CN114107702A - Cleaning treatment method of waste petroleum catalyst - Google Patents
Cleaning treatment method of waste petroleum catalyst Download PDFInfo
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- CN114107702A CN114107702A CN202111468272.0A CN202111468272A CN114107702A CN 114107702 A CN114107702 A CN 114107702A CN 202111468272 A CN202111468272 A CN 202111468272A CN 114107702 A CN114107702 A CN 114107702A
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- deoiling
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- waste petroleum
- roasting
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- 239000002699 waste material Substances 0.000 title claims abstract description 70
- 239000003054 catalyst Substances 0.000 title claims abstract description 64
- 239000003208 petroleum Substances 0.000 title claims abstract description 53
- 238000000034 method Methods 0.000 title claims abstract description 36
- 238000004140 cleaning Methods 0.000 title claims abstract description 17
- 239000000463 material Substances 0.000 claims abstract description 62
- 238000002485 combustion reaction Methods 0.000 claims abstract description 25
- 238000002156 mixing Methods 0.000 claims abstract description 13
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 229910052720 vanadium Inorganic materials 0.000 claims description 72
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims description 72
- 238000000605 extraction Methods 0.000 claims description 21
- 239000000843 powder Substances 0.000 claims description 13
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 12
- 239000002893 slag Substances 0.000 claims description 10
- 229910000831 Steel Inorganic materials 0.000 claims description 6
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 6
- 239000010959 steel Substances 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 7
- 238000003912 environmental pollution Methods 0.000 abstract description 4
- 238000004064 recycling Methods 0.000 abstract description 4
- 238000011084 recovery Methods 0.000 description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 13
- 239000003921 oil Substances 0.000 description 12
- 238000002386 leaching Methods 0.000 description 11
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 8
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 7
- 229910052750 molybdenum Inorganic materials 0.000 description 7
- 239000011733 molybdenum Substances 0.000 description 7
- 229910052799 carbon Inorganic materials 0.000 description 6
- 239000000428 dust Substances 0.000 description 6
- 239000000295 fuel oil Substances 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 150000002739 metals Chemical class 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000000779 smoke Substances 0.000 description 3
- CMZUMMUJMWNLFH-UHFFFAOYSA-N sodium metavanadate Chemical compound [Na+].[O-][V](=O)=O CMZUMMUJMWNLFH-UHFFFAOYSA-N 0.000 description 3
- 239000011684 sodium molybdate Substances 0.000 description 3
- 235000015393 sodium molybdate Nutrition 0.000 description 3
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 description 3
- 229910000166 zirconium phosphate Inorganic materials 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- 239000002910 solid waste Substances 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000009854 hydrometallurgy Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- WUJISAYEUPRJOG-UHFFFAOYSA-N molybdenum vanadium Chemical compound [V].[Mo] WUJISAYEUPRJOG-UHFFFAOYSA-N 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/20—Obtaining niobium, tantalum or vanadium
- C22B34/22—Obtaining vanadium
- C22B34/225—Obtaining vanadium from spent catalysts
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/005—Preliminary treatment of scrap
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/02—Roasting processes
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/001—Dry processes
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/04—Working-up slag
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Geology (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention discloses a cleaning treatment method of a waste petroleum catalyst, which comprises the following steps: (1) mixing materials: mixing and stirring the waste petroleum catalyst and the auxiliary materials uniformly to obtain a mixed material; (2) preheating treatment: sending the mixed material into a preheating kiln for preheating treatment, wherein the preheating temperature is not more than 200 ℃; (3) deoiling treatment: feeding the preheated mixed material into a combustion furnace for deoiling treatment, wherein the deoiling temperature is 550-650 ℃, and the deoiling time is 30-60 min, so as to obtain a deoiled mixed material; (4) roasting: and (3) delivering the deoiled mixed material into a rotary kiln for roasting at the roasting temperature of 780-880 ℃ for 60-120 min to obtain roasted clinker, wherein the roasted clinker is recycled as a resource. The treatment process flow of the invention is short, saves energy, avoids the problem of environmental pollution caused by direct outdoor combustion, achieves the technical effect of clean roasting, and realizes the clean recycling of the waste petroleum catalyst.
Description
Technical Field
The invention relates to the technical field of waste petroleum treatment, in particular to a clean treatment method of a waste petroleum catalyst.
Background
The waste petroleum catalyst is a waste petroleum catalyst which is formed by the failure of the catalyst due to the adsorption of vanadium element in petroleum in the process of refining and hydrogenating the petroleum. The waste petroleum catalyst contains more useful metals such as vanadium, molybdenum, aluminum, nickel and the like, and belongs to important secondary solid waste resources. According to statistics, the quantity of the waste catalysts generated every year in the world is more than 100 million tons, and a large quantity of the waste catalysts are dumped at present, so that the land is occupied, and the environment is polluted, so that the method has very important significance for realizing the recovery of useful metals in the waste petroleum catalysts from the perspective of comprehensive utilization of resources and environmental protection.
The research of recovering valuable metals from waste catalysts in China starts at the initial stage of 21 st century, and the technologies of 'extracting vanadium, molybdenum and nickel from oil refining waste catalysts by an oxidation-reduction full-hydrometallurgy process' and 'adding alkali for roasting, water leaching and precipitating vanadium and molybdenum' are carried out successively, so that the comprehensive recovery of vanadium and molybdenum can be realized, but the recovery rate of vanadium is only 72%, the recovery rate of molybdenum is only 50%, the recovery rate is lower, the cost is higher, and the large-scale popularization and application are difficult. For example, patent 201510813956.8 discloses a method for recovering vanadium and molybdenum from waste petroleum catalyst, which is characterized in that vanadium and molybdenum can be recovered comprehensively, but heavy oil, light oil and carbon in the waste petroleum catalyst are ignited in air, the direct combustion causes great environmental pollution, and wastes such fuel resources, but if the waste petroleum catalyst is sealed in a rotary kiln and combusted, local temperature is too high, which damages the furnace lining and even causes deformation of the kiln body. Therefore, how to reasonably utilize the combustible in the waste petroleum catalyst and how to improve the recovery rate of valuable metals has important significance for the comprehensive utilization of the waste petroleum catalyst.
Chinese patent CN200410050503.6 discloses a method for producing vanadium pentoxide by using vanadium-containing spent catalyst, which comprises the following steps: firstly removing 30-40% of deposited oil in the vanadium-containing waste catalyst, crushing the deoiled waste catalyst, sieving more than 95% of the crushed waste catalyst through a 100-mesh sieve of 120 meshes, then putting the crushed waste catalyst into water with the weight of 2.5-3 times of that of the crushed waste catalyst for leaching, oxidizing the crushed waste catalyst through air/an oxidant, adding alkali to adjust the pH value to be 8.5-9.5, leaching for 1-2 hours at the temperature of 50-60 ℃, filtering the waste catalyst by a filter to separate solid from liquid, and recovering sodium vanadate and sodium molybdate solution as primary leaching solution; calcining the filter residue after filtering and washing in a rotary kiln, wherein the calcining temperature at the kiln head is 850-; dissolving the calcined material in hot water of 80-85 ℃, leaching for 40-60 minutes under stirring, filtering by a filter, and recovering sodium vanadate and sodium molybdate to obtain a secondary leaching solution; mixing the leachate, removing impurity phosphorus, adding excessive ammonium chloride into the leachate after the essence treatment at normal temperature to enable sodium vanadate to generate ammonium metavanadate precipitate, and leaving sodium molybdate in the solution to achieve vanadium-molybdenum separation; and putting the separated ammonium metavanadate into a tabletting furnace, and decomposing the ammonium vanadate at 800-850 ℃ to prepare the molten vanadium pentoxide. According to the patent technology, deoiling treatment is carried out by heating to 130-140 ℃, the deoiling rate of oil reaches 30-40%, then crushing and water leaching are carried out, the deoiling effect is poor, the deoiled oil cannot be directly used as a heat source, the recovery rate of vanadium is only 82.4%, the recovery rate is low, the tailings after vanadium extraction can only be used as waste for treatment, and the purpose of comprehensive utilization of vanadium resources is not achieved.
Disclosure of Invention
The invention aims to: aiming at the existing problems, a clean treatment method of the waste petroleum catalyst is provided to overcome the defects in the prior art.
The technical scheme adopted by the invention is as follows: a cleaning treatment method of a waste petroleum catalyst comprises the following steps:
(1) mixing materials: mixing and stirring the waste petroleum catalyst and the auxiliary materials uniformly to obtain a mixed material;
(2) preheating treatment: sending the mixed material into a preheating kiln for preheating treatment, wherein the preheating temperature is not more than 200 ℃;
(3) deoiling treatment: feeding the preheated mixed material into a combustion furnace for deoiling treatment, wherein the deoiling temperature is 550-650 ℃, and the deoiling time is 30-60 min, so as to obtain a deoiled mixed material;
(4) roasting: and (3) delivering the deoiled mixed material into a rotary kiln for roasting at the roasting temperature of 780-880 ℃ for 60-120 min to obtain roasted clinker, wherein the roasted clinker is recycled as a resource.
In the invention, the purpose of preheating the mixed material is to primarily remove water in the mixed material so as to improve the later-stage deoiling efficiency. The deoiling treatment is carried out at 550-650 ℃, and in the temperature range, the residual oil in the waste catalyst can be oxidized and removed above the ignition point, the generation amount of carbon particles can be controlled, and the phenomenon that too many carbon particles are formed due to overhigh temperature is avoided, so that the deoiling difficulty is increased. Furthermore, the deoiled waste petroleum catalyst is roasted instead of directly leaching vanadium by water, and roasting is carried out after deoiling, so that vanadium in the mixed material can be oxidized from low valence to pentavalent vanadium which is more soluble in water, and further the water leaching rate can be improved.
In the invention, the auxiliary materials are selected from one or more of vanadium extraction tailings, vanadium-containing steel slag and vanadium slag. The auxiliary materials basically belong to waste materials, the use cost is low, the auxiliary materials are added into the waste petroleum catalyst, the combustion value of combustible materials in the waste petroleum catalyst can be reduced, the kiln body is prevented from being damaged due to the overhigh combustion value, the combustion degree is controllable, the energy consumption of the treatment process is reduced, meanwhile, the auxiliary materials are reused, valuable metals in the waste materials can be recycled, and the purpose of comprehensively recycling vanadium resources is achieved.
Furthermore, the addition amount of the auxiliary materials is 0.5-1.5 times of the mass of the waste petroleum catalyst. Experiments prove that the impurities can be dissolved out more due to the excessively high addition amount of the auxiliary materials, the difficulty of an impurity removal process is increased, the risk is caused to the quality of a finished product, the amount of the auxiliary materials required for converting the vanadium from insoluble to soluble is insufficient due to the excessively low addition amount of the auxiliary materials, and the using effect of the auxiliary materials is not obvious.
In the invention, the roasted clinker is crushed to obtain clinker powder, and the clinker powder is used as a raw material of a subsequent vanadium extraction process.
In order to achieve the purpose of comprehensively recycling vanadium resources, the roasting clinker is subjected to vanadium extraction through a vanadium extraction process to obtain vanadium extraction tailings, and the vanadium extraction tailings are used as auxiliary materials.
In the present invention, the time of the preheating treatment is 30 to 60min, preferably 60 min. The preheating treatment time is not suitable to be too long or too short, energy is wasted if the time is too long, and the moisture cannot be dried in time if the time is too short.
Furthermore, when the materials are mixed, a certain amount of sodium carbonate is added and mixed together, the main purpose is to reduce the erosion effect on refractory materials and prolong the service life of the kiln, and the adding amount is proper, and no special requirement exists.
In the present invention, the combustible obtained by the deoiling treatment is used as a heat source. The method realizes reasonable utilization of combustible materials such as heavy oil, light oil, carbon and the like in the waste petroleum catalyst, avoids the problem of environmental pollution caused by direct outdoor combustion, and achieves the technical effect of clean roasting, thereby realizing clean reutilization of the waste petroleum catalyst.
In the invention, the deoiling temperature is preferably 650 ℃, and the deoiling time is preferably 60 min; the roasting temperature is preferably 880 ℃, and the roasting time is preferably 120 min.
In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that:
1. the invention reduces the combustion value of combustible materials in the waste petroleum catalyst by adding auxiliary materials, thereby avoiding the problem that the kiln body is damaged due to overhigh combustion value, controlling the combustion degree, reducing the energy consumption of the treatment process, realizing the reutilization of waste materials by selecting the auxiliary material materials, recycling valuable metals in the waste materials and achieving the purpose of comprehensively recovering vanadium resources;
2. according to the invention, the roasting clinker treated by the vanadium extraction process is used as an auxiliary material, so that the waste of vanadium resources is avoided, the generation of solid wastes is reduced, and the treatment cost of the process is reduced;
3. the treatment process flow of the invention is short, the utilization of combustible substances such as heavy oil, light oil, carbon and the like in the waste petroleum catalyst is realized, the energy is saved, the problem of environmental pollution caused by direct outdoor combustion is avoided, the technical effect of clean roasting is achieved, and the clean reutilization of the waste petroleum catalyst is realized.
Drawings
FIG. 1 is a schematic process flow diagram of a method for cleaning waste petroleum catalyst according to the present invention.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings.
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
As shown in fig. 1, a method for cleaning and treating waste petroleum catalyst comprises the following steps:
(1) mixing vanadium-containing steel slag and a waste petroleum catalyst according to the mass ratio of 50: 100, adding a certain amount of sodium carbonate, mixing, and uniformly stirring to obtain a mixed material;
(2) sending the mixed material into a preheating kiln for preheating treatment, wherein the preheating temperature is less than 200 ℃;
(3) feeding the preheated mixed material into a combustion furnace for combustion deoiling treatment at 650 ℃, and combusting for 60 min;
(4) feeding the mixed material subjected to the deoiling treatment of the combustion furnace into a rotary kiln for roasting, and roasting at 880 ℃ for 120min to obtain roasted clinker;
(5) and crushing the roasted clinker obtained after roasting in the rotary kiln to obtain clinker powder, and supplying the clinker powder to the subsequent vanadium extraction operation to obtain vanadium pentoxide.
The combustion furnace of this embodiment is equipped with dust collecting system, collects the smoke and dust that heavy oil burning produced among the waste petroleum catalyst, avoids the polluted environment.
In the cleaning treatment method of the embodiment, the waste petroleum catalyst containing 17.5% of vanadium and the steel slag containing 1.7% of vanadium are mixed and roasted, the removal rate of the oil is 85.3%, the obtained roasted clinker powder is subjected to vanadium recovery by a water vanadium extraction process (the existing water vanadium extraction process is adopted, no special requirement is required), and the comprehensive recovery rate of the vanadium is 87.59%.
Example 2
A cleaning treatment method of a waste petroleum catalyst comprises the following steps:
(1) mixing vanadium extraction tailings and a waste petroleum catalyst according to a mass ratio of 100: 100, adding a certain amount of sodium carbonate, mixing, and uniformly stirring to obtain a mixed material;
(2) sending the mixed material into a preheating kiln for preheating treatment, wherein the preheating temperature is less than 200 ℃;
(3) feeding the preheated mixed material into a combustion furnace for combustion and deoiling treatment at 600 deg.C for 50 min;
(4) feeding the mixed material subjected to the deoiling treatment of the combustion furnace into a rotary kiln for roasting, and roasting at 850 ℃ for 120min to obtain roasted clinker;
(5) and crushing the roasted clinker obtained after roasting in the rotary kiln to obtain clinker powder, and supplying the clinker powder to the subsequent vanadium extraction operation to obtain vanadium pentoxide.
The combustion furnace of this embodiment is equipped with dust collecting system, collects the smoke and dust that heavy oil burning produced among the waste petroleum catalyst, avoids the polluted environment.
In the cleaning treatment method of the embodiment, the vanadium extraction tailings containing vanadium 0.4% are mixed and roasted aiming at the waste petroleum catalyst containing vanadium 17.5%, the removal rate of the oil is 89.7%, the obtained roasted clinker powder recovers vanadium by a water vanadium extraction process, and the comprehensive recovery rate of the vanadium is 89.48%.
Example 3
A cleaning treatment method of a waste petroleum catalyst comprises the following steps:
(1) mixing vanadium slag and a waste petroleum catalyst according to a mass ratio of 50: 150, adding a certain amount of sodium carbonate, mixing, and uniformly stirring to obtain a mixed material;
(2) sending the mixed material into a preheating kiln for preheating treatment, wherein the preheating temperature is less than 200 ℃;
(3) feeding the preheated mixed material into a combustion furnace for combustion deoiling treatment at 650 ℃, and combusting for 60 min;
(4) feeding the mixed material subjected to the deoiling treatment of the combustion furnace into a rotary kiln for roasting, and roasting at 800 ℃ for 90min to obtain roasted clinker;
(5) and crushing the roasted clinker obtained after roasting in the rotary kiln to obtain clinker powder, and supplying the clinker powder to the subsequent vanadium extraction operation to obtain vanadium pentoxide.
The combustion furnace of this embodiment is equipped with dust collecting system, collects the smoke and dust that heavy oil burning produced among the waste petroleum catalyst, avoids the polluted environment.
In the cleaning treatment method of the embodiment, the vanadium slag containing 12% of vanadium is mixed and roasted aiming at the waste petroleum catalyst containing 17.5% of vanadium, the removal rate of the oil is 84.22%, the obtained roasted clinker powder recovers the vanadium by a water vanadium leaching process, and the comprehensive recovery rate of the vanadium is 85.14%.
Comparative example 1
Comparative example 1 is the same as example 1, except that no steel slag containing vanadium 1.7% is added, and the same amount of sodium carbonate is added to mix with the waste petroleum catalyst containing vanadium 17.5%, and then the mixture is preheated, deoiled, and roasted, and the test result is: the comprehensive recovery rate of vanadium is 82.12%, and the deoiling rate is 80.09%, so that the oil content needs to be diluted by adding oil-free additives in the deoiling process, the deoiling efficiency is improved, the local overhigh temperature is prevented, and the risk of equipment damage is reduced.
Comparative example 2
Comparative example 2 is the same as example 1 except that steel slag containing 1.7% vanadium is added in an amount of 2 times the mass of the waste petroleum catalyst. The test results are as follows: the comprehensive recovery rate of vanadium is 79.04%, and the deoiling rate is 89.7%, which shows that although the deoiling rate is higher, the recovery rate of vanadium is obviously reduced, so that the proper adding proportion of the auxiliary materials is beneficial to simultaneously improving the recovery rate and the deoiling rate.
Comparative example 3
Comparative example 3 is the same as example 1 except that the preheating treatment is not performed but the baking treatment is directly performed. The test results are as follows: the overall recovery of vanadium was 79.04% and the deoiling rate was 77.26%, indicating that without preheating, the loss of heat energy reduces the deoiling efficiency and the recovery of vanadium.
Comparative example 4
Comparative example 4 is the same as example 1, except that after the auxiliary materials are added and mixed, the mixed material is heated to 130-140 ℃ for deoiling treatment by adopting the deoiling mode of the prior patent CN200410050503.6, and vanadium is recovered by water leaching directly after the deoiling. The test results are as follows: the comprehensive recovery rate of vanadium is 67.52%, and the deoiling rate is 51.17%, so that the deoiling mode of the prior patent has a poorer technical effect compared with the deoiling mode of the invention, and the technical scheme of the invention not only greatly improves the recovery rate of vanadium, but also improves the deoiling efficiency and reduces the environmental risk.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (9)
1. A cleaning treatment method of a waste petroleum catalyst is characterized by comprising the following steps:
(1) mixing materials: mixing and stirring the waste petroleum catalyst and the auxiliary materials uniformly to obtain a mixed material;
(2) preheating treatment: sending the mixed material into a preheating kiln for preheating treatment, wherein the preheating temperature is not more than 200 ℃;
(3) deoiling treatment: feeding the preheated mixed material into a combustion furnace for deoiling treatment, wherein the deoiling temperature is 550-650 ℃, and the deoiling time is 30-60 min, so as to obtain a deoiled mixed material;
(4) roasting: and (3) delivering the deoiled mixed material into a rotary kiln for roasting at the roasting temperature of 780-880 ℃ for 60-120 min to obtain roasted clinker, wherein the roasted clinker is recycled as a resource.
2. The method for cleaning the waste petroleum catalyst as claimed in claim 1, wherein the auxiliary material is selected from one or more of vanadium extraction tailings, vanadium-containing steel slag and vanadium slag.
3. The method for cleaning the waste petroleum catalyst as claimed in claim 2, wherein the addition amount of the auxiliary material is 0.5-1.5 times of the mass of the waste petroleum catalyst.
4. The method of claim 3, wherein the roasted clinker is crushed to obtain clinker powder, and the clinker powder is used as a raw material for a subsequent vanadium extraction process.
5. The method for cleaning the waste petroleum catalyst as claimed in claim 4, wherein the roasted clinker is subjected to vanadium extraction to obtain vanadium extraction tailings, and the vanadium extraction tailings are used as auxiliary materials.
6. The method for cleaning a waste petroleum catalyst as claimed in any one of claims 1 to 5, wherein the preheating treatment is carried out for 30 to 60 minutes.
7. The method of claim 6, wherein a predetermined amount of sodium carbonate is added and mixed together when the materials are mixed.
8. The method of claim 7, wherein the combustible obtained by the deoiling treatment is used as a heat source.
9. The method for cleaning the waste petroleum catalyst as claimed in claim 8, wherein the deoiling temperature is 650 ℃, the deoiling time is 60 min; the roasting temperature is 880 ℃, and the roasting time is 120 min.
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