CN202558637U - Novel lithium hexafluorophosphate production device - Google Patents

Novel lithium hexafluorophosphate production device Download PDF

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Publication number
CN202558637U
CN202558637U CN2012201454987U CN201220145498U CN202558637U CN 202558637 U CN202558637 U CN 202558637U CN 2012201454987 U CN2012201454987 U CN 2012201454987U CN 201220145498 U CN201220145498 U CN 201220145498U CN 202558637 U CN202558637 U CN 202558637U
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CN
China
Prior art keywords
pipeline
jar
tank
hexafluoro phosphate
hydrogen fluoride
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Expired - Fee Related
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CN2012201454987U
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Chinese (zh)
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不公告发明人
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BEIJING SHENLONG PURIFICATION TECHNOLOGY Co Ltd
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BEIJING SHENLONG PURIFICATION TECHNOLOGY Co Ltd
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Priority to CN2012201454987U priority Critical patent/CN202558637U/en
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Abstract

The utility model discloses a novel lithium hexafluorophosphate production device, which belongs to the chemical field, and comprises a hydrogen fluoride rectifying column, a phosphorus pentafluoride generation tank, a seal tank, a lithium hexafluorophosphate generation tank, a tail gas treatment tank, a crystallizing tank and a vacuum drying tank, wherein a first pipeline is arranged between the hydrogen fluoride rectifying column and the phosphorus pentafluoride generation tank, a second pipeline is arranged between the phosphorus pentafluoride generation tank and the lithium hexafluorophosphate generation tank, a slurry pump and a third pipeline are arranged between the seal tank and the lithium hexafluorophosphate generation tank, a fourth pipeline is arranged between the lithium hexafluorophosphate generation tank and the tail gas treatment tank, a slurry pump and a fifth pipeline are arranged between the lithium hexafluorophosphate generation tank and the crystallizing tank, and a slurry pump and a sixth pipeline are arranged between the crystallizing tank and the vacuum drying tank. A finished product outlet is arranged on the vacuum drying tank, and lithium hexafluorophosphate is produced by adopting phosphorus trichloride and lithium fluoride and the like as raw materials. The novel lithium hexafluorophosphate production device has the advantages of short process synthesis route, high raw material conversion rate and high product purity.

Description

Novel lithium hexafluoro phosphate production equipment
Technical field
The utility model belongs to chemical field, relates in particular to a kind of mechanism of producing lithium hexafluoro phosphate.
Background technology
Lithium hexafluoro phosphate, relative molecular mass: 151.91, outward appearance is white crystals or powder; Specific density 1.50; Deliquescence is strong, is dissolved in organic solvents such as lower concentration methyl alcohol, ethanol, acetone, carbonates, but is insoluble in organic solvents such as alkane and benzene; Expose in the air or during heating lithium hexafluoro phosphate in air because the effect of water vapour and decomposing rapidly, emit PF5 and produce white smoke.Lithium hexafluoro phosphate is the topmost electrolyte lithium salt that present lithium ion battery uses, and the organic electrolyte that contains lithium hexafluoro phosphate has good electrical conductivity and electrochemical stability, therefore is chosen to be the ionogen of lithium ion battery.Lithium ion battery is current internationally recognized desirable chemical energy source; Have that volume is little, electrical capacity is big, electrical capacity only reduces by 3% after the repeated charge 500 times; Be widely used in electronic product and electromobile industry such as mobile telephone, laptop computer and camcorder, also be used to electronic industry and make the doping agent of wafer and the catalyzer of organic synthesis.The lithium hexafluoro phosphate main preparation methods has 4 kinds: 1. gas-solid reaction method, its advantage are to operate comparatively simply, but preparation homogeneous porous lithium fluoride difficulty is big; 2. organic solvent method, defective are to be difficult to obtain highly purified product; 3. ion exchange method, defective are that production cost is high; 4. homogeneous reaction though the hydrogen fluoride that uses has stronger corrodibility, because phosphorus pentafluoride and lithium fluoride all are soluble in the hydrogen fluoride, can take place in the hydrogen fluoride solvent method in liquid phase, makes entire reaction be easy to carry out and control, and is convenient to produce in enormous quantities.The utility model device uses the hydrogen fluoride solvent method to produce lithium hexafluoro phosphate; With hydrogen fluoride rectifying tower, phosphorus pentafluoride generation jar, sealed can, lithium hexafluoro phosphate generation jar, vent gas treatment jar, crystallizer, vacuum drying tank is equipment; With phosphorus trichloride, purifying hydrogen fluoride, chlorine, lithium fluoride is main raw material, through purifying hydrogen fluoride, produce and fluoridize phosphorus gas, process the lithium hexafluoro phosphate product at last.The great advantage of this device is: synthesis route is short, feed stock conversion is high, reaction conditions gentle easy to control, product purity is high, be convenient to produce in batches, environmental protection.
Summary of the invention
The problem that the utility model mainly solves provides a kind of mechanism of producing lithium hexafluoro phosphate in batches; This device generates jar, sealed can, lithium hexafluoro phosphate by hydrogen fluoride rectifying tower, phosphorus pentafluoride and generates jar, vent gas treatment jar, crystallizer, vacuum drying tank and forms, and its advantage is: synthesis route is short, feed stock conversion is high, reaction conditions gentle easy to control, product purity is high, be convenient to batch process, environmental protection.
The technical scheme that the utility model adopts is:
A kind of lithium hexafluoro phosphate production equipment comprises: hydrogen fluoride rectifying tower 1, phosphorus pentafluoride generate jar 2, sealed can 3, lithium hexafluoro phosphate generation jar 4, vent gas treatment jar 5, crystallizer 6, vacuum drying tank 7; Hydrogen fluoride rectifying tower 1 is provided with hydrogen fluoride import 8; Hydrogen fluoride rectifying tower 1 generates 2 in jar to phosphorus pentafluoride and is provided with first pipeline 9; Phosphorus pentafluoride generates jar 2 and is provided with phosphorus trichloride import 10, chlorine inlet 11; Phosphorus pentafluoride generates jar 2 and is provided with second pipeline 12 to 4 in lithium hexafluoro phosphate generation jar; Sealed can 3 is provided with lithium fluoride import 13, hydrogen fluoride import 14, and sealed can 3 generates jars 4 to lithium hexafluoro phosphate and is provided with shurry pump and the 3rd pipeline 15, lithium hexafluoro phosphate generate jars 4 to 5 in vent gas treatment jar be provided with the 4th pipeline 16, vent gas treatment jar 5 is provided with water inlet 17, hydrochloric acid outlet 18; Lithium hexafluoro phosphate generates jars 4 and is provided with shurry pump and the 5th pipeline 19 to 6 of crystallizers; Crystallizer 6 is provided with hydrogen fluoride liquid exit 20, and crystallizer 6 is provided with shurry pump and the 6th pipeline 21 to 7 of vacuum drying tanks, and vacuum drying tank 7 is provided with product outlet 22.
The further technical scheme of the utility model is:
Described whole shurry pump is the corrosion-resistant stainless steel propeller pump.
Described whole pipeline is a polyvinyl chloride pipeline.
The beneficial effect of the utility model is: a kind of novel lithium hexafluoro phosphate production equipment is provided, and the advantage of this production equipment is: synthesis route is short, feed stock conversion is high, reaction conditions gentle easy to control, product purity is high, be convenient to produce in batches, environmental protection.
Description of drawings:
Like figure is the utility model principle schematic.
Embodiment
Further specify the particular content that uses this device to produce the lithium hexafluoro phosphate most preferred embodiment below in conjunction with accompanying drawing:
1. rough hydrogen fluoride is sent into hydrogen fluoride rectifying tower 1 through import 8 and purify, it is for use to obtain purifying hydrogen fluoride.
With the phosphorus trichloride of liquid state through import 10 be lower than 10 ℃, security seal do not have leak and complete anhydrous condition under send into phosphorus pentafluoride and generate jars 2; Through import 11 chlorine is sent into phosphorus pentafluoride then and generate jar 2; Its mol ratio is phosphorus trichloride: chlorine=1:1.3; Generate in jars 2 at phosphorus pentafluoride and phosphorus trichloride and chlorine to be reacted through stirring, the time be about 0.5 hour after generation phosphorus pentachloride xln residual a spot of chlorine also; Purifying hydrogen fluoride is sent into phosphorus pentafluoride through first pipeline 9 generate jars 2 being lower than under 5 ℃, the environment of sealing then, its mol ratio is phosphorus pentachloride: hydrogen fluoride=1:1, and stirring reaction obtains phosphorus pentafluoride gas, hydrochloric acid gas and a small amount of chlorine after 1 hour.
With lithium fluoride through import 13, hydrogen fluoride through import 14 in molar ratio the ratio of 1:1 send into and be stirred to dissolving after mixing in the sealed can 3; Send into lithium hexafluoro phosphate through shurry pump and the 3rd pipeline 15 again and generate jar 4; Phosphorus pentafluoride is generated jar 2 interior phosphorus pentafluoride gas, hydrochloric acid gas and a small amount of chlorine introduce lithium hexafluoro phosphate generation jar 4 through second pipeline 12; Temperature is that stirring reaction generates lithium hexafluoro phosphate and residual hydrochloric acid gas and chlorine under 9 ℃, the environment of normal pressure sealing after 1.5 hours in keeping jar.
4. the hydrochloric acid gas, the chlorine that lithium hexafluoro phosphate are generated in jars 4 are introduced vent gas treatment jars 5 through the 4th pipeline 16 under the environment below 10 ℃, add water through import 17 to vent gas treatment jar 5, process behind the hydrochloric acid liquid that to discharge storages through outlet 18 for use.
5. lithium hexafluoro phosphate being generated jars 4 includes lithium hexafluoro phosphate and hydrofluoric liquid form mixt and sends into crystallizer 6 through shurry pump and the 5th pipeline 19 and carry out crystallization; The very fast crystallization of lithium hexafluoro phosphate is a solid; (because lithium hexafluoro phosphate different) and hydrogen fluoride still is liquid with hydrogen fluoride solidified temperature; Open outlet 20 hydrogen fluoride liquid is discharged, the crystal of lithium hexafluoro phosphate is sent into vacuum drying tank 7 through shurry pump and the 6th pipeline 21, the oven dry back is packaged to be finished product through exporting 22 dischargings.

Claims (3)

1. a novel lithium hexafluoro phosphate production equipment is characterized in that: comprise that hydrogen fluoride rectifying tower (1), phosphorus pentafluoride generate jar (2), a sealed can (3), lithium hexafluoro phosphate generates jar (4), a vent gas treatment jar (5), crystallizer (6), vacuum drying tank (7); Hydrogen fluoride rectifying tower (1) is provided with hydrogen fluoride import (8); Hydrogen fluoride rectifying tower (1) generates between jar (2) to phosphorus pentafluoride and is provided with first pipeline (9); Phosphorus pentafluoride generates jar (2) and is provided with phosphorus trichloride import (10), chlorine inlet (11); Phosphorus pentafluoride generates jar (2) and between lithium hexafluoro phosphate generation jar (4), is provided with second pipeline (12); Sealed can (3) is provided with lithium fluoride import (13), hydrogen fluoride import (14); Sealed can (3) generates between jar (4) to lithium hexafluoro phosphate and is provided with shurry pump and the 3rd pipeline (15); Lithium hexafluoro phosphate generate jar (4) to be provided with the 4th pipeline (16) between vent gas treatment jar (5), vent gas treatment jar (5) is provided with water inlet (17), hydrochloric acid outlet (18), lithium hexafluoro phosphate generates jar (4) to being provided with shurry pump and the 5th pipeline (19) between crystallizer (6), crystallizer (6) is provided with hydrogen fluoride liquid exit (20); Crystallizer (6) is to being provided with shurry pump and the 6th pipeline (21) between vacuum drying tank (7), vacuum drying tank (7) is provided with product outlet (22).
2. a kind of novel lithium hexafluoro phosphate production equipment according to claim 1, it is characterized in that: described whole shurry pumps are the corrosion-resistant stainless steel propeller pump.
3. a kind of novel lithium hexafluoro phosphate production equipment according to claim 1, it is characterized in that: said whole pipelines are polyvinyl chloride pipeline.
CN2012201454987U 2012-04-09 2012-04-09 Novel lithium hexafluorophosphate production device Expired - Fee Related CN202558637U (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN2012201454987U CN202558637U (en) 2012-04-09 2012-04-09 Novel lithium hexafluorophosphate production device

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Application Number Priority Date Filing Date Title
CN2012201454987U CN202558637U (en) 2012-04-09 2012-04-09 Novel lithium hexafluorophosphate production device

Publications (1)

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CN202558637U true CN202558637U (en) 2012-11-28

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104093668A (en) * 2012-01-19 2014-10-08 朗盛德国有限责任公司 Low-chloride lipf6
CN105460893A (en) * 2016-01-04 2016-04-06 江苏九九久科技股份有限公司 Method and dedicated device for lithium hexafluorophosphate synthesis tail gas treatment
CN106698384A (en) * 2017-02-21 2017-05-24 江苏九九久科技有限公司 Lithium hexafluorophate production device

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104093668A (en) * 2012-01-19 2014-10-08 朗盛德国有限责任公司 Low-chloride lipf6
CN104093668B (en) * 2012-01-19 2016-03-02 朗盛德国有限责任公司 Subchloride-LiPF 6
CN105460893A (en) * 2016-01-04 2016-04-06 江苏九九久科技股份有限公司 Method and dedicated device for lithium hexafluorophosphate synthesis tail gas treatment
CN107758620A (en) * 2016-01-04 2018-03-06 江苏九九久科技有限公司 The succinct lithium hexafluoro phosphate synthesis tail gas processing method of technological process and special purpose device
CN106698384A (en) * 2017-02-21 2017-05-24 江苏九九久科技有限公司 Lithium hexafluorophate production device
CN106698384B (en) * 2017-02-21 2019-01-11 江苏九九久科技有限公司 Lithium hexafluoro phosphate process units

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C17 Cessation of patent right
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Granted publication date: 20121128

Termination date: 20140409