CN109399673A - Lithia water decomposition method - Google Patents
Lithia water decomposition method Download PDFInfo
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- CN109399673A CN109399673A CN201811589102.6A CN201811589102A CN109399673A CN 109399673 A CN109399673 A CN 109399673A CN 201811589102 A CN201811589102 A CN 201811589102A CN 109399673 A CN109399673 A CN 109399673A
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- reaction kettle
- solution
- temperature
- decomposition
- lithia water
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- 238000000354 decomposition reaction Methods 0.000 title claims abstract description 58
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 229910001947 lithium oxide Inorganic materials 0.000 title claims abstract description 48
- 238000000034 method Methods 0.000 title claims abstract description 35
- 238000006243 chemical reaction Methods 0.000 claims abstract description 114
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims abstract description 29
- 229910052808 lithium carbonate Inorganic materials 0.000 claims abstract description 29
- 239000012452 mother liquor Substances 0.000 claims abstract description 16
- HQRPHMAXFVUBJX-UHFFFAOYSA-M lithium;hydrogen carbonate Chemical compound [Li+].OC([O-])=O HQRPHMAXFVUBJX-UHFFFAOYSA-M 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 6
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 5
- 239000001257 hydrogen Substances 0.000 claims abstract description 5
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims abstract description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 4
- 238000005979 thermal decomposition reaction Methods 0.000 claims description 45
- 238000003756 stirring Methods 0.000 claims description 40
- 230000035484 reaction time Effects 0.000 claims description 20
- 238000000926 separation method Methods 0.000 claims description 7
- 239000002002 slurry Substances 0.000 claims description 7
- 238000010828 elution Methods 0.000 claims description 6
- 238000010792 warming Methods 0.000 claims description 6
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 claims 1
- 238000001035 drying Methods 0.000 abstract description 10
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 239000002253 acid Substances 0.000 abstract description 2
- 238000000197 pyrolysis Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 description 16
- 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
- 230000008569 process Effects 0.000 description 4
- 239000003638 chemical reducing agent Substances 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000001816 cooling Methods 0.000 description 2
- 239000012043 crude product Substances 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000012824 chemical production Methods 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
Classifications
-
- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention discloses a kind of lithia water decomposition method, this method includes one, heat exchange: by the lithia water Jing Guo secondary filter and thermally decomposing mother liquor progress heat exchange；Two, the first order thermally decomposes；Three, the second level thermally decomposes；Four, the third level thermally decomposes；Five, the fourth stage thermally decomposes；Six, level V thermally decomposes；Seven, it purifies.The effect of lithia water decomposition method provided by the invention is: technical solution is simple and easy, the method that the present invention decomposes control decomposition rate using low carbon acid hydrogen lithium concentration in reaction system and step, to achieve the purpose that reduce lithium bicarbonate package in lithium carbonate product, product quality preferably ensure that.Pyrolysis device continuous operation is high-efficient.Lithium carbonate product drying equipment can use steam heating, drying, it is no longer necessary to be dried using far infrared high temperature, reduce energy consumption, improve safety.
Description
Technical field
The present invention relates to chemical production technical fields, more particularly to a kind of lithia water decomposition method.
Background technique
Currently, since lithium electricity industry all uses the higher battery-level lithium carbonate of purity although other industries will use industry
Level lithium carbonate, but dosage is seldom, so industrial level lithium carbonate or crude product lithium carbonate are largely purified as battery-level lithium carbonate.
Purifying industrial level lithium carbonate or crude product lithium carbonate are that the method for battery lithium carbonate is usually all depth carbonizatin method, i.e., logical
It crosses carbon dioxide to react with lithium carbonate, generates soluble lithium bicarbonate, then by removing impurity, reheat and decompose, obtain battery
The lithium carbonate product of level lithium carbonate or higher purity.
Under normal circumstances, the thermal decomposition of lithium bicarbonate is all to complete entire decomposable process in a reaction kettle, i.e., by carbon
Sour hydrogen lithium solution squeezes into reaction kettle, steam heating is led in collet, lithium bicarbonate is thermally decomposed, and after the completion of to be decomposed, then is carried out
Solid-liquor separation.It is also enclosed with a small amount of lithium bicarbonate in the lithium carbonate product obtained in this way, generally 1.8% or so, and wraps up
It is not easily decomposed when the steam drying of lithium bicarbonate inside, only drying temperature could be decomposed gradually to 350 DEG C or more.Thus
This wet product of lithium carbonate must carry out high temperature drying using coated infrared drier, compared with steam-heated disk dryer,
Coated infrared drier equipment investment is high, energy consumption is high, production efficiency is low, operation and maintenance are more troublesome.
Summary of the invention
Based on this, the embodiment of the present invention proposes a kind of lithia water decomposition method, and it is low to solve existing production efficiency
Problem.
One embodiment of the invention provides a kind of lithia water decomposition method, and specific technical solution is as follows:
A kind of lithia water decomposition method, which comprises
(1) heat exchange: by the lithia water Jing Guo secondary filter and mother liquor progress heat exchange is thermally decomposed, so that described
Lithia water is warming up to 40~45 DEG C；
(2) first order thermally decomposes: the lithia water after step (1) heat exchange is squeezed into the first reaction kettle
It is interior, in the case where keeping stirring, heated so that solution temperature is increased to 60 DEG C, and constant temperature is kept to carry out decomposing instead at 58~62 DEG C
It answers；
(3) second level thermally decomposes: the solution after step (2) thermal decomposition is reacted by connecting tube by described first
In kettle overflow to the second reaction kettle, in the case where keeping stirring, heated so that the solution temperature is increased to 70 DEG C, and keeps permanent
Temperature is in 68~72 DEG C of progress decomposition reactions；
(4) third level thermally decomposes: the solution after step (3) thermal decomposition is reacted by connecting tube by described second
In kettle overflow to third reaction kettle, in the case where keeping stirring, heated so that the solution temperature is increased to 80 DEG C, and keeps permanent
Temperature is in 78~82 DEG C of progress decomposition reactions；
(5) fourth stage thermally decomposes: the solution after step (4) thermal decomposition is reacted by connecting tube by the third
In kettle overflow to the 4th reaction kettle, in the case where keeping stirring, heated so that the solution temperature is increased to 90 DEG C, and keeps permanent
Temperature is in 88~92 DEG C of progress decomposition reactions；
(6) level V thermally decomposes: the solution after step (5) thermal decomposition is by connecting tube by the 4th reaction
In kettle overflow to the 5th reaction kettle, in the case where keeping stirring, heated so that the solution temperature is increased to 98 DEG C, and keeps permanent
Temperature is in 96~100 DEG C of progress decomposition reactions；
(7) purify: by step (6) thermal decomposition after the solution pass through connecting tube by the 5th reaction kettle overflow extremely
Slurry vessel, and squeeze into centrifuge, it to carry out solid-liquor separation and elution by the centrifuge, enters back into dryer, with logical
The dryer is crossed to be dried to obtain lithium carbonate dryed product.
The embodiment of the present invention decomposes the decomposition rate of control lithia water by Pyatyi step, to reach lithium carbonate production
The purpose that lithium bicarbonate package is reduced in product preferably ensure that product quality, each reaction kettle continuous operation imitate production
Rate is high, solves the problems, such as that existing production efficiency is low.
Further, described in the case where keeping stirring, the step of heating are as follows:
It is kept stirring by the blender of each reaction kettle；
Heating to reaction kettle is realized to steam is passed through in the collet of each reaction kettle.
Further, the blender is upper-turn-type blade, and the revolving speed of the blender is 30~60 revs/min.
Further, first reaction kettle is provided with the thermal decomposition mother liquor, and the lithia water enters to institute
It is lower so that the lithia water is mixed with the thermal decomposition mother liquor, so that molten keeping stirring when stating the first reaction kettle
The concentration of lithium bicarbonate is lower in liquid.
Further, each reaction kettle controls different reaction temperatures, and is kept substantially temperature constant state.Described first is anti-
Answering the control of kettle temperature degree is 58~62 DEG C, and the second temperature of reaction kettle control is 68~72 DEG C, the third temperature of reaction kettle control
78~82 DEG C are made as, the 4th temperature of reaction kettle control is 88~92 DEG C, and the 5th temperature of reaction kettle control is 96~100
℃。
Further, reaction time of the solution in each reaction kettle is 30~36 minutes, the solution it is total anti-
It is 150~180 minutes between seasonable.
Detailed description of the invention
Fig. 1 is the flow chart for the lithia water decomposition method that the embodiment of the present invention proposes.
Fig. 2 is the production technological process for the lithia water decomposition method that the embodiment of the present invention proposes.
Specific embodiment
In order to make the foregoing objectives, features and advantages of the present invention clearer and more comprehensible, with reference to the accompanying drawing to the present invention
Specific embodiment be described in detail.Many details are explained in the following description in order to fully understand this hair
It is bright.But the invention can be embodied in many other ways as described herein, those skilled in the art can be not
Similar improvement is done in the case where violating intension of the present invention, therefore the present invention is not limited to the specific embodiments disclosed below.
Fig. 1 is please referred to, for the flow chart for the lithia water decomposition method that the embodiment of the present invention proposes, this method packet
It includes:
Step S11, heat exchange: by the lithia water Jing Guo secondary filter and thermally decomposing mother liquor progress heat exchange, with
The lithia water is set to be warming up to 40~45 DEG C.
First order thermal decomposition: the lithia water after step S11 heat exchange is squeezed into first by step S12
In reaction kettle, in the case where keeping stirring, heated so that solution temperature is increased to 60 DEG C, and constant temperature is kept to carry out at 58~62 DEG C
Decomposition reaction.
First order thermal decomposition: the lithia water after step S12 heat exchange is squeezed into first by step S13
In reaction kettle, in the case where keeping stirring, heated so that solution temperature is increased to 60 DEG C, and constant temperature is kept to carry out at 58~62 DEG C
Decomposition reaction.
Step S14, third level thermal decomposition: the solution after step S13 thermal decomposition is by connecting tube by described the
In two reaction kettle overflows to third reaction kettle, in the case where keeping stirring, heated so that the solution temperature is increased to 80 DEG C, and
Keep constant temperature in 78~82 DEG C of progress decomposition reactions.
Step S15, fourth stage thermal decomposition: the solution after step S14 thermal decomposition is by connecting tube by described the
In three reaction kettle overflows to the 4th reaction kettle, in the case where keeping stirring, heated so that the solution temperature is increased to 90 DEG C, and
Keep constant temperature in 88~92 DEG C of progress decomposition reactions.
Step S16, level V thermal decomposition: the solution after step S15 thermal decomposition is by connecting tube by described the
In four reaction kettle overflows to the 5th reaction kettle, in the case where keeping stirring, heated so that the solution temperature is increased to 98 DEG C, and
Keep constant temperature in 96~100 DEG C of progress decomposition reactions.
Step S17, purification: the solution after step S16 thermal decomposition is by connecting tube by the 5th reaction kettle
Overflow is squeezed into centrifuge to slurry vessel, to carry out solid-liquor separation and elution by the centrifuge, is entered back into drying
Machine, to be dried to obtain lithium carbonate dryed product by the dryer.
Wherein, which carries out decomposition reaction to lithia water by five reaction kettles arranged in parallel,
In, the reaction kettle include autoclave body, the driving motor set on autoclave body top middle portion and speed reducer, be set to autoclave body inside and with driving electricity
The blender and collet set on autoclave body outer wall of machine and speed reducer connection, wherein on the side wall of autoclave body it is opposite be equipped with feed inlet and
Discharge port, the outer wall upper and lower side of autoclave body are equipped with the inlet and outlet of connection collet, and autoclave body top is connected with gas outlet.It is wherein each
The discharge port of reaction kettle is connect by connecting tube with the feed inlet of next reaction kettle.
The mode wherein kept stirring is to drive blender by driving motor and speed reducer, passes through each reaction kettle
Interior blender realization keeps stirring the solution in reaction kettle, so that realizing mixing thoroughly for solution, wherein blender is upper
Formula blade is turned over, and the revolving speed of blender is 30~60 revs/min；The mode wherein heated is the collet to each reaction kettle
It is inside passed through steam and realizes heating to reaction kettle, be specially passed through steam in entrance steam is placed in collet and be condensed into
By outlet outflow to realize the heating to reaction kettle after liquid.Wherein it should be understood that the import can also be passed through cooling water with
Realize the cooling to reaction kettle.Wherein each reaction kettle controls different reaction temperatures, and is kept substantially temperature constant state.First
Temperature of reaction kettle control is 58~62 DEG C, and the control of the second temperature of reaction kettle is 68~72 DEG C, and the control of third temperature of reaction kettle is 78
~82 DEG C, the control of the 4th temperature of reaction kettle is 88~92 DEG C, and the control of the 5th temperature of reaction kettle is 96~100 DEG C.
Wherein, as shown in Fig. 2, lithia water and thermal decomposition mother liquor by secondary filter carry out heat exchange, heat is handed over
Lithia water after changing is squeezed by the feed inlet of the first reaction kettle to the first reaction kettle, wherein in first reaction kettle
It is pre-loaded with thermal decomposition mother liquor, it is lower so that lithium bicarbonate is molten keeping stirring when lithia water enters to the first reaction kettle
Liquid is mixed with thermal decomposition mother liquor, so that the lower solution of lithium bicarbonate concentration is formed in the first reaction kettle, wherein anti-first
Under the stirring and heating of answering kettle, maintain solution temperature in 58~62 DEG C of progress decomposition reactions, the lithia water after heating is opened
Beginning is gradually decomposed to form lithium carbonate, and the carbon dioxide for decomposing generation is discharged from the gas outlet on the first reaction kettle top, and be discharged
Carbon dioxide is recycled in carbon dioxide storage tank through compressor compresses.Wherein, reaction time of the solution in each reaction kettle is
30~36 minutes, the total reaction time of solution was 150~180 minutes.
Its while the continuous continuous-stable of solution enters the first reaction kettle, through the solution that mixing and heat up constantly by
The discharge port of first reaction kettle enters to the feed inlet of the second reaction kettle by connecting tube continuous overflow, to flow into the second reaction
It is stirred and heats up in kettle, above-mentioned according to this, solution passes through connecting tube continuous overflow under by the discharge port of each reaction kettle
In the feed inlet of one reaction kettle, finally by the discharge port overflow of the 5th reaction kettle positioned at end into slurry vessel, wherein each
Solution in reaction kettle carries out decomposition reaction and forms lithium carbonate, and the temperature of each reaction kettle is stepped up, so that solution
Decomposition rate is gradually accelerated, so that remaining lower lithium bicarbonate from the solution that the discharge port of the 5th reaction kettle flows out, simultaneously
Its solution continuously carries out continuous decomposition reaction by the first reaction kettle into the 5th reaction kettle, so that operational efficiency is high.
Further, the solution after decomposition is squeezed into centrifuge and is passed through pure water and be centrifuged and elute, with
To the wet product of battery-level lithium carbonate, wherein the lithium bicarbonate content in the wet product of the lithium carbonate is within 0.3%, using drying
Machine steam heating, drying, obtains battery-level lithium carbonate dryed product.Wherein, it is passed through by the thermal decomposition mother liquor that centrifuge is separated
The burden process after heat exchange cooling for previous step is crossed, it is small to be periodically discharged one after thermal decomposition mother liquor impurity content increases
Part is to keep the balance of impurity to guarantee qualified product；Wherein recycling is stored to the carbon dioxide of carbon dioxide storage tank
In depth carbonation process needed for can be used for producing lithium carbonate, so that carbon dioxide is recycled.
Beneficial effects of the present invention: 1, technical solution is simple and easy, and the present invention is dense using low carbon acid hydrogen lithium in reaction system
The method that degree and step decompose control decomposition rate, to achieve the purpose that reduce lithium bicarbonate package in lithium carbonate product, more preferably
Ensure that product quality.2, each reaction kettle continuous operation is high-efficient in thermal decomposition.3, drying equipment can be added using steam
Heat drying, it is no longer necessary to be dried using far infrared high temperature, reduce energy consumption, improve safety.
Embodiment 1
A kind of lithia water decomposition method, this method comprises:
(1) heat exchange: by the lithia water Jing Guo secondary filter and mother liquor progress heat exchange is thermally decomposed, so that described
Lithia water is warming up to 40 DEG C；
(2) first order thermally decomposes: the lithia water after step (1) heat exchange is squeezed into the first reaction kettle
It is interior, in the case where keeping stirring, heated so that solution temperature is increased to keep constant temperature in 58 DEG C of progress decomposition reactions, reaction time
30 minutes, the revolving speed of blender was 30 revs/min；
(3) second level thermally decomposes: the solution after step (2) thermal decomposition is reacted by connecting tube by described first
In kettle overflow to the second reaction kettle, in the case where keeping stirring, heated so that the solution temperature is increased to keep constant temperature 68
DEG C decomposition reaction is carried out, the reaction time 30 minutes, the revolving speed of blender was 30 revs/min；
(4) third level thermally decomposes: the solution after step (3) thermal decomposition is reacted by connecting tube by described second
In kettle overflow to third reaction kettle, in the case where keeping stirring, heated so that the solution temperature is increased to keep constant temperature 78
DEG C decomposition reaction is carried out, the reaction time 30 minutes, the revolving speed of blender was 30 revs/min；
(5) fourth stage thermally decomposes: the solution after step (4) thermal decomposition is reacted by connecting tube by the third
In kettle overflow to the 4th reaction kettle, in the case where keeping stirring, heated so that the solution temperature is increased to keep constant temperature 88
DEG C decomposition reaction is carried out, the reaction time 30 minutes, the revolving speed of blender was 30 revs/min；
(6) level V thermally decomposes: the solution after step (5) thermal decomposition is by connecting tube by the 4th reaction
In kettle overflow to the 5th reaction kettle, in the case where keeping stirring, heated so that the solution temperature is increased to keep constant temperature 96
DEG C decomposition reaction is carried out, the reaction time 30 minutes, the revolving speed of blender was 30 revs/min；
(7) purify: by step (6) thermal decomposition after the solution pass through connecting tube by the 5th reaction kettle overflow extremely
Slurry vessel, and squeeze into centrifuge, it to carry out solid-liquor separation and elution by the centrifuge, enters back into dryer, with logical
The dryer is crossed to be dried to obtain lithium carbonate dryed product.
Embodiment 2
A kind of lithia water decomposition method, this method comprises:
(1) heat exchange: by the lithia water Jing Guo secondary filter and mother liquor progress heat exchange is thermally decomposed, so that described
Lithia water is warming up to 42 DEG C；
(2) first order thermally decomposes: the lithia water after step (1) heat exchange is squeezed into the first reaction kettle
It is interior, in the case where keeping stirring, heated so that solution temperature is increased to keep constant temperature in 60 DEG C of progress decomposition reactions, reaction time
33 minutes, the revolving speed of blender was 45 revs/min；
(3) second level thermally decomposes: the solution after step (2) thermal decomposition is reacted by connecting tube by described first
In kettle overflow to the second reaction kettle, in the case where keeping stirring, heated so that the solution temperature is increased to keep constant temperature 70
DEG C decomposition reaction is carried out, the reaction time 33 minutes, the revolving speed of blender was 45 revs/min；
(4) third level thermally decomposes: the solution after step (3) thermal decomposition is reacted by connecting tube by described second
In kettle overflow to third reaction kettle, in the case where keeping stirring, heated so that the solution temperature is increased to keep constant temperature 80
DEG C decomposition reaction is carried out, the reaction time 33 minutes, the revolving speed of blender was 45 revs/min；
(5) fourth stage thermally decomposes: the solution after step (4) thermal decomposition is reacted by connecting tube by the third
In kettle overflow to the 4th reaction kettle, in the case where keeping stirring, heated so that the solution temperature is increased to keep constant temperature 90
DEG C decomposition reaction is carried out, the reaction time 33 minutes, the revolving speed of blender was 45 revs/min；
(6) level V thermally decomposes: the solution after step (5) thermal decomposition is by connecting tube by the 4th reaction
In kettle overflow to the 5th reaction kettle, in the case where keeping stirring, heated so that the solution temperature is increased to keep constant temperature 98
DEG C decomposition reaction is carried out, the reaction time 33 minutes, the revolving speed of blender was 45 revs/min；
(7) purify: by step (6) thermal decomposition after the solution pass through connecting tube by the 5th reaction kettle overflow extremely
Slurry vessel, and squeeze into centrifuge, it to carry out solid-liquor separation and elution by the centrifuge, enters back into dryer, with logical
The dryer is crossed to be dried to obtain lithium carbonate dryed product.
Embodiment 3
A kind of lithia water decomposition method, this method comprises:
(1) heat exchange: by the lithia water Jing Guo secondary filter and mother liquor progress heat exchange is thermally decomposed, so that described
Lithia water is warming up to 45 DEG C；
(2) first order thermally decomposes: the lithia water after step (1) heat exchange is squeezed into the first reaction kettle
It is interior, in the case where keeping stirring, heated so that solution temperature is increased to keep constant temperature in 62 DEG C of progress decomposition reactions, reaction time
36 minutes, the revolving speed of blender was 60 revs/min；
(3) second level thermally decomposes: the solution after step (2) thermal decomposition is reacted by connecting tube by described first
In kettle overflow to the second reaction kettle, in the case where keeping stirring, heated so that the solution temperature is increased to keep constant temperature 72
DEG C decomposition reaction is carried out, the reaction time 36 minutes, the revolving speed of blender was 60 revs/min；
(4) third level thermally decomposes: the solution after step (3) thermal decomposition is reacted by connecting tube by described second
In kettle overflow to third reaction kettle, in the case where keeping stirring, heated so that the solution temperature is increased to keep constant temperature 82
DEG C decomposition reaction is carried out, the reaction time 36 minutes, the revolving speed of blender was 60 revs/min；
(5) fourth stage thermally decomposes: the solution after step (4) thermal decomposition is reacted by connecting tube by the third
In kettle overflow to the 4th reaction kettle, in the case where keeping stirring, heated so that the solution temperature is increased to keep constant temperature 92
DEG C decomposition reaction is carried out, the reaction time 36 minutes, the revolving speed of blender was 60 revs/min；
(6) level V thermally decomposes: the solution after step (5) thermal decomposition is by connecting tube by the 4th reaction
In kettle overflow to the 5th reaction kettle, in the case where keeping stirring, heated so that the solution temperature is increased to keep constant temperature 100
DEG C decomposition reaction is carried out, the reaction time 36 minutes, the revolving speed of blender was 60 revs/min；
(7) purify: by step (6) thermal decomposition after the solution pass through connecting tube by the 5th reaction kettle overflow extremely
Slurry vessel, and squeeze into centrifuge, it to carry out solid-liquor separation and elution by the centrifuge, enters back into dryer, with logical
The dryer is crossed to be dried to obtain lithium carbonate dryed product.
In the description of this specification, reference term " one embodiment ", " some embodiments ", " example ", " specifically show
The description of example " or " some examples " etc. means specific features, structure, material or spy described in conjunction with this embodiment or example
Point is included at least one embodiment or example of the invention.In the present specification, schematic expression of the above terms are not
Centainly refer to identical embodiment or example.Moreover, particular features, structures, materials, or characteristics described can be any
One or more embodiment or examples in can be combined in any suitable manner.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
Limitations on the scope of the patent of the present invention therefore cannot be interpreted as.It should be pointed out that for those of ordinary skill in the art
For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to guarantor of the invention
Protect range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (6)
1. a kind of lithia water decomposition method, which is characterized in that the described method includes:
(1) heat exchange: by the lithia water Jing Guo secondary filter and mother liquor progress heat exchange is thermally decomposed, so that the carbonic acid
Hydrogen lithium solution is warming up to 40 ~ 45 DEG C；
(2) first order thermally decomposes: the lithia water after step (1) heat exchange is squeezed into the first reaction kettle,
In the case where keeping stirring, heated so that solution temperature is increased to 60 DEG C, and keeps constant temperature in 58 ~ 62 DEG C of progress decomposition reactions；
(3) second level thermally decomposes: the solution after step (2) thermal decomposition is overflow by connecting tube by first reaction kettle
It flow in the second reaction kettle, in the case where keeping stirring, is heated so that the solution temperature is increased to 70 DEG C, and constant temperature is kept to exist
68 ~ 72 DEG C of progress decomposition reactions；
(4) third level thermally decomposes: the solution after step (3) thermal decomposition is overflow by connecting tube by second reaction kettle
It flow in third reaction kettle, in the case where keeping stirring, is heated so that the solution temperature is increased to 80 DEG C, and constant temperature is kept to exist
78 ~ 82 DEG C of progress decomposition reactions；
(5) fourth stage thermally decomposes: the solution after step (4) thermal decomposition is overflow by connecting tube by the third reaction kettle
It flow in the 4th reaction kettle, in the case where keeping stirring, is heated so that the solution temperature is increased to 90 DEG C, and constant temperature is kept to exist
88 ~ 92 DEG C of progress decomposition reactions；
(6) level V thermally decomposes: the solution after step (5) thermal decomposition is overflow by connecting tube by the 4th reaction kettle
It flow in the 5th reaction kettle, in the case where keeping stirring, is heated so that the solution temperature is increased to 98 DEG C, and constant temperature is kept to exist
96 ~ 100 DEG C of progress decomposition reactions；
(7) purify: the solution after step (6) thermal decomposition is by connecting tube by the 5th reaction kettle overflow to slurry
Slot, and squeeze into centrifuge, to carry out solid-liquor separation and elution by the centrifuge, enter back into dryer, to pass through
Dryer is stated to be dried to obtain lithium carbonate dryed product.
2. lithia water decomposition method according to claim 1, it is characterised in that: it is described in the case where keeping stirring, into
The step of row heating are as follows:
It is kept stirring by the blender of each reaction kettle；
Heating to reaction kettle is realized to steam is passed through in the collet of each reaction kettle.
3. lithia water decomposition method according to claim 2, which is characterized in that the blender is upper-turn-type paddle
Leaf, the revolving speed of the blender are 30 ~ 60 revs/min.
4. lithia water decomposition method according to claim 1, which is characterized in that first reaction kettle is provided with
The thermal decomposition mother liquor, it is lower so that the carbon keeping stirring when the lithia water enters to first reaction kettle
Sour hydrogen lithium solution is mixed with the thermal decomposition mother liquor, so that the concentration of lithium bicarbonate is lower in solution.
5. lithia water decomposition method according to claim 1, which is characterized in that each reaction kettle controls different
Reaction temperature, and it is kept substantially temperature constant state；The first temperature of reaction kettle control is 58 ~ 62 DEG C, second reaction kettle
Temperature control is 68 ~ 72 DEG C, and third temperature of reaction kettle control is 78 ~ 82 DEG C, the 4th temperature of reaction kettle control for 88 ~
92 DEG C, the 5th temperature of reaction kettle control is 96 ~ 100 DEG C.
6. lithia water decomposition method according to claim 1, which is characterized in that the solution is in each reaction kettle
In reaction time be 30 ~ 36 minutes, the total reaction time of the solution is 150 ~ 180 minutes.
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| CN106315629A (en) * | 2016-08-30 | 2017-01-11 | 山东瑞福锂业有限公司 | Technology for preparing high-purity lithium carbonate through recovering of battery-grade lithium carbonate lithium precipitation mother liquor |
| CN107188206A (en) * | 2017-06-27 | 2017-09-22 | 瓮福（集团）有限责任公司 | A kind of lithium salts process for refining |
| EP2855735B1 (en) * | 2012-05-30 | 2018-03-07 | Nemaska Lithium Inc. | Processes for preparing lithium carbonate |
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| EP2855735B1 (en) * | 2012-05-30 | 2018-03-07 | Nemaska Lithium Inc. | Processes for preparing lithium carbonate |
| CN103833053A (en) * | 2014-01-21 | 2014-06-04 | 四川天齐锂业股份有限公司 | Method of preparing high-purity lithium carbonate of the 5 N grade |
| CN106315629A (en) * | 2016-08-30 | 2017-01-11 | 山东瑞福锂业有限公司 | Technology for preparing high-purity lithium carbonate through recovering of battery-grade lithium carbonate lithium precipitation mother liquor |
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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. |