CN116236991A - Continuous battery-level fluorobenzene preparation device and preparation method - Google Patents
Continuous battery-level fluorobenzene preparation device and preparation method Download PDFInfo
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- CN116236991A CN116236991A CN202310262310.XA CN202310262310A CN116236991A CN 116236991 A CN116236991 A CN 116236991A CN 202310262310 A CN202310262310 A CN 202310262310A CN 116236991 A CN116236991 A CN 116236991A
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- fluorobenzene
- shell
- casing
- preparation
- equipment
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- PYLWMHQQBFSUBP-UHFFFAOYSA-N monofluorobenzene Chemical compound FC1=CC=CC=C1 PYLWMHQQBFSUBP-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 239000002808 molecular sieve Substances 0.000 claims abstract description 21
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims abstract description 21
- 230000003014 reinforcing effect Effects 0.000 claims abstract description 13
- 230000018044 dehydration Effects 0.000 claims description 21
- 238000006297 dehydration reaction Methods 0.000 claims description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 239000002994 raw material Substances 0.000 claims description 13
- 239000010410 layer Substances 0.000 claims description 12
- 238000012423 maintenance Methods 0.000 claims description 11
- 238000011069 regeneration method Methods 0.000 claims description 11
- 238000003860 storage Methods 0.000 claims description 11
- 230000008929 regeneration Effects 0.000 claims description 9
- 238000005728 strengthening Methods 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000002356 single layer Substances 0.000 claims description 3
- 230000001502 supplementing effect Effects 0.000 claims description 3
- 238000003466 welding Methods 0.000 claims description 3
- 230000008676 import Effects 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 238000001914 filtration Methods 0.000 abstract description 9
- 238000000746 purification Methods 0.000 abstract description 2
- 238000000926 separation method Methods 0.000 abstract description 2
- 238000001179 sorption measurement Methods 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 239000007789 gas Substances 0.000 description 26
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 8
- 229910001416 lithium ion Inorganic materials 0.000 description 8
- 238000000034 method Methods 0.000 description 5
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- VEFXTGTZJOWDOF-UHFFFAOYSA-N benzene;hydrate Chemical compound O.C1=CC=CC=C1 VEFXTGTZJOWDOF-UHFFFAOYSA-N 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 238000009833 condensation Methods 0.000 description 3
- 230000005494 condensation Effects 0.000 description 3
- 230000005611 electricity Effects 0.000 description 3
- 230000001172 regenerating effect Effects 0.000 description 3
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 description 2
- 239000012159 carrier gas Substances 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- 229910000040 hydrogen fluoride Inorganic materials 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 239000003513 alkali Substances 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000012442 inert solvent Substances 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- -1 lithium hexafluorophosphate Chemical group 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/38—Separation; Purification; Stabilisation; Use of additives
- C07C17/389—Separation; Purification; Stabilisation; Use of additives by adsorption on solids
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/38—Separation; Purification; Stabilisation; Use of additives
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a continuous battery-level fluorobenzene preparation device and a preparation method thereof, and relates to the technical fields of separation and purification, adsorption and filtration chemical industry. The continuous battery-level fluorobenzene preparation device comprises a shell, wherein a reinforcing structure is arranged in the shell, a filter is arranged in the reinforcing structure, a molecular sieve is filled between the inner wall of the shell and the reinforcing structure, a rocker arm is arranged at the top of the shell, a discharge opening is arranged in the middle of the bottom end of the shell, a feed inlet is formed in one side of the middle lower part of the shell, and a heat medium inlet is formed in one side of the middle lower part of the shell. The invention has simple structure, small occupied area of equipment and less equipment investment, and meanwhile, the shell seal head of the equipment adopts quick-opening and detachable type, so that the filter and the molecular sieve can be conveniently and quickly replaced, the molecular sieve can be repeatedly utilized, and the equipment is not influenced by residual fluorobenzene when a worker overhauls the equipment.
Description
Technical Field
The invention relates to the technical field of separation, purification, adsorption and filtration chemical industry, in particular to a continuous battery-grade fluorobenzene preparation device and a preparation method.
Background
The battery-level fluorobenzene is mainly used for lithium ion batteries, and in the lithium ion batteries, fluorobenzene can be used as an inert solvent to improve the infiltration performance of electrolyte, improve the low-temperature performance and the cycle performance of the lithium ion batteries and ensure the safety of the lithium ion batteries when overcharge safety is out of control.
The increase of the water content in the lithium ion battery electrolyte can lead to the decomposition of lithium hexafluorophosphate to generate hydrogen fluoride, the performances of charge and discharge, cycle efficiency and the like of the lithium ion battery are obviously reduced, and the lithium ion battery is completely destroyed along with the increase of the water content, so that the water content of the added fluorobenzene is required to be not more than 10ppm by the lithium ion battery.
The fluorobenzene is mainly produced by aniline, hydrogen fluoride and diazotizing reagent, so that the fluorobenzene contains hydrofluoric acid and organic impurities, the subsequent treatment process of the fluorobenzene usually adopts water washing or alkali washing, and then the fluorobenzene is purified by layering and rectifying.
The conventional treatment means mainly have the following disadvantages:
(1) The molecular sieve has less repeated utilization times, low regeneration efficiency and even no regeneration;
(2) The fluorobenzene is adsorbed by the molecular sieve and then passes through the filter, so that the safety distance of equipment is ensured and the equipment maintenance space is reserved according to the design specification requirement, and the occupied area of the device is large;
(3) The equipment has fluorobenzene residue in the maintenance process, and has serious influence on the environment and personnel health.
Therefore, a continuous battery-grade fluorobenzene preparation device and a preparation method are proposed by the person skilled in the art.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a continuous battery-level fluorobenzene preparation device and a preparation method thereof, which solve the problem that residual fluorobenzene affects the environment and surrounding staff in the equipment maintenance process.
In order to achieve the above purpose, the invention is realized by the following technical scheme: the utility model provides a serialization battery level fluorobenzene preparation facilities, includes the casing, the inside of casing is provided with additional strengthening, additional strengthening's inside is provided with the filter, it has the molecular sieve to fill between shells inner wall and the additional strengthening, the top of casing is provided with the rocking arm, the bottom middle part of casing is provided with the discharge opening, well lower part one side of casing is provided with the feed inlet, well lower part one side of casing is provided with the thermal medium import.
Preferably, a reflux port is arranged on one side of the middle upper part of the shell, a discharge port is arranged on one side of the middle upper part of the shell, a plurality of quick-opening bolts are arranged on the middle upper part of the shell close to the edge, an exhaust port is arranged on one side of the middle top end of the shell, and an air supplementing port is arranged on one side of the middle top end of the shell.
Preferably, the shell adopts one of a single-layer jacket type or a multi-layer jacket type, the number of layers of the multi-layer jacket type is more than 1 layer, and the seal head of the shell adopts one of an integrated type, a detachable type and a quick-opening seal head.
Preferably, the reinforcing structure adopts one of a slit type and a mesh type, and the connection mode of the filter and the outlet pipeline is one of welding, buckling, bolting or threaded connection.
Preferably, the continuous preparation method of the battery-grade fluorobenzene comprises the following preparation steps:
s1: preparation of battery grade fluorobenzene
Pressurizing and circulating the raw material industrial grade fluorobenzene of a raw material storage tank by a pump, dehydrating and purifying the fluorobenzene by a dehydration device, and then conveying the fluorobenzene after the treatment to a product storage tank;
s2: regeneration and maintenance of dewatering equipment
And heating the gas by a heater, introducing the heated gas into a dehydration device, taking out the water and residual fluorobenzene in the dehydration device, recovering the gas by a regenerated tail gas treatment device, and finally cooling the device, and opening a quick-opening valve of the dehydration device to replace a filter element and replace a molecular sieve for maintenance.
The invention provides a continuous battery-level fluorobenzene preparation device and a preparation method. The device comprises the following
The beneficial effects are that:
1. the invention has simple structure, small equipment occupation area and small equipment investment, and the end socket of the shell adopts quick-opening and detachable type, thereby being convenient for quick replacement of the filter and the molecular sieve and convenient for users to use.
2. The filter is connected by the threads, and the filter connected by the threads is convenient to detach, so that the filter is more convenient to overhaul or replace by a worker, and the overhaul difficulty of the worker on the filter is reduced.
3. According to the invention, the dehydration equipment is adopted to heat the gas through steam, electricity, heat conducting oil and the like, and then the dehydration equipment is introduced to carry out water and fluorobenzene adsorbed by the molecular sieve, so that the aim of regenerating, cleaning and replacing the molecular sieve can be achieved, and the regeneration efficiency is high through hot gas regeneration.
4. According to the invention, the fluorobenzene is regenerated through the filtering equipment, and then the fluorobenzene is treated through the heater, the dewatering equipment and the filtering equipment in sequence, the actual carrier gas is condensed to recover the fluorobenzene, and the regenerated equipment does not detect residual fluorobenzene, so that no dangerous material remains in equipment inspection and maintenance, safety and environmental protection are realized, and the maintenance operation of staff is convenient.
Drawings
FIG. 1 is a schematic view of the apparatus of the present invention;
FIG. 2 is a flow chart of the present invention.
101, a feed inlet; 102. a discharge port; 103. a thermal medium inlet; 104. a reinforcing structure; 105. a filter; 106. a discharge port; 107. an air supplementing port; 108. a rocker arm; 1-9, an exhaust port; 110. quick-opening bolts; 111. a return port; 112. a housing; 113. a molecular sieve; 201. raw materials; 202. a finished product; 203. a gas; 204. tail gas; 205. and (3) water.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Examples:
as shown in fig. 1, the embodiment of the invention provides a continuous battery-level fluorobenzene preparation device, which comprises a shell 112, wherein a reinforcing structure 104 is arranged in the shell 112, a filter 105 is arranged in the reinforcing structure 104, a molecular sieve 113 is filled between the inner wall of the shell 112 and the reinforcing structure 104, a rocker arm 108 is arranged at the top of the shell 112, a discharge opening 102 is arranged in the middle of the bottom end of the shell 112, a feed inlet 101 is arranged at one side of the middle lower part of the shell 112, and a heat medium inlet 103 is arranged at one side of the middle lower part of the shell 112.
The casing 112 adopts multilayer jacket type, and the head of casing 112 adopts quick-opening head, installs filter 105 and additional strengthening 104 in the inner chamber of casing 112, and filter 105 adopts threaded connection with the pipeline, and additional strengthening 104 adopts the mesh type, welded fastening, and dewatering equipment lower part is equipped with the valve, opens when changing molecular sieve or packing and releases.
The middle upper part of casing 112 is provided with the return port 111, and the middle upper part of casing 112 is provided with discharge gate 106, and the middle upper part of casing 112 is close to the edge and is provided with a plurality of quick-open bolts 110, and the top middle part of casing 112 is provided with gas vent 1-9 on one side, and the top middle part of casing 112 is provided with air compensating port 107 on one side.
The shell 112 is one of a single-layer jacket type or a multi-layer jacket type, preferably the shell 112 is a jacket type, the end enclosure of the shell 112 is a detachable or quick-opening end enclosure, the number of layers of the multi-layer jacket type refers to more than 1 layer, and the end enclosure of the shell 112 is one of an integrated type, a detachable type and a quick-opening end enclosure.
The reinforcing structure 104 adopts one of a crack type reinforcing structure and a mesh type reinforcing structure, preferably a mesh type reinforcing structure, can play a role in blocking the molecular sieve 113 and allowing liquid to pass through, and the connection mode of the filter 105 and the outlet pipeline is one of welding, buckling, bolting or threaded connection, preferably threaded connection, and the threaded connection of the filter 105 is convenient to detach and convenient for workers to overhaul or replace.
The regeneration method of the dehydration equipment adopted by the invention comprises the following steps: after the gas (preferably nitrogen) is heated by steam, electricity, heat conducting oil and the like, the gas is introduced into dehydration equipment to carry out the water and fluorobenzene adsorbed by the molecular sieve, so that the purposes of regenerating, cleaning and replacing the molecular sieve are achieved.
As shown in fig. 2, the embodiment of the invention provides a continuous battery-grade fluorobenzene preparation method, which comprises the following preparation steps:
s1: preparation of battery grade fluorobenzene
Pressurizing and circulating the raw material industrial grade fluorobenzene of a raw material storage tank by a pump, dehydrating and purifying the fluorobenzene by a dehydration device, and then conveying the fluorobenzene after the treatment to a product storage tank;
s2: regeneration and maintenance of dewatering equipment
And heating the gas by a heater, introducing the heated gas into a dehydration device, taking out the water and residual fluorobenzene in the dehydration device, recovering the gas by a regenerated tail gas treatment device, and finally cooling the device, and opening a quick-opening valve of the dehydration device to replace a filter element and replace a molecular sieve for maintenance.
As shown in fig. 2, wherein a: a raw material storage tank; b: a transfer pump; c: a filtering device; d: a finished product storage tank; e: a gas heater; f: tail gas condensation recovery equipment; h: a water separator; g: tail gas treatment equipment.
The regeneration method of the dehydration equipment adopted by the invention comprises the following steps: after the gas (preferably nitrogen) is heated by steam, electricity, heat conducting oil and the like, the gas is introduced into dehydration equipment to carry out the water and fluorobenzene adsorbed by the molecular sieve, so that the purposes of regenerating, cleaning and replacing the molecular sieve are achieved.
The raw material fluorobenzene in the equipment raw material storage tank A has the fluorobenzene content of 99.9 percent and the water content of 1000ppm, the fluorobenzene is conveyed to the filtering equipment C through the conveying pump B, the raw material enters the finished product storage tank D after being circulated for 3 hours at the temperature of 40 ℃ in advance through the dehydration equipment, the water content of 8ppm is detected through the Karl Fischer method moisture meter, the purity of the raw material is improved to 99.95 percent, meanwhile, part of tail gas generated by the filtering equipment C in the regeneration process enters the tail gas treatment equipment G through the tail gas condensation recovery equipment F to be discharged, and the other part of the tail gas returns to the inside of the raw material storage tank A through the water separator H.
The continuous battery-level fluorobenzene preparation is regenerated by a dehydration device of a filtering device C, 203 nitrogen is heated to 158 ℃ after passing through a gas heater E, then the nitrogen is introduced into the dehydration device and the filtering device C, the fluorobenzene is recovered by carrier gas through condensation, the residual fluorobenzene is not detected when the residual condition of organic matters in the device is detected by a flammable gas analyzer after regeneration, the pollution of the residual fluorobenzene to the surrounding environment is reduced, and the influence of the fluorobenzene on the health of surrounding workers can be reduced.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (5)
1. The utility model provides a serialization battery level fluorobenzene preparation facilities, includes casing (112), its characterized in that: the inside of casing (112) is provided with additional strengthening (104), the inside of additional strengthening (104) is provided with filter (105), it has molecular sieve (113) to fill between casing (112) inner wall and the additional strengthening (104), the top of casing (112) is provided with rocking arm (108), the bottom middle part of casing (112) is provided with discharge opening (102), well lower part one side of casing (112) is provided with feed inlet (101), well lower part one side of casing (112) is provided with heat medium import (103).
2. The continuous battery-grade fluorobenzene preparation device as claimed in claim 1, wherein: the novel automatic feeding device is characterized in that a backflow port (111) is formed in one side of the middle upper portion of the shell (112), a discharge port (106) is formed in one side of the middle upper portion of the shell (112), a plurality of quick-opening bolts (110) are arranged at the position, close to the edge, of the middle upper portion of the shell (112), exhaust ports (1-9) are formed in one side of the middle top end of the shell (112), and an air supplementing port (107) is formed in the other side of the middle top end of the shell (112).
3. The continuous battery-grade fluorobenzene preparation device as claimed in claim 1, wherein: the shell (112) adopts one of a single-layer jacket type or a multi-layer jacket type, the number of layers of the multi-layer jacket type is more than 1 layer, and the seal head of the shell (112) adopts one of an integrated type, a detachable type and a quick-opening seal head.
4. The continuous battery-grade fluorobenzene preparation device as claimed in claim 1, wherein: the reinforcing structure (104) adopts one of a slit type and a mesh type, and the connection mode of the filter (105) and the outlet pipeline is one of welding, buckling, bolting or threaded connection.
5. The method for producing a continuous battery-grade fluorobenzene as claimed in any one of claims 1 to 4, comprising the steps of:
s1: preparation of battery grade fluorobenzene
Pressurizing and circulating the raw material industrial grade fluorobenzene of a raw material storage tank by a pump, dehydrating and purifying the fluorobenzene by a dehydration device, and then conveying the fluorobenzene after the treatment to a product storage tank;
s2: regeneration and maintenance of dewatering equipment
And heating the gas by a heater, introducing the heated gas into a dehydration device, taking out the water and residual fluorobenzene in the dehydration device, recovering the gas by a regenerated tail gas treatment device, and finally cooling the device, and opening a quick-opening valve of the dehydration device to replace a filter element and replace a molecular sieve for maintenance.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310262310.XA CN116236991A (en) | 2023-03-17 | 2023-03-17 | Continuous battery-level fluorobenzene preparation device and preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310262310.XA CN116236991A (en) | 2023-03-17 | 2023-03-17 | Continuous battery-level fluorobenzene preparation device and preparation method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN116236991A true CN116236991A (en) | 2023-06-09 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310262310.XA Pending CN116236991A (en) | 2023-03-17 | 2023-03-17 | Continuous battery-level fluorobenzene preparation device and preparation method |
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| CN (1) | CN116236991A (en) |
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|---|---|---|---|---|
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| CN217247361U (en) * | 2022-05-13 | 2022-08-23 | 合肥工业大学智能制造技术研究院 | Purification and filtration integrated equipment for lithium ion battery electrolyte and solvent |
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2023
- 2023-03-17 CN CN202310262310.XA patent/CN116236991A/en active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN202376797U (en) * | 2011-11-24 | 2012-08-15 | 江苏沿江化工资源开发研究院有限公司 | Adsorber with functions of dehydration, tar production, granulation and regeneration |
| CN202355933U (en) * | 2011-12-06 | 2012-08-01 | 史长伟 | Filler type oil dehydration filtering machine |
| CN205235696U (en) * | 2015-12-24 | 2016-05-18 | 西安超滤环保科技股份有限公司 | Wave energy regenerative molecular sieve dewatering equipment |
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