CN103243341A - Stirring fluorination electrolytic cell - Google Patents
Stirring fluorination electrolytic cell Download PDFInfo
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- CN103243341A CN103243341A CN2013101407646A CN201310140764A CN103243341A CN 103243341 A CN103243341 A CN 103243341A CN 2013101407646 A CN2013101407646 A CN 2013101407646A CN 201310140764 A CN201310140764 A CN 201310140764A CN 103243341 A CN103243341 A CN 103243341A
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Abstract
The invention discloses a stirring fluorination electrolytic cell which comprises a motor, a coupling, a stirring shaft, a shaft seal, an electrode mast, an electrode beam, an electrolytic cell, an electrolytic cell cover plate, an electrolytic cell jacket, a sleeve pipe, a blind plate, a guide drum, a stirring paddle and an insulating gasket. According to the invention, materials are dissolved and dispersed uniformly in the whole system, fluoridation is carried out in the electrolytic cell simultaneously, the reaction induction period is reduced to one day from 3-5 days, a cell blocking phenomenon is eliminated by and large, the frequency of cleaning the cell by treating cell blocking is reduced, the cell blocking phenomenon occurs 3-4 times per year in the prior art when the stirring cell is not used while the cell blocking phenomenon is avoided when the stirring cell provided by the invention is used, the material consumption is reduced by over 20%, the capacity in unit cell is improved by 30%, polymers generated in the electrolytic cell are reduced, the cell cleaning period is prolonged by one time, and the labor intensity in manually cleaning the cell is reduced.
Description
Technical field
The present invention relates to the technical field of the synthetic electrolyzer of organic electrochemistry, relate in particular to a kind of stirring-type and fluoridize electrolyzer.
Background technology
The organic fluorocompound nature exists few, and how fluorine being introduced becomes the problem that people are badly in need of solving in the organism, and the preparation of organic fluoride can be used F
2Directly fluoridize, also available XeF
2, fluorination reagent such as Hydroxyl fluoride, high-valency metal fluorochemical, the N2F compounds method of fluoridizing indirectly.These chemical fluorination process, reaction and operation are all complicated, and the equipment that needs is relatively harsher; The fluorination reagent toxicity of using 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.Americanized scholar Simons had invented electrochemical fluorination (ECF) method in 1941, produce perfluor or partially fluorinated organic compound, for example full-fluorine octyl sulfuryl fluoride, perfluoro butyl sulfonic acid fluoride, perfluoro triethylamine etc., its invention is for a brand-new and marvellous approach has been opened up in the preparation of fluorocarbon.Initial Simons method is in the steel electrolyzer of rectangle or circle one group of nickel anode and iron cathode pole plate to be installed alternately, adds anhydrous hydrogen fluoride and a small amount of organism, and logical direct current carries out electrolysis.Electrolyzer external application cooling jacket is removed the heat that produces in the electrolytic process.Usually bath voltage is 5V-8V, and current density is greater than 500A/dm2, and temperature range is 0 ℃-9 ℃.With this understanding, F
2Can not overflow, fluorinated product then generates at anode.The fluorochemical that generates is owing to be insoluble to anhydrous hydrogen fluoride, or is deposited on bottom of electrolytic tank, or is gas phase and evaporates in the cold-trap and be collected.But traditional electrolyzer has following shortcoming: the HF in the groove does not flow, and the ionogen and the pole plate contact probability that are dissolved among the HF are little, so the electrofluorination reaction efficiency is low; Reaction electrofluorination decomposition induction time is long, be generally 3 days-5 days, and dead groove phenomenon is more frequent, and behind making alive, the no current input.
Summary of the invention
At above-mentioned defective 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 a kind of stirring-type that can reduce dead groove phenomenon is fluoridized electrolyzer.
In order to achieve the above object, the invention provides following technical scheme: a kind of stirring-type is fluoridized electrolyzer, by motor, shaft coupling, stir shaft, shaft seal, electrode column, electrode bundle, electrolyzer, the electrolyzer cover plate, the electrolyzer chuck, axle sleeve, blind plate, guide shell, stirring rake, insulating washer is formed, the electrolyzer cover plate covers on electrolyzer, electrolyzer arranges discharge port and opening for feed, the discharge port place arranges bleeder valve, the electrolyzer chuck is arranged on around the electrolyzer outside and the bottom, the electrolyzer chuck arranges refrigerant import and refrigerant exit, shaft coupling is connected motor with stir shaft, stir shaft passes the electrolyzer cover plate by shaft seal, after being connected, electrode bundle in electrode column and the electrolyzer is fixed on the electrolyzer cover plate, separate with insulating washer with cover plate, the positive pole that electrode column comprises and negative pole, positive pole and the negative pole of corresponding connection electrode bundle, electrode bundle is according to conventional nickel positive pole, the iron negative pole is alternately arranged, just, adopt insulating trip to separate between the negative pole, electrode bundle is between guide shell outer wall and electrolyzer inwall, evenly arrange around guide shell, guide shell is fixed on the electrolyzer cover plate, the guide shell middle part arranges 2-4 openings in the following barrel of electrolysis liquid surface position, the guide shell bottom arranges 2-4 mouths, the guide shell bottom arranges blind plate, axle sleeve is set in the middle of the blind plate, stirring rake is positioned at guide shell, and stir shaft is connected with stirring rake.
In the technique scheme, described electrolyzer and electrolyzer cover plate are circle or rectangular configuration.
In the technique scheme, described electrode bundle around the outer wall circular of guide shell, evenly arrange two groups, three groups or multi-group electrode bundle, the pole plate of the electrode bundle centerline direction of arranging is consistent with the normal of guide shell.
In the technique scheme, set out gas port on the described electrolyzer cover plate.
Optimized technical scheme, described electrolyzer chuck outside arranges thermal insulation layer.
Optimized technical scheme also comprises thermometer, and the thermometer fixing port is set on the cell wall cover plate, and liquid level meter one end passes from the electrolyzer cover plate, and an other end is positioned at electrolyzer.
Optimized technical scheme also comprises liquidometer, and the electrolyzer wallboard powers on and separates the fixing port that cell wall plate upper and lower end vertically arranges two liquidometers respectively, and the liquidometer pipe adopts transparent fluorine to mould pipe.
Optimized 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 provided by the invention is fluoridized electrolyzer, make material in whole system, dissolve and disperse more even, in electrolyzer, carry out simultaneously fluoridation, reduced decomposition induction time, decomposition induction time reduced to one day from 3-5 days, also stopped dead groove phenomenon basically, minimizing is because of the number of times of the clear groove of handling dead groove, and the in the past annual dead groove of employing shunt slot 3-4 time adopts after the shunt slot of the present invention, dead groove phenomenon does not take place, reduce supplies consumption more than 20%, single groove output improves 30%, and the polymkeric substance that generates in the electrolyzer reduces, one times of clear groove time lengthening has alleviated artificial clear groove labour intensity.
Description of drawings
In order to be illustrated more clearly in the embodiment of the invention or technical scheme of the prior art, to do to introduce simply to the accompanying drawing of required use in embodiment or the description of the Prior Art below, apparently, accompanying drawing in describing below only is some embodiments of the present invention, for those of ordinary skills, under the prerequisite of not paying creative work, can also obtain other accompanying drawing according to these accompanying drawings.
Fig. 1 is embodiment of the invention structural representation.
Fig. 2 is embodiment electrode bundle distributed architecture synoptic diagram.
Fig. 3 is the guide shell structural representation.
Embodiment
Below in conjunction with accompanying drawing of the present invention, technical scheme of the present invention is clearly and completely described, obviously, described embodiment only is the present invention's part embodiment, rather than whole embodiment.Based on the embodiment among the present invention, those of ordinary skills belong to the scope of protection of the invention not making the every other embodiment that obtains under the creative work prerequisite.
According to Fig. 1, Fig. 2, shown in Figure 3, as preferred embodiment, a kind of stirring-type is fluoridized electrolyzer, is made up of motor 1, shaft coupling 2, stir shaft 3, shaft seal 4, electrode column 5, leg 6, electrode bundle 7, liquid level meter 8, electrolyzer 9, electrolyzer 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 general still step-down gear of electric drilling match, 10-150 rev/mins of rotating speeds, and according to stirring the circulation of elecrolyte number of times, the embodiment of the invention is set to 3 changes-20 rev/mins, also can install control module additional this motor speed is controlled.
Electrolyzer 9 is circle or rectangular configuration with electrolyzer cover plate 10, adopts low-carbon steel material to make; Electrolyzer cover plate 10 covers on electrolyzer 9, and electrolyzer arranges discharge port 91 and opening for feed 92, and the discharge port place 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, and three or four legs of operated by rotary motion are used for electrolyzer is positioned over ground, also can adopt hanger that electrolyzer is positioned on the operator's console; Discharge port 92 is discharge ports of the product of electrofluorination reaction, and discharge port adopts bend pipe to be convenient to operation, with bleeder valve 93 control dischargings.
Be fixed on the electrolyzer cover plate 10 after electrode bundle 7 in electrode column 5 and the electrolyzer is connected, separate with insulating washer 16 between electrode column 5 and the electrolyzer cover plate.
According to shown in Figure 2, the positive pole that electrode column 5 comprises and negative pole, positive pole and the negative pole of corresponding connection electrode bundle 7, electrode bundle is alternately arranged according to conventional nickel positive pole, iron negative pole, adopt tetrafluoroethylene pad mutually insulated between the positive and negative electrode, being arranged in parallel separates, and electrode bundle is evenly arranged around guide shell between guide shell outer wall and electrolyzer inwall.Electrode bundle around the outer wall circular of guide shell, evenly arrange two groups, three groups or multi-group electrode bundle, the pole plate of the electrode bundle centerline direction of arranging is consistent with the normal of guide shell, electrode bundle arranges quantity and interval, the electrolytic solution that guarantees to stir is under the effect that stirring arm 15 promotes, by the gap of electrode bundle.
According to shown in Figure 3, guide shell 14 is cylinders that are fixed on the electrolyzer cover plate, and guide shell is fixed on and can guarantees on the electrolyzer cover plate that agitator is consistent with the gap of guide shell; Guide shell 14 middle parts arrange 2-4 openings 141 in the following barrel of electrolysis liquid surface position, the size of opening is as the criterion can guarantee the internal circulating load that the electrolytic solution overflow enters guide shell, guide shell 14 bottoms arrange 2-4 openings 142, opening direction faces the direction of electrode bundle 7 centers, and electrolytic solution circulates by the electrode bundle gap from opening outflow 142 backs and gets back to opening 141; Guide shell 14 bottoms arrange blind plate 13, and axle sleeve 12 is set in the middle of the blind plate 17, and 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 does not simultaneously influence the precipitation of high fluorine product in the electrolyzer; Stirring rake 15 is positioned at guide shell, and stir shaft 3 is connected with stirring rake 15, promotes electrolytic solution during stirring rake 15 rotations and flows at the electrolyzer internal recycle.Electrolytic reaction by stir with in the electrolyzer as the anhydrous hydrogen fluoride of solvent and reaction reagent be dissolved in that organic materials circulates in the hydrogen fluoride, thereby increase the contact probability of material and pole plate, the electrofluorination reaction efficiency is improved greatly, also make the interior heat transfer efficiency of electrolyzer improve greatly.
Setting out gas port 101 on the electrolyzer cover plate, is the outlet of discharging the hydrogen that electrolysis produces, and also is that the outlet of gaseous products and the hydrogen fluoride taken out of can be collected after condensation, adopts the condenser of industry routine to be back to electrolyzer; Also a refluxing opening can be set separately on the cover board, discharge the hydrogen of electrolysis generation or the hydrogen fluoride that gaseous products is taken out of in order to collection.
The present invention adopts the stirring rake in the guide shell, under the effect of stirring rake, make material initiatively enter in the guide shell by the import 141 of guide shell, flow out from exporting 142, dissolving and dispersion is more even in whole system, and material carries out fluoridation in electrolyzer simultaneously, has reduced decomposition induction time, the liquid product of gained flows out from the bleeder valve 93 of discharge port and discharge port setting, and gaseous product evaporates into the cold-trap from the air outlet and is collected.。
The above; only be the specific embodiment of the present invention, but protection scope of the present invention is not limited thereto, anyly is familiar with those skilled in the art in the technical scope that the present invention discloses; can expect easily changing or replacing, all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion by described protection domain with claim.
Claims (8)
1. a stirring-type is fluoridized electrolyzer, by motor, shaft coupling, stir shaft, shaft seal, electrode column, electrode bundle, electrolyzer, the electrolyzer cover plate, the electrolyzer chuck, axle sleeve, blind plate, guide shell, stirring rake, insulating washer is formed, the electrolyzer cover plate covers on electrolyzer, electrolyzer arranges discharge port and opening for feed, the discharge port place arranges bleeder valve, the electrolyzer chuck is arranged on around the electrolyzer outside, the electrolyzer chuck arranges refrigerant import and refrigerant exit, shaft coupling is connected motor with stir shaft, stir shaft passes the electrolyzer cover plate by shaft seal, after being connected, electrode bundle in electrode column and the electrolyzer is fixed on the electrolyzer cover plate, separate with insulating washer with cover plate, the positive pole that electrode column comprises and negative pole, positive pole and the negative pole of corresponding connection electrode bundle, electrode bundle is according to conventional nickel positive pole, the iron negative pole is alternately arranged, just, adopt insulating trip to separate between the 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 the electrolyzer cover plate, the guide shell middle part arranges 2-4 openings in the following barrel of electrolysis liquid surface position, the guide shell bottom arranges 2-4 mouths, the guide shell bottom arranges blind plate, axle sleeve is set in the middle of the blind plate, stirring rake is positioned at guide shell, and stir shaft is connected with stirring rake.
2. a kind of stirring-type according to claim 1 is fluoridized electrolyzer, it is characterized in that: described electrolyzer and electrolyzer cover plate are circle or rectangular configuration.
3. a kind of stirring-type according to claim 2 is fluoridized electrolyzer, it is characterized in that: described electrode bundle around the outer wall circular of guide shell, evenly arrange two groups, three groups or multi-group electrode bundle, the pole plate of the electrode bundle centerline direction of arranging is consistent with the normal of guide shell.
4. a kind of stirring-type according to claim 1 is fluoridized electrolyzer, it is characterized in that: set out gas port on the described electrolyzer cover plate.
5. fluoridize electrolyzer according to the arbitrary described a kind of stirring-type of claim 1 to 4, it is characterized in that: described electrolyzer arranges chuck, and the chuck outside arranges thermal insulation layer.
6. a kind of stirring-type according to claim 5 is fluoridized electrolyzer, it is characterized in that: also comprise liquid level meter, the thermometer fixing port is set on the electrolyzer cover plate, liquid level meter one end passes from the electrolyzer cover plate, and an other end is positioned at electrolyzer.
7. a kind of stirring-type according to claim 6 is fluoridized electrolyzer, it is characterized in that: also comprise liquidometer, electrolyzer wallboard upper and lower end vertically arranges the fixing port of two liquidometers respectively, and the liquidometer pipe adopts transparent fluorine to mould pipe.
8. a kind of stirring-type according to claim 7 is fluoridized electrolyzer, it is characterized in that: also comprise leg, leg is arranged on bottom of electrolytic tank, and quantity arranges three or four.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310140764.6A CN103243341B (en) | 2013-04-23 | 2013-04-23 | A kind of stirring-type fluorination electrolytic cell |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310140764.6A CN103243341B (en) | 2013-04-23 | 2013-04-23 | A kind of stirring-type fluorination electrolytic cell |
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| Publication Number | Publication Date |
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| CN103243341A true CN103243341A (en) | 2013-08-14 |
| CN103243341B CN103243341B (en) | 2016-03-23 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104109881A (en) * | 2014-07-30 | 2014-10-22 | 天门福临金富精细化工有限公司 | Parallel circulating fluorination electrolysis bath |
| CN105202309A (en) * | 2014-06-24 | 2015-12-30 | 北大方正集团有限公司 | Pipeline stirring device and plasma chemical vapor deposition equipment |
| 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 |
| CN113731220A (en) * | 2021-09-29 | 2021-12-03 | 杭州原正工程技术装备有限公司 | Experimental device for light-density particle stirring equipment and industrial stirring equipment |
Citations (5)
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| US3037919A (en) * | 1958-07-22 | 1962-06-05 | Dow Chemical Co | Preparation of hexafluoroethane and higher fluorocarbons |
| 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 |
-
2013
- 2013-04-23 CN CN201310140764.6A patent/CN103243341B/en active Active
Patent Citations (6)
| 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 |
| 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 |
| CN1048294C (en) * | 1992-07-30 | 2000-01-12 | 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 |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105202309A (en) * | 2014-06-24 | 2015-12-30 | 北大方正集团有限公司 | Pipeline stirring device and plasma chemical vapor deposition equipment |
| 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 |
| CN104109881A (en) * | 2014-07-30 | 2014-10-22 | 天门福临金富精细化工有限公司 | Parallel circulating fluorination electrolysis bath |
| 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 |
| CN113731220A (en) * | 2021-09-29 | 2021-12-03 | 杭州原正工程技术装备有限公司 | Experimental device for light-density particle stirring equipment and industrial stirring equipment |
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| CN103243341B (en) | 2016-03-23 |
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