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April 19, 1938. A. POTT ' 2,114,456 METHOD OF PREPARING A POWDERED CABBONACEOUS MATERIAL FOR COMBUSTION ENGINES Filed April 5, 1935 "O 410 400 396 380 370 360 350 . 340 “Rummy-mm INVENTOR ALFRED POTT BY . ‘ ‘ . A . ORNEY . Patented Apr. 19, 1938 , 2,114,456 UNITED STATES PATENT ' OFFICE 2,114,456. ' ~ METHOD OF PREPARING A POWDEBEDICAR BONACEOUS MATERIAL FOR CQMBUSTION ENGINES ' Alfred Pott, Essen-on-the-Ruhr, Germany Application April 5, 1935, Serial No. 14,793 In Germany October 17, 1934 ' ~6 canine (01. 44-1) This invention relates to a method of prepar cause of the absence not only of incombustible " ing carbonaceous powdered fuel material. for material but of constituents which tend to in combustion engines, ‘particularly those of the Diesel type. In such engines, air for combustion crease the fuel’s heat capacity as well. - ‘ ‘ Various processes of manufacturing such ex 5 is compressed and thereby heated~to such an extent that the fuel is automatically ignited at tracts of goal, lignite, peat, etc. are known, us- .5. ing organic solvent media at- elevated tempera the desired moment. To this effect, in engines tures and, preferably, raised pressure during ex using liquid fuel, the latter is introduced into the traction. All ‘these extracts of coal, lignlte, etc. highly compressed and very hot air by means may be used for the purposes of the invention 10 of a ‘stream of more highly compressed air. In " provided they are .sufiiciently free or freed of in- ‘0 engines provided with pistons, the liquid fuel’ is thus injected just before the piston approaches the end of its stroke of compression. In engines to be fed with powdered solid fuel material, how 15 ever, dif?culties have been experienced when the ' fuel was simply injected. No complete vcom- ‘ combustible residues. If the normal purity of the extracts is still insufficient, ?ltration has to be effected preferably underraised pressure and at highly elevated temperatures. Furthermore, in order to obtain great e?l- 15 ciency of the original fuel material, high yields bustion of the fuel which apparently does not ignite as readily as liquid fuel could be obtained; of extracts are imperative. For this purpose, the - among other reasons this may be to its relatively tracts based on‘the following observation. invention uses 'almethod of producing the ex- - If no larger size and heat capacity and its relatively .e..g. coal is treated in an autoclave with a suit smaller active surface compared with ?nestv ' able solvent medium, such as a mixture of lower and higher- boiling oils, thereby gradually raise ing the temperature and registering the rising rial into the combustion air in ample time before pressure in the autoclave by means of an indica drops of liquid fuel._ Therefore, it is advisable to-introduce the powdered carbonaceous mate 25 the temperature of ignition is reached, in‘ order to permit the fuel to be thoroughly heated. In such engines another difficulty has been encountered due to the ash content in the fuel material. Ashes in amounts sufficient to grind 30 off the cylinder and piston surfaces remain in the machine after combustion. ‘The lubricating ' oil circulating in the machine transports the ash to other sensitive parts of the machine, result ing in considerable wear within a short time of 35 operation. . - I tor, a sudden increase of pressure can be ob- 25 served‘at a vcertain temperature.‘ This is due to the fact ‘that a decomposition of the material ' under treatment takes place whereby gases are evolved. Therefore, if the temperature at a subsequent treatment of material of the same 30 ‘kind, with the same solvent media, remains a few degrees centigrade below the temperature of decomposition, so established by a previous treat ment, a certain yield of extracts can be obtained. However, no matter how long such treatment at 35 , It is an object of the invention to present a this temperature might be extended, or how carbonaceous powdered fuel material in a state oftendt might be repeated, the yield of extracts of high purity, practically free from ash. does not materially increase. After having ob It is a further object of the invention to pre-‘ tained a ?rst yield of extracts in the way de 40 sent the powdered carbonaceous fuel material in scribed, the temperature of_ treatment may be 40 ' a state of high activity. __ .\45 _ w raised, however, without causing decomposition, ‘It is still another object. of the invention to i. e. the evolving of gases indicated by suddenly render the combustion, calculated upon the original solid fuel m'aterial, very effective. .incr'easing'pressure. By the ?rst treatment all the constituents capable of ‘decomposition at According to the invention, no natural carbo - the first. established temperature are extracted 45 “\ naceous powdered material but solid powdered ex from the carbonaceous material and taken in solution by the solvent medium, which protects them against further decomposition, 'and av bal ance of‘ solid carbonaceous material remains the constituents of which are incapable of decompo- 50 tracts of such material is used as fuel. Due- to their production, such extracts are free or freed of ash and other impurities .to any desired de 50 gree, therefore, not leaving in the machine any detrimental residues. Furthermore, the extracts ,bemg practically" pure carbon substance and sition at this temperature. If,~ however, the‘ ' temperature is gradually raised above the?rst \ L" forming depolymerized and slightly hydrogen 'mentioned level, a temperature will again be ' ated products, such extractsare more active than reached at which decomposition, indicated by.v a '55 the initial coal substance, all the more 'so be sudden rise‘loi' pressure, reoccurs; Therefore, a 55 2 , 2,114,456 . “second extraction has to be effected at a temper ature above the ?rst extraction temperature but ‘by a few degrees centigrade lower than the sec ond, higher temperature of decomposition estab lished in the way described. Surprisingly,‘ in this second‘stage in which the balance of the solid carbonaceous material is being‘ treated at a tem perature higher than the ?rst one, a new sub stantial yield of extracts will be obtained in ad dition to that obtained during the ?rst treat ment. In continuing this. procedure, one may cautiously raise‘ the temperature more and more, obtaining thereby additional yields of extracts until a temperature has been reached at which 15 the last yield of extracts is achieved and no ad ditional amounts of extracts are obtainable, neither by repeating nor by extending the heat treatment at the last and highest temperature nor by further raising this temperature. In the latter case neither’ a decomposition can be ob served (nd sudden increase of- pressure occurs any more) nor will additional extracts result. This last temperature depends upon the compo sition of the carbonaceous material under treat 25 ment, and this and all the foregoing tempera tures of treatment, which are close to but below the decomposition temperature of the carbo ‘so with this coal that a ?rstdecomposition occurs at 330° C. The constituents decomposing ‘at about this temperature having been extracted, the remaining solid carbonaceous material de~ composes a second time at 360° C., whereupon after additional extracts have been made at this second temperature range a third, fourth and ?fth decomposition temperature occurs at about 380°, 400° and 410° C., respectively. Therefore, as the diagram shows, the coal had been heated up to 330° C. when the ?rst extracts were made which may remain in the solvent medium or may be removed'from it. Thereupon the tem perature has been gradually or stepwise increased up‘ to 410° to 415° C., and a second, third, fourth 15 and ?fth extract were obtained at about 360°, 380°, ‘400° and 410° to 415° C., respectively. ‘As shown in the diagram, no additional extracts could be obtained at the sixth and seventh ex traction, and therefore further raising of the 20 temperature'or continuation of the treatment at about 410° C. is ineffective. -The ressure in the autoclave was ultimately raised to about 70 to 90 atmospheres. No destruction of the solvent medium took place because of this increased 25 pressure in spite of the temperature being sub stantially above the normal boiling temperature naceous material under treatment, are to be es under atmospheric pressure of some parts of the tablished for every individual, material in the solvent media. Calculated upon the weight of the original, not disintegrated coal material, by 30 way described hereinbefore. . If but a small amount of gases is evolvedv the ?rst extraction about 37% extracts were ob thereby and depending upon the nature of the ' tained, by the second extraction additional 8%, material, the treatment may also be performed with additional yields at further extractions so at about‘ the various decompositiontemperatures, that the entire yield of extracts amounted to 35 provided the decomposition of a small partvof about 74%. The remaining solid material con 35 the constituents ‘is of no consequence. sisted of _colée and ash not capable of further From this it results that the. extraction may be disintegration. ‘As a matter of fact, depending effected at elevated temperatures which are step upon the nature of the coal under. treatment, wise or gradually raised so that they. are close yields up to 94% may be obtained in this way.v 40 to the decomposition temperature of the solid Thus, any and all combustible constituents are 40 carbonaceous material under treatment and in extracted from the fuel material, and the high; creased with the increasing amount of substance est e?iciency is achieved as far as the given solid extracted from the material and taken in solu fuel material is ‘concerned. tion ‘by the solvent media used. The pressure The extracts so obtained are highly active. The extracts being solid at normal temperature 45 45 under which, the treatment is performed is usu ally the normal pressure originating at the tem up to about 200° C. and'over, coal extracts up to perature applied for} the treatment performed in a closed vessel (autoclave). Additional pressure may be applied, however. about 230° to 250° 0., they can be conveniently separated from the solvents by gradually cooling the solvents still containing the dissolved extracts. 50 ' As solvent media, among others, hydrogenated and/or acidic organic oils, alone or in mixture, If some undesired amounts of ash and other 50 may be used. By way of‘example only, a~mix tureof 40 parts naphthalene, 40 parts tetraline not disintegrated parts of the carbonaceous ‘ma _terial remain in the extracts, they may be sepa rated by centrifugalization or ?ltration or. by al and 20 parts of a tar phenol boiling at about lowing the solution to stand so that the heavier 55 230° C., or a mixture of tetraline and phenols in solid particles may precipitate. If, due to the 55 a ratio of e. g. 1:1, or anthracene oil alone, or ‘extremely ?ne dispersion of the impurities re ‘in mixture with phenols or other oils such as ferred to ‘none of these methods succeeds, then' tetraline or benzole, may be used. i - In the drawing, a diagram is shown for the 60 treatment of a long-?aming coal with a solvent medium consisting of 40 parts naphthalene, 40 parts tetraline and 20 parts tar phenols obtained by distillation of coal between"180° to 230° C. The long-?aming coal has‘ been powdered or 65 suitably broken up and then mixed with the sol vent medium. The amount of solvent medium applied depends upon its nature and that of ' the carbonaceous material to be extracted. The weight of the solvent medium may be, for in 70 stance, equal to that of the carbonaceous mate rial, or it may be higher or lower. 1 the extracts still dissolved in the solvent medium may be ?ltered under raised pressure and. at highly. elevated temperature. Thereby practi cally pure extracts are obtained, the content of undesirable solid particles being substantially below 1% and, as a great number of investiga tions have proven, amounting to only a few tenths of one per cent down to less thanyone tenth of one per cent. For this ?ltrationja/ny suitable ?lter and ?lter material may be used. ~The solid‘ ‘residue of extraction of carbprihceous material is most suitable as ?lter materiallfor the extracts. obtained therefrom. As average ‘temperatures 70' for this ?ltering 150° to_170° _C., may be men tioned, but higherv or lower temperatures may autoclave provided with a stirring device and’ be applied. As the lowest limit a temperature treated therein for about three to four‘ hours. range of about ‘75° to 100° C. may be given. The 75 It has been established by special experiments - pressure may be chosen above about 5 atmos 'I The coal and the solvent are deposited into an 3 2,114,456 of decomposition of the carbonaceous material pheres per square centimeter and very good re sults have been obtained within the range of 10 to 20 atmospheres. In this way extracts are ob under treatment and raised until no additional , .yields of extracts are obtained, said extracts sep tained which are both easily and fully combusti- - arated from the solid residues and powdered. 3. A carbonaceous fuel material for combus ble and extremely pure. These extracts being solid at normal and ele vated temperatures up to certain limits men tioned above, are now to be powdered in any tion engines consisting substantially of powdered solid extracts obtained from solid carbonaceous material by treating it in closed vessels with sol vents at gradually increasing temperatures and correspondingly rising pressures, said tempera 10 tures lying close to the increasing temperatures of decomposition of the carbonaceous material suitable way and to any desired ?neness. Ball mills may be used and the treatment therein ex tended sui?ciently long to obtain the desired size of powder. . - ' ~ under treatment and raised until no additional As an engine suitable for the powdered car yields of extracts are obtained, said extracts sep arated from the solid residues by ?ltration under 15 elevated temperatures above about 75° C. and under raised pressure above about 5 atmospheres per sq. cm., and ‘thereupon powdered. 4. A carbonaceous fuel material for combustion engines consisting substantially of powdered solid 20 extracts obtained from solid carbonaceous ma terial by treating it ‘in closed vessels with solvents bonaceous extract according to the invenion the 15 motor described in the periodical “Oel und Kohle’_’, December 1933, pages 135, 136, may be referred to. This motor uses an additional chamber in which measured quantities of pow dered solid fuel are delivered ahead of each com 20 pression stroke of the piston. The chamber is in open connection with the cylinder so that the compressed‘ and heated air enters'this chamber at stepwise increasing temperatures and corre and gradually heats the fuel deposited therein until its ignition starts automatically and the spondingly rising pressures, said temperatures lying close to the increasihg temperatures of de 25 25 evolved gases of combustion expand into the cyl composition of the carbonaceous material under inder, injecting into it simultaneously the still ' treatment and raised until no additional yields - burning fuel. It is to be understood, however, that the inven. tion is not limited to the use of this or any other 30 type of a reciprocating or‘ continuously turning engine adapted to be operated with powdered of extracts are obtained, said extracts separated from the solid residues by ?ltration under ele vated temperatures above about 75° 0.,‘ and un 80 der raised pressure above about 5 atmospheres ' 5. A method of producing carbonaceous fuel It is further to be understood that the fuel ma terial according to the invention may be used as - material for combustion engines comprising the solid fuel material. , - per sq. cm., and thereupon powdered. 35 such alone or in admixture to any other powdered . steps of extracting solid carbonaceous material with solventsin closed vessels at increasing tem solid or even liquid fuel material. In the appended claims the term "so1vent” comprises any suitable solvent medium for the' constituents to be extracted, or any mixture of 40 such solvent media. What I claim is: ‘ 1. A carbonaceous fuel material for combus peratures and correspondingly rising pressures, said temperatures lying close to the increasing temperatures of decomposition of said car bonaceous material, and raised until no addi tional yields of extracts are obtained, separating the extracts thus obtained from the solid residues of said material, allowing said extracts to solidify, and thereupon powdering said solid extracts. 6'. A method of producing carbonaceous fuel vents at gradually increasing temperatures and ' material for combustion engines comprising the steps of extracting solid carbonaceous material correspondingly rising pressures, said tempera tures lying close to the increasing temperatures with solvents in closed vessels at increasing tem-, of decomposition of the carbonaceous material peratures lying'close to the increasing tempera 50 under treatment and raised until no additional tures of decomposition of said carbonaceous ma tion engines consisting substantially of powdered solid extracts obtained from solid carbonaceous 45 material by treating it in closed vessels with sol yields of extracts are obtained, said extracts sep arated from the solid residues and powdered. 2. A carbonaceous fuel material for combus tion engines consisting substantially of powdered 55 solid extracts obtained fromv solid carbonaceous material by treating it in closed vessels with sol vents at stepwise increasing temperaturesand correspondingly rising pressures, said tempera tures lying close to the increasing temperatures terial, and raised until no additional yields of extracts are obtained, separating the extracts thus obtained from the solid residues of said ma terial by means of ?ltration at elevated tem peratures aboveabout 75° C. and raised pressure above about 5 atmospheres per sq. cm., allowing said extracts to solidify, and thereupon powder ing said solid extracts. AIFRED P011‘.