US3151942A - Carbon black process and apparatus - Google Patents

Carbon black process and apparatus Download PDF

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US3151942A
US3151942A US90557A US9055761A US3151942A US 3151942 A US3151942 A US 3151942A US 90557 A US90557 A US 90557A US 9055761 A US9055761 A US 9055761A US 3151942 A US3151942 A US 3151942A
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hydrocarbon
carbon black
zone
inert gas
gas
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US90557A
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Frederick E Frey
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Phillips Petroleum Co
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Phillips Petroleum Co
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/44Carbon
    • C09C1/48Carbon black
    • C09C1/50Furnace black ; Preparation thereof
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/12Surface area
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/19Oil-absorption capacity, e.g. DBP values

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  • the invention relates to the production of carbon black.
  • the invention provides a process for the production of carbon black wherein an organic compound such as a hydrocarbon which can be decomposed or cracked to produce carbon black is flowed into a reac tion zone into a hot, relatively inert gas flowing, in a preferred embodiment of the invention, in turbulent flow along a curved path whereby superfast transverse dispersion of hydrocarbon across the turbulent, relatively inert gas stream is obtained.
  • the invention relates to a process which comprises immediately radially distributing in an outwardly direction into a hot, relatively inert gas flowing in turbulent flow in a curved path, a hydrocarbon to be converted to carbon black.
  • a hot, relatively inert gas for use as herein described by passing an oxygen-containing gas such as air, air enriched with oxygen, oxygen, and/ or carbon monoxide through a preheated coke bed at a temperature sufiicient to produce a gas relatively low in carbon dioxide and water as compared with ordinary combustion gases utilized in carbon black producing operations.
  • an oxygen-containing gas such as air, air enriched with oxygen, oxygen, and/ or carbon monoxide
  • the invention in another of its aspects, relates to the execution of the process in an apparatus wherein "there is provided a substantially cylindrical combustion chamber and appended annulus, adapted to generate and to flow through the annulus a hot combustion gas, a reaction chamber disposed Within said combustion chamber and forming said annulus therewith, a corebuster substantially concentrically disposed in one portion of said reaction chamber, means for introducing a hot gas through a second annulus formed between said reaction chamber and said corebuster, means for introducing a hydrocarbon to be converted to carbon black into said reaction chamber substantially at the place along its length at which the corebuster terminates therein and means for removing gaseous decomposition products from said reaction chamber.
  • the invention in another of its aspects, relates to producing carbon black of small, ultimate particle size by introducing into a stream of hot gas, low in its content of the normal products of combustion, which ar carbon dioxide and water, a hydrocarbon which will crack to produce carbon black at a very high velocity of turbulent flow, high temperature, and short reaction time, thus producing a high yield of carbon black of small, ultimate particle size and having strong reinforcing properties in rubber.
  • an apparatus for producing carbon black which comprises an elongated, substantially cylindrical reaction zone, means for tangentially introducing a hot, relatively inert gas into said zone at one end thereof, means for introducing axially a hydrocarbon feed into said end of said zone, means in the end of said zone placed transversely to the axially introduced hydrocarbon so that said hydrocarbon impinges thereagainst and is thus radially distributed into said hot gas flowing in turbulent flow along a curved path, and means at the other end of said zone for recovering carbon black.
  • the black made at high velocities has high reinforcing properties, producing 4,000 pounds per square inch tensile strength in rubber, more or less; can have a small ultimate particle size, and is of a constitution such that in the compounded rubber high stress is shown at a moderate amount of stretching.
  • a carbon black of improved properties as set forth and described herein can be prepared employing high velocities of flow in excess of approximately 20 feet per second, preferably in excess of 45 feet per second, of a mixture of heat-carrying, relatively inert gas and hydrocarbon vapor, the gas being mixed with the hydrocarbon vapor by introducing the hydrocarbon vapor into a spirally flowing turbulent mass of said gas in a reaction zone of fairly small diameter.
  • the intermixing is essentially immediately accomplished and the residence time in the zone can be sharply limited, thus yielding an efiicient, economical,
  • conversion factor modus operandi for producing carbon black
  • An object of this invention is to provide a process for the production of carbon black. Another object of this invention is to provide an apparatus for the production of carbon black. It is an object of this invention to provide a process and apparatus for the production of carbon black in high yield and of small, ultimate particle size. It is another object of this invention to provide a carbon black having strong reinforcing properties in rubber.
  • a process and apparatus for the production of carbon black e3 which comprises cracking an organic compound or hydrocarbon which yields carbon black under carbon black producing conditions of temperature, pressure, and flow rate by flowing the hydrocarbon, preferably as a vapor, into a hot, relatively inert gas flowing in turbulent flow along a curved path whereby superfast transverse dispersion, as herein defined, of hydrocarbon or compound across the turbulent, relatively inert gas stream is obtained.
  • the rate of flow of gas and vapor mixture is at least about 20 feet per second.
  • a gas low in the usual products of combustion such as carbon dioxide and water is used as the relatively inert gas stream.
  • an apparatus in one of its forms, consists of a series of concentrically disposed elements, a cylindrical combustion zone having an annulus appended thereto, a reaction tube within said zone and forming said annulus, a corebuster extending throughout a portion of said reaction tube, means for regulating the heat transmitted from said combustion zone and annulus to the corebuster within said reaction tube and means for introducing a charge to be cracked to carbon black through said corebuster into the reaction zone within said reaction tube and means for collecting carbon black produced in said reaction tube.
  • the present invention produces a new result over the prior art in that there results a very high yield of a carbon which imparts high tensile strength to rubber and, while maintaining high tensile strength, permits production of a rubber product exhibiting moderate stress at a moderate stretch.
  • the essential features of the process of the invention are: (1) The use of heated, relatively inert gas, nitrogen, hydrogen, carbon monoxide or their mixtures, with little or no carbon dioxide or water, flowing in a turbulent spiral flow, (2) rapidly admixing hydrocarbon with this so-flowing preheated gas using a passageway of small cross section whereby linear velocities of at least 20 feet per second and preferably, at least 45 feet per second, in the gas are imposed to effect thermal cracking to carbon black very rapidly, and (3) effecting the reaction at an optimum temperature within the ranges 2,300 F. to 3,500 F. in a reaction time of under 0.1 second.
  • FIGURES 1 through 12 illustrate diagrammatically or schematically various arrangements in which one or more of the several concepts of the invention can be embodied.
  • FIGURES 9 and 10 are, respectively, vertical cross sections of an actual apparatus taken in a plane passing through the axis and a plane at right angles thereto.
  • FIGURE 11 is a modification of the apparatus as shown in FIGURES 9 and 10.
  • FIGURE 12 is a cross sectional view of a corebreaker adapted to be used in the'apparatus of FIGURE 9.
  • FIGURE 1 which is a schematic showing of one embodiment of the invention
  • 1 is a conventional preheating furnace in which the inert gas, nitrogen in this embodiment, is preheated.
  • the preheater can be omitted if desired and the gas can be available already sufiiciently hot for its intended use.
  • Superheater 2 is operated by indirect heat exchange through a ceramic wall. In a variation, it can be operated by electric heating, by electric discharge or resistors.
  • a small amount of oxygen, preferably preheated, can be added to the hydrocarbon feed in the reactor to boost the temperature slightly when the reactor temperature is already in a high temperature range.
  • reaction zone 3 there is provided, at the beginning of reaction zone 3, a constriction producing the required velocity of inert gas of at least 20 feet per second.
  • Zone 1 and 2 include a pebble heater to produce hot inert gas, a blow-and-run refractory heating plant using two or more units operating on staggered cycles of combustion heating alternating with superheating of the inert gas. Blending exit inert gas on a controlled varying ratio can be used to hold downward drift of superheat temperature in a suitable range to control efficiency and black quality.
  • Reaction zone 3 is substantially vertically disposed.
  • the heated, relatively inert gases are introduced substantially tangentially in a manner to create along the inner wall of zone 3 a downwardly moving blanket of turbulent gases flowing in a curved path.
  • Hydrocarbon vapor to be converted in this embodiment, benzene heated to about 2,500 F., is introduced substantially axially at the top of reaction zone 3 through pipe 4.
  • the relative sizes of the reaction pipe and volumes of gases at the operating temperature are chosen to maintain not only the turbulent curved path flow of the relatively inert gases but also to cause the introduced hydrocarbon to be immediately (superfast) admixed therewith.
  • the relative velocities of the relatively inert gas and hydrocarbon are adjusted to allow the hydrocarbon to pick up sufficient angular velocity from the relatively inert gas to be impelled thereinto by centrifugal force, the turbulent flow of said relatively inert gas then immediately causing the desired mixing to take place with great uniformity.
  • the hydrocarbon can be made to flow over a ceramic plate 5, thus causing the hydrocarbon to be moving in a film which is immediately sheared into the turbulently flowing, hot, relatively inert gas. By pointing the constricted portion of tube 2, slightly downwardly increased shear of the gases can be obtained.
  • the length of the reactor, its diameter, etc., are so proportioned that the reacted hydrocarbon streams can be immediately cooled to below 1,200 F., preferably 800 F., at the end of the desired residence time which, in this embodiment, is 0.1 second.
  • a water spray 6 is provided in tube portion '7 at the point at which the reacted hydrocarbon is cooled sufficiently by itself due to endotiermic reaction and radiant and convection heat loss, so that undesirable reaction between the carbon black and the water spray will not occur.
  • separator 8 which is conventional, gaseous products are removed at 9 and carbon black is recovered at 16.
  • the relatively inert gas used in this embodiment is essentially nitrogen and it can be recovered from the separator and can be returned at least in part to preheater 1.
  • FIGURE 2 shows admixing the hydrocarbon with the relatively inert gas at the point of maximum mixing rate in a curved tube.
  • the hydrocarbon is introduced into tube 20 by pipe 21.
  • the curved nature of tube 20 causes the relatively inert gas to spiral.
  • the spiralling, hot, relatively inert gas intro symbolized at 25 is passed through a constricted passageway 26 together with hydrocarbon axially introduced through pipe 27.
  • FIGURE 4 shows both relatively inert gas and hydrocarbon entering axially at high velocity.
  • the relatively inert gas is fed to the reactor through pipes 30 which are oriented to cause said gas to move in a spiral path in turbulent flow. Hydrocarbon is introduced at 31.
  • FIG- URE 5 shows the hydrocarbon entering the reactor axially and the relatively inert gas entering radially at high velo city.
  • the relatively inert gas is pumped in through pipe 35 and the hydrocarbon is pumped in through pipe 36.
  • FIGURE 6 shows the relatively inert gas entering the reactor axially at 40 with the hydrocarbon pumped in radially at 41.
  • the hydrocarbon stream flows in the highly turbulent curved flow and the relatively inert gas is caused to be admixed therewith.
  • FIGURE 7 shows opposing jets of relatively inert gas and hydrocarbon entering the reactor, resulting in fast mixing.
  • the hydrocarbon and the relatively inert gas enter mixing zone 45 through pipes 46 and 47, respectively. Since the inert gas is in considerable excess, the gas will govern the overall flow which will be in an essential spiral manner in tube 43. Substantially all of the mixing takes place in zone 45, however. Any slight additional mixing is caused by the spiralling gas, as earlier described.
  • FIGURE 8 shows opposing jets of inert gas and hydrocarbon and a stream of inert gas entering the reactor axially.
  • the gas enters through pipes 59 and 51 while hydrocarbon is introduced through pipe 52. Mixin immediately occurs in zone 53. The spiralling motion is again obtained due to the excess of gas entering at 51 over the hydrocarbon.
  • FIGURE 9 is a diagrammatic drawing of the reactor used to obtain the data of this invention which are shown in Table 1 below. This embodiment is similar to that shown schematically in FIGURE 4.
  • an axially disposed cylindrical section has a lining 111 of highly refractory sillimanite. Between this refractory liner 111 and a cylindrical steel shell 113 is a layer of insulation 112. Combustion section 114, coaxial with liner 111, is also lined with lining material 111. In combustion zone 114 are arranged inlets 123, which are so disposed that gas can be passed therethrough and into combustion zone 114 in a direction tangential to its cylindrical wall. Most of the tangentially introduced gas is burned within tunnels 126. Cooling assembly 118 downstream from the cylindrical section and adjacent thereto consists of water jacket (not shown) and water spray 134.
  • a combustion mixture of methane and oxygen or oxygen mixed with steam or air is charged to tangential burners 123. Tangentially introduced gas is burned in tunnels 126, the combustion gases thus produced traveling helically within combustion zone 114 and continuing along annular space 119 formed by the inner wall of liner 111 of the cylindrical section and outer wall 115 of reactor tube 116.
  • a seal 116a is provided between the outer wall of tube 116 at its left end, as hown, and liner 111.
  • Wall or surface 115 is provided with a helical protrusion 115a which serves to maintain centered outside wall 115 within the apparatus and also serves to force the gases to move spirally throughout the entire length of annulus 119.
  • the annular space between the reactor tube 116 and the cylindrical section is of uniform width approximately 1% inches maximum.
  • the burning taking place in tunnels 126 serves as a source of heat.
  • Sufficient heat is provided to heat the outside wall 115 of reactor tube 116 to a temperature of 2,875 F.
  • the gas is passed into cooling assembly 118 (described previously) and rapidly quenched to a temperature below 1,200" F. in both indirect and direct heat exchange relation with water.
  • the inside wall at 117 of reactor tube 116 becomes heated to a temperature of 2,750 F. by the hot gases flowing in annular space 119.
  • Nitrogen gas preheated to 1,200 F. (preheater not shown) is introduced through pipe 121' ⁇ and enters annular space 121 formed by corebreaker 122 placed inside reactor tube 116. This annular space 121 is inch in width.
  • the linear velocity of the nitrogen gas in annular space 121 is at least feet per second.
  • the nitrogen gas becomes heated to a temperature of 2,600 F. by the hot inside wall 117 of reactor tube 116.
  • the outside wall at 124 of corebreaker 122 reaches a temperature of 2,700 F.
  • the corebreaker 122 is positioned in reactor tube 116 to assist in obtaining a high ratio of heat transmitting surface to volume in a tube of large diameter and high throughput.
  • the reactor tube is made of silicon carbide for high heat transfer.
  • the 1% inch corebreaker 122 is made of alumina, but might, if desired, be made of other refractory material, such as for example fused quartz or illimanite.
  • the corebreaker placed centrally in the reactor tube, reduces the effective cross sectional area of the reactor tube.
  • the corebreaker outside surface 122 is provided with spiral ridge 122a which helps to create a spiral motion of the preheated nitrogen gas. Water is circulated in tube 127 positioned in corebreaker 122.
  • the preheated hydrocarbon vapor feed at 250 F.
  • the product enters tube 123 and is sprayed by orifice 12% into reaction chamber 116.
  • the efiiuent temperature at 131"; in the reaction chamber 116 is 2,000 F.
  • the product enters a cooling assembly 131 which consists of water jacket 132 and a water spray (not shown).
  • the water spray if used, is located sufliciently downstream to allow cooling of the product by water jacket 132 to a temperature low enough to avoid reaction of water with carbon.
  • An atmospheric cooling pipe can be used in place of a water spray. Such a pipe can also be used with a water jacket.
  • the black is, in any event, cooled preferably to a temperature at which it will not react with the water spray when such a spray is used, but precooling can be small if the volume of spray water is sufiiciently large to quench to below reacting temperatures.
  • a water spray is preferred provided the black is cooled to such a nonreacting temperature.
  • Any usual means not shown for separating solids from gases can be applied to the downstream end of pipe 133 to separate the carbon black in the course of its production.
  • the temperature within the reaction chamber 116 can be varied within wide limits, for example, within the range of 2,060 to 3,300 F. or higher. The upper limit depends on the temperature the refractory material will stand. Better yields of excellent quality carbon black resulted from operating periods when temperatures were of the order of 2,300 to 2,600 F. in reactor 115.
  • the reaction time was less than 0.1 second.
  • the reactor 116 was 2 inches in diameter and 18 inches long.
  • FIGURE 11 there is shown an embodiment of the invention in which the annular, hot, relatively inert gas is fed into the reaction section 216 substantially at the introduction of the feed at 229. This is accomplished in the instant embodiment by providing at least one set of holes or apertures 300 through which the hot gas is directed towards the axially introduced feed.
  • the annular space 221 is terminated at its reaction section end by a closure 301. This permits passing all of the annularly introduced gases through the holes 300 as indicated by the arrows.
  • FIGURE 12 which shows a corebreaker adapted to be used in the apparatus of FIGURE 9, 400 denotes the corebreaker body having spiral 401 on its outside surface.
  • Water or other cooling medium is circulated through the corebreaker by inlet 402 and outlet 403.
  • the cooling medium circulates around the tube to prevent its temperature from reaching a value at which undesired reaction of the hydrocarbon will take place.
  • insulation such as Alfrax packing, is provided as shown at 405. This material is preferably cast into place after insertion of the cooling medium pipes and surrounds said pipes.
  • the cooling medium passageway is surrounded by Fiberfrax packing or similar material.
  • the corebreaker is tapered in this modification .to assist in the acceleration of the inert gases which are passed to the reaction section 115 of FIGURE 9 by annulus 121 of said figure.
  • the corebreaker is made in this instance of alumina.
  • the inert gas is shown introduced parallel to the axis of the apparatus, it is within the scope of the invention to introduce tially or transversely to the tapered or inlet end of the corebreaker.
  • the butadiene-styrene rubber is a 71-29 butadienelstyreii e copolymer prepared by emulsion polymerization at 122 Table II gives properties imparted to a 122 F. rubber by these thermal blacks at 30 minutes cure at 307 F. and oven agent 24'hours at 212 F.
  • Ben- Com- 200 F Extrusion at Nitrogen Oil zene pres- 300% Elon Maxi- Flex Shore Abra- Corn- 250 F. Black surface pH absorpere sion mod- Tengation, mum liie, hardsion pounded,
  • the carbon black of the process of the present invention produces in a cured rubber product, as above described, certain highly desirably properties. Among these are very greatly increased flex life and greatly decreased abrasion loss over a well known commercially available carbon black made by a substantially conventional furnace operation. Another notable great improvement has been made in tensile strength. Also, 300 percent modulus has been very greatly increased. The nitrogen surface area, oil absorption, and benzene extract results are also quite noteworthy. In other properties also, the rubber product which was compounded as herein described, compared will with the commercial product.
  • the size and relative sizes of the various basic components of an apparatus according to the invention are as follows:
  • the reaction tube, 2 inches in diameter, containing the corebreaker will be about 60 inches long, the corebreaker will be about 34 inches long and will have an overall diameter of about 2 inches, and when tapered at the tapered end, will have a diameter of about 1 /2 inches.
  • the spiral on the corebreaker will have a 2 inch pitch and the space between successive ridges along the corebreaker will be about 1 /2 inches.
  • the hydrocarbon feed tube will measure about a A inch internal diameter and a inch outer diameter. It will be seen that the order of sizes are selected for effecting with optimum control the flow of hydrocarbon and heat carrier gas to either desired results by achieving flow rates herein set forth.
  • a process for the production of carbon black which comprises cracking a hydrocarbon under carbon black producing conditions of temperature, pressure, and flow rate by flowing a hot, relatively inert gas in turbulent flow along a curved path peripherally surrounding a place of impingement of said hydrocarbon and said hot, relatively inert gas in a carbon black producing zone, said path being at the outer peripheral boundary of said zone, and in an outwardly direction radially conveying said hydrocarbon to said path and there distributing said hydrocarbon into said hot, relatively inert gas in said zone whereby superfast transverse dispersion of said hydrocarbon in and across the turbulent, relatively inert gas stream is obtained in said path.
  • a process for producing carbon black which comprises introducing a relatively inert, preheated gas substantially tangentially into one end of a cylindrical reaction zone, also introducing into said zone axially at said end of said zone a hydrocarbon to be converted to carbon black, immediately radially distributing said hydrocarbon in an outwardly direction at a right angle to the axis of said reaction zone into said tangentially introduced hot gas so as to cause it to impinge with the tangentially introduced hot gas, thus obtaining superfast mixing by flowing said hydrocarbon with the hot gas flowing in turbulent flow along a curved path, passing the admixture thus obtained through said zone to its other end, at said other end quenching the reacted mixture, and recovering carbon black therefrom.
  • Apparatus for producing carbon black which comprises an elongated, substantially cylindrical reaction zone, means for tangentially introducing a hot, relatively inert gas into said Zone at one end thereof, means for introducing axially a hydrocarbon feed into said end of said zone, means in the said end of said zone placed transversely in said zone to the axially introduced hydrocarbon and extending substantially but incompletely to the outer peripheral boundary of said Zone, so that said hydrocarbon impinges thereagainst and is thus radially distributed there across into said hot gas flowing in turbulent flow along a curved path past the peripheral edge of said means, and means at the other end of said zone for recovering carbon black.
  • Apparatus according to claim 6 wherein the means for tangentially introducing said hot, relatively inert gas comprises a gas velocity increasing restriction disposed substantially at the place of entry of said gas into said zone.
  • a process for producing carbon black which comprises introducing into one end of a reaction zone and tangentially rotating in said zone a hot, relatively inert gas, passing said rotating gas through a constriction in said zone while passing it from one end of said zone to the other end thereof and introducing a hydrocarbon feed into said gas substantially as it passes through said constriction, thus obtaining turbulent, transverse superfast mixing of said feed and said gas.
  • a process for producing carbon black which comprises feeding a hot, relatively inert gas low in carbon dioxide and water into a carbon black producing Zone, cracking a hydrocarbon under carbon black producing conditions of temperature, pressure, and flow rate by flowing said hot, relatively inert gas flowing in turbulent flow along a curved path peripherally surrounding a place of impingement of said hydrocarbon and said hot, relatively inert gas in said carbon black producing zone, said path being at the outer peripheral boundary of said zone and in an outwardly direction radially conveying said hydrocarbon to said path and there distributing said hydrocarbon into said hot, relatively inert gas in said zone, whereby superfast transversed dispersion of said hydrocarbon across the turbulent, relatively inert gas stream is obtained.
  • a process for the production of carbon black which comprises bringing together under carbon black producing conditions a hydrocarbon and a hot, relatively inert gas by flowing said gas in a carbon black producing zone in a tangential curved rotating path peripherally surrounding said hydrocarbon as it is introduced into said zone, and immediately distributing said hydrocarbon into said gas flowing in a curved rotating path by flowing said hydrocarbon abruptly in an outwardly direction radially into said gas flowing in a curved rotating path.
  • a process for the production of carbon black which comprises bringing together under carbon black producing conditions, a hydrocarbon and a hot, relatively inert gas by flowing said gas in a carbon black producing zone in a tangential curved rotating path peripherally surrounding said hydrocarbon as it is introduced into said zone, passing said rotating gas through a constriction in said zone while passing it from one end of said zone to the other end thereof, and immediately distributing said hydrocarbon into said gas flowing in a curved rotating path by flowing said hydrocarbon abruptly in an outwardly direction radially into said gas flowing in a curved rotating path past said constriction.
  • a process for the production of a carbon black which comprises introducing into an end of a reaction zone and tangentially rotating therein a hot, relatively inert gas, passing said gas from said end of said zone toward the other end thereof, while passing said gas toward the other end of said zone passing the same through an annular section defined by a substantially circular obstruction disposed substantially at a right angle to the axis of said zone, introducing a hydrocarbon feed into said an end of said zone and causing it to impinge against said obstruction thereby distributing said hydrocarbon radially outwardly to the edge of said obstruction and otf from said edge and sheared into the gas passing into said annular section, thus obtaining turbulent, transverse superfast mixing of said feed and said gas, and recovering carbon black from the resulting admixture at the other end of said zone.
  • a process for producing carbon black which comprises introducing into one end of a reaction zone and tangentially rotating in said zone a hot, relatively inert gas, passing said rotating gas through a constriction in said zone while passing it from one end of said zone to the other end thereof and introducing a hydrocarbon feed radially into said gas substantially as it passesthrough said constriction, thus obtaining turbulent, transverse supertast mixing of said feed and said gas.

Description

Oct. 6, 1964 F. E. FREY 3,151,942
CARBON BLACK PROCESS AND APPARATUS Original Filed June 6, i958 s Sheets-Sheet 1 4 3 HYDROCARBON a 5 SUPERHEATER/ @\CERAMIC PLATE REACTOR INERT 1 9 GAS PREHEATER s .INERT 1.
" FIG.
SEPARATOR" "-8 l0 CARBON BLACK SMOKE TO COOLER HYDROCARBQN AND SEPARATOR POINT OF MAXIMUM MIXING RATE IN 0 CURV ED T UBE HYDROCARBON INERT A GAS A FIG. 2
INVENTOR. F.E. FREY Oct. 6, 1964 F. E. FREY CARBON BLACK PROCESS AND APPARATUS Original Filed June 6, 1958 3 Sheets-Sheet 2 EL 20mm UOmo I F.E FREY ATTORNEYS H zommsomnr um 6 zommfiomgr H on 2.
Oct. 6, 1964 F. E. FREY CARBON BLACK PROCESS AND APPARATUS 3 Sheets-Sheet 3 Original Filed June 6, 1958 QumE ZOmm vmT mwh INVENTOR. -F.E. FREY A TTOR/VEVS United States Patent 3,151,942 CARBQN SLACK PROESS AND APPARATUS redericl-r E. Frey, Bartlesville, Gide assignor to Phillips Petroleum Company, a corporation ct Delaware Grig'inal application dune d, 1958, Ser. No, 746,454, new Patent No. 3,015,543, dated Jan. 2, 1962. Divided and this application Feb. 253, 196i, Ser. No. 90,557
13 tliairns. (62, 23-29534) This is a divisional application of Serial Number 740,- 454, filed June 6, 1958, now US. Patent No. 3,015,543, issued .lanuary 2, 1962.
This invention relates to the production of carbon black. in one of its aspects, the invention provides a process for the production of carbon black wherein an organic compound such as a hydrocarbon which can be decomposed or cracked to produce carbon black is flowed into a reac tion zone into a hot, relatively inert gas flowing, in a preferred embodiment of the invention, in turbulent flow along a curved path whereby superfast transverse dispersion of hydrocarbon across the turbulent, relatively inert gas stream is obtained. In another of its aspects, the invention relates to a process which comprises immediately radially distributing in an outwardly direction into a hot, relatively inert gas flowing in turbulent flow in a curved path, a hydrocarbon to be converted to carbon black. In a further aspect of the invention, it relates to producing a hot, relatively inert gas for use as herein described by passing an oxygen-containing gas such as air, air enriched with oxygen, oxygen, and/ or carbon monoxide through a preheated coke bed at a temperature sufiicient to produce a gas relatively low in carbon dioxide and water as compared with ordinary combustion gases utilized in carbon black producing operations. In another of its aspects, the invention relates to the execution of the process in an apparatus wherein "there is provided a substantially cylindrical combustion chamber and appended annulus, adapted to generate and to flow through the annulus a hot combustion gas, a reaction chamber disposed Within said combustion chamber and forming said annulus therewith, a corebuster substantially concentrically disposed in one portion of said reaction chamber, means for introducing a hot gas through a second annulus formed between said reaction chamber and said corebuster, means for introducing a hydrocarbon to be converted to carbon black into said reaction chamber substantially at the place along its length at which the corebuster terminates therein and means for removing gaseous decomposition products from said reaction chamber. In another of its aspects, the invention relates to producing carbon black of small, ultimate particle size by introducing into a stream of hot gas, low in its content of the normal products of combustion, which ar carbon dioxide and water, a hydrocarbon which will crack to produce carbon black at a very high velocity of turbulent flow, high temperature, and short reaction time, thus producing a high yield of carbon black of small, ultimate particle size and having strong reinforcing properties in rubber. la a further aspect of the invention, it relates to an apparatus for producing carbon black which comprises an elongated, substantially cylindrical reaction zone, means for tangentially introducing a hot, relatively inert gas into said zone at one end thereof, means for introducing axially a hydrocarbon feed into said end of said zone, means in the end of said zone placed transversely to the axially introduced hydrocarbon so that said hydrocarbon impinges thereagainst and is thus radially distributed into said hot gas flowing in turbulent flow along a curved path, and means at the other end of said zone for recovering carbon black.
It is old to subject a hydrocarbon to direct heating by heat exchange, whereby carbon black is produced as in the Thermatonic process. in this process, hydrocarbon is passed through passageways in a preheated ceramic bed whereby heat is abstracted from the bed and carbon smoke produced in the stream as it passes therethrough. The rate of cracking is limited by the formation of a cooled surface layer on the ceramic through which heat passes from the subsurface ceramic by slow conduction to the stream. This can produce a black in high yield, approaching percent of the carbon in the stream, but its particle size is rather large and its reinforcing power in rubber is low, producing a tensile strength of 1,000 pounds per square inch more or less when blending it in a typical concentration of 35 percent by weight.
it is also old to admix a hydrocarbon at high velocity with combustion products of hydrocarbon and air or oxygen, whereby carbon smoke is produced. Substantial concentrations of carbon dioxide, water, or both, which are present in such gas, react with carbon and its precursors to produce carbon monoxide at the expense of carbon black yield.
The black made at high velocities has high reinforcing properties, producing 4,000 pounds per square inch tensile strength in rubber, more or less; can have a small ultimate particle size, and is of a constitution such that in the compounded rubber high stress is shown at a moderate amount of stretching.
It has now been found that a carbon black of improved properties as set forth and described herein can be prepared employing high velocities of flow in excess of approximately 20 feet per second, preferably in excess of 45 feet per second, of a mixture of heat-carrying, relatively inert gas and hydrocarbon vapor, the gas being mixed with the hydrocarbon vapor by introducing the hydrocarbon vapor into a spirally flowing turbulent mass of said gas in a reaction zone of fairly small diameter. In the reaction zone the intermixing is essentially immediately accomplished and the residence time in the zone can be sharply limited, thus yielding an efiicient, economical,
conversion factor modus operandi for producing carbon black.
Certain designs, construction, and operations which in one manner or another, as described herein, have also been provided according to the invention.
An object of this invention is to provide a process for the production of carbon black. Another object of this invention is to provide an apparatus for the production of carbon black. It is an object of this invention to provide a process and apparatus for the production of carbon black in high yield and of small, ultimate particle size. It is another object of this invention to provide a carbon black having strong reinforcing properties in rubber.
Other aspects, objects, and the several advantages of the invention are apparent from this disclosure, the drawings, and the appended claims.
According to the present invention, there are provided a process and apparatus for the production of carbon black e3 which comprises cracking an organic compound or hydrocarbon which yields carbon black under carbon black producing conditions of temperature, pressure, and flow rate by flowing the hydrocarbon, preferably as a vapor, into a hot, relatively inert gas flowing in turbulent flow along a curved path whereby superfast transverse dispersion, as herein defined, of hydrocarbon or compound across the turbulent, relatively inert gas stream is obtained. The rate of flow of gas and vapor mixture is at least about 20 feet per second.
Further, according to the present invention, a gas low in the usual products of combustion such as carbon dioxide and water is used as the relatively inert gas stream.
In one of its forms, an apparatus according to the present invention consists of a series of concentrically disposed elements, a cylindrical combustion zone having an annulus appended thereto, a reaction tube within said zone and forming said annulus, a corebuster extending throughout a portion of said reaction tube, means for regulating the heat transmitted from said combustion zone and annulus to the corebuster within said reaction tube and means for introducing a charge to be cracked to carbon black through said corebuster into the reaction zone within said reaction tube and means for collecting carbon black produced in said reaction tube.
While it is preferred, as above noted, to provide for means to control the temperature of the feed to be fed through the corebuster, it is within the scope of the invention to so design the relative sizes of apparatus elements that the hydrocarbon or other feed will reach vapor phase when this is desired and a desired temperature just as it leavm the corebuster. In such event, means for cooling or otherwise adjusting the temperature in the corebuster can be dispensed with.
The present invention produces a new result over the prior art in that there results a very high yield of a carbon which imparts high tensile strength to rubber and, while maintaining high tensile strength, permits production of a rubber product exhibiting moderate stress at a moderate stretch.
The essential features of the process of the invention are: (1) The use of heated, relatively inert gas, nitrogen, hydrogen, carbon monoxide or their mixtures, with little or no carbon dioxide or water, flowing in a turbulent spiral flow, (2) rapidly admixing hydrocarbon with this so-flowing preheated gas using a passageway of small cross section whereby linear velocities of at least 20 feet per second and preferably, at least 45 feet per second, in the gas are imposed to effect thermal cracking to carbon black very rapidly, and (3) effecting the reaction at an optimum temperature within the ranges 2,300 F. to 3,500 F. in a reaction time of under 0.1 second.
Embodiments and variations of embodiments of this invention are given in FIGURES 1 through 12 which illustrate diagrammatically or schematically various arrangements in which one or more of the several concepts of the invention can be embodied. FIGURES 9 and 10 are, respectively, vertical cross sections of an actual apparatus taken in a plane passing through the axis and a plane at right angles thereto. FIGURE 11 is a modification of the apparatus as shown in FIGURES 9 and 10.
FIGURE 12 is a cross sectional view of a corebreaker adapted to be used in the'apparatus of FIGURE 9.
In FIGURE 1, which is a schematic showing of one embodiment of the invention, 1 is a conventional preheating furnace in which the inert gas, nitrogen in this embodiment, is preheated. The preheater can be omitted if desired and the gas can be available already sufiiciently hot for its intended use. Superheater 2 is operated by indirect heat exchange through a ceramic wall. In a variation, it can be operated by electric heating, by electric discharge or resistors. A small amount of oxygen, preferably preheated, can be added to the hydrocarbon feed in the reactor to boost the temperature slightly when the reactor temperature is already in a high temperature range.
In the modification being described, there is provided, at the beginning of reaction zone 3, a constriction producing the required velocity of inert gas of at least 20 feet per second.
Variations of zones 1 and 2 include a pebble heater to produce hot inert gas, a blow-and-run refractory heating plant using two or more units operating on staggered cycles of combustion heating alternating with superheating of the inert gas. Blending exit inert gas on a controlled varying ratio can be used to hold downward drift of superheat temperature in a suitable range to control efficiency and black quality.
In an important combination of operations according to this invention, by feeding oxygen or preheated air or air enriched with oxygen to a preheated coke bed operating above 2,600 F., nitrogen and carbon monoxide are formed while the formation of much deleterious carbon dioxide is avoided. Preheated carbon monoxide in addition can be introduced through the bed.
Reaction zone 3 is substantially vertically disposed. The heated, relatively inert gases are introduced substantially tangentially in a manner to create along the inner wall of zone 3 a downwardly moving blanket of turbulent gases flowing in a curved path. Hydrocarbon vapor to be converted, in this embodiment, benzene heated to about 2,500 F., is introduced substantially axially at the top of reaction zone 3 through pipe 4. The relative sizes of the reaction pipe and volumes of gases at the operating temperature are chosen to maintain not only the turbulent curved path flow of the relatively inert gases but also to cause the introduced hydrocarbon to be immediately (superfast) admixed therewith. To this end, the relative velocities of the relatively inert gas and hydrocarbon are adjusted to allow the hydrocarbon to pick up sufficient angular velocity from the relatively inert gas to be impelled thereinto by centrifugal force, the turbulent flow of said relatively inert gas then immediately causing the desired mixing to take place with great uniformity. As an especial feature of the invention, shown also in FIGURE 1A, the hydrocarbon can be made to flow over a ceramic plate 5, thus causing the hydrocarbon to be moving in a film which is immediately sheared into the turbulently flowing, hot, relatively inert gas. By pointing the constricted portion of tube 2, slightly downwardly increased shear of the gases can be obtained. The length of the reactor, its diameter, etc., are so proportioned that the reacted hydrocarbon streams can be immediately cooled to below 1,200 F., preferably 800 F., at the end of the desired residence time which, in this embodiment, is 0.1 second. A water spray 6 is provided in tube portion '7 at the point at which the reacted hydrocarbon is cooled sufficiently by itself due to endotiermic reaction and radiant and convection heat loss, so that undesirable reaction between the carbon black and the water spray will not occur. In separator 8, which is conventional, gaseous products are removed at 9 and carbon black is recovered at 16. The relatively inert gas used in this embodiment is essentially nitrogen and it can be recovered from the separator and can be returned at least in part to preheater 1.
Other embodiments of reaction zone 3 are shown in FIGURES 2 through 9. FIGURE 2 shows admixing the hydrocarbon with the relatively inert gas at the point of maximum mixing rate in a curved tube. Thus, the hydrocarbon is introduced into tube 20 by pipe 21. The curved nature of tube 20 causes the relatively inert gas to spiral. In FIGURE 3 the spiralling, hot, relatively inert gas intro duced at 25 is passed through a constricted passageway 26 together with hydrocarbon axially introduced through pipe 27. FIGURE 4 shows both relatively inert gas and hydrocarbon entering axially at high velocity. The relatively inert gas is fed to the reactor through pipes 30 which are oriented to cause said gas to move in a spiral path in turbulent flow. Hydrocarbon is introduced at 31. FIG- URE 5 shows the hydrocarbon entering the reactor axially and the relatively inert gas entering radially at high velo city. Thus, the relatively inert gas is pumped in through pipe 35 and the hydrocarbon is pumped in through pipe 36. There are two or more radial jets 35 to give the desired high velocity. FIGURE 6 shows the relatively inert gas entering the reactor axially at 40 with the hydrocarbon pumped in radially at 41. In this modification, which is used to illustrate the point that the hydrocarbon vapor and inert gas flows can be interchanged, the hydrocarbon stream flows in the highly turbulent curved flow and the relatively inert gas is caused to be admixed therewith. Since the hot, relatively inert gases are in considerable excess over the hydrocarbon in the now preferred operations, better mixing is obtained with the other embodiments of the invention in which the gas is on the periphery of the hydrocarbon being admixed therewith. FIGURE 7 shows opposing jets of relatively inert gas and hydrocarbon entering the reactor, resulting in fast mixing. The hydrocarbon and the relatively inert gas enter mixing zone 45 through pipes 46 and 47, respectively. Since the inert gas is in considerable excess, the gas will govern the overall flow which will be in an essential spiral manner in tube 43. Substantially all of the mixing takes place in zone 45, however. Any slight additional mixing is caused by the spiralling gas, as earlier described. FIGURE 8 shows opposing jets of inert gas and hydrocarbon and a stream of inert gas entering the reactor axially. Thus, the gas enters through pipes 59 and 51 while hydrocarbon is introduced through pipe 52. Mixin immediately occurs in zone 53. The spiralling motion is again obtained due to the excess of gas entering at 51 over the hydrocarbon.
FIGURE 9 is a diagrammatic drawing of the reactor used to obtain the data of this invention which are shown in Table 1 below. This embodiment is similar to that shown schematically in FIGURE 4.
Referring now to FIGURES 9 and 10, an axially disposed cylindrical section has a lining 111 of highly refractory sillimanite. Between this refractory liner 111 and a cylindrical steel shell 113 is a layer of insulation 112. Combustion section 114, coaxial with liner 111, is also lined with lining material 111. In combustion zone 114 are arranged inlets 123, which are so disposed that gas can be passed therethrough and into combustion zone 114 in a direction tangential to its cylindrical wall. Most of the tangentially introduced gas is burned within tunnels 126. Cooling assembly 118 downstream from the cylindrical section and adjacent thereto consists of water jacket (not shown) and water spray 134. A combustion mixture of methane and oxygen or oxygen mixed with steam or air is charged to tangential burners 123. Tangentially introduced gas is burned in tunnels 126, the combustion gases thus produced traveling helically within combustion zone 114 and continuing along annular space 119 formed by the inner wall of liner 111 of the cylindrical section and outer wall 115 of reactor tube 116. A seal 116a is provided between the outer wall of tube 116 at its left end, as hown, and liner 111. Wall or surface 115 is provided with a helical protrusion 115a which serves to maintain centered outside wall 115 within the apparatus and also serves to force the gases to move spirally throughout the entire length of annulus 119. The annular space between the reactor tube 116 and the cylindrical section is of uniform width approximately 1% inches maximum. The burning taking place in tunnels 126 serves as a source of heat. Sufficient heat is provided to heat the outside wall 115 of reactor tube 116 to a temperature of 2,875 F. The gas is passed into cooling assembly 118 (described previously) and rapidly quenched to a temperature below 1,200" F. in both indirect and direct heat exchange relation with water.
The inside wall at 117 of reactor tube 116 becomes heated to a temperature of 2,750 F. by the hot gases flowing in annular space 119. Nitrogen gas preheated to 1,200 F. (preheater not shown) is introduced through pipe 121'} and enters annular space 121 formed by corebreaker 122 placed inside reactor tube 116. This annular space 121 is inch in width. The linear velocity of the nitrogen gas in annular space 121 is at least feet per second. The nitrogen gas becomes heated to a temperature of 2,600 F. by the hot inside wall 117 of reactor tube 116. The outside wall at 124 of corebreaker 122 reaches a temperature of 2,700 F. The corebreaker 122 is positioned in reactor tube 116 to assist in obtaining a high ratio of heat transmitting surface to volume in a tube of large diameter and high throughput. The reactor tube is made of silicon carbide for high heat transfer. The 1% inch corebreaker 122 is made of alumina, but might, if desired, be made of other refractory material, such as for example fused quartz or illimanite. The corebreaker, placed centrally in the reactor tube, reduces the effective cross sectional area of the reactor tube. The corebreaker outside surface 122 is provided with spiral ridge 122a which helps to create a spiral motion of the preheated nitrogen gas. Water is circulated in tube 127 positioned in corebreaker 122. The preheated hydrocarbon vapor feed at 250 F. enters tube 123 and is sprayed by orifice 12% into reaction chamber 116. The efiiuent temperature at 131"; in the reaction chamber 116 is 2,000 F. The product enters a cooling assembly 131 which consists of water jacket 132 and a water spray (not shown). The water spray, if used, is located sufliciently downstream to allow cooling of the product by water jacket 132 to a temperature low enough to avoid reaction of water with carbon. An atmospheric cooling pipe can be used in place of a water spray. Such a pipe can also be used with a water jacket. The black is, in any event, cooled preferably to a temperature at which it will not react with the water spray when such a spray is used, but precooling can be small if the volume of spray water is sufiiciently large to quench to below reacting temperatures. A water spray is preferred provided the black is cooled to such a nonreacting temperature. Any usual means not shown for separating solids from gases can be applied to the downstream end of pipe 133 to separate the carbon black in the course of its production.
It is seen that in the operation of the embodiment of FEGURE 9, both the relatively inert gas, nitrogen, and the hydrocarbon vapor enter the reactor 116 axially at high velocity. 1n the runs made, there was approximately 100 percent conversion of benzene to carbon black.
The temperature within the reaction chamber 116 can be varied within wide limits, for example, within the range of 2,060 to 3,300 F. or higher. The upper limit depends on the temperature the refractory material will stand. Better yields of excellent quality carbon black resulted from operating periods when temperatures were of the order of 2,300 to 2,600 F. in reactor 115. The reaction time was less than 0.1 second.
The reactor 116 was 2 inches in diameter and 18 inches long.
The temperatures during the runs were as follows.
Location: Temperature, F. Gutside wail reactor tube 115 2,875 inside wall reactor tube 117 2,750 Corebreaker wall 124 2,700 Nitrogen preheat entering annulus 119 1,200 Feed preheat 128 250 Efduent temperature 134 2,000
Data on the runs made with the apparatus of FiGURE 9 are given in Table I.
TABLE I Feed (250 F.) Initial Velocities Res. N c.f.h Photelo- N Sur- Sample Time, at meter Nigromface 0. Milli- 1,200 F. Hydro- HG, gal. Oil Reactor, (CHO1 eter area, seconds carbon per hr. N c.i.h. Tube, ft./sec. M /g ft./sec.
Referring now to FIGURE 11, there is shown an embodiment of the invention in which the annular, hot, relatively inert gas is fed into the reaction section 216 substantially at the introduction of the feed at 229. This is accomplished in the instant embodiment by providing at least one set of holes or apertures 300 through which the hot gas is directed towards the axially introduced feed. Although not necessary to each embodiment of this type of construction, in the embodiment of FIGURE 11, the annular space 221 is terminated at its reaction section end by a closure 301. This permits passing all of the annularly introduced gases through the holes 300 as indicated by the arrows.
Referring now to FIGURE 12, which shows a corebreaker adapted to be used in the apparatus of FIGURE 9, 400 denotes the corebreaker body having spiral 401 on its outside surface. Water or other cooling medium is circulated through the corebreaker by inlet 402 and outlet 403. At the discharge end of hydrocarbon feed tube 404, namely at 425 the cooling medium circulates around the tube to prevent its temperature from reaching a value at which undesired reaction of the hydrocarbon will take place. Over the remainder of tube 404 insulation, such as Alfrax packing, is provided as shown at 405. This material is preferably cast into place after insertion of the cooling medium pipes and surrounds said pipes. At the discharge end of the hydrocarbon feed pipe, the cooling medium passageway is surrounded by Fiberfrax packing or similar material. The corebreaker is tapered in this modification .to assist in the acceleration of the inert gases which are passed to the reaction section 115 of FIGURE 9 by annulus 121 of said figure. The corebreaker is made in this instance of alumina. Although in FIGURE 9 the inert gas is shown introduced parallel to the axis of the apparatus, it is within the scope of the invention to introduce tially or transversely to the tapered or inlet end of the corebreaker.
To illustrate the quality of the carbon black made as disclosed herein and to compare its properties with those of other carbon blacks, batches of rubber compound were prepared according to the compounding formula, as follows:
Parts by weight Butadiene/styrene rubber 100 Carbon black 40 Zinc om'de 3 BRT #7 6 Sulfur 1.75 Santocure 0.8
1 The butadiene-styrene rubber is a 71-29 butadienelstyreii e copolymer prepared by emulsion polymerization at 122 Table II gives properties imparted to a 122 F. rubber by these thermal blacks at 30 minutes cure at 307 F. and oven agent 24'hours at 212 F.
These thermal blacks, made in a two-inch diameter by 18-inch reactor using benzene or n-hexane feedstocks, ex-
hibited relatively high surface area and low oil absorption indicating that low structure blacks of relatively fine particle size were produced. Carbon black made from benzene possessed a finer particle size and gave better abrasion resistance and much better electrical conductivity than the n-hexane black although the black made from hexane was an acceptable product of the invention. These thermal blacks gave higher modulus and appreciably better abrasion resistance than P-33 (a commercial the preheated inert or carrier gas substantially tangen-' fine thermal black).
TABLE 11 Properties Imparted to 122 F. Rubber by Thermal Carbon Blacks 30 Minutes Cure at 307 F.
Ben- Com- 200 F. Extrusion at Nitrogen Oil zene pres- 300% Elon Maxi- Flex Shore Abra- Corn- 250 F. Black surface pH absorpere sion mod- Tengation, mum liie, hardsion pounded,
area, tion, tract, set, ulus, sile pertensile, M. ness loss, MS 1% sq. m./g. cc./g. perperp.s.i. cent p.s.i. g. In./ Rating cent cent min.
(Benzene) 87.6 8. 0 0.96 0. 08 24. 3 700 2, 760 660 1, 140 5. 5 51 13. 18 27 23. 4 9 (n-Hexane) 59. 0 8. 2 0. 62 0. 14 27. 2 475 2, 570 740 820 7. 3 16 17. 93 24 26. 6 9- A well' known commercial furnace black. 13.6 7. 6 0.56 1 64 28. 5 275 1, 425 805 250 2. 6 42 55.90 20 21. 9 8+ Oven Aged 24 Hours at 212 F.
(B enzene) 1, 360 2, 780 460 1. 7 9. 67 (n-Hexane) 960 2, 480 1. 0 55. 5 14. 39 A well known commercial furnace black. 480 650 415 0.3 52
From Table II, it will be noted that the carbon black of the process of the present invention produces in a cured rubber product, as above described, certain highly desirably properties. Among these are very greatly increased flex life and greatly decreased abrasion loss over a well known commercially available carbon black made by a substantially conventional furnace operation. Another notable great improvement has been made in tensile strength. Also, 300 percent modulus has been very greatly increased. The nitrogen surface area, oil absorption, and benzene extract results are also quite noteworthy. In other properties also, the rubber product which was compounded as herein described, compared will with the commercial product.
Generally, although the invention is not to be limited thereto, the size and relative sizes of the various basic components of an apparatus according to the invention are as follows: The reaction tube, 2 inches in diameter, containing the corebreaker will be about 60 inches long, the corebreaker will be about 34 inches long and will have an overall diameter of about 2 inches, and when tapered at the tapered end, will have a diameter of about 1 /2 inches. The spiral on the corebreaker will have a 2 inch pitch and the space between successive ridges along the corebreaker will be about 1 /2 inches. The hydrocarbon feed tube will measure about a A inch internal diameter and a inch outer diameter. It will be seen that the order of sizes are selected for effecting with optimum control the flow of hydrocarbon and heat carrier gas to either desired results by achieving flow rates herein set forth.
Reasonable variation and modification are possible within the scope of the foregoing disclosure, the drawings, and the appended claims to the invention the essence of which is that there have been provided a process and apparatus for producing carbon black from certain organic compounds, preferably hydrocarbons, by flowing such a compound into a hot, relatively inert gas flowing in turbulent flow along a curved path whereby superfast transverse dispersion of hydrocarbon across the turbulent, relatively inert gas stream is obtained, in an embodiment utilizing a gas low in carbon dioxide and water as said inert gas, substantially as described.
I claim:
1. A process for the production of carbon black which comprises cracking a hydrocarbon under carbon black producing conditions of temperature, pressure, and flow rate by flowing a hot, relatively inert gas in turbulent flow along a curved path peripherally surrounding a place of impingement of said hydrocarbon and said hot, relatively inert gas in a carbon black producing zone, said path being at the outer peripheral boundary of said zone, and in an outwardly direction radially conveying said hydrocarbon to said path and there distributing said hydrocarbon into said hot, relatively inert gas in said zone whereby superfast transverse dispersion of said hydrocarbon in and across the turbulent, relatively inert gas stream is obtained in said path.
2. A process according to claim 1 wherein the flow of mixing hydrocarbon and gas is substantially entirely unobstructed, the inert gas is nitrogen, and the rate of flow of the mixture of hydrocarbon and inert gas is at least about 20 feet per second.
3. A process according to claim 1 wherein the reac tion is efiected during a residence time of less than onetenth second and at a temperature in the range 2300- 3500 F.
4. A process for producing carbon black which comprises introducing a relatively inert, preheated gas substantially tangentially into one end of a cylindrical reaction zone, also introducing into said zone axially at said end of said zone a hydrocarbon to be converted to carbon black, immediately radially distributing said hydrocarbon in an outwardly direction at a right angle to the axis of said reaction zone into said tangentially introduced hot gas so as to cause it to impinge with the tangentially introduced hot gas, thus obtaining superfast mixing by flowing said hydrocarbon with the hot gas flowing in turbulent flow along a curved path, passing the admixture thus obtained through said zone to its other end, at said other end quenching the reacted mixture, and recovering carbon black therefrom.
5. A process according to claim 4 wherein the preheated gas is passed through a zone adapted to increase its velocity immediately preceding its introduction into said reaction zone.
6. Apparatus for producing carbon black which comprises an elongated, substantially cylindrical reaction zone, means for tangentially introducing a hot, relatively inert gas into said Zone at one end thereof, means for introducing axially a hydrocarbon feed into said end of said zone, means in the said end of said zone placed transversely in said zone to the axially introduced hydrocarbon and extending substantially but incompletely to the outer peripheral boundary of said Zone, so that said hydrocarbon impinges thereagainst and is thus radially distributed there across into said hot gas flowing in turbulent flow along a curved path past the peripheral edge of said means, and means at the other end of said zone for recovering carbon black.
7. Apparatus according to claim 6 wherein the means for tangentially introducing said hot, relatively inert gas comprises a gas velocity increasing restriction disposed substantially at the place of entry of said gas into said zone.
8. A process for producing carbon black which comprises introducing into one end of a reaction zone and tangentially rotating in said zone a hot, relatively inert gas, passing said rotating gas through a constriction in said zone while passing it from one end of said zone to the other end thereof and introducing a hydrocarbon feed into said gas substantially as it passes through said constriction, thus obtaining turbulent, transverse superfast mixing of said feed and said gas.
9. A process for producing carbon black which comprises feeding a hot, relatively inert gas low in carbon dioxide and water into a carbon black producing Zone, cracking a hydrocarbon under carbon black producing conditions of temperature, pressure, and flow rate by flowing said hot, relatively inert gas flowing in turbulent flow along a curved path peripherally surrounding a place of impingement of said hydrocarbon and said hot, relatively inert gas in said carbon black producing zone, said path being at the outer peripheral boundary of said zone and in an outwardly direction radially conveying said hydrocarbon to said path and there distributing said hydrocarbon into said hot, relatively inert gas in said zone, whereby superfast transversed dispersion of said hydrocarbon across the turbulent, relatively inert gas stream is obtained.
10. A process for the production of carbon black which comprises bringing together under carbon black producing conditions a hydrocarbon and a hot, relatively inert gas by flowing said gas in a carbon black producing zone in a tangential curved rotating path peripherally surrounding said hydrocarbon as it is introduced into said zone, and immediately distributing said hydrocarbon into said gas flowing in a curved rotating path by flowing said hydrocarbon abruptly in an outwardly direction radially into said gas flowing in a curved rotating path.
11. A process for the production of carbon black which comprises bringing together under carbon black producing conditions, a hydrocarbon and a hot, relatively inert gas by flowing said gas in a carbon black producing zone in a tangential curved rotating path peripherally surrounding said hydrocarbon as it is introduced into said zone, passing said rotating gas through a constriction in said zone while passing it from one end of said zone to the other end thereof, and immediately distributing said hydrocarbon into said gas flowing in a curved rotating path by flowing said hydrocarbon abruptly in an outwardly direction radially into said gas flowing in a curved rotating path past said constriction.
12. A process for the production of a carbon black which comprises introducing into an end of a reaction zone and tangentially rotating therein a hot, relatively inert gas, passing said gas from said end of said zone toward the other end thereof, while passing said gas toward the other end of said zone passing the same through an annular section defined by a substantially circular obstruction disposed substantially at a right angle to the axis of said zone, introducing a hydrocarbon feed into said an end of said zone and causing it to impinge against said obstruction thereby distributing said hydrocarbon radially outwardly to the edge of said obstruction and otf from said edge and sheared into the gas passing into said annular section, thus obtaining turbulent, transverse superfast mixing of said feed and said gas, and recovering carbon black from the resulting admixture at the other end of said zone.
13. A process for producing carbon black which comprises introducing into one end of a reaction zone and tangentially rotating in said zone a hot, relatively inert gas, passing said rotating gas through a constriction in said zone while passing it from one end of said zone to the other end thereof and introducing a hydrocarbon feed radially into said gas substantially as it passesthrough said constriction, thus obtaining turbulent, transverse supertast mixing of said feed and said gas.
References Cited in the file of this patent UNITED STATES PATENTS 2,368,827 Hanson et a1. Feb. 6, 1945 2,773,744 Antonsen Dec. 11, 1956 2,864,673 Nannini Dec. 16, 1958 2,865,717 Krejci Dec. 23, 1958 2,915,371 Sweitzer Dec. 1, 1959 3,046,096 Heller et a1. July 24, 1962

Claims (1)

1. A PROCESS FOR THE PRODUCTION OF CARBON BLACK WHICH COMPRISES CRACKING A HYDROCARBON UNDER CARBON BLACK PRODUCING CONDITIONS OF TEMPERATURE, PRESSURE, AND FLOW RATE BY FLOWING A HOT, RELATIVELY INERT GAS IN TURBULENT FLOW ALONG A CURVED PATH PERIPHERALLY SURROUNDING A PLACE OF IMPINGEMENT OF SAID HYDROCARBON AND SAID HOT, RELATIVELY INERT GAS IN A CARBON BLACK PRODUCING ZONE, SAID PATH BEING AT THE OUTER PERIPHERAL BOUNDARY OF SAID ZONE, AND IN AN OUTWARDLY DIRECTION RADIALLY CONVEYING SAID HYDROCARBON TO SAID PATH AND THERE DISTRIBUTING SAID HYDROCARBON INTO SAID HOT, RELATIVELY INERT GAS IN SAID ZONE WHEREBY SUPERFAST TRANSVERSE DISPERSION OF SAID HYDROCARBON IN AND ACROSS THE TURBULENT, RELATIVELY INERT GAS STREAM IS OBTAINED IN SAID PATH.
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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2368827A (en) * 1941-04-21 1945-02-06 United Carbon Company Inc Apparatus for producing carbon black
US2773744A (en) * 1952-03-28 1956-12-11 Cabot Godfrey L Inc Continuous thermal process of making carbon black
US2864673A (en) * 1956-02-06 1958-12-16 Phillips Petroleum Co Carbon black furnace dual fluid injector
US2865717A (en) * 1956-05-07 1958-12-23 Phillips Petroleum Co Furnace carbon black process and apparatus
US2915371A (en) * 1955-06-10 1959-12-01 Columbian Company Carbon black process
US3046096A (en) * 1958-12-02 1962-07-24 Columbian Carbon Carbon black manufacture

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2368827A (en) * 1941-04-21 1945-02-06 United Carbon Company Inc Apparatus for producing carbon black
US2773744A (en) * 1952-03-28 1956-12-11 Cabot Godfrey L Inc Continuous thermal process of making carbon black
US2915371A (en) * 1955-06-10 1959-12-01 Columbian Company Carbon black process
US2864673A (en) * 1956-02-06 1958-12-16 Phillips Petroleum Co Carbon black furnace dual fluid injector
US2865717A (en) * 1956-05-07 1958-12-23 Phillips Petroleum Co Furnace carbon black process and apparatus
US3046096A (en) * 1958-12-02 1962-07-24 Columbian Carbon Carbon black manufacture

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