CN106076238B - Liquid lithium salts micro-pipe reactor and the liquid lithium technology of threonates using the reactor - Google Patents
Liquid lithium salts micro-pipe reactor and the liquid lithium technology of threonates using the reactor Download PDFInfo
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- CN106076238B CN106076238B CN201610575929.6A CN201610575929A CN106076238B CN 106076238 B CN106076238 B CN 106076238B CN 201610575929 A CN201610575929 A CN 201610575929A CN 106076238 B CN106076238 B CN 106076238B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/24—Stationary reactors without moving elements inside
- B01J19/2415—Tubular reactors
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
- B01J8/06—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds in tube reactors; the solid particles being arranged in tubes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
- B01J2208/00008—Controlling the process
- B01J2208/00017—Controlling the temperature
- B01J2208/00106—Controlling the temperature by indirect heat exchange
- B01J2208/00168—Controlling the temperature by indirect heat exchange with heat exchange elements outside the bed of solid particles
- B01J2208/00176—Controlling the temperature by indirect heat exchange with heat exchange elements outside the bed of solid particles outside the reactor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
- B01J2208/06—Details of tube reactors containing solid particles
- B01J2208/065—Heating or cooling the reactor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
- B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
- B01J2219/00087—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
Liquid lithium technology of threonates the present invention relates to liquid lithium salts micro-pipe reactor and using the reactor, including chuck, the micro-pipe reactor body of more than one in chuck and it is connected to discharge nozzle outside chuck arranged on chuck bottom and by extension in chuck；The under-filled of the micro-pipe reactor body has lithium fluoride solid, top is equipped with material input port, middle part is connected with the connecting tube for blasting gas into micro-pipe reactor body, the bottom of the micro-pipe reactor body is connected with discharge nozzle, end on the discharge nozzle outside chuck is equipped with discharge port, and the filtration apparatus for being used for filtering lithium fluoride solid is equipped with discharge nozzle.It is the configuration of the present invention is simple, easy to use, manufacture lithium salts that can be rapidly and efficiently, solid lithium salts is arranged on to the bottom of micro-pipe reactor body, discharge port is arranged on to the bottom of micro-pipe reactor body, make solution flow through solid lithium salts to flow out from discharge port again, ensure the continuity of preparation process and the adequacy of reactant contact.
Description
Technical field
The present invention relates to lithium salts manufacturing field, and in particular to a kind of liquid lithium salts micro-pipe reactor and using the reactor
Liquid lithium technology of threonates.
Background technology
Lithium ion battery is secondary cell more highest than energy so far, is widely used as the power supply of portable electric appts,
Such as：Mobile phone, digital camera, laptop etc..Traditional lithium salts manufacture method is usually all to launch various reactants
Reaction generation lithium salts is carried out into reaction kettle, but there are many defects, lithium fluoride usually can all be deposited to bottom, lead for this technique
Cause contact of the phosphorus pentafluoride with lithium fluoride and insufficient, phosphorus pentafluoride is without the reaction was complete, so that lithium hexafluoro phosphate product
Quality is not up to standard, and whole reaction process is non-successional, and reaction efficiency is low.
The content of the invention
The purpose of the present invention is for above shortcoming, there is provided and it is a kind of simple in structure, easy to use, can be rapidly and efficiently
Manufacture liquid lithium salts liquid lithium salts micro-pipe reactor and using the reactor liquid lithium technology of threonates, the reactor and
Production technology can not only make lithium fluoride and phosphorus pentafluoride react abundant, improve reaction efficiency, and can reduce final reacting product
The generation of middle HF gases.
Scheme is used by the present invention solves technical problem：A kind of liquid lithium salts micro-pipe reactor, including chuck, be arranged on
The micro-pipe reactor body of more than one in chuck and it is connected to arranged on chuck bottom and by extending in chuck outside chuck
Discharge nozzle；The under-filled of the micro-pipe reactor body has lithium fluoride solid, and top is equipped with material input port, and middle part is with using
Connected in the connecting tube that gas is blasted into micro-pipe reactor body, bottom and the discharge nozzle of the micro-pipe reactor body connect
Logical, the end on the discharge nozzle outside chuck is equipped with discharge port, and the mistake for being used for filtering lithium fluoride solid is equipped with discharge nozzle
Filter device.
Further, more micro-pipe reactor bodies are provided with the chuck, the connecting tube is reacted with each micro-pipe
Device body is all connected with ventilating, and discharge port plate is additionally provided with the chuck, and the bottom of each micro-pipe reactor body passes through discharge port plate
Connected with discharge nozzle；More micro-pipe reactor bodies are set to pass through connecting tube easy to the yield of increase liquid lithium salts in chuck
Easy to blast phosphorus pentafluoride gas to micro-pipe reactor, and discharge port plate is arranged on the lower section of micro-pipe reactor body, ensure that
Reactant is sufficiently contacted in preparation process.
Further, the discharge port plate is hollow disc shape structure, the upper surface of the discharge port plate be equipped with it is multiple be used for
The connecting hole of micro-pipe reactor body connection, the lower face of discharge port plate from side to center under convex into an arc-shaped curved surface and discharging
The connector for being used for being connected with discharge nozzle is equipped with the center of disk lower face；Hollow disc shape structure ensure that discharge port plate and every
Micro-pipe reactor body all connects, and the arcuate structure of the lower surface of discharge port plate is conducive to the collection and outflow of solution.
Further, one end of the connecting tube is extended to outside chuck, and the junction of connecting tube and chuck is equipped with fluid sealant,
The external part of the connecting tube is equipped with the opening for being used for blasting phosphorus pentafluoride gas；Connecting tube is extended to outside chuck and set and opens
Mouthful, easy to blast phosphorus pentafluoride gas externally to micro-pipe reactor body, and both are tightly connected, and ensure cold in chuck
But liquid will not be revealed.
In order to constantly cool down to micro-pipe reactor to ensure the temperature of micro-pipe reactor, and ensure that coolant constantly carries out
Circulation with fully take away heat prevent coolant absorb heat after temperature rise can not effective temperature-reducing, and the Sheng for making coolant not reveal
It is put in chuck；The chuck is closed columnar structured, and the lower part of chuck is equipped with water inlet, and the top of chuck is equipped with water outlet
Mouthful, the chuck is connected with coolant circulation system by water inlet and water outlet, and the lower part of the chuck, which is equipped with, to be used to wear
The mounting hole of discharge nozzle, the mounting hole are tightly connected with discharge nozzle.
A kind of production technology that liquid lithium salts is manufactured with micro-pipe reactor, comprises the following steps：
1. it is pre-charged with lithium fluoride solid in the lower part of micro-pipe reactor body；Coolant is passed through into jacket body；
2. the mixed reaction solvent of lithium fluoride and organic solvent is put into from the material input port of micro-pipe reactor body
In micro-pipe reactor body；
3. being passed through phosphorus pentafluoride gas into micro-pipe reactor body from connecting tube, make phosphorus pentafluoride and mixed reaction solvent
Reaction intermediate of the chemical reaction generation containing lithium hexafluoro phosphate is carried out in micro-pipe reactor body；
4. the reaction intermediate containing lithium hexafluoro phosphate continues to flow downward, with being embedded in micro-pipe reactor body lower part
Lithium fluoride solid further fully react after, discharged from the discharge port of discharge nozzle, the remaining filtered device mistake of lithium fluoride solid
Filter, obtains the reaction final product containing lithium hexafluoro phosphate that the reaction was complete.
In order to reaction dissolvent is provided with promote reaction generation；The organic solvent is dimethyl carbonate or methyl ethyl carbonate
Ester.
Prevent that micro-pipe temperature of reactor is excessive to effectively take away heat；The coolant is water or ethylene glycol.
For the prior art, the present invention has the following advantages：
(1) for the present invention using micro-pipe reactor as reaction vessel, energy consumption is low, and technological operation is simple and easy, and prepares
Electrolyte process does not have to the excessive lithium salts of dissolving, effectively reduces manufacture cost, increases economic efficiency；
(2) present invention need not recycle solid lithium salts, avoid in traditional handicraft because used in the recrystallization process of solid lithium salts
The security risk that solvent flash-point is low and brings, security are higher；
(3) present invention is directly used in micro-pipe reactor lower part filled solid lithium salts, avoids passing through for traditional handicraft use
Excessive lithium salts is dissolved to reduce the generation of HF, and reduce solid lithium salts without again recycling excessive lithium salts after the reaction
The solvent volatilization and the generation of reduction waste gas containing fluoride recrystallized in preparation process, than traditional lithium salts manufacture method more ring
Protect；
(4) present invention obtains end reaction thing, the fixation lithium fluoride that lower part is set, easy to preparation process using from lower part
In, the lithium fluoride that the dimethyl carbonate or methyl ethyl carbonate ester solution of lithium hexafluoro phosphate first flow through micro-pipe reactor body lower part is consolidated
Flowed out again from discharge port after body, with lithium fluoride again secondary response, so as to ensure that the adequacy of reaction, continuity.
Brief description of the drawings
The invention will be further described in conjunction with the embodiments with reference to the accompanying drawings：
Fig. 1 is the structure diagram of the present invention；
Fig. 2 is the A-A sectional views in Fig. 1.
In figure：
1- chucks；101- water inlets；102- water outlets；2- coolants；3- lithium fluoride solids；4- discharge nozzles；401- discharges
Mouthful；402- filtration apparatuses；5- micro-pipe reactor bodies；501- is open；6- connecting tubes；7- discharge port plates.
Embodiment
Present invention is described in detail with reference to Figure of description and specific embodiment：
As shown in Figs. 1-2, a kind of liquid lithium salts micro-pipe reactor, including chuck 1, more than one in chuck 1
Micro-pipe reactor body 5 and the discharge nozzle 4 being connected to arranged on 1 bottom of chuck and by the interior extension of chuck 1 outside chuck 1；It is described
The under-filled of micro-pipe reactor body 5 has lithium fluoride solid 3, and top is equipped with material input port 501, and middle part is with being used for micro-pipe
The connecting tube 6 that gas is blasted in reactor body 5 connects, and the bottom of the micro-pipe reactor body 5 is connected with discharge nozzle 4, institute
State the end on discharge nozzle 4 outside chuck 1 and be equipped with discharge port 401, be equipped with discharge nozzle 4 and be used to filter lithium fluoride solid 3
Filtration apparatus 402.
In the present embodiment, be provided with more micro-pipe reactor bodies 5 in the chuck 1, the connecting tube 6 and each it is micro-
Pipe reactor body 5 is all connected with ventilating；Discharge port plate 7 is additionally provided with the chuck 1, the bottom of each micro-pipe reactor body 5 is equal
Connected by discharge port plate 7 with discharge nozzle 4；Production of the more micro-pipe reactor bodies 5 easy to increase liquid lithium salts is set in chuck 1
Amount, is easy to blast phosphorus pentafluoride gas to micro-pipe reactor by connecting tube 6, and discharge port plate 7 is arranged on micro-pipe reactor sheet
The lower section of body 5, ensure that reactant is sufficiently contacted in preparation process.
In the present embodiment, the discharge port plate 7 is hollow disc shape structure, and the upper surface of the discharge port plate 7 is equipped with multiple
For the connecting hole being connected with micro-pipe reactor body 5, the lower face of discharge port plate 7 from side to center under convex into arc song
The level height in face, i.e. center is more lower slightly than the level height at edge, and is equipped with and is used for going out at the center of 7 lower face of discharge port plate
The connector that expects pipe 4 connects；Hollow disc shape structure ensure that discharge port plate 7 is all connected with every micro-pipe reactor body 5, discharging
The arcuate structure of the lower surface of disk 7 is conducive to the collection and outflow of solution.
In the present embodiment, one end of the connecting tube 6 is extended to outside chuck 1, and connecting tube 6 and the junction of chuck 1 are set
There is fluid sealant, the external part of the connecting tube 6 is equipped with the opening for being used for blasting phosphorus pentafluoride gas；Connecting tube 6 extends to chuck 1
Outside and opening is set, easy to blast phosphorus pentafluoride gas externally to micro-pipe reactor body 5, and both are tightly connected, and protect
Coolant 2 in card chuck 1 will not be revealed.
In the present embodiment, in order to constantly cool down to micro-pipe reactor to ensure the temperature of micro-pipe reactor, and ensure
Coolant 2 is constantly circulated, and fully to take away, temperature rise can not effective temperature-reducing after heat prevents the heat absorption of coolant 2；The folder
1 cylindrical structure is covered, the lower part of chuck 1 is equipped with water inlet 101, and the top of chuck 1 is equipped with water outlet 102, and the chuck 1 is logical
Cross water inlet 101 and be connected with coolant circulation system with water outlet 102, the lower part of the chuck 1, which is equipped with, to be used to wear discharge nozzle 4
Mounting hole, the mounting hole is tightly connected with discharge nozzle 4.
A kind of production technology that liquid lithium salts is manufactured with micro-pipe reactor, comprises the following steps：
1. it is pre-charged with lithium fluoride solid in the lower part of micro-pipe reactor body 5；Coolant is passed through into 1 body of chuck；
2. the mixed reaction solvent of lithium fluoride and organic solvent is thrown from the material input port 501 of micro-pipe reactor body 5
Enter into micro-pipe reactor body 5；
3. being passed through phosphorus pentafluoride gas into micro-pipe reactor body 5 from connecting tube 6, make phosphorus pentafluoride molten with hybrid reaction
Agent carries out reaction intermediate of the chemical reaction generation containing lithium hexafluoro phosphate in micro-pipe reactor body 5；
4. the reaction intermediate containing lithium hexafluoro phosphate continues to flow downward, with being embedded under micro-pipe reactor body 5
After the lithium fluoride solid in portion further fully reacts, discharged from the discharge port 401 of discharge nozzle 4, remaining lithium fluoride solid is filtered
Device filters, and obtains the reaction final product containing lithium hexafluoro phosphate that the reaction was complete.
In order to reaction dissolvent is provided with promote reaction generation；The organic solvent is dimethyl carbonate or methyl ethyl carbonate
Ester.
Prevent that micro-pipe temperature of reactor is excessive to effectively take away heat；The coolant is water or ethylene glycol.
In the present embodiment, coolant 2 is set in chuck 1 and makes the constantly circulation of coolant 2 be liquid to take away heat
The manufacture of body lithium salts provides suitable reaction environment temperature；And discharge port 401 is arranged on bottom, in micro-pipe reactor body
5 under-filled lithium fluoride solids 3, ensure due to gravity the defluent reaction final product containing lithium hexafluoro phosphate again with fluorine
Change lithium solid 3 to contact, reaction is carried out more complete, ensure that the quality of lithium hexafluoro phosphate, meanwhile, set in discharge nozzle 4
Filtration apparatus 402, ensure that lithium fluoride solid 3 will not be flowed out with end reaction solution.
Above-listed preferred embodiment, is further described the object, technical solutions and advantages of the present invention, answers
Understand, the foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
With within principle, any modification, equivalent replacement, improvement and so on, should all be included in the protection scope of the present invention god.
Claims (7)
- A kind of 1. liquid lithium salts micro-pipe reactor, it is characterised in that：Including chuck (1), more than one in chuck (1) Micro-pipe reactor body (5) and it is connected to the discharging of chuck (1) outside arranged on chuck (1) bottom and by extension in chuck (1) To manage (4), the under-filled of the micro-pipe reactor body (5) has lithium fluoride solid (3), and top is equipped with material input port (501), Middle part is connected with the connecting tube (6) for blasting gas into micro-pipe reactor body (5), the micro-pipe reactor body (5) Bottom connected with discharge nozzle (4), be equipped with discharge port (401) positioned at the end of chuck (1) outside on the discharge nozzle (4), discharge The filtration apparatus (402) for being used for filtering lithium fluoride solid (3) is equipped with pipe (4)；It is anti-that more micro-pipes are provided with the chuck (1) Device body (5) is answered, the connecting tube (6) is all connected with ventilating with each micro-pipe reactor body (5), is also set in the chuck (1) There is discharge port plate (7), the bottom of each micro-pipe reactor body (5) is connected by discharge port plate (7) with discharge nozzle (4).
- 2. liquid lithium salts micro-pipe reactor according to claim 1, it is characterised in that：The discharge port plate (7) is hollow circle Disk-like structure, the upper surface of the discharge port plate (7) are equipped with multiple connecting holes for being connected with micro-pipe reactor body (5), go out The lower face of charging tray (7) from side to center under convex into be equipped with the center an of arc-shaped curved surface and discharge port plate (7) lower face and use In the connector being connected with discharge nozzle (4).
- 3. liquid lithium salts micro-pipe reactor according to claim 1, it is characterised in that：Prolong one end of the connecting tube (6) Reach chuck (1) outside, connecting tube (6) and the junction of chuck (1) are equipped with fluid sealant, and the external part of the connecting tube (6) is equipped with For blasting the opening of phosphorus pentafluoride gas.
- 4. liquid lithium salts micro-pipe reactor according to claim 1, it is characterised in that：The cylindrical knot of the chuck (1) Structure, the lower part of chuck (1) are equipped with water inlet (101), and the top of chuck (1) is equipped with water outlet (102), and the chuck (1) passes through Water inlet (101) is connected with coolant circulation system with water outlet (102), and the lower part of the chuck (1), which is equipped with, to be used to wear out The mounting hole of expects pipe (4), the mounting hole are tightly connected with discharge nozzle (4).
- A kind of 5. production technology that liquid lithium salts is manufactured with any micro-pipe reactors of claim 1-4, it is characterised in that： Comprise the following steps：1. it is pre-charged with lithium fluoride solid (3) in the lower part of micro-pipe reactor body (5)；Coolant is passed through in vivo to chuck (1)；2. the mixed reaction solvent of lithium fluoride and organic solvent is thrown from the material input port (501) of micro-pipe reactor body (5) Enter into micro-pipe reactor body (5)；3. being passed through phosphorus pentafluoride gas in from connecting tube (6) to micro-pipe reactor body (5), make phosphorus pentafluoride molten with hybrid reaction Agent carries out reaction intermediate of the chemical reaction generation containing lithium hexafluoro phosphate in micro-pipe reactor body (5)；4. the reaction intermediate containing lithium hexafluoro phosphate continues to flow downward, with being embedded in micro-pipe reactor body (5) lower part Lithium fluoride solid (3) further fully after reaction, discharged from the discharge ports (401) of discharge nozzle (4), remaining lithium fluoride solid (3) filtered device (402) filtering, obtains the reaction final product containing lithium hexafluoro phosphate that the reaction was complete.
- 6. production technology according to claim 5, it is characterised in that：The organic solvent is dimethyl carbonate or carbonic acid first Ethyl ester.
- 7. production technology according to claim 5, it is characterised in that：The coolant is water or ethylene glycol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610575929.6A CN106076238B (en) | 2016-07-21 | 2016-07-21 | Liquid lithium salts micro-pipe reactor and the liquid lithium technology of threonates using the reactor |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610575929.6A CN106076238B (en) | 2016-07-21 | 2016-07-21 | Liquid lithium salts micro-pipe reactor and the liquid lithium technology of threonates using the reactor |
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| Publication Number | Publication Date |
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| CN106076238A CN106076238A (en) | 2016-11-09 |
| CN106076238B true CN106076238B (en) | 2018-04-13 |
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| CN114471386B (en) * | 2022-04-01 | 2023-04-25 | 西南化工研究设计院有限公司 | Ammonolysis reactor and amide preparation method |
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| JP3894851B2 (en) * | 2002-07-09 | 2007-03-22 | 株式会社エルブ | Method for producing functional silicone resin composition |
| CN101544361B (en) * | 2009-05-07 | 2012-10-03 | 洛阳森蓝化工材料科技有限公司 | Process for continuous preparation of lithium hexafluorophosphate |
| CN104162388B (en) * | 2014-08-26 | 2016-05-11 | 河南省科学院化学研究所有限公司 | A kind of serialization ultralow temperature reaction unit |
| CN205914164U (en) * | 2016-07-21 | 2017-02-01 | 宁德市凯欣电池材料有限公司 | Little reactor of liquid lithium salt |
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