CN113025834A - Method for recovering molybdenum from waste catalyst - Google Patents
Method for recovering molybdenum from waste catalyst Download PDFInfo
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- CN113025834A CN113025834A CN202011526178.1A CN202011526178A CN113025834A CN 113025834 A CN113025834 A CN 113025834A CN 202011526178 A CN202011526178 A CN 202011526178A CN 113025834 A CN113025834 A CN 113025834A
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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
- C22B34/30—Obtaining chromium, molybdenum or tungsten
- C22B34/34—Obtaining molybdenum
- C22B34/345—Obtaining molybdenum from spent catalysts
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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
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/02—Roasting processes
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- 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
- C22B7/006—Wet processes
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Abstract
The embodiment of the invention relates to a method for recovering molybdenum in a waste catalyst, which comprises the following steps: respectively grinding the waste catalyst and sodium carbonate, and stirring and mixing the ground waste catalyst and the sodium carbonate; placing the mixed waste catalyst and sodium carbonate into a vacuum resistance furnace for roasting to obtain a roasted product, wherein the roasting temperature is 140-200 ℃; leaching the roasted product by using distilled water to obtain a mixture of leachate and leaching residues; and separating the mixture of the leaching solution and the leaching residue to obtain the leaching solution. According to the method for recovering molybdenum from the waste catalyst, on one hand, a vacuum technology is used, the process flow is simple, the process period is short, so that the process energy consumption is reduced, on the other hand, additives in the process are relatively harmless, the molybdenum recovery rate is high, waste residue components generated after molybdenum recovery of the waste catalyst are not obviously damaged, the recovery of other subsequent ions is not influenced, secondary pollution is not caused, and the method is environment-friendly.
Description
Technical Field
The embodiment of the invention relates to the technical field of environmental protection and comprehensive utilization of resource recovery, in particular to a method for recovering molybdenum in a waste catalyst.
Background
Petrochemical catalysts are commonly used in the petrochemical industry to eliminate sulfur from various organic materials present in different parts of petroleum. These catalysts mostly consist of molybdenum, cobalt and nickel supported on alumina, mainly including molybdenum-cobalt-alumina systems, molybdenum-nickel-alumina systems, molybdenum-cobalt-nickel-alumina systems catalysts. With the continuous use for a long time, the petrochemical catalyst is gradually contaminated with impurities such as carbon, vanadium, oxygen, sulfur, etc. in the crude oil to become ineffective, and the deactivated catalyst is classified as a hazardous solid waste due to its contents of components harmful to the environment, requiring strict disposal.
The waste petrochemical catalyst contains rare metals and is regarded as an important secondary resource. In the related art, in order to recover valuable metals such as molybdenum from the waste petrochemical catalyst, for example, pyrometallurgical, hydrometallurgical or a combination thereof is generally used.
With regard to the above technical solutions, the inventors have found that at least some of the following technical problems exist: the process flow is too long, the environment is harsh, the energy consumption is too large, and the resource waste is caused; the recovery rate of precious metals is low; because a large amount of additives are added during the treatment of the waste catalyst, compared with the waste catalyst before treatment, the waste residue after treatment has serious damage to the components, can not be reused and recycled, and causes serious secondary pollution.
Accordingly, there is a need to ameliorate one or more of the problems with the related art solutions described above.
It is noted that this section is intended to provide a background or context to the embodiments of the invention that are recited in the claims. The description herein is not admitted to be prior art by inclusion in this section.
Disclosure of Invention
It is an object of embodiments of the present invention to provide a method for recovering molybdenum from a spent catalyst, thereby overcoming, at least to some extent, one or more of the problems due to limitations and disadvantages of the related art.
According to a first aspect of embodiments of the present invention, there is provided a method for recovering molybdenum from a spent catalyst, comprising:
respectively grinding the waste catalyst and sodium carbonate, and stirring and mixing the ground waste catalyst and the sodium carbonate;
placing the mixed waste catalyst and sodium carbonate into a vacuum resistance furnace for roasting to obtain a roasted product, wherein the roasting temperature is 140-200 ℃;
leaching the roasted product by using distilled water to obtain a mixture of leachate and leaching residues;
and separating the mixture of the leaching solution and the leaching residue to obtain the leaching solution.
In an embodiment of the present invention, the waste catalyst and the sodium carbonate are ground respectively until the particle sizes of the waste catalyst and the sodium carbonate are 50 to 200 meshes.
In an embodiment of the present invention, the waste catalyst and the sodium carbonate are ground separately until the particle size of the waste catalyst and the sodium carbonate is 200 meshes.
In one embodiment of the present invention, when the ground waste catalyst and the sodium carbonate are stirred and mixed, the mass of the sodium carbonate is 25% to 40% of the mass of the waste catalyst.
In one embodiment of the present invention, when the ground waste catalyst and the sodium carbonate are stirred and mixed, the mass of the sodium carbonate is 30% of the mass of the waste catalyst.
In an embodiment of the invention, the mixed waste catalyst and sodium carbonate are put into a vacuum resistance furnace for roasting to obtain a roasted product, wherein the roasting time is 20-50 min.
In an embodiment of the invention, the mixed waste catalyst and sodium carbonate are put into a vacuum resistance furnace to be roasted to obtain a roasted product, wherein the roasting time is 30min, and the roasting temperature is 160 ℃.
In an embodiment of the present invention, when the roasted product is leached with distilled water, the mass ratio of the roasted product to the distilled water is 1: 4-8, the leaching time is 10-30 min, the leaching temperature is 60-100 ℃, and the stirring intensity is 200-500 rpm.
In one embodiment of the invention, when the roasted product is leached by using distilled water, the mass ratio of the roasted product to the distilled water is 1:6, the leaching time is 20min, the leaching temperature is 80 ℃, and the stirring intensity is 300 rpm.
In an embodiment of the present invention, a suction filter or a centrifuge is used to separate the leachate from the leaching residue.
The technical scheme provided by the embodiment of the invention can have the following beneficial effects:
in the embodiment of the invention, on one hand, the method for recovering molybdenum from the waste catalyst uses a vacuum technology, has simple process flow and short process period, so that the process energy consumption is greatly reduced, and on the other hand, the additive in the process is relatively harmless and the molybdenum recovery rate is high, and the waste residue component after molybdenum recovery of the waste catalyst is not obviously damaged, the recovery of other subsequent ions is not influenced, secondary pollution is not caused, and the method is environment-friendly.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments consistent with the present disclosure and together with the description, serve to explain the principles of the disclosure. It is to be understood that the drawings in the following description are merely exemplary of the disclosure, and that other drawings may be derived from those drawings by one of ordinary skill in the art without the exercise of inventive faculty.
FIG. 1 illustrates a process flow diagram of a method for recovering molybdenum from spent catalyst in an exemplary embodiment of the invention;
FIG. 2 is a graph showing the trend of the effect of the calcination temperature on the leaching rate of molybdenum in a leachate in a method for recovering molybdenum from a spent catalyst according to an exemplary embodiment of the present invention;
FIG. 3 is a graph showing the trend of the effect of the amount of sodium carbonate added in the method for recovering molybdenum from a spent catalyst on the leaching rate of molybdenum in a leachate according to an exemplary embodiment of the present invention
FIG. 4 is a graph showing the trend of the effect of calcination time on the leaching rate of molybdenum in a leachate in a method for recovering molybdenum from a spent catalyst according to an exemplary embodiment of the present invention;
FIG. 5 is a graph showing the trend of the effect of leaching temperature on the leaching rate of molybdenum in a leachate in a method for recovering molybdenum from a spent catalyst according to an exemplary embodiment of the present invention;
FIG. 6 is a graph showing the trend of the effect of leaching time on the leaching rate of molybdenum in a leachate in a method for recovering molybdenum from a spent catalyst according to an exemplary embodiment of the present invention;
FIG. 7 is a graph showing the tendency of the stirring intensity in the method for recovering molybdenum from a spent catalyst according to the exemplary embodiment of the present invention to affect the leaching rate of molybdenum from a leachate;
fig. 8 is a graph showing the tendency of the leaching rate of molybdenum in a leachate to the mass ratio of a roast product to distilled water in the method for recovering molybdenum from a spent catalyst according to an exemplary embodiment of the present invention.
Detailed Description
Example embodiments will now be described more fully with reference to the accompanying drawings. Example embodiments may, however, be embodied in many different forms and should not be construed as limited to the examples set forth herein; rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the concept of example embodiments to those skilled in the art. The described features, structures, or characteristics may be combined in any suitable manner in one or more embodiments.
Furthermore, the drawings are merely schematic illustrations of embodiments of the invention, which are not necessarily drawn to scale. The same reference numerals in the drawings denote the same or similar parts, and thus their repetitive description will be omitted. Some of the block diagrams shown in the figures are functional entities and do not necessarily correspond to physically or logically separate entities.
In this exemplary embodiment, a method for recovering molybdenum from a spent catalyst is first provided. Referring to fig. 1, the method for recovering molybdenum from the spent catalyst may include:
s101: respectively grinding the waste catalyst and sodium carbonate, and stirring and mixing the ground waste catalyst and the sodium carbonate;
s102: placing the mixed waste catalyst and sodium carbonate into a vacuum resistance furnace for roasting to obtain a roasted product, wherein the roasting temperature is 140-200 ℃;
s103: leaching the roasted product by using distilled water to obtain a mixture of leachate and leaching residues;
s104: and separating the mixture of the leaching solution and the leaching residue to obtain the leaching solution.
Specifically, in S101, the waste catalyst and sodium carbonate are respectively ground, and after being ground into powder, the powder is stirred and mixed to be uniformly mixed.
In S102, the uniformly mixed waste catalyst and sodium carbonate are put into a vacuum resistance furnace for roasting, because the waste catalyst contains alumina, the alumina can also react with the sodium carbonate, but the temperature at which the alumina can also react with the sodium carbonate spontaneously is about 690 ℃, and the temperature at which the molybdenum oxide in the waste curing agent can react with the sodium carbonate spontaneously is lower than that of the alumina, the roasting temperature is kept within the range of 140-200 ℃ under the vacuum condition, the molybdenum oxide can react with the sodium carbonate sufficiently, the leaching rate of molybdenum in the subsequent leaching process is higher, and the reaction of the alumina and the sodium carbonate can also be inhibited to a certain extent.
In S103, the waste catalyst and the sodium carbonate are put into a vacuum resistance furnace to be roasted to obtain a roasted product, and distilled water is used for leaching to obtain a mixture of leaching liquid and leaching slag, wherein the leaching liquid contains molybdenum, and the leaching slag contains other solid matters of the molybdenum element removed from the solidifying agent.
In S104, the leachate is separated from the leaching residue to obtain a leachate containing molybdenum ions.
According to the method for recovering molybdenum from the waste catalyst, on one hand, a vacuum technology is used, the process flow is simple, the process period is short, so that the process energy consumption is greatly reduced, on the other hand, additives in the process are relatively harmless, the molybdenum recovery rate is high, waste residue components generated after molybdenum recovery of the waste catalyst are not obviously damaged, the recovery of other subsequent ions cannot be influenced, secondary pollution cannot be caused, and the method is environment-friendly.
Next, each part of the above-described method for recovering molybdenum from the spent catalyst in the present exemplary embodiment will be described in more detail with reference to fig. 1.
In one embodiment, the waste catalyst and the sodium carbonate are ground separately until the particle size of the waste catalyst and the particle size of the sodium carbonate can be 50-200 meshes. Specifically, when the particle size of the waste catalyst and the sodium carbonate is within the parameter range, the contact area between the waste catalyst and the sodium carbonate after the waste catalyst and the sodium carbonate are mixed is large, so that molybdenum in the waste catalyst and the sodium carbonate can be fully reacted to a certain extent, and the recovery rate of the molybdenum is improved to a certain extent.
In one embodiment, the spent catalyst and sodium carbonate are separately ground until the particle size of the spent catalyst and sodium carbonate can be 200 mesh. Specifically, when the particle size of the waste catalyst and the particle size of the sodium carbonate are 200 meshes, the effect is best, the waste catalyst and the sodium carbonate can be fully contacted, so that molybdenum in the waste catalyst and the sodium carbonate react more fully, and the recovery rate of the molybdenum is further improved.
In one embodiment, when the ground waste catalyst is mixed with the sodium carbonate with stirring, the mass of the sodium carbonate may be 25% to 40% of the mass of the waste catalyst. Referring to fig. 3 specifically, the sodium carbonate is too low in quality, which may cause incomplete reaction of molybdenum in the curing agent, thereby reducing the extraction rate of molybdenum; if the quality of the sodium carbonate is too high, the sodium carbonate is easily surplus, so that the waste of materials is caused.
In one embodiment, when the ground spent catalyst is mixed with the sodium carbonate with stirring, the mass of the sodium carbonate may be 30% of the mass of the spent catalyst. Particularly, the mass of the sodium carbonate is preferably 30% of that of the waste catalyst, and at this ratio, the molybdenum in the waste catalyst reacts with the sodium carbonate more completely, and the waste of the sodium carbonate is greatly reduced.
In one embodiment, the mixed waste catalyst and sodium carbonate are placed into a vacuum resistance furnace for roasting to obtain a roasted product, wherein the roasting time can be 20-50 min. Specifically, within the time range, the molybdenum in the waste catalyst can completely react with the sodium carbonate.
In one embodiment, the mixed waste catalyst and sodium carbonate are placed into a vacuum resistance furnace to be roasted to obtain a roasted product, wherein the roasting time can be 30min, and the roasting temperature can be 160 ℃. Specifically, referring to fig. 2 and 4, the reaction condition of molybdenum and sodium carbonate in the roasting of the waste catalyst is better when the mixed waste catalyst and sodium carbonate are roasted at the roasting time and roasting temperature, so that the better leaching rate of molybdenum can be ensured, the resource is not wasted as much as possible, and the process time is reduced.
In one embodiment, when the roast product is leached with distilled water, the mass ratio of the roast product to the distilled water may be 1: 4-8, the leaching time can be 10-30 min, the leaching temperature can be 60-100 ℃, and the stirring intensity can be 200-500 rpm. Specifically, referring to fig. 5, 6, 7 and 8, when the roast is leached with distilled water, the leaching time, the leaching temperature, the stirring intensity and the ratio of the roast and the distilled water are within the above-mentioned parameter ranges, and the leaching rate for molybdenum ions is within a higher range.
In one embodiment, when the roasted product is leached by using distilled water, the mass ratio of the roasted product to the distilled water may be 1:6, the leaching time may be 20min, the leaching temperature may be 80 ℃, and the stirring intensity may be 300 rpm. Specifically, when the roasted product is leached by using distilled water, the leaching time, the leaching temperature, the stirring strength and the ratio of the roasted product to the distilled water are optimal, and under the process parameters, the leaching rate of molybdenum can be kept better, and the problems of resource waste or overlong process can be avoided to a certain extent.
In one embodiment, a suction filter or centrifuge may be used to separate the leachate from the leachate. Specifically, when the amount of the waste curing agent to be treated is large, the amount of the mixture of the leachate and the leaching slag is large after the leaching process, and the leachate and the leaching slag can be separated by using a suction filter; when the amount of the waste curing agent to be treated is small, the amount of the mixture of the leaching solution and the leaching slag is small after the leaching process, the leaching solution and the leaching slag can be separated by using a centrifugal machine, and when the leaching solution and the leaching slag can also be separated by using other equipment.
The first embodiment is as follows:
in this embodiment, vacuum condition calcination and non-vacuum condition calcination are respectively adopted to recover molybdenum from the spent GDS-30 catalyst, and the recovery steps are as follows:
s1011: respectively grinding the waste GDS-30 catalyst and sodium carbonate to 200 meshes, and uniformly stirring and mixing the ground waste catalyst and the sodium carbonate, wherein the mass of the sodium carbonate is 30% of that of the waste GDS-30 catalyst;
s1021: roasting the mixed waste GDS-30 catalyst and sodium carbonate to obtain a roasted product, wherein the roasting temperature is 160 ℃, and the roasting time is 30 min;
s1031: leaching the roasted product by using distilled water to obtain a mixture of leachate and leaching slag, wherein the mass ratio of the roasted product to the distilled water in the leaching process is 1:6, the leaching time is 20min, and the stirring intensity is 300 rpm;
s1041: and separating the mixture of the leachate and the leaching residues by using a pumping separator to obtain the leachate.
In the embodiment, the leaching solution obtained by recovering molybdenum in the waste GDS-30 catalyst by adopting vacuum condition roasting and non-vacuum condition roasting mainly comprises the following components:
| Al | Mo | Ni | Co | K | Fe | Cr | Na | |
| vacuum (ppm) | 13.007 | 85574.256 | 101.187 | 21.098 | 510.93 | 218.097 | 23.023 | 10830.021 |
| Non-vacuum (ppm) | 14.214 | 26894.040 | 83.359 | 17.087 | 356.562 | 188.419 | 19.617 | 28927.038 |
As can be seen from the above table, under the condition that other recovery steps are the same and parameters are the same, vacuum roasting and non-vacuum roasting are respectively adopted to treat the same amount of the waste GDS-30 catalyst, and the content of molybdenum in the leachate is far higher than that in the leachate under the non-vacuum state under the vacuum state, so that the vacuum state has a good effect on improving the molybdenum recovery rate in the molybdenum recovery process.
According to the method for recovering molybdenum from the waste catalyst, on one hand, a vacuum technology is used, the process flow is simple, the process period is short, so that the process energy consumption is greatly reduced, on the other hand, additives in the process are relatively harmless, the molybdenum recovery rate is high, waste residue components after molybdenum recovery of the waste catalyst are not obviously damaged, the recovery of other subsequent ions is not influenced, secondary pollution is not caused, and the method is environment-friendly.
It is to be understood that the terms "central," "longitudinal," "lateral," "length," "width," "thickness," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," "clockwise," "counterclockwise," and the like in the foregoing description are used for indicating or indicating the orientation or positional relationship illustrated in the drawings, and are used merely for convenience in describing embodiments of the present invention and for simplifying the description, and do not indicate or imply that the device or element so referred to must have a particular orientation, be constructed and operated in a particular orientation, and therefore should not be construed as limiting the embodiments of the present invention.
Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the embodiments of the present invention, "a plurality" means two or more unless specifically limited otherwise.
In the embodiments of the present invention, unless otherwise explicitly specified or limited, the terms "mounted," "connected," "fixed," and the like are to be construed broadly, e.g., as being fixedly connected, detachably connected, or integrated; can be mechanically or electrically connected; either directly or indirectly through intervening media, either internally or in any other relationship. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
In embodiments of the invention, unless expressly stated or limited otherwise, the first feature "on" or "under" the second feature may comprise the first and second features being in direct contact, or the first and second features being in contact, not directly, but via another feature therebetween. Also, the first feature being "on," "above" and "over" the second feature includes the first feature being directly on and obliquely above the second feature, or merely indicating that the first feature is at a higher level than the second feature. A first feature being "under," "below," and "beneath" a second feature includes the first feature being directly under and obliquely below the second feature, or simply meaning that the first feature is at a lesser elevation than the second feature.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples described in this specification can be combined and combined by those skilled in the art.
Other embodiments of the invention will be apparent to those skilled in the art from consideration of the specification and practice of the invention disclosed herein. This application is intended to cover any variations, uses, or adaptations of the invention following, in general, the principles of the invention and including such departures from the present disclosure as come within known or customary practice within the art to which the invention pertains. It is intended that the specification and examples be considered as exemplary only, with a true scope and spirit of the invention being indicated by the following claims.
Claims (10)
1. A method for recovering molybdenum from waste catalyst is characterized by comprising the following steps:
respectively grinding the waste catalyst and sodium carbonate, and stirring and mixing the ground waste catalyst and the sodium carbonate;
placing the mixed waste catalyst and sodium carbonate into a vacuum resistance furnace for roasting to obtain a roasted product, wherein the roasting temperature is 140-200 ℃;
leaching the roasted product by using distilled water to obtain a mixture of leachate and leaching residues;
and separating the mixture of the leaching solution and the leaching residue to obtain the leaching solution.
2. The molybdenum recovery method according to claim 1, wherein the waste catalyst and sodium carbonate are ground separately until the particle size of the waste catalyst and the particle size of the sodium carbonate are 50 to 200 mesh.
3. The molybdenum recovery method according to claim 2, wherein the spent catalyst and sodium carbonate are separately ground until the particle size of the spent catalyst and the sodium carbonate is 200 mesh.
4. The molybdenum recovery method according to claim 1, wherein when the ground spent catalyst and the sodium carbonate are mixed with stirring, the mass of the sodium carbonate is 25% to 40% of the mass of the spent catalyst.
5. The molybdenum recovery method according to claim 4, wherein when the ground spent catalyst and the sodium carbonate are mixed with stirring, the mass of the sodium carbonate is 30% of the mass of the spent catalyst.
6. The molybdenum recovery method according to claim 1, wherein the mixed waste catalyst and sodium carbonate are placed in a vacuum resistance furnace for roasting to obtain a roasted product, wherein the roasting time is 20-50 min.
7. The molybdenum recovery method according to claim 6, wherein the mixed spent catalyst and sodium carbonate are placed in a vacuum resistance furnace and roasted to obtain a roasted product, wherein the roasting time is 30min and the roasting temperature is 160 ℃.
8. The molybdenum recovery method according to claim 1, wherein when the roast product is leached with distilled water, the mass ratio of the roast product to the distilled water is 1: 4-8, the leaching time is 10-30 min, the leaching temperature is 60-100 ℃, and the stirring intensity is 200-500 rpm.
9. The molybdenum recovery method according to claim 8, wherein when the roast product is leached with distilled water, the mass ratio of the roast product to the distilled water is 1:6, the leaching time is 20min, the leaching temperature is 80 ℃, and the stirring intensity is 300 rpm.
10. A molybdenum recovery method according to any one of claims 1 to 9, wherein the leachate is separated from the leachate by a suction filter or a centrifuge.
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| 刘建周等: "《工业催化工程》", 中国矿业大学出版社有限责任公司 * |
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