CN101423207A - Synthetic process of lithium hexafluorophosphate - Google Patents
Synthetic process of lithium hexafluorophosphate Download PDFInfo
- Publication number
- CN101423207A CN101423207A CNA2008101945525A CN200810194552A CN101423207A CN 101423207 A CN101423207 A CN 101423207A CN A2008101945525 A CNA2008101945525 A CN A2008101945525A CN 200810194552 A CN200810194552 A CN 200810194552A CN 101423207 A CN101423207 A CN 101423207A
- Authority
- CN
- China
- Prior art keywords
- lithium
- solid
- hexafluoro phosphate
- crude product
- lithium hexafluorophosphate
- 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
- 238000000034 method Methods 0.000 title claims abstract description 26
- -1 lithium hexafluorophosphate Chemical compound 0.000 title claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims abstract description 27
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 claims abstract description 20
- 239000007787 solid Substances 0.000 claims abstract description 18
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910000040 hydrogen fluoride Inorganic materials 0.000 claims abstract description 13
- 239000007788 liquid Substances 0.000 claims abstract description 13
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 12
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 12
- 239000012043 crude product Substances 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 9
- OBCUTHMOOONNBS-UHFFFAOYSA-N phosphorus pentafluoride Chemical compound FP(F)(F)(F)F OBCUTHMOOONNBS-UHFFFAOYSA-N 0.000 claims abstract description 7
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 19
- 229910052744 lithium Inorganic materials 0.000 claims description 19
- QGHDLJAZIIFENW-UHFFFAOYSA-N 4-[1,1,1,3,3,3-hexafluoro-2-(4-hydroxy-3-prop-2-enylphenyl)propan-2-yl]-2-prop-2-enylphenol Chemical group C1=C(CC=C)C(O)=CC=C1C(C(F)(F)F)(C(F)(F)F)C1=CC=C(O)C(CC=C)=C1 QGHDLJAZIIFENW-UHFFFAOYSA-N 0.000 claims description 18
- 229910019142 PO4 Inorganic materials 0.000 claims description 18
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 18
- 239000010452 phosphate Substances 0.000 claims description 18
- 239000007789 gas Substances 0.000 claims description 8
- 230000008014 freezing Effects 0.000 claims description 4
- 238000007710 freezing Methods 0.000 claims description 4
- 238000009434 installation Methods 0.000 claims description 4
- 239000003125 aqueous solvent Substances 0.000 abstract description 5
- 238000000926 separation method Methods 0.000 abstract 2
- 238000010924 continuous production Methods 0.000 abstract 1
- 230000036632 reaction speed Effects 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000012452 mother liquor Substances 0.000 description 2
- 239000012265 solid product Substances 0.000 description 2
- 229910015015 LiAsF 6 Inorganic materials 0.000 description 1
- 229910013063 LiBF 4 Inorganic materials 0.000 description 1
- 229910013684 LiClO 4 Inorganic materials 0.000 description 1
- 229910013870 LiPF 6 Inorganic materials 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 229910003002 lithium salt Inorganic materials 0.000 description 1
- 159000000002 lithium salts Chemical class 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
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- Secondary Cells (AREA)
Abstract
The invention discloses a synthesis process of a lithium hexafluorophosphate non-aqueous solvent method. The gas-phase phosphorus pentafluoride is arranged in a super-micro bubble generation device to generate micro-bubbles with the diameter of 0.1-2000 microns; subsequently, the phosphorus pentafluoride reacts with lithium fluoride which is dissolved in anhydrous hydrogen fluoride in advance in a reaction unit to generate a lithium hexafluorophosphate crude product which is frozen and then separated by a solid liquid separation device; the solid gained by separation is transferred to a drying device and dried, thus gaining the lithium hexafluorophosphate solid. The process has the advantages that the interface mixing efficiency is high, the reaction speed is high, the jamming phenomenon of solid outcome is not generated, the continuous production is easy to achieve, and the generated solid has uniform granularity and high purity.
Description
Technical field
The present invention relates to a kind of synthesis technique of lithium hexafluoro phosphate, more specifically to a kind of Technology of utilizing the synthetic lithium hexafluoro phosphate of non-aqueous solvent method.
Background technology
Since the eighties in 20th century, lithium ion battery came out,, big as specific energy, self-discharge is little, it is fast to have extended cycle life, discharge and recharge, memory-less effect etc., becomes first-selected high-performance secondary cell because of it possesses many high-performances.
The known electrolytical lithium salts of secondary lithium battery that can be used as comprises LiAsF
6, LiPF
6, LiBF
4, LiClO
4, LiCF
3SO
3, Li (CF
3SO
3)
2N etc., wherein lithium hexafluoro phosphate is used widely commercial because of good comprehensive performances, and output improves day by day.
Lithium hexafluoro phosphate has multiple synthetic method, comprises gas-solid reaction method, organic solvent method, ion exchange method, anhydrous hydrogen fluoride non-aqueous solvent method, have only in the above method success of anhydrous hydrogen fluoride non-aqueous solvent method realization commercially produce.
Although in the method for the synthetic lithium hexafluoro phosphate of anhydrous hydrogen fluoride non-aqueous solvent method several different technology circuits are arranged, but the core process of final synthesis technique has all utilized the reaction of the anhydrous hydrogen fluoride solution of gaseous state phosphorus pentafluoride and lithium fluoride, thus synthetic lithium hexafluoro phosphate product.Traditional gas-liquid synthesis method is utilized the hybrid reaction of liquid-gas interface in the reactor, and mixing efficiency is low, and speed of response is slow.
Summary of the invention
The purpose of this invention is to provide and a kind ofly can improve gas-liquid mixed efficient, thereby improve the synthesis technique of the lithium hexafluorophosphate of speed of response.
For achieving the above object, the present invention adopts following synthesis technique:
The gaseous state phosphorus pentafluoride feeds in the ultramicro air bubble generating unit, after the generation diameter is the microbubble of 0.1～2000 μ m, in reaction unit, react generation lithium hexafluoro phosphate crude product with the lithium fluoride that is dissolved in anhydrous hydrogen fluoride in advance, the lithium hexafluoro phosphate crude product is freezing, separate through equipment for separating liquid from solid again, separating obtained solid transfer is carried out drying treatment to drying installation, obtain the lithium hexafluoro phosphate solid;
The described weight concentration that is dissolved in the lithium fluoride of anhydrous hydrogen fluoride is controlled between 5～25%;
Described lithium hexafluoro phosphate crude product freezing temp is between-30～0 ℃;
Liquid is 50:1～1:50 with the mixed volume ratio of gas in the described reaction unit, and best mixed volume is than being 10:1～1:10.
The present invention has the following advantages:
1, gas-liquid mixed efficient height, speed of response is fast;
2, can not produce the latch up phenomenon of solid product, realize serialization production easily;
3, the solid particulate of Chan Shenging is even, the purity height.
Embodiment
Below in conjunction with embodiment the present invention is further described:
Embodiment 1
In the present embodiment ultramicro air bubble generating unit is arranged on still reaction device inside, add 50 liter weight concentration in the still reaction device in advance and be the anhydrous hydrogen fluoride solution of 15% lithium fluoride, start the ultramicro air bubble generating unit, in the ultramicro air bubble generating unit, feed phosphorus pentafluoride gas, the generation diameter is the bubble about 10 μ m, bubble enters the anhydrous hydrogen fluoride solution afterreaction of lithium fluoride, generate the lithium hexafluoro phosphate crude product, the volume ratio of liquid and gas is 9:1 in the control still reaction device in this process, crude product is cooled to-15 ℃, separates through equipment for separating liquid from solid, mother liquor can be transferred in the still reaction device, proceed the next batch reaction, solid transfer is carried out drying treatment in drying installation, obtain 15 kilograms of lithium hexafluoro phosphate solids, purity 99.8%.
Embodiment 2
The ultramicro air bubble generating unit is arranged on the outside of pipe reaction device in the present embodiment, add 80 liter weight concentration in the pipe reaction device in advance and be the anhydrous hydrogen fluoride solution of 20% lithium fluoride, start the ultramicro air bubble generating unit, and in the ultramicro air bubble generating unit, feed phosphorus pentafluoride gas, the generation diameter is the bubble about 10 μ m, bubble enters in the anhydrous hydrogen fluoride solution of the lithium fluoride in the pipe reaction device, the reaction back generates the lithium hexafluoro phosphate crude product, the volume ratio of liquid and gas is 8:3 in the control tubular type reaction unit in this engineering, crude product is cooled to-28 ℃, separates through equipment for separating liquid from solid, mother liquor can be transferred in the pipe reaction device 2, in order to the next batch reaction, solid product is transferred to and is carried out drying treatment in the drying installation, obtains 35 kilograms of lithium hexafluoro phosphate solids, purity 99.8%.
When in actual production, adopting synthesis technique of the present invention, the ultramicro air bubble generating unit both can be arranged on the outside of reaction unit, also can be arranged on the inside of reaction unit, and described reaction unit can be in pipe reaction device, still reaction device, tower-type reaction device, the tubular reactor any.
Claims (5)
1, the synthesis technique of lithium hexafluorophosphate, it is characterized in that: the gaseous state phosphorus pentafluoride feeds in the ultramicro air bubble generating unit, after the generation diameter is the microbubble of 0.1～2000 μ m, in reaction unit, react generation lithium hexafluoro phosphate crude product with the lithium fluoride that is dissolved in anhydrous hydrogen fluoride in advance, the lithium hexafluoro phosphate crude product is freezing, separate through equipment for separating liquid from solid, separating obtained solid transfer is carried out drying treatment to drying installation, obtain the lithium hexafluoro phosphate solid again.
2, synthesis technique according to claim 1 is characterized in that: the described weight concentration that is dissolved in the lithium fluoride of anhydrous hydrogen fluoride is controlled between 5～25%.
3, synthesis technique according to claim 1 is characterized in that: described lithium hexafluoro phosphate crude product freezing temp is between-30～0 ℃.
4, according to claim 1 or 2 or 3 described synthesis techniques, it is characterized in that: liquid is 50: 1～1: 50 with the mixed volume ratio of gas in the described reaction unit.
5, synthesis technique according to claim 4 is characterized in that: liquid is 10: 1～1: 10 with the mixed volume ratio of gas in the described reaction unit.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008101945525A CN101423207B (en) | 2008-11-17 | 2008-11-17 | Synthetic process of lithium hexafluorophosphate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008101945525A CN101423207B (en) | 2008-11-17 | 2008-11-17 | Synthetic process of lithium hexafluorophosphate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101423207A true CN101423207A (en) | 2009-05-06 |
| CN101423207B CN101423207B (en) | 2011-03-16 |
Family
ID=40614119
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2008101945525A Expired - Fee Related CN101423207B (en) | 2008-11-17 | 2008-11-17 | Synthetic process of lithium hexafluorophosphate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101423207B (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102153064A (en) * | 2011-03-29 | 2011-08-17 | 张家港市亚源高新技术材料有限公司 | Synthesis method of a lithium hexafluorophosphate non-aqueous solvent method |
| CN102502566A (en) * | 2011-11-01 | 2012-06-20 | 江苏九九久科技股份有限公司 | Technology for synthesizing lithium hexafluorophosphate |
| CN106698384A (en) * | 2017-02-21 | 2017-05-24 | 江苏九九久科技有限公司 | Lithium hexafluorophate production device |
| CN114713154A (en) * | 2022-04-30 | 2022-07-08 | 南京佳华工程技术有限公司 | System and process method for preparing lithium hexafluorophosphate |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3973329B2 (en) * | 1999-12-09 | 2007-09-12 | ステラケミファ株式会社 | Method for producing lithium hexafluorophosphate |
| CN1124975C (en) * | 2001-09-25 | 2003-10-22 | 天津化工研究设计院 | Method for preparing lithium hexafluorophosphate |
| CN101104761A (en) * | 2007-07-25 | 2008-01-16 | 浙江省丽水传人笔业有限公司 | Preparation method and preparation device of nano carbon black color paste suitable for neutral ink |
-
2008
- 2008-11-17 CN CN2008101945525A patent/CN101423207B/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102153064A (en) * | 2011-03-29 | 2011-08-17 | 张家港市亚源高新技术材料有限公司 | Synthesis method of a lithium hexafluorophosphate non-aqueous solvent method |
| CN102502566A (en) * | 2011-11-01 | 2012-06-20 | 江苏九九久科技股份有限公司 | Technology for synthesizing lithium hexafluorophosphate |
| 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 |
| CN114713154A (en) * | 2022-04-30 | 2022-07-08 | 南京佳华工程技术有限公司 | System and process method for preparing lithium hexafluorophosphate |
| CN114713154B (en) * | 2022-04-30 | 2022-12-16 | 南京佳华工程技术有限公司 | System and process method for preparing lithium hexafluorophosphate |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101423207B (en) | 2011-03-16 |
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Owner name: ZHANGJIAGANG YAYUAN HIGH-TECH MATERIAL CO.,LTD. Free format text: FORMER OWNER: YUAN XIANGYUN Effective date: 20130514 |
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Effective date of registration: 20130514 Address after: 215600, Yu Town, Jiangsu, Zhangjiagang Province sand village Patentee after: Zhangjiagang Yayuan High-Tech Material Co.,Ltd. Address before: Jiangsu province Zhangjiagang city yangshe 215600 Yangtze River town building 7 Room 305 Patentee before: Yuan Xiangyun |
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