CN102320588B - Lithium hexafluorophosphate synthesizer - Google Patents
Lithium hexafluorophosphate synthesizer Download PDFInfo
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- CN102320588B CN102320588B CN 201110259731 CN201110259731A CN102320588B CN 102320588 B CN102320588 B CN 102320588B CN 201110259731 CN201110259731 CN 201110259731 CN 201110259731 A CN201110259731 A CN 201110259731A CN 102320588 B CN102320588 B CN 102320588B
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- lithium hexafluorophosphate
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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 hexafluorophosphate synthesis device.
Background technology: lithium hexafluoro phosphate (LiPF
6) be most popular electrolyte lithium salt in the present commercial lithium-ion batteries.The synthetic 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 now suitability for industrialized production still only have 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, then pass into phosphorus pentafluoride (PF
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 the efficient that gas-liquid two-phase mixes is comparatively remarkable on the impact 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 at present the gas-liquid mixed reaction mainly contains aeration, absorption tower absorption and Venturi tube absorption etc.Venturi principle is when flow is crossed restraining mass, and pressure is relatively low near the back side of restraining mass, thus produce adsorption and cause adsorb the mixed flow of 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 (such as high temperature, high pressure, high-speed micro-jet and generation free radical etc.) and the mixing effect of reinforcement fluid.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 the synthetic report of lithium hexafluoro phosphate.
At present more about lithium hexafluoro phosphate synthetic patent and academic documents, but mostly pay attention to and the preparation of phosphorus pentafluoride and the purification of lithium hexafluoro phosphate, and less to the report of the HF solution reaction efficient that improves 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 larger, invests larger problem.Patent CN101544361A realizes the gas-liquid mixed reaction with phosphorus pentafluoride gas and HF liquid by tubular reactor.In order to improve the hybrid reaction effect, tubular reactor needs long crooked pipeline.There are the problems such as mixing duct is long, device structure is complicated, the easy obstruction of pipeline in this method.Patent CN101423207A passes into 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 advance anhydrous hydrogen fluoride.This method by micro-pore aeration can improve gas-liquid mixed efficient, but because HF, PF
5Corrodibility larger, the material of micro-hole aerator is required very high, also have simultaneously the risk in the phosphofluoric acid crystalline lithium blocking aeration hole of reaction generation when lithium fluoride concentration is high.For improving the utilization ratio of unreacted phosphorus pentafluoride, unreacted phosphorus pentafluoride gas continued to be passed in another anhydrous hydrogen fluoride solution that fills lithium fluoride after patent CN 101570328A will react, and continued reaction and obtained the lithium hexafluoro phosphate finished product.Improve like this utilization ratio of raw material phosphorus pentafluoride by increasing conversion unit, greatly increased facility investment.Therefore in order to overcome the deficiencies in the prior art, improve efficient and the utilization ratio of phosphorus pentafluoride gas and the non-aqueous solvent solution reaction of lithium fluoride, the present invention adopts Venturi tube realization raw material gas-liquid hybrid reaction, and makes the unreacted unstripped gas absorption reaction that circulated.
Summary of the invention: the object of the present invention is to provide a kind of lithium hexafluorophosphate synthesis device, it is to utilize venturi principle with fully the mixing of the non-aqueous solvent solution of realizing phosphorus pentafluoride gas and lithium fluoride, contact reacts, and the unreacted unstripped gas of circulation absorption, solve the problem and shortage that above-mentioned prior art exists.
Formation of the present invention: by tank body, Venturi tube, recycle pump, pipeline and valve form, tank body is comprised of cylindrical straight tube part and upper lower cover, straight drum part is cylindrical, between inwall and urceolus, be provided with the heat-eliminating medium chuck, upper cover is circular arc, lower cover is taper, at tank body cooling medium inlet and heat-eliminating medium outlet are arranged, at upper cover temperature is arranged, pressure, liquid level measurer, vent valve, the gas circulation outlet, the outlet pipe of Venturi tube enters in the straight tube of tank body by upper cover, the liquid circulation inlet pipe of Venturi tube is connected with recycle pump, at recycle pump liquid feed pipe is housed, in gas circulation outlet and Venturi tube gas circulating tube and gas feed-pipe is housed; At lower cover liquid turnover loop exit is arranged, at liquid turnover loop exit the liquid discharge nozzle 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 comprised of collapsible tube, trunnion, increaser, nozzle and outlet damper, the angle α of collapsible tube and trunnion
1Be 0-60 °, preferred 15 °, the angle α 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 described device, Venturi tube and recycle pump are made by material such as tetrafluoroethylene, polyfluorinated ethylene, 316L stainless steel, 904L stainless steel or the Hastelloy of the corrosion of ability anhydrous HF, perhaps realize anti-HF corrosion function by applying tetrafluoro coating, preferred 316L stainless steel applies tetrafluoro coating.
Compared with the 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 by Venturi tube, improves the utilization ratio of reaction efficiency and raw material, reduces facility investment.
Description of drawings: Fig. 1 is the lithium hexafluorophosphate synthesis device synoptic diagram, and Fig. 2 is the venturi tube structure synoptic diagram, 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, the 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, the gas feed pipe, 20, outlet pipe, 21, the liquid circulation inlet pipe, 22, liquid feed pipe, 23, the liquid discharge nozzle, 24, collapsible tube, 25, trunnion, 26, increaser, 27, nozzle, 28, outlet damper.
Embodiment: as Figure 1-3, a kind of lithium hexafluorophosphate synthesis device, by tank body, Venturi tube, recycle pump, pipeline and valve form, tank body 1 is comprised of cylindrical straight tube part and upper lower cover, straight drum part is cylindrical, between inwall 3 and urceolus, be provided with heat-eliminating medium chuck 2, upper cover is circular arc, lower cover is taper, at tank body 1 heat-eliminating medium outlet 4 and cooling medium inlet 11 are arranged, at upper cover temperature is arranged, pressure, liquid level measurer 5, vent valve 6, gas circulation outlet 7, the outlet pipe 20 of Venturi tube 8 enters in the straight tube of tank body 1 by upper cover, the liquid circulation inlet pipe 21 of Venturi tube is connected with recycle pump 9, at recycle pump 9 liquid feed pipe 22 is housed, and in gas circulation outlet 7 and Venturi tube 8 gas circulating tube 18 and gas feed-pipe 19 is housed; At lower cover liquid turnover loop exit 10 is arranged, at liquid turnover loop exit 10 liquid discharge nozzle 23 is housed.
Venturi tube 8 is comprised of collapsible tube 24, trunnion 25, increaser 26, nozzle 27 and outlet damper 28, the angle α of collapsible tube 24 and trunnion 25
1Be 0-60 °, preferred 15 °, the angle α 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 described device, Venturi tube and recycle pump are made by material tetrafluoroethylene, polyfluorinated ethylene, 316L stainless steel, 904L stainless steel, the Hastelloy of the corrosion of ability anhydrous HF, perhaps realize anti-HF corrosion function by applying tetrafluoro coating, preferred 316L stainless steel applies tetrafluoro coating.
At gas circulating tube 18 by-pass valve control F17 is arranged, at gas feed pipe 19 by-pass valve control E16 is arranged, at liquid circulation inlet pipe 21 by-pass valve control D15 is arranged, at liquid feed pipe 22 by-pass valve control A12 and by-pass valve control C14 are arranged, at liquid discharge nozzle 23 by-pass valve control B13 is arranged.
Claims (3)
1. lithium hexafluorophosphate synthesis device, by tank body, Venturi tube, recycle pump, pipeline and valve form, it is characterized in that: tank body (1) is comprised of cylindrical straight tube part and upper lower cover, straight drum part is cylindrical, between inwall (3) and urceolus, be provided with heat-eliminating medium chuck (2), upper cover is circular arc, lower cover is taper, at tank body (1) heat-eliminating medium outlet (4) and cooling medium inlet (11) are arranged, at upper cover temperature is arranged, pressure, liquid level measurer (5), vent valve (6), gas circulation outlet (7), the outlet pipe (20) of Venturi tube (8) enters in the straight tube of tank body (1) by upper cover, the liquid circulation inlet pipe (21) of Venturi tube is connected with recycle pump (9), at recycle pump (9) liquid feed pipe (22) is housed, in gas circulation outlet (7) and Venturi tube (8) gas circulating tube (18) and gas feed-pipe (19) is housed; At lower cover liquid turnover loop exit (10) is arranged, at liquid turnover loop exit (10) liquid discharge nozzle (23) is housed.
2. lithium hexafluorophosphate synthesis device according to claim 1, it is characterized in that: Venturi tube (8) is comprised of collapsible tube (24), trunnion (25), increaser (26), nozzle (27) and outlet damper (28), the angle α of collapsible tube (24) and trunnion (25)
1Be 0-60 °, the angle α of increaser (26) and trunnion (25)
2It is 0～60 °.
3. lithium hexafluorophosphate synthesis device according to claim 1 is characterized in that: the upper cover of circular arc is replaced by the upper cover of taper or flat cover; The lower cover of taper is replaced by circular arc or flat lower cover.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110259731 CN102320588B (en) | 2011-09-05 | 2011-09-05 | Lithium hexafluorophosphate synthesizer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110259731 CN102320588B (en) | 2011-09-05 | 2011-09-05 | Lithium hexafluorophosphate synthesizer |
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| CN102320588A CN102320588A (en) | 2012-01-18 |
| CN102320588B true CN102320588B (en) | 2013-03-13 |
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| CN 201110259731 Expired - Fee Related CN102320588B (en) | 2011-09-05 | 2011-09-05 | Lithium hexafluorophosphate synthesizer |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| KR102135267B1 (en) | 2017-06-07 | 2020-07-17 | 주식회사 엘지화학 | Electrolyte re-injection system of battery cell, battery pack, battery pack which can re-inject electrolyte and re-injection method of electrolyte of electric car battery pack |
| 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 |
| 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 |
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 |
-
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 |
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Granted publication date: 20130313 Termination date: 20160905 |