CN109399673B - Method for decomposing lithium bicarbonate solution - Google Patents
Method for decomposing lithium bicarbonate solution Download PDFInfo
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- CN109399673B CN109399673B CN201811589102.6A CN201811589102A CN109399673B CN 109399673 B CN109399673 B CN 109399673B CN 201811589102 A CN201811589102 A CN 201811589102A CN 109399673 B CN109399673 B CN 109399673B
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- HQRPHMAXFVUBJX-UHFFFAOYSA-M lithium;hydrogen carbonate Chemical compound [Li+].OC([O-])=O HQRPHMAXFVUBJX-UHFFFAOYSA-M 0.000 title claims abstract description 67
- 238000000034 method Methods 0.000 title claims abstract description 33
- 238000006243 chemical reaction Methods 0.000 claims abstract description 121
- 238000005979 thermal decomposition reaction Methods 0.000 claims abstract description 83
- 238000000354 decomposition reaction Methods 0.000 claims abstract description 45
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims abstract description 30
- 229910052808 lithium carbonate Inorganic materials 0.000 claims abstract description 30
- 239000012452 mother liquor Substances 0.000 claims abstract description 14
- 238000001914 filtration Methods 0.000 claims abstract description 8
- 239000000243 solution Substances 0.000 claims description 153
- 238000003756 stirring Methods 0.000 claims description 39
- 238000010438 heat treatment Methods 0.000 claims description 33
- 230000035484 reaction time Effects 0.000 claims description 21
- 238000000926 separation method Methods 0.000 claims description 8
- 238000002386 leaching Methods 0.000 claims description 7
- 238000005086 pumping Methods 0.000 claims description 7
- 239000002002 slurry Substances 0.000 claims description 7
- 239000007787 solid Substances 0.000 claims description 7
- 238000000746 purification Methods 0.000 claims description 6
- 239000010413 mother solution Substances 0.000 claims description 5
- 229910000032 lithium hydrogen carbonate Inorganic materials 0.000 claims 5
- 238000001035 drying Methods 0.000 abstract description 6
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract 1
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 14
- 229910002092 carbon dioxide Inorganic materials 0.000 description 7
- 239000001569 carbon dioxide Substances 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 6
- 239000003638 chemical reducing agent Substances 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 238000000197 pyrolysis Methods 0.000 description 3
- 238000003763 carbonization Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000012824 chemical production Methods 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000008213 purified water Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- 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
Abstract
The invention discloses a method for decomposing a lithium bicarbonate solution, which comprises the following steps of: carrying out heat exchange on the lithium bicarbonate solution subjected to the precision filtration and the thermal decomposition mother liquor; second, first-stage thermal decomposition; thirdly, performing secondary thermal decomposition; fourthly, third-stage thermal decomposition; fifthly, fourth-stage thermal decomposition; sixth and fifth thermal decomposition; and seventhly, purifying. The method for decomposing the lithium bicarbonate solution has the following effects: the technical scheme is simple and easy to implement, and the method adopts the low lithium bicarbonate concentration and the gradient decomposition in the reaction system to control the decomposition speed so as to achieve the aim of reducing the lithium bicarbonate package in the lithium carbonate product and better ensure the product quality. The continuous operation efficiency of the thermal decomposition equipment is high. The lithium carbonate product drying equipment can be heated and dried by adopting steam, and far infrared high-temperature drying is not needed, so that the energy consumption is reduced, and the safety is improved.
Description
Technical Field
The invention relates to the technical field of chemical production, in particular to a method for decomposing a lithium bicarbonate solution.
Background
Currently, the lithium battery industry uses battery grade lithium carbonate with high purity, and other industries use industrial grade lithium carbonate but the usage amount is small, so that most of industrial grade lithium carbonate or crude lithium carbonate is purified into battery grade lithium carbonate.
The method for purifying industrial grade lithium carbonate or crude lithium carbonate into battery lithium carbonate is generally a deep carbonization method, i.e. carbon dioxide reacts with lithium carbonate to generate soluble lithium bicarbonate, and then impurities are removed, and the lithium bicarbonate is heated and decomposed to obtain battery grade lithium carbonate or a lithium carbonate product with higher purity.
Generally, the thermal decomposition of lithium bicarbonate is completed in a reaction kettle, i.e. a lithium bicarbonate solution is pumped into the reaction kettle, steam is introduced into a jacket for heating, the lithium bicarbonate is thermally decomposed, and after the decomposition is completed, liquid-solid separation is performed. The lithium carbonate product obtained in the way also wraps a small amount of lithium bicarbonate, generally about 1.8%, and the lithium bicarbonate wrapped in the lithium carbonate product is not easy to decompose when being dried by steam and can be gradually decomposed only when the drying temperature is higher than 350 ℃. Therefore, the lithium carbonate wet product is dried at high temperature by adopting a far infrared dryer, and compared with a disc dryer heated by steam, the far infrared dryer has the advantages of high equipment investment, high energy consumption, low production efficiency and more trouble in operation and maintenance.
Disclosure of Invention
Based on the above, the embodiment of the invention provides a method for decomposing a lithium bicarbonate solution, which solves the problem of low production efficiency in the prior art.
An embodiment of the invention provides a method for decomposing a lithium bicarbonate solution, which has the following specific technical scheme:
a method of decomposing a lithium bicarbonate solution, the method comprising:
(1) heat exchange: carrying out heat exchange on the lithium bicarbonate solution subjected to precise filtration and a thermal decomposition mother solution so as to heat the lithium bicarbonate solution to 40-45 ℃;
(2) first-stage thermal decomposition: the lithium bicarbonate solution after heat exchange in the step (1) is injected into a first reaction kettle, is heated to raise the temperature of the solution to 60 ℃ under continuous stirring, and is kept at a constant temperature of 58-62 ℃ for decomposition reaction;
(3) second-stage thermal decomposition: overflowing the solution subjected to thermal decomposition in the step (2) from the first reaction kettle to a second reaction kettle through a connecting pipe, heating the solution to enable the temperature of the solution to rise to 70 ℃ under continuous stirring, and keeping the constant temperature at 68-72 ℃ for decomposition reaction;
(4) third-stage thermal decomposition: overflowing the solution subjected to thermal decomposition in the step (3) from the second reaction kettle to a third reaction kettle through a connecting pipe, heating the solution to raise the temperature of the solution to 80 ℃ under continuous stirring, and keeping the constant temperature at 78-82 ℃ for decomposition reaction;
(5) fourth-stage thermal decomposition: overflowing the solution subjected to thermal decomposition in the step (4) from the third reaction kettle to a fourth reaction kettle through a connecting pipe, heating the solution to raise the temperature of the solution to 90 ℃ under continuous stirring, and keeping the constant temperature at 88-92 ℃ for decomposition reaction;
(6) and (3) fifth-stage thermal decomposition: overflowing the solution subjected to thermal decomposition in the step (5) from the fourth reaction kettle to a fifth reaction kettle through a connecting pipe, heating the solution to enable the temperature of the solution to rise to 98 ℃ under continuous stirring, and keeping the constant temperature at 96-100 ℃ to perform decomposition reaction;
(7) and (3) purification: and (4) overflowing the solution subjected to thermal decomposition in the step (6) from the fifth reaction kettle to a slurry tank through a connecting pipe, pumping into a centrifugal machine, performing liquid-solid separation and leaching through the centrifugal machine, and then feeding into a dryer to be dried through the dryer to obtain a lithium carbonate dry product.
According to the embodiment of the invention, the decomposition speed of the lithium bicarbonate solution is controlled through five-stage step decomposition, so that the purpose of reducing the lithium bicarbonate package in the lithium carbonate product is achieved, the product quality is better ensured, the production efficiency is high due to the continuous operation of each reaction kettle, and the problem of low production efficiency in the prior art is solved.
Further, the heating step is carried out under the condition of continuous stirring:
stirring continuously by the stirrer of each reaction kettle;
and steam is introduced into the jacket of each reaction kettle to heat the reaction kettles.
Further, the stirrer is an upturning type blade, and the rotating speed of the stirrer ranges from 30 to 60 revolutions per minute.
Further, the thermal decomposition mother liquor is filled in the first reaction kettle, and when the lithium bicarbonate solution enters the first reaction kettle, the lithium bicarbonate solution and the thermal decomposition mother liquor are mixed under continuous stirring, so that the concentration of lithium bicarbonate in the solution is low.
Further, each reaction kettle controls different reaction temperatures and is basically kept in a constant temperature state. The temperature of the first reaction kettle is controlled to be 58-62 ℃, the temperature of the second reaction kettle is controlled to be 68-72 ℃, the temperature of the third reaction kettle is controlled to be 78-82 ℃, the temperature of the fourth reaction kettle is controlled to be 88-92 ℃, and the temperature of the fifth reaction kettle is controlled to be 96-100 ℃.
Further, the reaction time of the solution in each reaction kettle is 30-36 minutes, and the total reaction time of the solution is 150-180 minutes.
Drawings
Fig. 1 is a flow chart of a method for decomposing a lithium bicarbonate solution according to an embodiment of the present invention.
Fig. 2 is a flow chart of a production process of a decomposition method of a lithium bicarbonate solution according to an embodiment of the present invention.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in detail below. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein, but rather should be construed as broadly as the present invention is capable of modification in various respects, all without departing from the spirit and scope of the present invention.
Referring to fig. 1, a flow chart of a method for decomposing a lithium bicarbonate solution according to an embodiment of the present invention is shown, the method including:
step S11, hot-swapping: and carrying out heat exchange on the lithium bicarbonate solution subjected to the precision filtration and the thermal decomposition mother liquor so as to heat the lithium bicarbonate solution to 40-45 ℃.
Step S12, first stage pyrolysis: and (4) injecting the lithium bicarbonate solution subjected to heat exchange in the step S11 into a first reaction kettle, heating the solution to raise the temperature of the solution to 60 ℃ under continuous stirring, and keeping the constant temperature at 58-62 ℃ for decomposition reaction.
Step S13, first stage pyrolysis: and (4) injecting the lithium bicarbonate solution subjected to heat exchange in the step S12 into a first reaction kettle, heating the solution to raise the temperature of the solution to 60 ℃ under continuous stirring, and keeping the constant temperature at 58-62 ℃ for decomposition reaction.
Step S14, third stage thermal decomposition: and overflowing the solution subjected to thermal decomposition in the step S13 from the second reaction kettle to a third reaction kettle through a connecting pipe, heating the solution to raise the temperature of the solution to 80 ℃ under continuous stirring, and keeping the constant temperature at 78-82 ℃ for decomposition reaction.
Step S15, fourth stage thermal decomposition: and overflowing the solution subjected to thermal decomposition in the step S14 from the third reaction kettle to the fourth reaction kettle through a connecting pipe, heating the solution to raise the temperature of the solution to 90 ℃ under continuous stirring, and keeping the constant temperature at 88-92 ℃ for decomposition reaction.
Step S16, fifth stage pyrolysis: and overflowing the solution subjected to thermal decomposition in the step S15 from the fourth reaction kettle to the fifth reaction kettle through a connecting pipe, heating the solution to enable the temperature of the solution to rise to 98 ℃ under continuous stirring, and keeping the constant temperature at 96-100 ℃ to perform decomposition reaction.
Step S17, purification: and the solution subjected to the thermal decomposition in the step S16 overflows from the fifth reaction kettle to a slurry tank through a connecting pipe, is thrown into a centrifugal machine to be subjected to liquid-solid separation and leaching through the centrifugal machine, and then enters a dryer to be dried through the dryer to obtain a lithium carbonate dry product.
The decomposition method comprises the step of carrying out decomposition reaction on a lithium bicarbonate solution by five reaction kettles which are arranged in parallel, wherein each reaction kettle comprises a kettle body, a driving motor and a speed reducer which are arranged in the middle of the top end of the kettle body, a stirrer which is arranged in the kettle body and connected with the driving motor and the speed reducer, and a jacket which is arranged on the outer wall of the kettle body, a feeding port and a discharging port are oppositely arranged on the side wall of the kettle body, an inlet and an outlet which are communicated with the jacket are arranged at the upper end and the lower end of the outer wall of the kettle body, and an air outlet is. Wherein the discharge hole of each reaction kettle is connected with the feed inlet of the next reaction kettle through a connecting pipe.
The stirring mode is that the stirrers are driven by a driving motor and a speed reducer, the solution in the reaction kettles is stirred continuously by the stirrers in the reaction kettles, so that the solution is stirred uniformly, wherein the stirrers are upturned blades, and the rotating speed of the stirrers is 30-60 r/min; the heating mode is to heat the reaction kettles by introducing steam into the jackets of the reaction kettles, and specifically, the steam is introduced at the inlet to enable the steam to be contained in the jackets and condensed into liquid, and then the liquid flows out from the outlet to heat the reaction kettles. Wherein it can be understood that the inlet can also be filled with cooling water to realize the cooling of the reaction kettle. Wherein each reaction kettle controls different reaction temperature and basically keeps a constant temperature state. The temperature of the first reaction kettle is controlled to be 58-62 ℃, the temperature of the second reaction kettle is controlled to be 68-72 ℃, the temperature of the third reaction kettle is controlled to be 78-82 ℃, the temperature of the fourth reaction kettle is controlled to be 88-92 ℃, and the temperature of the fifth reaction kettle is controlled to be 96-100 ℃.
As shown in fig. 2, the lithium bicarbonate solution after being subjected to the fine filtration is subjected to heat exchange with a thermal decomposition mother solution, the lithium bicarbonate solution after the heat exchange is injected into a first reaction kettle from a feed inlet of the first reaction kettle, wherein the thermal decomposition mother solution is pre-filled in the first reaction kettle, when the lithium bicarbonate solution enters the first reaction kettle, the lithium bicarbonate solution and the thermal decomposition mother solution are mixed under continuous stirring, so that a solution with a low lithium bicarbonate concentration is formed in the first reaction kettle, wherein under the stirring and heating of the first reaction kettle, the solution temperature is maintained at 58-62 ℃ for a decomposition reaction, the heated lithium bicarbonate solution starts to be gradually decomposed to form lithium carbonate, carbon dioxide generated by the decomposition is discharged from a gas outlet at the top end of the first reaction kettle, and the discharged carbon dioxide is compressed and recycled to a carbon dioxide storage tank by a compressor. Wherein the reaction time of the solution in each reaction kettle is 30-36 minutes, and the total reaction time of the solution is 150-180 minutes.
The solution continuously and stably enters a first reaction kettle, and simultaneously, the mixed and heated solution continuously overflows from a discharge port of the first reaction kettle to a feed port of a second reaction kettle through a connecting pipe and flows into the second reaction kettle to be stirred and heated, and the solution continuously overflows from the discharge port of each reaction kettle to a feed port of the next reaction kettle through the connecting pipe and finally overflows into a slurry tank through a discharge port of a fifth reaction kettle positioned at the tail end, wherein the solution in each reaction kettle is subjected to decomposition reaction to form lithium carbonate, the temperature of each reaction kettle is gradually increased, the decomposition speed of the solution is gradually increased, lower lithium bicarbonate is remained in the solution flowing out from the discharge port of the fifth reaction kettle, and meanwhile, the solution is continuously subjected to decomposition reaction from the first reaction kettle to the fifth reaction kettle, so that the operation efficiency is high.
And further, feeding the decomposed solution into a centrifuge, introducing purified water, performing centrifugal separation and leaching to obtain a battery-grade wet lithium carbonate product, wherein the content of lithium bicarbonate in the wet lithium carbonate product is within 0.3%, and heating and drying by using steam of a dryer to obtain a battery-grade dry lithium carbonate product. The method comprises the following steps of separating a thermal decomposition mother liquor from a centrifugal machine, carrying out heat exchange and cooling on the thermal decomposition mother liquor, and then using the separated thermal decomposition mother liquor in a batching process of a previous step, wherein a small part of the thermal decomposition mother liquor can be periodically discharged after the impurity content of the thermal decomposition mother liquor is increased so as to keep the balance of impurities and ensure that the product quality is qualified; the carbon dioxide recovered and stored to the carbon dioxide storage tank can be used in a deep carbonization process required by the production of lithium carbonate, so that the carbon dioxide is recycled.
The invention has the beneficial effects that: 1. the technical scheme is simple and easy to implement, and the method adopts the low lithium bicarbonate concentration and the gradient decomposition in the reaction system to control the decomposition speed so as to achieve the aim of reducing the lithium bicarbonate package in the lithium carbonate product and better ensure the product quality. 2. Each reaction kettle in the thermal decomposition has high continuous operation efficiency. 3. The drying equipment can be heated and dried by adopting steam, and far infrared high-temperature drying is not needed, so that the energy consumption is reduced, and the safety is improved.
Example 1
A method for decomposing a lithium bicarbonate solution, the method comprising:
(1) heat exchange: carrying out heat exchange on the lithium bicarbonate solution subjected to precision filtration and the thermal decomposition mother liquor so as to heat the lithium bicarbonate solution to 40 ℃;
(2) first-stage thermal decomposition: the lithium bicarbonate solution after heat exchange in the step (1) is injected into a first reaction kettle, and is heated to raise the temperature of the solution to a constant temperature of 58 ℃ for decomposition reaction under continuous stirring, wherein the reaction time is 30 minutes, and the rotating speed of a stirrer is 30 revolutions per minute;
(3) second-stage thermal decomposition: overflowing the solution subjected to thermal decomposition in the step (2) from the first reaction kettle to a second reaction kettle through a connecting pipe, heating the solution under continuous stirring to enable the temperature of the solution to be raised to a constant temperature, and keeping the temperature at 68 ℃ for decomposition reaction, wherein the reaction time is 30 minutes, and the rotating speed of a stirrer is 30 revolutions per minute;
(4) third-stage thermal decomposition: overflowing the solution subjected to thermal decomposition in the step (3) from the second reaction kettle to a third reaction kettle through a connecting pipe, heating the solution under continuous stirring to enable the temperature of the solution to be raised to be constant at 78 ℃ for decomposition reaction, wherein the reaction time is 30 minutes, and the rotating speed of a stirrer is 30 revolutions per minute;
(5) fourth-stage thermal decomposition: overflowing the solution subjected to thermal decomposition in the step (4) from the third reaction kettle to a fourth reaction kettle through a connecting pipe, heating the solution under continuous stirring to enable the temperature of the solution to be raised to be kept constant at 88 ℃ for decomposition reaction, wherein the reaction time is 30 minutes, and the rotating speed of a stirrer is 30 revolutions per minute;
(6) and (3) fifth-stage thermal decomposition: overflowing the solution subjected to thermal decomposition in the step (5) from the fourth reaction kettle to a fifth reaction kettle through a connecting pipe, heating the solution under continuous stirring to enable the temperature of the solution to be raised to a constant temperature of 96 ℃ for decomposition reaction, wherein the reaction time is 30 minutes, and the rotating speed of a stirrer is 30 revolutions per minute;
(7) and (3) purification: and (4) overflowing the solution subjected to thermal decomposition in the step (6) from the fifth reaction kettle to a slurry tank through a connecting pipe, pumping into a centrifugal machine, performing liquid-solid separation and leaching through the centrifugal machine, and then feeding into a dryer to be dried through the dryer to obtain a lithium carbonate dry product.
Example 2
A method for decomposing a lithium bicarbonate solution, the method comprising:
(1) heat exchange: carrying out heat exchange on the lithium bicarbonate solution subjected to precision filtration and the thermal decomposition mother liquor so as to heat the lithium bicarbonate solution to 42 ℃;
(2) first-stage thermal decomposition: pumping the lithium bicarbonate solution subjected to heat exchange in the step (1) into a first reaction kettle, heating the solution under continuous stirring to raise the temperature of the solution to a constant temperature of 60 ℃ for decomposition reaction, wherein the reaction time is 33 minutes, and the rotating speed of a stirrer is 45 revolutions per minute;
(3) second-stage thermal decomposition: overflowing the solution subjected to thermal decomposition in the step (2) from the first reaction kettle to a second reaction kettle through a connecting pipe, heating the solution under continuous stirring to enable the temperature of the solution to be raised to a constant temperature, and keeping the temperature at 70 ℃ for decomposition reaction, wherein the reaction time is 33 minutes, and the rotating speed of a stirrer is 45 revolutions per minute;
(4) third-stage thermal decomposition: overflowing the solution subjected to thermal decomposition in the step (3) from the second reaction kettle to a third reaction kettle through a connecting pipe, heating the solution under continuous stirring to enable the temperature of the solution to be raised to be constant at 80 ℃ for decomposition reaction, wherein the reaction time is 33 minutes, and the rotating speed of a stirrer is 45 revolutions per minute;
(5) fourth-stage thermal decomposition: overflowing the solution subjected to thermal decomposition in the step (4) from the third reaction kettle to a fourth reaction kettle through a connecting pipe, heating the solution under continuous stirring to enable the temperature of the solution to be raised to a constant temperature, and keeping the temperature at 90 ℃ for decomposition reaction, wherein the reaction time is 33 minutes, and the rotating speed of a stirrer is 45 revolutions per minute;
(6) and (3) fifth-stage thermal decomposition: overflowing the solution subjected to thermal decomposition in the step (5) from the fourth reaction kettle to a fifth reaction kettle through a connecting pipe, heating the solution under continuous stirring to enable the temperature of the solution to be raised to a constant temperature, and keeping the constant temperature at 98 ℃ for decomposition reaction, wherein the reaction time is 33 minutes, and the rotating speed of a stirrer is 45 revolutions per minute;
(7) and (3) purification: and (4) overflowing the solution subjected to thermal decomposition in the step (6) from the fifth reaction kettle to a slurry tank through a connecting pipe, pumping into a centrifugal machine, performing liquid-solid separation and leaching through the centrifugal machine, and then feeding into a dryer to be dried through the dryer to obtain a lithium carbonate dry product.
Example 3
A method for decomposing a lithium bicarbonate solution, the method comprising:
(1) heat exchange: carrying out heat exchange on the lithium bicarbonate solution subjected to precision filtration and the thermal decomposition mother liquor so as to heat the lithium bicarbonate solution to 45 ℃;
(2) first-stage thermal decomposition: pumping the lithium bicarbonate solution subjected to heat exchange in the step (1) into a first reaction kettle, heating the solution under continuous stirring to raise the temperature of the solution to a constant temperature of 62 ℃ for decomposition reaction, wherein the reaction time is 36 minutes, and the rotating speed of a stirrer is 60 revolutions per minute;
(3) second-stage thermal decomposition: overflowing the solution subjected to thermal decomposition in the step (2) from the first reaction kettle to a second reaction kettle through a connecting pipe, heating the solution under continuous stirring to enable the temperature of the solution to be raised to be constant at 72 ℃ for decomposition reaction, wherein the reaction time is 36 minutes, and the rotating speed of a stirrer is 60 revolutions per minute;
(4) third-stage thermal decomposition: overflowing the solution subjected to thermal decomposition in the step (3) from the second reaction kettle to a third reaction kettle through a connecting pipe, heating the solution under continuous stirring to enable the temperature of the solution to be raised to a constant temperature of 82 ℃ for decomposition reaction, wherein the reaction time is 36 minutes, and the rotating speed of a stirrer is 60 revolutions per minute;
(5) fourth-stage thermal decomposition: overflowing the solution subjected to thermal decomposition in the step (4) from the third reaction kettle to a fourth reaction kettle through a connecting pipe, heating the solution under continuous stirring to enable the temperature of the solution to be raised to be constant at 92 ℃ for decomposition reaction, wherein the reaction time is 36 minutes, and the rotating speed of a stirrer is 60 revolutions per minute;
(6) and (3) fifth-stage thermal decomposition: overflowing the solution subjected to thermal decomposition in the step (5) from the fourth reaction kettle to a fifth reaction kettle through a connecting pipe, heating the solution under continuous stirring to enable the temperature of the solution to be raised to be constant at 100 ℃ for decomposition reaction, wherein the reaction time is 36 minutes, and the rotating speed of a stirrer is 60 revolutions per minute;
(7) and (3) purification: and (4) overflowing the solution subjected to thermal decomposition in the step (6) from the fifth reaction kettle to a slurry tank through a connecting pipe, pumping into a centrifugal machine, performing liquid-solid separation and leaching through the centrifugal machine, and then feeding into a dryer to be dried through the dryer to obtain a lithium carbonate dry product.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (5)
1. A method for decomposing a lithium bicarbonate solution, the method comprising:
(1) heat exchange: carrying out heat exchange on the lithium bicarbonate solution subjected to precise filtration and a thermal decomposition mother solution so as to heat the lithium bicarbonate solution to 40-45 ℃;
(2) first-stage thermal decomposition: the lithium bicarbonate solution after heat exchange in the step (1) is injected into a first reaction kettle, is heated to raise the temperature of the solution to 60 ℃ under continuous stirring, and is kept at a constant temperature of 58-62 ℃ for decomposition reaction;
(3) second-stage thermal decomposition: overflowing the solution subjected to thermal decomposition in the step (2) from the first reaction kettle to a second reaction kettle through a connecting pipe, heating the solution to enable the temperature of the solution to rise to 70 ℃ under continuous stirring, and keeping the constant temperature at 68-72 ℃ for decomposition reaction;
(4) third-stage thermal decomposition: overflowing the solution subjected to thermal decomposition in the step (3) from the second reaction kettle to a third reaction kettle through a connecting pipe, heating the solution to raise the temperature of the solution to 80 ℃ under continuous stirring, and keeping the constant temperature at 78-82 ℃ for decomposition reaction;
(5) fourth-stage thermal decomposition: overflowing the solution subjected to thermal decomposition in the step (4) from the third reaction kettle to a fourth reaction kettle through a connecting pipe, heating the solution to raise the temperature of the solution to 90 ℃ under continuous stirring, and keeping the constant temperature at 88-92 ℃ for decomposition reaction;
(6) and (3) fifth-stage thermal decomposition: overflowing the solution subjected to thermal decomposition in the step (5) from the fourth reaction kettle to a fifth reaction kettle through a connecting pipe, heating the solution to enable the temperature of the solution to rise to 98 ℃ under continuous stirring, and keeping the constant temperature at 96-100 ℃ to perform decomposition reaction;
(7) and (3) purification: and (4) overflowing the solution subjected to thermal decomposition in the step (6) from the fifth reaction kettle to a slurry tank through a connecting pipe, pumping into a centrifugal machine, performing liquid-solid separation and leaching through the centrifugal machine, and then feeding into a dryer to be dried through the dryer to obtain a lithium carbonate dry product.
2. The method for decomposing a lithium hydrogencarbonate solution according to claim 1, characterized in that: the heating step without stirring comprises the following steps:
stirring continuously by the stirrer of each reaction kettle;
and steam is introduced into the jacket of each reaction kettle to heat the reaction kettles.
3. The method for decomposing the lithium bicarbonate solution according to claim 2, wherein the stirrer is an upturned paddle, and the rotation speed of the stirrer is 30-60 rpm.
4. The method for decomposing a lithium hydrogencarbonate solution according to claim 1, wherein the thermal decomposition mother liquor is filled in the first reaction tank, and when the lithium hydrogencarbonate solution is fed into the first reaction tank, the lithium hydrogencarbonate solution and the thermal decomposition mother liquor are mixed with each other without stirring so that the concentration of lithium hydrogencarbonate in the solution is low.
5. The method for decomposing the lithium bicarbonate solution according to claim 1, wherein the reaction time of the solution in each reaction kettle is 30 to 36 minutes, and the total reaction time of the solution is 150 to 180 minutes.
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Effective date of registration: 20240118 Address after: 338000 North of Yangguan Avenue and East of Quanzhou Avenue in Xinyu High tech Development Zone, Jiangxi Province Patentee after: Jiangxi Chunpeng Lithium Industry Co.,Ltd. Address before: 330072 high tech Economic Development Zone, Xinyu City, Jiangxi Province Patentee before: JIANGXI DONGPENG NEW MATERIALS Co.,Ltd. |