CN102320588A - Lithium hexafluorophosphate synthesizer - Google Patents
Lithium hexafluorophosphate synthesizer Download PDFInfo
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- CN102320588A CN102320588A CN201110259731A CN201110259731A CN102320588A CN 102320588 A CN102320588 A CN 102320588A CN 201110259731 A CN201110259731 A CN 201110259731A CN 201110259731 A CN201110259731 A CN 201110259731A CN 102320588 A CN102320588 A CN 102320588A
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Abstract
The invention discloses a lithium hexafluorophosphate synthesizer. The lithium hexafluorophosphate synthesizer is characterized in that a tank (1) comprises a cylindrical straight tube part, an upper head and a lower head; a cooling medium jacket (2) is arranged between an inner wall (3) and an outer cylinder; a cooling medium outlet (4) and a cooling medium inlet (11) are arranged on the tank (1); an appliance (5) for measuring temperatures, pressure and liquid levels, a vent valve (6) and a circulating gas outlet (7) are arranged on the upper head; an outlet pipe of a Venturi tube (8) enters into the tank through the upper head; the Venturi tube is connected with a circulating pump (9); a liquid feed tube is installed on the circulating pump (9); a gas circulation tube and a gas feed tube are installed on the circulating gas outlet (7) and the Venturi tube (8); and a mouth (10) for liquid entrance, discharge and circulation and a liquid discharge tube (23) are arranged on the lower head. The lithium hexafluorophosphate synthesizer adopts the Venturi principle to synthesize lithium hexafluorophosphate. Through the lithium hexafluorophosphate synthesizer, phosphorus pentafluoride gas and a lithium fluoride nonaqueous solution can undergo an effective gas-liquid mixing reaction in a Venturi tube and unreacted raw material gas is subjected to circulation absorption in the Venturi tube. Therefore, the lithium hexafluorophosphate synthesizer can improve reaction efficiency and a raw material utilization ratio, and reduce an equipment investment.
Description
Technical field: the present invention relates to lithium ion battery electrolyte lithium hexafluoro phosphate producing apparatus, particularly a kind of lithium hexafluoro phosphate synthesizer.
Background technology: lithium hexafluoro phosphate (LiPF
6) be most popular electrolyte lithium salt in the present commercialization lithium ion battery.The compound method of lithium hexafluoro phosphate has hydrogen fluoride (HF) solvent method, organic solvent (acetonitrile, ethers, ester class etc. are as solvent) method, gas-solid method and ion exchange method etc., but can realize suitability for industrialized production now still have only the hydrogen fluoride solvent method.Hydrogen fluoride solvent method and organic solvent method are that lithium fluoride (LiF) is dissolved in liquid anhydrous HF or the organic solvent (or being suspended in organic solvent) as solute, feed phosphorus pentafluoride (PF then
5) gas reaction generation lithium hexafluoro phosphate, reaction equation is:
LiF+PF
5→LiPF
6
This reaction is the gas-liquid two-phase reaction, and gas-liquid two-phase blended efficient is comparatively remarkable to the influence of speed of reaction, raw material availability and transformation efficiency.Because the price of the synthetic raw materials used especially phosphorus pentafluoride of lithium hexafluoro phosphate is comparatively expensive, it is significant for enhancing productivity, reducing production costs therefore to improve two phase hybrid reaction efficient.The technology that is used for the gas-liquid mixed reaction at present mainly contains aeration, absorption tower absorption and venturi tube absorption etc.Venturi principle is when fluid flows through restraining mass, and pressure is relatively low near the back side of restraining mass, thereby produces adsorption and cause the mixed flow of adsorbed another phase fluid and this phase fluid.When fluid passes through venturi tube, because the rapid variation of pressure, flow velocity can produce a series of cavitation effects (like high temperature, high pressure, high-speed micro-jet and generation radical etc.) and reinforcement fluidic mixing effect.Venturi tube absorbs the fields such as flue gas desulfurization, water cycle vacuum pump and mass transport that have been widely used in, but have so far venturi principle is not applied to lithium hexafluoro phosphate synthetic report.
More about lithium hexafluoro phosphate synthetic patent and academic documents at present, but mostly pay attention to the preparation and the purification of lithium hexafluoro phosphate with phosphorus pentafluoride, and less to the report of the HF solution reaction efficient of raising phosphorus pentafluoride gas and lithium fluoride.Patent CN 1210810A proposes the gaseous mixture of phosphorus pentafluoride gas or phosphorus pentafluoride and HCl and the hydrogen fluoride solution of lithium fluoride are carried out contact reacts in the absorption tower.This method gas-to-liquid contact is abundant, and reaction efficiency is high, but exists the required equipment volume bigger, invests bigger problem.Patent CN101544361A realizes the gas-liquid mixed reaction with phosphorus pentafluoride gas and HF liquid through tubular reactor.In order to improve the hybrid reaction effect, tubular reactor needs long crooked pipeline.There are problems such as mixing duct is long, device structure is complicated, the easy obstruction of pipeline in this method.Patent CN101423207A feeds the gaseous state phosphorus pentafluoride in the ultramicro air bubble generating unit, after the generation diameter is the microbubble of 0.1～2000 μ m, with the lithium fluoride reaction that is dissolved in anhydrous hydrogen fluoride in advance.This method through micro-pore aeration can improve gas-liquid mixed efficient, but owing to HF, PF
5Corrodibility bigger, the material of micro-hole aerator is required very high, also have the risk in the phosphofluoric acid crystalline lithium blocking aeration hole of reaction generation when lithium fluoride concentration is high simultaneously.For improving the utilization ratio of unreacted phosphorus pentafluoride, patent CN 101570328A will react the unreacted phosphorus pentafluoride gas in back and continue to be passed in another anhydrous hydrogen fluoride solution that fills lithium fluoride, continue reaction and obtain the lithium hexafluoro phosphate finished product.Through increasing the utilization ratio that conversion unit improves the raw material phosphorus pentafluoride, increased facility investment greatly like this.Therefore in order to overcome the deficiency of prior art, improve the efficient and the utilization ratio of the non-aqueous solvent solution reaction of phosphorus pentafluoride gas and lithium fluoride, the present invention adopts venturi tube to realize raw material gas-liquid hybrid reaction, and makes unreacted virgin gas be able to the absorption reaction that circulates.
Summary of the invention: the object of the present invention is to provide a kind of lithium hexafluoro phosphate synthesizer; It is to utilize thorough mixing, the contact reacts of venturi principle with the non-aqueous solvent solution of realization phosphorus pentafluoride gas and lithium fluoride; And the unreacted virgin gas of circulation absorption, solve the problem and shortage that above-mentioned prior art exists.
Formation of the present invention: form by tank body, venturi tube, recycle pump, pipeline and valve; Tank body is made up of cylindrical straight drum part and last lower cover, and straight drum part is cylindrical, between inwall and urceolus, is provided with the heat-eliminating medium chuck; Upper cover is a circular arc; Lower cover is taper, and the outlet of cooling medium inlet and heat-eliminating medium is arranged on tank body, and temperature, pressure, liquid level measurer, vent valve, gas circulation outlet are arranged on upper cover; The outlet pipe of venturi tube gets in the straight tube of tank body through upper cover; The liquid circulation inlet pipe of venturi tube is connected with recycle pump, and liquid feed pipe is housed on recycle pump, on gas circulation outlet and venturi tube, gas circulating tube and gas feed-pipe is housed; Liquid turnover loop exit is arranged on lower cover, on liquid turnover loop exit, the liquid extraction line is housed.
Gas-liquid mixed partly adopts venturi tube to realize effective mixing of gas-liquid, and realizes the circulation absorption reaction of unreacting gas, and venturi tube is made up of collapsible tube, trunnion, increaser, nozzle and outlet damper, the angle of collapsible tube and trunnion
1Be 0-60 °, preferred 15 °, the angle of increaser and trunnion
2Be 0～60 °, preferred 7 °.
Upper cover also can be done tapered or flat cover; Lower cover also can be made circular arc or flat.
The tank body of said device, venturi tube and recycle pump are processed by ability anhydrous HF corrosive material such as tetrafluoroethylene, polyfluorinated ethylene, 316L stainless steel, 904L stainless steel or Hastelloy; Perhaps realize anti-HF corrosion function through applying tetrafluoro coating, preferred 316L stainless steel applies tetrafluoro coating.
Compare with prior art, the invention has the beneficial effects as follows that the non-aqueous solvent solution of phosphorus pentafluoride gas and lithium fluoride can be realized effective hybrid reaction of gas-liquid in venturi tube; Unreacted gas can be realized the circulation absorption reaction through venturi tube, improves reaction efficiency and utilization ratio of raw materials, reduces facility investment.
Description of drawings: Fig. 1 is a lithium hexafluoro phosphate synthesizer synoptic diagram, and Fig. 2 is the venturi tube structural representation, and Fig. 3 is the A-A sectional view of Fig. 2.
Among the figure: 1, tank body, 2, the heat-eliminating medium chuck, 3, inwall, 4, the heat-eliminating medium outlet, 5, temperature, pressure, liquid level measurer, 6, vent valve; 7, gas circulation outlet, 8, venturi tube, 9, recycle pump, 10, liquid turnover loop exit, 11, cooling medium inlet, 12, by-pass valve control A; 13, by-pass valve control B, 14, by-pass valve control C, 15, by-pass valve control D, 16, by-pass valve control E, 17, by-pass valve control F, 18, gas circulating tube; 19, gas feed pipe, 20, outlet pipe, 21, the liquid circulation inlet pipe, 22, liquid feed pipe, 23, the liquid extraction line; 24, collapsible tube, 25, trunnion, 26, increaser, 27, nozzle, 28, outlet damper.
Embodiment: shown in Fig. 1-3, a kind of lithium hexafluoro phosphate synthesizer is made up of tank body, venturi tube, recycle pump, pipeline and valve; Tank body 1 is made up of cylindrical straight drum part and last lower cover, and straight drum part is cylindrical, between inwall 3 and urceolus, is provided with heat-eliminating medium chuck 2; Upper cover is a circular arc; Lower cover is taper, and heat-eliminating medium outlet 4 and cooling medium inlet 11 are arranged on tank body 1, and temperature, pressure, liquid level measurer 5, vent valve 6, gas circulation outlet 7 are arranged on upper cover; The outlet pipe 20 of venturi tube 8 gets in the straight tube of tank body 1 through upper cover; The liquid circulation inlet pipe 21 of venturi tube is connected with recycle pump 9, and liquid feed pipe 22 is housed on recycle pump 9, on gas circulation outlet 7 and venturi tube 8, gas circulating tube 18 and gas feed-pipe 19 is housed; Liquid turnover loop exit 10 is arranged on lower cover, on liquid turnover loop exit 10, liquid extraction line 23 is housed.
Venturi tube 8 is made up of collapsible tube 24, trunnion 25, increaser 26, nozzle 27 and outlet damper 28, the angle of collapsible tube 24 and trunnion 25
1Be 0-60 °, preferred 15 °, the angle of increaser 26 and trunnion 25
2Be 0～60 °, preferred 7 °.
Upper cover also can be done tapered or flat cover, and lower cover also can be made circular arc or flat.
The tank body of said device, venturi tube and recycle pump are processed by ability anhydrous HF corrosive material tetrafluoroethylene, polyfluorinated ethylene, 316L stainless steel, 904L stainless steel, Hastelloy; Perhaps realize anti-HF corrosion function through applying tetrafluoro coating, preferred 316L stainless steel applies tetrafluoro coating.
By-pass valve control F17 is arranged on gas circulating tube 18; By-pass valve control E16 is arranged on gas feed pipe 19; By-pass valve control D15 is arranged on liquid circulation inlet pipe 21, by-pass valve control A12 and by-pass valve control C14 are arranged on liquid feed pipe 22, by-pass valve control B13 is arranged on liquid extraction line 23.
Claims (4)
1. lithium hexafluoro phosphate synthesizer; Form by tank body, venturi tube, recycle pump, pipeline and valve; It is characterized in that: tank body (1) is made up of cylindrical straight drum part and last lower cover, and straight drum part is cylindrical, between inwall (3) and urceolus, is provided with heat-eliminating medium chuck (2); Upper cover is a circular arc; Lower cover is taper, and heat-eliminating medium outlet (4) and cooling medium inlet (11) are arranged on tank body (1), and temperature, pressure, liquid level measurer (5), vent valve (6), gas circulation outlet (7) are arranged on upper cover; The outlet pipe (20) of venturi tube (8) gets in the straight tube of tank body (1) through upper cover; The liquid circulation inlet pipe (21) of venturi tube is connected with recycle pump (9), and liquid feed pipe (22) is housed on recycle pump (9), on gas circulation outlet (7) and venturi tube (8), gas circulating tube (18) and gas feed-pipe (19) is housed; Liquid turnover loop exit (10) is arranged on lower cover, on liquid turnover loop exit (10), liquid extraction line (23) is housed.
2. lithium hexafluoro phosphate synthesizer according to claim 1; It is characterized in that: gas-liquid mixed partly adopts venturi tube to realize effective mixing of gas-liquid; And the circulation absorption reaction of realization unreacting gas; Venturi tube (8) is made up of collapsible tube (24), trunnion (25), increaser (26), nozzle (27) and outlet damper (28), the angle of collapsible tube (24) and trunnion (25)
1Be 0-60 °, preferred 15 °, the angle of increaser (26) and trunnion (25)
2Be 0～60 °, preferred 7 °.
3. lithium hexafluoro phosphate synthesizer according to claim 1 is characterized in that: upper cover also can be done tapered or flat cover; Lower cover also can be made circular arc or flat.
4. lithium hexafluoro phosphate synthesizer according to claim 1; It is characterized in that: the tank body of said device, venturi tube and recycle pump are processed by ability anhydrous HF corrosive material such as tetrafluoroethylene, polyfluorinated ethylene, 316L stainless steel, 904L stainless steel or Hastelloy etc.; Perhaps realize anti-HF corrosion function through applying tetrafluoro coating, preferred 316L stainless steel applies tetrafluoro coating.
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|---|---|---|---|
| CN 201110259731 CN102320588B (en) | 2011-09-05 | 2011-09-05 | Lithium hexafluorophosphate synthesizer |
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|---|---|---|---|
| CN 201110259731 CN102320588B (en) | 2011-09-05 | 2011-09-05 | Lithium hexafluorophosphate synthesizer |
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| CN102320588A true CN102320588A (en) | 2012-01-18 |
| CN102320588B CN102320588B (en) | 2013-03-13 |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103508432A (en) * | 2013-07-17 | 2014-01-15 | 多氟多化工股份有限公司 | Synthesis apparatus of lithium hexafluorophosphate |
| CN105561896A (en) * | 2016-01-28 | 2016-05-11 | 杭州海虹精细化工有限公司 | Efficient gas-liquid reaction device |
| CN105668538A (en) * | 2016-01-15 | 2016-06-15 | 江苏新泰材料科技股份有限公司 | Crystallization method of lithium hexafluorophosphate |
| CN108671705A (en) * | 2018-06-22 | 2018-10-19 | 江苏昌吉利新能源科技有限公司 | Device is absorbed and utilized in a kind of venturi VOC |
| CN109997249A (en) * | 2017-06-07 | 2019-07-09 | 株式会社Lg化学 | The battery unit of electrolyte, battery pack can be reinjected, reinject system and electrolyte for battery pack reinjects method for the electrolyte of battery pack |
| CN112551565A (en) * | 2021-01-07 | 2021-03-26 | 岳阳明科催化技术有限公司 | Carbonizing device and method for producing macroporous pseudo-boehmite by carbonization method |
| CN114794442A (en) * | 2022-05-23 | 2022-07-29 | 福建胜美鲜生物科技有限公司 | Method and device for brewing fish sauce by microbial fermentation |
| CN116825215A (en) * | 2023-02-28 | 2023-09-29 | 福建省龙德新能源有限公司 | Fluid circulation reaction control system and method for lithium hexafluorophosphate preparation |
Citations (4)
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|---|---|---|---|---|
| US6387340B1 (en) * | 1998-12-31 | 2002-05-14 | Ulsan Chemical Co., Ltd. | Manufacturing method for lithium hexafluoro phosphate |
| CN101570327A (en) * | 2008-04-28 | 2009-11-04 | 多氟多化工股份有限公司 | Method for producing lithium hexafluorophosphate |
| CN201634427U (en) * | 2009-12-10 | 2010-11-17 | 多氟多化工股份有限公司 | Device for synthesizing lithium hexafluorophosphate |
| CN202279694U (en) * | 2011-09-05 | 2012-06-20 | 贵州省化工研究院 | Lithium hexafluorophosphate synthesis device |
-
2011
- 2011-09-05 CN CN 201110259731 patent/CN102320588B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6387340B1 (en) * | 1998-12-31 | 2002-05-14 | Ulsan Chemical Co., Ltd. | Manufacturing method for lithium hexafluoro phosphate |
| CN101570327A (en) * | 2008-04-28 | 2009-11-04 | 多氟多化工股份有限公司 | Method for producing lithium hexafluorophosphate |
| CN201634427U (en) * | 2009-12-10 | 2010-11-17 | 多氟多化工股份有限公司 | Device for synthesizing lithium hexafluorophosphate |
| CN202279694U (en) * | 2011-09-05 | 2012-06-20 | 贵州省化工研究院 | Lithium hexafluorophosphate synthesis device |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103508432A (en) * | 2013-07-17 | 2014-01-15 | 多氟多化工股份有限公司 | Synthesis apparatus of lithium hexafluorophosphate |
| CN103508432B (en) * | 2013-07-17 | 2016-01-13 | 多氟多化工股份有限公司 | Lithium hexafluorophosphate synthesis device |
| CN105668538A (en) * | 2016-01-15 | 2016-06-15 | 江苏新泰材料科技股份有限公司 | Crystallization method of lithium hexafluorophosphate |
| CN105561896A (en) * | 2016-01-28 | 2016-05-11 | 杭州海虹精细化工有限公司 | Efficient gas-liquid reaction device |
| CN109997249A (en) * | 2017-06-07 | 2019-07-09 | 株式会社Lg化学 | The battery unit of electrolyte, battery pack can be reinjected, reinject system and electrolyte for battery pack reinjects method for the electrolyte of battery pack |
| US11081765B2 (en) | 2017-06-07 | 2021-08-03 | Lg Chem, Ltd. | Battery cell refillable with electrolyte, battery pack, electrolyte refilling system for battery pack, and electrolyte refilling method for battery pack |
| CN109997249B (en) * | 2017-06-07 | 2022-03-04 | 株式会社Lg化学 | Electrolyte re-injection system for battery pack and method thereof |
| CN108671705A (en) * | 2018-06-22 | 2018-10-19 | 江苏昌吉利新能源科技有限公司 | Device is absorbed and utilized in a kind of venturi VOC |
| CN112551565A (en) * | 2021-01-07 | 2021-03-26 | 岳阳明科催化技术有限公司 | Carbonizing device and method for producing macroporous pseudo-boehmite by carbonization method |
| CN114794442A (en) * | 2022-05-23 | 2022-07-29 | 福建胜美鲜生物科技有限公司 | Method and device for brewing fish sauce by microbial fermentation |
| CN116825215A (en) * | 2023-02-28 | 2023-09-29 | 福建省龙德新能源有限公司 | Fluid circulation reaction control system and method for lithium hexafluorophosphate preparation |
| CN116825215B (en) * | 2023-02-28 | 2024-04-16 | 福建省龙德新能源有限公司 | Fluid circulation reaction control system and method for lithium hexafluorophosphate preparation |
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