washing proceeds to reactor, first molten with the dilute sodium hydroxide of concentration 4%
Liquid washs, and control temperature is at 20 DEG C, and after diluted sodium hydroxide solution washing, the strong caustic adding concentration 30% is washed
Washing, controlling temperature is 50 DEG C, keeps 8h, and the pressure in alkaline cleaning procedure is maintained at about 0.2MPa；Then with under room temperature state
Deionized water wash is to pH=6～8；Finally drying, the catalyst after drying is available for next step screening and uses；
(2) automatic splinter screening device for screening poured into by the inactivation alloyed powder catalyst after drying, and device works continuously, automatically will catalysis
Agent is divided into 2～4 kinds, and large granular catalysts more than 50 mesh is defined as the catalyst that high regeneration is worth by us, by 250 mesh
Following catalyst particle is defined as the catalyst that low regeneration is worth；
(3), after sifting sort, the inactivation alloyed powder catalyst that height regeneration is worth is sent into vulcanization plant, in vulcanization plant
With the weathered catalyst of sulfur dioxide sulfuration, with dioxygen oxidation carbon on sulphurized catalyst, then urge with hydrogen reduction
Agent, is simultaneously introduced lightweight mercaptan and mixes with hydrogen as vulcanizing agent, vulcanizing agent, and temperature is 200 DEG C, pressure be normal pressure extremely
Vulcanize under 3.6MPa, until outlet streams can detect vulcanizing agent；Catalyst after sulfuration is dense in suitable temperature and oxygen
Burning carbon under degree, burn the oxygen flow oxygen-containing 8% during carbon, temperature is 250 DEG C, is simultaneously introduced the sulfur dioxide of 1%；After burning carbon terminates,
With hydrogen reducing, reduction temperature 350 DEG C, pressure is normal pressure～2.9MPa, reduction 6h；Finally, catalyst entrance acidifying still enters
Row acidifying regeneration, be simultaneously introduced inactivation alloyed powder catalyst weight 3% active metal Co and Ni with promote regeneration after urging
Agent activity；
(4), after sifting sort, the inactivation alloyed powder catalyst that low regeneration is worth enters Acid leaching reclaimer, first will catalysis
Calciner is sent in agent, adds Na at 300 DEG C2CO3Roasting 4h；Then pour the catalyst after roasting into Acid leaching groove, select
Acid be sulphuric acid, oxalic acid, gluconic acid, tartaric mixture.
Through the process of above-mentioned steps, inactivation alloyed powder catalyst energy activity recovery causes the 85% of fresh catalyst, metal
The response rate reaches 95%.
Embodiment 2: the renovation process of the alloyed powder catalyst of the present embodiment is specific as follows:
(1) deionized water is heated to about 75 DEG C, then chooses slimy inactivation alloyed powder catalyst, with 5 DEG C of left sides
Right deionized water wash；Inactivation alloyed powder catalyst after washing proceeds to reactor, first molten with the dilute sodium hydroxide of concentration 8%
Liquid washs, and control temperature is at 40 DEG C, and after diluted sodium hydroxide solution washing, the strong caustic adding concentration 40% is washed
Washing, controlling temperature is 65 DEG C, keeps 5h, and the pressure in alkaline cleaning procedure is maintained at about 0.4MPa；Then with under room temperature state
Deionized water wash is to pH=6～8；Finally drying, the catalyst after drying is available for next step screening and uses；
(2) automatic splinter screening device for screening poured into by the inactivation alloyed powder catalyst after drying, and device works continuously, automatically will catalysis
Agent is divided into 2～4 kinds, and large granular catalysts more than 50 mesh is defined as the catalyst that high regeneration is worth by us, by 250 mesh
Following catalyst particle is defined as the catalyst that low regeneration is worth；
(3), after sifting sort, the inactivation alloyed powder catalyst that height regeneration is worth is sent into vulcanization plant, in vulcanization plant
With the weathered catalyst of sulfur dioxide sulfuration, with dioxygen oxidation carbon on sulphurized catalyst, then urge with hydrogen reduction
Agent, is simultaneously introduced hydrogen sulfide and mixes with hydrogen as vulcanizing agent, vulcanizing agent, and temperature is 150 DEG C, and pressure is normal pressure under 3.6MPa
Sulfuration, until can detect vulcanizing agent in outlet streams；Cured catalyst burns carbon at suitable temperature and oxygen concentration,
Burning the oxygen flow oxygen-containing 15% during carbon, temperature is 300 DEG C, is simultaneously introduced the sulfur dioxide of 2%；Burn after carbon terminates, with hydrogen and
The mixed gas reduction of hydrogen sulfide, hydrogen sulfide content is 5%, reduction temperature 400 DEG C, and pressure is normal pressure～2.9MPa, reduction
8h；Finally, catalyst enter acidifying still carries out acidifying regeneration, be simultaneously introduced inactivation alloyed powder catalyst weight 4.5% work
Property metal Mo and W with promote regeneration after catalyst activity；
(4), after sifting sort, the inactivation alloyed powder catalyst that low regeneration is worth enters Acid leaching reclaimer, first will catalysis
Calciner is sent in agent, adds Na at 400 DEG C2CO3Roasting 2～5h；Then the catalyst after roasting is poured into Acid leaching groove,
The acid selected is nitric acid, hydrochloric acid, citric acid, tartaric mixture.
Through the process of above-mentioned steps, inactivation alloyed powder catalyst energy activity recovery causes the 89% of fresh catalyst, metal
The response rate reaches 99%.
Comparative example: original inactivation alloyed powder catalyst regeneration process method is as follows:
(1) first to inactivation alloyed powder catalyst deionized water at room temperature wash, after washing again with about 20% hydrogen
Sodium hydroxide solution is washed, and wash time is 3～5h, and during alkali cleaning, temperature is maintained at 40 DEG C～50 DEG C, goes by room temperature the most again
Ionized water is washed, and finally dries；
(2) the alloyed powder catalyst after drying enters vulcanization plant and carries out vulcanizing treatment, with sulfur dioxide sulfuration inactivation
Alloyed powder catalyst, with dioxygen oxidation carbon on sulphurized catalyst, then uses hydrogen reduction catalyst, and curing temperature is less than
300 DEG C, pressure, at normal pressure to 2MPa, carries out burning carbon and processes after sulfuration, in processing procedure, the concentration of oxygen is about 5%, and temperature is
Less than 750 DEG C, burn under conditions of temperature about 500 DEG C, pressure 2 about MPa, after carbon terminates, directly use hydrogen reducing, finally
Acidification is carried out with acid.
After being processed by this kind of method, inactivation alloyed powder catalyst energy activity recovery causes about the 60% of fresh catalyst, but
Being that the response rate of metal is the lowest is less than 50%.
Compared with conventional method, first catalyst is screened and classifies by the present invention, urges sorted high value
Agent and low value catalyst use dual channel mode to process simultaneously, and wash catalyst pretreatment alkali liquor before treatment
Use linear gradient elution method when washing, and the stage of making charcoal adds a certain amount of sulfur, greatly reduces noble metal in alloyed powder catalyst
Agglomeration, the last acid treatment stage adds a small amount of active metal component to promote the catalyst activity after regeneration, and processes
The final result resurrection probability being greatly improved decaying catalyst compared with the past, and the response rate of metal is the most greatly
Improve, 95～99% can be reached.
Claims (6)
1. the renovation process of an alloyed powder catalyst, it is characterised in that: pretreated inactivation alloyed powder catalyst is carried out
After sifting sort, then dual pathways route is used to carry out Regeneration Treatment sorted high value catalyst and low value catalyst,
Specifically comprise the following steps that
(1) pretreatment: inactivation alloyed powder catalyst is first washed with deionized, then priority diluted sodium hydroxide solution and dense hydrogen
Sodium hydroxide solution carries out gradient type washing, then is washed with deionized, last dry for standby；
(2) screening: separating screen device poured into by the inactivation alloyed powder catalyst after drying, is divided into 2～4 according to screening criteria by catalyst
Individual kind, and distinguish the inactivation alloyed powder catalyst of high value and low value；
(3) dual pathways route carries out Regeneration Treatment to inactivation alloyed powder catalyst: the high value catalyst after differentiation and low value
Catalyst uses different routes to process, wherein simultaneously:
A: high value catalyst regeneration route: the inactivation alloyed powder catalyst of high value successively through vulcanizing treatment, burn carbon, also
Former, acidifying regenerative process, particularly as follows:
A: vulcanizing treatment: inactivation alloyed powder catalyst enters vulcanization plant, has inactivated with vulcanizing agent sulfuration in vulcanization plant
Catalyst；
B: burn carbon: cured catalyst burns carbon under oxygen；
C: reduction: after burning carbon terminates, with hydrogen reduction catalyst 1～10h；
D: acidifying regeneration: the catalyst after over cure, burning carbon, reduction enters acidizing device and carries out acidification, finally obtains
Catalyst after regeneration；
B: low value catalyst regeneration route: the inactivation alloyed powder catalyst of low value is introduced into calciner, adds Na2CO3Roasting
Burning 2～5h, then Acid leaching groove poured into by the catalyst after roasting, reclaims metal by Acid leaching；
It is acidified described in described step 3 route A in regenerative process and adds active metal component；Described active metal component be Co,
At least one in Ni, Mo, W, the addition of described active metal component is the weight of the alloyed powder catalyst needing regeneration
2.5%～5.5%；
Described screening criteria is: large granular catalysts more than 50 mesh is defined as high value catalyst, below 250 mesh
Little granule is defined as low value catalyst；
Described step 1 is particularly as follows: by uneven slimy inactivation alloyed powder catalyst, with the deionized water wash after heating,
The temperature of hot water is 30 DEG C～100 DEG C；Then with the diluted sodium hydroxide solution washing that concentration is 2%～10%, temperature is controlled 3
DEG C～50 DEG C, then with the washing of strong caustic that concentration is 20%～50%, controlling temperature is 30 DEG C～100 DEG C, keeps 1
～10h, during a steady state value being maintained between 0.1～0.5MPa of pressure；Then with the deionized water wash of room temperature
To pH=6～8；Finally drying, the catalyst after drying is available for next step screening and uses.
The renovation process of a kind of alloyed powder catalyst the most according to claim 1, it is characterised in that: described step 3 route A
Described in vulcanizing agent employed in sulfidation processes include in sulfur dioxide, lightweight mercaptan, hydrogen sulfide one or both,
Temperature during sulfuration is 50 DEG C～250 DEG C, and pressure is normal pressure to 3.6MPa.
The renovation process of a kind of alloyed powder catalyst the most according to claim 1, it is characterised in that: described step 3 route A
Described in burn the sulfur dioxide that can also add 100ppm～2% during carbon, temperature during described burning carbon is 200 DEG C～500
DEG C, oxygen concentration is 0.5%～20%.
The renovation process of a kind of alloyed powder catalyst the most according to claim 1, it is characterised in that: described step 3 route A
Described in temperature when reducing in reduction process be 300 DEG C～500 DEG C, pressure is normal pressure～2.9MPa.
The renovation process of a kind of alloyed powder catalyst the most according to claim 1, it is characterised in that: described step 3 route B
In, Na2CO3The temperature used during roasting is 200 DEG C～600 DEG C.
The renovation process of a kind of alloyed powder catalyst the most according to claim 1, it is characterised in that: described step 3 route B
In, Acid leaching reclaims in metal process, and acid used is sulphuric acid, nitric acid, hydrochloric acid, oxalic acid, citric acid, gluconic acid, tartaric acid
In one or more.
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| CN1179118A (en) * | 1995-03-20 | 1998-04-15 | 国际壳牌研究有限公司 | Process for catalyst regeneration |
| US6559085B1 (en) * | 1998-05-12 | 2003-05-06 | Mitsubishi Rayon Co., Ltd. | Method for regenerating molybdenum-containing oxide fluidized-bed catalyst |
| CN1697815A (en) * | 2003-08-22 | 2005-11-16 | 三菱化学株式会社 | Method of regenerating catalyst |
| CN101147865A (en) * | 2006-09-20 | 2008-03-26 | 中国石油化工股份有限公司 | Method for preparing hydrogenation refined catalyst from waste catalyst |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6800579B2 (en) * | 2002-01-29 | 2004-10-05 | Exxonmobil Research And Engineering Company | Catalyst regeneration |
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|---|---|---|---|---|
| CN1179118A (en) * | 1995-03-20 | 1998-04-15 | 国际壳牌研究有限公司 | Process for catalyst regeneration |
| US6559085B1 (en) * | 1998-05-12 | 2003-05-06 | Mitsubishi Rayon Co., Ltd. | Method for regenerating molybdenum-containing oxide fluidized-bed catalyst |
| CN1697815A (en) * | 2003-08-22 | 2005-11-16 | 三菱化学株式会社 | Method of regenerating catalyst |
| CN101147865A (en) * | 2006-09-20 | 2008-03-26 | 中国石油化工股份有限公司 | Method for preparing hydrogenation refined catalyst from waste catalyst |
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