CN103508432A - Synthesis apparatus of lithium hexafluorophosphate - Google Patents
Synthesis apparatus of lithium hexafluorophosphate Download PDFInfo
- Publication number
- CN103508432A CN103508432A CN201310299968.4A CN201310299968A CN103508432A CN 103508432 A CN103508432 A CN 103508432A CN 201310299968 A CN201310299968 A CN 201310299968A CN 103508432 A CN103508432 A CN 103508432A
- Authority
- CN
- China
- Prior art keywords
- shell part
- lithium hexafluorophosphate
- feed
- cylindrical shell
- upper shell
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Landscapes
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention relates to a synthesis apparatus of lithium hexafluorophosphate. The apparatus comprises a cylinder body; the cylinder body is provided with a filter structure dividing the cylinder body into an upper cylinder body and a lower cylinder body; the upper end of the upper cylinder body is provided with a feed part and an exhaust port, the lower end of the upper cylinder is provided with a drain outlet; the upper cylinder body is provided with a cooling crystallization device for cooling the region above the filter structure; and heating and drying device for drying crystalline substances is arranged at the joint of the upper cylinder body and the lower cylinder body. The invention reduces transfer equipment required in the synthesis process of lithium hexafluorophosphate.
Description
Technical field
The present invention relates to use the lithium hexafluorophosphate synthesis device of the synthetic lithium hexafluoro phosphate of sewage hydrofluoric acid solvent method.
Background technology
The excellent properties such as lithium cell is current desirable chemical energy source, and concrete volume is little, electrical capacity large, can repeatedly charge, are widely used in electronic product and ev industries such as mobile telephone, computer power tools.Lithium hexafluoro phosphate is the most widely used electrolyte lithium salt in current commercialization lithium cell, the organic electrolyte that contains lithium hexafluoro phosphate has good electroconductibility and electrochemical stability, lithium hexafluoro phosphate has multiple production method, what be applicable at present fairly large production is to adopt anhydrous hydrofluoric acid solvent method to produce, and needs to use corresponding lithium hexafluorophosphate synthesis device in anhydrous hydrofluoric acid solvent method.Existing lithium hexafluoro phosphate synthetic method as disclosed in Chinese patent literature CN102153064A " a kind of synthetic method of lithium hexafluoro phosphate non-aqueous solvent ", the building-up process of lithium hexafluoro phosphate is: in reaction unit, add in advance the anhydrous hydrogen fluoride solution that contains lithium fluoride, gaseous state phosphorus pentafluoride is also passed in reaction unit, after reaction finishes, decrease temperature crystalline, the reactant containing lithium hexafluoro phosphate that reaction generates is transferred to and in solid product sedimentation device, is carried out separation by output channel, solid product after separation is transferred in drying installation and is dried by output channel, after dry, obtain solid-state lithium hexafluoro phosphate.Wherein reaction unit, solid product sedimentation device and drying installation have formed part lithium hexafluorophosphate synthesis device, the problem that existing this lithium hexafluorophosphate synthesis device exists is: material successively need to carry out transfer through reaction unit, solid product sedimentation device and drying installation etc. in building-up process, transferring equipment is more, technical process is longer, need a large amount of equipment to have enough to meet the need transition, facility investment is large, simultaneously a large amount of HF is as solvent cycle in whole system, and production cost is high; Because equipment is more, between equipment, pipeline connects complexity in addition, in pipeline, easily forms and stops up, and may have influence on normal production, if overhaul not in time discharging, also can directly have influence on the quality of product.
Summary of the invention
The object of the present invention is to provide a kind of lithium hexafluorophosphate synthesis device, to reduce transferring equipment required in lithium hexafluoro phosphate building-up process.
In order to address the above problem, technical scheme of the present invention is:
Lithium hexafluorophosphate synthesis device, comprise device cylindrical shell, in device cylindrical shell, be provided with the filtration that device cylindrical shell is separated into upper and lower shell portion, the upper end of upper shell part offers cylindrical shell opening for feed and venting port, the lower end of upper shell part offers barrel discharge hole, the lower end of lower shell part offers leakage fluid dram, in upper shell part, be provided with the decrease temperature crystalline device for filtration upper area is lowered the temperature, upper shell part is provided with the junction of lower shell part the intensification drying installation being dried for the crystalline material on filtration.
Described decrease temperature crystalline device comprises the refrigerant chuck that is sheathed on upper shell part periphery, and refrigerant chuck has the refrigerant entrance entering for coolant media and the refrigerant exit of discharging for coolant media, and described refrigerant entrance is positioned at the below of refrigerant exit.
Described intensification drying installation comprises the heating agent chuck that is arranged at lower shell part periphery, the heating agent outlet that heating agent chuck has the heating agent entrance entering for thermal medium and discharges for thermal medium, and described heating agent import is positioned at the top of heating agent outlet.
On described cylindrical shell opening for feed, be provided with feed pipe, feed pipe has inlet end setting up and down and exit end, wherein the exit end of feed pipe extends to the inner chamber lower end of upper shell part, the inlet end of feed pipe extends to the outside of upper shell part, and on the inlet end of feed pipe, is provided with gas feed and the material inlet being arranged in parallel.
On described leakage fluid dram, Drainage pipe is set, on Drainage pipe, is provided with mother liquor discharge outlet setting up and down and residual liquid discharge mouth.
The upper end of described upper shell part is provided with mouth spray.
On described venting port, be provided with gas recovery device.
In described upper shell part, be provided with agitator, agitator has height and the agitating vane of the contour setting of described cylindrical shell opening for feed.
Described device cylindrical shell is other is provided with spiral conveyer, and the material inlet of spiral conveyer is communicated with described cylindrical shell opening for feed, and the material outlet of spiral conveyer is connected with sample spliter.
Described sample spliter comprises the Vibrating funnel that is provided with sub-sieve plate, on the Vibrating funnel of sub-sieve plate upside, is provided with product outlet, is provided with waste product outlet on the Vibrating funnel of sub-sieve plate downside.
Beneficial effect of the present invention is: in use, by question response feed liquid and question response gas by cylindrical shell opening for feed adding apparatus cylindrical shell, question response feed liquid and question response gas carry out chemical reaction in device cylindrical shell, decrease temperature crystalline device can be adjusted the envrionment temperature of filtration top conversion zone, resultant of reaction matter (the being lithium hexafluoro phosphate) decrease temperature crystalline that simultaneously decrease temperature crystalline device can also generate the question response feed liquid of filtration top and question response gas reaction, the resultant of reaction matter of filtration below is because temperature is compared with high and seldom have crystallization to occur, resultant of reaction matter after crystallization is filtered structure and filters and stay above filtration, reacted gas is discharged through venting port, reacted feed liquid is discharged through leakage fluid dram, the resultant of reaction matter drying treatment to crystallization by intensification drying installation subsequently, after dry, just obtain solid-state lithium hexafluoro phosphate finished product.The present invention is in the building-up process of lithium hexafluoro phosphate, and synthetic, crystallization and the filtration drying of lithium hexafluoro phosphate are all realized in same device cylindrical shell, have reduced the transferring equipment in synthesizer, have reduced facility investment; Also shorten technical process simultaneously, when shortening product generating period, can also avoid too much equipment interface or too much pipeline to connect the potential safety hazard existing, be convenient to mass production.
Accompanying drawing explanation
Fig. 1 is the structural representation of one embodiment of the present of invention;
Fig. 2 is the structural representation of spiral conveyer in Fig. 1;
Fig. 3 is the left view of Fig. 2.
Embodiment
The embodiment of lithium hexafluorophosphate synthesis device is as shown in Fig. 1 ~ 3: comprise device cylindrical shell 1, in device cylindrical shell, be provided with filtration, filtration comprises the orifice filter 21 with filter pore, filtration is separated into upper shell part 1-1 and lower shell part 1-2 by device cylindrical shell, the upper end of upper shell part is provided with mouth spray, cylindrical shell opening for feed and venting port 27, mouth spray has two, on each mouth spray all according to there being spray header 9; On cylindrical shell opening for feed, be provided with feed pipe 31, feed pipe has inlet end setting up and down and exit end, the inner chamber lower end that wherein exit end of feed pipe extends to upper shell part is until the position of close orifice filter, the inlet end of feed pipe extends to the outside of upper shell part, and on the inlet end of feed pipe, is provided with gas feed 10 and the material inlet 11 being arranged in parallel; On venting port, be provided with gas recovery device 8, gas recovery device is a condensation of gas withdrawer, and the inlet mouth of gas recovery device is communicated with venting port, and the air outlet 28 of gas recovery device is towards the outside of upper shell part.In upper shell part, be provided with agitator 20, the drive-motor 7 of agitator is arranged at the crown center of upper shell part, agitator has the agitating vane 32 of the inner chamber lower end that is positioned at upper shell part, agitating vane, a little more than orifice filter, is also provided with the height barrel discharge hole 29 consistent with agitating vane in upper shell part.The lower end of lower shell part offers leakage fluid dram, and the Drainage pipe of vertical setting is set on leakage fluid dram, is provided with mother liquor discharge outlet 4 setting up and down and residual liquid discharge mouth 5 on Drainage pipe, and raffinate leakage fluid dram is positioned at the end, lower end of Drainage pipe.In upper shell part, be provided with the decrease temperature crystalline device for filtration top is lowered the temperature, decrease temperature crystalline device comprises the refrigerant chuck 2 that is sheathed on upper shell part periphery, refrigerant chuck has the refrigerant entrance 12 entering for coolant media and the refrigerant exit 13 of discharging for coolant media, and refrigerant entrance is positioned at the below of refrigerant exit.Upper shell part is provided with the junction of lower shell part the intensification drying installation being dried for the crystalline material on filtration, intensification drying installation comprises the heating agent chuck 3 that is arranged at lower shell part periphery, the heating agent outlet 15 that heating agent chuck has the heating agent entrance 14 entering for thermal medium and discharges for thermal medium, heating agent import is positioned at the top of heating agent outlet, refrigerant chuck and heating agent chuck belong to prior art, and its concrete structure no longer describes in detail.The other spiral conveyer 24 that is provided with of device cylindrical shell, spiral conveyer is connected with device cylindrical shell by joint flange 35, the material inlet 33 of spiral conveyer is communicated with cylindrical shell opening for feed, the material outlet 30 of spiral conveyer is connected with sample spliter, spiral conveyer is placed in a material guard box 6, on material guard box, be provided with guard box protection gas import and export 22 and observe gathering hole 26, the material outlet of spiral conveyer and sample spliter are flexible coupling by corrugated tube 23, sample spliter comprises the Vibrating funnel 17 that is provided with sub-sieve plate 19, on the Vibrating funnel of sub-sieve plate upside, be provided with product outlet 18, on the Vibrating funnel of sub-sieve plate downside, be provided with waste product outlet 16, on Vibrating funnel, be provided with funnel protector and import and export 22.In figure, part 25 represents the drive-motor of spiral conveyer; Part 34 represents the screw-blade of spiral conveyer.
In use, feed liquid joins in device cylindrical shell by material inlet, turn on agitator, the agitating vane forward of agitator, synthesis gas is by reacting in gas feed access to plant cylindrical shell and with feed liquid, temperature of reaction when refrigerant chuck can be controlled reaction, after reaction finishes, refrigerant chuck passes into the region cooling of coolant media to filtration top, lithium hexafluoro phosphate cooling post crystallization is separated out, reacted gas reclaims through gas recovery device, and discharge through the air outlet of gas recovery device, after feed liquid is filtered via orifice filter, mother liquor is discharged from mother liquor discharge outlet, if orifice filter lower zone produces a small amount of crystallization, crystallization is discharged by residual liquid discharge mouth.After filtration finishes; if needed, can to material, wash by mouth spray; then by pass into thermal medium in heating agent chuck, come lithium hexafluoro phosphate crystallizing and drying; now can also in device cylindrical shell, pass into shielding gas by gas feed; shielding gas is directly passed in the crystallization of orifice filter top, can play good protection effect.After dry end, it is solid-state that lithium hexafluoro phosphate becomes, the agitating vane of reversion agitator, start spiral conveyer simultaneously, solid-state lithium hexafluoro phosphate is deposited in the material inlet place of spiral conveyer gradually, agitating vane can make feed liquid reaction evenly on the one hand, on the other hand for solid-state lithium hexafluoro phosphate being pushed to the material inlet place of spiral conveyer.Spiral conveyer is delivered to solid-state lithium hexafluoro phosphate in material guard box, and enters a preparation minute sample in sample spliter by the material outlet of spiral conveyer.Then open sample spliter, solid-state lithium hexafluoro phosphate slowly enters sample spliter, through sub-sieve plate, finished product is sifted out to product outlet and is packed, and residual waste is discharged by waste outlet, in order to recycling.
The inlet end of feed pipe extends to the position near filter screen, can make synthesis gas react more even with feed liquid on the one hand, also can guarantee on the other hand in lithium hexafluoro phosphate drying process protection gas adequately protecting to lithium hexafluoro phosphate; Refrigerant chuck is arranged at the top of filter screen, can be only to processings of lower the temperature of the region of filter screen top, below the temperature control effect assurance filter screen by hot and cold matchmaker's chuck, there is no or seldom have crystallization; Heating agent chuck is arranged at the link position place of upper and lower shell portion, like this can be directly dry to the lithium hexafluoro phosphate of filter screen top, save energy consumption.The present invention has only used a device cylindrical shell to complete synthetic, crystallization and the filtration drying of product, realized " trinity " of synthetic, crystallization and filtration drying operation, saved the usage quantity of equipment, reduced the connection complexity of pipeline, also the production cycle that has shortened whole product, promoted the handling of technique simultaneously.This patent belongs to project name for the innovation in " lithium ion battery full industrial chain ionogen exploitation ", the project number National 863 project that is 2012AA110402.
In other embodiments of the invention: gas feed and material inlet can not be also to utilize same feed pipe, such as gas feed and material inlet be arranged at respectively on different feed pipes, now two cylindrical shell opening for feeds need to be set in upper shell part; Mouth spray can also not established; Agitator can not be also mechanical stirrer, such as agitator comprises by single Huo Duogen lower end and extends to the inlet pipe in upper shell part, the lower end of inlet pipe sets out pore, with time by pass into high pressure gas in inlet pipe, complete the stirring to feed liquid, now owing to there is no agitating vane, orifice filter can be obliquely installed, barrel discharge hole is arranged at the downside of orifice filter, realizes the conveying of solid-state lithium hexafluoro phosphate by gravity; Orifice filter can also be replaced by filter screen; Refrigerant chuck can also be replaced by the scatterer of other type, such as is the heat exchanger that can absorb cylindrical shell internal heat, and heating agent chuck also can be replaced by other heating unit, such as can be to exothermic heat exchanger in cylindrical shell; The refrigerant entrance of refrigerant chuck can also be positioned at refrigerant exit top or with the contour setting of refrigerant exit; The heating agent outlet of heating agent chuck can also be positioned at heating agent outlet below or export contour setting with heating agent.
Claims (10)
1. lithium hexafluorophosphate synthesis device, it is characterized in that: comprise device cylindrical shell, in device cylindrical shell, be provided with device cylindrical shell is separated into, the filtration of lower shell part, the upper end of upper shell part offers cylindrical shell opening for feed and venting port, the lower end of upper shell part offers barrel discharge hole, the lower end of lower shell part offers leakage fluid dram, in upper shell part, be provided with the decrease temperature crystalline device for filtration upper area is lowered the temperature, upper shell part is provided with the junction of lower shell part the intensification drying installation being dried for the crystalline material on filtration.
2. lithium hexafluorophosphate synthesis device according to claim 1, it is characterized in that: described decrease temperature crystalline device comprises the refrigerant chuck that is sheathed on upper shell part periphery, refrigerant chuck has the refrigerant entrance entering for coolant media and the refrigerant exit of discharging for coolant media, and described refrigerant entrance is positioned at the below of refrigerant exit.
3. lithium hexafluorophosphate synthesis device according to claim 1, it is characterized in that: described intensification drying installation comprises the heating agent chuck that is arranged at lower shell part periphery, the heating agent outlet that heating agent chuck has the heating agent entrance entering for thermal medium and discharges for thermal medium, described heating agent import is positioned at the top of heating agent outlet.
4. lithium hexafluorophosphate synthesis device according to claim 1, it is characterized in that: on described cylindrical shell opening for feed, be provided with feed pipe, feed pipe has inlet end setting up and down and exit end, wherein the exit end of feed pipe extends to the inner chamber lower end of upper shell part, the inlet end of feed pipe extends to the outside of upper shell part, and on the inlet end of feed pipe, is provided with gas feed and the material inlet being arranged in parallel.
5. lithium hexafluorophosphate synthesis device according to claim 1, is characterized in that: on described leakage fluid dram, Drainage pipe is set, is provided with mother liquor discharge outlet setting up and down and residual liquid discharge mouth on Drainage pipe.
6. lithium hexafluorophosphate synthesis device according to claim 1, is characterized in that: the upper end of described upper shell part is provided with mouth spray.
7. lithium hexafluorophosphate synthesis device according to claim 1, is characterized in that: on described venting port, be provided with gas recovery device.
8. according to the lithium hexafluorophosphate synthesis device described in claim 1 ~ 7 any one, it is characterized in that: in described upper shell part, be provided with agitator, agitator has height and the agitating vane of the contour setting of described cylindrical shell opening for feed.
9. lithium hexafluorophosphate synthesis device according to claim 8, is characterized in that: described device cylindrical shell is other is provided with spiral conveyer, and the material inlet of spiral conveyer is communicated with described cylindrical shell opening for feed, and the material outlet of spiral conveyer is connected with sample spliter.
10. lithium hexafluorophosphate synthesis device according to claim 9, it is characterized in that: described sample spliter comprises the Vibrating funnel that is provided with sub-sieve plate, on the Vibrating funnel of sub-sieve plate upside, be provided with product outlet, on the Vibrating funnel of sub-sieve plate downside, be provided with waste product outlet.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310299968.4A CN103508432B (en) | 2013-07-17 | 2013-07-17 | Lithium hexafluorophosphate synthesis device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310299968.4A CN103508432B (en) | 2013-07-17 | 2013-07-17 | Lithium hexafluorophosphate synthesis device |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103508432A true CN103508432A (en) | 2014-01-15 |
| CN103508432B CN103508432B (en) | 2016-01-13 |
Family
ID=49891931
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310299968.4A Active CN103508432B (en) | 2013-07-17 | 2013-07-17 | Lithium hexafluorophosphate synthesis device |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103508432B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106159368A (en) * | 2016-08-24 | 2016-11-23 | 合肥国轩高科动力能源有限公司 | A kind of retracting device for lithium ion battery positive and negative electrode material |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1433960A (en) * | 2003-03-08 | 2003-08-06 | 汕头市金光高科有限公司 | Method and equipment for synthesizing hexafluorophosphate |
| CN102320588A (en) * | 2011-09-05 | 2012-01-18 | 贵州省化工研究院 | Lithium hexafluorophosphate synthesizer |
-
2013
- 2013-07-17 CN CN201310299968.4A patent/CN103508432B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1433960A (en) * | 2003-03-08 | 2003-08-06 | 汕头市金光高科有限公司 | Method and equipment for synthesizing hexafluorophosphate |
| CN102320588A (en) * | 2011-09-05 | 2012-01-18 | 贵州省化工研究院 | Lithium hexafluorophosphate synthesizer |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106159368A (en) * | 2016-08-24 | 2016-11-23 | 合肥国轩高科动力能源有限公司 | A kind of retracting device for lithium ion battery positive and negative electrode material |
| CN106159368B (en) * | 2016-08-24 | 2019-01-08 | 合肥国轩高科动力能源有限公司 | A kind of recyclable device for lithium ion battery positive and negative electrode material |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103508432B (en) | 2016-01-13 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN203486906U (en) | Device for synthesizing lithium hexafluorophosphate | |
| CN104091944B (en) | The preparation method of LiFePO4 | |
| CN106517268B (en) | A kind of waste sulfuric acid from alkylation Sulphuric acid magnesium method and device | |
| CN104401966B (en) | Continuous type production equipment and method of carbon nano tube | |
| CN216170061U (en) | Sublimation crystallization purification device system of vinyl sulfate | |
| CN108808156A (en) | The recovery method of electrolyte in a kind of waste and old lithium ion battery | |
| CN105084370A (en) | Slag slurry treatment method and treatment apparatus in high-pressure low-temperature hydrogenation process | |
| CN105460893A (en) | Method and dedicated device for lithium hexafluorophosphate synthesis tail gas treatment | |
| CN207204078U (en) | A kind of machining graphite steam boiler | |
| CN103508432B (en) | Lithium hexafluorophosphate synthesis device | |
| CN113083204B (en) | NMP synthesis process | |
| WO2016119593A1 (en) | Lithium iron phosphate solvothermal preparation process | |
| CN101817541B (en) | Method and device for separating magnesium chloride hexammoniate during silane production by the magnesium silicide method | |
| CN206121512U (en) | Exhaust gas treatment system | |
| CN203048616U (en) | Continuous pyrolysis tank for high-purity-magnesium water | |
| CN215389170U (en) | Catalyst feeding device | |
| CN202379748U (en) | Reverse disproportionation reaction device for preparing trichlorosilane | |
| CN103936009B (en) | A kind of thermal decomposition of silane produces the device and method of nano level high-purity silicon powder | |
| CN204407414U (en) | LiFePO4 solvent heat Preparation equipment | |
| CN106076238B (en) | Liquid lithium salts micro-pipe reactor and the liquid lithium technology of threonates using the reactor | |
| CN203639168U (en) | Weak acid process-based full-automatic zinc oxide preparation device | |
| CN203379628U (en) | Medium pressure steam-stripping decomposition tower of urea production equipment | |
| CN207361793U (en) | A kind of lithium iron phosphate positive material preparation facilities | |
| CN105217576A (en) | Filtration washing control method in hydrogen fluoride preparation technology | |
| CN106669577B (en) | A kind of closed cycle production and gas recycling device |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CP03 | Change of name, title or address |
Address after: 454191 Henan Province, Jiaozuo City Station area coke Rd Patentee after: Duofudo New Material Co.,Ltd. Address before: 454191, Feng County, Henan Province, Jiaozuo Feng Feng Chemical Industry Zone Patentee before: DO-FLUORIDE CHEMICALS Co.,Ltd. |
|
| CP03 | Change of name, title or address |