Battery-grade lithium carbonate purification method and purification device
阅读说明:本技术 一种电池级碳酸锂提纯方法及提纯装置 (Battery-grade lithium carbonate purification method and purification device ) 是由 周伟 徐继胜 于 2019-12-26 设计创作,主要内容包括:本发明涉及碳酸锂生产技术领域,且公开了一种电池级碳酸锂提纯装置,包括反应釜,所述反应釜的正面固定连接有加料管。该电池级碳酸锂提纯方法及提纯装置,通过振动电机的使用,振动电机的输出轴带动活动架在过滤管的内部振动,活动架带动滤网振动,避免固体将滤网堵塞,影响固液分离的效率,通过压缩弹簧的使用,在活动架受到振动时,压缩弹簧被压缩,产生弹性形变,避免活动架和过滤管直接接触,产生噪音,通过紧固块的使用,在需要将杂质从除渣箱的内部取出时,旋钮紧固块内部的螺杆即可将滤板从除渣箱的内部取出,从而将杂质取出,同时便于更换滤板,避免堵塞,实现了防堵塞的目的,提高了工作效率,方便了使用。(The invention relates to the technical field of lithium carbonate production, and discloses a battery-grade lithium carbonate purification device which comprises a reaction kettle, wherein a charging pipe is fixedly connected to the front side of the reaction kettle. This battery level lithium carbonate purification method and purification device, use through vibrating motor, vibrating motor's output shaft drives the internal vibration of movable frame at the filter tube, the movable frame drives the filter screen vibration, avoid the solid to block up the filter screen, influence solid-liquid separation's efficiency, use through compression spring, when the movable frame receives the vibration, compression spring is compressed, produce elastic deformation, avoid movable frame and filter tube direct contact, the noise produces, use through the grip block, when needs take out impurity from the inside of slagging-off case, the inside screw rod of knob grip block can be taken out the filter plate from the inside of slagging-off case, thereby take out impurity, be convenient for change the filter plate simultaneously, avoid blockking up, the mesh of preventing blockking up has been realized, the work efficiency is improved, and the use is facilitated.)
1. The utility model provides a battery level lithium carbonate purification device, includes reation kettle (1), its characterized in that: the front surface of the reaction kettle (1) is fixedly connected with a feeding pipe (2), the left side of the reaction kettle (1) is fixedly connected with an air inlet pipe (3), a feeding pipe (4) is fixedly connected with the left side of the reaction kettle (1) and the bottom of the air inlet pipe (3), a grinding box (5) is fixedly connected to the left side of the feeding pipe (4), a placing rack (6) is fixedly connected to the bottom of the grinding box (5) and is positioned on the back of the reaction kettle (1), the top of the crushing box (5) is fixedly connected with a feed hopper (7), the interior of the crushing box (5) is movably connected with a grinding cylinder (8), a first motor (9) is fixedly connected inside the placing rack (6), the output end of the first motor (9) is movably connected with a rolling cylinder (8) through a belt, the inner bottom wall of the reaction kettle (1) is fixedly connected with a liquid outlet pipe (10);
the outer side of the liquid outlet pipe (10) is fixedly connected with a first electromagnetic liquid discharge valve (11), the bottom of the liquid outlet pipe (10) is fixedly connected with a deslagging box (12), the left side and the right side of the top of the deslagging box (12) are both in threaded connection with fastening blocks (13), the inner part of the deslagging box (12) is movably connected with a filter plate (14) through a fastening block (13), the front surface of the filter plate (14) is fixedly connected with a pulling block (15), the bottom of the deslagging box (12) is fixedly connected with a liquid delivery pipe (16), the right end of the liquid sending pipe (16) is fixedly connected with a purification box (17) at the top of the placing rack (6), the top of the purifying box (17) is fixedly connected with a first pure water pipe (18), a collecting pipe (19) is fixedly connected to the top of the purifying box (17) and positioned on the left side of the first pure water pipe (18), and a condenser (20) is fixedly connected to the left side of the collecting pipe (19);
the left ends of the collecting pipe (19) and the condenser (20) are fixedly connected with a second pure water pipe (21), the outer sides of the second pure water pipe (21), the collecting pipe (19) and the first pure water pipe (18) are fixedly connected with a second electromagnetic liquid discharge valve (22), the right side of the inner wall of the purifying box (17) is fixedly connected with a fixed block (23), the bottom of the fixed block (23) is movably connected with a stirring device (24), the right side of the purifying box (17) is fixedly connected with a second motor (25), the output shaft of the second motor (25) is movably connected with the stirring device (24) through a belt, the right side of the inner wall of the purifying box (17) is positioned at the bottom of the fixed block (23) and is fixedly connected with a heating pipe (26), the inner bottom wall of the purifying box (17) is fixedly connected with a filtering pipe (27), the left side of the inner wall of the filtering pipe (, the right side fixedly connected with adjustable shelf (29) of compression spring (28), the inside fixedly connected with filter screen (30) of adjustable shelf (29), the right side of adjustable shelf (29) just is located inside fixedly connected with vibrating motor (31) of filter tube (27), the bottom fixedly connected with of filter tube (27) returns liquid pipe (32), the outside fixedly connected with third electromagnetism flowing back valve (33) of returning liquid pipe (32), the left end fixedly connected with reation kettle (1) of returning liquid pipe (32).
2. The battery grade lithium carbonate purification device of claim 1, wherein: one end of the feeding pipe (4) far away from the reaction kettle (1) penetrates through and extends to the interior of the grinding box (5), and the rear end of the grinding barrel (8) penetrates through and extends to the outer side of the grinding box (5).
3. The battery grade lithium carbonate purification device of claim 1, wherein: the deslagging box (12) is a stainless steel cuboid which is hollow inside and is missing on the front side, and the size of the inner space of the deslagging box (12) is matched with that of the filter plate (14).
4. The battery grade lithium carbonate purification device of claim 1, wherein: the fastening block (13) is composed of an L-shaped rod, a pressing sheet and a screw rod, the pressing sheet is fixedly connected to the top of the L-shaped rod, and the screw rod is connected to the inner threads of the pressing sheet.
5. The battery grade lithium carbonate purification device of claim 1, wherein: the filter plate (14) comprises square frame and gauze, the inside fixedly connected with gauze of square frame, the one end that slagging-off case (12) was kept away from in liquid sending pipe (16) runs through reation kettle (1) and purification case (17) and extends to the inside of purification case (17).
6. The battery grade lithium carbonate purification device of claim 1, wherein: the stirring device (24) is composed of a driving wheel, a rotating shaft and stirring blades, the bottom of the driving wheel is fixedly connected with the rotating shaft, the outer side of the rotating shaft is fixedly connected with the stirring blades, and the number of the stirring blades is not less than two and is uniformly distributed on the outer side of the rotating shaft.
7. The battery grade lithium carbonate purification device of claim 1, wherein: the number of the compression springs (28) is not less than two and the compression springs are the same in size, and the compression springs (28) are evenly distributed on the left side of the inner wall of the filter pipe (27).
8. The battery grade lithium carbonate purification device of claim 1, wherein: one end of the liquid return pipe (32) far away from the filter pipe (27) penetrates through the purification box (17) and the reaction kettle (1) and extends to the inside of the reaction kettle (1).
9. A purification method of battery-grade lithium carbonate is characterized by comprising the following steps:
1) turning on a first motor (9), driving a grinding cylinder (8) to rotate, then putting the calcined carbonate type lithium source into a feed hopper (7), and grinding and crushing the calcined carbonate type lithium source by the grinding cylinder (8) to obtain the carbonate type lithium source with the particle size of less than eighty microns;
2) feeding the carbonate type lithium source with the particle size of less than eighty microns obtained in the step 1) into a reaction kettle (1) through a feeding pipe (4), feeding pure water into the reaction kettle (1) through a second pure water pipe (21), and feeding carbon dioxide gas through an air inlet pipe (3) until the pH value of the liquid is 7.0-8.5, so as to obtain a hydrogenation liquid;
3) adding a precipitator into the hydrogenated liquid obtained in the step 2) from a feeding pipe (2) on the front surface of the reaction kettle (1), separating out impurities, then opening a first electromagnetic liquid discharge valve (11), allowing the hydrogenated liquid and the impurities to enter a deslagging box (12), and then performing solid-liquid separation through a filter plate (14) to obtain pure hydrogenated liquid;
4) feeding the pure hydrogenated liquid obtained in the step 3) into a purification box (17) through a liquid feeding pipe (16), heating the pure hydrogenated liquid through a heating pipe (26), stirring the pure hydrogenated liquid through a stirring device (24) until lithium carbonate is completely precipitated, opening a third liquid discharging pipe (33), filtering the pure hydrogenated liquid through a filtering pipe (27), keeping a solid in the purification box (17), and discharging the liquid through a liquid returning pipe (32) to obtain a crude lithium carbonate product;
5) adding pure water into the lithium carbonate crude product obtained in the step 4), stirring by using a stirring device (24), washing the lithium carbonate crude product, and then discharging liquid to obtain a lithium carbonate wet refined product;
6) and (3) stirring the wet refined lithium carbonate obtained in the step 5) through a stirring device (24) and a heating pipe (26) for heating, and drying the wet refined lithium carbonate to obtain the battery-grade lithium carbonate.
Technical Field
The invention relates to the technical field of lithium carbonate production, in particular to a purification method and a purification device for battery-grade lithium carbonate.
Background
Lithium carbonate is used as the most important basic lithium salt, is widely applied in important industrial fields such as batteries, smelting, lubricants, glass and the like, along with the gradual exhaustion of global petroleum resources, lithium batteries are more and more concerned in research and development and application as new energy, and the high-purity lithium carbonate is a key raw material for producing positive electrode materials of lithium batteries, and the demand for the lithium carbonate is gradually increased year by year.
For example, the present invention in chinese patent CN 102583453B provides an industrial process for producing battery grade lithium carbonate or high purity lithium carbonate, which comprises the steps of, (i) carbonizing, taking a carbonate type lithium source, wherein the content of Li2O is 5.0-40.3% w/w, placing the lithium carbonate in a hydrogenation reaction kettle for carbonization treatment for one or more times to obtain a lithium carbonate wet refined product, drying the lithium carbonate wet refined product obtained by the primary carbonization treatment, obtaining battery-grade lithium carbonate, drying the lithium carbonate fine wet product obtained by more than two times of carbonization treatment, the method provided by the invention can continuously produce the battery-grade lithium carbonate and the high-purity lithium carbonate on a large scale, has low energy consumption, is environment-friendly, has strong practical value, however, in this method, when solid-liquid separation is performed, the filter screen is easily clogged, and there is a disadvantage that clogging cannot be prevented, which affects production efficiency.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a purification method and a purification device for battery-grade lithium carbonate, which have the advantages of blockage prevention and the like, and solve the problems that when the existing purification method and purification device for battery-grade lithium carbonate are used for carrying out solid-liquid separation, a filter screen is easy to block, the defect that the blockage cannot be prevented exists, and the production efficiency is influenced.
(II) technical scheme
In order to achieve the purpose of preventing blockage, the invention provides the following technical scheme: the utility model provides a battery level lithium carbonate purification device, includes reation kettle, reation kettle's positive fixedly connected with filling tube, reation kettle's left side fixedly connected with intake pipe, reation kettle's left side and the bottom fixedly connected with conveying pipe that is located the intake pipe, the left side fixedly connected with of conveying pipe pulverizes the case, pulverize the bottom of case and be located reation kettle's back fixedly connected with rack, pulverize the top fixedly connected with feeder hopper of case, the inside swing joint that pulverizes the case has a section of thick bamboo of grinding, the first motor of inside fixedly connected with of rack, the output of first motor has a section of thick bamboo of grinding through belt swing joint, reation kettle's interior diapire fixedly connected with drain pipe.
The utility model discloses a purification device, including drain pipe, the first electromagnetism flowing back valve of outside fixedly connected with of drain pipe, the bottom fixedly connected with slagging-off case of drain pipe, the equal threaded connection in the left and right sides at slagging-off roof portion has the grip, the inside of slagging-off case has the filter plate through grip swing joint, the positive fixedly connected with pull block of filter plate, the bottom fixedly connected with liquid delivery pipe of slagging-off case, the right-hand member of liquid delivery pipe just is located the top fixedly connected with purification case of rack, the first pure water pipe of top fixedly connected with of purification case, the top of purification case just is located the left side fixedly connected with collecting pipe of first pure water pipe, the left side fixedly connected with condenser of collecting pipe.
The left ends of the collecting pipe and the condenser are fixedly connected with a second pure water pipe, the outer sides of the second pure water pipe, the collecting pipe and the first pure water pipe are fixedly connected with a second electromagnetic liquid discharge valve, the right side of the inner wall of the purifying box is fixedly connected with a fixed block, the bottom of the fixed block is movably connected with a stirring device, the right side of the purifying box is fixedly connected with a second motor, the output shaft of the second motor is movably connected with a stirring device through a belt, the right side of the inner wall of the purifying box is fixedly connected with a heating pipe at the bottom of the fixed block, the inner bottom wall of the purifying box is fixedly connected with a filter pipe, the left side of the inner wall of the filter pipe is fixedly connected with a compression spring, the right side of the compression spring is fixedly connected with a movable frame, the inner part of the movable frame is fixedly connected with a, the bottom fixedly connected with of filter tube returns the liquid pipe, the outside fixedly connected with third electromagnetism flowing back valve of returning the liquid pipe, the left end fixedly connected with reation kettle of returning the liquid pipe.
Preferably, one end of the feed pipe, which is far away from the reaction kettle, penetrates through and extends to the interior of the grinding box, and the rear end of the grinding drum penetrates through and extends to the outer side of the grinding box.
Preferably, the deslagging box is a hollow stainless steel cuboid with a missing front surface, and the size of the inner space of the deslagging box is matched with that of the filter plate.
Preferably, the fastening block consists of an L-shaped rod, a pressing sheet and a screw rod, the pressing sheet is fixedly connected to the top of the L-shaped rod, and the screw rod is connected to the inner thread of the pressing sheet.
Preferably, the filter plate comprises square frame and gauze, the inside fixedly connected with gauze of square frame, the one end that the slagging-off case was kept away from to the liquid sending pipe runs through reation kettle and purification case and extends to the inside of purification case.
Preferably, the stirring device consists of a driving wheel, a rotating shaft and stirring blades, the bottom of the driving wheel is fixedly connected with the rotating shaft, the outer side of the rotating shaft is fixedly connected with the stirring blades, and the number of the stirring blades is not less than two and is uniformly distributed on the outer side of the rotating shaft.
Preferably, the number of the compression springs is not less than two and the compression springs are the same in size, and the compression springs are uniformly distributed on the left side of the inner wall of the filter pipe.
Preferably, one end of the liquid return pipe, which is far away from the filter pipe, penetrates through the purification box and the reaction kettle and extends to the interior of the reaction kettle.
Another technical problem to be solved by the invention is a battery-grade lithium carbonate purification method, which comprises the following steps:
1) turning on a first motor to drive a rolling cylinder to rotate, then putting the calcined carbonate type lithium source into a feed hopper, and rolling and crushing the calcined carbonate type lithium source by the rolling cylinder to obtain the carbonate type lithium source with the particle size of less than eighty microns;
2) feeding the carbonate type lithium source with the particle size of less than eighty microns obtained in the step 1) into a reaction kettle through a feeding pipe, feeding pure water into the reaction kettle through a second pure water pipe, and feeding carbon dioxide gas through an air inlet pipe until the pH value of the liquid is 7.0-8.5, so as to obtain hydrogenated liquid;
3) adding a precipitator into the hydrogenated liquid obtained in the step 2) from a feeding pipe on the front surface of the reaction kettle to separate out impurities, then opening a first electromagnetic liquid discharge valve, allowing the hydrogenated liquid and the impurities to enter a deslagging box, and then performing solid-liquid separation through a filter plate to obtain pure hydrogenated liquid;
4) feeding the pure hydrogenated liquid obtained in the step 3) into a purification box through a liquid feeding pipe, heating the pure hydrogenated liquid by a heating pipe, stirring by a stirring device until lithium carbonate is completely precipitated, opening a third liquid discharge pipe, filtering by a filter pipe, keeping the solid in the purification box, and discharging the liquid through a liquid return pipe to obtain a crude lithium carbonate product;
5) adding pure water into the lithium carbonate crude product obtained in the step 4), stirring by using a stirring device, washing the lithium carbonate crude product, and then discharging liquid to obtain a lithium carbonate wet refined product;
6) and 5) stirring the wet refined lithium carbonate obtained in the step 5) by a stirring device and a heating pipe for heating, and drying the wet refined lithium carbonate to obtain the battery-grade lithium carbonate.
(III) advantageous effects
Compared with the prior art, the invention provides a purification method and a purification device for battery-grade lithium carbonate, which have the following beneficial effects:
1. this battery level lithium carbonate purification method and purification device, use through vibrating motor, vibrating motor's output shaft drives the internal vibration of movable frame at the filter tube, the movable frame drives the filter screen vibration, avoid the solid to block up the filter screen, influence solid-liquid separation's efficiency, use through compression spring, when the movable frame receives the vibration, compression spring is compressed, produce elastic deformation, avoid movable frame and filter tube direct contact, the noise produces, use through the grip block, when needs take out impurity from the inside of slagging-off case, the inside screw rod of knob grip block can be taken out the filter plate from the inside of slagging-off case, thereby take out impurity, be convenient for change the filter plate simultaneously, avoid blockking up, the mesh of preventing blockking up has been realized, the work efficiency is improved, and the use is facilitated.
2. This battery level lithium carbonate purification method and purification device, through first electromagnetism flowing back valve, the cooperation of second electromagnetism flowing back valve and third electromagnetism flowing back valve is used, utilize liquid discharge and the transport in the electric signal control device, convenient and fast, through the use of returning the liquid pipe, retrieve liquid to reation kettle's inside, recycle, cooperation through collecting pipe and condenser is used, the vapor that produces when will drying carries out the condensation and retrieves, and send into reation kettle's inside through second pure water pipe, carry out cyclic utilization with the liquid of purification in-process, reduce the waste of resource, energy-conserving purpose has been realized.
Drawings
Fig. 1 is a schematic structural diagram of a battery-grade lithium carbonate purification method and purification apparatus according to the present invention;
fig. 2 is an enlarged view of a point a in fig. 1 of a battery-grade lithium carbonate purification method and purification apparatus according to the present invention;
fig. 3 is an enlarged view of B in fig. 1 of a method and an apparatus for purifying battery-grade lithium carbonate according to the present invention.
In the figure: 1 reaction kettle, 2 feed pipes, 3 air inlet pipes, 4 feed pipes, 5 crushing boxes, 6 placing racks, 7 feed hoppers, 8 crushing cylinders, 9 first motors, 10 liquid outlet pipes, 11 first electromagnetic liquid discharge valves, 12 deslagging boxes, 13 fastening blocks, 14 filter plates, 15 pulling blocks, 16 liquid feeding pipes, 17 purifying boxes, 18 first pure water pipes, 19 collecting pipes, 20 condensers, 21 second pure water pipes, 22 second electromagnetic liquid discharge valves, 23 fixing blocks, 24 stirring devices, 25 second motors, 26 heating pipes, 27 filtering pipes, 28 compression springs, 29 movable racks, 30 filter screens, 31 vibrating motors, 32 liquid return pipes and 33 third electromagnetic liquid discharge valves.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious 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. 1-3, a battery-grade lithium carbonate purification device comprises a reaction kettle 1, a
The outer side of the
The left ends of the
Another technical problem to be solved by the invention is a battery-grade lithium carbonate purification method, which comprises the following steps:
1) turning on a
2) feeding the carbonate type lithium source with the particle size of less than eighty microns obtained in the step 1) into a reaction kettle 1 through a feeding pipe 4, feeding pure water into the reaction kettle 1 through a second
3) adding a precipitator into the hydrogenated liquid obtained in the step 2) from a
4) feeding the pure hydrogenated liquid obtained in the step 3) into the
5) adding pure water into the lithium carbonate crude product obtained in the step 4), stirring by using a
6) and (3) stirring and heating the wet refined lithium carbonate obtained in the step 5) through a
When using, the output shaft that leads to vibrating
In summary, according to the battery-grade lithium carbonate purification method and purification device, through the use of the
And through the cooperation use of first electromagnetism flowing back
It is to be noted that the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
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