Conoco Inc.

Conocophillips Company

James R McConaghy

H Ernest Romine

John A Rodgers

Ardis L Anderson

Andrea K Zimmerman

Lorita Davis

Hugh E Romine

Charles J Swartz

William H Kegler

Paul C Poynor

John R Friday

The present invention provides a process for thermosetting pitch fibers in reduced times, at low concentrations of oxygen and at higher temperatures than previously possible. Additionally, the present invention provides a pitch fiber which has an oxygen diffusion rate to the center of the fiber which is competitive with the rate of oxidation at the fiber's surface. Further, the present invention provides a high density pitch fiber batt which thermosets without loss of fiber structure.

High temperature, low oxidation stabilization of pitch fibers

Organometallic containing mesophase pitches for spinning into pitch carbon fibers

An improved process is disclosed for producing a unique metals-containing anisotropic pitch suitable for carbon fiber manufacture. Soluble, aromatic-organometallic compounds are added to a carbonaceous feedstock which is substantially free of mesophase pitch and the resulting composition is heat soaked to produce an isotropic pitch product containing mesogens and soluble, aromatic-organometallic compounds. Next, the pitch product is solvent fractionated to separate mesogens which contain metals from the organometallic compounds. The metals-containing mesogens are heated to a temperature sufficient to cause fusion to produce a metals-containing mesophase pitch. In another method, the carbonaceous feedstock is heat soaked to produce an isotropic pitch product containing mesogens and high molecular weight, soluble, aromatic-organometallic compounds are added to the mesogen containing isotropic pitch product prior to solvent fractionation. Metals-containing carbon fibers produced from the mesophase pitch exhibit enhanced stabilization, tensile strength and modulus properties. Alternatively, the solvent fractionation or separation is conducted under supercritical extraction conditions to produce a metals-containing mesophase pitch. Organometallic compounds may be added to the carbonaceous feedstock either prior to or after the heat soak step.

Organometallic containing mesophase pitches for spinning into pitch

Isotropic pitch containing mesogens is combined with a solvent and subjected to dense phase or supercritical conditions and the mesogens are phase separated. In one aspect the isotropic pitch containing mesogens is fluxed with a solvent to solubilize the mesogens, the flux mixture is filtered to remove nonsolubles and the mesogens are phase separated by use of the same solvent under dense phase or supercritical conditions of temperature and pressure. The phase separation conditions are such that the mesogens are recovered as mesophase.

Process for isolating mesophase pitch

An internally-fired vertical shaft kiln for calcining coke wherein a downwardly moving coke bed has a co-current preheat gas stream in the upper portion of the kiln and a counter-current combustion gas stream in the lower portion of the kiln. Both gases are removed at the midportion of the kiln. Combustion air is introduced to the kiln through an inclined grate at the bottom of the kiln which retains a layer of coke thereon for internal combustion. The calcined coke moves over the combusting coke layer on the grate and then through a passage to a cooling chamber where a gas stream is passed through the calcined coke for cooling. The gas stream heated in the cooling chamber can be used as the co-current gas preheat stream in the upper section of the kiln.

Apparatus for calcining coke

Heavy hydrocarbon oil is subjected to hydrogen donor diluent cracking under conditions of high temperature, moderate pressure and short residence time.

Short residence time hydrogen donor diluent cracking process

Vacuum resid and cracked residuum such as decant oil or thermal tar are processed together to reduce the ultimate yield of coke, asphalt and fuel oil. The vacuum resid is donor cracked, and the donor cracker effluent is quenched with decant oil or thermal tar and then fractionated. Fractionator bottoms are vacuum distilled, and vacuum tower overheads are hydrogenated to produce donor for the donor cracker.

Co-processing of straight run vacuum resid and cracked residua

A oil shale retorting process in which oil shale particles are separated into fines and large particles. The large particles are preheated and combined with hot spent shale from a combustor and introduced into a retorting vessel. The fines are introduced into the disengaging section of the retorting vessel. Retort vapors are processed to produce an upgraded syncrude. The portion of the retort vessel where the oil shale and spent shale are introduced has a smaller diameter than the retorting section.

Oil shale retorting process

Heavy hydrocarbonaceous materials are converted to distillate products and pitch in a hydrogen donor diluent cracking process, and the pitch is utilized as feed to a delayed coker. Green coke is calcined in a vertical shaft kiln, and steam is injected into the bottom of the kiln to produce hydrogen by reaction of steam with coke. The hydrogen is drawn from the kiln and used to hydrogenate recycle donor solvent for the cracking step. High sulfur coke can be desulfurized in the kiln, and distillate products in addition to donor solvent can be hydrotreated using hydrogen from the kiln.

Upgrading of heavy hydrocarbons

Carbonaceous material such as petroleum coke is calcined in the upper part of an air-injected vertical shaft kiln, and steam injected into the lower part of the kiln reacts with hot coke below the combustion zone to produce hydrogen and carbon monoxide. A product gas stream rich in hydrogen and low in nitrogen is withdrawn from a level below the combustion zone in the kiln. High sulfur coke can be desulfurized in the process by maintaining the temperature in the calcining zone above 1400.degree. C.

Process for producing calcined coke and rich synthesis gas

A petroleum refinery residual oil derived from a naphthenic crude oil is catalytically demetalized, catalytically desulfurized and then fed to a delayed coker to produce premium delayed coke.

Method for producing premium coke from residual oil

Low value heavy hydrocarbonaceous material such as a petroleum refinery vacuum residuum is converted to distillate products and pitch in a hydrogen donor diluent cracking process, and the pitch is utilized as feedstock to a delayed premium coker.

Process for producing premium coke from vacuum residuum

A petroleum refinery vacuum residuum stream is subjected to hydrogen donor diluent cracking, the liquid cracking effluent is hydrodesulfurized, the hydrodesulfurizer effluent is fractionated, and the fractionator bottoms stream is fed to a delayed coker where premium type delayed coke is produced. The gas oil boiling range fraction from the fractionator is utilized as the donor diluent in the cracking step.

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Ponca City, OK, United States of America

James R McConaghy