CN112522525A - Continuous hydrolysis device and hydrolysis method for metal lithium slag - Google Patents
Continuous hydrolysis device and hydrolysis method for metal lithium slag Download PDFInfo
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- CN112522525A CN112522525A CN202011387651.2A CN202011387651A CN112522525A CN 112522525 A CN112522525 A CN 112522525A CN 202011387651 A CN202011387651 A CN 202011387651A CN 112522525 A CN112522525 A CN 112522525A
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- 238000006460 hydrolysis reaction Methods 0.000 title claims abstract description 158
- 230000007062 hydrolysis Effects 0.000 title claims abstract description 140
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 138
- 239000002893 slag Substances 0.000 title claims abstract description 121
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 96
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 72
- 239000002184 metal Substances 0.000 title claims abstract description 72
- 238000000034 method Methods 0.000 title claims abstract description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 97
- 229910001868 water Inorganic materials 0.000 claims abstract description 97
- 239000007788 liquid Substances 0.000 claims abstract description 58
- 238000005192 partition Methods 0.000 claims abstract description 32
- 238000003825 pressing Methods 0.000 claims abstract description 14
- 238000005086 pumping Methods 0.000 claims abstract description 12
- 239000007787 solid Substances 0.000 claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims description 36
- 238000007667 floating Methods 0.000 claims description 32
- 230000003301 hydrolyzing effect Effects 0.000 claims description 21
- 239000000243 solution Substances 0.000 claims description 19
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 18
- 239000003513 alkali Substances 0.000 claims description 17
- 239000000463 material Substances 0.000 claims description 16
- 238000007599 discharging Methods 0.000 claims description 13
- 239000012670 alkaline solution Substances 0.000 claims description 9
- 239000002912 waste gas Substances 0.000 claims description 9
- 239000002699 waste material Substances 0.000 claims description 7
- 239000007924 injection Substances 0.000 claims description 6
- 238000002347 injection Methods 0.000 claims description 6
- 238000000605 extraction Methods 0.000 claims description 5
- 238000011049 filling Methods 0.000 claims description 5
- 239000013049 sediment Substances 0.000 abstract description 16
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 8
- 239000001301 oxygen Substances 0.000 abstract description 8
- 229910052760 oxygen Inorganic materials 0.000 abstract description 8
- 238000009776 industrial production Methods 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 229910052783 alkali metal Inorganic materials 0.000 abstract description 2
- 150000001340 alkali metals Chemical class 0.000 abstract description 2
- 238000005516 engineering process Methods 0.000 abstract description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 16
- 239000001257 hydrogen Substances 0.000 description 16
- 229910052739 hydrogen Inorganic materials 0.000 description 16
- 230000036632 reaction speed Effects 0.000 description 5
- 239000012535 impurity Substances 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 238000004880 explosion Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000000413 hydrolysate Substances 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 238000005292 vacuum distillation Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 239000005662 Paraffin oil Substances 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 1
- 229910052808 lithium carbonate Inorganic materials 0.000 description 1
- IDBFBDSKYCUNPW-UHFFFAOYSA-N lithium nitride Chemical compound [Li]N([Li])[Li] IDBFBDSKYCUNPW-UHFFFAOYSA-N 0.000 description 1
- FUJCRWPEOMXPAD-UHFFFAOYSA-N lithium oxide Chemical compound [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 description 1
- 229910001947 lithium oxide Inorganic materials 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 238000011085 pressure filtration Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/10—Obtaining alkali metals
- C22B26/12—Obtaining lithium
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/04—Working-up slag
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Materials Engineering (AREA)
- Geology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Manufacturing & Machinery (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention discloses an alkali metal slag treatment technology. The invention relates to a continuous hydrolysis device for metal lithium slag, which comprises a closed hydrolysis tank provided with a water inlet pipe, wherein a top partition plate is arranged in the closed hydrolysis tank, the top partition plate divides the closed hydrolysis tank into an upper independent space and a lower independent space, namely a hydrolysis cavity and an exhaust cavity, and comprises a solid section and a mesh section; the device comprises a pressing device extending into a hydrolysis cavity, the pressing device is connected with a feeding device, a circulating water pump is further arranged, the circulating water pump is connected with a liquid pumping circulating pipe and a liquid returning circulating pipe, the liquid pumping circulating pipe is communicated with the bottom of a closed hydrolysis tank, the liquid returning circulating pipe is communicated with the side wall of the closed hydrolysis tank, an air pumping device communicated with an exhaust cavity is further arranged, and the port of an air pumping cylinder of the air pumping device corresponds to the mesh section of a top partition plate. The device simple structure realizes that the metal lithium sediment hydrolysis process is isolated with oxygen, can avoid burning and exploding, and the metal lithium sediment hydrolysis process can go on in succession, and production efficiency is high, do benefit to industrial production.
Description
Technical Field
The invention relates to an alkali metal slag treatment technology, in particular to a continuous hydrolysis device and a continuous hydrolysis method for metal lithium slag.
Background
The metal lithium is the most ideal cathode material of the high-energy battery due to the specific chemical property, and the compound of the metal lithium plays an irreplaceable role in various industries such as metallurgy, petroleum, chemical engineering, organic synthesis, high-energy batteries, medicine, ceramics, glass, daily necessities and the like. In the process of producing metallic lithium, a residue containing a large amount of metallic lithium, paraffin oil, lithium nitride, lithium oxide, carbon, potassium, sodium, oxides thereof, and the like, called metallic lithium slag, is generated, and the mass thereof is about 3% of the yield of metallic lithium. Because the content of lithium in the metallic lithium slag can reach 50wt%, the economic value is high, and the recycling of the metallic lithium slag has important economic value.
However, the produced lithium metal slag is not suitable for long-time stacking, and as the protective oil film on the surface of the lithium slag becomes thinner along with the increase of the stacking time, the lithium metal can react with water, oxygen and nitrogen in the air, a large amount of generated heat and hydrogen can not be discharged in time, the heat is accumulated gradually, the temperature of the lithium slag is gradually increased, spontaneous combustion and even explosion can occur when the temperature of the lithium slag is accumulated to a certain degree, and fire disasters are caused, so that property loss and personal injury are caused. In areas with heavy rain, high air humidity and high air temperature, the storage of the lithium metal slag is more difficult, so that the rapid and safe recovery and treatment of the lithium metal slag are problems to be solved urgently, and the method has great significance for improving the lithium recovery and utilization efficiency.
The existing lithium metal slag treatment devices comprise three types, the first type is to recover the lithium metal through vacuum distillation, melt filtration or high-temperature combustion, for example, the method and the device used in patents CN201811234901.1 and CN201811229986.4 adopt negative pressure filtration, and the vacuum distillation is combined to realize the direct recovery of the lithium metal in the lithium slag; the second type is that the lithium carbonate is converted for recycling; the third type is direct hydrolysis, and the technical scheme of patent CN201811230878.9 proposes to utilize a layered oil phase and water phase liquid phase system to press the lithium metal slag into the water phase, so that the lithium metal reacts at the water bottom to isolate oxygen, thereby increasing the hydrolysis rate of the lithium slag and avoiding the risk of fire and hydrogen explosion of the lithium slag.
However, the three types of metal lithium slag treatment devices have the problems of complex equipment structure, high requirements on the material and the sealing property of the equipment, high energy consumption during operation and difficulty in realizing industrial production, and the three types of treatment devices cannot realize continuous hydrolysis treatment of metal lithium slag, have low production efficiency and cannot avoid secondary pollutants. Therefore, there is a high necessity for an optimized design of a lithium metal slag treatment apparatus to solve the above problems.
Disclosure of Invention
The invention aims to overcome the technical problems of complex structure, high requirements on the material and the sealing property of equipment, incapability of realizing continuous hydrolysis, low production efficiency and difficulty in realizing industrial production of the conventional lithium metal slag treatment device, and provides a continuous lithium metal slag hydrolysis device and a hydrolysis method.
In order to achieve the above purpose, the invention provides the following technical scheme:
the continuous metal lithium slag hydrolyzing device comprises a closed hydrolyzing tank provided with a water inlet pipe, wherein a top clapboard is arranged in the closed hydrolyzing tank, the top clapboard divides the closed hydrolyzing tank into an upper independent space and a lower independent space which are respectively a hydrolyzing cavity and an exhaust cavity, and the top clapboard comprises a solid body section and a mesh section;
still including stretching into the press device who hydrolysises the chamber, press device links to each other with material feeding unit, still is equipped with circulating water pump outside the closed pond of hydrolysising, circulating water pump even has drawing liquid circulating pipe and liquid return circulating pipe, drawing liquid circulating pipe and closed hydrolysis bottom of the pool portion intercommunication, liquid return circulating pipe and closed hydrolysis lateral wall intercommunication still are equipped with the air exhaust device with the exhaust chamber intercommunication on the closed pond of hydrolysising, air exhaust device's aspirator port corresponds the setting with the mesh section of top baffle.
The continuous metal lithium slag hydrolyzing device is provided with a closed hydrolyzing tank, a top partition plate is arranged in the closed hydrolyzing tank to separate a hydrolyzing cavity for hydrolysis reaction and an exhaust cavity for exhausting reaction waste gas, a liquid pumping circulating pipe communicated with the bottom of the closed hydrolyzing tank pumps out alkali solution after the reaction of metal lithium slag through a circulating water pump, and the alkali solution is pumped into the closed hydrolyzing tank through a liquid returning circulating pipe, so that the liquid on the upper part of the partition plate is the alkali solution with higher concentration, and the newly-fed metal lithium slag in a mesh cylinder above the partition plate cannot immediately undergo hydrolysis reaction when being submerged into the hydrolyzing tank, thereby avoiding the situation that the lithium slag rapidly reacts in pure water, the heat is concentrated in short time and the lithium slag is combusted; the floating oil flow above the hydrolysis cavity can be accelerated through the liquid circulation flow, and the gas extraction device designed corresponding to the mesh section can discharge the hydrogen gas of the hydrolysis product of the metal lithium slag material in time; the pressing device extending into the hydrolysis cavity can directly press the metal lithium slag into the hydrolysis cavity, so that the metal lithium slag is isolated from oxygen when being hydrolyzed, and when the concentration of the alkali solution in the hydrolysis tank meets the requirement, the metal lithium slag can be taken out through a liquid discharge pipe at the bottom of the hydrolysis tank; the device simple structure, and all processes of hydrolysising are all gone on under water, can avoid the metal lithium sediment because of floating the dangerous condition that takes place burning and hydrogen to fire and explode when hydrolysising on the surface of water, and the metal lithium sediment process of hydrolysising can go on in succession simultaneously, and production efficiency is high, do benefit to industrial production.
Preferably, the top baffle plate comprises a flat plate baffle plate and an L-shaped baffle plate, the flat plate baffle plate comprises a solid section and a mesh section, the L-shaped baffle plate is connected with the end of the mesh section of the flat plate baffle plate, and a floating oil collecting groove is formed between the L-shaped baffle plate and the inner wall of the closed hydrolysis tank. Specially designed flat plate separator and L-shaped separator form a floating oil collecting groove, and when the liquid in the hydrolysis cavity circulates, the floating oil generated by the hydrolysis reaction of the metal lithium slag is automatically collected into a floating oil collecting groove by matching with the mesh section of the flat plate separator, and a waste liquid discharging pipe is arranged corresponding to the floating oil collecting groove and used for discharging the floating oil.
Preferably, the vertical plate of the L-shaped partition is connected with the flat partition, and the top end of the vertical plate is higher than the top end face of the flat partition. The top of the vertical plate is higher than the top end face of the flat plate clapboard, is used for limiting the height of the water level in the hydrolysis cavity and collecting the floating oil generated by the hydrolysis reaction.
Preferably, the material pressing device comprises a feeding section cylinder and a reaction section cylinder which are connected into a whole, a screw shaft is arranged in the cylinder, the screw shaft is provided with a screw blade and a driving device for driving the screw shaft to rotate, the feeding section cylinder is provided with a feeding hole, and the reaction section cylinder is positioned in the closed hydrolysis tank. The reaction section cylinder is positioned in the closed hydrolysis tank, so that the lithium metal slag is isolated from oxygen when being hydrolyzed, the lithium metal slag is transported downwards by matching with the selected spiral blade, and after the slag is submerged in water, the spiral blade can enable the slag to be pressed in the water all the time and gradually move downwards, so that the lithium metal slag is always in the water to react in the rotating and moving state; and the length of the reaction section cylinder can be adjusted according to the reaction speed of the lithium metal slag and the rotating speed of the control screw shaft, so that the method is suitable for the particle size and the treatment capacity requirements of different slag materials.
Preferably, the wall of the reaction section cylinder is in a mesh structure, and the air exhaust device is provided with an air exhaust branch pipe communicated with the feeding section cylinder. The reaction section barrel wall structure of mesh structure, the hydrogen and the oil slick that are convenient for metal lithium slag material hydrolysis process to produce discharge along with the rivers in the pond of hydrolysising, and air exhaust device and feed section barrel intercommunication for waste gases such as discharge metal lithium slag material's among the press device hydrolysate hydrogen, the waste gas centralized processing after the collection prevents secondary pollution.
Preferably, the feeding device is a gap feeding device, a hopper is connected between the gap feeding device and the feeding hole, and the hopper and the feeding hole are both positioned above the closed hydrolysis tank. The gap feeding device is suitable for the reaction speed of the metal lithium slag, and the hopper and the feeding hole are positioned above the closed hydrolysis tank.
Preferably, the bottom of the closed hydrolysis tank is provided with a filter screen box, and the end part of the liquid pumping circulation pipe extending into the closed hydrolysis tank is positioned in the filter screen box. Utilize the filter screen box to filter the insoluble impurity in the intracavity of hydrolysising, the protection water pump, reduce the impurity in the alkali solution, can set up the filter screen box in the closed pond bottom of hydrolysising of keeping away from press device one side, the intracavity of being convenient for hydrolysising forms the liquid flow circulation, is favorable to the hydrogen of the sub-regional of top baffle and floats to the flow of top baffle mesh section.
Preferably, the liquid return circulating pipe extends into the closed hydrolysis tank, and the liquid outlet end part of the liquid return circulating pipe is positioned in the exhaust cavity and is arranged corresponding to the reaction section cylinder, so that the pumped alkali solution is poured into the reaction section cylinder. Through the reaction section barrel of mesh structure, the aqueous alkali in returning the liquid circulating pipe is drenched into, can make the liquid of division board upper portion be the higher alkaline liquor of concentration, then the metal lithium sediment of newly advancing in the mesh barrel that is located on the division board can not take place hydrolysis immediately when submerging the pond of hydrolysising, has avoided the lithium sediment to react in the pure water rapidly, and the heat is concentrated in the short time, takes place the condition that the lithium sediment was burnt.
Preferably, the device further comprises an alkaline solution drain pipe, and the end part of the alkaline solution drain pipe extending into the closed hydrolysis tank is positioned in the filter screen box.
Preferably, the inlet tube includes the water inlet main pipe and many inlet branch pipes, many inlet branch pipes all link up with the chamber of hydrolysising through closed pond lateral wall of hydrolysising. The water inlet pipe is used for initial water filling of the hydrolysis tank and water replenishing in the process.
Preferably, the device also comprises a frame, and the closed hydrolysis tank, the circulating water pump and the feeding device are all arranged on the frame.
A hydrolysis method of a continuous metal lithium slag hydrolysis device comprises the following steps of:
A. filling water into a hydrolysis cavity of the closed hydrolysis tank through a water inlet pipe, closing a valve, and continuously injecting water with small water flow; opening a circulating water pump to enable water in the closed hydrolysis tank to start to circularly flow;
B. the metal lithium slag is sent out through the feeding device and the pressing device, and meanwhile, the air exhaust device is opened, so that the metal lithium slag gradually moves from the feeding section cylinder to the reaction section cylinder through the helical blades, and the metal lithium slag is subjected to hydrolysis reaction in a rotating and moving state;
C. under the action of a circulating water pump, floating oil generated by the metal lithium slag hydrolysis reaction passes through the mesh section of the top partition plate and is collected into a floating oil collecting tank, and then is collected and treated through a waste liquid discharge pipe; meanwhile, waste gases such as hydrogen generated by the hydrolysis reaction of the metal lithium slag are collected and treated by an air extractor;
D. after reacting for a period of time, discharging and collecting the lithium hydroxide solution in the hydrolysis cavity through an alkaline solution discharge pipe after the lithium hydroxide solution reaches the extraction concentration, and continuously adding clear water into the hydrolysis cavity through a water inlet pipe;
E. during water injection and liquid drainage, the injection amount of clear water is matched with the feeding amount of the lithium metal slag, and the mass ratio of the feeding amount of the lithium metal slag to the water feeding amount in the same time is lower than 20.
Compared with the prior art, the invention has the beneficial effects that:
1. the device has a simple structure, all the hydrolysis processes are carried out underwater, the condition that the metal lithium slag is burnt due to heat concentration and contact with oxygen when floating on the water surface for hydrolysis is avoided, and the generated hydrolysis heat is transferred and diffused in the hydrolysis tank, so that the problem of explosion of air and hydrogen mixed gas due to the heat concentration on the surface of the hydrolysis tank at present is solved, the production efficiency is high, and the industrial production is facilitated;
2. the specially designed flat plate partition plate and the L-shaped partition plate form a floating oil collecting groove, floating oil generated by the metal lithium slag hydrolysis reaction is automatically collected into a floating oil collecting groove while liquid in a hydrolysis cavity circulates by matching with a mesh section of the flat plate partition plate, and a waste liquid discharging pipe is arranged corresponding to the floating oil collecting groove and used for discharging the floating oil;
3. the reaction section cylinder is positioned in the closed hydrolysis tank, so that the lithium metal slag is prevented from contacting with air in the hydrolysis process, the lithium metal slag is conveyed downwards by matching with the selected spiral blade, and after the slag is submerged in water, the spiral blade can enable the slag to be pressed in the water all the time and gradually move downwards, so that the lithium metal slag is always in water reaction in the rotating and moving state; the length of the reaction section cylinder body can be adjusted according to the reaction speed of the metal lithium slag and the rotating speed of the control screw shaft, so that the method is suitable for different processing requirements;
4. the reaction section cylinder barrel wall structure with the mesh structure is convenient for discharging hydrogen and floating oil generated in the metal lithium slag hydrolysis process along with water flow in the hydrolysis tank, the air exhaust device is communicated with the feeding section cylinder and is used for discharging hydrolysate hydrogen of the metal lithium slag in the material pressing device, and waste gases such as hydrogen collected from the exhaust cavity are intensively treated to prevent secondary pollution;
5. through the reaction section barrel of mesh structure, the aqueous alkali in the liquid circulation pipe that will return drenches into, and the aqueous alkali mixes the back with the metal lithium sediment that newly gets into for the metal lithium sediment that newly gets into can not take place hydrolysis immediately when submerging in the pond of hydrolysising, avoids the lithium sediment to react in pure water rapidly, and the heat is concentrated in the short time, takes place the condition that lithium sediment was burnt.
Description of the drawings:
FIG. 1 is a schematic structural diagram of the continuous hydrolysis device for metal lithium slag.
Fig. 2 is a top view of fig. 1.
Fig. 3 is a schematic structural diagram of the spiral pressing device in the embodiment.
Fig. 4 is a schematic view of the top bulkhead in the embodiment.
FIG. 5 is a schematic structural diagram of a continuous hydrolysis device for lithium metal slag in another embodiment.
The labels in the figure are: 1-frame, 2-circulating water pump, 201-liquid pumping circulating pipe, 202-liquid returning circulating pipe, 3-water inlet pipe, 4-oil pumping pipe, 5-gap feeding device, 6-hopper, 7-material pressing device, 701-motor, 702-motor supporting plate, 703-helical blade, 704-helical shaft, 705-feeding section barrel, 706-reaction section barrel, 8-flat plate partition plate, 801-solid section, 802-mesh section, 9-exhaust fan, 10-closed hydrolysis tank, 11-L partition plate, 12-waste liquid discharging pipe, 13-filter screen box, 14-alkaline solution discharging pipe, a-first valve and b-second valve.
Detailed Description
The present invention will be described in further detail with reference to test examples and specific embodiments. It should be understood that the scope of the above-described subject matter is not limited to the following examples, and any techniques implemented based on the disclosure of the present invention are within the scope of the present invention.
Example 1
As shown in fig. 1 to 4, the continuous hydrolysis device for metal lithium slag of the present embodiment includes a closed hydrolysis tank 10 provided with a water inlet pipe 3, a top partition board is arranged in the closed hydrolysis tank 10, the top partition board divides the closed hydrolysis tank 10 into an upper independent space and a lower independent space, which are a hydrolysis chamber and an exhaust chamber, respectively, and the top partition board includes a solid section and a mesh section;
still including stretching into the press device 7 in the chamber of hydrolysising, press device 7 links to each other with material feeding unit, still is equipped with circulating water pump 2 outside closed hydrolysis tank 10, circulating water pump 2 even has drawing liquid circulating pipe 201 and liquid return circulating pipe 202, drawing liquid circulating pipe 201 and closed hydrolysis tank 10 bottom intercommunication, liquid return circulating pipe 202 and closed hydrolysis tank 10 lateral wall intercommunication, still be equipped with the air exhaust device with the exhaust chamber intercommunication on closed hydrolysis tank 10, air exhaust device's aspirator port corresponds the setting with the mesh section of top baffle.
In this embodiment, the water inlet pipe 3 is provided with a first valve a, and the air extractor is an exhaust fan 9.
The continuous metal lithium slag hydrolyzing device of the embodiment is provided with a closed hydrolyzing tank, a top partition plate is arranged in the closed hydrolyzing tank to separate a hydrolyzing cavity for hydrolysis reaction and an exhaust cavity for exhausting reaction waste gas, a liquid pumping circulating pipe communicated with the bottom of the closed hydrolyzing tank pumps out alkali solution after the reaction of metal lithium slag through a circulating water pump, and the alkali solution is pumped into the closed hydrolyzing tank through a liquid returning circulating pipe, so that part of liquid on the partition plate is the alkali solution with higher concentration, and newly-fed metal lithium slag in a mesh cylinder above the partition plate cannot immediately undergo hydrolysis reaction when being submerged into the hydrolyzing tank, thereby avoiding the situation that the lithium slag rapidly reacts in pure water, the heat is concentrated in short time and the lithium slag is combusted; the floating oil flow above the hydrolysis cavity can be accelerated through the liquid circulation flow, and the gas extraction device designed corresponding to the mesh section can discharge the hydrogen gas of the hydrolysis product of the metal lithium slag material in time; the pressing device extending into the hydrolysis cavity can directly press the metal lithium slag into the hydrolysis cavity, so that the metal lithium slag is isolated from oxygen when being hydrolyzed, and when the concentration of the alkali solution in the hydrolysis tank meets the requirement, the metal lithium slag can be taken out through a liquid discharge pipe at the bottom of the hydrolysis tank; the device simple structure, and all processes of hydrolysising are all gone on under water, can avoid the metal lithium sediment because of floating the dangerous condition that takes place burning and hydrogen to fire and explode when hydrolysising on the surface of water, and the metal lithium sediment process of hydrolysising can go on in succession simultaneously, and production efficiency is high, do benefit to industrial production.
Example 2
As shown in fig. 1 to 4, according to the continuous hydrolysis apparatus for lithium metal slag according to embodiment 1, the top separator of this embodiment includes a flat separator 8 and an L-shaped separator 11, the flat separator 8 includes a solid section 801 and a mesh section 802, the L-shaped separator 11 is connected to an end of the mesh section of the flat separator 8, and a floating oil collecting tank is formed between the L-shaped separator 11 and an inner wall of the closed hydrolysis tank 10. Specially designed flat plate separator and L-shaped separator form a floating oil collecting groove, and when the liquid in the hydrolysis cavity circulates, the floating oil generated by the hydrolysis reaction of the metal lithium slag is automatically collected into a floating oil collecting groove by matching with the mesh section of the flat plate separator, and a waste liquid discharging pipe is arranged corresponding to the floating oil collecting groove and used for discharging the floating oil.
As shown in fig. 1, the L-shaped partition 11 has a riser connected to the flat partition 8, and a top end of the riser is higher than a top end surface of the flat partition 8. The top of the vertical plate is higher than the top end face of the flat plate clapboard, is used for limiting the height of the water level in the hydrolysis cavity and collecting the floating oil generated by the hydrolysis reaction.
Example 3
As shown in fig. 1 to 4, according to the continuous hydrolysis device for lithium metal slag described in embodiment 1 or embodiment 2, the pressing device 7 of this embodiment includes a feeding section cylinder 705 and a reaction section cylinder 706 which are connected into a whole, a screw shaft 704 is disposed in the cylinder, a screw blade 703 is disposed on the screw shaft 704, and a driving device for driving the screw shaft 704 to rotate is disposed, the motor 701 is provided in this embodiment, a feeding port is disposed on the feeding section cylinder 705, a motor support plate 702 is connected to an end of the feeding section cylinder 705, and the reaction section cylinder 706 is located in the closed hydrolysis tank 10. The reaction section cylinder is positioned in the closed hydrolysis tank, so that the lithium metal slag is isolated from oxygen when being hydrolyzed, the lithium metal slag is transported downwards by matching with the selected spiral blade, and after the slag is submerged in water, the spiral blade can enable the slag to be pressed in the water all the time and gradually move downwards, so that the lithium metal slag is always in the water to react in the rotating and moving state; and the length of the reaction section cylinder can be adjusted according to the reaction speed of the lithium metal slag and the rotating speed of the control screw shaft, so that the method is suitable for the particle size and the treatment capacity requirements of different slag materials.
In this embodiment, the wall of the reaction section cylinder 706 is a mesh structure, and the exhaust fan 9 is provided with an exhaust branch pipe communicated with the feeding section cylinder 705. The reaction section barrel wall structure of mesh structure, the hydrogen and the oil slick that are convenient for metal lithium slag material hydrolysis process to produce discharge along with the rivers in the pond of hydrolysising, and air exhaust device and feed section barrel intercommunication for waste gases such as discharge metal lithium slag material's among the press device hydrolysate hydrogen, the waste gas centralized processing after the collection prevents secondary pollution.
Example 4
As shown in fig. 1 to 4, according to the continuous hydrolysis device of lithium metal slag according to one of embodiments 1 to 3, the feeding device 7 of this embodiment is a gap feeding device 5, a hopper 6 is connected between the gap feeding device 5 and the feeding port, the hopper 6 and the feeding port are both located above the closed hydrolysis tank 10, and the gap feeding device 5 is further provided with an oil discharge pipe 4. The gap feeding device is suitable for the reaction speed of the metal lithium slag, and the hopper and the feeding hole are positioned above the closed hydrolysis tank.
Further, a filter screen box 13 is arranged at the bottom of the closed hydrolysis tank 10, and the end of the liquid pumping circulation pipe 201 extending into the closed hydrolysis tank is located in the filter screen box 13. Utilize the filter screen box to filter the insoluble impurity in the intracavity of hydrolysising, the protection water pump, reduce the impurity in the alkali solution, can set up the filter screen box in the closed pond bottom of hydrolysising of keeping away from press device one side, the intracavity of being convenient for hydrolysising forms the liquid flow circulation, is favorable to the hydrogen of the sub-regional of top baffle and floats to the flow of top baffle mesh section.
Furthermore, the liquid-returning circulation pipe 202 extends into the closed hydrolysis tank 10, and the liquid outlet end of the liquid-returning circulation pipe 202 is located in the exhaust cavity and arranged corresponding to the reaction section cylinder 706, so that the pumped alkali solution is poured into the reaction section cylinder 706. Through the reaction section barrel of mesh structure, the aqueous alkali in returning the liquid circulating pipe is drenched into, can make the liquid of division board upper portion be the higher alkaline liquor of concentration, then the metal lithium sediment of newly advancing in the mesh barrel that is located on the division board can not take place hydrolysis immediately when submerging the pond of hydrolysising, has avoided the lithium sediment to react in the pure water rapidly, and the heat is concentrated in the short time, takes place the condition that the lithium sediment was burnt.
In this embodiment, the device further comprises an alkaline solution drain pipe 14, wherein the end of the alkaline solution drain pipe 14 extending into the closed hydrolysis tank is positioned in the filter screen box 13, and a second valve b is arranged on the alkaline solution drain pipe 14.
Further, inlet tube 3 includes that the water inlet is responsible for and many water inlet branch pipe, many water inlet branch pipe all hydrolyzes 10 lateral walls of pond and the chamber intercommunication of hydrolysising through the closed. The water inlet pipe is used for initial water filling of the hydrolysis tank and water replenishing in the process.
In the embodiment, the device further comprises a rack 1, and the closed hydrolysis tank 10, the circulating water pump 2 and the feeding device 7 are all arranged on the rack.
Example 5
As shown in fig. 5, the continuous hydrolysis apparatus for lithium metal slag of the present embodiment includes a plurality of sets of closed hydrolysis tanks 10, and is correspondingly configured with the gap feeding apparatus 5, the pressing apparatus 7 and other components as described in any one of embodiments 1 to 4, so as to satisfy the situation of larger lithium metal slag processing capacity.
Example 6
As shown in fig. 1 to 5, the hydrolysis method of the continuous hydrolysis device for lithium metal slag according to the embodiment, when the continuous hydrolysis device for lithium metal slag according to one of embodiments 1 to 5 is used for treating lithium metal slag, includes the following steps:
A. filling water into a hydrolysis cavity of the closed hydrolysis tank through a water inlet pipe, closing a valve, and continuously injecting water with small water flow; opening a circulating water pump to enable water in the closed hydrolysis tank to start to circularly flow;
B. the metal lithium slag is sent out through the feeding device and the pressing device, and meanwhile, the air exhaust device is opened, so that the metal lithium slag gradually moves from the feeding section cylinder to the reaction section cylinder through the helical blades, and the metal lithium slag is subjected to hydrolysis reaction in a rotating and moving state;
C. under the action of a circulating water pump, floating oil generated by the metal lithium slag hydrolysis reaction passes through the mesh section of the top partition plate and is collected into a floating oil collecting tank, and then is collected and treated through a waste liquid discharge pipe; meanwhile, hydrogen generated by the hydrolysis reaction of the metal lithium slag is collected and treated by an air extractor;
D. after reacting for a period of time, discharging and collecting the lithium hydroxide solution in the hydrolysis cavity through an alkaline solution discharge pipe after the lithium hydroxide solution reaches the extraction concentration, and continuously adding clear water into the hydrolysis cavity through a water inlet pipe;
E. during water injection and liquid drainage, the injection amount of clear water is matched with the feeding amount of the lithium metal slag, and the mass ratio of the feeding amount of the lithium metal slag to the water feeding amount in the same time is lower than 20.
Claims (10)
1. The continuous hydrolysis device for the metal lithium slag is characterized by comprising a closed hydrolysis tank provided with a water inlet pipe, wherein a top partition plate is arranged in the closed hydrolysis tank, the top partition plate divides the closed hydrolysis tank into an upper independent space and a lower independent space, namely a hydrolysis cavity and an exhaust cavity, and the top partition plate comprises a solid section and a mesh section;
still including stretching into the press device who hydrolysises the chamber, press device links to each other with material feeding unit, still is equipped with circulating water pump outside the closed pond of hydrolysising, circulating water pump even has drawing liquid circulating pipe and liquid return circulating pipe, drawing liquid circulating pipe and closed hydrolysis bottom of the pool portion intercommunication, liquid return circulating pipe and closed hydrolysis lateral wall intercommunication still are equipped with the air exhaust device with the exhaust chamber intercommunication on the closed pond of hydrolysising, air exhaust device's aspirator port corresponds the setting with the mesh section of top baffle.
2. The continuous lithium metal slag hydrolyzing device as claimed in claim 1, wherein the top baffle comprises a plate baffle and an L-shaped baffle, the plate baffle comprises a solid section and a mesh section, the L-shaped baffle is connected with the end of the mesh section of the plate baffle, and a floating oil collecting groove is formed between the L-shaped baffle and the inner wall of the closed hydrolyzing tank.
3. The continuous hydrolysis device for the metal lithium slag according to claim 2, wherein a vertical plate of the L-shaped partition is connected to the flat partition, and a top end of the vertical plate is higher than a top end surface of the flat partition.
4. The continuous hydrolysis device for the metal lithium slag charge according to any one of claims 1 to 3, wherein the pressing device comprises a feeding section cylinder and a reaction section cylinder which are connected into a whole, a screw shaft is arranged in the cylinder, a screw blade is arranged on the screw shaft, a driving device for driving the screw shaft to rotate is arranged on the screw shaft, a feeding hole is arranged on the feeding section cylinder, and the reaction section cylinder is positioned in the closed hydrolysis tank.
5. The continuous hydrolysis device for the metal lithium slag charge according to claim 4, wherein the wall of the reaction section cylinder is a mesh structure, and the air exhaust device is provided with an air exhaust branch pipe communicated with the feed section cylinder.
6. The continuous hydrolysis device for the metal lithium slag charge according to claim 5, wherein the feeding device is a gap feeding device, a hopper is connected between the gap feeding device and the feeding port, and the hopper and the feeding port are both positioned above the closed hydrolysis tank.
7. The continuous hydrolysis device for the metal lithium slag charge according to claim 5 or 6, wherein a filter screen box is arranged at the bottom of the closed hydrolysis tank, and the end part of the liquid pumping circulation pipe, which extends into the closed hydrolysis tank, is positioned in the filter screen box.
8. The continuous hydrolysis device for the metal lithium slag charge according to claim 5 or 6, wherein the liquid return circulation pipe extends into the closed hydrolysis tank, and the liquid outlet end part of the liquid return circulation pipe is positioned in the exhaust cavity and is arranged corresponding to the reaction section cylinder, so that the pumped alkali solution is poured into the reaction section cylinder.
9. The continuous hydrolysis device for the metal lithium slag charge according to claim 8, wherein the water inlet pipe comprises a main water inlet pipe and a plurality of branch water inlet pipes, and the plurality of branch water inlet pipes are communicated with the hydrolysis cavity through the side wall of the closed hydrolysis tank.
10. A hydrolysis method of a continuous hydrolysis device for lithium metal slag, which is characterized in that when the continuous hydrolysis device for lithium metal slag of any one of claims 5 to 9 is used for processing lithium metal slag, the method comprises the following steps:
A. filling water into a hydrolysis cavity of the closed hydrolysis tank through a water inlet pipe, closing a valve, and continuously injecting water with small water flow; opening a circulating water pump to enable water in the closed hydrolysis tank to start to circularly flow;
B. the metal lithium slag is sent out through the feeding device and the pressing device, and meanwhile, the air exhaust device is opened, so that the metal lithium slag gradually moves from the feeding section cylinder to the reaction section cylinder through the helical blades, and the metal lithium slag is subjected to hydrolysis reaction in a rotating and moving state;
C. under the action of a circulating water pump, floating oil generated by the metal lithium slag hydrolysis reaction passes through the mesh section of the top partition plate and is collected into a floating oil collecting tank, and then is collected and treated through a waste liquid discharge pipe; meanwhile, collecting and treating waste gas generated by the hydrolysis reaction of the metal lithium slag through an air extractor;
D. after reacting for a period of time, discharging and collecting the lithium hydroxide solution in the hydrolysis cavity through an alkaline solution discharge pipe after the lithium hydroxide solution reaches the extraction concentration, and continuously adding clear water into the hydrolysis cavity through a water inlet pipe;
E. during water injection and liquid drainage, the injection amount of clear water is matched with the feeding amount of the lithium metal slag, and the mass ratio of the feeding amount of the lithium metal slag to the water feeding amount in the same time is lower than 20.
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