US1590609A - Electrolytic apparatus - Google Patents

Description

June 29 1926.

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Patented June 29, 1926.

UNITED STATES PATENT OFFICE.

EDWIN TAYLOR AND EDWARD F. CHANDLER, F BROOKLYN, NEW YORK, ABBIGNORS i TO TAYLOR LABORATORIES INC;l A CORPORATION 0l' NEW YORK.

ELECTBOLYTIO APPARATUS.

Original application Med December 8, 1918, Serial lo. 941,953. Divided and this application 111ml Inl-ch 10, 1926. Serial No. 85,914. i

This invention elates to improvements in electrolytic a pa atus and this application is a division o our prior application Ser. No. 341,953 tiled December 2, 1919. In our l prior oo-pending application for United States Letters Patent, Ser. No. 314,102, filed July 29, 1919, we have described a process wherein organic material such as cellulose in a fibrous or cellular condition may be l0 converted by dissolving the cellulose 1n a suitable solvent, such as `cupro-ammonia solution and electrolyzin the solution between a suitable anode an cathode whereby cellulose substantiallyl free of the solvent chemicals is deposited on the y anode and the copper is de osited on the cathode and v thence to a suitable drying system for the -ammoma is fr L The main object of the present invention `is-to provide improvements whereby such or nic matter may be so treated more expeditlously and in amore economical and useful manner. Further and more s ecific obects, features and advantages wi l more clearly appear from the detail description given below. In the preferred method of practicing the inventive idea the organic or cellulose material to be converted is dissolved preferably in an excess of cupro-ammonia solution, filtered to remove extraneous impurities, the solution concentrated by the partial removal of ammonia and water (as for instance bymeans of a vacuum), the resultin homogeneous Huid flowed on a carrienw ich may be a ilexible'band of metal suitable for employmentn as one` of the elements of an electrolytic cell, the said carrier being adapted c to convey the flowed material through preferabl a dry and inert gas, thereby excluding eleterious atmospheric contamination.

4 rIhe carrier conveying the flowed material fnow enters and becomes preferably one of f the elements or electrodes in a bath -which y may be provided with another element 01" electrode so as to constitute an electrolytic cell upon the energization of the said elements and through which the carrier which ma be the,anode,' is" adapted to continu ousy convey the 4flowed material. `Owing tothe electrolytic characteristics of cellulose 5 in colloidal state the flowed material as `1t vpasses througlitlle influence ofthe said iieldf'or fields is converted" from.'

' or recovering 4tion from the conveyor or carrier.

vencion as applied to t the colloidal solution to a solid or more dense state-which transformation should be completed under 'proper conditions of 'time and current density before the carrier and material leaves the cell. During the period of transformation the volatile constituent is released from the mass'and is in a condition to be'conveyed to a, suitable condensing stem, the metallic constituent being deposited on the cathode in recoverable condition. The transformed or anic material free of all traces of any ingre ient that mi ht cause future deterioration is referably gonveyed throu h 4a suitable was ing system where any a ering or extraneous traces of forei materials are removed and removal of any moisture content after which the converted material is ready for sepTalis separation may be effected by means of a V-islgiaped fixed edge supplemented by two ro The material, now in a transparent Hexible band resemblincelluloid in appearance is then led throu a bath containing a volatile solvent suc as amyl-acetate which possesses a slight solvent or softening effect on the cellulose and materially aids in increasing its surface lustre, its density, and its resistance to moisture. The material still wet with solvent is now paed through warm calender rolls whereon it is surfaced,

brought to exact thickness and dried and the solvent recovered. From the calenders the finished product may be wound on reels, cut or trimmed in sheets or strips or otherwise dis of. a

It wil be seen that this process is economical, as well as continuous. All the solvent materials are recovered in usable form for re-solution even the trimmings from the finished material being returned to the solution tanks. The power factor is low and the amount of labor required is almost negligible. It is evident that the above process' can be advantageously carrierout y the use of a concentrated zinc chloride solution, etc.,`in place of the capro-ammonia.

In the accompanlying drawings we have illustrated a suitab e application of our ine manufacturing of photographic films. In said drawings, Fig. 1 illustrates in vertical cross-section, parts being' broken away, the arrangement of a suitable lplant for manufacturing hotographic lms, and Fig. 2 is van en arged cross-sectional detail of the endless belt and film formed thereon.

3-4 indicates suitable tanks carrying concentrated solution of cupro-ammonia or concentrated solution of zinc chloride both being good solvents for cotton which ma be used in the manufacturing of the film. A ut one pound of cotton may be used to about twenty pounds of the solution and suitable means such as the valve 5 may be provided for regulating the fiow of the material upon the endless belt 6 which passes entirely through the closed tray or chamber 7 as shown.

The belt may be made of copier and may be plated with other metal an bufed and may be suitably perforated as indicated at 8 in Fi 2 to receive the teeth of sprocket wheels for driving the same, suitable means for driving the belt being provided such as 9, an electric motor connected to the driving shaft 10. Upon the' belt maybe provide suitable stri sof material such as11 between which the owing material from the tanks 3-4 is deposited. In the drawing I have illustrated the belt as traveling from left to ri ht looking at Fig. 1.

he ammonia from the closed tray 7 is drawn through the outlet dpiple 12 by the suction fan 13 and is passe t rough the drying chamber 14 provided with suitable grids 15 upon which lime or other suitable material 15' may be piled, the dry ammonia returning through the pipe 16 into the closed tray 7 as shown. This provides a constant circulation of dry ammonia gas in the closed chamber 7 and prevents waste of-I material x and contamination from theloutside.

17 indicates an electrol ic'cell to be hereafter more full referre to and is in coinmunication wit the supem osed chamber 18 throu h which ammonia, ydrogen, oxyen or ot er gases rise and escape by way of t e pipe 19 controlled by the valve 20 mto the chamber 21 esca ingunder the hood 22 for condensation an recovery except when the valve 23 is o n to allow the same to pass to the drying c mber 14.

The eleotrolytic bath 17 may be provided with copper electrodes 24 or when the process is worked with zinc chloride, zinc electrodes may be used. An acidulated solution of nitric or sulphuric acid 25 is provided as an electrolyte sufliciently strong to carry the current. l A,

-As the cellulose fed upon the belt 6 passes down through the chamber 18, it passes beneath the Erst electrode 24 at the right side of the figure over the pulley 26, beneath the next electrode, over the next pulley and eq on until it enters the chamber 27, said pulleys being driven by the worms 28 upon the motor shaft 10 and said electrodes being connected to the negative side of a suitable source of electricity as shown, with the result that the metallic content of the cellulose upon the belt is electro-deposited therefrom upon` the electrodes 24 leaving the cellulose gradually becoming white instead of blue or green as itpasses through the electrolytic bath until upon leaving said bath the cellulose is quite white whereupon it enters the washing tank 27 before referred to. The film is now sufliciently tou h and flexible for washing whereas if t e metallic content remained in the film, it would upon drying be brittle and liable to break un. In the washing tank 27 water enters by the pi 29 controlled by the valve 30 and escapes y the pipe 31 which may be provided with a valve 32, the film passingover the pulle s 33 driven by the worms 34 upon the sai motor shaft 10, and a sutiable partition 35 may be provided with an opening at the bottom as indicated at 36 so as to bring the film in contact with the cleaner water of the wash as it leaves the tank 27. All of these tanks are referably closed to prevent foreign matter rom coniing in contact with the film and if desired suitable means may be provided for evacuating air therefrom as any carbonio acid pres ent in the room is apt to form carbonate, and

various other obectionable results may beencountered. This especially applies to the drying tank. The washixg tank removes any a hering ammonia, aci or particles of matter, after which the film passes to the drying chamber 37 where it again passes over pulleys such as 38 driven by worms such as 39 and benath pulleys such as 40 until it finally emerges over the pulley 41 as shown. This drying tank may of course be heated by any suitable means to a. tem erature, say perhaps 120 degrees Fahrenheit. The film f is now loosened from the belt upon which it was formed and due to the heat, shrinkage, etc., is readily separated therefrom, and in this connection a suitable knife or stripper such as 42 may be provided adjacent the eriphery of the roll 4I so as to allow the lm to pass leftwardly between the rollers 43 of the tank 44 while the belt or carrier passes downwardly beneath the pulleys 45 rom which point it returns to the starting place'and again passes through the close tra e detached film upon entering the tank 44 passes over the roller 46 driven by the worm 47 and downwardly through theamylacetate bath 48 assing upwardly again over the roller 49 an u on the rolls 50 preferably of highly olish surface. acetate ta the film is softened, densified, and is increased in its resistance to moisture,

after which, upon passing first 'leftwardly In the amyl- .i

around the top roll 50, then x" litwardly around the next roll below,and eftwardly again, and so' on alternately, it becomes thoroughly dried and finished and is wound upon the reel 51, while the amyl-acetate vapors cscapin through the outlet 52 may be condensed or re-use, thus eprovi a continuons, economic, and pra ical me ducing Elm in which there are Practically no loss but complete recovery o materials, the film ing adapted to traveL through the dit of production higher om present well known roduci durabi s st em with a t an in any methods, while at the same time a film of ateitransparency a ity one w ich an of numerous other properties and advantages.

One of the advantages in the use of our film for photographic purposes is that it may be im re ated from one side (prefora ly unca e ered) with a solution o silver salt, anchas nitrate of silver, after which the lilm may be ex oecd to an atmosphere of, and impregna with bromine, chlorine, iodine or a combination thereof, thereby depositing insoluble bromide or chloride etc. of silver in the film itself. It will be found that by reparing hotographic films in this manrliler llliat after dhe siie heismn lphotogra cayex an evo tereis no Kalring E git'jsecratchi 0H of the negative surface, thus preventing the obectionable elfects in photography somu com- Elained of, as even if the surface of our lm scratched or mutilated, the chemicals having penetrated the lilmI still photographie image, which in the light registers the characters notwithstanding the mutilated surface of the Elin. Another advan of our process resides in the fact that by passing the illm from the drying chamber 37 throu h any well known foi-m of nitrate bath o any desired con sistcncy, a pyroxyline may .be obtained in a dense continuous sheet having the same nitrogen content as the ori nal cottoin immersed under equal conditions in the same bath. This provides a ready means for manufacturing granulated smokeless powder without the use of a volatile solvent.

The cuproammonia solution hereinbefore referred to is preferably made by dissolving hydrated cupric-oxide CuHgO, in approtimatel an equal weight of ammonia water containing thirty per cent ammonia hydrate NHOH. The resulting solution is of an intensely blue color und may be considered to be merely a mixture of cupricoxide, (CuO) ammonia (NH.) and water. We have found even under adverse conditions that with about two amperes per square inch of anode, that we can obtain about forty grams of cellulose and about twenty-thxee and onelialf of oopresent the e path of is practically non-combustble per in about an hour and a half. This how. ever is not submitted as an accurato statnl ment as to what may hejdone under more ifavorable conditions.

While we have described our improiements in great detail 4'and with-respect to a referred. form thereof, we do 4not desire i be limited to such details or form since many changes and modifications may be made andt e invention embodied in widely diterent forms without departing from the l spirtist and scope thereof in its broader as What we claim as new and desire to secure by Letters Patent is l. In an apparatus of the class described, the combination of an clectrolytic cell substantial'ly closed to the outside atmosphere, a chamber substantially closed to the outside atmosphere means for f=-= a carrier through said chamber and and means lfor applyin to said carrier u said chamber,

material to e electrolyzed in said cell.

2. In an apparatus of the class described the combination of a chamber substantially closed to the outside atmosphere, an elec trolytc cell, means for passing a carrier through said chamber, means for applying to said carrier in said chamber material to be electrolyzed in said cell, and means whereby said material is paed continuously from said chamber through said cell to be electrolyzed therein.

3. In an apparatus of the class described the combination of a chamber substantially closed to the outside atmosphere, an e1ectrolytic cell substantially closed to the outside atmosphere, means for passing a carrier throuhsaid climber, means for applying to sai carrier in said chamber material to .be electmlyzed in said cell, and means whereb said material 'is assed through .said cel to bc electrolyze therein, and means for withdrawing gases from said chamber and cell. e

4. In an apparatus of the clase described,` the combination of an electrolytic cell substantially closed to the outside atmosphere, and a movin carrier passing into and out of-the electro yte in said oel whereby mi teria] may be electrolyziedpn'the carrier in lthe cell, and means for stripping the materal 'electro-deposited on the carrier in the cell, -from the carrier after 'it leaves the elec'- trolyte in the cell.

5. [n an apparatus of the class described, a continuous metallic belt and an electrclytic bath, said belt being electrically connected to the positive terminal of a source o1' electric current and a metallic cathode in said bath and means for moving thebelt continuously while said electrical current is applied.

6. [n an apparatus of the class described, the combination of an electrolytic bath, a cariio rier moving thmu'ghsaid bath, said earlier, moving the carrier throu h the bath wherebein? connected to one `terminal of a. source by the materiel is electro yzed inutile bath.

of e ctric current to form one electrode in In testimony whereoi.z we have slgned our 1u the bath, an opposite electrode in the bath, names to this speclicatzon.

means for up' lying tothe carrier before it ruters the bat material to .be electrolyzed EDWIN TAYLOR.

on the carrier in the bath, .and means for EDWARD F. CHANDLER.

lier moving through-said bath, said carrier4 moving the Carrier through the bath wherebeing connected to one terminal of a source by the material is electrolyzed in, the bath.

of electric current to form one electrode in In testimony whereof we have signed our 1u the bath, an opposite electrode in the bath, names bo thls speclcatlon.

means for applying to the carrier before it rnters the bath, material to be electrolyzed EDWIN TAYLOR. on the carrier in the bath, and means for EDWARD F CHANDLER.

CERTIFICATE 0F CORRECTION.

Patent No. 1,599,609, i mma 1m e9, 1926.

u Timm- TAYLCR ET AL.

It is hereby certified that error appears in the printed specification of the, above mentioned patent requiring correction as follows: Page l, line 99,` for the word "Carrier" read "carried"; page 2, line 88, for the misspelled word "sutiable"v read "suitablef', and line 106, for "benath" read "beneath"; and that the said Let ters Patent should be read with these corrections therein that the same may conform'to the record of the case in the Patent Office.

Signed and sealed this 8th day of March, A. \D. 1927.

. M. J. Moore, Seal. Acting Commissioner of Patents.

CERTIFICATE OF CORRECTION.

Patent No. 1,590,609, granted June 29, 1926.

to EDWIN- TAYLOR ET AL.

p lt is hereby certified that error appears in the printed specification of the. above mentioned patent requiring correction as follow: Page l, line 99, for the word "carrier" read "carried"; page 2, line 88,v for the misspelled word "sutiable" read "suitable", and line 106, for "benath" reed "beneath"; and that the said Letters Patent should be read with these corrections therein that the same may conform 'to the record of the case in the Patent Office.

'signed an@ sealed this sin any 0f March, A. \D. 1921.

M. J. Moore, Seal. Acting Commissioner of Patents.

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