CN204898094U - Novel fluoridize electrolysis trough - Google Patents

Abstract

The utility model relates to a novel fluoridize electrolysis trough, including the electrolysis trough, the electrolysis trough presss from both sides the cover, electrode post and electrode are restrainted, be provided with the electrolysis trough apron on the electrolysis trough, the electrolysis trough presss from both sides the cover and sets up around the electrolysis trough outside, the electrolysis trough presss from both sides the cover and sets up refrigerant import and refrigerant outlet, the refrigerant import sets up presss from both sides the cover upper end at the electrolysis trough, refrigerant outlet sets up and presss from both sides the cover bottom at the electrolysis trough, the discharge gate passes through the discharging pipe and is connected with the liquid pump, electrolysis trough apron center is provided with the water distributor, be provided with a plurality of outlet pipes on the circumference of water distributor, the delivery port of outlet pipe is provided with the atomizer, the liquid pump pass through the feed pipe with cloth water piping connection, the refrigerant that presss from both sides the electrolysis trough in the cover gets into the bottom play from the upper end that the electrolysis trough pressed from both sides the cover for inslot electrolyte temperature is more even, and the electrolytic efficiency is high, takes electrolyte from the bottom out through the liquid pump, spouts to electrolysis trough inside through the shower nozzle at the electrolysis trough top, makes pneumatolytic HF erodeed by electrolyte and washes down, and in the electrolysis trough, it is littleer to make HF lose.

Description

A kind of novel fluorination electrolytic cell

Technical field

This practicality relates to the technical field of the electrolyzer of Organic Electrochemical Synthesis, particularly relates to a kind of novel fluorination electrolytic cell.

Background technology

Organic fluorocompound nature exists few, how fluorine to be introduced in organism the problem becoming people and be badly in need of solving, the preparation of organic fluoride directly can be fluoridized with F2, the method also indirectly can fluoridized with fluorination reagents such as XeF2, Hydroxyl fluoride, high-valence metal fluoride, N2F compounds.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, F2 can not overflow, and 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: 1, in existing fluorination electrolytic cell, chilled brine in external jacket generally enters bottom chuck, on bring out, make electrolyte bath non-uniform temperature, electrolysis effectiveness is not good, 2, 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, after making alive, and no current input, 3, in existing electrolyzer, HF collects by condenser again to recycle, and efficiency is not high.

Utility model content

In order to solve the technical problem of above-mentioned existence, the utility model provides a kind of novel fluorination electrolytic cell, and concrete technical scheme is:

A kind of novel fluorination electrolytic cell, it is characterized in that: 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, described electrolyzer is provided with reduction cell cover plate, motor is connected with stir shaft by shaft coupling, stir shaft passes reduction cell cover plate by shaft seal, described guide shell is fixed on reduction cell cover plate, bottom described guide shell, blind plate is set, in the middle of blind plate, axle sleeve is set, stirring rake is positioned at guide shell, stir shaft is connected with stirring rake, in described electrolyzer, electrode bundle is set, described electrode column is fixed on reduction cell cover plate after being connected with the electrode bundle in electrolyzer, described electrode column and cover plate insulating washer separate, electrode column comprises positive pole and negative pole, the positive pole of described electrode column positive pole and the corresponding connection electrode bundle of negative pole 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, described electrolyzer chuck is arranged on the outside surrounding of electrolyzer, described electrolyzer chuck arranges refrigerant import and refrigerant exit, described refrigerant import is arranged on electrolyzer chuck upper end, described refrigerant exit is arranged on electrolyzer chuck lower end, electrolyzer arranges discharge port and opening for feed, described discharge port is connected with liquid pump by discharge nozzle, described reduction cell cover plate center is provided with liquid distributor, described liquid distributor be circumferentially provided with multiple drain pipe, the liquid outlet of each drain pipe is separately positioned on top position in electrolyzer, the liquid outlet of described drain pipe is provided with shower nozzle, described liquid pump is connected with described liquid distributor by feed pipe, each drain pipe is all connected with feed pipe, discharge outlet arranges bleeder valve.

Further: what described refrigerant import was placed is chilled brine or organic refrigerant.

Further: described electrolyzer and reduction cell cover plate are circular or rectangular configuration, described 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, described reduction cell cover plate sets out gas port, outside described electrolyzer chuck, thermal insulation layer is set.

The compared with prior art acquired technique effect of the utility model is: entered the upper end of the refrigerant in electrolyzer chuck from electrolyzer chuck, bottom goes out, and make electrolyte bath electrolytic solution overhead temperature low, lower surface temperature is higher, because electrolyte temperature is low above, compare greatly important, the electrolytic solution that temperature is low sinks, and electrolytic solution higher below floats, therefore, electrolytic solution forms an internal recycle in groove, and make groove electrolyte inside temperature more even, electrolytic efficiency is higher.

Add pump circulation device additionally by electrolytic solution electrolytic solution is extracted out from bottom, spray to electrolyte bath at electrolyzer top by shower nozzle, the HF gasified is washed away by electrolytic solution and washes down, come back in electrolyzer, HF is lost less, energy-conserving and environment-protective.

Finally in electrolyzer, be provided with whipping appts, the tilting stirring rake of polylith is provided with between two agitator arms stirring frame, between the plate face of stirring rake and horizontal plane, the angle of angle is 55 degree ~ 65 degree, material in reactor can fully be uniformly mixed, 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

Fig. 1 is the utility model fluorination electrolytic cell structural representation.

Fig. 2 is the partial enlarged drawing of A in Fig. 1.

Embodiment

Below in conjunction with accompanying drawing 1,2, the utility model is described.

Fig. 1, the novel fluorination electrolytic cell of one shown in Fig. 2, by motor 1, shaft coupling 2, stir shaft 3, shaft seal 4, electrode column 5, electrode bundle 6, electrolyzer 7, reduction cell cover plate 8, electrolyzer chuck 9, axle sleeve 10, blind plate 11, guide shell 12, stirring rake 13, insulating washer 14 forms, described electrolyzer 7 is provided with reduction cell cover plate 8, motor 1 is connected with stir shaft 3 by shaft coupling 2, stir shaft 3 passes reduction cell cover plate 8 by shaft seal 4, described guide shell 12 is fixed on reduction cell cover plate 8, bottom described guide shell 12, blind plate 11 is set, in the middle of blind plate 11, axle sleeve 10 is set, stirring rake 13 is positioned at guide shell 12, stir shaft 3 is connected with stirring rake 13, in described electrolyzer 7, electrode bundle 6 is set, described electrode column 5 is fixed on reduction cell cover plate 8 after being connected with the electrode bundle 6 in electrolyzer 7, described electrode column 5 separates with cover plate 8 insulating washer 14, electrode column 5 comprises positive pole and negative pole, the positive pole of described electrode column positive pole and the corresponding connection electrode bundle of negative pole 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 12 outer wall and electrolyzer 7 inwall, evenly arrange around guide shell 12, described electrolyzer chuck 9 is arranged on the outside surrounding of electrolyzer 7, described electrolyzer chuck 9 arranges refrigerant import 15 and refrigerant exit 16, described refrigerant import 15 is arranged on electrolyzer chuck 9 upper end, described refrigerant exit 16 is arranged on electrolyzer chuck 9 lower end, electrolyzer 7 arranges discharge port 17 and opening for feed 18, described discharge port 17 is connected with liquid pump 20 by discharge nozzle 19, described reduction cell cover plate 8 center is provided with liquid distributor 21, described liquid distributor 21 be circumferentially provided with multiple drain pipe 22, the liquid outlet of each drain pipe 22 is separately positioned on top position in electrolyzer 7, the liquid outlet of described drain pipe 22 is provided with shower nozzle 23, described liquid pump 20 is connected with described liquid distributor 21 by feed pipe 24, each drain pipe 22 is all connected with feed pipe 24, discharge port 17 place arranges bleeder valve 25.

Further: what described refrigerant import 15 was placed is chilled brine or organic refrigerant.

Further: described electrolyzer 7 and reduction cell cover plate 8 are circular or rectangular configuration, described electrode bundle 6 is around the outer wall circular of guide shell 12, evenly arrangement two groups, three groups or multi-group electrode bundle 6, the pole plate arrangement centerline direction of electrode bundle 6 is consistent with the normal of guide shell 12, arranges thermal insulation layer 26 outside described electrolyzer chuck 9.

The upper end of refrigerant in electrolyzer chuck from electrolyzer chuck enters by the utility model, bottom goes out, and make electrolyte bath electrolytic solution overhead temperature low, lower surface temperature is higher, because electrolyte temperature is low above, compare greatly important, the electrolytic solution that temperature is low sinks, and electrolytic solution higher below floats, therefore, electrolytic solution forms an internal recycle in groove, and make groove electrolyte inside temperature more even, electrolytic efficiency is higher.

Whipping appts is provided with in addition in electrolyzer, the tilting stirring rake of polylith is provided with between two agitator arms stirring frame, between the plate face of stirring rake and horizontal plane, the angle of angle is 55 degree ~ 65 degree, material in reactor can fully be uniformly mixed, 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.

Add pump circulation device finally by electrolytic solution electrolytic solution is extracted out from bottom, spray to electrolyte bath at electrolyzer top by shower nozzle, the HF gasified is washed away by electrolytic solution and washes down, come back in electrolyzer, HF is lost less, energy-conserving and environment-protective.

The above is only preferred implementation of the present utility model; should be understood that; for those skilled in the art; under the prerequisite not departing from the utility model know-why; can also make some improvement and modification, these improve and modification also should be considered as protection domain of the present utility model.

Claims (3)

1. a novel fluorination electrolytic cell, it is characterized in that: 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, described electrolyzer is provided with reduction cell cover plate, motor is connected with stir shaft by shaft coupling, stir shaft passes reduction cell cover plate by shaft seal, described guide shell is fixed on reduction cell cover plate, bottom described guide shell, blind plate is set, in the middle of blind plate, axle sleeve is set, stirring rake is positioned at guide shell, stir shaft is connected with stirring rake, in described electrolyzer, electrode bundle is set, described electrode column is fixed on reduction cell cover plate after being connected with the electrode bundle in electrolyzer, described electrode column and cover plate insulating washer separate, electrode column comprises positive pole and negative pole, the positive pole of described electrode column positive pole and the corresponding connection electrode bundle of negative pole 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, described electrolyzer chuck is arranged on the outside surrounding of electrolyzer, described electrolyzer chuck arranges refrigerant import and refrigerant exit, described refrigerant import is arranged on electrolyzer chuck upper end, described refrigerant exit is arranged on electrolyzer chuck lower end, electrolyzer arranges discharge port and opening for feed, described discharge port is connected with liquid pump by discharge nozzle, described reduction cell cover plate center is provided with liquid distributor, described liquid distributor be circumferentially provided with multiple drain pipe, the liquid outlet of each drain pipe is separately positioned on top position in electrolyzer, the liquid outlet of described drain pipe is provided with shower nozzle, described liquid pump is connected with described liquid distributor by feed pipe, each drain pipe is all connected with feed pipe, discharge outlet arranges bleeder valve.

2. novel fluorination electrolytic cell according to claim 1, is characterized in that: what described refrigerant import was placed is chilled brine or organic refrigerant.

3. novel fluorination electrolytic cell according to claim 1, it is characterized in that: described electrolyzer and reduction cell cover plate are circular or rectangular configuration, described 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, described reduction cell cover plate sets out gas port, outside described electrolyzer chuck, thermal insulation layer is set.