US3607716A
Expired / Lapsed
US
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Fractionation of coal liquefaction products in a mixture of heavy and light organic solvents
Assignee: Kerr McGee Corp
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Filing: 1970-01-09
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Granted: 1971-09-21
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Expires: 1990-01-09
Abstract
Abstract Coal liquefaction products are separated into a plurality of fractions of varying softening points and molecular complexity in a solvent mixture containing a heavy organic coal liquefaction solvent and a light organic fractionating solvent having a critical temperature below 800* F. under elevated temperature and pressure conditions. In one variant, coal is liquefied with a heavy organic coal liquefaction solvent, the light organic fractionating solvent is added to the solution thus produced, and thereafter the coal liquefaction products are separated into a plurality of fractions at elevated temperature and pressure. Preferred heavy organic solvents include anthracene oil, tetralin, catalytic cracker recycle stocks, thermally cracked stocks and lubricating oil aromatic extracts, and preferred light organic solvents include pyridine, benzene and hexane. In a preferred variant, a mixture of the light and heavy organic solvents is recovered directly from the final fractionating stage, the solvent mixture is separated in a solvent separating vessel directly into a heavy organic solvent phase and a light organic solvent phase, and the two solvent phases are passed in heat exchange relationship with incoming solvent-rich streams to preceding fractionating stages to recover the heat content and produce cooled liquid heavy and light organic solvent streams for recycle. The invention further provides a method of separating finely divided insoluble material from products of coal liquefaction present in a solvent comprising a heavy organic coal liquefaction solvent.
Inventors
- 👤 Jack W Roach
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-28 09:00
CPC Classifications
C; C10; C10G; C10G1/00; C10G1/002; C10G1/04
Claims Analysis
Total Claims: 30
Claim 1
Independent Claim
22 words
The method of claim 1 wherein said light organic fractionating solvent is selected from the group consisting of pyridine, benzene and hexane.
Claim 2
Dependent Claim
111 words
The method of claim 1 wherein said organic solvent solution contains initially finely divided insoluble material derived from coal during liquefaction, the temperature and pressure are adjusted to provide a light organic fractionating solvent density in the treating zone of about 0.40-0.65 g./cc. when separating the first heavy fraction, a body of slurry containing the insoluble material and the first heavy fraction is separated in a lower portion of the treating zone, the body of slurry contains the first heavy fraction in an amount to flux the insoluble material present therein under the temperature and pressure conditions existing in the treating zone, and the slurry is withdrawn from the treating zone.
Claim 3
Dependent Claim
33 words
The method of claim 1 wherein said heavy organic coal liquefying solvent is selected from the group consisting anthracene oil, tetralin, catalytic cracker recycle stocks, thermally cracked stocks, and lubricating oil aromatic extracts.
Claim 4
Dependent Claim
16 words
The method of claim 1 wherein said heavy organic coal-liquefying solvent is catalytic cracker slurry oil.
Claim 5
Dependent Claim
50 words
The method of claim 1 wherein said light organic fractionating solvent is selected from the group consisting of pyridine, benzene and hexane, and said heavy organic coal-liquefying solvent is selected from the group consisting of anthracene oil, tetralin, catalytic cracker recycle stocks, thermally cracked stocks and lubricating oil aromatic extracts.
Claim 6
Dependent Claim
16 words
The method of claim 6 wherein said heavy organic coal-liquefying solvent is catalytic cracker slurry oil.
Claim 7
Dependent Claim
158 words
The method of claim 1 wherein the first solvent-rich phase is further treated in a treating zone under elevated temperature and pressure conditions to separate at least one additional fluidlike heavy fraction of coal liquefaction products including a fluidlike final heavy fraction of residual coal liquefaction products which is separated from a lighter organic solvent phase containing mixed heavy organic coal liquefying solvent and light organic fractionating solvent, the temperature and pressure are adjusted to provide a light organic fractionating solvent density in the treating zone during separation of the final heavy fraction not greater than about 0.35 g./cc. and sufficiently low to separAte the residual coal liquefaction products from the organic solvent phase, the final heavy fraction having a viscosity under the temperature and pressure conditions existing in the treating zone during separation thereof whereby it is flowable from the treating zone, and withdrawing the final heavy fraction of residual coal liquefaction products from the treating zone.
Claim 8
Dependent Claim
67 words
The method of claim 8 wherein the pressure in the treating zone during separation of the first heavy fraction and at least one additional heavy fraction including the final heavy fraction is approximately the same, and the temperature of the organic solvent is adjusted to provide the desired light organic fractionating solvent density for separation of at least one additional heavy fraction including the final heavy fraction.
Claim 9
Dependent Claim
82 words
The method of claim 8 wherein the temperature and pressure of said organic solvent phase are adjusted in a treating zone to provide a light organic fractionating solvent density not greater than about 0.10-0.20 g/cc. and sufficiently low to form a light organic fractionating solvent phase and a heavy organic coal-liquefying solvent phase. said heavy organic coal-liquefying solvent phase having a viscosity whereby it is flowable from the treating zone, and withdrawing said heavy organic coal-liquefying solvent phase from the treating zone.
Claim 10
Dependent Claim
48 words
The method of claim 10 wherein said light organic fractionating solvent phase is withdrawn from the treating zone, and at least one of said withdrawn solvent phases is passed in heat exchange relationship with a coolant comprising at least one relatively cool solvent-rich phase whereby heat is recovered.
Claim 11
Dependent Claim
110 words
The method of claim 8 wherein at least one fluidlike intermediate heavy fraction of coal liquefaction products is obtained by treating the first solvent-rich phase in at least one treating zone under elevated temperature and pressure conditions providing a light organic fractionating solvent density therein which is less than that existing in the treating zone when separating the first heavy fraction and greater than 0.2 g./cc., at least one intermediate heavy fraction separate by this treatment having a viscosity under the temperature and pressure conditions existing in the treating zone whereby it is freely flowable therefrom, and withdrawing at least one intermediate heavy fraction from at least one treating zone.
Claim 12
Dependent Claim
111 words
The method of claim 12 wherein said organic solvent solution contains initially finely divided insoluble material derived from coal during liquefaction, the temperature and pressure are adjusted to provide a light organic fractionating solvent density in the treating zone of about 0.40-0.65 g./cc. when separating the first heavy fraction, a body of slurry containing the insoluble material and the first heavy fraction is separated in a lower portion of the treating zone, the body of slurry contains the first heavy fraction in an amount to flux the insoluble material present therein under the temperature and pressure conditions existing in the treating zone, and the slurry is withdrawn from the treating zone.
Claim 13
Dependent Claim
67 words
The method of claim 13 wherein the pressure in the treating zone during separation of the first heavy fraction and at least one additional heavy fraction including the final heavy fraction is approximately the same, and the temperature of the organic solvent is adjusted to provide the desired light organic fractionating solvent density for separation of at least one additional heavy fraction including the final heavy fraction.
Claim 14
Dependent Claim
82 words
The method of claim 14 wherein the temperature and pressure of said organic solvent phase are adjusted in a treating zone to provide a light organic fractionating solvent density not greater than about 0.10-0.20 g./cc. and sufficiently low to form a light organic fractionating solvent phase and a heavy organic coal-liquefying solvent phase, said heavY organic coal-liquefying solvent phase having a viscosity whereby it is flowable from the treating zone, and withdrawing said heavy organic coal-liquefying solvent phase from the treating zone.
Claim 15
Dependent Claim
48 words
The method of claim 15 wherein said light organic fractionating solvent phase is withdrawn from the treating zone, and at least one of said withdrawn solvent phases is passed in heat exchange relationship with a coolant comprising at least one relatively cool solvent-rich phase whereby heat is recovered.
Claim 16
Independent Claim
464 words
A method of liquefying and fractionating coal comprising intimately contacting each part by weight of coal in particulate form with at least two parts by weight of a heavy organic solvent consisting essentially of an organic coal liquefaction solvent having a critical temperature above about 800* F. to produce a heavy organic solvent solution containing coal liquefaction products and finely divided insoluble material, the coal being contacted with the solvent in a liquefaction zone at a temperature of about 550*-1,000* F. and under a pressure providing a solvent density of at least 0.5 g./cc. the temperature in the liquefaction zone being below the solvent decomposition temperature and the solution thus produced containing at least two parts by weight of the heavy organic solvent for each part by weight of the coal liquefaction products, withdrawing the heavy organic solvent solution of coal liquefaction products from the liquefaction zone, admixing at least two parts by weight of light organic fractionating solvent with each part by weight of the organic solvent solution of coal liquefaction products to produce a mixed organic solvent solution of coal liquefaction products, the light organic fractionating solvent consisting essentially of at least one substance having a critical temperature below about 800* F. selected from the group consisting of aromatic hydrocarbons having a single benzene nucleus and normal boiling points below about 310* F., cycloparaffin hydrocarbons having normal boiling points below about 310* F., open chain mono-olefin hydrocarbons having normal boiling points below about 310* F., open chain saturated hydrocarbons having normal boiling points below about 310* F., mono-, di-, and tri-open chain amines, carbocyclic amines having a monocyclic structure, heterocyclic amines, and phenol and its homologs, treating said organic solvent solution of coal liquefaction products at an elevated temperature and pressure in a first treating zone to separate a fluidlike first heavy fraction containing coal liquefaction products and said finely divided insoluble material and a first solvent-rich phase containing dissolved coal liquefaction products, the organic solvent solution of coal liquefaction products being treated in the first treating zone at a temperature of at least 400* F. and the temperature being sufficiently elevated to form a liquid-to-liquid bulk interface between the first heavy fraction and the first solvent-rich phase, the temperature and pressure being adjusted to provide a light organic fractionating solvent density in the treating zone of less than about 0.65 g./cc., the solvent density being sufficiently low to separate the first heavy fraction from the first solvent-rich phase and sufficiently high to retain the remaining coal liquefaction products in solution in the first solvent-rich phase, the first heavy fraction having a viscosity under the temperature and pressure conditions existing in the treating zone whereby it is flowable from the treating zone, and withdrawing the first heavy fraction from the treating zone.
Claim 17
Dependent Claim
22 words
The method of claim 17 wherein said light organic fractionating solvent is selected from the group consisting of pyridine, benzene and hexane.
Claim 18
Dependent Claim
111 words
The method of claim 17 wherein said organic solvent solution contains Initially finely divided insoluble material derived from coal during liquefaction, the temperature and pressure are adjusted to provide a light organic fractionating solvent density in the treating zone of about 0.40-0.65 g./cc. when separating the first heavy fraction, a body of slurry containing the insoluble material and the first heavy fraction is separated in a lower portion of the treating zone, the body of slurry contains the first heavy fraction in an amount to flux the insoluble material present therein under the temperature and pressure conditions existing in the treating zone, and the slurry is withdrawn from the treating zone.
Claim 19
Dependent Claim
34 words
The method of claim 17 wherein said heavy organic coal liquefying solvent is selected from the group consisting of anthracene oil, tetralin, catalytic cracker recycle stocks, thermally cracked stocks, and lubricating oil aromatic extracts.
Claim 20
Dependent Claim
16 words
The method of claim 17 wherein said heavy organic coal-liquefying solvent is catalytic cracker slurry oil.
Claim 21
Dependent Claim
50 words
The method of claim 17 wherein said light organic fractionating solvent is selected from the group consisting of pyridine, benzene and hexane, and said heavy organic coal-liquefying solvent is selected from the group consisting of anthracene oil, tetralin, catalytic cracker recycle stocks, thermally cracked stocks and lubricating oil aromatic extracts.
Claim 22
Dependent Claim
16 words
The method of claim 22 wherein said heavy organic coal-liquefying solvent is catalytic cracker slurry oil.
Claim 23
Dependent Claim
188 words
The method of claim 17 wherein said first solvent-rich phase is withdrawn from the first treating zone and is introduced into at least one additional treating zone including a final treating zone, the first solvent-rich phase is further treated under elevated temperature and pressure conditions to separate at least one additional fluidlike heavy fraction of coal liquefaction products including a fluidlike heavy fraction of residual coal liquefaction products which is separated in the final treating zone from a lighter organic solvent phase containing mixed heavy organic coal-liquefying solvent and light organic fractionating solvent, the temperature and pressure are adjusted to provide a light organic fractionating solvent density in the final treating zone during separation of the final heavy fraction not greater than about 0.35 g./cc. and sufficiently low to separate the residual coal liquefaction products from the organic solvent phase. the final heavy fraction has a viscosity under the temperature and pressure conditions existing in the final treating zone during the separation thereof whereby it is flowable from the treating zone, and the final heavy fraction of residual coal liquefaction products is withdrawn from the final treating zone.
Claim 24
Dependent Claim
67 words
The method of claim 24 wherein the pressure in the treating zone during separation of the first heavy fraction and at least one additional heavy fraction including the final heavy fraction is approximately the same, and the temperature of the organic solvent is adjusted to provide the desired light organic fractionating solvent density for separation of at least one additional heavy fraction including the final heavy fraction.
Claim 25
Dependent Claim
82 words
The method of claim 24 wherein the temperature and pressure of said organic solvent phase are adjusted in a treating zone to provide a light organic fractionating solvent density not greater than about 0.10-0.20 g./cc. and sufficiently low to form a light organic fractionating solvent phase and a heavy organic coal-liquefying solvent phase, said heavy organic coal-liquefying solvent phase having a viscosity whereby it is flowable from the treating zone, and withdrawing said heavy organic coal-liquefying solvent phase from the treating zone.
Claim 26
Dependent Claim
48 words
The method of claim 26 wherein said light organic fractionating solvent phase is withdrawn from the treating zone, and at least one of said withdrawn solvent phases is passed in heat exchange relationship With a coolant comprising at least one relatively cool solvent-rich phase whereby heat is recovered.
Claim 27
Dependent Claim
112 words
The method of claim 24 wherein at least one fluidlike intermediate heavy fraction of coal liquefaction products is obtained by treating the first solvent-rich phase in at least one treating zone under elevated temperature and pressure conditions providing a light organic fractionating solvent density therein which is less than that existing in the first treating zone when separating the first heavy fraction and greater than about 0.2 g./cc., at least one intermediate heavy fraction separated by this treatment having a viscosity under the temperature and pressure conditions existing in the treating zone whereby it is freely flowable therefrom, and withdrawing at least one intermediate heavy fraction from at least one treating zone.
Claim 28
Dependent Claim
67 words
The method of claim 28 wherein the pressure in the treating zone during separation of the first heavy fraction and at least one additional heavy fraction including the final heavy fraction is approximately the same, and the temperature of the organic solvent is adjusted to provide the desired light organic fractionating solvent density for separation of at least one additional heavy fraction including the final heavy fraction.
Claim 29
Dependent Claim
82 words
The method of claim 29 wherein the temperature and pressure of said organic solvent phase are adjusted in a treating zone to provide a light organic fractionating solvent density not greater than about 0.10-0.20 g./cc. and sufficiently low to form a light organic fractionating solvent phase and a heavy organic coal-liquefying solvent phase, said heavy organic coal-liquefying solvent phase having a viscosity whereby it is flowable from the treating zone, and withdrawing said heavy organic coal-liquefying solvent phase from the treating zone.
Claim 30
Dependent Claim
48 words
The method of claim 30 wherein said light organic fractionating solvent phase is withdrawn from the treating zone, and at least one of said withdrawn solvent phases is passed in heat exchange relationship with a coolant comprising at least one relatively cool solvent-rich phase whereby heat is recovered.
References Cited (Backward Citations)
No citation records indexed.
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1974-09-20 | 1975-03-22 | 1975-09-21 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1978-09-20 | 1979-03-22 | 1979-09-21 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1982-09-20 | 1983-03-22 | 1983-09-21 | $7700.00 | Window Closed / Lapsed |