US3004822A - Method for utilizing detonation waves to effect chemical reactions - Google Patents

Method for utilizing detonation waves to effect chemical reactions Download PDF

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Publication number
US3004822A
US3004822A US712401A US71240158A US3004822A US 3004822 A US3004822 A US 3004822A US 712401 A US712401 A US 712401A US 71240158 A US71240158 A US 71240158A US 3004822 A US3004822 A US 3004822A
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Prior art keywords
detonation
reaction
gas
zone
barrel
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US712401A
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Richard M Poorman
George P Hawley
Herbert B Sargent
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Union Carbide Corp
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Union Carbide Corp
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Priority to BE575189A priority patent/BE575189A/fr
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    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21B—MANUFACTURE OF IRON OR STEEL
    • C21B13/00—Making spongy iron or liquid steel, by direct processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/28—Moving reactors, e.g. rotary drums
    • B01J19/285—Shaking or vibrating reactors; reactions under the influence of low-frequency vibrations or pulsations
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05B—SPRAYING APPARATUS; ATOMISING APPARATUS; NOZZLES
    • B05B7/00—Spraying apparatus for discharge of liquids or other fluent materials from two or more sources, e.g. of liquid and air, of powder and gas
    • B05B7/0006—Spraying by means of explosions
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/90—Carbides
    • C01B32/914—Carbides of single elements
    • C01B32/949—Tungsten or molybdenum carbides
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
    • C23C4/12—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the method of spraying
    • C23C4/126—Detonation spraying
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/80—Compositional purity
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/10—Reduction of greenhouse gas [GHG] emissions
    • Y02P10/134—Reduction of greenhouse gas [GHG] emissions by avoiding CO2, e.g. using hydrogen
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S423/00—Chemistry of inorganic compounds
    • Y10S423/09—Reaction techniques
    • Y10S423/11—High pressure

Definitions

  • detonation is meant a very rapid burning or other exothermic reaction in which the flame front moves through the unburned material at velocities higher than the velocity of sound in the unburned material, and therefore characterized as supersonic velocities.
  • Typical calculated velocities of sound at normal pressure are 1085 feet per second at 18 C. in a 50% oxygen-50% acetylene mixture, 1384 feet per second in the same mixture at 200 C. and 1122 feet per second at 18 C.
  • the rate of flame propagation is far greater in a detonation than in a deflagra tion, which is a burning or other exothermic reaction in which the velocity of flame propagation does not exceed the velocity of sound in the unburned material.
  • a deflagra tion which is a burning or other exothermic reaction in which the velocity of flame propagation does not exceed the velocity of sound in the unburned material.
  • the velocity of the flame front in gas detonations thus far investigated is from 1 to 4 kilometers per second (about 3,280 to 13,120 feet per second), as compared to, for instance, 50 feet per second for a typical deflagration.
  • a detonation wave Once a detonation wave has been established in a gaseous medium in a long tube, it travels at a constant velocity. However, except in the special case where the initiation is by a shock wave source, the detonation wave is not established immediately, but only after the flame has travelled some distance as a deflagration. The region through which the flame travels before its transition to detonation occurs will be called the predetonation region.
  • 2,714,563 is termed a detonation gun and comprises an elongated barrel having an open end, means for introducing a detonatable body of detonatable fluid into said barrel, means for providing powder material in said detonatable body of detonatable fluid in said barrel, means for controlling the supply of fluid fuel and oxidant of said detonatable fluid, and a mixing and ignition zone at the rear of the barrel including ignition means for igniting said detonatable fluid in said barrel.
  • the powdered material is carried into the barrel either through the fuel gas stream, oxidant stream, or by a separate stream which introduces the powdered material into the stream of detonatable fluid mixture which carries it into the barrel of the detonation gum
  • An improved detonation gun is disclosed and claimed in US. Patent No. 2,774,625. This improved detonation gun employs a powder injection tube projecting axially into the gun barrel to introduce the powder into the barrel downstream from the zone in which the detonation is established.
  • the powder is symmetrically disposed in the cross-section of the barrel and does not build-up deposits in one area of the wall as when introduced from the side of the barrel, and at the same time avoids fouling the mixing and ignition zone with particles as when introduced through that zone.
  • the above apparatus and associated processes have been used to produce coatings, to spheroidize particles, to clean or roughen surfaces, and to pulverize frangible material.
  • the temperature, gas velocity, ignition characteristics and composition of the products of a detonation wave are determined primarily by the composition of the detonatable material.
  • an acetylene-oxygen mixture When an acetylene-oxygen mixture is used, the highest flame velocity and temperature are attained at an oxygen/carbon atomic ratio of 1.0.
  • This mixture is carbon rich or oxygen deficient with relation to stoichiometric amounts forcomplete combustion to carbon dioxide and water. Therefore, detonation of this particular fuel-oxidant mixture results in an atmosphere that is slightly carburizing or reducing toward many substances. Also there is no appreciable free carbon in the combustion products allowing the walls of the ignition chamber and of the barrel to remain clean and free of carbon deposits. Furthermore the transition of the flame from the original deflagration to the desired detonation takes place rapidly and in a short distance thus producing a relatively small predetonation region.
  • the oxygen/ carbon atomic ratio of an acetylene-oxygen mixture should be reduced below 1.0. Under these conditions the transition of the flame from the deflagration to the detonation form may be delayed so much that the desired reaction conditions are not attained in the reaction zone. Also carbon and gummy materials from the incomplete combustion tend to deposit on the walls of the detonation chamber in the predetonation region of the barrel. Little or no deposit occurs downstream of the predetonation region because all material in this downstream region is pushed forward by the forces in the detonation wave. Deposits of carbonaceous material in the predetonation region of the barrel interfere with the operation and make frequent cleaning necessary. Moreover, if the reaction product is a coating, these solid deposits become detached from the wall and are deposited in the coating itself, seriously lowering the quality of the coating.
  • the oxygen/carbon atomic ratio should be increased above 1.0 for an oxygen-acetylene mixture.
  • the ignition characteristics of the mixture may not be as desired; that is, the predetonation region may be too large to enable proper reaction conditions to be obtained and gummy deposits may result.
  • composition of the detonation gas mixture is desirably varied to provide a method for readily oxidizing or carburizing metal or other materials in the detonation gun.
  • the material being treated in the reaction zone is not capable itself of sustaining a detonation.
  • the detonation wave must be propagated by the gases surrounding the reactant material being treated in the reaction zone.
  • the material being treated should preferably be a solid or liquid in order to obtain maximum amount of material in the reaction zone in a given time.
  • gaseous reactant materials can also be treated.
  • FIG. 1 is a schematic view of a detonation gun in which the method of the invention may be practiced
  • FIG. 2 is a diagrammatic viewof the device of FIG. 1; and 7 'FIG. 3 is a diagrammatic view of another device in which the invention may be practiced.
  • the method of this invention is carried out in a detonation gunhaving an elongated barrel.
  • the barrel has a length-.to-diameter ratio sufficiently high to permit the establishment and propagation of a detonation therein.
  • a mixing and ignition chamber directly and continuously connects with one end of the gun barrel and functions to mix and pass to the gun barrel the gases comprising the detonatable body, such as oxidant and fuel gases.
  • Conduitmeans and valves are provided to. introduce the gases into the ignition and mixing chamber.
  • Means are provided to introduce material to be acted upon by the detonation, such as comminuted solid material, into the fuel gas and oxidant gas mixture in the gun barrel.
  • Means are also provided in the 'mixing and ignition chamber to ignite the gas mixture therein and to establish the detonation in the gun barrel.
  • the oxidant-fuel mixture can 1 be varied. to give desireddetonation properties.
  • improved method ofoperation of the present invention comprises maintaining the oxidant gas-fuel gas mixture in the ignition and mixing chamber and in the portion of the barrel upstream of the entry for powder or other reactant so as to provide desired characteristics of ignition and detonation formation, and modifying the oxidant gas-fuel gas mixture in the downstream reactive portion of the barrel to the composition there desired by concurrently introducing an additional and separate quantity of reactive hydrocarbon, oxidant gas or other reactant into the reaction portionof the barrel.
  • an 'oxidant reaction gas such as oxygen
  • oxygen may be added to the detonatable gas mixture in the reaction zone to effect more oxidizing conditions during the combustion reaction; or, by the addition of a hydrocarbon fuel gas at that point, the combustion reaction maybe made more carburizing.
  • detonation gun D comprising an elongated barrel 10 having an open end 12 from which the products of the detonation and powders pass to the object to be coated or from which reaction products are removed. Cooling water circulating jacket 14 is pro vided around barrel 10 to, prevent overheating. Cooling a water is supplied to the annular space 16 between jacket 14 and barrel 10 through inlet means 18, and water passes from annular space 16 through outlet means 20.
  • Oxidant and fuel are supplied to port means 22 and 24, respectively, of mixing block 26 which is provided with poppet valves 28 for regulating the flow of such fluids at timed intervals. Mixing of the fuel and oxidant takes place in mixing and ignition zone or chamber 30 of mixing block 26 and the detonatable mixture is passed to barrel 1!? of the detonation gun' D. Mixing block 26 is also provided with purging gas inlet port means 36 and poppet valve means 38 for purging mixing chamber 30 and barrel 10 of gases in the intervals between each successive detonation and the introduction of the following detonatable charge into elongated barrel 10 of the detonation gun.
  • Means are provided in the walls of mixing chamber 30 for insertion of ignition means 42, such as a spark plug or the like, into the mixing chamberyand energizing lines 44 are also provided.
  • Reactant entry tube assembly 46 passes through the rear or breech end 48 of cooling water jacket 14 and the elongated barrel 10 and passes axially through the barrel to a point downstream of the zone (in the region of ignition means 42) where ignition occurs and downstream of the point where the establishment of the detonation phenomenon occurs.
  • the powder entry tube assembly 46 preferably comprises powder entry tube 50, cooling jacket 54 surrounding entry tube 50 over at least that portion of entry tube 50 which is positioned in the interior or barrel 10, cooling fluid irflet and outlet parts 56 and 58 respectively, and guide bracket means 60 for properly supporting entry tube 50 to prevent bending or breakage. Entry tube 50 is supplied'with reactant gas and powder by a line 62.
  • a suitable powder dispenser is employed for suspending the material in a gas stream in which it is carried into the barrel 10 of the detonation gun.
  • FIG. 2 shows the two gas concentration zones A and B capable of provision in accordance with the instant invention.
  • Zone A represents the reaction portion of the gun barrel where the material to be treated is injected. In this portion, the oxygen/fuel gas ratio is maintained at a value so as to provide the desired chemical action.
  • Zone B is the mixing, ignition and predetonation zone, wherein the oxygen/ fuel gas ratio is maintained at a value to provide-desired ignition and detonation promotion.
  • the oxygen-carbon atomic ratio in zone A can be maintained at a value different from that in zone B by introducing to zone A an oxidant or hydrocarbon.
  • This reactant gas is conveniently introduced through tube 59.
  • the reactant gas can act as the powder carrier gas or as a replacement for part of the powder carrier gas. This result may, however, be accomplished by other means such as a third auxiliary gas inlet either parallel or perpendicular to the gun barrel axis.
  • FIG. 3 shows such auxiliary gas entry means.
  • Gas entry tube 70 is concentric 'with reactant entry tube 50 thus introducing the desired amount of oxidant or hydrocarbon into zone A of the gun barrel.
  • Tube 71 in broken hues, shows the alternative method for introducing the auxiliary gas into zone A.
  • This invention has several uses;.the first being a method by which chemical reactions are promoted through use of detonations and in which the desired oxidizing or reducing conditions can be obtained by varying the detonation mixture in the reaction zone. 7
  • the second use being a method by which thedetonatable gas mixture in the gun barrel can be varied advantageously in composition along the length of the gun barrel. This has been accomplished by introducingactive gases through the reactant feed tube, thus, producing two gas zones in the gun barrel whose compositions are different. If more than one auxiliary gas supply tube or station were used, the composition of thefuel could be varied in many steps or nearly continuously along the barrel length.
  • the reaction of solid and liquid particles with the products of detonation of the gas in which they are suspended is surprisingly rapid, perhaps because of the very high relative velocity between particle and gas, leading to high rates of transfer of heat and material.
  • the velocity of the detonation products of equimolar acetylene-oxygen mixture in respect to particles originally at rest in the unreacted gas mixture is calculated to be 1200 meters/sec. initially. This relative, velocity decreases, of course, as the particles are accelerated.
  • EXAMPLE I Carburization of tungsten Acetylene at 3.02 c.f.m. and oxygen at 2.94 c.f.m. (O/C ratio of 0.97) were fed into the detonation gun. Tungsten powder (average size 4.5 microns) was fed at a rate of about 6 lbs. per hour entrained in an ethylene gas stream of 0.4 c.f.m. through the axial feed tube. The oxygen/carbon atomic ratio in the reaction zone was 0.86. The gun was operated at about 4 detonations per second with attendant nitrogen purge. The
  • tungsten carbide coating with useful hardness, grindability and wear resistance properties.
  • EXAMPLE HI Reduction of iron oxide (N.B. 478-135) Oxygen at 3.3 c.f.m. and 1.25 c.f.m. propane were fed into a detonation chamber to form a detonation EXAMPLE IV carburization.
  • molybdenum (Run 2B-3299) Oxygen at 3.36 c.f.m. and 3.14 c.f.m. acetylene were fed into a detonation gun to form a. detonation mixture having an oxygen/carbon atomic ratio of 1.07.
  • a powder mixture of molybdenum and 20 wt. percent Type 302 stainless steel binder was introduced in a 0.4 c.-f.m.
  • the oxygen/carbon atomic ratio in this downstream reaction zone was 0.95.
  • the detonation mixture was ignited about 4 times per second with nitrogen purge between detonations.
  • the powder was propelled out of the detonation gun and impinged on a steel baseplate to produce a molybdenum carbide coating containing 82.2 wt. percent Mo, 4.66 wt. percent total C and 0.19 wt. percent free C.
  • a wide variety of reactive gases may be employed for modifying the composition of the detonatable mixture in the reaction zone.
  • propane and ethylene disclosed above, acetylene, ethane, methane, butane could be used to increase reducing and carburizing action.
  • Oxygen could also be added to increase oxidizing action.
  • liquid and gaseous materials could be used.
  • liquid or vaporous silicon tetrachloride could be injected into an oxidizing detonation mixture and be converted to silica.
  • the improved method of operating a detonation gun including an ignition chamber and gun barrel which comprises the steps of introducing into the ignition chamber and gun barrel of the gun, the detonatable fuel gas-oxidant gas mixture of acetylene and oxygen respectively having an oxygen/carbon atomic ratio .of about 1/1, introducing downstream in the gun barrel with respect to said ignition chamber a charge of comminuted solid material and at the same time, introducing an additional'and separate quantityof a hydrocarbon gas in quantity sufiicient to provide a fuel gas-oxidant gas detonatable mixture in said downstream portion of the gun barrel having an oxygen/carbon atomic ratio lessthan that in the ignitionfchamber, and igniting the detonatable fuel oxygen mixture in said, ignition chamber.
  • a process for promoting chemical reactions such as oxidation, reduction and carbun'zation of comminuted solid reactant'materialby detonation which comprises forming a detonatable gas body in anignition zone, in-

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US712401A 1958-01-31 1958-01-31 Method for utilizing detonation waves to effect chemical reactions Expired - Lifetime US3004822A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3251648A (en) * 1961-06-14 1966-05-17 Sun Oil Co Process for extremely rapidly carrying out gas phase reactions and cooling the reaction products thereof
US3356492A (en) * 1959-04-27 1967-12-05 Commissariat Energie Atomique Method of remote starting of exothermic chemical reactions for the production of uranium
US3485888A (en) * 1963-05-24 1969-12-23 Vickers Zimmer Ag Method of carrying out endothermic gas reactions
WO2001030506A1 (es) * 1999-10-28 2001-05-03 Aerostar Coatings, S.L. Pistola de proyeccion por detonacion de alta frecuencia de disparo y alta productividad
RU2236910C2 (ru) * 1999-10-28 2004-09-27 Аэростар Коатингс, С.Л. Высокопроизводительный детонационный пистолет-распылитель с высокой частотой повторения импульсов
WO2007132028A1 (es) 2006-05-12 2007-11-22 Fundacion Inasmet Procedimiento de obtención de recubrimientos cerámicos y recubrimientos cerámicos obtenidos

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2690960A (en) * 1951-05-09 1954-10-05 Cabot Godfrey L Inc Detonation process of making carbon black
US2714563A (en) * 1952-03-07 1955-08-02 Union Carbide & Carbon Corp Method and apparatus utilizing detonation waves for spraying and other purposes
GB737555A (en) * 1950-03-21 1955-09-28 Schmidt Paul Process for carrying out chemical reactions in gases and aerosols
US2774625A (en) * 1954-10-21 1956-12-18 Union Carbide & Carbon Corp Apparatus utilizing detonation waves for spraying powders

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB737555A (en) * 1950-03-21 1955-09-28 Schmidt Paul Process for carrying out chemical reactions in gases and aerosols
US2690960A (en) * 1951-05-09 1954-10-05 Cabot Godfrey L Inc Detonation process of making carbon black
US2714563A (en) * 1952-03-07 1955-08-02 Union Carbide & Carbon Corp Method and apparatus utilizing detonation waves for spraying and other purposes
US2774625A (en) * 1954-10-21 1956-12-18 Union Carbide & Carbon Corp Apparatus utilizing detonation waves for spraying powders

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3356492A (en) * 1959-04-27 1967-12-05 Commissariat Energie Atomique Method of remote starting of exothermic chemical reactions for the production of uranium
US3251648A (en) * 1961-06-14 1966-05-17 Sun Oil Co Process for extremely rapidly carrying out gas phase reactions and cooling the reaction products thereof
US3485888A (en) * 1963-05-24 1969-12-23 Vickers Zimmer Ag Method of carrying out endothermic gas reactions
WO2001030506A1 (es) * 1999-10-28 2001-05-03 Aerostar Coatings, S.L. Pistola de proyeccion por detonacion de alta frecuencia de disparo y alta productividad
US6745951B2 (en) 1999-10-28 2004-06-08 Aerostar Coatings, S.L. High frequency pulse rate and high productivity detonation spray gun
RU2236910C2 (ru) * 1999-10-28 2004-09-27 Аэростар Коатингс, С.Л. Высокопроизводительный детонационный пистолет-распылитель с высокой частотой повторения импульсов
AU778971B2 (en) * 1999-10-28 2004-12-23 Aerostar Coatings, S.L. Detonation gun for projection with high frequency shooting and high productivity
WO2007132028A1 (es) 2006-05-12 2007-11-22 Fundacion Inasmet Procedimiento de obtención de recubrimientos cerámicos y recubrimientos cerámicos obtenidos

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