CN103318961B - Preparation method of high-purity molybdenum disulfide - Google Patents
Preparation method of high-purity molybdenum disulfide Download PDFInfo
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- CN103318961B CN103318961B CN201310283123.6A CN201310283123A CN103318961B CN 103318961 B CN103318961 B CN 103318961B CN 201310283123 A CN201310283123 A CN 201310283123A CN 103318961 B CN103318961 B CN 103318961B
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Abstract
The invention discloses a preparation method of high-purity molybdenum disulfide. The preparation method comprises the following steps of: 1, sieving a molybdenum concentrate, adding water to screen underflow for blending, and then placing the mixture in a ceramic box or a quartz crucible so as to press the mixture into molybdenum concentrate wet cakes; 2, placing the ceramic box or the quartz crucible containing the molybdenum concentrate wet cakes in a microwave muffle surface, and carrying out microwave treatment under the nitrogen protection; 3, adding water to the molybdenum concentrate wet cakes subjected to the microwave treatment so as to pound the wet cakes to pieces, thus obtaining paste, carrying out superconductive magnetic separation treatment on the paste, and then filtering to obtain filter cakes; and 4, carrying out acid leaching on the filter cakes, then filtering, washing, drying and smashing the filtered filter cakes to obtain the molybdenum disulfide. According to the preparation method, the molybdenum concentrate is refined by removing out-of-phase dirt in the molybdenum concentrate through microwave treatment and superconducting magnetic separation, and finally, the high-purity molybdenum disulfide with the purity no less than 99.3% is obtained through acid leaching, thus the product quality is substantially improved.
Description
Technical field
The invention belongs to molybdenumdisulphide lubricant preparing technical field, be specifically related to a kind of preparation method of high-purity molybdenumdisulphide.
Background technology
Molybdenumdisulphide, is commonly called as the king of solid lubrication.There is the characteristics such as high temperature resistant, vacuum-resistant, anti-extreme pressure, diamagneticization, wear-resisting, corrosion-resistant, stable chemical performance, be widely used in Aeronautics and Astronautics and work, agriculture, industry, military project power lubrication, material and the field such as prepare.
Method for preparing molybdenum disulfide is divided into two kinds, i.e. natural method and synthesis method.Natural legal system is generally to take molybdenum glance ore as raw material for high-purity molybdenumdisulphide, and through ore grinding, flotation obtains concentrated molybdenum ore, through processes such as Chemical Leachings, isolates the molybdenumdisulphide of lubricated level, MoS again
2content is generally in 98%~99% left and right.Because not destroying the structure construction of molybdenumdisulphide in its whole purification process, natural brightness molybdenum six side's laminated structure crystal formation crystallographic systems have been remained.In concentrated molybdenum ore, molybdenumdisulphide content is generally 80%~94%, and other impurity is mainly the silicate mineralss such as the sulfide minerals such as sulphide ores, pyrite, cupric sulfide, lead glance, chalcopyrite and feldspar, mica, chlorite.While producing molybdenumdisulphide, concentrated molybdenum ore impurity elimination, main method has that hydrochloric acid oxidizer leaches, hydrochloric acid (sulfuric acid) adds hydrofluoric acid leachings, villaumite leaching etc., for improve leaching effect conventionally minutes two sections, three sections nitration mixture leach or two sections, three sections acidleach under auxiliary or hydrochlorate leaching in microwave or ultrasonic wave.
Chemical synthesis is by ammonium molybdate solution sulfuration, is converted into ammonium thiomolybdate; Then acidifying, obtains molybdenum trisulfide precipitation, and pyrolysis desulfurization, pulverizing, obtain molybdenumdisulphide finished product.Synthetic molybdenumdisulphide Crystal Structure belongs to synthetic, and lubricity is not as natural molybdenumdisulphide.Other method is as (1) calcium molybdate, sulphur, sodium carbonate reaction; (2) molybdenum and sulphur combination reaction; (3) molybdic oxide, sulphur, salt of wormwood pyroreaction; (4) Sodium orthomolybdate, thiocarbamide reaction etc.
In recent years, along with scientific and technical fast development, molybdenumdisulphide application is more and more extensive, but also in continuous expansion, the segmentation in market has brought client to propose requirements at the higher level to molybdenumdisulphide quality.Need the molybdenumdisulphide that purity is higher, make a general survey of the natural method production technique of domestic and international molybdenumdisulphide, except remove silicon-dioxide hydrofluoric acid indispensable, the acid of concentrated molybdenum ore nothing more than, one section, two sections of salinities or three sections of leachings.Or one section, two sections of acid, salinities or three sections of leachings under microwave, ultrasonic wave are assisted.Although some technique is progressive to some extent.But it is comparatively outstanding that the repeatedly acidleach exposing causes contaminated wastewater and synthesis method production molybdenumdisulphide technique to expose waste gas, waste water pollution problem.Bibliographical information, U.S. Climax company is this drawback for a change once, by concentrated molybdenum ore under nitrogen protection, in the rotary kiln of 650 ℃, by calcining molybdenum ore concentrate 2~5 hours, although concentrated molybdenum ore impurity pyrite transition.But also there is change in the molybdenumdisulphide continuous high temperature character in concentrated molybdenum ore, this technique also fails to be widely applied.Therefore be badly in need of seeking a kind of new technique, can significantly promote molybdenumdisulphide quality, and can reduce the pollution in molybdenumdisulphide production process.
Summary of the invention
Technical problem to be solved by this invention is for above-mentioned the deficiencies in the prior art, provides a kind of method unique, simple to operate, has the preparation method of high-purity molybdenumdisulphide of the advantage such as efficient, energy-conservation.The method.The method is removed the out-phase dirt in concentrated molybdenum ore by microwave treatment and superconducting magnetic separating treatment, has refined concentrated molybdenum ore, finally by acidleach, can obtain quality product purity and be not less than high-purity molybdenumdisulphide of 99.3%, has significantly promoted product quality.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of preparation method of high-purity molybdenumdisulphide, it is characterized in that, and the method comprises the following steps:
Step 1, the concentrated molybdenum ore after adopting screen cloth that aperture is 2.00mm to fragmentation sieve, to adding in the screen underflow after sieving 8%~12% deionized water of screen underflow quality to be in harmonious proportion, then the screen underflow after being in harmonious proportion is placed in ceramic box body or quartz crucible, is pressed into the wet cake of concentrated molybdenum ore;
Step 2, the ceramic box body or the quartz crucible that in step 1, are contained with the wet cake of concentrated molybdenum ore are placed in to microwave Muffle furnace, microwave treatment 50s~150s under nitrogen protection;
Step 3, the wet cake of the concentrated molybdenum ore after microwave treatment in step 2 is added to water smash to pieces, obtain solid masses content and be 25%~30% slurry, described slurry is carried out to superconducting magnetic separating treatment, then the slurry after superconducting magnetic separating treatment is filtered, obtain filter cake;
Step 4, filter cake described in step 3 is carried out to acidleach, then filter, the filter cake after filtering is washed, dry, pulverize, obtain quality purity and be not less than 99.3% molybdenumdisulphide.
The preparation method of above-mentioned a kind of high-purity molybdenumdisulphide, described in step 1, in concentrated molybdenum ore, the quality percentage composition of molybdenum is not less than 54%.
The preparation method of above-mentioned a kind of high-purity molybdenumdisulphide, the electrical conductivity of water of deionization described in step 1 is not more than 0.6 μ S/cm.
The preparation method of above-mentioned a kind of high-purity molybdenumdisulphide, the quality purity of nitrogen described in step 2 is not less than 99%.
The preparation method of above-mentioned a kind of high-purity molybdenumdisulphide, the frequency of microwave treatment described in step 2 is 2450MHz, power is 800W~2000W.
The preparation method of above-mentioned a kind of high-purity molybdenumdisulphide, the magneticstrength of the separation of superconducting magnetic described in step 3 is not less than 30 kilogausss.
The preparation method of above-mentioned a kind of high-purity molybdenumdisulphide, the pickling liquor that acidleach described in step 4 adopts is the mixing solutions of hydrofluoric acid, water and hydrochloric acid, the mass concentration that in mixing solutions, the mass concentration of HF is 11%~16%, HCl is 2%~4%.
The preparation method of above-mentioned a kind of high-purity molybdenumdisulphide, the temperature of acidleach described in step 4 is 60 ℃~85 ℃, the time is 5h~6h.
The present invention compared with prior art has the following advantages:
1, the present invention leaches with traditional two steps and synthesis method purification and ultrasonic wave or microwave-assisted two sections, three sections leach to purify and compare, by the out-phase dirt in microwave treatment removal separated with superconducting magnetic concentrated molybdenum ore, refined concentrated molybdenum ore, finally by acidleach, can obtain quality product purity and be not less than high-purity molybdenumdisulphide of 99.3%, significantly promote product quality.
2, the present invention adopts and concentrated molybdenum ore is carried out in filling the microwave Muffle furnace of nitrogen to microwave treatment; because the time is short, only there are 50~150 seconds; in the whole process of concentrated molybdenum ore, temperature is the highest not over 150 ℃; and omnidistance by nitrogen protection; there is not any change in the structure of molybdenumdisulphide and character; whole microwave power is only 2000W, not only energy-conservation, and efficiency is high.
3, the present invention adopts superconducting magnetic separator, and magnetic current intensity reaches as high as 55 kilogausss, has greatly improved the magnetic in concentrated molybdenum ore or weak magnetic mineral as the removal of magnetic pyrite, mica, meteoric iron etc.Owing to adopting, superconductor technology energy consumption is low, is only 1/30 of traditional impurity elimination, and running cost is very low.
4, the inventive method is unique, simple to operate, has the advantages such as efficient, energy-conservation.
Below by embodiment, technical scheme of the present invention is described in further detail.
Embodiment
Embodiment 1
Step 1, the concentrated molybdenum ore that adopts screen cloth that aperture is 2.00mm the quality percentage composition of molybdenum to be not less than after 54% fragmentation sieve, to adding in the screen underflow after sieving 12% deionized water of screen underflow quality to be in harmonious proportion, then the screen underflow after being in harmonious proportion is placed in ceramic box body (or quartz crucible), is pressed into the wet cake of concentrated molybdenum ore; Described deionization electrical conductivity of water is 0.6 μ S/cm;
Step 2, the ceramic box body (or quartz crucible) that is contained with the wet cake of concentrated molybdenum ore in step 1 is placed in to microwave Muffle furnace, under nitrogen protection, frequency is 2450MHz, microwave treatment 50s under the condition that power is 2000W; The quality purity of described nitrogen is not less than 99%;
Step 3, the wet cake of the concentrated molybdenum ore after microwave treatment in step 2 is added to water smash to pieces, obtain solid masses content and be 25% slurry, the superconducting magnetic separator (for example Weifang zero volatilization 5.5T low-temperature superconducting magnetic separator, Britain MK4 type superconducting magnetic separator, the reciprocal tandem tank type superconducting magnetic separator of German DEsCOS cartridge type superconducting magnetic separator or Czech) that adopts magneticstrength to be not less than 30 kilogausss carries out superconducting magnetic separating treatment to described slurry, remove the magnetic mineral impurity in slurry, then filter, obtain filter cake;
Step 4, filter cake described in step 3 is added and in pickling liquor, carries out acidleach, then filter, the filter cake after filtering is washed, dry, pulverize, obtain quality purity and be 99.3% molybdenumdisulphide; Described pickling liquor is the mixing solutions of hydrofluoric acid, water and hydrochloric acid, and the mass concentration that in mixing solutions, the mass concentration of HF is 13.5%, HCl is 3%.
Embodiment 2
Step 1, the concentrated molybdenum ore that adopts screen cloth that aperture is 2.00mm the quality percentage composition of molybdenum to be not less than after 54% fragmentation sieve, to adding in the screen underflow after sieving 8% deionized water of screen underflow quality to be in harmonious proportion, then the screen underflow after being in harmonious proportion is placed in quartz crucible (or ceramic box body), is pressed into the wet cake of concentrated molybdenum ore; Described deionization electrical conductivity of water is 0.5 μ S/cm;
Step 2, by being contained with the quartz crucible (or ceramic box body) of the wet cake of concentrated molybdenum ore in step 1, be placed in microwave Muffle furnace, under nitrogen protection, frequency is 2450MHz, microwave treatment 100s under the condition that power is 1500W; The quality purity of described nitrogen is not less than 99%;
Step 3, the wet cake of the concentrated molybdenum ore after microwave treatment in step 2 is added to water smash to pieces, obtain solid masses content and be 28% slurry, the superconducting magnetic separator (for example Weifang zero volatilization 5.5T low-temperature superconducting magnetic separator, Britain MK4 type superconducting magnetic separator, the reciprocal tandem tank type superconducting magnetic separator of German DEsCOS cartridge type superconducting magnetic separator or Czech) that adopts magneticstrength to be not less than 30 kilogausss carries out superconducting magnetic separating treatment to described slurry, remove the magnetic mineral impurity in slurry, then filter, obtain filter cake;
Step 4, filter cake described in step 3 is added and in pickling liquor, carries out acidleach, then filter, the filter cake after filtering is washed, dry, pulverize, obtain quality purity and be 99.51% molybdenumdisulphide; Described pickling liquor is the mixing solutions of hydrofluoric acid, water and hydrochloric acid, and the mass concentration that in mixing solutions, the mass concentration of HF is 11%, HCl is 4%.
Embodiment 3
Step 1, the concentrated molybdenum ore that adopts screen cloth that aperture is 2.00mm the quality percentage composition of molybdenum to be not less than after 54% fragmentation sieve, to adding in the screen underflow after sieving 10% deionized water of screen underflow quality to be in harmonious proportion, then the screen underflow after being in harmonious proportion is placed in ceramic box body (or quartz crucible), is pressed into the wet cake of concentrated molybdenum ore; Described deionization electrical conductivity of water is 0.2 μ S/cm;
Step 2, by being contained with the ceramic box body (or quartz crucible) of the wet cake of concentrated molybdenum ore in step 1, be placed in microwave Muffle furnace, under nitrogen protection, frequency is 2450MHz, microwave treatment 150s under the condition that power is 800W; The quality purity of described nitrogen is not less than 99%;
Step 3, the wet cake of the concentrated molybdenum ore after microwave treatment in step 2 is added to water smash to pieces, obtain solid masses content and be 30% slurry, the superconducting magnetic separator (for example Weifang zero volatilization 5.5T low-temperature superconducting magnetic separator, Britain MK4 type superconducting magnetic separator, the reciprocal tandem tank type superconducting magnetic separator of German DEsCOS cartridge type superconducting magnetic separator or Czech) that adopts magneticstrength to be not less than 30 kilogausss carries out superconducting magnetic separating treatment to described slurry, remove the magnetic mineral impurity in slurry, then filter, obtain filter cake;
Step 4, filter cake described in step 3 is added and in pickling liquor, carries out acidleach, then filter, the filter cake after filtering is washed, dry, pulverize, obtain quality purity and be 99.62% molybdenumdisulphide; Described pickling liquor is the mixing solutions of hydrofluoric acid, water and hydrochloric acid, and the mass concentration that in mixing solutions, the mass concentration of HF is 16%, HCl is 2%.
Comparative example 1
Screen underflow after sieving in embodiment 1 is directly carried out to acidleach (acidleach process is identical with embodiment 1), then filter, the filter cake after filtering is washed, dry, pulverize, obtain quality purity and be 97.6% molybdenumdisulphide.
Comparative example 2
To directly carrying out acidleach (acidleach process is identical with embodiment 1) after the wet cake fragmentation of the concentrated molybdenum ore after microwave treatment in embodiment 1, then filter, the filter cake after filtering is washed, to dry, pulverizing, obtains quality purity and is 98.8% molybdenumdisulphide.
Comparative example 3
It is 25% slurry that screen underflow after sieving in embodiment 1 is tempered into solid masses content, and the superconducting magnetic separator that then adopts magneticstrength to be not less than 30 kilogausss carries out superconducting magnetic separation to slurry, filters, and obtains filter cake; Again filter cake is carried out to acidleach (acidleach process is identical with embodiment 1), then filter, the filter cake after filtering is washed, dry, pulverize, obtain quality purity and be 98.4% molybdenumdisulphide.
By the contrast of embodiment 1,2,3 and comparative example 1,2,3, can obviously find out, the present invention, by microwave treatment, superconducting magnetic separation and acidleach combination, can obviously improve the purity of molybdenumdisulphide, and the quality purity of the molybdenumdisulphide of preparation is not less than 99.3%.
The above; it is only preferred embodiment of the present invention; not the present invention is done to any restriction, every any simple modification of above embodiment being done according to invention technical spirit, change and equivalent structure change, and all still belong in the protection domain of technical solution of the present invention.
Claims (8)
1. a preparation method for high-purity molybdenumdisulphide, is characterized in that, the method comprises the following steps:
Step 1, the concentrated molybdenum ore after adopting screen cloth that aperture is 2.00mm to fragmentation sieve, to adding in the screen underflow after sieving 8%~12% deionized water of screen underflow quality to be in harmonious proportion, then the screen underflow after being in harmonious proportion is placed in ceramic box body or quartz crucible, is pressed into the wet cake of concentrated molybdenum ore;
Step 2, the ceramic box body or the quartz crucible that in step 1, are contained with the wet cake of concentrated molybdenum ore are placed in to microwave Muffle furnace, microwave treatment 50s~150s under nitrogen protection;
Step 3, the wet cake of the concentrated molybdenum ore after microwave treatment in step 2 is added to water smash to pieces, obtain solid masses content and be 25%~30% slurry, described slurry is carried out to superconducting magnetic separating treatment, then the slurry after superconducting magnetic separating treatment is filtered, obtain filter cake;
Step 4, filter cake described in step 3 is carried out to acidleach, then filter, the filter cake after filtering is washed, dry, pulverize, obtain quality purity and be not less than 99.3% molybdenumdisulphide.
2. the preparation method of a kind of high-purity molybdenumdisulphide according to claim 1, is characterized in that, described in step 1, in concentrated molybdenum ore, the quality percentage composition of molybdenum is not less than 54%.
3. the preparation method of a kind of high-purity molybdenumdisulphide according to claim 1, is characterized in that, the electrical conductivity of water of deionization described in step 1 is not more than 0.6 μ S/cm.
4. the preparation method of a kind of high-purity molybdenumdisulphide according to claim 1, is characterized in that, the quality purity of nitrogen described in step 2 is not less than 99%.
5. the preparation method of a kind of high-purity molybdenumdisulphide according to claim 1, is characterized in that, the frequency of microwave treatment described in step 2 is 2450MHz, and power is 800W~2000W.
6. the preparation method of a kind of high-purity molybdenumdisulphide according to claim 1, is characterized in that, the magneticstrength of the separation of superconducting magnetic described in step 3 is not less than 30 kilogausss.
7. the preparation method of a kind of high-purity molybdenumdisulphide according to claim 1, it is characterized in that, the pickling liquor that acidleach described in step 4 adopts is the mixing solutions of hydrofluoric acid, water and hydrochloric acid, and the mass concentration that in mixing solutions, the mass concentration of HF is 11%~16%, HCl is 2%~4%.
8. the preparation method of a kind of high-purity molybdenumdisulphide according to claim 1, is characterized in that, the temperature of acidleach described in step 4 is 60 ℃~85 ℃, and the time is 5h~6h.
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CN103667676B (en) * | 2013-12-31 | 2016-04-20 | 金堆城钼业股份有限公司 | The method of a kind of microwave-acidleach recombining process purifying molybdenum concentrate |
JP6401080B2 (en) * | 2015-03-06 | 2018-10-03 | 国立大学法人九州大学 | Beneficiation method |
JP6401081B2 (en) * | 2015-03-06 | 2018-10-03 | 国立大学法人九州大学 | Beneficiation method |
CN106011454A (en) * | 2016-07-04 | 2016-10-12 | 西安建筑科技大学 | Method for activating molybdenum concentrate |
CN110436525B (en) * | 2019-07-22 | 2021-09-28 | 金堆城钼业股份有限公司 | Preparation method of micro/nano molybdenum disulfide |
CN110357162B (en) * | 2019-07-22 | 2021-11-09 | 金堆城钼业股份有限公司 | Method for efficiently synthesizing high-purity molybdenum disulfide |
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