Method of performing hydrous pyrolysis for studying the kinetic parameters of hydrocarbons generated from source material

• US 5,082,787 A
• Filed: 12/22/1989
• Issued: 01/21/1992
• Est. Priority Date: 12/22/1989
• Status: Expired due to Fees

• Current Assignee: Houston Advanced Research Center
• Original Assignee: Texaco Incorporated (Chevron Corp.)
• Inventors: Nolte, David G., Colling, Edwin L. Jr., Haskin, Helen K.
• Primary Examiner(s): Lacey, David L.
• Assistant Examiner(s): REDDING, DAVID A
• Application Number:
  US07/455,112
• Time in Patent Office: 760 Days
• Field of Search: 436/29, 436/30, 436/31, 436/32, 436/34, 436/155, 436/157, 436/139, 436/143, 436/177
• US Class Current: 436/31
• CPC Class Codes: G01N 1/44 Sample treatment involving radiation, e.g. heat
• CPC Class Codes: G01N 5/04 by removing a component, e.g. by evaporation, and weighing the remainder
• CPC Class Codes: Y10T 436/25375 Liberation or purification of sample or separation of material from a sample [e.g., filtering, centrifuging, etc.]

Abstract

A method for studying the rate and type of hydrocarbon generated from a hydrocarbon source utilizes hydrous pyrolysis to generate hydrocarbons from the sample and then utilizes cryogenic methods to remove the fluid portions to a transfer vessel. The gaseous components are removed to a further vessel of known dimensions for determination of weight. The hydrocarbons in the transfer vessel are passed through a dryer to separate the water and their makeup determined. The hydrocarbons remaining in the reactor vessel are removed by working with solvents and their weights are determined after separation and evaporation of the solvents.

Claims

1. A method of performing hydrous pyrolysis on a sample of hydrocarbon source material for studying the kinetic parameters of hydrocarbons generated from said source material, comprising the steps of:

enclosing a measured amount of hydrocarbon source material in a sample holder closed at both ends by fluid permeable discs and sealing said sample holder in a pressure chamber of a reactor;

sequentially charging said reactor with inert gas and evacuating said chamber to completely purge it of oxygen;

at lease partially flooding said evacuated chamber with pure water;

briefly evacuating said chamber to remove any remaining gases therefrom;

heating said sample to a specified temperature for a specified period of time during which hydrocarbons generated by thermal maturation will be driven from said sample;

transferring the water and more volatile generated hydrocarbons cryogenically into a transfer vessel which has also been purged of oxygen;

recovering soluble bitumen and insoluble kerogen from said sample holder and chamber by washing;

cryogenically recovering a first portion of said hydrocarbons from said transfer vessel; and

recovering a remaining portion of said hydrocarbons by drying any residue materials remaining in said transfer vessel as a result of said cryogenic recovery step.

2. The method according to claim 1, wherein said inert gas is helium.

3. The method according to claim 1, wherein said pure water is oxygen-free HPLC grade.

4. The method according to claim 1, wherein said pure water is pretreated with helium to purge it of oxygen.

5. The method according to claim 1, wherein said temperature and period of time are determined empirically.

6. The method according to claim 1, wherein said temperature to which the sample is heated to cause it to generate hydrocarbons by thermal maturation is in the range of 225°

to 360°

C.

7. The method according to claim 1, wherein the time for which said sample is heated to cause it to generate hydrocarbons by thermal maturation is in the range of 1 day to 6 months.

8. The method according to claim 1, wherein said first cryogenic transfer takes place at temperatures less than 0°

C.

9. The method according to claim 1, wherein said soluble bitumen is recovered by washing said holder and reactor chamber with solvent and evaporating the solvent therefrom, said insoluble kerogen being also removed by said washing.

10. The method according to claim 1, wherein said cryogenic recovering takes place at temperatures not greater than 0°

C.

11. The method according to claim 1, wherein said drying of said residue materials is accomplished by passing said remaining portion of said hydrocarbons through tubes formed of desiccant material whereby water vapor is removed by hygroscopic ion exchange membranes.