Preparation method of special tetrabasic lead sulfate for lead storage battery

Abstract

The invention discloses a preparation method of special tetrabasic lead sulfate for a lead storage battery, and relates to the technical field of lead storage battery production.The preparation method comprises a reaction mechanism, a spiral feeding device is arranged at one end of the reaction mechanism, a discharging mechanism is arranged at one end of the top of the reaction mechanism, and a mixing mechanism is arranged on the inner side of the reaction mechanism; the discharging mechanism comprises a discharging hopper, the discharging hopper is installed at the top of the dilute sulfuric acid feeding pipe, a protruding shaft is rotatably installed at the top of the inner side of the discharging hopper, a movable rod is installed on the outer side of the protruding position of the protruding shaft, and a piston is installed at the bottom of the movable rod. A movable rod can be driven to move up and down through rotation of a convex shaft, then a piston can be driven to adjust the size of an opening of a dilute sulphuric acid feeding pipe, the feeding amount of dilute sulphuric acid can be conveniently controlled, lead oxide, pure water and dilute sulphuric acid can be fully mixed and reacted through a mixing mechanism, and the reaction efficiency is improved. And the production efficiency of the tetrabasic lead sulfate can be improved.

Description

Technical Field

[0001] The invention relates to the technical field of lead-acid battery production, and in particular to a method for preparing tetrabasic lead sulfate special for lead-acid batteries. Background Art

[0002] Lead-acid battery is a kind of battery that converts chemical energy into electrical energy and belongs to DC power supply. It is composed of one or more battery cells and is usually used in electric vehicles, UPS and other fields. In the production of lead-acid batteries, in order to extend the cycle life of the battery, one of the most effective measures is usually to use lead paste with high content of tetrabasic lead sulfate, which can be obtained by high temperature and paste or high temperature curing. The preparation methods of tetrabasic lead sulfate mainly include liquid phase method, ball milling method, hydrothermal synthesis method, thermal decomposition method and sintering method. These methods have their own advantages and disadvantages and are suitable for different production needs and conditions. When preparing tetrabasic lead sulfate by ball milling method, lead oxide, pure water and dilute sulfuric acid need to be put into the reactor to react to obtain a mixed solution of tetrabasic lead sulfate.

[0003] The prior art has the following deficiencies: in the preparation process of the prior tetrabasic lead sulfate, the feeding amount of the dilute sulfuric acid cannot be conveniently controlled, so that the dilute sulfuric acid, pure water and lead oxide cannot be fully mixed, and the raw materials are easily adhered to the inner wall of the reactor, and the reaction cannot be fully carried out, which affects the production efficiency of the tetrabasic lead sulfate. Summary of the invention

[0004] The purpose of the present invention is to provide a preparation method of tetrabasic lead sulfate for lead-acid batteries, wherein the rotation of a convex shaft can drive a movable rod to move up and down, and the piston can be driven to adjust the opening size of a dilute sulfuric acid feeding pipe, so that the feeding amount of the dilute sulfuric acid can be conveniently controlled, and the lead oxide, pure water and dilute sulfuric acid can be fully mixed and reacted through a mixing mechanism, so that the production efficiency of the tetrabasic lead sulfate can be improved, so as to solve the above-mentioned shortcomings in the technology.

[0005] In order to achieve the above object, the present invention provides the following technical solution: a method for preparing tetrabasic lead sulfate for lead-acid batteries, comprising the following steps:

[0006] S1, using a ball mill to grind the lead block to obtain refined lead powder;

[0007] S2, conveying the ground refined lead powder into a rotary kiln, and further converting the free lead into lead oxide by heating and oxidation;

[0008] S3, transporting the lead oxide to a reaction device, and reacting the lead oxide with pure water and dilute sulfuric acid through the reaction device to obtain a mixed solution of tetrabasic lead sulfate;

[0009] S4. The reacted solution is transported to a centrifugal device, and the solid-liquid separation is performed by centrifugation to obtain a wet blocky white solid;

[0010] S5, putting the blocky white solid into a drying oven for drying to obtain a blocky tetrabasic lead sulfate solid;

[0011] S6. Putting the blocky tetrabasic lead sulfate solid into a pulverizer for grinding and pulverizing to obtain tetrabasic lead sulfate for lead-acid batteries.

[0012] Preferably, in S3, a tetrabasic lead sulfate mixed solution is obtained by a reaction device, wherein the reaction device comprises a reaction mechanism, a spiral feeding device is provided at one end of the reaction mechanism, a feeding mechanism is provided at one end of the top of the reaction mechanism, and a mixing mechanism is provided inside the reaction mechanism;

[0013] The reaction mechanism comprises a reactor body, a lead oxide feed pipe is fixedly installed on the top of one end of the reactor body, the lead oxide feed pipe is connected with the discharge port of the spiral feed device, a cover plate is movably installed on the top of the reactor body, a pure water feed pipe is fixedly installed on the inner wall of one end of the cover plate, and a dilute sulfuric acid feed pipe is fixedly installed on the inner wall of the other end of the cover plate;

[0014] The feeding mechanism includes a feeding hopper, which is fixedly installed on the top of the dilute sulfuric acid feed pipe. A cam is rotatably installed on the top of the inner side of the feeding hopper. A first motor is provided on one side of the cam. A movable rod is rotatably installed on the outer side of the protruding position of the cam. A piston is rotatably installed on the bottom of the movable rod, and the outer wall of the piston is movably connected to the inner wall of the dilute sulfuric acid feed pipe.

[0015] Preferably, the reaction device further comprises a support frame, one end of the top of the support frame is movably connected to the outer wall of the bottom of the reactor body, and the other end of the top of the support frame is movably connected to the outer wall of the spiral feeding device.

[0016] Preferably, a discharge pipe is fixedly installed on the bottom of the outer wall of one end of the reactor body away from the lead oxide feed pipe, and a waste discharge pipe is fixedly installed on the inner wall at the bottom of the reactor body.

[0017] Preferably, the mixing mechanism includes a rotating shaft, which is rotatably installed in the middle position of the inner wall of the cover plate, and a second motor is arranged on the top of the rotating shaft. The outer sides of the top and bottom of the rotating shaft are fixedly sleeved with mounting plates, and three cleaning plates are fixedly installed on the outer sides of two of the mounting plates, and the outer walls of the three cleaning plates are movably connected to the inner wall of the reactor body.

[0018] Preferably, three mounting rods are rotatably mounted between the two mounting plates, a plurality of stirring rods are fixedly sleeved on the outer sides of the mounting rods, and the diameter of the stirring rods is smaller than the distance between the outer wall of the rotating shaft and the inner side of the cleaning plate.

[0019] Preferably, a blanking plate is fixedly sleeved on the outer side of the top of the rotating shaft, and the blanking plate is arranged on the top of the mounting plate at the top, and a plurality of holes for blanking are opened on the inner wall of the bottom of the blanking plate.

[0020] Preferably, the middle position of the top of the cover plate is fixedly connected to the second motor, and the second motor is transmission-connected to the top of the rotating shaft via an output shaft.

[0021] Preferably, the top of the outer wall on one side of the lower hopper is fixedly connected to the first motor, the first motor is connected to the cam shaft through an output shaft transmission, and the rotation radius of the cam shaft is smaller than the radius of the top of the lower hopper.

[0022] In the above technical solution, the technical effects and advantages provided by the present invention are:

[0023] 1. The spiral feeding device is provided so that the lead oxide treated by the rotary kiln can be conveniently fed into the reactor body, which is beneficial to the feeding of the lead oxide. At the same time, the cam shaft is rotated by the operation of the first motor, and the piston is driven to move by the traction of the movable rod, so that the opening and closing of the dilute sulfuric acid feeding pipe can be conveniently adjusted, and the feeding amount of the dilute sulfuric acid can be conveniently controlled, so that the situation of excessive addition at one time can be avoided, and the stable preparation reaction of tetrabasic lead sulfate can be ensured;

[0024] 2. The lead oxide, pure water and dilute sulfuric acid entering the reactor body can be evenly sprayed by the rotation of the unloading plate, so that the lead oxide, pure water and dilute sulfuric acid can be evenly distributed inside the reactor body, and then the lead oxide, pure water and dilute sulfuric acid can be fully stirred and mixed by the rotation of the three mounting rods and the multiple stirring rods, which can effectively improve the generation efficiency of tetrabasic lead sulfate;

[0025] 3. The rotation of the rotating shaft can drive the mounting plate and the cleaning plate to rotate. The rotation of the cleaning plate can clean the inner wall of the reactor body, which can prevent lead oxide, pure water or dilute sulfuric acid from adhering to the inner wall of the reactor body, so that the raw materials can be fully mixed. At the same time, the setting of the waste pipe can facilitate the subsequent cleaning of the reactor body by the staff, which can effectively ensure the cleanliness of the inside of the reactor body. BRIEF DESCRIPTION OF THE DRAWINGS

[0026] In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings required for use in the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments recorded in the present invention. For ordinary technicians in this field, other drawings can also be obtained based on these drawings.

[0027] Figure 1The figure is a flow chart of the steps of the preparation method of the present invention.

[0028] Figure 2 It is the overall structural diagram of the reaction device of the present invention.

[0029] Figure 3 It is a front vertical sectional view of the reaction device of the present invention.

[0030] Figure 4 It is an exploded view of the three-dimensional structure of the reaction mechanism of the present invention.

[0031] Figure 5 It is an exploded view of the three-dimensional structure of the blanking mechanism of the present invention.

[0032] Figure 6 It is an exploded view of the three-dimensional structure of the mixing mechanism of the present invention.

[0033] Description of reference numerals:

[0034] 1. Support frame;

[0035] 2. Reaction mechanism; 201. Reactor body; 202. Lead oxide feed pipe; 203. Discharge pipe; 204. Waste discharge pipe; 205. Cover plate; 206. Pure water feed pipe; 207. Dilute sulfuric acid feed pipe;

[0036] 3. Screw feeding device;

[0037] 4. Feeding mechanism; 401. Feeding hopper; 402. Cam shaft; 403. First motor; 404. Movable rod; 405. Piston;

[0038] 5. Mixing mechanism; 501. Rotating shaft; 502. Second motor; 503. Unloading plate; 504. Mounting plate; 505. Cleaning plate; 506. Mounting rod; 507. Stirring rod. DETAILED DESCRIPTION

[0039] The present invention provides Figure 1 The method for preparing tetrabasic lead sulfate for lead-acid batteries shown in the figure comprises the following steps:

[0040] S1, using a ball mill to grind the lead block to obtain refined lead powder;

[0041] S2, conveying the ground refined lead powder into a rotary kiln, and further converting the free lead into lead oxide by heating and oxidation;

[0042] S3, transporting the lead oxide to a reaction device, and reacting the lead oxide with pure water and dilute sulfuric acid through the reaction device to obtain a mixed solution of tetrabasic lead sulfate;

[0043] S4. The reacted solution is transported to a centrifugal device, and the solid-liquid separation is performed by centrifugation to obtain a wet blocky white solid;

[0044] S5, putting the blocky white solid into a drying oven for drying to obtain a blocky tetrabasic lead sulfate solid;

[0045] S6. Putting the blocky tetrabasic lead sulfate solid into a pulverizer for grinding and pulverizing to obtain tetrabasic lead sulfate for lead-acid batteries.

[0046] In order to conveniently prepare tetrabasic lead sulfate, Figure 2 As shown, in S3, a tetrabasic lead sulfate mixed solution is obtained by a reaction device, and the reaction device includes a reaction mechanism 2, a spiral feeding device 3 is arranged at one end of the reaction mechanism 2, a feeding mechanism 4 is arranged at one end of the top of the reaction mechanism 2, and a mixing mechanism 5 is arranged inside the reaction mechanism 2.

[0047] In order to facilitate the addition of materials to the reactor body 201, Figure 2-4 As shown, the reaction mechanism 2 includes a reactor body 201, a lead oxide feed pipe 202 is fixedly installed on the top of one end of the reactor body 201, the lead oxide feed pipe 202 is connected to the discharge port of the spiral feeding device 3, a cover plate 205 is movably installed on the top of the reactor body 201, a pure water feed pipe 206 is fixedly installed on the inner wall of one end of the cover plate 205, and a dilute sulfuric acid feed pipe 207 is fixedly installed on the inner wall of the other end of the cover plate 205. Lead oxide raw materials can be added to the reactor body 201 through the spiral feeding device 3 and the lead oxide feed pipe 202, and pure water and dilute sulfuric acid can be added to the reactor body 201 through the pure water feed pipe 206 and the dilute sulfuric acid feed pipe 207.

[0048] In order to conveniently control the feed amount of dilute sulfuric acid, Figure 2-3 and Figure 5 As shown, the unloading mechanism 4 includes a unloading hopper 401, which is fixedly installed on the top of the dilute sulfuric acid feed pipe 207. A convex shaft 402 is rotatably installed on the inner top of the unloading hopper 401. A first motor 403 is arranged on one side of the convex shaft 402. A movable rod 404 is rotatably installed on the outer side of the protruding position of the convex shaft 402. A piston 405 is rotatably installed on the bottom of the movable rod 404. The outer wall of the piston 405 is movably connected to the inner wall of the dilute sulfuric acid feed pipe 207. The rotation of the convex shaft 402 can drive the piston 405 to move up and down under the traction of the movable rod 404, thereby controlling the opening of the dilute sulfuric acid feed pipe 207.

[0049] In order to keep the device stable during operation, Figure 2-4As shown, the reaction device also includes a support frame 1, one end of the top of the support frame 1 is movably connected to the bottom outer wall of the reactor body 201, and the other end of the top of the support frame 1 is movably connected to the outer wall of the spiral feeding device 3. The reaction mechanism 2 and the spiral feeding device 3 can be supported and fixed by the support frame 1, so that the device remains stable during operation.

[0050] In order to conveniently discharge the tetrabasic lead sulfate mixed solution, Figure 2-4 As shown, a discharge pipe 203 is fixedly installed at the bottom of the outer wall of one end of the reactor body 201 away from the lead oxide feeding pipe 202, and a waste pipe 204 is fixedly installed on the inner wall at the bottom of the reactor body 201. The tetrabasic lead sulfate mixed solution generated by the reaction can be discharged through the discharge pipe 203, and the waste liquid generated during the cleaning process of the reactor body 201 can be discharged through the waste pipe 204.

[0051] In order to prevent the raw materials from adhering to the inner wall of the reactor body 201, Figure 2-3 and Figure 6 As shown, the mixing mechanism 5 includes a rotating shaft 501, which is rotatably installed in the middle position of the inner wall of the cover plate 205, and a second motor 502 is arranged on the top of the rotating shaft 501. The outer sides of the top and bottom of the rotating shaft 501 are fixedly sleeved with mounting plates 504, and three cleaning plates 505 are fixedly installed on the outer sides of the two mounting plates 504. The outer walls of the three cleaning plates 505 are movably connected to the inner wall of the reactor body 201. The cleaning plates 505 can rotate to clean the inner wall of the reactor body 201, so as to prevent lead oxide, pure water or dilute sulfuric acid from adhering to the inner wall of the reactor body 201.

[0052] In order to make lead oxide, pure water and dilute sulfuric acid fully mixed, Figure 2-3 and Figure 6 As shown, three mounting rods 506 are rotatably mounted between the two mounting plates 504, and a plurality of stirring rods 507 are fixedly sleeved on the outer sides of the mounting rods 506. The diameter of the stirring rods 507 is smaller than the distance between the outer wall of the rotating shaft 501 and the inner side of the cleaning plate 505. A discharge plate 503 is fixedly sleeved on the outer side of the top of the rotating shaft 501. The discharge plate 503 is arranged on the top of the mounting plate 504 at the top, and a plurality of holes for discharge are provided on the bottom inner wall of the discharge plate 503. The raw materials can be evenly added to the interior of the reactor body 201 through the discharge plate 503, and the raw materials can be fully stirred and mixed through the three mounting rods 506 and the plurality of stirring rods 507, thereby improving the reaction efficiency of tetrabasic lead sulfate.

[0053] In order to provide power for the operation of the mixing mechanism 5, as Figure 3As shown, the middle position at the top of the cover plate 205 is fixedly connected to the second motor 502, and the second motor 502 is connected to the top of the rotating shaft 501 through an output shaft transmission. The cover plate 205 can install and fix the second motor 502. The operation of the second motor 502 causes the rotating shaft 501 to rotate, thereby allowing the mixing mechanism 5 to stably mix the raw materials.

[0054] In order to provide power for the movement of piston 405, as Figure 3 and Figure 5 As shown, the top of the outer wall on one side of the lower hopper 401 is fixedly connected to the first motor 403, and the first motor 403 is connected to the cam shaft 402 through an output shaft transmission. The rotation radius of the cam shaft 402 is smaller than the radius of the top of the lower hopper 401. The lower hopper 401 can install and fix the first motor 403. The first motor 403 drives the cam shaft 402 to rotate, and then can drive the piston 405 to move up and down under the traction of the movable rod 404.

[0055] The specific implementation method is as follows: the lead oxide processed by the ball mill and the rotary kiln is transported to the feed port of the spiral feed device 3, and then the lead oxide can be added to the reactor body 201 from the lead oxide feed pipe 202 through the operation of the spiral feed device 3, and pure water can be added to the reactor body 201 through the pure water feed pipe 206, and dilute sulfuric acid can be transported to the lower hopper 401 and stored, and the convex shaft 402 can be driven to rotate by the operation of the first motor 403, and then the movable rod 404 can be driven to move up and down. The movable rod 404 can be pulled to drive the piston 405 to move up and down, thereby adjusting the opening and closing of the dilute sulfuric acid feeding pipe 207, and conveniently controlling the amount of dilute sulfuric acid entering the reactor body 201. At the same time, the second motor 502 works to rotate the rotating shaft 501, thereby driving the unloading plate 503 to rotate, so that the lead oxide, pure water and dilute sulfuric acid falling into the unloading plate 503 can be evenly added to the reactor body 201 through the rotation of the unloading plate 503. When the rotating shaft 501 rotates, the two mounting plates 504 can be driven to rotate. Since the mounting rod 506 is rotatably connected to the mounting plate 504, the mounting rod 506 rotates itself as the mounting plate 504 rotates, so that the plurality of stirring rods 507 can fully stir and mix the lead oxide, pure water and dilute sulfuric acid, so that the raw materials are mixed more fully. At the same time, the rotation of the mounting plate 504 can drive the cleaning plate 505 to rotate, so that it can clean the inner wall of the reactor body 201, and can prevent the lead oxide, pure water or dilute sulfuric acid from adhering to the inner wall of the reactor body 201, so that the raw materials are mixed more fully. The tetrabasic lead sulfate mixed solution obtained after the reaction can be transported from the inside of the reactor body 201 to the centrifugal device through the discharge pipe 203, and tetrabasic lead sulfate for lead-acid batteries can be obtained by centrifugation, drying and crushing. This embodiment specifically solves the problem that the amount of dilute sulfuric acid discharged in the prior art cannot be conveniently controlled, so that the lead oxide, pure water and dilute sulfuric acid cannot be fully mixed, which affects the reaction efficiency of the tetrabasic lead sulfate.

[0056] The above description is only by way of illustration of certain exemplary embodiments of the present invention. It is undoubted that those skilled in the art can modify the described embodiments in various ways without departing from the spirit and scope of the present invention. Therefore, the above drawings and descriptions are illustrative in nature and should not be construed as limiting the scope of protection of the claims of the present invention.

Claims

1. A method for preparing tetrabasic lead sulfate for lead-acid batteries, It is characterized in that The following steps are involved: S1, using a ball mill to grind the lead block to obtain refined lead powder; S2, conveying the ground refined lead powder into a rotary kiln, and further converting the free lead into lead oxide by heating and oxidation; S3, transporting the lead oxide to a reaction device, and reacting the lead oxide with pure water and dilute sulfuric acid through the reaction device to obtain a mixed solution of tetrabasic lead sulfate; S4. The reacted solution is transported to a centrifugal device, and the solid-liquid separation is performed by centrifugation to obtain a wet blocky white solid; S5, putting the blocky white solid into a drying oven for drying to obtain a blocky tetrabasic lead sulfate solid; S6. Putting the blocky tetrabasic lead sulfate solid into a pulverizer for grinding and pulverizing to obtain tetrabasic lead sulfate for lead-acid batteries.

2. A method for preparing tetrabasic lead sulfate for lead-acid batteries according to claim 1, Features: In S3, a tetrabasic lead sulfate mixed solution is obtained by a reaction device, wherein the reaction device comprises a reaction mechanism (2), a screw feeding device (3) is arranged at one end of the reaction mechanism (2), a feeding mechanism (4) is arranged at one end of the top of the reaction mechanism (2), and a mixing mechanism (5) is arranged inside the reaction mechanism (2); The reaction mechanism (2) comprises a reactor body (201), a lead oxide feed pipe (202) is fixedly mounted on the top of one end of the reactor body (201), the lead oxide feed pipe (202) is connected to the discharge port of the spiral feed device (3), a cover plate (205) is movably mounted on the top of the reactor body (201), a pure water feed pipe (206) is fixedly mounted on the inner wall of one end of the cover plate (205), and a dilute sulfuric acid feed pipe (207) is fixedly mounted on the inner wall of the other end of the cover plate (205); The feeding mechanism (4) comprises a feeding hopper (401), wherein the feeding hopper (401) is fixedly mounted on the top of the dilute sulfuric acid feed pipe (207), a convex shaft (402) is rotatably mounted on the top of the inner side of the feeding hopper (401), a first motor (403) is arranged on one side of the convex shaft (402), a movable rod (404) is rotatably mounted on the outer side of the protruding position of the convex shaft (402), a piston (405) is rotatably mounted on the bottom of the movable rod (404), and the outer wall of the piston (405) is movably connected to the inner wall of the dilute sulfuric acid feed pipe (207).

3. The method for preparing tetrabasic lead sulfate for lead-acid batteries according to claim 2, Features: The reaction device further comprises a support frame (1), one end of the top of the support frame (1) being movably connected to the bottom outer wall of the reaction kettle body (201), and the other end of the top of the support frame (1) being movably connected to the outer wall of the spiral feeding device (3).

4. The method for preparing tetrabasic lead sulfate for lead-acid batteries according to claim 2, Features: A discharge pipe (203) is fixedly installed on the bottom of the outer wall of one end of the reactor body (201) away from the lead oxide feed pipe (202), and a waste discharge pipe (204) is fixedly installed on the inner wall of the bottom of the reactor body (201).

5. The method for preparing tetrabasic lead sulfate for lead-acid batteries according to claim 2, Features: The mixing mechanism (5) comprises a rotating shaft (501), the rotating shaft (501) is rotatably mounted at the middle position of the inner wall of the cover plate (205), a second motor (502) is arranged at the top of the rotating shaft (501), mounting plates (504) are fixedly sleeved on the outer sides of the top and bottom of the rotating shaft (501), three cleaning plates (505) are fixedly mounted on the outer sides of the two mounting plates (504), and the outer walls of the three cleaning plates (505) are movably connected to the inner wall of the reactor body (201).

6. The method for preparing tetrabasic lead sulfate for lead-acid batteries according to claim 5, Features: Three mounting rods (506) are rotatably mounted between the two mounting plates (504), and a plurality of stirring rods (507) are fixedly sleeved on the outer sides of the mounting rods (506). The diameter of the stirring rods (507) is smaller than the distance between the outer wall of the rotating shaft (501) and the inner side of the cleaning plate (505).

7. The method for preparing tetrabasic lead sulfate for lead-acid batteries according to claim 5, Features: A blanking plate (503) is fixedly sleeved on the outer side of the top of the rotating shaft (501), and the blanking plate (503) is arranged on the top of the mounting plate (504) at the top. The inner wall of the bottom of the blanking plate (503) is provided with a plurality of holes for blanking.

8. The method for preparing tetrabasic lead sulfate for lead-acid batteries according to claim 5, Features: The middle position of the top of the cover plate (205) is fixedly connected to the second motor (502), and the second motor (502) is transmission-connected to the top of the rotating shaft (501) via an output shaft.

9. The method for preparing tetrabasic lead sulfate for lead-acid batteries according to claim 2, Features: The top of the outer wall on one side of the lower hopper (401) is fixedly connected to the first motor (403), and the first motor (403) is connected to the convex shaft (402) through an output shaft transmission, and the rotation radius of the convex shaft (402) is smaller than the radius of the top of the lower hopper (401).

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