CN103243341B - A kind of stirring-type fluorination electrolytic cell - Google Patents
A kind of stirring-type fluorination electrolytic cell Download PDFInfo
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- CN103243341B CN103243341B CN201310140764.6A CN201310140764A CN103243341B CN 103243341 B CN103243341 B CN 103243341B CN 201310140764 A CN201310140764 A CN 201310140764A CN 103243341 B CN103243341 B CN 103243341B
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Abstract
A kind of stirring-type fluorination electrolytic cell, by motor, shaft coupling, stir shaft, shaft seal, electrode column, electrode bundle, electrolyzer, reduction cell cover plate, electrolyzer chuck, axle sleeve, blind plate, guide shell, stirring rake, insulating washer forms, a kind of stirring-type fluorination electrolytic cell provided by the invention, material is dissolved in whole system and disperse evenly, carry out fluoridation in a cell simultaneously, decrease decomposition induction time, decomposition induction time reduced to one day from 3-5 days, also dead groove phenomenon has substantially been stopped, reduce the number of times of the clear groove because of handling dead groove, adopt stirring-type groove former annual dead groove 3-4 time, after adopting the present invention, there is not dead groove phenomenon, reduce supplies consumption more than 20%, single groove output increased 30%, the polymkeric substance generated in electrolyzer reduces, clear groove time lengthening one times, alleviate artificial clear groove labour intensity.
Description
Technical field
The present invention relates to the technical field of the electrolyzer of Organic Electrochemical Synthesis, particularly relate to a kind of stirring-type fluorination electrolytic cell.
Background technology
Organic fluorocompound nature exists few, and how fluorine being introduced in organism the problem becoming people and be badly in need of solving, the preparation of organic fluoride can use F
2directly fluoridize, also can use XeF
2, Hydroxyl fluoride, high-valence metal fluoride, the fluorination reagent such as the N2F compounds method of indirectly fluoridizing.These electrochemical fluorination methods, react and operate all more complicated, the equipment of needs is harsher; The fluorination reagent toxicity used is high or be absolutely unsafe, and what have is very expensive; And wayward fluorine adding content, be difficult to obtain target product.Therefore, people have to seek other method.Nineteen forty-one, Americanized scholar Simons invented electrochemical fluorination (ECF) method, produce perfluor or partially fluorinated organic compound, such as full-fluorine octyl sulfuryl fluoride, perfluoro butyl sulfonic acid fluoride, perfluoro triethylamine etc., its invention, the preparation for fluorocarbon opens a brand-new and marvellous approach.Initial Simons method has alternately installed one group of nickel anode and iron cathode pole plate in the steel electrolyzer of rectangle or circle, and add anhydrous hydrogen fluoride and a small amount of organism, logical direct current carries out electrolysis.Electrolyzer external application cooling jacket removes the heat produced in electrolytic process.Usual bath voltage is 5V-8V, and current density is greater than 500A/dm2, and temperature range is 0 DEG C-9 DEG C.With this understanding, F
2can not overflow, fluorinated product then generates at anode.The fluorochemical generated, owing to being insoluble to anhydrous hydrogen fluoride, or is deposited on bottom of electrolytic tank, or evaporates in cold-trap in gas phase and be collected.But traditional electrolyzer has following shortcoming: the HF in groove does not flow, be dissolved in ionogen in HF and pole plate contact probability little, therefore electrofluorination reaction efficiency is low; Reaction electrofluorination decomposition induction time is long, is generally 3 days-5 days, and dead groove phenomenon is comparatively frequent, and after making alive, no current inputs.
Summary of the invention
For above-mentioned defect and the problem of prior art, the invention provides a kind of electrofluorination reaction efficiency and do; Reaction electrofluorination decomposition induction time is short, and can reduce a kind of stirring-type fluorination electrolytic cell of dead groove phenomenon.
In order to achieve the above object, the invention provides following technical scheme: a kind of stirring-type fluorination electrolytic cell, by motor, shaft coupling, stir shaft, shaft seal, electrode column, electrode bundle, electrolyzer, reduction cell cover plate, electrolyzer chuck, axle sleeve, blind plate, guide shell, stirring rake, insulating washer forms, reduction cell cover plate covers on electrolyzer, electrolyzer arranges discharge port and opening for feed, discharge outlet arranges bleeder valve, electrolyzer chuck is arranged on the outside surrounding of electrolyzer and bottom, electrolyzer chuck arranges refrigerant import and refrigerant exit, motor is connected with stir shaft by shaft coupling, stir shaft passes reduction cell cover plate by shaft seal, electrode column is fixed on reduction cell cover plate after being connected with the electrode bundle in electrolyzer, separates with cover plate insulating washer, the positive pole that electrode column comprises and negative pole, the positive pole of corresponding connection electrode bundle and negative pole, electrode bundle is nickel positive pole conveniently, iron negative pole is alternately arranged, just, insulating trip is adopted to separate between negative pole, electrode bundle is between guide shell outer wall and electrolyzer inwall, evenly arrange around guide shell, guide shell is fixed on reduction cell cover plate, arranges 2-4 openings in the middle part of guide shell in the following barrel position of electrolysis liquid surface, guide shell bottom arranges 2-4 openings, opening direction faces electrode bundle center, arranges blind plate bottom guide shell, arranges axle sleeve in the middle of blind plate, stirring rake is positioned at guide shell, and stir shaft is connected with stirring rake.
In technique scheme, described electrolyzer and reduction cell cover plate are circular or rectangular configuration.
In technique scheme, described electrode bundle is around the outer wall circular of guide shell, evenly arrangement two groups, three groups or multi-group electrode bundle, and the pole plate arrangement centerline direction of electrode bundle is consistent with the normal of guide shell.
In technique scheme, described reduction cell cover plate sets out gas port.
Preferred technical scheme, arranges thermal insulation layer outside described electrolyzer chuck.
Preferred technical scheme, also comprises thermometer, and set temperature meter fixing port on cell wall cover plate, thermometer one end passes from reduction cell cover plate, and one end is positioned at electrolyzer in addition.
Preferred technical scheme, also comprises liquidometer, and cell wall upper and lower end vertically arranges the fixing port of two liquidometers respectively, and liquidometer pipe adopts transparent fluorine to mould pipe.
Preferred technical scheme, also comprises leg, and leg is arranged on bottom of electrolytic tank, and quantity arranges three or four.
A kind of stirring-type fluorination electrolytic cell provided by the invention, material is dissolved in whole system and disperse evenly, carry out fluoridation in a cell simultaneously, decrease decomposition induction time, decomposition induction time reduced to one day from 3-5 days, also dead groove phenomenon has substantially been stopped, reduce the number of times of the clear groove because of handling dead groove, adopt shunt slot former annual dead groove 3-4 time, after adopting shunt slot of the present invention, there is not dead groove phenomenon, reduce supplies consumption more than 20%, single groove output increased 30%, the polymkeric substance generated in electrolyzer reduces, clear groove time lengthening one times, alleviate artificial clear groove labour intensity.
Accompanying drawing explanation
In order to be illustrated more clearly in the embodiment of the present invention or technical scheme of the prior art, be briefly described to the accompanying drawing used required in embodiment or description of the prior art below, apparently, accompanying drawing in the following describes is only some embodiments of the present invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can also be obtained according to these accompanying drawings.
Fig. 1 is embodiment of the present invention structural representation.
Fig. 2 is embodiment electrode bundle distributed architecture schematic diagram.
Fig. 3 is guide shell structural representation.
Embodiment
Below in conjunction with accompanying drawing of the present invention, be clearly and completely described technical scheme of the present invention, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
According to Fig. 1, Fig. 2, Fig. 3, as preferred embodiment, a kind of stirring-type fluorination electrolytic cell, is made up of motor 1, shaft coupling 2, stir shaft 3, shaft seal 4, electrode column 5, leg 6, electrode bundle 7, liquidometer 8, electrolyzer 9, reduction cell cover plate 10, electrolyzer chuck 11, axle sleeve 12, blind plate 13, guide shell 14, stirring rake 15, insulating washer 16, thermal insulation layer 17, thermometer 18.
The motor 1 of electrolyzer adopts the step-down gear of general still electric drilling match, rotating speed 10-150 revs/min, and according to stirring circulation of elecrolyte number of times, the embodiment of the present invention is set to 3 turns-20 revs/min, also can install control module additional and control this motor speed.
Electrolyzer 9 and reduction cell cover plate 10 are circular or rectangular configuration, adopt low-carbon steel material to make; Reduction cell cover plate 10 covers on electrolyzer 9, and electrolyzer arranges discharge port 91 and opening for feed 92, and discharge outlet arranges bleeder valve 93; Opening for feed 91 is imports of electrolytic solution and material, and leg 6 is arranged on bottom of electrolytic tank, generally arranges three or four legs, for electrolyzer is positioned over ground, hanger also can be adopted to be positioned on operator's console by electrolyzer; Discharge port 92 is discharge ports of the product of electrofluorination reaction, and discharge port adopts bend pipe convenient operation, controls discharging with bleeder valve 93.
Electrolyzer chuck 11 is arranged on the outside surrounding of electrolyzer and bottom, and electrolyzer chuck 11 arranges refrigerant import 111 and refrigerant exit 112; Refrigerant import 111 and refrigerant exit 112 are import and export of electrolyzer chuck 11 refrigerant, refrigerant adopts general chilled brine or organic refrigerant to take away the heat of electrolytic reaction, be used for controlling electrolyte temperature in electrolyzer, general electrolysis temperature controls between-10 DEG C-19 DEG C; One layer of heat preservation layer 17 is had to reduce the cold loss of refrigerant outside electrolyzer chuck 11.
Motor is connected with stir shaft 3 by shaft coupling 2.Stir shaft 3 is by shaft seal 4 through reduction cell cover plate, and stir shaft keeps hydrogen fluoride in electrolyzer can not leak in air by the shaft seal 4 on reduction cell cover plate.
Electrode column 5 is fixed on reduction cell cover plate 10 after being connected with the electrode bundle 7 in electrolyzer, separates between electrode column 5 and reduction cell cover plate with insulating washer 16.
According to Fig. 2, the positive pole that electrode column 5 comprises and negative pole, the positive pole of corresponding connection electrode bundle 7 and negative pole, electrode bundle conveniently nickel positive pole, iron negative pole is alternately arranged, tetrafluoroethylene pad mutually insulated is adopted between positive and negative electrode, arranged in parallelly separate, electrode bundle, between guide shell outer wall and electrolyzer inwall, is evenly arranged around guide shell.Electrode bundle is around the outer wall circular of guide shell, evenly arrangement two groups, three groups or multi-group electrode bundle, the pole plate arrangement centerline direction of electrode bundle is consistent with the normal of guide shell, electrode bundle magnitude setting and interval, under ensureing the effect that the electrolytic solution stirred promotes at stirring arm 15, by the gap of electrode bundle.
According to Fig. 3, guide shell 14 is the cylinders be fixed on reduction cell cover plate, and guide shell is fixed on reduction cell cover plate can ensure that agitator is consistent with the gap of guide shell; In the middle part of guide shell 14,2-4 openings 141 are set in the following barrel position of electrolysis liquid surface, the size of opening is as the criterion with the internal circulating load that can ensure electrolytic solution overflow and enter guide shell, guide shell 14 bottom arranges 2-4 openings 142, opening direction faces the direction that electrode bundle 7 hits exactly, and is circulated get back to opening 141 after electrolytic solution flows out 142 from opening by electrode bundle gap; Arrange blind plate 13 bottom guide shell 14, arrange axle sleeve 12 in the middle of blind plate 17, the spindle nose of stir shaft 3 can rotate and can reduce the swing of stir shaft 3 in axle sleeve 16, and the setting of blind plate simultaneously does not affect the precipitation of high fluorine product in electrolyzer; Stirring rake 15 is positioned at guide shell, and stir shaft 3 is connected with stirring rake 15, promotes electrolytic solution at electrolyzer internal circulation flow when stirring rake 15 rotates.Electrolytic reaction by stir using in electrolyzer as the anhydrous hydrogen fluoride of solvent and reaction reagent be dissolved in organic residue cycling in hydrogen fluoride and flow, thus increase the contact probability of material and pole plate, electrofluorination reaction efficiency is improved greatly, also makes heat transfer efficiency in electrolyzer improve greatly.
Liquidometer 8 is used to refer to the liquid level of electrolyzer electrolyte inside, and thermometer 18 is used for measuring the temperature of electrolytic solution; The fixing port of thermometer on reduction cell cover plate, thermometer one end passes from reduction cell cover plate, liquidometer or the other one end of thermometer are positioned at electrolyzer and also comprise liquidometer, and cell wall upper and lower end vertically arranges the fixing port of two liquidometers respectively, and liquidometer pipe adopts transparent fluorine to mould pipe.
Reduction cell cover plate setting out gas port 101, is discharge the outlet of hydrogen that electrolysis produces, and is also that outlet and the hydrogen fluoride taken out of of gaseous products can be collected after condensation, adopts the condenser reflux of industry routine to electrolyzer; Also can a refluxing opening be on the cover board set separately, the hydrogen fluoride that hydrogen or gaseous products in order to collect discharge electrolysis generation are taken out of.
The present invention adopts the stirring rake in guide shell, under the effect of stirring rake, material is made initiatively to enter in guide shell by the import 141 of guide shell, flow out from outlet 142, dissolve in whole system and dispersion evenly, simultaneously material carries out fluoridation in a cell, decreases decomposition induction time, the bleeder valve 93 that the liquid product of gained is arranged from discharge port and discharge outlet flows out, and gaseous product evaporates into cold-trap from air outlet and is collected.。
The above; be only the specific embodiment of the present invention, but protection scope of the present invention is not limited thereto, is anyly familiar with those skilled in the art in the technical scope that the present invention discloses; change can be expected easily or replace, all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should described be as the criterion with the protection domain of claim.
Claims (8)
1. a stirring-type fluorination electrolytic cell, by motor, shaft coupling, stir shaft, shaft seal, electrode column, electrode bundle, electrolyzer, reduction cell cover plate, electrolyzer chuck, axle sleeve, blind plate, guide shell, stirring rake, insulating washer forms, reduction cell cover plate covers on electrolyzer, electrolyzer arranges discharge port and opening for feed, discharge outlet arranges bleeder valve, electrolyzer chuck is arranged on the outside surrounding of electrolyzer and bottom, electrolyzer chuck arranges refrigerant import and refrigerant exit, motor is connected with stir shaft by shaft coupling, stir shaft passes reduction cell cover plate by shaft seal, electrode column is fixed on reduction cell cover plate after being connected with the electrode bundle in electrolyzer, separates with cover plate insulating washer, the positive pole that electrode column comprises and negative pole, the positive pole of corresponding connection electrode bundle and negative pole, electrode bundle is nickel positive pole conveniently, iron negative pole is alternately arranged, just, insulating trip is adopted to separate between negative pole, electrode bundle is between guide shell outer wall and electrolyzer inwall, evenly arrange around guide shell, it is characterized in that: guide shell is fixed on reduction cell cover plate, in the middle part of guide shell, 2-4 openings are set in the following barrel position of electrolysis liquid surface, guide shell bottom arranges 2-4 openings, opening direction faces electrode bundle center, arranges blind plate bottom guide shell, arranges axle sleeve in the middle of blind plate, stirring rake is positioned at guide shell, and stir shaft is connected with stirring rake.
2. a kind of stirring-type fluorination electrolytic cell according to claim 1, is characterized in that: described electrolyzer and reduction cell cover plate are circular or rectangular configuration.
3. a kind of stirring-type fluorination electrolytic cell according to claim 2, it is characterized in that: described electrode bundle is around the outer wall circular of guide shell, evenly arrangement two groups, three groups or multi-group electrode bundle, and the pole plate arrangement centerline direction of electrode bundle is consistent with the normal of guide shell.
4. a kind of stirring-type fluorination electrolytic cell according to claim 1, is characterized in that: described reduction cell cover plate sets out gas port.
5., according to the arbitrary described a kind of stirring-type fluorination electrolytic cell of Claims 1-4, it is characterized in that: outside described electrolyzer chuck, thermal insulation layer is set.
6. a kind of stirring-type fluorination electrolytic cell according to claim 5, is characterized in that: also comprise thermometer, and set temperature meter fixing port on cell wall cover plate, thermometer one end passes from reduction cell cover plate, and one end is positioned at electrolyzer in addition.
7. a kind of stirring-type fluorination electrolytic cell according to claim 6, is characterized in that: also comprise liquidometer, and cell wall upper and lower end vertically arranges the fixing port of two liquidometers respectively, and liquidometer pipe adopts transparent fluorine to mould pipe.
8. a kind of stirring-type fluorination electrolytic cell according to claim 7, it is characterized in that: also comprise leg, leg is arranged on bottom of electrolytic tank, and quantity arranges three or four.
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| CN201310140764.6A CN103243341B (en) | 2013-04-23 | 2013-04-23 | A kind of stirring-type fluorination electrolytic cell |
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| CN201310140764.6A CN103243341B (en) | 2013-04-23 | 2013-04-23 | A kind of stirring-type fluorination electrolytic cell |
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| CN103243341B true CN103243341B (en) | 2016-03-23 |
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| CN105202309B (en) * | 2014-06-24 | 2017-09-26 | 北大方正集团有限公司 | Pipeline mixing device and plasma chemical vapor deposition equipment |
| CN104109881B (en) * | 2014-07-30 | 2017-09-15 | 天门福临金富精细化工有限公司 | A kind of parallel circulating type fluorination electrolytic cell |
| CN109161918A (en) * | 2018-11-22 | 2019-01-08 | 铜陵华兴精细化工股份有限公司 | A kind of electrolytic cell convenient for crystallization |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1236828A (en) * | 1992-07-30 | 1999-12-01 | 明尼苏达矿产制造公司 | Bipolar flow cell and process for electrochemical fluorination |
| CN202465278U (en) * | 2012-02-17 | 2012-10-03 | 湖北诺邦化学有限公司 | Device for preparing high purity phosphorus pentafluoride gas by solid-phase method |
| CN102839384A (en) * | 2011-06-21 | 2012-12-26 | 叶姝菡 | Compulsory internal recycle fluorination electrolysis reactor |
| CN203270046U (en) * | 2013-04-23 | 2013-11-06 | 湖北诺邦化学有限公司 | Stirring type fluorinated electrolytic bath |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3037919A (en) * | 1958-07-22 | 1962-06-05 | Dow Chemical Co | Preparation of hexafluoroethane and higher fluorocarbons |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1236828A (en) * | 1992-07-30 | 1999-12-01 | 明尼苏达矿产制造公司 | Bipolar flow cell and process for electrochemical fluorination |
| CN102839384A (en) * | 2011-06-21 | 2012-12-26 | 叶姝菡 | Compulsory internal recycle fluorination electrolysis reactor |
| CN202465278U (en) * | 2012-02-17 | 2012-10-03 | 湖北诺邦化学有限公司 | Device for preparing high purity phosphorus pentafluoride gas by solid-phase method |
| CN203270046U (en) * | 2013-04-23 | 2013-11-06 | 湖北诺邦化学有限公司 | Stirring type fluorinated electrolytic bath |
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