CN113929143B - Method for extracting high-purity molybdenum oxide from low-grade molybdenite through microwave roasting separation - Google Patents
Method for extracting high-purity molybdenum oxide from low-grade molybdenite through microwave roasting separation Download PDFInfo
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Abstract
The invention discloses a method for microwave roasting, separating and extracting high-purity molybdenum oxide from low-grade molybdenite, belonging to the technical field of molybdenum metallurgy; the method comprises the following steps: crushing molybdenite, adding an alkaline solution and a glycerol aqueous solution for grinding, then adding silicon carbide and nickel chloride, roasting by microwave to obtain molybdenum trioxide steam, and then cooling; according to the invention, the alkaline solution and the glycerol aqueous solution are added in the grinding process, so that the molybdenum in the low-grade molybdenite can be promoted to dissolve out, and more molybdenum can participate in the oxidation reaction in the microwave roasting process, thereby improving the yield of the product molybdenum trioxide and improving the utilization rate of the molybdenum in the low-grade molybdenite; meanwhile, nickel chloride is added as a catalyst in the microwave roasting process, so that the oxidation temperature of molybdenum disulfide can be reduced, the reaction rate can be increased, the oxidation reaction can be completed at a lower temperature in a shorter time, and molybdenum trioxide is generated, thereby greatly reducing the energy consumption and shortening the production period.
Description
Technical Field
The invention belongs to the technical field of molybdenum metallurgy, and particularly relates to a method for extracting high-purity molybdenum oxide from low-grade molybdenite through microwave roasting separation.
Background
Molybdenum is distributed very little in nature, and the average content of molybdenum in the earth crust is only 0.001%, but molybdenum is a precious rare high-melting-point metal and is widely applied to the production of alloy steel, alloy cast iron, heat-resistant steel, stainless steel and the like. Molybdenum and its alloy have good physical and chemical properties, and become indispensable modern metals in industrial departments such as petroleum, chemical industry and steel.
Molybdenite is the most common and important mineral of the molybdenum supply in the world today, and is often produced in the contact zone of granite with limestone and in pegmatite gas deposits. Molybdenite is the most important mineral raw material for extracting molybdenum, and is treated by an oxidation roasting-ammonia leaching method which is widely adopted in the industry at present, but has the advantages of mature process, complex process, longer flow, high cost and great environmental pollution. The microwave roasting method can oxidize molybdenum disulfide into molybdenum trioxide, and the molybdenum trioxide is heated and sublimated to obtain a high-purity molybdenum trioxide product.
Although the molybdenum content of most molybdenite is 40-50%, the molybdenum content of some molybdenite is lower, the molybdenum content is below 20%, in the low-grade molybdenite, molybdenum is included and coated in other substance phases, and when molybdenum oxide is separated and extracted by adopting a microwave roasting method, because molybdenum disulfide is difficult to contact oxygen in a large area, the molybdenum trioxide generated by the reaction is less, and the extraction rate of molybdenum in minerals is lower. In order to obtain molybdenum trioxide products as much as possible, the thickness of the minerals is often controlled to be in millimeter level in the microwave roasting process, and the minerals are ground to be finer particles as much as possible, so that the microwave roasting method has small treatment capacity on low-grade molybdenite and the grinding process is complicated.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a method for extracting high-purity molybdenum oxide from low-grade molybdenite through microwave roasting separation.
In order to realize the purpose, the invention provides the following technical scheme:
the invention provides a method for extracting high-purity molybdenum oxide from low-grade molybdenite through microwave roasting separation, which comprises the following steps: crushing molybdenite, adding an alkaline solution and a glycerol aqueous solution for grinding, then adding silicon carbide and nickel chloride, roasting by microwave to obtain molybdenum trioxide steam, and then cooling.
Further, the alkaline solution is a sodium carbonate solution or a sodium hypochlorite solution, and the concentration is 10-15 wt%; the concentration of the glycerol aqueous solution is 20-30 wt%.
Furthermore, the mass-volume ratio of the molybdenite to the alkaline solution to the glycerin aqueous solution is (10-15) g to (2-3) mL to 1 mL.
Further, the grinding is carried out to 50-100 meshes.
Further, the operation of stirring for 30-50 min is carried out after grinding, so that molybdenum in the low-grade molybdenite can be fully dissolved out.
Further, the mass ratio of the nickel chloride to the molybdenite is 1: 15-20; the mass ratio of the silicon carbide to the molybdenite is 1: 8-10.
Adding silicon carbide as a strong wave absorbing substance to assist in heating low-grade molybdenite in the subsequent microwave roasting process.
Further, the thickness of the molybdenite during microwave roasting is 5-10 cm.
Further, the specific conditions of the microwave roasting are as follows: firstly, heating to 320-380 ℃, and preserving heat for 30-60 min; and then heating to 700-900 ℃, and preserving the heat for 30-40 min.
Further, compressed air is introduced during microwave roasting, and the introduction amount is 5-15 m 3 /h。
Compared with the prior art, the invention has the following beneficial effects:
the alkaline solution and the glycerol aqueous solution are added in the grinding process, so that the dissolution of molybdenum in the low-grade molybdenite can be promoted, more molybdenum can participate in the oxidation reaction in the microwave roasting process, the yield of the product molybdenum trioxide is increased, and the utilization rate of the molybdenum in the low-grade molybdenite is increased.
Meanwhile, nickel chloride is added as a catalyst in the microwave roasting process, so that the oxidation temperature of molybdenum disulfide can be reduced, the reaction rate can be increased, the oxidation reaction can be completed at a lower temperature in a shorter time, and molybdenum trioxide is generated, thereby greatly reducing the energy consumption and shortening the production period.
The method of the invention is simple and easy to operate, has short process flow and high product purity, and is suitable for popularization and application.
Detailed Description
Reference will now be made in detail to various exemplary embodiments of the invention, the detailed description should not be construed as limiting the invention but as a more detailed description of certain aspects, features and embodiments of the invention. It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
Further, for numerical ranges in this disclosure, it is understood that each intervening value, between the upper and lower limit of that range, is also specifically disclosed. Every smaller range between any stated value or intervening value in a stated range and any other stated or intervening value in a stated range is encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference herein for the purpose of disclosing and describing the methods and/or materials associated with the documents. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the present disclosure without departing from the scope or spirit of the disclosure. Other embodiments will be apparent to those skilled in the art from consideration of the specification. The description and examples are intended to be illustrative only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are open-ended terms that mean including, but not limited to.
The effective components and mass percentage of the low-grade molybdenite adopted in the following examples are as follows: 18.36% of molybdenum, 25.87% of sulfur, 1.32% of potassium oxide, 41.23% of silicon dioxide, 0.78% of copper, 0.21% of calcium oxide, 3.25% of iron, 0.01% of zinc, 0.45% of magnesium oxide, 0.09% of lead, 0.035% of phosphorus, 0.03% of tin, 7.61% of aluminum oxide, 0.01% of tungsten trioxide, 0.02% of bismuth and 0.38% of titanium dioxide; the particle size of the silicon carbide used in the following examples was 50 mesh.
The description will not be repeated below.
Example 1
The microwave roasting separation of low-grade molybdenite to extract high-purity molybdenum oxide includes the following steps:
(1) crushing low-grade molybdenite, adding a sodium carbonate solution with the concentration of 12 wt% and a glycerol aqueous solution with the concentration of 25 wt%, wherein the mass-volume ratio of the molybdenite to the sodium carbonate solution to the glycerol aqueous solution is 12 g: 2.5 mL: 1mL, performing ball milling until the granularity is 80 meshes, continuing stirring for 40min, then adding silicon carbide and nickel chloride, wherein the mass ratio of the nickel chloride to the molybdenite is 1: 18, the mass ratio of the silicon carbide to the molybdenite is 1: 9, uniformly stirring, then flatly paving the mixture until the thickness is 7cm, and placing the mixture in a microwave cavity;
(2) the microwave output switch is turned on according to the 10m 3 Blowing compressed air at a flow rate of/h, adjusting the microwave output power to 3kW, heating from room temperature to 350 ℃ at a speed of 50 ℃/min, and keeping the temperature for 45 min; and then heating to 800 ℃ at the speed of 50 ℃/min, preserving the temperature for 35min, overflowing the molybdenum trioxide steam from the top of the microwave reactor, cooling by water, and collecting by a cloth bag dust collector to obtain a high-purity molybdenum trioxide product.
The molybdenum trioxide product prepared in the example was tested to have a purity of 99.97 wt%.
Calculating theoretical yield of the molybdenum trioxide according to the content of molybdenum in the raw material (namely molybdenum in the raw material is oxidized to generate molybdenum trioxide and sublimed to obtain a molybdenum trioxide product), and calculating the yield of the molybdenum trioxide according to the actual yield of the molybdenum trioxide, wherein the calculation formula is as follows: the yield (%) of molybdenum trioxide was equal to the actual yield of molybdenum trioxide/theoretical yield of molybdenum trioxide × 100%, and the yield of molybdenum trioxide according to this example was calculated to be 97.8%.
Example 2
The microwave roasting separation and extraction of high-purity molybdenum oxide from low-grade molybdenite comprises the following steps:
(1) crushing low-grade molybdenite, adding a sodium hypochlorite solution with the concentration of 10 wt% and a glycerol aqueous solution with the concentration of 20 wt%, wherein the mass-volume ratio of the molybdenite to the sodium hypochlorite solution to the glycerol aqueous solution is 15 g: 3 mL: 1mL, performing ball milling until the granularity is 50 meshes, continuing stirring for 50min, then adding silicon carbide and nickel chloride, wherein the mass ratio of the nickel chloride to the molybdenite is 1: 15, the mass ratio of the silicon carbide to the molybdenite is 1: 8, uniformly stirring, then flatly paving the mixture until the thickness is 5cm, and placing the mixture in a microwave cavity;
(2) starting a microwave output switch according to the length of 5m 3 Blowing compressed air at a flow rate of/h, adjusting the microwave output power to 3kW, heating from room temperature to 380 ℃ at a speed of 50 ℃/min, and keeping the temperature for 30 min; heating to 700 deg.C at a rate of 50 deg.C/min, maintaining for 40min, and subjecting molybdenum trioxide steam to micro-heatingOverflowing from the top of the wave reactor, and collecting the molybdenum trioxide product with high purity through a bag dust collector after water cooling.
The molybdenum trioxide product prepared in the example was tested to have a purity of 99.96 wt% and a yield of 96.5%.
Example 3
The microwave roasting separation and extraction of high purity molybdenum oxide from low grade molybdenite includes the following steps:
(1) crushing low-grade molybdenite, adding a sodium carbonate solution with the concentration of 15 wt% and a glycerol aqueous solution with the concentration of 30 wt%, wherein the mass-volume ratio of the molybdenite to the sodium carbonate solution to the glycerol aqueous solution is 10 g: 2 mL: 1mL, performing ball milling until the granularity is 100 meshes, continuing stirring for 30min, then adding silicon carbide and nickel chloride, wherein the mass ratio of the nickel chloride to the molybdenite is 1: 20, the mass ratio of the silicon carbide to the molybdenite is 1: 10, uniformly stirring, then flatly paving the mixture until the thickness is 10cm, and placing the mixture in a microwave cavity;
(2) the microwave output switch is turned on according to 15m 3 Blowing compressed air at a flow rate of/h, adjusting the microwave output power to 3kW, heating from room temperature to 320 ℃ at a speed of 50 ℃/min, and keeping the temperature for 60 min; and then heating to 900 ℃ at the speed of 50 ℃/min, preserving the heat for 30min, overflowing the molybdenum trioxide steam from the top of the microwave reactor, cooling by water, and collecting by a cloth bag dust collector to obtain a high-purity molybdenum trioxide product.
The molybdenum trioxide product prepared by the embodiment is detected to have the purity of 99.94 wt% and the yield of 97.3%.
Example 4
The microwave roasting separation of low-grade molybdenite to extract high-purity molybdenum oxide includes the following steps:
(1) crushing low-grade molybdenite, adding a sodium carbonate solution with the concentration of 12 wt%, a glycerol aqueous solution with the concentration of 25 wt% and a surfactant of ammonium laureth sulfate, wherein the mass-volume ratio of the molybdenite to the ammonium laureth sulfate to the sodium carbonate solution to the glycerol aqueous solution is 12 g: 1 g: 2.5 mL: 1mL, performing ball milling until the granularity is 80 meshes, continuing stirring for 40min, then adding silicon carbide and nickel chloride, wherein the mass ratio of the nickel chloride to the molybdenite is 1: 18, the mass ratio of the silicon carbide to the molybdenite is 1: 9, uniformly stirring, then flatly paving until the thickness is 7cm, and placing the mixture in a microwave cavity;
(2) starting a microwave output switch according to the length of 10m 3 Blowing compressed air at a flow rate of/h, adjusting the microwave output power to 3kW, heating from room temperature to 350 ℃ at a speed of 50 ℃/min, and keeping the temperature for 45 min; and then heating to 800 ℃ at the speed of 50 ℃/min, preserving the temperature for 35min, overflowing the molybdenum trioxide steam from the top of the microwave reactor, cooling by water, and collecting by a cloth bag dust collector to obtain a high-purity molybdenum trioxide product.
The molybdenum trioxide product prepared by the embodiment is detected to have the purity of 99.97 wt% and the yield of 98.5%.
Comparative example 1
The microwave roasting separation of low-grade molybdenite to extract high-purity molybdenum oxide includes the following steps:
(1) crushing low-grade molybdenite, adding 25 wt% of glycerol aqueous solution, wherein the mass-volume ratio of the molybdenite to the glycerol aqueous solution is 12 g: 1mL, performing ball milling until the granularity is 80 meshes, continuing to stir for 40min, then adding silicon carbide and nickel chloride, wherein the mass ratio of the nickel chloride to the molybdenite is 1: 18, the mass ratio of the silicon carbide to the molybdenite is 1: 9, uniformly stirring, then flatly paving the mixture until the thickness is 7cm, and placing the mixture in a microwave cavity;
(2) starting a microwave output switch according to the length of 10m 3 Blowing compressed air at a flow rate of/h, adjusting the microwave output power to 3kW, heating from room temperature to 350 ℃ at a speed of 50 ℃/min, and keeping the temperature for 45 min; and then heating to 800 ℃ at the speed of 50 ℃/min, preserving the temperature for 35min, overflowing the molybdenum trioxide steam from the top of the microwave reactor, cooling by water, and collecting by a cloth bag dust collector to obtain a high-purity molybdenum trioxide product.
The molybdenum trioxide product prepared in the example was tested to have a purity of 99.93 wt% and a yield of 90.3%.
Comparative example 2
The microwave roasting separation of low-grade molybdenite to extract high-purity molybdenum oxide includes the following steps:
(1) crushing low-grade molybdenite, adding a sodium carbonate solution with the concentration of 12 wt%, wherein the mass volume ratio of the molybdenite to the sodium carbonate solution is 12 g: 2.5mL, performing ball milling until the granularity is 80 meshes, continuing to stir for 40min, then adding silicon carbide and nickel chloride, wherein the mass ratio of the nickel chloride to the molybdenite is 1: 18, the mass ratio of the silicon carbide to the molybdenite is 1: 9, uniformly stirring, then flatly paving the mixture to the thickness of 7cm, and placing the mixture in a microwave cavity;
(2) starting a microwave output switch according to the length of 10m 3 Blowing compressed air at a flow rate of/h, adjusting the microwave output power to 3kW, heating from room temperature to 350 ℃ at a speed of 50 ℃/min, and keeping the temperature for 45 min; and then heating to 800 ℃ at the speed of 50 ℃/min, preserving the temperature for 35min, overflowing the molybdenum trioxide steam from the top of the microwave reactor, cooling by water, and collecting by a cloth bag dust collector to obtain a high-purity molybdenum trioxide product.
The molybdenum trioxide product prepared in the example was tested to have a purity of 99.94 wt% and a yield of 88.9%.
Comparative example 3
The microwave roasting separation of low-grade molybdenite to extract high-purity molybdenum oxide includes the following steps:
(1) crushing low-grade molybdenite, adding a sodium carbonate solution with the concentration of 12 wt% and a glycerol aqueous solution with the concentration of 25 wt%, wherein the mass-volume ratio of the molybdenite to the sodium carbonate solution to the glycerol aqueous solution is 12 g: 2.5 mL: 1mL, ball-milling until the granularity is 80 meshes, continuing stirring for 40min, then adding silicon carbide, the mass ratio of the silicon carbide to the molybdenite is 1: 9, stirring uniformly, then flatly paving the mixture until the thickness is 7cm, and placing the mixture in a microwave cavity;
(2) starting a microwave output switch according to the length of 10m 3 Blowing compressed air at a flow rate of/h, adjusting the microwave output power to 3kW, heating from room temperature to 350 ℃ at a speed of 50 ℃/min, and keeping the temperature for 45 min; and then heating to 800 ℃ at the speed of 50 ℃/min, preserving the temperature for 35min, overflowing the molybdenum trioxide steam from the top of the microwave reactor, cooling by water, and collecting by a cloth bag dust collector to obtain a high-purity molybdenum trioxide product.
The molybdenum trioxide product prepared in this example was tested to have a purity of 99.95 wt% and a yield of 48.9%.
Comparative example 4
The microwave roasting separation of low-grade molybdenite to extract high-purity molybdenum oxide includes the following steps:
(1) crushing low-grade molybdenite, adding a sodium carbonate solution with the concentration of 12 wt% and a glycerol aqueous solution with the concentration of 25 wt%, wherein the mass-volume ratio of the molybdenite to the sodium carbonate solution to the glycerol aqueous solution is 12 g: 2.5 mL: 1mL, performing ball milling until the granularity is 80 meshes, continuing stirring for 40min, then adding silicon carbide and nickel chloride, wherein the mass ratio of the nickel chloride to the molybdenite is 1: 18, the mass ratio of the silicon carbide to the molybdenite is 1: 9, uniformly stirring, then flatly paving the mixture until the thickness is 7cm, and placing the mixture in a microwave cavity;
(2) starting a microwave output switch according to the length of 10m 3 Blowing compressed air at a flow rate of/h, adjusting the microwave output power to 3kW, heating to 800 ℃ from room temperature at a speed of 50 ℃/min, keeping the temperature for 80min, overflowing molybdenum trioxide steam from the top of the microwave reactor, cooling by water, and collecting by a cloth bag dust collector to obtain a high-purity molybdenum trioxide product.
The molybdenum trioxide product prepared in the example was tested to have a purity of 99.94 wt% and a yield of 92.1%.
Comparing the yields of molybdenum trioxide of example 1 and example 4, it can be seen that the addition of ammonium laureth sulfate as a surfactant during the milling process can improve the yield of molybdenum trioxide, since the addition of ammonium laureth sulfate further promotes the dissolution of molybdenum from the low-grade molybdenite and further increases the amount of molybdenum participating in the oxidation reaction; comparing the yields of molybdenum trioxide of example 1 and comparative examples 1-2, it can be seen that the yield of molybdenum trioxide is reduced when only alkaline solution or only glycerol aqueous solution is added during the grinding process, which indicates that the dissolution of molybdenum can be better promoted when alkaline solution and glycerol aqueous solution act together; comparing the yields of molybdenum trioxide of example 1 and comparative example 3, it can be seen that the yield of molybdenum trioxide is significantly reduced when no nickel chloride catalyst is added, since the oxidation temperature of molybdenum disulfide is higher when no nickel chloride catalyst is added, and the reaction temperature of comparative example 3 is lower, thus less molybdenum trioxide is produced; comparing the yields of molybdenum trioxide of example 1 and comparative example 4, it can be seen that when the system is directly heated to the sublimation temperature of molybdenum trioxide, the same heating time results in a reduction in the yield of molybdenum trioxide, since the higher temperature adversely inhibits the oxidation of molybdenum disulfide and thus reduces the yield of molybdenum trioxide.
The above description is only for the preferred embodiment of the present invention, and the protection scope of the present invention is not limited thereto, and any person skilled in the art should be able to cover the technical scope of the present invention, the technical solution and the inventive concept of the present invention equivalent or change within the technical scope of the present invention.
Claims (5)
1. The method for extracting high-purity molybdenum oxide from low-grade molybdenite through microwave roasting separation is characterized by comprising the following steps of: crushing molybdenite, adding an alkaline solution and a glycerol aqueous solution for grinding, then adding silicon carbide and nickel chloride, roasting by microwave to obtain molybdenum trioxide steam, and then cooling;
the alkaline solution is a sodium carbonate solution or a sodium hypochlorite solution, and the concentration of the alkaline solution is 10-15 wt%; the concentration of the glycerol aqueous solution is 20-30 wt%;
the mass-volume ratio of the molybdenite to the alkaline solution to the glycerin aqueous solution is (10-15) g to (2-3) mL to 1 mL;
the mass ratio of the nickel chloride to the molybdenite is 1: 15-20; the mass ratio of the silicon carbide to the molybdenite is 1: 8-10;
the specific conditions of the microwave roasting are as follows: firstly, heating to 320-380 ℃, and preserving heat for 30-60 min; and then heating to 700-900 ℃, and preserving the heat for 30-40 min.
2. The method for microwave roasting, separating and extracting high-purity molybdenum oxide from low-grade molybdenite according to claim 1, wherein the low-grade molybdenite is ground to 50-100 meshes.
3. The method for microwave roasting, separating and extracting high-purity molybdenum oxide from low-grade molybdenite according to claim 1, wherein the operation of stirring for 30-50 min is further included after grinding.
4. The method for separating and extracting high-purity molybdenum oxide from low-grade molybdenite through microwave roasting according to claim 1, wherein the thickness of the molybdenite during microwave roasting is 5-10 cm.
5. The method for microwave roasting, separating and extracting high-purity molybdenum oxide from low-grade molybdenite according to claim 1, wherein compressed air is introduced during microwave roasting, and the introduction amount is 5-15 m 3 /h。
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