US3928164A

US3928164A - Alternating current electrolytic cell

Info

Publication number: US3928164A
Application number: US423913A
Authority: US
Inventors: Jr John C Shepard; Robert C Wight; Phillip W Kosted
Original assignee: Nalco Chemical Co
Current assignee: ChampionX LLC
Priority date: 1973-12-12
Filing date: 1973-12-12
Publication date: 1975-12-23
Anticipated expiration: 1992-12-23

Abstract

Electrolytic cell operable by alternating current for producing organometallic compounds electrolyzing a liquid electrolyte in the presence of a particulate consumable metal, wherein the cell includes a tubular metal vessel having a main shell, a top closure member mounted at the upper end of the shell and electrically insulated therefrom, a bottom closure member mounted at the lower end of the shell and electrically insulated therefrom, a tubular liquid permeable spacer of insulating material in the main shell containing therein a particulate consumable electrically conductive material and defining one electrode and a second electrode defined by particulate consumable electrically conductive material surrounding the spacer and in contact with the main shell.

Description

[ Dec. 23, 1975 ALTERNATING CURRENT ELECTROLYTIC CELL [75] Inventors: John C. Shepard, Jr., Lake Jackson;

Robert C. Wight, Sugar Land; Phillip W. Kosted, Rusk, all of Tex.

[73] Assignee: Nalco Chemical Company, Chicago,

Ill.

[22] Filed: Dec. 12, 1973 [21] Appl. No.: 423,913

[52] US. Cl. 204/260; 204/59 L; 204/59 QM; 204/283 [51] Int. Cl. C25B 9/00 [58] Field of Search 204/59 L, 59 QM, 260, 263, 204/283 [56] References Cited UNITED STATES PATENTS 3,287,248 ll/l966 Braithwaite 204/260 3,573,178 3/1971 Blackmar 3,630,858 l2/l971 Ganci et al. 204/59 QM FOREIGN PATENTS OR APPLICATIONS 1,194,181 6/1970 United Kingdom 204/260 Primary Examiner.lohn H. Mack Assistant Examiner-W. l. Solomon Attorney, Agent, or FirmLockwood, Dewey, Zickert & Alex [57] ABSTRACT Electrolytic cell operable by alternating current for producing organometallic compounds electrolyzing a liquid electrolyte in the presence of a particulate consumable metal, wherein the cell includes a tubular metal vessel having a main shell, a top closure member mounted at the upper end of the shell and,electrically insulated therefrom, a bottom closure member mounted at the lower end of the shell and electrically insulated therefrom, a tubular liquid permeable spacer of insulating material in the main shell containing therein a particulate consumable electrically conductive material and defining one electrode and a second electrode defined by particulate consumable electrically conductive material surrounding the spacer and in contact with the main shell.

11 Claims, 5 Drawing Figures 5 E I/ t I III/Ill US. Patent Dec. 23, 1975 Sheet 1 of2 3,928,164

FIGJ

ALTERNATING CURRENT ELECTROLYTIC CELL This invention relates in general to an electrolytic cell for producing organometallic compounds from an electrolyte and a consumable metal,'and more particularly to an alternating current"operating electrolytic cell for producing alkyl lead compounds from a Grignard reagent and lead.

The present invention is particularly concerned with a new and improved electrolytic cell for manufacturing alkyl lead compounds, suchas tetramethyl lead, tetraethyl lead, and the like, by the electrolysis of Grignard reagents in the'presence of sacrificial metal electrodes. Usually, the electrode would consist of lead particles, such as lead shot or beebees. whichcan be easily added to a cell during operation as the lead particles are consumed by the electrolytic process.

The production of organometallic compounds by the electrolysis ofGrignard reagents'in the presence of lead shot is well known, as set forth in several US. Pats., including the following U.Sv Pats. Nos:

3,497,428 and It has also been known to provide an alternating current electrolytic cell, as set forth in US. Pat. No. 3,630,858.

The heretofore known direct current electrolytic cells involve the expense of rectifying the usually available alternating current or the direct production of direct current by meansof a direct current generator, either of which adds to the production expenses. It is also known that direct current electrolytic cells frequently short out during lowv alkyl chloride or active Grignard concentrations, thereby requiring shutdown which interrupts continuous operation and necessitates dismantling and reconditioning of the cell.

The alternating current electrolytic cell of the invention utilizes a readily available lower cost alternating current, thereby eliminating rectification problems and expense. Moreover, it has been found that alternating current cells do not short out at low alkyl chloride levels and very low active Grignard concentrations, thereby enhancing continuous operation to provide better overall production. I

The cell of the present invention generally includes a closed vessel of electrically conductive material, such as steel, composed of a main cell and upper and lower closure members. Within the main shell a liquid porous tubular spacer or membrane of insulating material separates the two electrodes of the cell, wherein the electrodes preferably consist of a mass of lead shot. Accordingly, the interior of the tubular spacer is filled with lead shot, while the space between the spacer and the main shell is also filled with lead shot. The spacer is porous and defines an electrolyte path, wherein the application of alternating current to the electrodes functions to electrolyze the elecctrolyte being passed through the cell in the presence of the lead shot to produce an organometallic compound which is recovered from the cell. The tubular spacer preferably includes a hair-curler core of suitable electrically insulating material, such as polypropylene, covered on both sides by a non-conductive fabric, such as nylon or fiberglass mesh.'Accordingly, the spacer electrically insulates one electrode from the other and additionally provides an electrolytic path through which the electrolyte passes as it moves through the cell. It should be appreciated that any number of spacers should be provided in the main shell of the cell to define any number of columns of lead shot within the cell, all of which are electrically connected together, wherein one of the electrodes may be defined by the plurality of columns of lead shot arranged in a cell and where the other electrode inthe form of a column of lead shot essentially surrounds all of the tubular columns of shot.

The alternating current employed is preferably of low frequency on the order of no more than Hz. or within the range of 5 to 60 Hz. and preferably within the range of 5 to 30 Hz. The voltage may vary between 1 and 60, although it is preferred that the voltage be within" the range of 20 to 30. The amperage of the potential depends upon the size of the cell. Preferably, the electrolysis is conducted at temperatures within the range of 50 to 60C. in the production of organolead compounds, although it may be increased or decreased so long at the temperature is less than the boiling point of the electrolyte.

It is therefore an object of the present invention to provide a new and improved alternating current electrolytic cell for producing organometallic compounds, wherein the elimination of current rectification and the use of the more readily available economical current is achieved.

Another object of this invention is in the provision of an alternating current electrolytic cell which will not short at low alkyl chloride levels or at very low active Grignard concentrations.

Another object of this invention is in the provision of an alternating current electrolytic cell which enhances continuous operation and therefore increases production in the making of organometallic compounds.

Other objects, features and advantages of the invention will be apparent from the following detailed disclosure, taken in conjunction with the accompanying sheets of drawings, wherein like reference numerals refer to like parts, in which:

FIG. 1 is a vertical sectional view taken through one form of an alternating current electrolytic cell according to the invention and broken for purposes of clarity;

FIG. 2 is a transverse cross-sectional view taken along the line 22 of FIG. 1;

FIG. 3 is a vertical sectional view partially broken of a modified alternating current electrolytic cell according to the invention;

FIG. 4 is a transverse sectional view taken substantially along the line 44 of FIG. 3; and

FIG. 5 is a transverse sectional view taken along the line 5-5 of FIG. 3.

In general, the cell structures according to the present invention include a main shell, upper and lower closure members secured to the upper and lower ends of the main shell, and a pair of electrodes within the main shell formed of particulate metal, such as lead shot, wherein one of the electrodes is formed by one or more columns of lead shot separated from the other electrode by a hair-curler insulator which generally provides the path for electrolyte flow through the cell. Alternating current, preferably of a low frequency, on

the order of 60 or less H7.., is supplied to the electrodes at a voltage preferably within the range of 20 to 30 volts. wherein electrolysis of a substantially anhydrous solution of a Grignard reagent in the presence of a sacrificial metal electrode produces the desired organometallic compound. The type of compounds produced, as well as the ingredients utilized. are referred to in the heretofore mentioned prior art patents.

Referring now to the drawings, the alternating current electrolytic cell illustrated in FIGS. 1 and 2 includes generally a main shell 10, an upper closure member 11 and a lower closure member 12. The upper and lower closure members are suitably connected to the main shell and insulated therefrom.

The main shell includes a cylindrical body 13 having a radial flange 14 at the upper end and a radial flange 15 at the lower end. The upper closure member 11 includes a cylindrical body portion 16 of a smaller diameter than the main shell body 13 but axially aligned therewith and a dome-shaped cover 17. The lower closure member includes a cylindrical body portion 18 of a size diametrically smaller than the main body shell 13 and a cover member 19.

The lower end of the upper closure member cylindrical body portion 16 includes a radial flange 20, while the upper end includes a radial flange 21. An insulating gasket 22 between the flanges of the main shell and the upper closure member electrically insulates the upper closure member from the main shell. The gasket 22 may be of any suitable electrically insulated material, such as polypropylene. Suitable fasteners 23 are provided for securing the flange of the upper closure member cylindrical body 16 to the main shell body 13.

Within the main shell,

electrodes

26 and 27 formed of particulate metal, such as lead shot, are separated from each other by a tubular insulating spacer or membrane 28. The spacer or membrane 28 includes a haircurler core 29 of electrically insulating material, such as polypropylene, of relatively large open mesh somewhat rigid lattice-work to facilitate electrolyte flow, and a fabric mesh inner layer 30 and outer layer 31 of 60 to 80 mesh, and preferably double 80 mesh. The fabric mesh is of a suitable electrically insulating material, suchas nylon, fiberglass, or the like, and of a mesh that will not permit the passage of the lead shot therethrough. Accordingly, the spacer or membrane 28 electrically insulates between the

electrodes

26 and 27 and also provides a path for electrolyte flow through the cell. While electrolyte may move through the lead shot, it will generally take the path of least resistance which will be along the membrane.

The main shell, together with the upper and lower closure members, is preferably made of a suitable metal, such as steel, which can readily withstand the weight of the lead shot and the electrolyte during the operation of the cell, and which is electrically conductive.

The membrane 28 is supported at its upper end by the upper closure member 11, wherein a stubend 34 of a suitable electrically insulating material and a stubend 35 of steel coact to grip the upper end ofthe membrane and are held in place by the connection of the cover 17 to the cylindrical body 16. The stubends include a flange portion and a cylindrical portion. The cylindrical portion of the steel stubend 35 is tapered and sized so that when it coacts with the plastic stubend 34 that also may be tapered, it tightly squeezes and grips the upper end of the membrane to support it at the upper closure member. The flange portions of the stubends are stacked and sandwiched between the upper flange 21 of the cylindrical body 16 and a lower flange 36 of the cover member 17. Suitable fasteners are provided to secure the flange of the cover member to the flange of the cylindrical body and to tightly hold the flange portions of the stubends in place. An opening 37 is provided in the cover member 17 for effluent flow from the cell. A flange 38 is provided about the opening for the purpose of assisting in attaching the cover member to other plumbing. Accordingly, the opening 37 will function as the outlet where the flow of electrolyte moves upwardly through the cell. The opening 37 also functions to permit the addition of lead shot to the electrode 26 it is consumed. It should also be appreciated that the cover member 17 of the upper closure is electrically insulated from the cylindrical body 16 by the stubend 34.

The lower end of the membrane 28 is supported by a stubend 41 and a bushing 42 which as an assembly is supported between the main shell and the lower closure member. Both the stubend 41 and the bushing 42 are of an electrically insulating material, such as polypropylene, whereby the lower closure member 12 is insulated from the main shell 10. The external face of the bushing 42 and the internal face of the cylindrical portion of the stubend 41 are complementarily tapered so that when the bushing is assembled with the stubend and the lower end of the membrane is in place, the lower end of the membrane is wedged or gripped by the assembly to hold it in place. The flange portion of the stubend 41 is held between the lower flange 15 of the main shell cylindrical body 13 and an upper flange 43 of the lower closure member cylindrical body portion 18. Suitable fasteners are provided to lock the flanges together and provide a sealed assembly.

The lower end of the cylindrical body portion 18 includes a radial flange 44 for attaching thereto the cover member 19. The cover member 19 includes a cylindrical portion 45 of a diametrical dimension substantially smaller than the diametrical dimension of the cylindrical body portion 18 and defining an opening 46 at the lower end of the cell. An upper flange 47 is formed on the cover member 19 for attaching the cover member 19 to the flange 44 of the body section 18. A lower flange 48 is provided for attaching the cover member to other plumbing in the system. Where the flow of electrolyte is upwardly through the cell, the opening 46 then functions as the inlet to the cell.

The electrode 26 is in the form of a column of lead shot which extends through the center of the membrane 28 and is supported at its lower end by the lower closure member cover member 19 as it extends through the lower assembly which holds the lower end of the membrane in place. In order to prevent the lead shot from falling through the opening 46, a suitable screen, preferably of metal and designated by the numeral 49, is mounted at the opening and coplanar with the flange 47. Accordingly, the mesh of the screen is such that it will not permit the lead shot to pass therethrough but will readily permit the flow ofelectrolytc therethrough. The electrode 27 is in the form of an annular column of lead shot and supported between the membrane 28 and the inner surface of the main shell body 13 and is supported at its lower end by the stubend 41.

As already mentioned, additional lead may be added to the electrode 26 through the upper opening 37, while .a fitting 50 is provided in the upper closure memher cylindrical body 16 to facilitate. the addition of lead to the electrode 27. A lead dumping valve is provided at the lower end of the main shell body 13 for dumping lead from the electrode 27 when dismantling the cell.

Alternating current potential is supplied to the

electrodes

26 and 27 of the cell by respective connections to the lower closure member 18 and to the main shell, as illustrated by the

conductors

53 and 54.

Another embodiment of the invention, as shown in FIGS. 3 to 5, differs from the embodiment of FIGS. 1 and 2 primarily in that one of the electrodes is defined by a plurality of columns of particulate metal by the use of a plurality of membranes which generally increase the capacity of the cell. This embodiment includes generally a main shell 60, an upper closure member 61 and a lower closure member 62.

The main shell 60 includes a cylindrical body portion 63, an upper plate flange 64 and a lower plate flange 65 suitably welded to the cylindrical body 63. The upper plate flange 64 is provided with six holes for receiving stubends 66 which support the upper end of membranes 67. The membranes 67 are constructed like the membrane 28 in the embodiment of FIGS. 1 and 2 in that they include a polypropylene hair-curler core with double 80 mesh nylon sock on the inside and a double 80 mesh nylon sock on the outside. The upper end of each membrane 67 is fastened to the stubend 66 by means of a nylon band 68. Since the stubends are flanged, they are supported on the plate flange 64.

The lower ends of the membranes 67 are fastened to the lower plate flange 65 which is provided with six openings by means of an assembly including a stubend 70 and a retaining ring or bushing 71. Both the stubend 70 and the bushing 71 are preferably made of polypropylene to completely electrically insulate the membranes from the lower plate flange 65. The coacting surfaces of the stubends 70 and the bushings 71 are formed so that when they are assembled they will wedge and/or grip the lower ends of the membranes 67 and hold them in place. The holes in the upper and lower plate flanges which serve to be aligned with the membranes 67 are equally spaced apart within the main shell body 63 so as to facilitate substantially uniform interaction between the electrolyte and the lead shot which flows through the cell.

The lower closure member 62 includes a relatively dome-shaped portion 73 in inverted position and having a plate flange 74 suitably secured to its large open end and in alignment with the plate flange 65. The plate flange 74 includes a plurality of openings which align with the openings in the flange 65 of the main shell to provide intercommunication between the interior portions of the tubular membranes 67 and the bottom closure member. A gasket 75 of suitable electrically insulating material, such as polypropylene, is arranged between the

plate flanges

65 and 74 to electrically insulate the lower closure member from the main shell. Suitable fasteners are provided for the flanges in order to hold them together and to effect a liquid tight seal between the main shell and the lower closure member. An opening is provided in the dome-shaped portion 73 in the bottom and connected to a pipe 76 which terminates in a flange 77. The pipe 76 is connected to a T fitting 78 having a pipe outlet 79 which can function as the outlet for effluent from the cell.

Two electrodes are defined, one ofwhich is identified by the numeral 82 and consists of a plurality of columns of lead shot extending within the tubular membranes 67 and through the

plate flanges

65 and 74 and supported by the lower closure member 62. The other electrode is identified by the numeral 83, which is in the form of lead shot that is supported within the cylindrical body 63 of the main shell and around the tubular membranes 67. This electrode is supported on the lower plate flange 65 of the main shell and electrically isolated from the electrode 82. In order to prevent the lead shot from passing through the pipe 76 in the lower closure member, a screen member 84 is supported within the pipe and also between the flanges of the pipe and the T fitting 78; the screen member is preferably of 16 mesh stainless steel screen over 4 mesh stainless steel screen.

The upper closure member includes a plate flange 87 having holes formed therein which correspond to the holes aligned with the membranes 67. The plate flange 87 is suitably secured, such as by welding or the like, to a dome-shaped cover member 88 which is provided at its upper end with an inlet pipe 89 having an opening 90 and a lead inlet pipe 91. Both electrolyte and additional lead shot can be supplied to the cell through the inlet opening 90. Thelead shot feeding to the electrode 82, which is composed of the columns of lead shot supported by the tubular membranes 67,is electrically insulated from the electrode 83. An electrically insulating gasket 92 of suitable material, such as polypropylene, is provided between the

plate flanges

64 and 87 to electrically insulate the upper closure member from the main shell. Suitable fasteners are provided for the plate flanges in order to securely fasten the upper closure member to the main shell and also to seal at the plate flanges. The stubends 66 electrically insulate the columns of lead shot for the electrode 82 from the main shell.

In order to add lead shot to the electrode 83, the lead inlet pipe 91 forms a support for a stubend 94 of polypropylene, which is held in place on the flanged end of the pipe 91 by means of a flanged fitting 95. A tube or pipe 96 is telescopically press-fitted onto the sleeve portion of the stubend 94 and extends down through an opening in the plate flange 87 and aligns with an opening in the plate flange 64 so as to provide a supply inlet for make-up lead to the electrode 83. The tube 96 is preferably made of metal but coated with an electrically insulating material, such as an epoxy, in order to electrically insulate the lead in the upper closure member being supplied to the electrode 82 from the lead shot of the electrode 83. Accordingly, make-up lead for the

electrodes

82 and 83 is supplied respectively through the inlet and the inlet fitting 95. As already mentioned, the Grignard reagent is supplied through the inlet 90 and exits through the outlet 79 after being electrolyzed in the cell. A lead dump nozzle and valve assembly 98 is provided at the main shell for dismantling the cell.

The main shell and the upper and lower closure members are made from electrically conductive material, preferably of steel. Inasmuch as the electrode 82 which consists of a plurality of columns of lead shot contained within the membranes 67 is effectively supported by the lower closure member dome-shaped body 73, one electrical conductor 100 connected to the dome-shaped body 73 serves to connect the electrode 82 to an electrical potential. Similarly, a conductor 101 connected to the main shell body 63 serves to connect the electrode 83 to the electrical potential.

In operation of the embodiment of FIGS. 3 to 5, the electrical contacts or

conductors

100 and 101 are connected to a source of alternating current, and a Grignard reagent dissolved in an appropriate solvent is added the lower end of the main shell, means electrically insulating said top and bottom closure members from the main shell, at least one tubular perforate electrode insulating spacer extending through the main shell,

to the cell through the inlet90. As the Grignard reagent 5 means supporting said spacer at the opposite ends passes through the cell, it is electrolyzed in the presthereof and electrically insulating same from said main ence of the lead shot to produce the desired organomeshell and from the closure members, a particulate contallic compound. To illustrate the invention, the followsumable electrically conductive material in said tubular ing example is presented. The cell was of the type spacer defining one electrode and being supported by shown in FIGS. 1 and 2 and completed 530 hours of and in contact with the bottom closure member, a operation electrolyzing cell effluent at active Grignard particulate consumable electrically conductive matelevels below 0.05 moles (0.035 average). The cell, rial surrounding said tubular spacer and in contact with which showed signs of plugging after 190 hours of operthe main shell defining a second electrode, first openation, was washed once with THF (tetrahydrofuran) to ing means in said upper closure member for permitting remove an etherate buildup. After 500 hours the cell the addition of particulate material to said first elecagain developed signs of plugging. A THF wash did not trode, second opening means in said upper closure solve the problem this time and the cell was then dismember for permitting the addition of particulate mamantled. The lead in the center bed was found to be terial to said second electrode, means supporting and electrolyzed" together. The average feed rate for the electrically insulating the lower end of the second eleccell was 22 pounds of lead per hour. The feed to the trode from the bottom closure member, means concell was obtained from a direct current cell at an avermeeting said first and second electrodes to a source of age active Grignard of0.18 moles. Methyl chloride was alternating current potential, and openings in said top added either batchwise to the cell or as an excess and bottom closure members for permittingaGrignard methyl chloride from the direct current cell. Sixty Hz. reagent solution to flow through the vessel to be eleccurrent was applied to the cell at an average of 24.5 25 trolyzed and thereby produce an organometallic comvolts and 127 amps, both root mean squared values. pound. The results of operation are presented below in Table I. 2. An electrolytic cell as defined in claim 1, wherein said tubular perforate electrode insulating spacer in- TABLE 1 Active Lb Grignard Amp OH Current KWHrs/ Amps/ Amps/ Run Hours Feed In Out Volts Amps Hrs Yield Eff Lb Pb F1 Volt Ft No.1 70 2683 0.12 0.05 27.5 129 9,042 114% 90% 7.19 13.7 0.50 No.2 68.5 1391 0.12 0.02 25.2 125 8,298 139% 74% 8.06 13.3 0.53 No.3 54 1021 0.12 0.01 27.3 110 5.930 68% 16.2 11.7 0.43 No.4 70 1102 0.27 0.04 25.3 137 9.603 73% 46% 13.06 14.6 0.58 No.5 70 1229 0.28 0.03 24.0 133 9.336 61% 48% 11.9 14.1 0.59 No.6 70 1256 0.23 0.04 21.4 132 9,226 88% 63% 7.26 14.0 0.65 No.7 76 1770 0.19 0.04 22.8 124 9,413 84% 63% 8.58 13.2 0.58 No.8 52 1095 019 0.03 22.7 122 6.360 92% 71% 7.55 13.0 0.57

Cell Washed with THF hetwecn runs "Openning temperature raised from 137 to 157 F. for remaining runs The average OH yield was 94 percent, while the cludesatubular large open mesh hair-curler member of current efficiencies averaged 66 percent, which is subrelatively inflexible rigid material through which the stantially lower than that of a direct current cell. When particulate material could pass, the rigidity of the hairthe cell was dismantled, the outer lead bed was freecurler member being such that the shape thereofwill be flowing and the shot was very clean. Approximately, substantially undisturbed by the pressure of the particthe top 6 feet of the center lead bed was fused together. ulate material, an outer layer of fine mesh nylon sock, The average operating temperature for runs 1 to 5 was and an inner layer offine mesh nylon sock, the mesh of 137F., while the temperature for runs 6 to 8 was the socks being such that the particulate material will 157F. not pass therethrough.

it has therefore been demonstrated that the alternat- 3. An electrolytic cell as defined in claim 2, wherein ing current cell of the invention can electrolyze effluent said hair-curler member is of electrical insulating matehaving low active concentrations of Grignard without rial. shorting out. Further, electrolysis is produced with 4. An electrolytic cell as defined in claim 3, wherein inexpensive and available alternating current. said nylon socks are about to 80 mesh, and said It will be understood that modifications and variahair-curler member is of polypropylene. tions may be effected without departing from the scope 5. An electrolytic cell as defined in claim 3, wherein of the novel concepts of the present invention. but it is 60 said nylon socks are double 80 mesh, and said hairunderstood that this application is to be limited only by curler member is of polypropylene. the scope of the appended claims. 6. An electrolytic cell as defined in claim 1, wherein The invention is hereby claimed follows: a plurality of perforate electrode insulating spacers are 1. An electrolytic cell for producing organometallic mounted within said main shell defining a plurality of electrodes all of which are in common electrical compounds comprising, a substantially tubular upstanding metal vessel including a central main shell, a top closure member mounted at the upper end of the main shell, and a bottom closure member mounted at contact.

7. An electrolytic cell for producing organometallic compounds comprising, a substantially upstanding cylindrical metal vessel including a central cylindrical main shell, a top closure member mounted on the upper end of the main shell, and a bottom closure member mounted on the lower end of the main shell, means electrically insulating said top and bottom closure members from the main shell, a tubular perforate member means of insulating material supported at the upper and lower ends thereof in the main shell and insulated therefrom and from the closure members, said tubular member means defining a first chamber within said member means and a second chamber outside said member means with said main shell, a bottom wall on said main shell separating the main shell from the bottom closure member and defining therewith a lower chamber in the bottom closure member, an opening in the bottom wall intercommunicating the first chamber and the lower chamber, a first electrode in the form of lead shot within said first chamber and said lower chamber, a second electrode in the form of lead shot within said second chamber, first opening means in said upper closure member communicating with said first chamber for permitting the addition of lead shot to the first electrode, second opening means in said upper closure member communicating with said second chamber for permitting the addition of lead shot to the second electrode, means connecting said first and second electrodes to a source of alternating 10 current potential, and ports in said top and bottom closure members for permitting a Grignard reagent solution to flow through the vessel to be electrolyzed and thereby produce an organometallic compound.

8. An electrolytic cell as defined in claim 7, wherein said tubular perforate member means includes a tubular large open mesh hair-curler member of relatively inflexible rigid material through which particulate material could pass, the rigidity of the hair-curler member being such that the shape thereof will be substantially undisturbed by the pressure of the particulate material, an outer fine mesh nylon sock, and an inner fine mesh nylon sock, the mesh of the socks being such that the particulate material will not pass therethrough.

9. An electrolytic cell as defined in claim 8, wherein said hair-curler member is of electrical insulating material.

10. An electrolytic cell as defined in claim 9, wherein said nylon socks are double mesh, and said haircurler member is of polypropylene II. An electrolytic cell as defined in claim 7, wherein said tubular member means includes a plurality of perforate electrode insulating spacers mounted within said main shell defining a plurality of electrodes all of which are in common electrical contact through the lead shot in the lower chamber.

Claims

1. AN ELECTROLYTIC CELL FOR PRODUCING ORGAOMETALLIC COMPOUNDS COMPRISING, A SUBSTANTIALLY TUBULAR UPSTANDING METAL VESSEL INCLUDING A CENTRAL MAIN SHELL, A TOP CLOSURE MEMBER MOUNTED AT THE UPPER END OF THE MAIN SHELL, AND A BOTTOM CLOSURE MEMBER MOUNTED AT THE LOWER END OF THE MAIN SHELL, MEANS ELCTRICALLY INSULATING SAID TOP AND BOTTOM CLOSURE MEMBERS FROM THE MAIN SHELL, AT LEAST ONE TUBULAR PERFORATE ELECTRODE INSULATING SPACER AT THE OPPOSITE ENDS THEREOF AND MEANS SUPPORTING SAID SPACER AT THE OPPOSITE ENDS THEREOF AND ELECTRICALLY INSULATING SAME FROM SAID SHELL AND FROM THE CLOSURE MEMBERS, A PARTICULATE CONSUMABLE ELECTRICALLY CONDUCTIVE MATERIAL IN SAID TUBULAR SPACER DEFINING ONE ELECTRODE AND BEING SUPPORTED BY AND IN CONTACT WITH THE BOTTOM CLOSURE MEMBER, A PARTICULATE CONSUMABLE ELECTRICALLY CONDUCTIVE

2. An electrolytic cell as defined in claim 1, wherein said tubular perforate electrode insulating spacer includes a tubular larGe open mesh hair-curler member of relatively inflexible rigid material through which the particulate material could pass, the rigidity of the hair-curler member being such that the shape thereof will be substantially undisturbed by the pressure of the particulate material, an outer layer of fine mesh nylon sock, and an inner layer of fine mesh nylon sock, the mesh of the socks being such that the particulate material will not pass therethrough.

3. An electrolytic cell as defined in claim 2, wherein said hair-curler member is of electrical insulating material.

4. An electrolytic cell as defined in claim 3, wherein said nylon socks are about 60 to 80 mesh, and said hair-curler member is of polypropylene.

5. An electrolytic cell as defined in claim 3, wherein said nylon socks are double 80 mesh, and said hair-curler member is of polypropylene.

6. An electrolytic cell as defined in claim 1, wherein a plurality of perforate electrode insulating spacers are mounted within said main shell defining a plurality of electrodes all of which are in common electrical contact.

7. An electrolytic cell for producing organometallic compounds comprising, a substantially upstanding cylindrical metal vessel including a central cylindrical main shell, a top closure member mounted on the upper end of the main shell, and a bottom closure member mounted on the lower end of the main shell, means electrically insulating said top and bottom closure members from the main shell, a tubular perforate member means of insulating material supported at the upper and lower ends thereof in the main shell and insulated therefrom and from the closure members, said tubular member means defining a first chamber within said member means and a second chamber outside said member means with said main shell, a bottom wall on said main shell separating the main shell from the bottom closure member and defining therewith a lower chamber in the bottom closure member, an opening in the bottom wall intercommunicating the first chamber and the lower chamber, a first electrode in the form of lead shot within said first chamber and said lower chamber, a second electrode in the form of lead shot within said second chamber, first opening means in said upper closure member communicating with said first chamber for permitting the addition of lead shot to the first electrode, second opening means in said upper closure member communicating with said second chamber for permitting the addition of lead shot to the second electrode, means connecting said first and second electrodes to a source of alternating current potential, and ports in said top and bottom closure members for permitting a Grignard reagent solution to flow through the vessel to be electrolyzed and thereby produce an organometallic compound.

10. An electrolytic cell as defined in claim 9, wherein said nylon socks are double 80 mesh, and said hair-curler member is of polypropylene.

11. An electrolytic cell as defined in claim 7, wherein said tubular member means includes a plurality of perforate electrode insulating spacers mounted within said main shell defining a plurality of electrodes all of which are in common electrical contact through the lead shot in the lower chamber.