# US 5,348,718 A · Method and apparatus for producing carbride products

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- Number: US 5,348,718 A
- Document ID: US5348718A
- Status: Granted
- Kind: A
- Application number: 07/504,450
- Filed: 1990-04-04
- Granted: 1994-09-20
- Earliest claimed: 1990-04-04
- Assignees: Phillips Petroleum Company
- Inventors: Michael C. Carter; Bruce W. Gerhold
- Web page: https://patentgrep.com/patent/US5348718A

## CPC

- B01J 19/26: Nozzle-type reactors, i.e. the distribution of the initial reactants within the reactor is effected by their introduction or injection through nozzles
- B01J 12/02: for obtaining at least one reaction product which, at normal temperature, is in the solid state
- B82Y 30/00: Nanotechnology for materials or surface science, e.g. nanocomposites
- C01B 32/90: Carbides
- C01B 32/956: Silicon carbide
- C01B 32/963: Preparation from compounds containing silicon
- B01J 2219/00063: of the reactants
- B01J 2219/0009: Coils
- B01J 2219/00094: Jackets
- B01J 2219/00119: Heat exchange inside a feeding nozzle or nozzle reactor
- B01J 2219/00132: using electric heating or cooling elements
- B01J 2219/00155: using insulating materials or refractories
- B01J 2219/00159: controlling multiple zones along the direction of flow, e.g. pre-heating and after-cooling
- B01J 2219/00162: controlling the pressure
- B01J 2219/00164: controlling the flow
- B01J 2219/00252: Formation of deposits other than coke
- C01P 2002/72: by d-values or two theta-values, e.g. as X-ray diagram
- C01P 2004/51: Particles with a specific particle size distribution
- C01P 2004/62: Submicrometer sized, i.e. from 0.1-1 micrometer
- C01P 2004/64: Nanometer sized, i.e. from 1-100 nanometer
- C01P 2006/80: Compositional purity
- B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B82Y: SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C}
- C01P: INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS

## Abstract

A method and apparatus are provided for producing a product comprising a carbide compound, such as for example silicon carbide. A reactor is provided which has a chamber defined therein which is divided into a combustion zone and a reaction zone. A combustible mixture is injected into the combustion zone in a direction generally toward the reaction zone, and is accordingly combusted in the combustion zone. At least one reactant (i.e. silane) is injected at the boundary between the zones into the reactor chamber in a direction generally parallel to the longitudinal axis of the chamber so as to react to form raw product comprising the carbide compound.

## Claims

### Claim 1

A method comprising the steps of:
providing a reactor having a chamber defined therein which has a longitudinal axis and longitudinally separated upstream and downstream ends, wherein the chamber comprises a combustion zone and a reaction zone such that the combustion zone longitudinally extends from said upstream end to a surface boundary between the zones and such that the reaction zone longitudinally extends from said surface boundary to said downstream end;
establishing a flow of a combustible mixture in the combustion zone so as to generally flow in a direction generally toward the reaction zone, wherein the combustible mixture comprises a mixture of a fuel and an oxidant;
combusting the combustibel mixture in the combustion zone to produce hot combustion products which flow generally toward and into the reaction zone;
injecting at least one reactant into the chamber from at least one outlet of at least one reactant nozzle such that said at least one reactant exits said at least one reactant nozzle outlet at said surface boundary in a direction generally parallel to said longitudinal axis, wherein temperature conditions in at least a portion of the reaction zone are at least about 1400.degree. C. and wherein the elemental molar ratio of carbon to oxygen for the combination of the combustible mixture and said at least one reactant is at least about 0.8:1, said at least one reactant being capable of reacting in the reaction zone to form a carbide compound;
whereby a product powder comprising the carbide compound is produced in the reaction zone.

### Claim 2 (depends on 1)

A method as recited in claim 1 wherein the flow of combustible mixture is established in the combustion zone by injecting the combustible mixture into the combustion zone from at least one outlet of at least one combustion nozzle, said at least one combustion nozzle outlet defining at least one linear boundary whose projection in a direction generally parallel to said longitudinal axis and onto said surface boundary generally surrounds said at least one reaction nozzle outlet.

### Claim 3 (depends on 2)

A method as recited in claim 2 wherein said at least one reaction nozzle outlet comprises a single reaction nozzle outlet positioned substantially on said longitudinal axis such that said at least one reactant exits said at least one reactant nozzle outlet generally along said longitudinal axis and toward said downstream end.

### Claim 4 (depends on 3)

A method as recited in claim 3 wherein said reaction nozzle outlet is positioned so as to be generally centrally located within said projection of said at least one linear boundary.

### Claim 5 (depends on 4)

A method as recited in claim 4 wherein said at least one combustion nozzle comprises a plurality of combustion nozzles, each combustion nozzle having a corresponding outlet.

### Claim 6 (depends on 5)

A method as recited in claim 5 wherein said plurality of combustion nozzle outlets are equidistantly spaced from one another.

### Claim 7 (depends on 6)

A method as recited in claim 6 wherein said plurality of combustion nozzle outlets are positioned to define a generally triangular linear boundary.

### Claim 8 (depends on 7)

A method as recited in claim 7 wherein said plurality of combustion nozzle outlets are positioned closely adjacent to said upstream end.

### Claim 9 (depends on 1)

A method as recited in claim 1 wherein said elemental molar ratio is in the range of about 0.9:1 to about 1.5:1.

### Claim 10 (depends on 9)

A method as recited in claim 9 wherein said elemental molar ratio is in the range of about 1:1 to about 1.3:1.

### Claim 11 (depends on 10)

A method as recited in claim 10 wherein the elemental molar ratio for the combustible mixture is at least about 0.7:1.

### Claim 12 (depends on 11)

A method as recited in claim 11 wherein the elemental molar ratio for the combustible mixture is in the range of about 0.9:1 to about 1.1:1.

### Claim 13 (depends on 12)

A method as recited in claim 12 wherein said temperature conditions are in the range of about 1400.degree. C. to about 1700.degree. C.

### Claim 14 (depends on 1)

A method as recited in claim 1 wherein the fuel comprises a hydrocarbon selected from the group consisting of ethylene, propylene, butene, propadiene, butadiene, propyne, butyne, and mixtures thereof.

### Claim 15 (depends on 14)

A method as recited in claim 14 wherein the fuel comprises a mixture of ethylene and acetylene.

### Claim 16 (depends on 1)

A method as recited in claim 1 wherein said at least one reactant comprises a first reactant, which includes a first component, and also a second reactant containing a second, carbon component, wherein said first and second reactants react to form said carbide compound, said carbide compound being a compound of said first component and said second, carbon component.

### Claim 17 (depends on 16)

A method as recited in claim 16 wherein said first component is selected from the group consisting of silicon, boron, tungsten, chromium, titanium, zirconium, molybdenum, and iron.

### Claim 18 (depends on 17)

A method as recited in claim 17 wherein said first component is silicon.

### Claim 19 (depends on 18)

A method as recited in claim 18 wherein said first reactant is silane.

### Claim 20 (depends on 16)

A method as recited in claim 16 wherein said second reactant comprises a C.sub.1 -C.sub.9 carbon compound.

### Claim 21 (depends on 20)

A method as recited in claim 20 wherein said C.sub.1 -C.sub.9 carbon compound is a hydrocarbon selected from the group consisting of methane, ethane, propane, butane, pentane, hexane, heptane, octane, nonane, ethlyene, propylene, acetylene, benzene, toluene, cyclopropane, cyclobutane, cyclopentane, cyclohexane, and mixtures thereof.

### Claim 22 (depends on 16)

A method as recited in claim 16 wherein a mass ratio is provided of no more than about 0.3.

### Claim 23 (depends on 3)

A method as recited in claim 3 wherein said at least one reactant comprises a first reactant, which includes a first component, and also a second reactant containing a second, carbon component, wherein said first and second reactants react to form said carbide compound which is a compound of said first component and said second, carbon component, and wherein both said first and second reactants are injected into the chamber from said single reaction nozzle outlet.

### Claim 24

A method comprising the steps of:
providing a reactor having a chamber defined therein which has a longitudinal axis and longitudinally separated upstream and downstream ends, wherein the chamber comprises a combustion zone and a reaction zone such that the combustion zone longitudinally extends from said upstream end to a surface boundary between the zones and such that the reaction zone longitudinally extends from said surface boundary to said downstream end;
establishing a flow of a combustible mixture in the combustion zone so as to flow in a direction generally toward the reaction zone, wherein the combustible mixture comprises a mixture of a fuel and an oxidant comprising oxygen:
combusting the combustible mixture in the combustion zone to produce hot combustion products which flow generally toward and into the reaction zone;
injecting at least one reactant into the chamber from at least one outlet of at least one reactant nozzle such that said at least one reactant exits said at least one reactant nozzle outlet at said surface boundary in a direction generally parallel to said longitudinal axis, wherein temperature conditions in at least a portion of the reaction zone are at least about 1400.degree. C. and wherein the elemental molar ratio of carbon to oxygen for the combination of the combustible mixture and said at least one reactant is at least about 0.8:1, said at least one reactant being capable of reacting in the reaction zone to form a carbide compound;
whereby a product powder comprising the carbide compound is produced in the reaction zone.

### Claim 25

A method comprising the steps of:
providing a reactor having a chamber defined therein which has a longitudinal axis and longitudinally separated upstream and downstream ends, wherein the chamber comprises a combustion zone and a reaction zone such that the combustion zone longitudinally extends from said upstream end to a surface boundary between the zones and such that the reaction zone longitudinally extends from said surface boundary to said downstream end;
establishing a flow of a combustible mixture in the combustion zone so as to generally flow in a direction generally toward the reaction zone, wherein the combustible mixture comprises a mixture of a fuel and an oxidant;
combusting the combustible mixture in the combustion zone to produce hot combustion products which flow generally toward and into the reaction zone;
injecting at least one reactant into the chamber from at least one outlet of at least one reactant nozzle such that said at least one reactant is substantially gaseous as injected into said chamber and such that said at least one reactant exits said at least one reactant nozzle outlet at said surface boundary in a direction generally parallel to said longitudinal axis, wherein temperature conditions in at least a portion of the reaction zone are at least about 1400.degree. C. and wherein the elemental molar ratio of carbon to oxygen for the combination of the combustible mixture and said at least one reactant is at least about 0.8:1, said at least one reactant being capable of reacting in the reaction zone to form a carbide compound;
whereby a product powder comprising the carbide compound is produced in the reaction zone.
