CN104003428A - Method for producing lithium hydroxide by dissolving spodumene out of pipeline reactor - Google Patents
Method for producing lithium hydroxide by dissolving spodumene out of pipeline reactor Download PDFInfo
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- CN104003428A CN104003428A CN201410256305.9A CN201410256305A CN104003428A CN 104003428 A CN104003428 A CN 104003428A CN 201410256305 A CN201410256305 A CN 201410256305A CN 104003428 A CN104003428 A CN 104003428A
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Abstract
The invention provides a method for producing lithium hydroxide by dissolving spodumene out of a pipeline reactor. The method comprises the following steps: carrying out size mixing on water and beta spodumene powder, sodium hydroxide and lime which are obtained by transforming a calcined crystal, delivering into the pipeline reactor by using a pump, mixing by utilizing the flow of slurry in a pipeline, and reacting at a certain temperature and pressure; after the reacted slurry flows out of the pipeline reactor, carrying out solid-liquid separation; and carrying out concentration, impurity removal, crystallization and mother solution circulation on filter liquor to obtain a lithium hydroxide product. The method provided by the invention is simple in lithium hydroxide production process, small in investment, low in production energy consumption and high in lithium extraction rate without sodium sulphate frozen precipitation or sulfuric acid transformation.
Description
Technical field
The invention belongs to ore and put forward lithium technical field, be specifically related to a kind of method of triphane pipeline reactor stripping production lithium hydroxide.
Background technology
Lithium and lithium salts have been expanded to the high-technology fields such as Al-Li alloy, lithium cell, nucleosynthesis as glass-ceramic, electrolytic aluminum, lubricating grease, refrigeration etc. by traditional Application Areas, the explosive type demand growth that particularly new forms of energy may exist for efficient store battery, the technical progress of lithium salts industry has been proposed to urgent challenge, and the lithium minerals of Low-cost is put forward lithium technology the development tool of world's new forms of energy is of great significance.
The production of lithium hydroxide is at present mainly to adopt beta spodumene and sulfuric acid calcination reaction, and reaction slag obtains the solution that contains Lithium Sulphate by leaching, is adding sodium hydroxide through removal of impurities, and the steps such as saltcake are separated out in concentrated frozen cooling, and crystallization obtains monohydrate lithium hydroxide; Or produce lithium hydroxide taking Quilonum Retard as raw material causticization; Or triphane reacts with limestone calcination produces lithium hydroxide.These methods production lithium hydroxide steps are numerous and diverse, and facility investment is large, and raw material consumption is large, and the saltcake of by-product is worth low, and energy consumption is high.
Summary of the invention
The object of the present invention is to provide a kind of triphane pipeline reactor stripping to produce the method for lithium hydroxide, flow process is simple, and less investment does not need freezing separate out saltcake and sulfuric acid conversion, and production energy consumption is low, and lithium extraction yield is high.
For achieving the above object, the present invention adopts following technical scheme:
A kind of method that lithium hydroxide is produced in triphane pipeline reactor stripping comprises the following steps:
1) the beta spodumene powder, sodium hydroxide, lime and the water that calcining crystal formation conversion are obtained are sized mixing, and utilize slurry mobile hybrid reaction of carrying out in pipeline by pump delivery in pipeline reactor;
2), after reaction paste reacts completely under certain temperature and pressure in pipeline reactor, through heat exchange cooling, flow out solid-liquid separation from pipeline;
3) by filtrate by concentrated, removal of impurities, crystallization and Recycling Mother Solution, obtain lithium hydroxide product.
In described beta spodumene powder, contain Lithium Oxide 98min 4.5-6.5wt.%.
The mass ratio of described beta spodumene powder, sodium hydroxide, lime and water is 1:0.05-0.35:0-0.3:1.5-6.
The velocity of flow of reaction paste in pipeline reactor is 0.08-0. 8 meter per seconds.
The reaction times of reaction paste in pipeline reactor is 0.5-5 hour, and temperature of reaction is 90-250 DEG C, and reaction pressure is 0.1-1.5MPa.
Remarkable advantage of the present invention is:
1) in operational path provided by the present invention, beta spodumene does not need and sulfuric acid calcination reaction, with and subsequent the freezing process except saltcake of leaching liquid, step is simple, material consumption is few, energy consumption is lower.
2) pipeline reactor technology of the present invention, equipment is simple, and facility investment greatly reduces.
Embodiment
A method for lithium hydroxide is produced in the stripping of triphane pipeline reactor, carries out according to the following steps:
1) the beta spodumene powder, sodium hydroxide, lime and the water that calcining crystal formation conversion are obtained are sized mixing according to a certain percentage, heat stripping by pump delivery in pipeline reactor;
2), after reaction paste reacts completely under certain temperature, the residence time, pressure in pipeline reactor, after heat exchange cooling, liquid-solid separation is also cleaned filter residue, the solution that the filtrate of acquisition being contained lithium hydroxide;
3) by obtain containing the solution of lithium hydroxide by steps such as concentrated, removal of impurities, crystallization, Recycling Mother Solution, obtain monohydrate lithium hydroxide product;
In raw material beta spodumene fine ore, contain Lithium Oxide 98min 4.5%-6.5%, the weight ratio of the material of sizing mixing is: beta spodumene fine ore: sodium hydroxide: lime: water=1:(0.05-0.35): (0-0.3): (1.5-6).
Pipeline reactor be for can bear peak pressure 1.5MPa, the metallic conduit that front and back that top temperature is 250 DEG C are connected or the metallic conduit of overcoat steam jacket, and reaction paste velocity of flow is therein: 0.08 meter per second-0. 8 meter per second.
Reaction paste was controlled in the velocity of flow of pipeline and the length of pipeline by controlling slurry in the reaction times of pipeline reactor, and the reaction times is: 0.5 hour-5 hours; In pipeline reactor, the temperature range of slurry reaction is: 90 DEG C-250 DEG C, conducted heat and obtained this temperature of reaction from the mode that directly passes into high pressure steam in pipeline by pipeline chuck; In pipeline reactor, reaction pressure is: 0.1 MPa-1.5MPa, is transported to pipeline reactor by slurry transferpump and obtains.
Embodiment 1: the beta spodumene fine ore that contains Lithium Oxide 98min 5% that the conversion of calcining crystal formation is obtained, according to weight ratio be: beta spodumene breeze: sodium hydroxide: lime: water=1:0.15:0.1:2 sizes mixing, by pump delivery in the metallic conduit reactor of the connected metallic conduit in front and back or overcoat steam jacket, reaction paste velocity of flow is therein: 0.10 meter per second, reaction times is: 2.5 hours, reaction pressure is: 0.6 MPa, and the temperature range of reaction is: 90 DEG C-180 DEG C heating strippings; Reaction disposed slurry is after heat exchange cooling, and liquid-solid separation is also cleaned filter residue, the solution that the filtrate of acquisition being contained lithium hydroxide, and in triphane, the solubility rate of lithium reaches 91%; The solution containing lithium hydroxide obtaining, by steps such as concentrated, removal of impurities, crystallizations, is obtained to monohydrate lithium hydroxide product.
Embodiment 2: the beta spodumene fine ore that contains Lithium Oxide 98min 5.5% that the conversion of calcining crystal formation is obtained, according to weight ratio be: beta spodumene breeze: sodium hydroxide: lime: water=1:0.3:0.1:2.5 sizes mixing, by pump delivery in the metallic conduit reactor of the connected metallic conduit in front and back or overcoat steam jacket, reaction paste velocity of flow is therein: 0.30 meter per second, reaction times is: 4.5 hours, reaction pressure is: 0.2MPa, and the temperature range of reaction is: 90 DEG C-130 DEG C heating strippings; Reaction disposed slurry is after heat exchange cooling, and liquid-solid separation is also cleaned filter residue, the solution that the filtrate of acquisition being contained lithium hydroxide, and in triphane, the solubility rate of lithium reaches 92%; The solution containing lithium hydroxide obtaining, by steps such as concentrated, removal of impurities, crystallizations, is obtained to monohydrate lithium hydroxide product.
Embodiment 3: the beta spodumene fine ore that contains Lithium Oxide 98min 5.5% that the conversion of calcining crystal formation is obtained, according to weight ratio be: beta spodumene breeze: sodium hydroxide: lime: water=1:0.3:0.1:2.5 sizes mixing, by pump delivery in the metallic conduit reactor of the connected metallic conduit in front and back or overcoat steam jacket, reaction paste velocity of flow is therein: 0.30 meter per second, reaction times is: 1.5 hours, reaction pressure is: 0.8MPa, and the temperature range of reaction is: 120 DEG C-220 DEG C heating strippings; Reaction disposed slurry is after heat exchange cooling, and liquid-solid separation is also cleaned filter residue, the solution that the filtrate of acquisition being contained lithium hydroxide, and in triphane, the solubility rate of lithium reaches 96%; The solution containing lithium hydroxide obtaining, by steps such as concentrated, removal of impurities, crystallizations, is obtained to monohydrate lithium hydroxide product.
Embodiment 4: the beta spodumene fine ore that contains Lithium Oxide 98min 6.2% that the conversion of calcining crystal formation is obtained, according to weight ratio be: beta spodumene breeze: sodium hydroxide: lime: water=1:0.4:0.1:3.5 sizes mixing, by pump delivery in the metallic conduit reactor of the connected metallic conduit in front and back or overcoat steam jacket, reaction paste velocity of flow is therein: 0.30 meter per second, reaction times is: 3.5 hours, reaction pressure is: 1.2MPa, and the temperature range of reaction is: 120 DEG C-250 DEG C heating strippings; Reaction disposed slurry is after heat exchange cooling, and liquid-solid separation is also cleaned filter residue, the solution that the filtrate of acquisition being contained lithium hydroxide, and in triphane, the solubility rate of lithium reaches 98%; The solution containing lithium hydroxide obtaining, by steps such as concentrated, removal of impurities, crystallizations, is obtained to monohydrate lithium hydroxide product.
Embodiment 5: the beta spodumene fine ore that contains Lithium Oxide 98min 5.2% that the conversion of calcining crystal formation is obtained, according to weight ratio be: beta spodumene breeze: sodium hydroxide: lime: water=1:0.4:0:3.5 sizes mixing, by pump delivery in the metallic conduit reactor of the connected metallic conduit in front and back or overcoat steam jacket, reaction paste velocity of flow is therein: 0.20 meter per second, reaction times is: 2.5 hours, reaction pressure is: 1.0MPa, and the temperature range of reaction is: 120 DEG C-200 DEG C heating strippings; Reaction disposed slurry is after heat exchange cooling, and liquid-solid separation is also cleaned filter residue, the solution that the filtrate of acquisition being contained lithium hydroxide, and in triphane, the solubility rate of lithium reaches 94%; The solution containing lithium hydroxide obtaining, by steps such as concentrated, removal of impurities, crystallizations, is obtained to monohydrate lithium hydroxide product.
Embodiment 6: the beta spodumene fine ore that contains Lithium Oxide 98min 4.5% that the conversion of calcining crystal formation is obtained, according to weight ratio be: beta spodumene breeze: sodium hydroxide: lime: water=1:0.3:0.12:3.5 sizes mixing, by pump delivery in the metallic conduit reactor of the connected metallic conduit in front and back or overcoat steam jacket, reaction paste velocity of flow is therein: 0.78 meter per second, reaction times is: 1.5 hours, reaction pressure is: 1.2MPa, and the temperature range of reaction is: 120 DEG C-250 DEG C heating strippings; Reaction disposed slurry is after heat exchange cooling, and liquid-solid separation is also cleaned filter residue, the solution that the filtrate of acquisition being contained lithium hydroxide, and in triphane, the solubility rate of lithium reaches 95%; The solution containing lithium hydroxide obtaining, by steps such as concentrated, removal of impurities, crystallizations, is obtained to monohydrate lithium hydroxide product.
The foregoing is only preferred embodiment of the present invention, all equalizations of doing according to the present patent application the scope of the claims change and modify, and all should belong to covering scope of the present invention.
Claims (5)
1. a method for lithium hydroxide is produced in the stripping of triphane pipeline reactor, it is characterized in that: comprise the following steps:
1) the beta spodumene powder, sodium hydroxide, lime and the water that calcining crystal formation conversion are obtained are sized mixing, by pump delivery in pipeline reactor;
2) after reaction paste reacts in pipeline reactor, through heat exchange cooling, flow out solid-liquid separation washing from pipeline;
3) by filtrate by concentrated, removal of impurities, crystallization and Recycling Mother Solution, obtain lithium hydroxide product.
2. the method for lithium hydroxide is produced in triphane pipeline reactor stripping according to claim 1, it is characterized in that: described beta spodumene powder is that α triphane is changed and obtained through calcining crystal formation, wherein contains Lithium Oxide 98min 4.5-6.5wt.%.
3. the method for lithium hydroxide is produced in triphane pipeline reactor stripping according to claim 1, it is characterized in that: the mass ratio of described beta spodumene powder, sodium hydroxide, lime, water is 1:0.05-0.35:0-0.3:1.5-6.
4. the method for lithium hydroxide is produced in triphane pipeline reactor stripping according to claim 1, it is characterized in that: the velocity of flow of reaction paste in pipeline reactor is 0.08-0. 8 meter per seconds, utilizes slurry to flow and mix and react in pipeline.
5. the method for lithium hydroxide is produced in triphane pipeline reactor stripping according to claim 1, it is characterized in that: the reaction times of reaction paste in pipeline reactor is 0.5-5 hour, and temperature of reaction is 90-250 DEG C, and reaction pressure is 0.1-1.5MPa.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105439207A (en) * | 2015-11-20 | 2016-03-30 | 王立卓 | Method for preparing lithium nickel cobalt manganese oxide battery cathode material by using quick pipe reactor |
| CN106319245A (en) * | 2016-09-19 | 2017-01-11 | 福州大学 | Lepidolite continuous reaction lithium extracting method |
| WO2018023159A1 (en) * | 2016-08-02 | 2018-02-08 | Lithium Australia Nl | Caustic digestion process |
| CN107739039A (en) * | 2017-10-16 | 2018-02-27 | 福州大学 | A kind of method that defluorinate lepidolite pipeline dissolution carries lithium |
| CN107815557A (en) * | 2017-10-16 | 2018-03-20 | 福州大学 | A kind of spodumene pipe reaction puies forward lithium technique |
| CN109437251A (en) * | 2018-12-11 | 2019-03-08 | 湖南中大联合创新科技发展有限公司 | A method of pressure leaching spodumene, which is activated, using white lime mentions lithium salts |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105439207A (en) * | 2015-11-20 | 2016-03-30 | 王立卓 | Method for preparing lithium nickel cobalt manganese oxide battery cathode material by using quick pipe reactor |
| WO2018023159A1 (en) * | 2016-08-02 | 2018-02-08 | Lithium Australia Nl | Caustic digestion process |
| CN109890990A (en) * | 2016-08-02 | 2019-06-14 | 澳大利亚锂公司 | Caustic digestion method |
| AU2017306576B2 (en) * | 2016-08-02 | 2019-12-12 | Lithium Australia Limited | Caustic digestion process |
| CN109890990B (en) * | 2016-08-02 | 2022-03-04 | 澳大利亚锂公司 | Caustic digestion process |
| CN106319245A (en) * | 2016-09-19 | 2017-01-11 | 福州大学 | Lepidolite continuous reaction lithium extracting method |
| CN107739039A (en) * | 2017-10-16 | 2018-02-27 | 福州大学 | A kind of method that defluorinate lepidolite pipeline dissolution carries lithium |
| CN107815557A (en) * | 2017-10-16 | 2018-03-20 | 福州大学 | A kind of spodumene pipe reaction puies forward lithium technique |
| CN109437251A (en) * | 2018-12-11 | 2019-03-08 | 湖南中大联合创新科技发展有限公司 | A method of pressure leaching spodumene, which is activated, using white lime mentions lithium salts |
| CN109437251B (en) * | 2018-12-11 | 2020-12-08 | 湖南中大联合创新科技发展有限公司 | Method for extracting lithium salt by activating, pressing and immersing spodumene by using hydrated lime |
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