CN112038711A - Method for preparing lead sulfide ultrafine powder by using lead plaster of waste lead-acid storage battery - Google Patents
Method for preparing lead sulfide ultrafine powder by using lead plaster of waste lead-acid storage battery Download PDFInfo
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- CN112038711A CN112038711A CN202010934919.3A CN202010934919A CN112038711A CN 112038711 A CN112038711 A CN 112038711A CN 202010934919 A CN202010934919 A CN 202010934919A CN 112038711 A CN112038711 A CN 112038711A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/06—Lead-acid accumulators
- H01M10/12—Construction or manufacture
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G21/00—Compounds of lead
- C01G21/21—Sulfides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/54—Reclaiming serviceable parts of waste accumulators
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
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- Y02W30/84—Recycling of batteries or fuel cells
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Abstract
The invention discloses a method for preparing lead sulfide ultrafine powder by utilizing lead plaster of a waste lead-acid storage battery, which is used for solving the problems of insufficient technology and low added value of recovered products in the prior art of recovering the waste lead-acid storage battery, and aims to solve the problems of resource waste and environmental pollution caused by the waste lead-acid storage battery; the dry lead plaster is crushed by sawing, grinding and the crushing degree can be adjusted according to the requirement between the two rotating shafts, and the lead plaster has the advantages of high production efficiency, low power consumption, convenient adjustment and the like.
Description
Technical Field
The invention relates to lead sulfide ultrafine powder, in particular to a method for preparing lead sulfide ultrafine powder by utilizing lead plaster of a waste lead-acid storage battery.
Background
At present, waste lead-acid batteries are mainly used for recycling secondary lead, processes of the waste lead-acid batteries are mainly divided into pyrometallurgy and hydrometallurgy, wherein hydrometallurgy is more popularized at present, high-purity secondary lead can be prepared by the processes, but the additional value of the secondary lead is low, and secondary processing オ is required to be applied to specific industries.
The invention patent CN103146923B discloses a method for producing lead oxide by recycling waste lead-acid batteries based on an atom economy approach, belonging to the chemical field of cleaning and recycling the waste lead-acid batteries. Lead paste and lead powder of a lead-acid battery are heated to carry out solid-phase mixing reaction, sodium hydroxide alkaline desulfurization and sodium hydroxide leaching processes to directly obtain a lead-containing alkaline solution and filter residue, the solution is purified and cooled to crystallize to obtain high-purity lead oxide, and sodium sulfate is a byproduct, so that the defect that a large amount of chemical raw materials are consumed in the conventional lead oxide synthesis process is overcome, and the method is a novel technology with clean, energy-saving and large-scale industrial application prospects. These recovery methods all require a desulfurization process, fail to fully utilize sulfur element, and have a long and complicated operation flow.
Therefore, a method for preparing lead sulfide ultrafine powder by using lead paste of waste lead-acid storage batteries is provided.
Disclosure of Invention
The invention aims to provide a method for preparing lead sulfide ultrafine powder by using waste lead-acid storage battery lead plaster, which is used for solving the problems of the prior art that the waste lead-acid storage battery is not sufficient and the additional value of the recovered product is low. The method comprises the following steps of (1) crushing dry lead plaster of a waste lead-acid battery by using a crusher, further grinding the dry lead plaster into fine powdery particles by using a grinder, carrying out reduction by using heating carbon, simultaneous vulcanization by evaporation and gasification and quenching by introducing inert gas under a vacuum condition to prepare high-purity and high-dispersion cubic superfine lead sulfide powder; the main working parts of the pulverizer are a pair of cylindrical rotating shafts, the surfaces of the rotating shafts are provided with pulverizing teeth, and dry lead paste is pulverized by sawing, grinding and the like between the two rotating shafts. The degree of comminution can be adjusted as desired. Has the advantages of high production efficiency, low power consumption, convenient adjustment and the like; the upper end of the discharge hopper is provided with a hook, one side of the protective outer cover close to the discharge hopper is provided with a hanging rod, and the inside of the machine body frame is provided with a material sliding plate, so that the crushed particles can move towards the discharge hopper under the driving of the crushing teeth of the crusher, and can also move towards the discharge hopper under the driving of the gravity of the crushing teeth of the crusher, and the crushed particles are very easy to discharge from the crusher and can not be adhered to the inside of the crusher; crushing, grinding and crushing, heating and condensing, opening a nitrogen supply system when the heating chamber and the condensing chamber reach the set temperature, introducing nitrogen into the tubular furnace, controlling the pressure to be 300-6000Pa, keeping constant, and keeping the time for 1-3.5 h; under the conditions of inert gas quenching and temperature difference gradient of the heating chamber and the condensing chamber, the collection substrate horizontally placed in the condensing chamber collects the condensed lead sulfide steam until the lead sulfide steam is cooled to room temperature, the lead sulfide ultrafine powder is obtained, the sulfur element is fully utilized, and waste is avoided.
The purpose of the invention can be realized by the following technical scheme: a method for preparing lead sulfide ultrafine powder by using lead plaster of a waste lead-acid storage battery comprises the following steps:
the method comprises the following steps: crushing and separating the waste lead-acid storage battery to obtain lead plaster; drying the obtained lead plaster at low temperature by using a low-temperature belt type drying machine;
step two: crushing the dry lead plaster obtained in the step 1 by using a crusher, and further grinding the dry lead plaster into finer powdery particles by using a grinder;
step three: fully mixing powdery lead plaster with a reducing agent, placing the mixture into a high-temperature-resistant crucible, placing the crucible into a tubular furnace, wherein the tubular furnace is divided into a heating chamber and a condensing chamber, two ends of the heating chamber are isolated by a perforated pipe plug, the crucible filled with sulfur powder is placed at the front end of the perforated pipe plug at one end of the heating chamber, and a collecting substrate is horizontally placed at the rear end of the perforated pipe plug at the other end of the heating chamber;
step four: starting a vacuum pump to pump air after the tubular furnace is sealed, so that the pressure in the tubular furnace is 0.2-1.5 Pa;
step five: starting a power supply of the tubular furnace, and respectively heating the heating chamber and the condensing chamber to 800-900 ℃ and 250-500 ℃ at the heating rate of 15-30 ℃/min;
step six: when the heating chamber and the condensing chamber reach the set temperature, opening a nitrogen supply system, introducing nitrogen into the tubular furnace, controlling the pressure to be 300-6000Pa, and keeping the pressure constant for 1-3.5 h;
step seven: and under the conditions of inert gas quenching and temperature difference gradient of the heating chamber and the condensing chamber, collecting condensed lead sulfide steam by a collection substrate horizontally placed in the condensing chamber until the lead sulfide steam is cooled to room temperature to obtain the lead sulfide ultrafine powder.
Preferably, the mass ratio of the lead paste, the reducing agent and the sulfur powder in the third step is as follows:
lead paste, reducing agent and sulfur powder in the weight ratio of 1 to 0.13-0.63 to 0.5-1.3; wherein, the reducing agent is carbon powder, scrap iron, magnesium powder or one of the carbon powder, the scrap iron and the magnesium powder.
Preferably, in the first step, the temperature for drying the lead plaster by the low-temperature belt drier is 30-90 ℃, and in the second step, the particle size of the fine powder particles is 0.01-0.1 mm; in the third step, the thickness of the perforated pipe plug is 2-6cm, the diameter of the perforated pipe plug is 80-120mm, and the diameter of a central vent hole of the perforated pipe plug is 50-132 mm; in the third step, the specific position of the crucible filled with the sulfur powder is 15-25mm away from the perforated pipe plug, and the specific position of the collecting substrate is 30-85cm away from the perforated pipe plug; in the third step, the collecting substrate is 150-.
Preferably, the pulverizer comprises a machine body frame, a screw rod, a protective shell, a conveying groove, a rocker, a switch box, a hanging rod, a hook, a discharge hopper, a motor, a moving wheel, a driving wheel, an auxiliary wheel, a driven rotating tooth, a motor support, a main rotating tooth, a pulverizing tooth, a third shaft, a main rotating shaft, a chain, a driven rotating shaft, a rotating wheel, a protective outer cover, a sliding plate and an auxiliary shaft, wherein the motor is arranged in the machine body frame;
the crushing mechanism comprises a protective outer cover, a conveying groove, a transmission mechanism, a sliding material plate and a discharging hopper, wherein a switch box is installed on the upper side of the protective outer cover, a rocker is installed on the upper side of the switch box, the conveying groove is installed on one side of the protective outer cover, the discharging hopper is installed on the other side, away from the conveying groove, of the protective outer cover, a hook is installed at the upper end of the discharging hopper, a hanging rod is installed on one side, close to the discharging hopper, of the protective outer cover, and the sliding material plate is installed inside;
the transmission mechanism comprises a motor, a driving wheel, a driven wheel, a main rotating tooth and an auxiliary rotating tooth, wherein the output shaft of the motor is provided with the rotating wheel, the upper side of the machine body frame is provided with a main rotating shaft, the main rotating shaft penetrates through the protective outer cover to be rotatably arranged on the upper side of the machine body frame, one side of the main rotating shaft, which is close to the rotating wheel, is provided with the driving wheel, the main rotating shaft is positioned on the outer side of the driving wheel and is provided with the auxiliary wheel, the upper side of the machine body frame is provided with the auxiliary rotating shaft, the auxiliary rotating shaft penetrates through the protective outer cover to be rotatably arranged on the upper side of the machine body frame, one side of the auxiliary rotating shaft, which is close to the rotating wheel, is provided with the auxiliary rotating tooth, the upper side of the auxiliary shaft is provided with a third shaft, the third shaft is connected with the driven rotating shaft through a chain, and a protective shell is arranged on the outer side of the chain;
crushing teeth are installed on the third shaft and the part wrapped by the protective outer cover from the rotating shaft, and the crushing teeth are in irregular shapes.
Preferably, the bearing is all installed to main pivot, follow pivot, countershaft and third axle, the race groove has all been seted up with from driving wheel inside to rotation wheel, auxiliary wheel, action wheel, and the race groove matches with driving belt.
Preferably, the hanging rod is matched with the hook.
Preferably, the fixed block is installed to the protection dustcoat side, protection dustcoat internally mounted has the arc piece, protruding piece is installed on the arc piece top, the L-shaped piece is installed to the protection dustcoat upside, be connected with the elastic component under the L-shaped piece, the elastic component cover is on protruding piece surface, the fixed block is connected with the third axle.
Preferably, the step of crushing and drying the lead paste by the crusher is as follows:
the method comprises the following steps: preparing two transmission belts outside, connecting the rotating wheel and the auxiliary wheel by using one transmission belt, connecting the driving wheel and the driven wheel by using the other transmission belt, and connecting the other transmission belt with a power supply of the pulverizer;
step two: pouring the dry lead paste into a conveying groove, and shifting a rocker on the upper side of the switch box to an open state;
step three: when the motor is started, the motor rotates to drive the rotating wheel on the output shaft of the motor to rotate, the rotating wheel drives the auxiliary wheel to rotate through the transmission belt, the auxiliary wheel drives the driving wheel, the driving wheel drives the driven wheel to rotate, and further the main rotating shaft and the driven rotating shaft are driven to rotate; the auxiliary rotating shaft drives the main rotating teeth to rotate, the main rotating teeth drive the auxiliary rotating teeth to rotate, and the auxiliary rotating shaft drives the third shaft to rotate through the chain;
step four: the third shaft and the part of the driven shaft wrapped by the protective outer cover are both provided with crushing teeth, and the third shaft is meshed with the crushing teeth driven by the rotation of the driven shaft so as to roll the dry lead plaster into fine particles;
step five: the discharge hopper is opened, the discharge hopper is hung on the hanging rod through the hook on the upper side of the discharge hopper, and fine particles slide through the sliding plate and are leaked from the discharge hopper.
Compared with the prior art, the invention has the beneficial effects that:
1. the method ensures that the lead in the waste lead-acid battery is recycled at high value, promotes the recycling of limited resources and relieves the potential lead pollution hazard of the waste lead-acid battery to human beings and the environment. The method for preparing the superfine lead sulfide powder by using the waste lead-acid battery lead paste has the characteristics of simple operation, high efficiency and the like; each component of the waste lead-acid battery can be properly recycled; compared with the traditional method for recovering lead in waste lead-acid batteries by pyrometallurgy, the method has outstanding advantages in the aspects of environmental protection and efficient utilization of resources.
2. The main working parts of the pulverizer are a pair of cylindrical rotating shafts, the surfaces of the rotating shafts are provided with pulverizing teeth, and dry lead paste is pulverized by sawing, grinding and the like between the two rotating shafts. The degree of comminution can be adjusted as desired. Has the advantages of high production efficiency, low power consumption, convenient adjustment and the like.
3. According to the pulverizer disclosed by the invention, the hook is arranged at the upper end of the discharge hopper, the hanging rod is arranged on one side, close to the discharge hopper, of the protective outer cover, and the sliding plate is arranged in the machine body frame, so that pulverized particles can move towards the discharge hopper under the driving of the pulverizing teeth of the pulverizer, and can be easily discharged from the pulverizer and cannot be adhered to the pulverizer.
4. The method adopts the mode of crushing firstly and then grinding and crushing, then heating and condensing, when the heating chamber and the condensing chamber reach the set temperature, opening a nitrogen supply system, introducing nitrogen into the tubular furnace, controlling the pressure to be 300-6000Pa, keeping constant, and keeping the time for 1-3.5 h; under the conditions of inert gas quenching and temperature difference gradient of the heating chamber and the condensing chamber, the collection substrate horizontally placed in the condensing chamber collects the condensed lead sulfide steam until the lead sulfide steam is cooled to room temperature, the lead sulfide ultrafine powder is obtained, the sulfur element is fully utilized, and waste is avoided.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic perspective view of the entire structure of a pulverizer of the present invention;
FIG. 2 is an isometric view of the shredder of the present invention;
FIG. 3 is a front view of the shredder of the present invention;
FIG. 4 is a left side view of the shredder of the present invention;
FIG. 5 is a top view of the shredder of the present invention;
fig. 6 is an enlarged view of a portion a in fig. 1.
In the figure: 1. a machine body frame; 2. a screw rod; 3. a protective shell; 4. a conveying trough; 5. a rocker; 6. a switch box; 7. a hanging rod; 8. hooking; 9. a discharge hopper; 10. a motor; 11. a moving wheel; 12. a driving wheel; 13. a secondary wheel; 14. a driven wheel; 15. the driven gear rotates; 16. a motor bracket; 17. a main rotating tooth; 18. crushing teeth; 19. a third axis; 20. a main rotating shaft; 21. a chain; 22. a slave shaft; 23. a rotating wheel; 24. a protective outer cover; 25. a material sliding plate; 26. a counter shaft; 27. an arc-shaped block; 28. a raised block; 29. an elastic member; 30. an L-shaped block; 31. and (5) fixing blocks.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1-6, a method for preparing lead sulfide ultrafine powder by using lead plaster of waste lead-acid storage batteries includes the following steps:
the method comprises the following steps: crushing and separating the waste lead-acid storage battery to obtain lead plaster; drying the obtained lead plaster at low temperature by using a low-temperature belt type drying machine;
step two: crushing the dry lead plaster obtained in the step 1 by using a crusher, and further grinding the dry lead plaster into finer powdery particles by using a grinder;
step three: fully mixing powdery lead plaster with a reducing agent, placing the mixture into a high-temperature-resistant crucible, placing the crucible into a tubular furnace, wherein the tubular furnace is divided into a heating chamber and a condensing chamber, two ends of the heating chamber are isolated by a perforated pipe plug, the crucible filled with sulfur powder is placed at the front end of the perforated pipe plug at one end of the heating chamber, and a collecting substrate is horizontally placed at the rear end of the perforated pipe plug at the other end of the heating chamber;
step four: starting a vacuum pump to pump air after the tubular furnace is sealed, so that the pressure in the tubular furnace is 0.2-1.5 Pa;
step five: starting a power supply of the tubular furnace, and respectively heating the heating chamber and the condensing chamber to 800-900 ℃ and 250-500 ℃ at the heating rate of 15-30 ℃/min;
step six: when the heating chamber and the condensing chamber reach the set temperature, opening a nitrogen supply system, introducing nitrogen into the tubular furnace, controlling the pressure to be 300-6000Pa, and keeping the pressure constant for 1-3.5 h;
step seven: and under the conditions of inert gas quenching and temperature difference gradient of the heating chamber and the condensing chamber, collecting condensed lead sulfide steam by a collection substrate horizontally placed in the condensing chamber until the lead sulfide steam is cooled to room temperature to obtain the lead sulfide ultrafine powder.
Wherein, the mass ratio of the lead plaster, the reducing agent and the sulfur powder in the third step is as follows:
lead paste, reducing agent and sulfur powder in the weight ratio of 1 to 0.13-0.63 to 0.5-1.3; wherein, the reducing agent is carbon powder, scrap iron, magnesium powder or one of the carbon powder, the scrap iron and the magnesium powder.
Wherein, in the first step, the temperature for drying the lead plaster by the low-temperature belt drier is 30-90 ℃, and in the second step, the grain diameter of the fine powder particles is 0.01-0.1 mm; in the third step, the thickness of the perforated pipe plug is 2-6cm, the diameter of the perforated pipe plug is 80-120mm, and the diameter of a central vent hole of the perforated pipe plug is 50-132 mm; in the third step, the specific position of the crucible filled with the sulfur powder is 15-25mm away from the perforated pipe plug, and the specific position of the collecting substrate is 30-85cm away from the perforated pipe plug; in the third step, the collecting substrate is 150-.
The crusher comprises a machine body frame 1, a screw rod 2, a protective shell 3, a conveying groove 4, a rocker 5, a switch box 6, a hanging rod 7, a hook 8, a discharge hopper 9, a motor 10, a moving wheel 11, a driving wheel 12, a secondary wheel 13, a driven wheel 14, a driven gear 15, a motor support 16, a main gear 17, a crushing tooth 18, a third shaft 19, a main rotating shaft 20, a chain 21, a driven rotating shaft 22, a rotating wheel 23, a protective outer cover 24, a sliding plate 25 and an auxiliary shaft 26, wherein the motor 10 is arranged in the machine body frame 1, the motor support 16 is fixed on the lower side of the motor 10, the screw rod 2 is arranged between the machine body frame 1 and the motor support 16, the moving wheels 11 are arranged on the lower side of the machine body frame 1, the moving wheels 11 are four in number and are respectively positioned at four corners of the bottom of the machine body frame 1;
the crushing mechanism comprises a protective outer cover 24, a conveying groove 4, a transmission mechanism, a material sliding plate 25 and a material discharging hopper 9, wherein a switch box 6 is installed on the upper side of the protective outer cover 24, a rocker 5 is installed on the upper side of the switch box 6, the conveying groove 4 is installed on one side of the protective outer cover 24, the material discharging hopper 9 is installed on the other side, away from the conveying groove 4, of the protective outer cover 24, a hook 8 is installed at the upper end of the material discharging hopper 9, a hanging rod 7 is installed on one side, close to the material discharging hopper 9, of the protective outer cover 24, and the material sliding plate 25;
the transmission mechanism comprises a motor 10, a driving wheel 12, a driven wheel 14, a main rotating tooth 17 and a secondary rotating tooth 15, wherein a rotating wheel 23 is installed on an output shaft of the motor 10, a main rotating shaft 20 is installed on the upper side of the machine body frame 1, the main rotating shaft 20 penetrates through a protective outer cover 24 and is installed on the upper side of the machine body frame 1 in a rotating mode, the driving wheel 12 is installed on one side, close to the rotating wheel 23, of the main rotating shaft 20, an auxiliary wheel 13 is installed on the outer side, located on the driving wheel 12, of the main rotating shaft 20, a secondary rotating shaft 22 is installed on the upper side of the machine body frame 1, the secondary rotating shaft 22 penetrates through the protective outer cover 24 and is installed on the upper side of the machine body frame 1 in a rotating mode, the main rotating tooth 17 is installed on one side, close to the rotating shaft 22, located on the outer side of the main rotating, the auxiliary rotating teeth 15 are arranged on one side of the auxiliary shaft 26 close to the rotating wheel 23, the third shaft 19 is arranged on the upper side of the auxiliary shaft 26, the third shaft 19 is connected with the auxiliary rotating shaft 22 through a chain 21, and the protective shell 3 is arranged on the outer side of the chain 21;
the third shaft 19 and the part wrapped by the protective cover 24 from the rotating shaft 22 are both provided with the crushing teeth 18, and the crushing teeth 18 are in irregular shapes.
The main rotating shaft 20, the auxiliary rotating shaft 22, the auxiliary shaft 26 and the third shaft 19 are all provided with bearings, belt grooves are formed in the rotating wheel 23, the auxiliary wheel 13, the driving wheel 12 and the driven wheel 14, and the belt grooves are matched with a transmission belt.
Wherein the hanging rod 7 is matched with the hook 8.
Wherein, fixed block 31 is installed to protection dustcoat 24 side, protection dustcoat 24 internally mounted has arc piece 27, protruding piece 28 is installed on arc piece 27 top, L-shaped piece 30 is installed to protection dustcoat 24 upside, be connected with elastic component 29 under the L-shaped piece, elastic component 29 covers on protruding piece 28 surface, fixed block 31 is connected with third axle 19.
The method comprises the following steps of:
the method comprises the following steps: preparing two transmission belts outside, connecting the rotating wheel 23 and the auxiliary wheel 13 by using one transmission belt, connecting the driving wheel 12 and the driven wheel 14 by using the other transmission belt, and connecting the two transmission belts with a power supply of the pulverizer;
step two: pouring dry lead paste into a conveying groove 4, and shifting a rocker 5 on the upper side of a switch box 6 to be in an open state;
step three: when the motor 10 is started, the motor 10 rotates to drive the rotating wheel 23 on the output shaft of the motor 10 to rotate, the rotating wheel 23 drives the secondary wheel 13 to rotate through the transmission belt, the secondary wheel 13 drives the driving wheel 12, the driving wheel 12 drives the driven wheel 14 to rotate, and further drives the main rotating shaft 20 and the driven rotating shaft 22 to rotate; the auxiliary rotating shaft 22 drives the main rotating tooth 17, the main rotating tooth 17 drives the auxiliary rotating tooth 15 to rotate, and the auxiliary rotating shaft 22 drives the third shaft 19 to rotate through the chain 21;
step four: the third shaft 19 and the part of the driven shaft 22 wrapped by the protective outer cover 24 are both provided with crushing teeth 18, and the third shaft 19 is meshed with the crushing teeth 18 driven by the rotation of the driven shaft 22 so as to crush the dry lead plaster into fine particles;
step five: the discharge hopper 9 is opened, the discharge hopper 9 is hung on the hanging rod 7 through the hook 8 on the upper side of the discharge hopper 9, and fine particles slide through the sliding plate 25 and leak out of the discharge hopper 9.
The preparation method comprises the following steps: the method for preparing the lead sulfide ultrafine powder by utilizing the lead plaster of the waste lead-acid storage battery comprises the following steps:
the method comprises the following steps: crushing and separating the waste lead-acid storage battery to obtain lead plaster; drying the obtained lead plaster at low temperature by using a low-temperature belt type drying machine;
step two: crushing the dry lead plaster obtained in the step 1 by using a crusher, and further grinding the dry lead plaster into finer powdery particles by using a grinder;
the crushing process of the crusher is as follows:
the first step is as follows: preparing two transmission belts outside, connecting the rotating wheel 23 and the auxiliary wheel 13 by using one transmission belt, connecting the driving wheel 12 and the driven wheel 14 by using the other transmission belt, and connecting the two transmission belts with a power supply of the pulverizer;
the second step is that: pouring dry lead paste into a conveying groove 4, and shifting a rocker 5 on the upper side of a switch box 6 to be in an open state;
the third step: when the motor 10 is started, the motor 10 rotates to drive the rotating wheel 23 on the output shaft of the motor 10 to rotate, the rotating wheel 23 drives the secondary wheel 13 to rotate through the transmission belt, the secondary wheel 13 drives the driving wheel 12, the driving wheel 12 drives the driven wheel 14 to rotate, and further drives the main rotating shaft 20 and the driven rotating shaft 22 to rotate; the auxiliary rotating shaft 22 drives the main rotating tooth 17, the main rotating tooth 17 drives the auxiliary rotating tooth 15 to rotate, and the auxiliary rotating shaft 22 drives the third shaft 19 to rotate through a chain (21);
the fourth step: the third shaft 19 and the part of the driven shaft 22 wrapped by the protective outer cover 24 are both provided with crushing teeth 18, and the third shaft 19 is meshed with the crushing teeth 18 driven by the rotation of the driven shaft 22 so as to crush the dry lead plaster into fine particles;
the fifth step: the discharge hopper 9 is opened, the discharge hopper 9 is hung on the hanging rod 7 through the hook 8 on the upper side of the discharge hopper 9, and fine particles slide through the sliding plate 25 and leak out of the discharge hopper 9.
Step three: fully mixing powdery lead plaster with a reducing agent, placing the mixture into a high-temperature-resistant crucible, placing the crucible into a tubular furnace, wherein the tubular furnace is divided into a heating chamber and a condensing chamber, two ends of the heating chamber are isolated by a perforated pipe plug, the crucible filled with sulfur powder is placed at the front end of the perforated pipe plug at one end of the heating chamber, and a collecting substrate is horizontally placed at the rear end of the perforated pipe plug at the other end of the heating chamber;
step four: starting a vacuum pump to pump air after the tubular furnace is sealed, so that the pressure in the tubular furnace is 0.2 Pa;
step five: starting a power supply of the tube furnace, and respectively heating the heating chamber and the condensing chamber to 800 ℃ and 250 ℃ at the heating rate of 15 ℃/min;
step six: when the heating chamber and the condensing chamber reach the set temperature, opening a nitrogen supply system, introducing nitrogen into the tubular furnace, controlling the pressure to be 6000Pa, keeping the pressure constant, and keeping the time for 1 h;
step seven: and under the conditions of inert gas quenching and temperature difference gradient of the heating chamber and the condensing chamber, collecting condensed lead sulfide steam by a collection substrate horizontally placed in the condensing chamber until the lead sulfide steam is cooled to room temperature to obtain the lead sulfide ultrafine powder.
The method comprises the following steps of (1) crushing dry lead plaster of a waste lead-acid battery by using a crusher, further grinding the dry lead plaster into fine powdery particles by using a grinder, carrying out reduction by using heating carbon, simultaneous vulcanization by evaporation and gasification and quenching by introducing inert gas under a vacuum condition to prepare high-purity and high-dispersion cubic superfine lead sulfide powder; the main working parts of the crusher are a pair of cylindrical rotating shafts, the surfaces of the rotating shafts are provided with crushing teeth, the dry lead paste is crushed by sawing, grinding and the like between the two rotating shafts, the crushing degree can be adjusted according to requirements, and the crusher has the advantages of high production efficiency, low power consumption, convenience in adjustment and the like; the upper end of the discharge hopper is provided with a hook, one side of the protective outer cover close to the discharge hopper is provided with a hanging rod, and the inside of the machine body frame is provided with a material sliding plate, so that the crushed particles can move towards the discharge hopper under the driving of the crushing teeth of the crusher, and can also move towards the discharge hopper under the driving of the gravity of the crushing teeth of the crusher, and the crushed particles are very easy to discharge from the crusher and can not be adhered to the inside of the crusher; crushing, grinding and crushing, heating and condensing, opening a nitrogen supply system when the heating chamber and the condensing chamber reach the set temperature, introducing nitrogen into the tubular furnace, controlling the pressure to be 300-6000Pa, keeping constant, and keeping the time for 1-3.5 h; under the conditions of inert gas quenching and temperature difference gradient of the heating chamber and the condensing chamber, the collection substrate horizontally placed in the condensing chamber collects the condensed lead sulfide steam until the lead sulfide steam is cooled to room temperature, the lead sulfide ultrafine powder is obtained, the sulfur element is fully utilized, and waste is avoided.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise forms disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims (7)
1. A method for preparing lead sulfide ultrafine powder by using lead plaster of a waste lead-acid storage battery is characterized by comprising the following steps:
the method comprises the following steps: crushing and separating the waste lead-acid storage battery to obtain lead plaster; drying the obtained lead plaster at low temperature by using a low-temperature belt type drying machine;
step two: crushing the dry lead plaster obtained in the step 1 by using a crusher, and further grinding the dry lead plaster into finer powdery particles by using a grinder;
step three: fully mixing powdery lead plaster with a reducing agent, placing the mixture into a high-temperature-resistant crucible, placing the crucible into a tubular furnace, wherein the tubular furnace is divided into a heating chamber and a condensing chamber, two ends of the heating chamber are isolated by a perforated pipe plug, the crucible filled with sulfur powder is placed at the front end of the perforated pipe plug at one end of the heating chamber, and a collecting substrate is horizontally placed at the rear end of the perforated pipe plug at the other end of the heating chamber;
step four: starting a vacuum pump to pump air after the tubular furnace is sealed, so that the pressure in the tubular furnace is 0.2-1.5 Pa;
step five: starting a power supply of the tubular furnace, and respectively heating the heating chamber and the condensing chamber to 800-900 ℃ and 250-500 ℃ at the heating rate of 15-30 ℃/min;
step six: when the heating chamber and the condensing chamber reach the set temperature, opening a nitrogen supply system, introducing nitrogen into the tubular furnace, controlling the pressure to be 300-6000Pa, and keeping the pressure constant for 1-3.5 h;
step seven: and under the conditions of inert gas quenching and temperature difference gradient of the heating chamber and the condensing chamber, collecting condensed lead sulfide steam by a collection substrate horizontally placed in the condensing chamber until the lead sulfide steam is cooled to room temperature to obtain the lead sulfide ultrafine powder.
2. The method for preparing the lead sulfide ultrafine powder by using the lead plaster of the waste lead-acid storage battery according to claim 1, wherein the mass ratio of the lead plaster, the reducing agent and the sulfur powder in the third step is as follows:
lead paste, reducing agent and sulfur powder in the weight ratio of 1 to 0.13-0.63 to 0.5-1.3; wherein, the reducing agent is carbon powder, scrap iron, magnesium powder mixture or one of the mixture.
3. The method for preparing the lead sulfide ultrafine powder by using the lead plaster of the waste lead-acid storage batteries according to claim 1, wherein in the first step, the temperature for drying the lead plaster by a low-temperature belt drier is 30-90 ℃, and in the second step, the particle size of the fine powder particles is 0.01-0.1 mm; in the third step, the thickness of the perforated pipe plug is 2-6cm, the diameter of the perforated pipe plug is 80-120mm, and the diameter of a central vent hole of the perforated pipe plug is 50-132 mm; in the third step, the specific position of the crucible filled with the sulfur powder is 15-25mm away from the perforated pipe plug, and the specific position of the collecting substrate is 30-85cm away from the perforated pipe plug; in the third step, the collecting substrate is 150-.
4. The method for preparing lead sulfide ultrafine powder by using lead plaster of waste lead-acid storage batteries according to claim 1, wherein the pulverizer comprises a machine body frame (1), a motor (10) is installed inside the machine body frame (1), a motor support (16) is fixed on the lower side of the motor (10), a screw rod (2) is installed between the machine body frame (1) and the motor support (16), moving wheels (11) are installed on the lower side of the machine body frame (1), the moving wheels (11) are four in number and are respectively located at four corners of the bottom of the machine body frame (1), and a pulverizing mechanism is installed on the upper side of the machine body frame (1);
the crushing mechanism comprises a protective outer cover (24), a conveying groove (4), a transmission mechanism, a sliding plate (25) and a discharging hopper (9), wherein a switch box (6) is installed on the upper side of the protective outer cover (24), a rocker (5) is installed on the upper side of the switch box (6), the conveying groove (4) is installed on one side of the protective outer cover (24), the discharging hopper (9) is installed on the other side, away from the conveying groove (4), of the protective outer cover (24), a hook (8) is installed at the upper end of the discharging hopper (9), a hanging rod (7) is installed on one side, close to the discharging hopper (9), of the protective outer cover (24), and the sliding plate (25) is installed inside the machine body frame (1);
the transmission mechanism comprises a motor (10), a driving wheel (12), a driven wheel (14), a main rotating tooth (17) and a driven rotating tooth (15), wherein a rotating wheel (23) is installed on an output shaft of the motor (10), a main rotating shaft (20) is installed on the upper side of the machine body frame (1), the main rotating shaft (20) penetrates through a protective outer cover (24) and is installed on the upper side of the machine body frame (1) in a rotating mode, the driving wheel (12) is installed on one side, close to the rotating wheel (23), of the main rotating shaft (20), an auxiliary wheel (13) is installed on the outer side of the main rotating shaft (20), a driven rotating shaft (22) is installed on the upper side of the machine body frame (1), the protective outer cover (24) penetrates through the rotating shaft (22) and is installed on the upper side of the machine body frame (1), the main rotating tooth (17) is installed on one side, close to the rotating wheel (23, an auxiliary shaft (26) is installed on the upper side of the auxiliary rotating shaft (22), the auxiliary shaft (26) penetrates through the protective outer cover (24) and is rotatably installed on the upper side of the machine body frame (1), an auxiliary rotating tooth (15) is installed on one side, close to the rotating wheel (23), of the auxiliary shaft (26), a third shaft (19) is installed on the upper side of the auxiliary shaft (26), the third shaft (19) is connected with the auxiliary rotating shaft (22) through a chain (21), and the protective shell (3) is installed on the outer side of the chain (21);
crushing teeth (18) are installed on the third shaft (19) and the part wrapped by the protective outer cover (24) from the rotating shaft (22), and the crushing teeth (18) are in irregular shapes.
5. The method for preparing lead sulfide ultrafine powder by using lead plaster of waste lead-acid storage batteries according to claim 4, wherein bearings are mounted on the main rotating shaft (20), the auxiliary rotating shaft (22), the auxiliary shaft (26) and the third shaft (19), belt grooves are formed in the rotating wheel (23), the auxiliary wheel (13), the driving wheel (12) and the driven wheel (14), and the belt grooves are matched with a transmission belt.
6. The method for preparing lead sulfide ultrafine powder by using lead plaster of waste lead-acid storage batteries according to claim 4, characterized in that the hanging rod (7) is matched with the hook (8).
7. The method for preparing the lead sulfide ultrafine powder by using the lead plaster of the waste lead-acid storage batteries as claimed in claim 4, wherein the step of crushing and drying the lead plaster by the crusher is as follows:
the method comprises the following steps: preparing two transmission belts outside, connecting a rotating wheel (23) and an auxiliary wheel (13) by using one transmission belt, connecting a driving wheel (12) and a driven wheel (14) by using the other transmission belt, and connecting a power supply of the pulverizer;
step two: pouring the dry lead paste into a conveying groove (4), and shifting a rocker (5) on the upper side of a switch box (6) to an open state;
step three: the motor (10) is started, the motor (10) rotates to drive the rotating wheel (23) on the output shaft of the motor (10) to rotate, the rotating wheel (23) drives the auxiliary wheel (13) to rotate through the transmission belt, the auxiliary wheel (13) drives the driving wheel (12), the driving wheel (12) drives the driven wheel (14) to rotate, and then the driving rotating shaft (20) and the driven rotating shaft (22) are driven to rotate; the auxiliary rotating shaft (22) drives the main rotating gear (17), the main rotating gear (17) drives the auxiliary rotating gear (15) to rotate, and the auxiliary rotating shaft (22) drives the third shaft (19) to rotate through the chain (21);
step four: the third shaft (19) and the part wrapped by the protective outer cover (24) from the rotating shaft (22) are both provided with crushing teeth (18), and the third shaft (19) and the part wrapped by the protective outer cover (24) from the rotating shaft (22) drive the crushing teeth (18) to be meshed so as to roll the dry lead plaster into fine particles;
step five: the discharge hopper (9) is opened, the discharge hopper (9) is hung on the hanging rod (7) through the hook (8) on the upper side of the discharge hopper (9), and fine particles slide through the sliding plate (25) and leak out of the discharge hopper (9).
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| CN202010934919.3A CN112038711A (en) | 2020-09-08 | 2020-09-08 | Method for preparing lead sulfide ultrafine powder by using lead plaster of waste lead-acid storage battery |
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| CN202010934919.3A CN112038711A (en) | 2020-09-08 | 2020-09-08 | Method for preparing lead sulfide ultrafine powder by using lead plaster of waste lead-acid storage battery |
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Application publication date: 20201204 |