CN111592020A - Precipitation formula, process and device of lithium carbonate - Google Patents
Precipitation formula, process and device of lithium carbonate Download PDFInfo
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- CN111592020A CN111592020A CN202010590296.2A CN202010590296A CN111592020A CN 111592020 A CN111592020 A CN 111592020A CN 202010590296 A CN202010590296 A CN 202010590296A CN 111592020 A CN111592020 A CN 111592020A
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- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D15/00—Lithium compounds
- C01D15/08—Carbonates; Bicarbonates
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Abstract
The invention provides a precipitation formula, a precipitation process and a precipitation device of lithium carbonate. The precipitation formula of the lithium carbonate comprises: the auxiliary materials comprise calcium sulfate and calcium carbonate, the mass of the calcium sulfate is 40-60% of that of the lepidolite ore, and the mass of the calcium carbonate is 5-18% of that of the lepidolite ore. A process for the precipitation of lithium carbonate, the steps of: s1: grinding and uniformly mixing the lepidolite ore, calcium sulfate and calcium carbonate to obtain a mixture A; s2: placing the mixture A in a rotary kiln for roasting, and filtering after roasting to obtain a roasted mixture B; s3: introducing the roasted mixture B into a reaction device and uniformly stirring; s4: and introducing carbon dioxide into the reaction device for precipitation and pressurization to obtain lithium carbonate precipitate. The precipitation formula, the process and the device of the lithium carbonate provided by the invention have the advantages of large precipitation particles and high precipitation efficiency.
Description
Technical Field
The invention relates to the technical field of lithium extraction from ores, in particular to a precipitation formula, a process and a device of lithium carbonate.
Background
Lithium carbonate, an inorganic compound, has the chemical formula of Li2CO3, is a colorless monoclinic crystal or white powder, is soluble in dilute acid, is slightly soluble in water, has a higher solubility in cold water than hot water, is insoluble in alcohol and acetone, and can be used as a common lithium ion battery raw material for preparing ceramics, medicaments, catalysts and the like. The lithium carbonate solid particles precipitated by the existing lithium carbonate precipitation process are small, and the precipitation efficiency is low.
Therefore, there is a need to provide a new lithium carbonate precipitation formulation, process and apparatus to solve the above problems.
Disclosure of Invention
The invention aims to provide a precipitation formula, a process and a device of lithium carbonate with large precipitation particles and high precipitation efficiency.
In order to solve the technical problem, the precipitation formula of lithium carbonate provided by the invention comprises: the auxiliary materials comprise calcium sulfate and calcium carbonate, the mass of the calcium sulfate is 40-60% of that of the lepidolite ore, and the mass of the calcium carbonate is 5-18% of that of the lepidolite ore.
A process for the precipitation of lithium carbonate, the steps of:
s1: grinding and uniformly mixing the lepidolite ore, calcium sulfate and calcium carbonate to obtain a mixture A;
s2: placing the mixture A in a rotary kiln for roasting, and filtering after roasting to obtain a roasted mixture B;
s3: introducing the roasted mixture B into a reaction device and uniformly stirring;
s4: and introducing carbon dioxide into the reaction device for precipitation and pressurization to obtain lithium carbonate precipitate.
A reaction device comprises a reaction kettle, a pressurizing device, a carbon dioxide steel cylinder and a precipitation filtering device.
Preferably, pressure device includes the shell, the mounting bracket is installed to one side of shell, install the cylinder on the mounting bracket, the output shaft of cylinder extends to in the shell and be connected with the piston, be connected with intake pipe and outlet duct on the shell, the intake pipe with the carbon dioxide steel bottle is connected, the outlet duct with reation kettle is connected.
Preferably, the cover is equipped with the sealing washer on the piston, the sealing washer with the sealed sliding connection of inner wall of shell, the shell is close to the air vent has been seted up to one side of cylinder, install first check valve in the intake pipe, the circulation direction of first check valve is followed the carbon dioxide steel bottle flow direction pressure device, install on the outlet duct the second check valve, the circulation direction of second check valve is followed pressure device flow direction reation kettle.
Preferably, the filtering device comprises a box body, a partition board is arranged in the box body, the partition board divides the box body into a filtering cavity and a drying cavity, a discharging pipe is connected onto a discharging port of the reaction kettle, a first valve is installed on the discharging pipe, the discharging pipe is communicated with the filtering cavity, the partition board is provided with the through hole, a filtering plate is arranged in the through hole, one side of the filtering plate extends into the filtering cavity, the other side of the filtering plate extends into the drying cavity, the filtering plate is obliquely arranged, a liquid outlet pipe and a material collecting pipe are respectively installed at the bottom side of the box body, the liquid outlet pipe is communicated with the filtering cavity, the material collecting pipe is communicated with the drying cavity, and a second valve is installed on the material collecting pipe.
Preferably, a heater is installed in the drying cavity, a ventilation fan is installed on the inner wall of one side, away from the filter cavity, of the drying cavity, and a third valve is installed on the liquid outlet pipe.
Preferably, be equipped with the inlet pipe on the reation kettle, install fourth valve and fifth valve on the inlet pipe, the intercommunication has the back flow on the inlet pipe, install the water pump on the back flow, the bottom of back flow with the drain pipe is connected, the back flow with the junction of inlet pipe is located between fourth valve and the fifth valve, the back flow with the junction of drain pipe is located the top of third valve.
Preferably, the top side of the reaction kettle is provided with an air release port, and the air release port is provided with a pressure release valve.
Preferably, the filter plate is rotatably connected with the inner wall of the bottom side of the through hole, a through hole is formed in the inner wall of one side, away from the drying cavity, of the filter cavity, a connecting plate is installed in the through hole, one side, close to the filter cavity, of the connecting plate extends into the filter cavity and is fixedly connected with the filter plate, the other side of the connecting plate extends out of the through hole and is provided with a vibration motor, a plurality of springs are fixedly installed on the bottom side of the connecting plate, and the bottom ends of the springs are fixedly connected with the inner wall of the bottom side of the through hole.
Compared with the related technology, the precipitation formula, the process and the device of the lithium carbonate provided by the invention have the following beneficial effects:
the invention provides a precipitation formula, a process and a device of lithium carbonate, wherein solid lithium carbonate is increased by 30-80 microns by carbon dioxide precipitation pressurization; the reaction kettle can be pressurized by the pressurizing device, the structure is simple, and the operation is convenient; the lithium carbonate solid after pressure precipitation can be filtered and dried through the precipitation filtering device, so that the solid lithium carbonate can be conveniently collected; the circulating sedimentation pressurization can be realized through the return pipe, and the utilization rate of the raw materials is improved.
Drawings
Fig. 1 is a flow chart of a lithium carbonate precipitation process provided by the present invention;
fig. 2 is a schematic structural diagram of a first embodiment of a lithium carbonate precipitation device provided by the present invention;
FIG. 3 is a schematic view of the pressurization device shown in FIG. 2;
FIG. 4 is a schematic view of the structure of the precipitation filter shown in FIG. 2;
fig. 5 is a schematic structural diagram of a lithium carbonate precipitation device according to a second embodiment of the present invention.
Reference numbers in the figures: 1. the device comprises a reaction kettle, 2, a pressurizing device, 3, a carbon dioxide steel cylinder, 4, a precipitation filtering device, 5, a shell, 6, a mounting rack, 7, a cylinder, 8, a piston, 9, a sealing ring, 10, an air inlet pipe, 11, a first one-way valve, 12, an air outlet pipe, 13, a second one-way valve, 14, an air vent, 15, a discharge pipe, 16, a first valve, 17, a box body, 18, a filtering cavity, 19, a drying cavity, 20, a through hole, 21, a filtering plate, 22, a heater, 23, a ventilating fan, 24, a liquid outlet pipe, 25, a material collecting pipe, 26, a second valve, 27, a third valve, 28, a return pipe, 29, a water pump, 30, a feed pipe, 31, a fourth valve, 32, a fifth valve, 33, an air release port, 34, a through hole, 35, a connecting plate, 36, a.
Detailed Description
The invention is further described with reference to the following figures and embodiments.
The first embodiment:
referring to fig. 2 to 4 in combination, in the first embodiment of the present invention, the precipitation formulation of lithium carbonate includes: the auxiliary materials comprise calcium sulfate and calcium carbonate, the mass of the calcium sulfate is 40-60% of that of the lepidolite ore, and the mass of the calcium carbonate is 5-18% of that of the lepidolite ore.
A process for the precipitation of lithium carbonate, the steps of:
s1: grinding and uniformly mixing the lepidolite ore, calcium sulfate and calcium carbonate to obtain a mixture A;
s2: placing the mixture A in a rotary kiln for roasting, and filtering after roasting to obtain a roasted mixture B;
s3: introducing the roasted mixture B into a reaction device and uniformly stirring;
s4: and introducing carbon dioxide into the reaction device for precipitation and pressurization to obtain lithium carbonate precipitate.
A reaction device comprises a reaction kettle 1, a pressurizing device 2, a carbon dioxide steel cylinder 3 and a precipitation filtering device 4.
Pressure device 2 includes shell 5, mounting bracket 6 is installed to one side of shell 5, install cylinder 7 on the mounting bracket 6, the output shaft of cylinder 7 extends to be connected with piston 8 in the shell 5, be connected with intake pipe 10 and outlet duct 12 on the shell 5, intake pipe 10 with carbon dioxide steel bottle 3 is connected, outlet duct 12 with reation kettle 1 is connected.
The cover is equipped with sealing washer 9 on the piston 8, sealing washer 9 with the sealed sliding connection of inner wall of shell 5, shell 5 is close to air vent 14 has been seted up to one side of cylinder 7, install first check valve 11 on the intake pipe 10, the circulation direction of first check valve 11 is followed 3 flow directions of carbon dioxide steel bottle 2, install on outlet duct 12 second check valve 13, the circulation direction of second check valve 13 is followed 2 flow directions of pressure device 1.
The filtering device comprises a box body 17, a partition board is arranged in the box body 17, the partition board divides the box body 17 into a filtering cavity 18 and a drying cavity 19, a discharge pipe 15 is connected to a discharge port of the reaction kettle 1, a first valve 16 is installed on the discharge pipe 15, the discharge pipe 15 is communicated with the filtering cavity 18, a through hole 20 is formed in the partition board, a filtering plate 21 is arranged in the through hole 20, one side of the filtering plate 21 extends into the filtering cavity 18, the other side of the filtering plate 21 extends into the drying cavity 19, the filtering plate 21 is obliquely arranged, a liquid outlet pipe 24 and a material collecting pipe 25 are respectively installed at the bottom side of the box body 17, the liquid outlet pipe 24 is communicated with the filtering cavity 18, the material collecting pipe 25 is communicated with the drying cavity 19, and a second valve 26 is installed on the material collecting pipe 25.
A heater 22 is installed in the drying cavity 19, an air exchange fan 23 is installed on the inner wall of one side, away from the filter cavity 18, of the drying cavity 19, and a third valve 27 is installed on the liquid outlet pipe 24.
Be equipped with inlet pipe 30 on reation kettle 1, install fourth valve 31 and fifth valve 32 on the inlet pipe 30, the intercommunication has back flow 28 on the inlet pipe 30, install water pump 29 on the back flow 28, the bottom of back flow 28 with drain pipe 24 is connected, back flow 28 with the junction of inlet pipe 30 is located between fourth valve 31 and the fifth valve 32, back flow 28 with the junction of drain pipe 24 is located the top of third valve 27.
The top side of reaction kettle 1 is equipped with relief port 33, install the relief valve on relief port 33.
A reservoir is arranged at the joint of the liquid outlet pipe 24 and the return pipe 28, and both the liquid outlet pipe 24 and the return pipe 28 are communicated with the reservoir.
The working principle of the precipitation formula, the process and the device of the lithium carbonate provided by the invention is as follows:
firstly, the valve on the carbon dioxide steel cylinder 3 is opened, the cylinder 7 is started, the cylinder 7 drives the piston 8 to move, the carbon dioxide enters the pressurizing device 2 from the carbon dioxide steel cylinder 3 through the air inlet pipe 10, when the piston 8 moves towards the direction close to the reaction kettle 1, the carbon dioxide is sent into the reaction kettle 1 through the air outlet pipe 12 to be precipitated and pressurized, after lithium carbonate solid is separated out, the pressure release valve on the air release port 33 is opened, the first valve 16 is opened, liquid and solid lithium carbonate in the reaction kettle 1 both enter the precipitation filtering device 4, the solid lithium carbonate is filtered through the filtering plate 21 and rolls into the drying cavity 19 to be dried, the liquid enters the reservoir, the first valve 16 is closed, and the liquid in the reservoir is subjected to cyclic pressurization and precipitation through the water pump 29 in the reaction kettle 1.
Compared with the related technology, the precipitation formula, the process and the device of the lithium carbonate provided by the invention have the following beneficial effects:
the invention provides a precipitation formula, a process and a device of lithium carbonate, wherein solid lithium carbonate is increased by 30-80 microns by carbon dioxide precipitation pressurization; the reaction kettle 1 can be pressurized by the pressurizing device 2, the structure is simple, and the operation is convenient; the lithium carbonate solid after pressure precipitation can be filtered and dried through the precipitation filtering device 4, so that the solid lithium carbonate can be conveniently collected; the circulating sedimentation pressurization can be realized through the return pipe 28, and the utilization rate of raw materials is improved.
Second embodiment:
based on the lithium carbonate precipitation formulation, the lithium carbonate precipitation process and the lithium carbonate precipitation device provided in the first embodiment of the present application, a second embodiment of the present application provides another lithium carbonate precipitation formulation, the lithium carbonate precipitation process and the lithium carbonate precipitation device. The second embodiment is merely a preferred way of the first embodiment, and the implementation of the second embodiment does not affect the implementation of the first embodiment alone.
The second embodiment of the present invention will be further described with reference to the drawings and the following description.
Referring to fig. 4, the present embodiment is different from the first embodiment in that the filter plate 21 is rotatably connected to the inner wall of the bottom side of the through hole 20, a through hole 34 is formed in the inner wall of one side of the filter chamber 18 away from the drying chamber 19, a connecting plate 35 is installed in the through hole 34, one side of the connecting plate 35 close to the filter chamber 18 extends into the filter chamber 18 and is fixedly connected to the filter plate 21, the other side of the connecting plate 35 extends out of the through hole 34 and is installed with a vibration motor 36, a plurality of springs 37 are fixedly installed on the bottom side of the connecting plate 35, and the bottom ends of the springs 37 are fixedly connected to the inner wall of the bottom side of the through hole 34.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes, which are made by using the contents of the present specification and the accompanying drawings, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (10)
1. The precipitation formula of lithium carbonate is characterized by comprising the following raw materials: the auxiliary materials comprise calcium sulfate and calcium carbonate, the mass of the calcium sulfate is 40-60% of that of the lepidolite ore, and the mass of the calcium carbonate is 5-18% of that of the lepidolite ore.
2. A lithium carbonate precipitation process, characterized by the steps of:
s1: grinding and uniformly mixing the lepidolite ore, calcium sulfate and calcium carbonate to obtain a mixture A;
s2: placing the mixture A in a rotary kiln for roasting, and filtering after roasting to obtain a roasted mixture B;
s3: introducing the roasted mixture B into a reaction device and uniformly stirring;
s4: and introducing carbon dioxide into the reaction device for precipitation and pressurization to obtain lithium carbonate precipitate.
3. A reaction apparatus according to any one of claims 1 to 2, wherein the reaction apparatus comprises a reaction vessel, a pressurizing means, a carbon dioxide cylinder, and a precipitation filtering means.
4. The lithium carbonate precipitation device according to claim 3, wherein the pressurizing device comprises a housing, a mounting frame is mounted on one side of the housing, a cylinder is mounted on the mounting frame, an output shaft of the cylinder extends into the housing and is connected with a piston, an air inlet pipe and an air outlet pipe are connected to the housing, the air inlet pipe is connected with the carbon dioxide steel cylinder, and the air outlet pipe is connected with the reaction kettle.
5. The lithium carbonate precipitation device according to claim 4, wherein a sealing ring is sleeved on the piston, the sealing ring is in sealing sliding connection with an inner wall of the outer shell, a vent hole is formed in one side, close to the cylinder, of the outer shell, a first one-way valve is installed on the air inlet pipe, the flowing direction of the first one-way valve is from the carbon dioxide steel cylinder to the pressurizing device, the second one-way valve is installed on the air outlet pipe, and the flowing direction of the second one-way valve is from the pressurizing device to the reaction kettle.
6. The lithium carbonate precipitation device according to claim 3, wherein the filtering device comprises a box body, a partition plate is arranged in the box body, the partition plate divides the box body into a filtering cavity and a drying cavity, a discharging pipe is connected to a discharging port of the reaction kettle, a first valve is arranged on the discharging pipe, the discharging pipe is communicated with the filtering cavity, the partition plate is provided with the through hole, a filtering plate is arranged in the through hole, one side of the filtering plate extends into the filtering cavity, the other side of the filtering plate extends into the drying cavity, the filtering plate is obliquely arranged, a liquid outlet pipe and a material collecting pipe are respectively arranged on the bottom side of the box body, the liquid outlet pipe is communicated with the filtering cavity, the material collecting pipe is communicated with the drying cavity, and a second valve is arranged on the material collecting pipe.
7. The lithium carbonate precipitation device according to claim 6, wherein a heater is installed in the drying cavity, a ventilation fan is installed on an inner wall of one side of the drying cavity, which is far away from the filtering cavity, and a third valve is installed on the liquid outlet pipe.
8. The lithium carbonate precipitation device according to claim 7, wherein a feed pipe is arranged on the reaction kettle, a fourth valve and a fifth valve are arranged on the feed pipe, a return pipe is communicated with the feed pipe, a water pump is arranged on the return pipe, the bottom end of the return pipe is connected with the drain pipe, the connection position of the return pipe and the feed pipe is located between the fourth valve and the fifth valve, and the connection position of the return pipe and the drain pipe is located above the third valve.
9. The lithium carbonate precipitation device according to claim 3, wherein a gas release port is arranged on the top side of the reaction kettle, and a pressure release valve is arranged on the gas release port.
10. The lithium carbonate precipitation device according to claim 6, wherein the filter plate is rotatably connected with the inner wall of the bottom side of the through hole, a through hole is formed in the inner wall of one side of the filter chamber, which is away from the drying chamber, a connecting plate is installed in the through hole, one side of the connecting plate, which is close to the filter chamber, extends into the filter chamber and is fixedly connected with the filter plate, the other side of the connecting plate extends out of the through hole and is provided with a vibration motor, a plurality of springs are fixedly installed on the bottom side of the connecting plate, and the bottom ends of the springs are fixedly connected with the inner wall of the bottom side of the through hole.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010590296.2A CN111592020A (en) | 2020-06-25 | 2020-06-25 | Precipitation formula, process and device of lithium carbonate |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010590296.2A CN111592020A (en) | 2020-06-25 | 2020-06-25 | Precipitation formula, process and device of lithium carbonate |
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| CN111592020A true CN111592020A (en) | 2020-08-28 |
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| CN202010590296.2A Pending CN111592020A (en) | 2020-06-25 | 2020-06-25 | Precipitation formula, process and device of lithium carbonate |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2024084233A1 (en) * | 2022-10-21 | 2024-04-25 | Research By British Lithium Ltd | Production of battery grade chemicals |
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| JP2005022925A (en) * | 2003-07-02 | 2005-01-27 | Toyota Motor Corp | Method and device for producing lithium salt |
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2020
- 2020-06-25 CN CN202010590296.2A patent/CN111592020A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2005022925A (en) * | 2003-07-02 | 2005-01-27 | Toyota Motor Corp | Method and device for producing lithium salt |
| CN202087125U (en) * | 2011-04-29 | 2011-12-28 | 陈锡林 | Anti-explosion vacuum filtration drying unit for insoluble sulfur production |
| CN106222450A (en) * | 2016-07-21 | 2016-12-14 | 温岭市亿林投资有限公司 | Lithium, rubidium and the extracting method of caesium in a kind of zinnwaldite ore deposit |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2024084233A1 (en) * | 2022-10-21 | 2024-04-25 | Research By British Lithium Ltd | Production of battery grade chemicals |
| GB2623751A (en) * | 2022-10-21 | 2024-05-01 | Res By British Lithium Limited | Production of battery grade chemicals |
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Application publication date: 20200828 |
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