CN100577882C - Fluoelectrolysis reactor and reaction method - Google Patents
Fluoelectrolysis reactor and reaction method Download PDFInfo
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- CN100577882C CN100577882C CN200710076607A CN200710076607A CN100577882C CN 100577882 C CN100577882 C CN 100577882C CN 200710076607 A CN200710076607 A CN 200710076607A CN 200710076607 A CN200710076607 A CN 200710076607A CN 100577882 C CN100577882 C CN 100577882C
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- 238000009795 derivation Methods 0.000 description 2
- 230000005518 electrochemistry Effects 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
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Abstract
The invention discloses a fluorinated and electrolytic reactor and a reaction method. The reactor includes an electrolytic reaction still, electropads, negative and positive electrode outlet terminals, negative and positive electrode fitted rods, an upper clip, a lower clip, a rotation shaft, a generator and a flow guide ring. Every electropad of similar shape is superposed according to presupposition distance, the middle portion is equipped with at least a first-deflector hole and every first-deflector hole forms into a first-diversion trench. Every electropad is provided with a pair of negative and positive fitted holes which are inserted by the negative and positive fitted rods to fix the electropads and are fixedly connected with every clip. The rotation shaft is fixedly connected with the upper clip, and the generator is connected with the rotation shaft. The electrolytic solution between the electropads can flow orderly by rotating the electropads. The invention has the advantages of simple contracture, convenient assembling and disassembling and high volume rate. The product of the reactor is easy to be controlled and be outlet, which enables the reaction product to better collected and be discharged, improves the productivity of the product, and enlarges the variety of the fluorinated product of electrolytic reaction and the range of use of the electrolysis trench. Besides, the invention also solves the problem that the fluorinated electrolysis trench is difficult to be made bigger.
Description
Technical field
The present invention relates to organic electrochemistry synthetic electrolysis reactor, in particular, a kind of rotating electrode is board-like fluoridizes electrolytic reactor and reaction method.
Background technology
Organic electrolyzer of fluoridizing of prior art, its electrolysis electrode all are that positive plate, negative plate become the spaced transposition insulator of rectangle, static hanging vertical and that become to flock together to be put in the electrolyzer, are connected to outside the electrolyzer by terminal stud.Mode of connection by electrode generally can be divided into acyclic type and multipole type two class electrolyzers.
The electrode of homopolarity and direct supply are connected in parallel in the acyclic type electrolyzer, and the polarity on electrode two sides is identical, promptly are anode or simultaneously for negative electrode simultaneously.The electrode at multipole type electrolyzer two ends links to each other with the positive and negative electrode of direct supply respectively, becomes male or female.When electric current was crossed electrolyzer by placed in-line electrode stream, the one side of middle each electrode was an anode, and another side is a negative electrode, therefore had bipolarity.But the groove structure of multipole type electrolyzer and technological operation management are than acyclic type electrolyzer complexity.
In the prior art, generally adopt the electrode stack structure of the electrolyzer of Simons formula, its interpolar electrolytic solution circulates by natural force in electrolytic process, and cold and hot exchange is wherein arranged, and has the rising of gas and the decline of liquid to replenish, thereby produces the gas-liquid exchange; And different the flowing of proportion that cause of the change of reaction product.Because above these variations all belong to due to the natural force in the electrolytic reaction process, so state of wayward heat transfer and mass transfer, caused like this be that electrolyte flow is inhomogeneous, velocity of flow Be Controlled not, the environment of electrolytic reaction is just unstable, condition easily changes, that electrolysate just is difficult in the electrolytic reaction process is controlled, therefore, fluoridize electrolyzer and will do greatly also to become in more technological difficulties.
Application number is that 99107127.1 Chinese invention patent has also proposed to rely on additionaling power pump and anti-shunting device to quicken the electrolyzer and the implementation method of the electrolyte flow between pole plate.But the pressure that this mode of production produces in reactive system causes corrosive liquid to be revealed, the security that influence is produced easily.
Therefore, prior art has improved space.
Summary of the invention
The object of the present invention is to provide a kind of electrolytic reactor and reaction method fluoridized, wherein Fan Ying electrolyte flow evenly, velocity of flow can be controlled, and the environment of electrolytic reaction is stable, condition is more consistent, and electrolysate is controlled easily and derivation in the electrolytic reaction process.
Technical scheme of the present invention is as follows:
A kind ofly fluoridize electrolytic reactor, it comprises electrolytic reaction still, at least one pair of battery lead plate, a pair of anodic-cathodic leading-out end; Described pair of electrodes plate is positive plate and the negative plate that a pair of mutually insulated is provided with, and described battery lead plate is arranged in the described electrolytic reaction still, and the electrode leads to client by correspondence is connected to outside power supply respectively; Wherein, described reactor also comprises at least one pair of anode and cathode positioning screw, train wheel bridge, lower plate, turning axle, motor, a pair of positive and negative electrode guide ring and at least one pair of brush;
Described positive plate and described negative plate are flat identical shaped, and each battery lead plate is stacked by default spacing, and the centre is provided with at least one first pod apertures, and each first pod apertures forms first diversion trench when each battery lead plate is stacked;
Each battery lead plate is provided with a pair of anode and cathode pilot hole at least respectively, be used for corresponding described anode and cathode positioning screw, and positioning screw is used for fixing each battery lead plate by pilot hole, and fixedly connected with described train wheel bridge, described lower plate respectively, be used for fixing the position of each battery lead plate; The anode positioning screw is connected with described positive plate conduction by described anode pilot hole, and insulation is connected with electrolytic solution with described negative plate, and conduction is connected to the positive electrode leading-out end; The negative electrode positioning screw is connected with described negative plate conduction by described negative electrode pilot hole, and insulation is connected with electrolytic solution with described positive plate, and conduction is connected to the negative electrode leading-out end;
Described turning axle is fixedlyed connected with described train wheel bridge, and connection section is provided with second diversion trench that is connected with described first diversion trench, and described motor is connected with described turning axle, is used to rotate described turning axle;
Described train wheel bridge and described lower plate are provided with second pod apertures, the 3rd pod apertures that is connected with described first diversion trench respectively;
The brush of external source contacts by the guide ring of positive and negative electrode with the anodic-cathodic leading-out end respectively, and forming movingly, conduction connects.
Described reactor, wherein, described reactor also comprises the silk screen layer that is arranged on described reactor inwall, is used for the separation of product.
Described reactor, wherein, described train wheel bridge and/or described lower plate are negative plate, they play the fixedly effect of entire reaction electrode stack with the negative electrode screw rod.And the battery lead plate adjacent with described train wheel bridge and/or described lower plate is positive plate.
Described reactor, wherein, described reactor comprises two counter electrode plates at least, the area of each battery lead plate is identical.
Described reactor, wherein, each battery lead plate of identical polar is parallel-connected to the electrode leads to client of identical polar.
Described reactor, wherein, described positive plate is flat identical rectangle, ellipse, circle or the umbrella shape of shape with described negative plate, and, described positive plate and described negative plate are rectangle, ellipse or when circular, each battery lead plate is stacked by default spacing horizontal parallel or level of approximation.
Described reactor, wherein, described first pod apertures is arranged on the center of each battery lead plate.
Described reactor, wherein, described reactor comprises at least two pairs of anode and cathode positioning screws, at least two pairs of anode and cathode pilot holes of the corresponding at least respectively setting of each battery lead plate.
A kind ofly fluoridize electrolytic reaction method, it is applied to comprise the reactor of electrolytic reaction still, at least one pair of battery lead plate, a pair of anodic-cathodic leading-out end, at least one pair of anode and cathode positioning screw, train wheel bridge, lower plate, turning axle, motor, a pair of positive and negative electrode guide ring and at least one pair of brush; Described pair of electrodes plate is a pair of mutually insulated, by default stacked flat identical shaped positive plate and the negative plate of spacing, be respectively arranged with at least one first pod apertures in the middle of each battery lead plate, each first pod apertures forms first diversion trench when each battery lead plate is stacked; Battery lead plate is arranged in the described electrolytic reaction still, and the electrode leads to client by correspondence is connected to outside power supply respectively; Positioning screw is fixed each battery lead plate by the pilot hole of each battery lead plate, and fixedlys connected with described train wheel bridge, described lower plate respectively, and described turning axle is fixedlyed connected with described train wheel bridge, and described motor is used to rotate described turning axle; Described reaction method comprises step: A1, described rotating speed of motor is set; A2, adding reactant; A3, rotating electrode plate carry out electrolytic reaction, and wherein, electrolytic solution forms respectively from first diversion trench, and first pod apertures, the polar plate spacing electrolysis passage through each battery lead plate arrives each battery lead plate outer successively.Because of reactor is the round sealed container, electrolytic solution can return the circulation of first diversion trench.
Described reaction method, wherein, steps A 1 is further comprising the steps of: according to the proportion of reactant or product, the spacing of each battery lead plate is set.
Adopt such scheme, the present invention is by rotating electrode plate mode, and plot ratio is improved; Allow the electrolyte flow of reaction mix, and may command electrolyte flow speed, make the each point temperature of electrolytic solution more aligned, guarantee heat and mass transfer process conditional stability, thereby a more stable electrolytic reaction environment and more consistent electrolytic reaction condition are provided; Electrolysate is controlled easily and derivation in the electrolytic reaction process, and reaction product can better be discharged in enrichment, therefore, has effectively improved the productive rate of product.Simultaneously, owing to can adjust the combination of each reaction conditions, and need not increase kinetic energy and potential energy, electrolytic solution is flowed between battery lead plate; Therefore the electrolytic reaction environment is more stable, has enlarged the kind of the fluorinated product of electrolytic reaction.By the relative movement and the transport motion of battery lead plate and electrolytic solution, electrolytic solution can be flowed with the speed of a setting at interpolar.Simultaneously, make contacting in controlled continuous conversion down of electrolytic solution and battery lead plate face, outside atmosphere and condition during change electrolysis that like this can be artificial have enlarged the use range of electrolyzer, have also solved to fluoridize that electrolyzer is difficult does big problem.
Description of drawings
Fig. 1 is that the structure of a kind of embodiment of reactor of the present invention is partly cutd open synoptic diagram;
Fig. 2 is the positioned internal structural representation of a kind of embodiment of reactor of the present invention;
Fig. 3 A, Fig. 3 B, Fig. 3 C, Fig. 3 D are respectively A, the B of Fig. 2, the enlarged diagram of C, D part;
Fig. 4 A is the oval-shaped electrode board plane synoptic diagram of a kind of embodiment of reactor of the present invention;
Fig. 4 B is the circular electrode plates floor map of a kind of embodiment of reactor of the present invention.
Embodiment
Below preferred embodiment of the present invention is described in detail.
As shown in Figure 1, the invention provides a kind of electrolytic reactor 100 of fluoridizing, it comprises electrolytic reaction still 105, it is provided with kettle cover 103, be used to seal described reactor 105, the dynamic seal state that tightness system 111 is guaranteed reactor can also be set, be used to strengthen level of safety; Reactor 100 also comprises at least one pair of battery lead plate 108, a pair of anodic-cathodic leading-out end; And, also be provided with cooling jacket 106 outside the electrolytic reaction still 105, be used to cool off reactor, cooling jacket 106 can adopt the mode of liquid cooling, specifically can realize the inflow and outflow of cooling fluid or the cooling or the like that circulates by input tube 104 and output tube 110.
Described reactor also comprises at least one pair of anode and cathode positioning screw 107, train wheel bridge 301, lower plate 302, turning axle 113, motor, a pair of positive and negative electrode guide ring and at least one pair of brush.
The brush of external source should be a pair of at least, is connected with the anodic-cathodic leading-out end by the positive and negative electrode guide ring respectively, is used to anodic-cathodic that direct supply is provided.How right brush also can be, is connected with the anodic-cathodic leading-out end by the positive and negative electrode guide ring respectively, can guarantee the stability of external source and the strength of current of increase electrolytic reaction so effectively; Positive brush 101 is connected with positive electrode leading-out end (not indicating among the figure) by anodal guide ring 121; Negative pole brush 112 is connected with negative electrode leading-out end (not indicating among the figure) by negative pole guide ring 102.Brush generally can adopt carbon brush.
Reactor of the present invention also comprises turning axle 113 and motor (not indicating among the figure); Described motor is connected with described turning axle 113, is used to drive described turning axle and rotates, thereby drive each battery lead plate rotation.In general, described motor is a reducing motor, for example gear reducing motor etc.; Simultaneously, in the reactor heat-exchanger rig can also be set, for example coil heat exchanger etc. is used for the conditioned reaction temperature.Described reactor can also be provided with a silk screen layer 109 at described reactor inwall, is used for the separation and the enrichment of product, and heavy product flows out by the discharge nozzle 303 of silk screen layer below; And as shown in Figure 1, silk screen layer 109 is near the position of discharge nozzle 303, can silk screen be set or leave the bigger access opening in aperture, be convenient to the outflow of product, prevent to stop up discharge nozzle 303 simultaneously, for example the resinoid high fluorine product that is easy to stop up discharge nozzle of reaction generation.Gas is collected from reactor top by gas phase pipe (not indicating among the figure).
Described pair of electrodes plate is positive plate and the negative plate that a pair of mutually insulated is provided with, and described battery lead plate 108 is arranged in the described electrolytic reaction still 105, and the electrode leads to client by correspondence is connected to outside power supply (not indicating among the figure) respectively; Anodic-cathodic plate in the reactor 105 is by lead, and mutually insulated passes revolving hollow spindle and is connected with the positive and negative electrode guide ring; Positive plate is connected to outside power supply by positive electrode leading-out end, anodal guide ring 121, the positive brush 101 of correspondence, negative plate is connected to outside power supply by negative electrode leading-out end, negative pole guide ring 102, the negative pole brush 112 of correspondence, in general, outside power supply can adopt direct supply, also can adopt AC/DC power.
Need to prove that positive plate and negative plate adopt the electrochemical fluorination reaction, electrolytic reaction promptly of the present invention is the preparation of inert electro-conductive material, for example, adopts anhydrous hydrogen fluoride is the preparation of inert electro-conductive material.Simultaneously, by the positive plate of electro-conductive material preparation, reaction is active to electrochemical fluorination.General negative plate can be set to Duo one than positive plate, and promptly all there is a negative plate on the both sides of each piece positive plate.
And positive plate of the present invention and described negative plate are flat identical shaped, for example rectangle, ellipse, circle or umbrella shape, and each battery lead plate is stacked by default spacing; When described positive plate and described negative plate are the identical rectangle of flat shape, ellipse or when circular, each battery lead plate is stacked by default spacing level or level of approximation.Described stacked by default spacing, being about to each battery lead plate gathers into folds from level to level, can be by the actual needs of electrolytic reaction, distance between each layer battery lead plate is set, for example adopt one section insulated column or collets that the yin, yang pole plate is separated, leave the slit between each layer battery lead plate, as the runner of electrolytic solution; This moment, each stacked battery lead plate was formed electrode stack, that is electrode sheetpile or electrode plate heap.At this, the implication that shape is identical comprise that area is identical and roughly the same, profile is identical with roughly the same, shape is identical and roughly the same; Positive plate and negative plate mutually insulated, open by default intervals the centre, and default spacing can be set according to the physical and chemical performance of reactant or product, and perhaps the intensity according to Faradaic current is provided with.
For position that reinforces each battery lead plate or the position of better locating each battery lead plate, positioning screw 107 can also be set, as shown in Figure 1, positioning screw 107 can be provided with a plurality of or how right, and for example 3 perhaps, generally is that positioning screw 107 is set in pairs; Like this, the centre of positive plate and negative plate just can be by firm spaced apart of default spacing.At this moment, each battery lead plate is provided with a pair of anode and cathode pilot hole at least respectively, is used for corresponding described anode and cathode positioning screw, and, positioning screw is used for fixing each battery lead plate by pilot hole, and fixedlys connected with described train wheel bridge, described lower plate respectively, is used for fixing the position of each battery lead plate; Specifically, as shown in Figure 2, anode positioning screw 401 is connected with described positive plate conduction by described anode pilot hole, is connected with described negative plate insulation, and is connected to the positive electrode leading-out end by positive wire 404 conductions; Negative electrode positioning screw 402 is connected with described negative plate conduction by described negative electrode pilot hole, is connected with described positive plate insulation, and is connected to the negative electrode leading-out end by cathode wire 405 conductions.Be more preferably, described reactor comprises at least two pairs of anode and cathode positioning screws, at least two pairs of anode and cathode pilot holes of the corresponding at least respectively setting of each battery lead plate.For example, described reactor comprises two pairs of anode and cathode positioning screws, and each battery lead plate correspondence respectively is provided with two pairs of anode and cathode pilot holes; Perhaps described reactor comprises three pairs of anode and cathode positioning screws, and each battery lead plate correspondence respectively is provided with three pairs of anode and cathode pilot holes.
Wherein, the enlarged diagram of the A of Fig. 2, B, C, D part is respectively shown in Fig. 3 A, Fig. 3 B, Fig. 3 C, Fig. 3 D.In Fig. 3 A, anode positioning screw 401 is connected to the positive electrode leading-out end by positive wire 404 conductions, when train wheel bridge 301 is negative electrode, is provided with insulation spacer 413 between the installation nut of anode positioning screw 401 and the train wheel bridge 301; The shaft of anode positioning screw 401 is electrically connected with positive plate 411, is provided with insulation covering 415 between the shaft of anode positioning screw 401 and the non-positive plate, and insulation covering 415 is generally used polytetrafluoroethylmaterial material, and insulation covering 415 can be used to locate positive plate; Be a positive plate 411 below the train wheel bridge 301, be provided with a lamellar spacing 410 therebetween, the height in gap 410 is set by insulating part 414, electrolytic solution can be from the gap 410 flow through; Under a still lamellar spacing 410, then, the below is provided with a negative plate 412; Under the negative plate 412 an or lamellar spacing 410, then, the below is provided with a positive plate 411, by that analogy, repeats no more.
In Fig. 3 B, negative electrode positioning screw 402 is connected to the negative electrode leading-out end by cathode wire 405 conductions, and when train wheel bridge 301 was negative electrode, the installation nut of negative electrode positioning screw 402 directly conducted electricity with train wheel bridge 301 and is connected; The shaft of negative electrode positioning screw 402 is electrically connected with negative plate 412, is provided with insulation covering 415 between the shaft of anode positioning screw 401 and the non-negative plate, and insulation covering 415 can be used to locate negative plate; Be a positive plate 411 below the train wheel bridge 301, be provided with a lamellar spacing 410 therebetween, the height in gap 410 is set by insulating part 414, electrolytic solution can be from the gap 410 flow through; Under a still lamellar spacing 410, then, the below is provided with a negative plate 412; Under the negative plate 412 an or lamellar spacing 410, then, the below is provided with a positive plate 411, by that analogy, repeats no more.
In Fig. 3 C, when lower plate 302 is negative electrode, be provided with insulation spacer 423 between the installation nut of anode positioning screw 401 and the lower plate 302; The shaft of anode positioning screw 401 is electrically connected with positive plate 411, is provided with insulation covering 415 between the shaft of anode positioning screw 401 and the non-positive plate, and insulation covering 415 can be used to locate positive plate; Be a positive plate 411 above the lower plate 302, be provided with a lamellar spacing 410 therebetween, the height in gap 410 is set by insulating part 414, electrolytic solution can be from the gap 410 flow through; On a still lamellar spacing 410, then, the top is provided with a negative plate 412; On the negative plate 412 an or lamellar spacing 410, then, the top is provided with a positive plate 411, by that analogy, repeats no more.
In Fig. 3 D, when lower plate 302 was negative electrode, the installation nut of negative electrode positioning screw 402 directly conducted electricity with lower plate 302 and is connected; The shaft of negative electrode positioning screw 402 is electrically connected with negative plate 412, is provided with insulation covering 415 between the shaft of anode positioning screw 401 and the non-negative plate, and insulation covering 415 can be used to locate negative plate; Be a positive plate 411 above the lower plate 302, be provided with a lamellar spacing 410 therebetween, the height in gap 410 is set by insulating part 414, electrolytic solution can be from the gap 410 flow through; On a still lamellar spacing 410, then, the top is provided with a negative plate 412; On the negative plate 412 an or lamellar spacing 410, then, the top is provided with a positive plate 411, by that analogy, repeats no more.
Simultaneously, shown in Fig. 4 A and Fig. 4 B, the centre of each battery lead plate 108, can be center or the not far place of distance center at each battery lead plate 108, be provided with at least one first pod apertures 501, in general, one first pod apertures 501 can be good at realizing the effect of the electrolytic reaction of reactor of the present invention, certainly, in the practical application, also a plurality of first pod apertures 501 can be set on each battery lead plate, the size of each first pod apertures of each battery lead plate is preferably identical with the position, help like this when stacked,, form first diversion trench 304 of a rule as Fig. 1 or shown in Figure 2.Wherein, the battery lead plate shown in Fig. 4 A is oval, and the battery lead plate shown in Fig. 4 B is circular, and each battery lead plate is fixing stacked by pilot hole 502.Each first pod apertures 501 forms first diversion trench, first diversion trench 304 promptly shown in Figure 2 when each battery lead plate is stacked; And described train wheel bridge and described lower plate are provided with second pod apertures, the 3rd pod apertures that is connected with described first diversion trench respectively; The size of second pod apertures, the 3rd pod apertures and position correspond respectively to the size and the position of first pod apertures, and preferably the size of each pod apertures is all consistent with the position; Certainly, also can be the size and about consistent the getting final product in position of each pod apertures.In general, described first pod apertures is arranged on the center of each battery lead plate of rectangle, ellipse, circle or umbrella shape, and for example, described first pod apertures is arranged on the circular center of circle.For example, in the reactor of the present invention, each positive plate is the flat identical circle of area with each negative plate, gather into folds as a plurality of disks and put together, inter-burst one first diversion trench.At this moment, be more preferably, as mentioned above, described first diversion trench vertically passes through the center of circle of each battery lead plate.
As depicted in figs. 1 and 2, described turning axle 113 is fixedlyed connected with described train wheel bridge 301, connection section is provided with second diversion trench that is connected with described first diversion trench, need to prove, second diversion trench can exist a plurality of, be used to be communicated with the electrolytic solution in the reactor and first diversion trench, flow to the reactor inwall from first diversion trench that roughly is positioned at the reactor center through electrolysis, flow to the circulation of first diversion trench then from the train wheel bridge top through second diversion trench thereby form electrolytic solution.For example, as shown in Figure 1, adopt at least two nonconducting joint pins 315 to link to each other between described turning axle and the described train wheel bridge, be more preferably the joint pin of employing more than three, electrolytic solution can flow through from a plurality of second diversion trenchs between each joint pin; Joint pin can be wholely set with described turning axle 113, described train wheel bridge 301, also can adopt to be spirally connected or other mode of connection are connected with described turning axle, described train wheel bridge 301; As shown in Figure 2, can also adopt at least two fins 406 to fixedly connected between described turning axle and the described train wheel bridge, be more preferably the fin that adopts more than three, electrolytic solution can flow through from a plurality of second diversion trenchs between each fin; Simultaneously, the below of lower plate 302 also can be provided with at least two fins 403, can play water conservancy diversion like this.And described motor is connected with described turning axle, is used to rotate described turning axle; Wherein, described motor can be an adjustable speed motor, and at this moment, described reactor also comprises control module (not indicating among the figure), is used to control the rotating speed of described adjustable speed motor.Control module can utilize prior art to realize very easily, does not give unnecessary details at this.
Reactor of the present invention can also comprise many counter electrode plate, and each counter electrode plate is the identical same shape of flat area, and the area of each counter electrode plate should be identical as far as possible, then should not differ too big if any nuance.The two sides of positive plate can be respectively by the default parallel or approximate stacked abreast negative plate of spacing, and when positive plate was in a certain end of electrode stack, positive plate also can only have one side by default spacing parallel stacked negative plate; Negative plate is as the same, repeats no more.When rectangle, circle or oval-shaped each battery lead plate were stacked, integral body cannot tilt, and each battery lead plate horizontal parallel is stacked.
Another embodiment is, reactor of the present invention comprises two counter electrode plates at least, and the area of each electrode is identical.General, for raising the efficiency, reactor of the present invention comprises many counter electrode plate, for example, 3 pairs, 4 pairs ... more than 20 to, more than 30 to, more than 50 to, more than 100 in addition hundreds of right; The structural state that can bear until existing lead electricity capacity and equipment load-carrying.
In the reactor of the present invention, each battery lead plate of identical polar is parallel-connected to the electrode leads to client of identical polar, and at this moment, described reactor is the acyclic type electrolyzer.Certainly, also can be with each battery lead plate series connection, each battery lead plate has bipolarity, and one side is an anode, and another side is a negative electrode, and described reactor is the multipole type electrolyzer.
At last, the product of reaction is by silk screen 109 enrichments.
And, the present invention also provides a kind of electrolytic reaction method of fluoridizing, and it is applied to comprise the reactor of electrolytic reaction still, at least one pair of battery lead plate, a pair of anodic-cathodic leading-out end, at least one pair of anode and cathode positioning screw, train wheel bridge, lower plate, turning axle, motor, a pair of positive and negative electrode guide ring and at least one pair of brush; Described pair of electrodes plate is a pair of mutually insulated, by default stacked flat identical shaped positive plate and the negative plate of spacing, be respectively arranged with at least one first pod apertures in the middle of each battery lead plate, each first pod apertures forms first diversion trench when each battery lead plate is stacked; Battery lead plate is arranged in the described electrolytic reaction still, and the electrode leads to client by correspondence is connected to outside power supply respectively; Positioning screw is fixed each battery lead plate by the pilot hole of each battery lead plate, and fixedlys connected with described train wheel bridge, described lower plate respectively, and described turning axle is fixedlyed connected with described train wheel bridge, and described motor is used to rotate described turning axle; Described reaction method comprises step: A1, described rotating speed of motor is set; A2, adding reactant; A3, rotating electrode plate carry out electrolytic reaction.
During electrolytic reaction, because the centrifugal force of rotation, electrolytic solution forms from the top of first diversion trench respectively or the below of first diversion trench, first pod apertures, spacing through each battery lead plate arrives in the reactor of each battery lead plate outer successively, returns the circulation of the below of the top of first diversion trench or first diversion trench.
Specifically, the invention provides a kind of electrochemical fluorination and key equipment, this method be with the mode of rotating electrode plate with one basically by AHF (anhydrous hydrogen fluoride) but and the liquid mixture formed of fluorinated organic compounds can make electrolytic solution controlled adjustment between its battery lead plate and forced-flow and can make reactants separate, and the electrolyzing synthesizing method and the equipment of effectively enrichment.Leave the fixed spacing between the plate of this rotating electrode slab reactor, promptly leave runner with one pole, in parallel mode and mutually insulated.Plate be connected and interval insulant to be AHF be that inert conduction and insulating material are made.It must be active to electrochemical fluorination when plate was anode.Wherein, the method for electrolytic solution controlled adjustment and forced-flow is that mode by the rotating electrode sheetpile realizes.The rotating electrode sheetpile is by adjustable speed motor and step-down gear control.
Wherein, the rotating electrode plate in the rotating electrode sheetpile is electrically connected with one pole, mode in parallel.Wherein said reactants separate, and effectively enrichment is that the structure with attached wall silk screen is separated in the container that the rotation fluid-tight is closed, the weight thing during the enrichment electrolytic reaction is synthetic.
The electrolysis reactor of fluoridizing of the present invention is with the rectangle pole plate of " Simons " formula as electrolytic pole board, change horizontal circle disc type pole of rotation plate into, utilize the rotation of horizontal circle disc type pole plate, drive directed flow and the rotation of whole reactor electrolyte inside and the circulation of electrolytic solution between pole plate, because rotation can be controlled, thereby the electrolyte flow speed between pole plate is also controlled, and then the environment and the condition of electrolytic reaction have been changed, the product of reaction is controlled under certain conditions, this equipment will improve the currently available products productive rate, can make the further expansion that kind tool industrial production is worth of fluoridizing that is difficult for production in existing equipment.And this kind structure formation, will change existing domestic electrolyzer can only be to repeat to increase the present situation that improves output.
The novel design of electrolysis cells of fluoridizing of the present invention is in a still type container, cathode-anode plate all is designed to collar plate shape, center delivery hole and pole plate support the electrical isolation clearance hole on the disk, the cathode-anode plate insulation that is overlapping, and it is in aggregates to connect support with the carriage at two ends up and down.The interpolar lead is drawn still type container by the central shaft hole on carriage top, axle is the hollow tubular axle, central shaft and its hardwired electrode stack of institute form a rotatable mechanism in still, can drive central shaft and battery lead plate rotation by deceleration device, the electrode wires of drawing links to each other with the anode and cathode carbon brush of external belt spring by the circular lead ring on the central shaft, carbon brush links to each other with the rectifier positive and negative electrode, makes system's anodic-cathodic form the loop line of an electrolytic synthesis.Such equipment has just been finished basic reaction unit.
When equipment is full of electrolytic solution, also be full of electrolytic solution between pole plate,, can have driven central shaft and pole plate and rotate by the rotation of deceleration device, interpolar electrolytic solution and battery lead plate do relative motion and transport motion like this, and this motion just can make electrolytic solution carry out centrifugal motion and be dished out between battery lead plate.Because still is a round sealed container, electrolytic solution can constantly be circulated between battery lead plate, electrolytic process is constantly carrying out under the effect of electric current, electrolysate after overflowing pole plate along constantly enrichment in the mesh-like structure of still wall device, heavy sinking, light come-up constantly repeats whole process.
A concrete example is, manufactured and designed a board-like electric fluorination reactor of pilot scale rotating electrode by basic design of the present invention, useful volume 146L, and yin, yang pole plate useful area is 26M2.Design current is 1500A.Rotating speed 3-80 rev/min, between stepless time adjustment.After dropping into AHF and octyl group sulfonic acid fluoride, be controlled at 17-19 ℃ at temperature in the kettle, rotating speed 12n-30n/ branch, voltage 5-7V, electric current 500-800A.Produced the goodish full-fluorine octyl sulfuryl fluoride of appearance effect.
By the relative movement and the transport motion of battery lead plate and electrolytic solution, electrolytic solution can be flowed with the speed of a setting at interpolar.Make contacting of electrolytic solution and battery lead plate face, outside atmosphere and condition during change electrolysis that like this can be artificial in controlled continuous conversion down; In the hope of enlarging the range of product and the use range of electrolyzer.That is, the electrolytic solution that organic electrochemistry is fluoridized between electrolytic pole board becomes the pump circulation state by elemental flow state, has changed the outside atmosphere and the condition of electrofluorination process like this, to electrolytic process and the more effective control of product energy thereof; Reaching increase can the organic kind of electric fluorizated, improves electricity and fluoridizes transformation efficiency and product yield.
Specifically, adopt the present invention, make the ionogen in the electrolytic solution more even, be more conducive to guarantee the mixture homogeneity of the reaction raw materials of required electrolysate; Make the each point temperature of electrolytic solution more aligned.Guarantee heat and mass transfer process conditional stability; Improve output and productive rate, reaction product can better be discharged in enrichment.Simultaneously,, need not increase hydraulic pressure, electrolytic solution is flowed between battery lead plate owing to can adjust the combination of each reaction conditions; Both be applicable to synthesis under normal pressure, and be applicable to reaction under high pressure again, so the electrolytic reaction environment is more stable, use range is more extensive, has therefore enlarged the kind of the fluorinated product of electrolytic reaction.
The structure of product of the present invention has solved existing fluoridizes that electrolyzer is difficult does big difficulty, and equipment is fairly simple, and mounting or dismounting are convenient, and the plot ratio height does not have band pressure operation link to AHF, especially when AHF is liquid phase, and the normal pressure operation; Reduce spillage risk, make process environments safer; And multiple operation can be finished in an equipment.Because the change of electrolytic process external conditions can make the range of product that is difficult to suitability for industrialized production in existing electrolyzer, is adopted the present invention to produce.
Should be understood that, for those of ordinary skills, can be improved according to the above description or conversion, and all these improvement and conversion all should belong to the protection domain of claims of the present invention.
Claims (10)
1, a kind ofly fluoridize electrolytic reactor, it comprises electrolytic reaction still, at least one pair of battery lead plate, a pair of anodic-cathodic leading-out end; Described pair of electrodes plate is positive plate and the negative plate that a pair of mutually insulated is provided with, and described battery lead plate is arranged in the described electrolytic reaction still, and the electrode leads to client by correspondence is connected to outside power supply respectively; It is characterized in that described reactor also comprises at least one pair of anode and cathode positioning screw, train wheel bridge, lower plate, turning axle, motor, a pair of positive and negative electrode guide ring and at least one pair of brush;
Described positive plate and described negative plate are flat identical shaped, and each battery lead plate is stacked by default spacing, and the centre is provided with at least one first pod apertures, and each first pod apertures forms first diversion trench when each battery lead plate is stacked;
Each battery lead plate is provided with a pair of anode and cathode pilot hole at least respectively, be used for corresponding described anode and cathode positioning screw, and positioning screw is used for fixing each battery lead plate by pilot hole, and fixedly connected with described train wheel bridge, described lower plate respectively, be used for fixing the position of each battery lead plate; The anode positioning screw is electrically connected with described positive plate by described anode pilot hole, and is electrically connected to the positive electrode leading-out end; The negative electrode positioning screw is connected with described negative plate conduction by described negative electrode pilot hole, and is electrically connected to the negative electrode leading-out end;
Described turning axle is fixedlyed connected with described train wheel bridge, and connection section is provided with second diversion trench that is connected with described first diversion trench, and described motor is connected with described turning axle, is used to rotate described turning axle;
Described train wheel bridge and described lower plate are provided with second pod apertures, the 3rd pod apertures that is connected with described first diversion trench respectively;
The brush of external source is connected with the anodic-cathodic leading-out end by the positive and negative electrode guide ring respectively.
2, reactor according to claim 1 is characterized in that, described reactor also comprises the silk screen layer that is arranged on described reactor inwall, is used for the separation of product.
3, reactor according to claim 1 is characterized in that, described train wheel bridge and/or described lower plate are negative plate, and the battery lead plate adjacent with described train wheel bridge and/or described lower plate is positive plate.
4, reactor according to claim 1 is characterized in that, described reactor comprises two counter electrode plates at least, and the area of each battery lead plate is identical.
5, reactor according to claim 4 is characterized in that, each battery lead plate of identical polar is parallel-connected to the electrode leads to client of identical polar.
6, reactor according to claim 1 is characterized in that, described positive plate is flat identical rectangle, ellipse, circle or the umbrella shape of shape with described negative plate; And described positive plate and described negative plate are rectangle, ellipse or when circular, each battery lead plate is stacked by default spacing horizontal parallel.
7, according to the arbitrary described reactor of claim 1 to 6, it is characterized in that described first pod apertures is arranged on the center of each battery lead plate.
8, reactor according to claim 1 is characterized in that, described reactor comprises at least two pairs of anode and cathode positioning screws, at least two pairs of anode and cathode pilot holes of the corresponding at least respectively setting of each battery lead plate.
9, a kind ofly fluoridize electrolytic reaction method, it is applied to comprise the reactor of electrolytic reaction still, at least one pair of battery lead plate, a pair of anodic-cathodic leading-out end, at least one pair of anode and cathode positioning screw, train wheel bridge, lower plate, turning axle, motor, a pair of positive and negative electrode guide ring and at least one pair of brush; Described pair of electrodes plate is a pair of mutually insulated, by default stacked flat identical shaped positive plate and the negative plate of spacing, be respectively arranged with at least one first pod apertures in the middle of each battery lead plate, each first pod apertures forms first diversion trench when each battery lead plate is stacked; Battery lead plate is arranged in the described electrolytic reaction still, and the electrode leads to client by correspondence is connected to guide ring respectively, by brush and outside power supply formation loop; Positioning screw is fixed each battery lead plate by the pilot hole of each battery lead plate, and fixedlys connected with described train wheel bridge, described lower plate respectively, and described turning axle is fixedlyed connected with described train wheel bridge, and described motor is used to rotate described turning axle; Described reaction method comprises step:
A1, described rotating speed of motor is set;
A2, adding reactant;
A3, rotating electrode plate carry out electrolytic reaction, and wherein, electrolytic solution forms respectively from first diversion trench, and first pod apertures, the spacing through each battery lead plate arrives in the reactor of each battery lead plate outer successively, returns the circulation of first diversion trench.
10, reaction method according to claim 9 is characterized in that, steps A 1 is further comprising the steps of: according to the proportion of reactant or product, the spacing of each battery lead plate is set.
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| CN200710076607A CN100577882C (en) | 2007-08-27 | 2007-08-27 | Fluoelectrolysis reactor and reaction method |
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| CN112376075B (en) * | 2020-10-08 | 2022-08-26 | 中船(邯郸)派瑞特种气体股份有限公司 | Electrochemical fluorination external circulation flexible electrolysis system |
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