Combined acid-base reaction device for lithium precipitation mother liquor in lithium carbonate preparation process
By designing a combined acid-base reaction device, two sequentially connected reaction tubes and cyclone internals are used to achieve full mixing of the mixed liquid and rapid adjustment of the pH value during the preparation of lithium carbonate, solving the problem that the traditional neutralization kettle cannot effectively control The problem of PH value improves production efficiency and safety.
Patent Information
- Application Number
- CN202411534260.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-10-31
- Publication Date
- 2025-01-21
AI Technical Summary
The traditional neutralization kettle cannot effectively control the pH value of the reaction mixture during the preparation of lithium carbonate, resulting in troublesome operation and low efficiency. It also requires additional liquid alkali to adjust the pH value, which increases the workload and production cost of the operator, which easily causes Process index fluctuations and evaporation equipment corrosion.
Design a combined acid-base reaction device, including two sequentially connected reaction tubes and cyclone internals. Through the setting of the cyclone internals, the mixed liquid is fully and rapidly mixed in the reaction tube, so that during the flow of the lithium precipitation mother liquor Complete the acid addition reaction and neutralization reaction, eliminate carbonate and lithium carbonate solid particles, and adjust the entry amount of acid and alkali liquid through a pH meter to quickly adjust the pH value of the mother liquor.
It achieves rapid and effective adjustment of the pH value of the reaction solution during the preparation of lithium carbonate, improves the efficiency of the reaction between lithium precipitation mother liquor and sulfuric acid, simplifies the operating process, reduces production costs, and reduces fluctuations in process indicators and evaporation equipment. corrosion risk.
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Figure CN119327405A_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the field of equipment, in particular to the technical field of chemical process equipment components, and specifically refers to a combined acid-base reaction device for lithium precipitation mother liquor in the process of lithium carbonate preparation. Background Art
[0002] During the preparation of battery-grade lithium carbonate, the lithium mother liquor in the lithium carbonate workshop needs to be neutralized with sulfuric acid to remove carbonate ions. The equipment to achieve this process is a neutralization kettle. The neutralization kettle is equipped with feeding valves and metering and detection devices for mother liquor and sulfuric acid. During normal production, the mother liquor feeding valve set on the neutralization kettle is opened to add lithium mother liquor, and the sulfuric acid feeding valve is opened later. The mother liquor and sulfuric acid undergo acid-base neutralization reaction. However, because the traditional method cannot implement the pH value of the reaction mixture, and the reaction is carried out in the neutralization kettle at the same time, the operation is cumbersome and inefficient. At the same time, since the mother liquor needs to further adjust the pH value, liquid alkali is also required, which will increase the workload of operators, reduce production efficiency, and easily cause fluctuations in the final process indicators, causing corrosion hazards to the evaporation equipment in the later process. Summary of the invention
[0003] In view of the deficiencies in the prior art, the present invention provides a combined acid-base reaction device for lithium precipitation mother liquor in the process of preparing lithium carbonate. Through two reaction tubes connected in sequence and the arrangement of cyclone internals, the mixed liquor is fully and quickly mixed and reacted in the reaction tube and in the process of descending, so that the lithium precipitation mother liquor completes the acid addition reaction and the neutralization reaction in the process of flowing downward, thereby eliminating carbonate ions and lithium carbonate solid particles, and facilitating the rapid adjustment of the final pH value of the mother liquor.
[0004] The present invention is achieved through the following technical scheme: a combined acid-base reaction device for lithium precipitation mother liquor in the process of preparing lithium carbonate, comprising two reaction tubes connected in sequence along the vertical direction, a cyclone internal part for breaking up the mixed liquid is arranged in the reaction tube, a liquid inlet pipe located above the cyclone internal part is connected to the side of the reaction tube, and a pH meter located below the cyclone internal part for measuring the mixed liquid is also arranged in the reaction tube. When the preferred solution is used, the lithium precipitation mother liquor is supplied at a constant flow rate through a centrifugal pump, and the lithium precipitation mother liquor enters the upper reaction tube from the liquid inlet of the reaction tube located above, and enters the upper reaction tube with the sulfuric acid from the sulfuric acid high-level tank through the liquid inlet pipe, and the lithium precipitation mother liquor and sulfuric acid contact and react in the reaction tube, and the mixed liquid of the lithium precipitation mother liquor and sulfuric acid is fully dispersed and mixed after passing through the cyclone internals, thereby eliminating carbonate and lithium carbonate solid particles, and the mother liquor reacts with sulfuric acid to become a reaction liquid, and the reaction liquid is measured when it flows through the pH meter. Since the flow rate of the lithium precipitation mother liquor is basically constant, the number of carbonate and lithium carbonate solid particles in the mother liquor varies. The process requires that the carbonate and lithium carbonate solid particles in the lithium precipitation mother liquor can be completely eliminated when the end pH value of the reaction liquid reaches the specified pH index, then the amount of sulfuric acid added during the reaction varies, so the pH value measured by the pH meter is used to adjust the amount of sulfuric acid entering, to ensure that the pH value of the reaction liquid reaches within the index range required by the process, and effectively improve the efficiency of the reaction between the lithium precipitation mother liquor and sulfuric acid; Next, the pH value of the reaction liquid needs to be further adjusted to meet the process requirements of the later stage. The reaction liquid and liquid alkali enter the reaction tube located below, and after being fully mixed and reacted by the cyclone internals, a neutralized liquid is formed. The pH value of the mother liquor is adjusted. The process requires that the pH value of the neutralized liquid must meet the specified pH index. Therefore, the pH value of the neutralized liquid is measured by a pH meter, and then the amount of liquid alkali entering is adjusted to ensure that the pH value of the neutralized liquid is within the index range required by the process. Through the two reaction tubes connected in sequence and the setting of the cyclone internal parts, the mixed liquid can be fully and quickly mixed and reacted in the reaction tube and during the circulation process, so that the lithium precipitation mother liquor can complete the acid addition reaction and the neutralization reaction during the flow process, thereby eliminating carbonate ions and lithium carbonate solid particles, and at the same time it is convenient to quickly adjust the pH value of the mother liquor and improve production efficiency.
[0005] Preferably, an intermediate tube is provided between the two reaction tubes, the liquid inlet of the intermediate tube is connected to the liquid outlet of the upper reaction tube, and the liquid outlet of the intermediate tube is connected to the liquid inlet of the lower reaction tube.
[0006] This preferred solution plays the role of connecting the two reaction tubes through the provision of the intermediate tube, thereby facilitating the connection of the two reaction tubes.
[0007] Preferably, the cyclone internal component comprises a plurality of spiral blades arranged vertically and connected in sequence, and the diameter of the blades is adapted to the inner diameter of the reaction tube.
[0008] When the preferred solution is in use, the three spiral blades are arranged to achieve full dispersion and mixing of the mixed liquid, thereby facilitating full reaction.
[0009] Preferably, a first flange is fixedly connected to the bottom end of the lowest blade, and the first flange is connected inside the reaction tube.
[0010] This preferred solution facilitates the fixation of the blades in the reaction tube by providing the first flange.
[0011] Preferably, plug-in grooves are provided on both end surfaces of the blades, and two adjacent blades are plug-connected via the two corresponding plug-in grooves.
[0012] The preferred solution plays a positioning role by providing the groove, thereby facilitating the sequential connection of a plurality of blades.
[0013] Preferably, between two adjacent blades, the bottom surface of the upper blade forms a certain angle with the bottom surface of the lower blade.
[0014] When the preferred embodiment is in use, after a plurality of blades form an angle, the mixed liquid is further broken up and mixed, thereby facilitating a full reaction.
[0015] Preferably, the reaction tube comprises a top pipe section, a middle pipe section, and a lower pipe section connected in sequence by flanges, the top pipe section is connected to the liquid inlet, the middle pipe section is provided with the blades, the detection end of the pH meter is inserted into the lower pipe section, and the two second flanges connecting the middle pipe section and the lower pipe section are connected to the first flange.
[0016] The preferred solution facilitates the replacement of various components and the installation of the cyclone internals in the middle pipe section through the arrangement of the reaction tube.
[0017] Preferably, the liquid inlet pipe is also provided with a regulating valve. The preferred solution facilitates adjusting the inlet amount of the acid or alkali solution by providing the regulating valve. The invention has the following beneficial effects: the lithium precipitation mother liquor is supplied at a constant flow rate by a centrifugal pump, the lithium precipitation mother liquor enters the upper reaction tube from the liquid inlet of the reaction tube located at the top, and enters the upper reaction tube with the sulfuric acid from the sulfuric acid high-level tank through the liquid inlet pipe, the lithium precipitation mother liquor and the sulfuric acid contact and react in the reaction tube, the mixed liquor of the lithium precipitation mother liquor and the sulfuric acid is fully dispersed and mixed after passing through the cyclone internal parts, thereby eliminating carbonate radicals and lithium carbonate solid particles, the mother liquor reacts with the sulfuric acid to become a reaction liquid, and the reaction liquid is measured when it flows through the pH meter, because the flow rate of the lithium precipitation mother liquor is basically constant, because the number of carbonate radicals and lithium carbonate solid particles in the mother liquor varies, the process requires that the carbonate radicals and lithium carbonate solid particles in the lithium precipitation mother liquor can be completely eliminated when the pH value of the reaction liquid endpoint reaches the specified pH index, then the amount of sulfuric acid added during the reaction process varies, so the amount of sulfuric acid introduced is adjusted by the pH value measured by the pH meter to ensure that the pH value of the reaction liquid reaches within the index range required by the process, and the efficiency of the reaction between the lithium precipitation mother liquor and sulfuric acid is effectively improved; Next, the pH value of the reaction liquid needs to be further adjusted to meet the process requirements of the subsequent stage. The reaction liquid and liquid alkali enter the reaction tube located below, and after sufficient mixing and reaction in the cyclone internals, a neutralizing liquid is formed. The pH value of the mother liquor is adjusted. The process requires that the pH value of the neutralizing liquid must reach the specified pH index. Therefore, the pH value is measured by the pH meter, and then the amount of alkali solution entering is adjusted to ensure that the pH value of the neutralizing liquid is within the index range required by the process. BRIEF DESCRIPTION OF THE DRAWINGS
[0018] Figure 1 It is a schematic diagram of the structure of the present invention; Figure 2 It is a three-dimensional schematic diagram of the swirl internals; As shown in the figure: 1. Reaction tube, 2. Intermediate tube, 3. Cyclone internals, 4. Regulating valve, 5. Lithium precipitation mother liquor inlet, 6. Sulfuric acid, 7. Liquid alkali, 8. Reaction liquid, 9. Neutralizing liquid, 10. pH meter, 11. Top pipe section, 12. Middle pipe section, 13. Lower pipe section. DETAILED DESCRIPTION
[0019] In order to clearly illustrate the technical features of this solution, this solution is described below through a specific implementation method.
[0020] See attached Figure 1-2 The present invention discloses a combined acid-base reaction device for lithium precipitation mother liquor in the process of preparing lithium carbonate, comprising two reaction tubes 1 arranged vertically and with axes extending vertically, an intermediate tube 2 is arranged between the two reaction tubes 1, a liquid inlet of the intermediate tube 2 is connected to a liquid outlet of the upper reaction tube 1, and a liquid outlet of the intermediate tube 2 is connected to a liquid inlet of the lower reaction tube 1. To resist strong acid and alkali corrosion, the pipe fittings in this scheme are all steel-lined polytetrafluoroethylene.
[0021] The reaction tube 1 comprises a top pipe section 11, a middle pipe section 12, and a lower pipe section 13 which are connected in sequence through flanges. A liquid inlet pipe is connected to the side of the top pipe section 11, and a regulating valve 4 is provided on the liquid inlet pipe.
[0022] A swirl internal part 3 is provided in the middle pipe section 12, and the swirl internal part 3 includes three spiral blades arranged vertically and connected in sequence. The diameter of the blades is adapted to the inner diameter of the reaction tube 1. The bottom end of the lowest blade is fixedly connected to a first flange plate, and the two second flanges connecting the middle pipe section 12 and the lower pipe section 13 are connected to the first flange.
[0023] In two adjacent blades, the bottom surface of the upper blade forms a certain angle with the lower blade, and plug-in grooves are provided on both end surfaces of the blades. When the two adjacent blades are connected, the corresponding two plug-in grooves are inserted into each other so that the bottoms of the two plug-in grooves are connected. The width of the plug-in groove is adapted to the thickness of the blade, and the two adjacent blades are plug-in connected through the corresponding two plug-in grooves. The blades are made of polytetrafluoroethylene material.
[0024] A pH meter 10 located outside the reaction tube 1 is provided on the side of the lower pipe section 13. The detection end of the pH meter 10 is inserted into the lower pipe section 13 to measure the pH value of the mixed liquid flowing through the lower pipe section 13. The actuator signal of the regulating valve 4 is connected to the controller, and the controller and the pH meter 10 are electrically connected to the control console.
[0025] When the present invention is in use, the lithium precipitation mother liquor is supplied at a constant flow rate through a centrifugal pump, the lithium precipitation mother liquor enters the upper reaction tube 1 from the liquid inlet of the upper reaction tube 1, and enters the upper reaction tube 1 with sulfuric acid 6 from the sulfuric acid high-level tank through the liquid inlet pipe, the lithium precipitation mother liquor and sulfuric acid contact and react in the reaction tube 1, the mixed liquid of the lithium precipitation mother liquor and sulfuric acid is fully dispersed and mixed after passing through the cyclone inner part 3, thereby eliminating carbonate and lithium carbonate solid particles, the mother liquor reacts with sulfuric acid to become a reaction liquid 8, and the reaction liquid 8 is measured for pH value when it flows through the pH meter 10; Since the flow rate of lithium precipitation mother liquor is basically constant, the number of carbonate ions and lithium carbonate solid particles in the mother liquor varies. The process requires that the carbonate ions and lithium carbonate solid particles in the lithium precipitation mother liquor can be completely eliminated only when the final pH value of the reaction liquid 8 reaches the specified pH index. Therefore, the amount of sulfuric acid added during the reaction varies. Therefore, the pH value measured by the pH meter 10 is used to adjust the amount of sulfuric acid entering to ensure that the pH value of the reaction liquid 8 is within the index range required by the process. By comparing the pH value of the reaction liquid 8 with the specified pH index, when the detected value is lower than the specified value, the controller sends a signal to the regulating valve 4 to adjust the opening of the regulating valve 4 to appropriately reduce the sulfuric acid flow rate. On the contrary, when the detected value is higher than the specified value, the controller sends a signal to the regulating valve 4 to adjust the opening of the regulating valve 4 to appropriately increase the sulfuric acid flow rate, to ensure that the pH value of the reaction liquid 8 is within the index range required by the process, and effectively improve the efficiency of the reaction between the lithium precipitation mother liquor and sulfuric acid. Next, the pH value of the reaction liquid 8 needs to be further adjusted to meet the process requirements of the subsequent stage. The reaction liquid 8 enters the reaction tube 1 through the intermediate tube 2. The reaction liquid 8 is supplied in a quantitative manner and mixed with the liquid alkali 7 from the liquid alkali high-level tank in the reaction tube below through the regulating valve. After sufficient mixing reaction of the swirl internal part 3, a neutralizing liquid 9 is formed. The process requires that the pH value of the neutralizing liquid 9 be adjusted back to the specified index to meet the requirements of the evaporation process. The controller sets a basic opening of the regulating valve, and the online pH meter detects the pH value of the neutralizing liquid in real time. The detected pH value of the neutralizing liquid is compared with the specified pH index. When the detected value is lower than the specified value, the controller sends a signal to the regulating valve to adjust the opening of the regulating valve to appropriately increase the liquid alkali flow rate. Conversely, when the detected value is higher than the specified value, the controller sends a signal to the regulating valve to adjust the opening of the regulating valve to appropriately reduce the liquid alkali flow rate to ensure that the pH value of the neutralizing liquid 9 is within the index range required by the process.
[0026] Of course, the above description is not limited to the above examples. Technical features not described in the present invention can be achieved by or by using existing technologies, which will not be described here. The above embodiments and drawings are only used to illustrate the technical scheme of the present invention and are not limitations of the present invention. The present invention is described in detail with reference to the preferred implementation methods. Ordinary technicians in this field should understand that changes, modifications, additions or substitutions made by ordinary technicians in this technical field within the essential scope of the present invention do not depart from the purpose of the present invention, and should also fall within the scope of protection of the claims of the present invention.
Claims
1. A combined acid-base reaction device for lithium precipitation mother liquor in the process of lithium carbonate preparation, characterized in that: The invention comprises two reaction tubes (1) connected in sequence along the vertical direction, wherein a cyclone inner part (3) for breaking up a mixed liquid is provided in the reaction tube (1), a liquid inlet pipe located above the cyclone inner part (3) is connected to the side of the reaction tube (1), and a pH meter (10) for measuring the mixed liquid is also provided on the side of the reaction tube (1) and located below the cyclone inner part (3).
2. The combined acid-base reaction device for lithium precipitation mother liquor in the lithium carbonate preparation process according to claim 1, characterized in that: An intermediate tube (2) is also provided between the two reaction tubes (1); the liquid inlet of the intermediate tube (2) is connected to the liquid outlet of the upper reaction tube (1), and the liquid outlet of the intermediate tube (2) is connected to the liquid inlet of the lower reaction tube (1).
3. The combined acid-base reaction device for lithium precipitation mother liquor in the lithium carbonate preparation process according to claim 1, characterized in that: The cyclone internal component (3) comprises a plurality of spiral blades arranged vertically and connected in sequence, and the diameter of the blades is adapted to the inner diameter of the reaction tube (1).
4. The combined acid-base reaction device for lithium precipitation mother liquor in the lithium carbonate preparation process according to claim 3, characterized in that: A first flange is fixedly connected to the bottom end of the lowest blade, and the first flange is connected to the reaction tube (1).
5. The combined acid-base reaction device for lithium precipitation mother liquor in the lithium carbonate preparation process according to claim 3, characterized in that: Both end surfaces of the blades are provided with plug-in grooves, and two adjacent blades are plug-connected through the corresponding two plug-in grooves.
6. The combined acid-base reaction device for lithium precipitation mother liquor in the lithium carbonate preparation process according to claim 3, characterized in that: In two adjacent blades, the bottom surface of the upper blade forms a certain angle with the bottom surface of the lower blade.
7. The combined acid-base reaction device for lithium precipitation mother liquor in the lithium carbonate preparation process according to claim 4, characterized in that: The reaction tube (1) comprises a top tube section (11), a middle tube section (12), and a lower tube section (13) which are connected in sequence via flanges; the top tube section is connected to the liquid inlet; the middle tube section (12) is provided with the blade; the detection end of the pH meter (10) is inserted into the lower tube section (13); and two second flanges connecting the middle tube section (12) and the lower tube section (13) are connected to the first flange.
8. The combined acid-base reaction device for lithium precipitation mother liquor in the lithium carbonate preparation process according to claim 1, characterized in that: The liquid inlet pipe is also provided with a regulating valve (4).