US1731473A - Method of treating carbonaceous material in an electric furnace or the like - Google Patents

Description

Oct. 15, 1929. J. J.. NAUGLE 1,731,473

METHOD OF TREATING CARBONACEOUS MATERIAL IN AN ELECTRIC FURNACE OR THE LIKE Filed April 21, 1923 2 Sheets-Sheet 2 lNl/EIVTUR JOHN J .NAUGLE A TTORNEY Patented 0a. 15, 1929 UNITED STATES PATENT, OFFICE dorm NAUGLE, or BROOKLYN, new Yoax IIETHOD 0F TREATINQ CARBONACEOUS MATERIAL IN AN ELECTRIC FURNACE OR THE LIKE Application filed Apri121,

My present invention relates to methods of treating carbonaceous material, particularly comminuted carbonaceous material, such as comminuted carbonized lignin residues obtained by carbonizingthe waste liquors derived from the treatment of Wood by the alkali (soda) process in the production of wood pulp, for the production from the materials designated of a very pure grade of carbon characterized by a very low ash or mineral content, high conductivity, and a remarkably high degree of activation corresponding to a high degree of decolorizing power. It is an object of the present invention to devise methods of the character specified above which shall be exceedingly simple in operation, requiring comparatively simple apparatus and a minimum of time, labor and material for this purpose; which shall produce the desired product in the desired condition of high purity, high conductivity and a high degree of activation and decolorizing power; and which shall render possible a very high yield of the desired product in proportion to the raw material used and the amount of power consumed.

In the accompanying specification I shall describe an illustrative embodiment of the method of the present invention. In the accompanying specification I shall also describe, and in the annexed drawing show, one form of apparatus in which the method of the present invention may be conveniently practiced. It is, however, to be clearly understood that my invention is not limited to the specific embodiment of the process described herein, nor to the use of the particular form of apparatus shown and described herein, said apparatus forming the subject matter of a separate application for Letters Patent filed by me of even date herewith.

Inorder that my invention may be more clearly understood,'reference may be made to a co-pending application of mine, filed of even date herewith, .Serial No. 633,643 and entitled Process for the treatment of com minu'ted carbonaceous materials and the like,

in an electric furnace and the like.

In practicing the aforesaid illustrative embodiment of the method of the present in- 1923. Serial No. 633,640.'

vention, I take first any suitable raw material, preferably a carbonaceous material in comminuted or finely divided form. While various types of comminuted carbonaceous material may be treated with success in accordance with the principles of the present invention, either in the production of a highly activated carbon from the raw material, or 111 the revivification of spent decolorizing carbon, I shall describe the present invention as applied more particularly to the preparation of a highly activated-carbon from carbonized lignin residues in comminuted form, such residues being obtained by carbonizing the cooking liquors derived from the treatment of wood by the alkali process in the production of wood pulp.

Taking, for example, the raw material specified above, which comprises comminuted carbonized lignin residues, such material may have an average analysis as follows:

Analysis of ooomm'nuted carbonized Zz'gm'n residues Carbon fi Ash 10 Analysis ofiash. Silicious matter 0.13 Silica I. 0.75 Ferric oxide 0.34 Alumina 0.47 Lime, CaO 0.23 Magnesia, MgO 0.11 Chlorine as chlorides 0.47 Sulphuric anhydride 2.65

Carbon dioxide 1.00

Alkalics (by diff.) 3.85

This material contains certain volatile mat- I fied above so as to expel the volatile substances and to fuse the mineral substances, characterized by a higl. resistivity, for the subseqiient removal of such fused mineral substances. This 1 preferably do by passing an electric current of regulated densit through the mass of the raw material untll 5 the mineral substances present therein have been fused. The degree of current employed should be such as to cause the mineral substances to aggregate or sinter together in the formation of clinkers.

The fused mineral substance is now removed in any suitable manner so as to yield a product which is characterized, by a very high conductivity, an'iounting often to as much as five times the conductivity of the raw material treated, and characterized, further, by a very substantial reduction in the mineral content of the final substance, which mineral content is often reduced to as little as one-fourth or less of the mineral content of the original raw material treated.

- l find that the conductivity of theiinal prodnet is a function of the degreeof activation or decolorizing power of such material, or vice versa, increased conductivity indicating increased activation and decolorizing power, and vice versa. Accordingly, by the removal of the fusible mineral substances, which are of comparatively high resistivity and which, therefore, reduce the conductivity of the final product, 1 am enabled to effect a very remarkable increase in the degree of activation and decolorizing power of the material treated in accordance With the principles of the method of the present invention.

The present method may be combined with considerable success with the means and method described and claimed in my copending application, filed May 22, 19:22, Serial No. 562,828, and entitled Prefiltering means and method, especially so far as the preliminary treatment of the raw materials is con cerned, particularly to effect by'decantation from a watery suspension of such material a partial preliminary separation by gravity of the portions of the material richer in car bon from the portions of the material poorer in carbon and containing an excess of heavy mineral substances. 1 may also use the feature of effecting a purification of the final product by forced filtration, under pressure, through a layer of the final product, of an aqueous acidified fluid and of wash waters. 1 may also add to the charge of material being treated in accordance with the principles of the methodof the present invention, certain reagents, such as sodium fluoride, which. will have the property of eliminating one or more of the mineral substances present in the charge, particularly silica, in the form of volatile by-products, such as silicon fluoride.

The resulting product possesses many advantages for the intended purpose, since it can be very cheaply made in accordance with the method of the present invention, and possesses the desired quality of high conductivity, corresponding to a remarkably high degree of activation and decolorizing power.

An average analysis of such material is as This product is also characterized by a very high degree of purity, corresponding to a high conductivity and a high degree of activation and decolorizing power. The condutivity of the final product is often increased as much as five times that of the raw material treated, and its mineral content is often reduced to as low as one-fourth or less that of the raw material treated in accordance With the method of the present inven-- tion. The method itself is exceedingly simple to practlce, requiring comparatively simple apparatus and a minimum of time, labor. power and material for this purpose. The

methodis also admirably calculated to produce the desired end product in the desired condition of purity, high conductivity, and high activation and decolorizing power. The method is also very economical in View of the very high yield which may be obtainedby its practice as compared with the methods liitherto employed for revivifying spent decolorizmg carbon or for producing highly activated carbons for decolorizing purposes.

Referringto the drawing wherein T have illustrated one form of apparatus in which the method outlined above may be conveniently practiced:

Fig. 1 is a view in longitudinal section,

partly broken away, and partly in elevation,

showing the furnace comprising the aforesaid form of apparatus;

Fig. 2 is a cross-sectional View of the same taken along line 2-2 of Fig. 1 of the draws;

Fig. 3 is a cross-sectional view of the same taken along line 33 of Fig. 1 of the drawmg;

Fig. 1 is a view similar to Fig. 3 taken along line 1-4 of Fig. 1 of the drawing; and

Fig. 5 is an enlarged detail longitudinal sectional View at the outlet end of the machine.

Referring to the aforesaid form of ap herein, I provide means ving bearing sleeves'15-and 16 for paratus in which the aforesaid illustrative embodiment of the method ofthe present invention may be conveniently practiced, the furnace comprising such apparatus includessubstantially cy-' d bars 20, which members are the casing 10, preferably lindrical form, having the inlet tube 11 an the outlet tube 12, sa d-tubes being likewise of substantially cylindrical form and com-- material and the proper distributionjof current through the mass being treated.

The electrodes 20 tudinally' arranged knobs or studs, prefer ably located on both sides of each of the memsulating material or are pro so as to avoid connection wit the electrodes,

are in the form of lon i;

prefe'rablyof inrly insulated,

rising bearings for the casing 10. The cas-' and also to avoid short-circuiting the furnace .mg and'the tubes 11 and 12 are supported through the metallic portions of the casing by apluralityof'standards 13-and 14, provldand other parts of the machine. While iva-v the tubular bearings 11 and 12.

In the form illustrated by way of example referably continuous, of the tion, which is t e parts carried by and with- -casing 10 and in the same.

' suitable means such as the annular toothed from of the material and the proper some or all of the members gear 17 carried by and surrounding the casi mg 10, and adapted to cooperate with a spur ear or pinion 18carried by a shaft 19"driven roin any suitable source of deemed necessary ing of the gears 17 and 18, the casing 10 and its associated parts may rate 'of speed.

' Within the casing 10 are a plurality of stirring and mixing also as supports for the electrodes, said members being generally indicated by reference character 20. Each of the members 20 is preferably replaceable or readily-removable the casing 10, as by having each such member pass through an opening or orifice 21 in the wall of the casing 10. By means of suitable bolts 22, passing through flanges 23 forming apart of the base24= of each member 20., each member 20 may be readily installed and asreadil'y removed for cleamng, repair or replacement, as desired.

, In order to bring about an effective mixing distribution of I prefer to. provide 20 with a hollowedout surface for the'reception and subsequent discharge of a portion of the material in the furnace. For this purpose, that face of each current through same,

' or some of the members 20 which, during the rotation of the casing 10, first comes into contact with the material M in the furnace, is dished out or made slightly concave, as indicated at 25.-' 4 It 'will be noted that each set of members 20 is disposed in spaced relation along the circumferential periphery of the inner face 10 of the casing 10. It will also be noted that themembers 20 of each such set are substan tially radially disposed. I have found, by

eriment, that this' disposition of the same is of considerable importance for the proper treatment of the material within.

' tion to the process already described will be the furnace, by insuring proper mixing of the for effecting a rota- Forthis purpose, I provide-any.

power not here to be shown. By the meshbe rotated at any desired 4 rings members, which mayserve 'bular outlet ends of the casinglO, respectively, and suitably insulated ture of the same.

from the metallic struc- At 32 and 33 I have indicated the leads or wires for supplying current to the conductor rings 30 and 31, respectively. I prefer that the electrodes20', of. whichseveral perlpheral sets or rows, here shown as lifn peripheral rows each including ei ht peripherally disposed electrodes, may ployed-,'shall be so connected to the conductor and 31, and the leads 32 and 33 supplying current thereto, that "successive elec trodes in each peripheral set will be oppositely charged and that successive electrodes in.

eem-DO' each longitudinalset will be likewise oppositely char d find that'this arrangement of electr es is highly desirablein that it assists' in effecting the proper distribution of current through the chargeof materialwithin the 79 furnace. r

In order to continuously feed material into ,the furnace for treatment and out of the fur* nace after the same has been subjected to the desired treatment for the desired time, I

provide any suitable means, but preferably an inlethopper 40 for feeding un-- treated material into the machine through the V tubular bearing 11. The tubular bearing 11 length of.

communicates with the central chamber 411 of a spiral feeding device, generally indicated by reference character 42. The spiral feeding device 42. is located at the inlet end of the machine, and is provided with the discharge openings 43 leading into the heating chamber 10" within the casing 1'0. Similarly, the discharge outlet is in the form of a conduit H communicating at its upper end with the tubearing 12 which leads intothe central opening 15 of a spiral outlet feeding device',

generally designated by referencecharacter 46, and similar in-most respects to the spiralinlet feeding device 42. The feeding device 46 has the inlet openings 4 communicating with the spiral passage in the feeding device 46 for the admission of treated material for its subsequent discharge from the ma-- chine. J

The operation of the machine and its relascription and may be briefiy 'summarized as follows: Comminuted carbonaceous material, particularly comminuted carbonized lignin residues, generally indicated by reference character M, is continuously fed into the 1 machine through the hopper 40 and the feeding means/12, and thus enters the heating chamber where it is brought into oper- 1O ative contact with the electrodes The electrodes -20','.by'the continuous rotation of the casing 10 carrying the same, are brought into intermittent contact with the material M and serve to intermittently and continuousxm ly stir and mix the same. This desired action is facilitated by the particular form which the members 20 possess. This form, resulting from the dished-out surfaces with which these members are provided, serves to cause the members20 intermittently to receive and subsequently to discharge a portion of the material M being treated Within the furnace.

The course of such material is diagrammatically illustrated in Fig. 2 of the drawing,

-25 which approximates the position of the mass of material M within the casing for a particular speed of operation 'of the machine.

What I claim as m invention is:

1. The method of treating carbonaceous material to obtain a highly activated, decol-- orizing carbon therefrom, which" comprises heating a mass of such material to fuse a art at least of the mineral content thereof w ile passing collecting m'embers through tliecmass to remove the fused material from the same.

2. The method of treating carbonized lignin residues to obtain a highly activated, decolorizing carbon therefrom, which 'comprises heatinga mass of such material by pass ng an e fuse a part at least of the mineral content thereof While passing collecting members through the mass to remove the fused material from the same.

3. The, method of treating carbonaceous materialto obtain a h orizing carbon therefrom, which comprises pa'ssing a plurality of electrodes through a mass of such material to heat the same sufficiently to fuse a part at least of the mineral content of the mass while stirring the same.

4. The method of treating carbonaceous ectric current therethrough to ighly activated, decol material to obtain a highly activated,.decolorizing carbon therefrom, which comprises The electrodes 20 srve, by reason of their passing a plurality of electrodes througgma connection with the conductor rings and 30 31; and the lead wires 32 and 33 supplying current thereto, to discharge a current of regulated and controlled density through the mass M of material being treated in the furnace. The current should be such as to read 35 ily volatilize volatile matter contained in the minutes. The resulting product, in addition to the desirable properties already specified, possesses a high degree of neutrality, which is very desirable, and possesses also a decolorv izing power substantially, and often as'much as ten per cent, greater than the best activated carbons hitherto produced. The resulting product is described and claimed in a copending application filed by me of even date herewith.

It may here be stated that the carbonized lignin residues referred to herein are the res1- dues remaining after leaching the residues obtained by carbonizing the spent pr used cooking liquors obtained in the treatment ofwood by the alkali (soda) process in the treatment of wood pulp; and that the terms activation and decolorizing, or their equivalents, as used in'the specification and'claims, include also deodorization, purification and filtration.

mass of such material to heat the same s ciently to fuse a part at least of the mineral content of the mass while stirring the-same to collect andremove therefrom the fused macolorizing carbon therefrom, which comprises continuously passing an electric current of regulated density through the mass,

from electrodes extending into the same, to

fuse'a part at least of the mineral content of the mass, and continuously removing the Y fused material therefrom.

7. The method of treating 1 carbonaceous material to obtain a highly activated, decolorizing carbon therefrom, passing an electric curren of regulated density through the mass, from electrodes passinginto and through the same, to fuse a part at least of the mineral content of the mass and removing the fused material therefrom by adhesion of said fused material to said electrodes.

8. The method of treating carbonized lignin residues to obtain a highly activated, decolorizing carbon therefrom, which comprises continuously passing an electric current of regulated density through the mass, from which comprises electrodes passing through the same, to fuse a part at least of the mineral content of the mass, and continuously removing the fused material therefrom by adhesion of said fused material to said electrodes.

9. The method of treating carbonaceous material to obtain a highly activated, decolorizing carbon therefrom, which comprises passing an electric currentof regulated density through the mass, from electrodes extending into the same and in the presence of foreign electrically conductive bodies, to fuse a part at least of the mineral content of the mass, and removing the fused material therefrom.

10. The method of treating carbonized lignin residues to obtain a highly activated, decolorizing carbon therefrom, which comprises continuously passing an electric current of regulated density through the mass, from electrodes extending into the same and in the presence of foreign carbonaceous bodies of comparatively great conductivity, to fuse a part at least of the mineral content of the mass, and continuously removing the fused material therefrom.

11. The method of treating carbonaceous material to obtain a highly activated, decolorizing carbon therefrom, which comprises passing an electric current of regulated density through the mass, from electrodes passing into and through the same and in the presence of foreign bodies of comparatively great conductivity, to fuse a part at least of the mineral content of the mass, and removing the fused material therefrom by adhesion of said fused material to said electrodes.

12. The method of treating carbonized lignin residues to obtain a highly activated, decolorizing carbon therefrom, which comprises continuously passing an electric cur: rent of regulated density through the mass,

from electrodes passing through the same, and m the presence of added carbonaceous bodies of comparatively great cont'luctivity, to fuse a part at least of the mineral content of the mass, and continuously removing the fused material therefrom by adhesion of said fuz-"ed material to said electrodes.

13. The process of continuously treating carbonaceous material, such as carbonized lignin residues, which comprises heating a mass of such material suflicient-ly to fuse a part at'leastof the mineral content thereof, continuously removing said fusible material, continuously adding untreated portions of material to the mass of material being treated, and continuously removing portions of treated material from the heating zone.

14. The process of continuously treating carbonaceous material, such as carbonized lignin residues, which comprises heating a mass of such material, by passing an electric current of regulated density therethrough,

sufficiently to fuse apart at 1 ast of ic mineral content thereof, continuously rel roving said fusible material, continuously adding untreated portions of material to the mass of material being treated, and continuously removing portions of treated material from the heating zone.

1t". The process of continuously treating carbonaceous material, such as carbonized lignin residues, which comprises heating a mass of such material, by passing an electric current of regulated density therethrough from electrodes rotating through the mass of material being heated. sufliciently to fuse a part at least of the mineral content thereof, continuously removing said fusible material, continuously adding untreated portions of material to the mass of material beng treated, and continuously removing portions of treated material from the heating zone.

16. The process of continuously treating carbonaceous material, such as carbonized lignin residues. which comprises heating a mass of such material, by passing an electric current of regulated density therethrough from electrodes rotating through the mass of material being heated, suflicient- 1y to fuse a part at least of the mineral content thereof, continuously removing said fusible material, continuously adding untreated portions of material to the mass of material being treated, and, continuously removing portions of treated material from the heating zone by adhesion of said fused material to said electrodes.

17. The method of treating carbon lignin residues containing mineral impurities to obtain a highly activated carbon therefrom, which comprises heating a mass of such material in an electric furnace in the presence of an addition agent to thereby volatilizea part, at least, of the mineral impurities present in such material.

18. The method of treating carbon lignin residues containing silicious mineral impurities to obtain a highly activated carbon therefrom, which comprises heating a-mass of such material in the presence of a fluoride to thereby volatilize a part, at least, of the silicious mineral impurities present in such material.

19. The method of treating carbonized lignin residues containing mineral impurities to obtain a highly activated decolorizing carbon therefrom, which comprises passing a heating electric current of regulated density through a mass of such material in the presence of an addition agent to thereby volatilize a part, at least, of the mineral impurities present in such material.

20. The method of treating carbonaceous material to obtain a highly activated carbon therefrom which comprises heating a mass of such material in an electric furnace to fuse a part at least of the mineral content thereof, in

the presence of an addition agent to thereby volatilize a part at least of the mineral content of the mass.

21. The method of treating carbonaceous material to obtain a highly activated carbon therefrom which comprises heating a mass of such material in an electric furnace to fuse a part at least of the mineral content thereof, in the presence of an addition agent to therebyv volatilize a part at least of the mineral content of the mass while agitating said mass.

22. The method of treating carbonaceous material to obtain a highly activated carbon therefrom which comprises heating a mass of such material to fuse a part at least of the mineral content thereof, said heating being in the presence of a fluoride to thereby volatilize a part at least of the mineral content of the mass.

I 23.- The method of treating carbonaceous material to obtain a highly activated'carbon therefrom which comprises heating a mass of such material to fuse a part at least of the mineral content thereof, said heating being in the presence of a fluoride to thereby volatilize a part at least of the mineral content of the mass while agitating said mass.

24. The method of obtaining a highly activated carbon which comprises heating carbonaceous material in an electric furnace to fuse a part at least of the mineral content of the carbonaceous material while passing collecting members through the material to remove the fused material from. the carbonaceous material.

In testimony whereof, I have signed my name to this specification this 30th day of March, 1923.

JOHN J NAUGLE.

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