Device for the production of high-purity nano-molybdenum trioxide
Patent Information
- Authority / Receiving Office
- DE · DE
- Patent Type
- Patents
- Current Assignee / Owner
- HUBEI ZHONGAO NANO MATERIAL TECH CO LTD
- Filing Date
- 2016-12-02
- Publication Date
- 2026-07-09
Abstract
Description
TECHNICAL AREA
[0001] The invention relates to a device and a method for producing high-purity nano-molybdenum trioxide. STATE OF THE ART
[0002] In general, the industrial production of molybdenum trioxide is carried out by calcining ammonium molybdate or chemically leaching the molybdenum concentrate with acid or base at high pressure and added oxygen in order to separate the molybdates from the impurities and to obtain high-purity molybdenum trioxide after decomposition. With the steady development of material science and application technology, the problems of molybdenum trioxide obtained by the above methods, e.g. B. the coarse particles in the form of aggregate and the low purity of the molybdenum trioxide, always stand out. Highly active molybdenum trioxide can be used in the field of catalysts, which not only places specific demands on the impurities and particle size distribution, but also places special demands on the reactive properties of the molybdenum trioxide in the solution.
[0003] US4551313 discloses a process for the rapid sublimation of molybdenum trioxide from a slag (of silicon, aluminum and heavy metals), but this only involves separating molybdenum trioxide from impurities and increasing the purity of molybdenum trioxide at a particle size above microns.
[0004] In US6468497 a method for the production of nano-molybdenum trioxide is published, in which it is essential that molybdenum trioxide is rapidly cooled (48° C.) with liquid nitrogen in order to strip-shaped nano-molybdenum trioxide with a length of approx. 80-90 nm and a diameter of approx. 20 - 30 nm.
[0005] With the above methods, of course, it is possible to produce nano-molybdenum trioxide, but there are the following problems: high manufacturing cost, difficult to spread to massive industrial applications, and an acicular product that meets the requirement of special wear-resistant materials in the special field e.g. B. the high-quality lubricants, in which spherical particles of nano-molybdenum trioxide are required, can not meet. Therefore, it is particularly important to achieve an apparatus and a method for the automated and continuous production of the nano molybdenum trioxide with a simple technical process, high safety and low cost. CONTENT OF THE PRESENT INVENTION
[0006] The invention provides an apparatus for producing high-purity nano-molybdenum trioxide, in which nano-molybdenum trioxide can be obtained by sublimating molybdenum trioxide with pollution-free and high-efficiency recovery.
[0007] The task is solved by the technical solution of the present invention:
[0008] An apparatus for the production of high-purity nano-molybdenum trioxide, which comprises a raw material silo 1, a material feed 2, a furnace for sublimation 7, a first ventilation pipe 24, a second ventilation pipe 25, a spray device 23 and a filter arrangement 12, the raw material silo 1 with the Material feeder 2 is connected, the material feeder 2 is connected to the bottom of the sublimating furnace 7, the sublimating furnace 7 is connected at its top to the horizontally arranged first ventilation pipe 24, one end of the first ventilation pipe 24 to the vertically arranged second ventilation pipe 25 is connected, and the second ventilation pipe 25 is connected to a recovery device 13; a product silo 11 is provided below the recovery apparatus 13; the filter assembly 12 is provided at the junction of the recovery apparatus 13 with the second ventilation pipe 25; the sprayer 23 is provided at the junction between the first aeration pipe 24 and the second aeration pipe 25; wherein the spray device 23 is connected to a dispersant connection 21 and a compressed air connection 22; the spray direction of the spray device 23 being coaxial with the axis of the second aeration tube 25; and a clean air inlet 10 is provided on the first ventilation pipe 24 .
[0009] Furthermore, an agitator 20 is arranged horizontally in the first aeration pipe 24, one end of the agitator 20 is connected to a rotary motor 18, and the rotary motor 18 is mounted on a drive shaft of a displacement motor 19 so that the displacement motor 19 rotates the rotary motor 18 in the linear direction of the first ventilation pipe 24 shifts back and forth.
[0010] Furthermore, a pipe of the recovery apparatus 13 is connected to a water spray pump 15 at one end and extends into the filter assembly 12 at the other end. The water spray pump 15 is connected to a deionized water pool 16 which is connected to the water spray pump 15 through a circuit. A circulation pump 17 is provided in the circuit.
[0011] Furthermore, a first valve 26 is provided in the pipe between the recovery device 13 and the water spray pump 15, a compressed air port 14 is provided between the first valve 26 and the recovery device 13, and the compressed air port 14 is formed with a second valve 27.
[0012] Further, the filter assembly 12 comprises a seal comprising a sealed, hollow, metal-blocking foil 2 encased by a layer of temperature-resistant filter cloth 1, with nano-molybdenum trioxide in the intermediate layer between the metal-blocking foil 2 and the temperature-resistant filter cloth 1 3 is inserted, and the interior of the metal-blocking foil 2 is connected to the compressed air connection 14 with the second valve 27 by a pipe.
[0013] Further, the bottom 6 of the furnace for sublimation 7 is formed obliquely, with the end at the junction with the material feeder 2 being higher, and a liquid drain 8 being provided at the lower end of the bottom 6. FIG.
[0014] Furthermore, a compressed air connection 9 is provided on one side under the sublimation oven 7 .
[0015] Furthermore, an observation port 3 is provided on a side wall of the sublimation furnace 7, and the observation port 3 is at the same level of the first ventilation pipe 24.
[0016] Also provided is a method for producing high-purity nano-molybdenum trioxide, in which pure molybdenum trioxide is used as a raw material, which is fed through a material feed (2) to a sublimation furnace (7) and stored in the sublimation furnace (7) at a controlled temperature is sublimated from 1100 - 1600°C; after starting a displacement engine (19) and a rotary engine (18), clean air at 10 - 18°C with a proportion of water less than 30% is introduced from a clean air inlet (10); and while maintaining a temperature in a first ventilation pipe (24) of 75 - 85°C, a spray device (23) is switched on to spray a mist with dispersing agent, whereby the raw material is sprayed into a recovery device, filtered and collected, while the air after the raw material has been filtered off in a filter, it is introduced into a pool for deionized water (16). Furthermore, compressed air with a water content of less than 30% is introduced from a compressed air connection 9 at the bottom of the sublimation furnace 7 to replenish the air and thereby increase the amount of molybdenum trioxide sublimated, the air having a temperature of 15 - 18°C, humidity 28% - 35% and pressure 0.75 - 0.8MPa.
[0017] The nano-molybdenum trioxide obtained in this way is spherical, with a particle size ≤ 100 nm, a sphericity of ≥ 0.92 and a specific surface area ≥ 40 m2 / g.
[0018] The term molybdenum trioxide means high-purity molybdenum trioxide with a total content of impurities ≤ 0.02% (weight), produced by the thermal decomposition of molybdic acid and ammonium molybdate, the oxidation of pure molybdenum powder or other method.
[0019] The invention has the following advantageous aspects: 1) The oven for sublimation can be operated safely. The furnace for sublimation in the invention uses a common sheet iron as a casing, preferably a fireproof brick as an inner lining, a U-shaped silicon-molybdenum rod as a heating element. The temperature control is carried out by a computer, which can run continuously for over 2000 hours. The elements that need to be repaired should be actively exchanged on a regular basis. The bottom pool of molybdenum trioxide should be drained once a year. When the shutdown is planned, the power supply for heating should be turned off, and then the liquid drain 8 should be opened to drain the liquid molybdenum trioxide, which contains impurities with a high melting point or a high density, to cool in a sand box, and as an alloy of molybdenum and iron drive out. Due to the obviously sensible design and training, the heating furnace is better than all previously recognized structures of the heating furnace. Although the heating furnace has the disadvantage that the general tightness is not ideal, the disadvantage here is overcome by the sublimation at the negative pressure. 2) The rotation motor and the translation motor are variable in frequency. The operating elements are driven by the motors in such a way that the cooling air mixes with the molybdenum trioxide gas (with a small amount of air) as quickly as possible in order to achieve the purpose of rapid cooling and thus enable the molybdenum trioxide powder to be crushed to nanoscale. 3) The components for blocking the recovered product are divided into several groups, and for each group clocked a vacuum valve is closed and a flushing air valve is opened for flushing. A manual-automatic lock is provided, which in the case of automatic control is controlled with a pulse control. Alternatively, the groups are used to rinse the recovered product. 4) A dispersant is added at a low temperature section in the process. The dispersing agent can achieve the effects of even division and prevention from agglomerate. 5) A vacuum unit for spraying deionized water is provided. The amount of air sucked in by the unit ensures the complete transfer of the sublimed molybdenum trioxide, adding the cooling air and meeting the material handling requirement for the entire system. In addition, the nano-molybdenum trioxide slightly leaked from the blocking unit is recovered by recovering the molybdenum element by adsorption with a special resin from the circulating deionized water pool. The system operates at negative pressure as a whole, and thus has better environmental friendliness and higher recovery rate. 6) Automatic and massive production. Also, since automatic control (or computer control) can be achieved for refrigeration in each unit according to the present invention, massive continuous production is enabled as long as raw materials are replenished and full containers for product are removed and replaced with new containers. As a result, the process has an incomparable advantage over the existing sublimation processes for the preparation of molybdenum trioxide. Using this process, a product line can produce approximately 50 tons of nano-molybdenum trioxide annually. 7) A nanoscale and spherical product. In the invention, the nano-molybdenum trioxide is treated by rapid cooling with inexpensive air. The product has a particle size of ≤ 100 nm, a specific surface area of ≤ 40 m2 / g and a sphericity of ≥ 0.92. The invention has the following advantageous aspects: nano-quasi-spherical molybdenum trioxide can be obtained by sublimating the molybdenum trioxide with pollution-free and highly efficient recovery. character list
[0020] In order to explain the exemplary embodiments according to the invention and the technical solutions in the prior art in more detail, the drawing required for the description of the exemplary embodiments or the prior art is briefly summarized below. It goes without saying that the following drawing represents only one embodiment of the invention and other drawings based on this drawing may be obtained by a person skilled in the art without the use of any inventive activity. figure 1 shows a schematic structural view of the present invention. DETAILED DESCRIPTION
[0021] The technical solutions according to the invention are described clearly and completely below with reference to the drawing in the exemplary embodiment according to the invention. Of course, the exemplary embodiment described does not represent all but part of the exemplary embodiments according to the invention. Due to the embodiment in the present invention, the other embodiments, which can be obtained by those skilled in the art without the use of the inventive faculty, should fall within the scope of the invention.
[0022] A device for the production of high-purity nano-molybdenum trioxide is in figure 1 shown showing a raw material silo 1 , a material feed 2 , a furnace for sublimation 7, a first ventilation pipe 24 , a second ventilation tube 25 , a spray device 23 and a filter arrangement 12 includes, wherein the raw material silo 1 with the material supply 2 is connected, the material feed 2 to the bottom of the oven for sublimation 7 is connected, the furnace for sublimation 7 is connected at its top to the horizontally arranged first ventilation pipe 24, one end of the first ventilation pipe 24 with the vertically arranged second ventilation pipe 25 is connected, and the second ventilation pipe 25 with a recovery device 13 connected is; being a product silo 11 below the recovery device 13 is provided; wherein the filter assembly 12 at the junction of the recovery device 13 with the second ventilation pipe 25 is provided; where the spray device 23 at the junction between the first vent tube 24 and the second vent tube 25 is provided; the spray device 23 with a dispersant connection 21 and a compressed air connection 22 is connected; the spraying direction of the spraying device 23 being coaxial with the axis of the second aeration pipe 25 is; and having a clean air inlet 10 on the first ventilation pipe 24 is provided.
[0023] In this embodiment is an agitator 20 in the first ventilation tube 24 placed horizontally, with one end of the agitator 20 is connected to a rotary motor 18 and the rotary motor 18 on a drive shaft of a displacement motor 19 is mounted so that the displacement motor 19 controls the rotation motor 18 in the linear direction of the first ventilation tube 24 shifts back and forth to the agglomerate and pulverization of the molybdenum trioxide in the first aeration tube 24 to avoid.
[0024] A tube of the reclamation device 13 is connected to a water spray pump 15 at one end and extends into the filter assembly 12 at the other end. The water spray pump 15 is equipped with a deionized water pool 16 connected, which is connected through a circuit with the water spray pump 15. A circulation pump 17 is provided in the circuit. A first valve 26 is in the pipe between the recovery device 13 and the water spray pump 15 intended. A compressed air connection 14 is between the first valve 26 and the recovery device 13 is provided. The compressed air connection 14 is with a second valve 27 educated. The filter assembly 12comprises a seal of a sealed hollow metal-blocking mesh enveloped by a layer of temperature-resistant filter cloth with nano-molybdenum trioxide sandwiched in the intermediate layer between the metal-blocking foil and the temperature-resistant filter cloth, and the interior of the metal- blocking foil through a tube with the compressed air connection 14 with the second valve 27 connected is.
[0025] The spray device sprays in this solution 23 a mist with a dispersant that carries the powdered molybdenum trioxide into the recovery equipment. The molybdenum trioxide is used in the filter assembly 12 filtered and into the product silo 11 collected. The air goes from the pipe into the water spray pump 15 , where the partially contained molybdenum trioxide after spraying and dissolving into the deionized water pool 16 enters After a period of manufacture, the first valve 26 closed and the second valve 27 opened to introduce pressurized air which, after entering the hollow core of the metal blocking foil of the filter assembly 12 the molybdenum trioxide adhering to the filter cloth at the high temperature is blown away, which goes into the product silo 11 enters Thereafter, the filter assembly can be reused.
[0026] In this embodiment, the floor 6 of the oven for sublimation 7 formed obliquely, with the end at the connection point with the material feed 2 is higher and a liquid outlet 8 at the lower end of the floor 6 is provided. A compressed air connection 9 is on one side under the oven for sublimation 7 intended. In addition, a silicon-molybdenum rod 4 and a temperature-controlled electrical resistor 5 are placed in the furnace for sublimation 7 are provided, which can regulate the temperature in the oven, detect it in real time and control it automatically.
[0027] An observation port 3 is on a side wall of the oven for sublimation 7 provided and the observation port 3 is at the same level as the first ventilation pipe 24 to observing the situation in the furnace for sublimation and the first ventilation tube 24 to facilitate.
[0028] Also provided is a method for producing high-purity nano-molybdenum trioxide, in which pure molybdenum trioxide is used as the raw material, which is fed through a material feed 2 an oven for sublimation 7 fed and in the oven for sublimation 7 sublimated at a controlled temperature of 1100 - 1600°C; after starting a displacement motor 19 and a rotary motor 18 clean air at 10 - 18°C with less than 30% water content from a clean air inlet 10 is initiated; and maintaining a temperature in a first vent tube 24 from 75 - 85°C a spray device 23 is switched on to spray a mist with dispersant, whereby the raw material is sprayed into a recovery device, filtered and collected, while the air, after filtering off the raw material in a filter, is fed into a deionized water pool 16 is initiated. Compressed air with a water content of less than 30% is supplied from a compressed air connection 9 at the bottom of the sublimation oven 7 is initiated to replenish the air to increase the amount of sublimated molybdenum trioxide, the air having a temperature of 15 - 18°C, a humidity of 28% - 35% and a pressure of 0.75 - 0.8MPa.
[0029] Only the preferred embodiments of the present invention have been explained above, but the invention shall not be limited thereto. All modifications, equivalent substitutions and extensions that fall within the scope of the idea and principle of the invention are intended to be included in the scope of the invention. QUOTES INCLUDED IN DESCRIPTION
[0000] This list of documents cited by the applicant was generated automatically and is included solely for the better information of the reader. The list is not part of the German patent or utility model application. The DPMA assumes no liability for any errors or omissions. Patent Literature Cited
[0000] US4551313
[0003] US6468497
[0004]
Claims
[1] Device for the production of high-purity nano-molybdenum trioxide, characterized bythat the device comprises a raw material silo (1), a material feed (2), a sublimation oven (7), a first ventilation tube (24), a second ventilation tube (25), a spraying device (23), and a filter arrangement (12), wherein the raw material silo (1) is connected to the material feed (2), the material feed (2) is connected to the underside of the sublimation oven (7), the sublimation oven (7) is connected at its top to the horizontally arranged first ventilation tube (24), one end of the first ventilation tube (24) is connected to the vertically arranged second ventilation tube (25), and the second ventilation tube (25) is connected to a recovery device (13); wherein a product silo (11) is provided below the recovery device (13); wherein the filter arrangement (12) is provided at the connection point of the recovery device (13) with the second ventilation tube (25);wherein the spray device (23) is provided at the connection point between the first ventilation tube (24) and the second ventilation tube (25); wherein the spray device (23) is connected to a dispersion medium connection (21) and a compressed air connection (22); wherein the spray direction of the spray device (23) is coaxial with the axis of the second ventilation tube (25); and wherein an inlet for clean air (10) is provided on the first ventilation tube (24). [2] Device for producing high-purity nano-molybdenum trioxide according to claim 1, characterized by , that an agitator (20) is arranged horizontally in the first ventilation tube (24), wherein one end of the agitator (20) is connected to a rotary motor (18) and the rotary motor (18) is mounted on a drive shaft of a displacement motor (19), so that the displacement motor (19) moves the rotary motor (18) back and forth in the linear direction of the first ventilation tube (24). [3] Device for producing high-purity nano-molybdenum trioxide according to claim 1, characterized by , that a pipe of the recovery device (13) is connected at one end to a water spray pump (15) and extends at the other end to the filter arrangement (12); that the water spray pump (15) is connected to a pool for deionized water (16) which is connected to the water spray pump (15) by a circuit; and that a circulation pump (17) is provided in the circuit. [4] Device for producing high-purity nano-molybdenum trioxide according to claim 3, characterized by , that a first valve (26) is provided in the pipe between the recovery device (13) and the water spray pump (15), a compressed air connection (14) is provided between the first valve (26) and the recovery device (13), and the compressed air connection (14) is equipped with a second valve (27). [5] Device for producing high-purity nano-molybdenum trioxide according to claim 4, characterized by , that the filter arrangement (12) comprises a seal consisting of a sealed, hollow, metal-blocking film which is enveloped by a layer of a temperature-resistant filter cloth, wherein nano-molybdenum trioxide is inserted in the intermediate layer between the metal-blocking film and the temperature-resistant filter cloth, and the interior of the metal-blocking film is connected to the second valve (27) via a pipe with the compressed air connection (14). [6] Device for producing high-purity nano-molybdenum trioxide according to claim 1, characterized by , that the bottom (6) of the sublimation oven (7) is inclined, with the end at the connection point with the material feed (2) being higher and a liquid outlet (8) being provided at the lower end of the bottom (6). [7] Device for producing high-purity nano-molybdenum trioxide according to claim 1, characterized by , that a compressed air connection (9) is provided on one side under the oven for sublimation (7). [8] Device for producing high-purity nano-molybdenum trioxide according to claim 1, characterized by , that an observation opening (3) is provided on a side wall of the furnace for sublimation (7) and the observation opening (3) is located at the same level as the first ventilation tube (24). [9] Methods for the production of high-purity nano-molybdenum trioxide, characterized by, that pure molybdenum trioxide is used as a raw material, which is fed by a material feed (2) to a sublimation oven (7) and sublimated in the sublimation oven (7) at a controlled temperature of 1100 - 1600°C; that after starting a displacement motor (19) and a rotary motor (18), clean air at 10 - 18°C with a water content of less than 30% is introduced from a clean air inlet (10); and that, while maintaining a temperature in a first ventilation tube (24) of 75 - 85°C, a spraying device (23) is switched on to spray a mist with dispersant, the raw material being sprayed into a recovery device, filtered and collected, while the air, after filtering out the raw material in a filter, is introduced into a pool for deionized water (16). [10] Method for producing high-purity nano-molybdenum trioxide according to claim 9, characterized by, that compressed air with a water content of less than 30% is introduced from a compressed air connection (9) on the lower part of the sublimation furnace (7) to replenish the air and thus increase the amount of sublimated molybdenum trioxide, wherein the air has a temperature of 15 - 18°C, a humidity of 28% - 35% and a pressure of 0.75 - 0.8MPa.