Method of supercritical fluid fractionation of oil seed extraction materials

• US 8,557,318 B2
• Filed: 03/23/2012
• Issued: 10/15/2013
• Est. Priority Date: 07/06/2007
• Status: Expired due to Fees

• Current Assignee: MOR Supercritical, LLC
• Original Assignee: MOR Supercritical, LLC
• Inventors: Marentis, Rodger T.
• Primary Examiner(s): WEIER, ANTHONY J
• Application Number:
  US13/428,612
• Publication Number:
  US 20120184757A1
• Time in Patent Office: 571 Days
• Field of Search: 426/430, 426/601, 426/417, 554/11
• US Class Current: 426/430
• CPC Class Codes: A23L 5/20 Removal of unwanted matter, e.g. deodorisation or detoxification
• CPC Class Codes: C11B 1/104 using super critical gases or vapours
• CPC Class Codes: C11B 3/00 Refining fats or fatty oils
• CPC Class Codes: Y02P 20/54 using solvents, e.g. supercritical solvents or ionic liquids

Abstract

Generally, a method of pressure regulated supercritical fluid fractionation of oil seed extraction materials which can be utilized to refine oil seed extraction material established in an amount of supercritical fluid. Specifically, a method of pressure regulated supercritical fluid fractionation of corn germ extraction material to produce a refined corn oil extraction material.

Claims

1. A method of fractionating oil seed extraction material, comprising the steps of:

a) establishing an amount of oil seed extraction material in an amount of supercritical carbon dioxide in a first oil seed extraction material separation zone at a temperature of between about 60°

C. and about 110°

C.;

b) adjusting pressure of said amount of oil seed extraction material in said amount of supercritical carbon dioxide in said first oil seed extraction material separation zone to between about 200 bar and about 400 bar to achieve a density of said supercritical fluid of between about 0.75 g/mL and about 0.85 g/mL; and

c) separating a phosphatide fraction from said oil seed extraction material in said amount of supercritical carbon dioxide resulting in a triglyceride fraction and a fatty acid fraction remaining in said amount of supercritical carbon dioxide.

2. The method of fractionating oil seed extraction material as described in claim 1, further comprising the steps of:

a) delivering said amount of oil seed extraction material in said amount of supercritical carbon dioxide having said phosphatide fraction separated in said first oil seed extraction material separation zone to a second oil seed extraction material separation zone;

b) maintaining said amount of oil seed extraction material in said amount of supercritical carbon dioxide having said phosphatid fraction separated in said first oil seed extraction material separation zone at a temperature of between about 60°

C. and about 100°

C.;

c) adjusting pressure of said amount of oil seed extraction material in said amount of supercritical carbon dioxide having said phosphatid fraction separated in said first oil seed extraction material separation zone to between about 150 bar and about 300 bar to achieve a density of said supercritical fluid of between about 0.65 g/mL and about 0.75 g/mL; and

d) separating a triglyceride fraction from said oil seed extraction material in said amount of supercritical carbon dioxide having said phosphatide fraction separated in said first oil seed extraction material separation zone.

3. The method of fractionating oil seed extraction material as described in claim 2, further comprising the steps of:

a) delivering said amount of oil seed extraction material in said amount of supercritical oil seed having said phosphatide fraction separated in said first oil seed extraction material separation zone and said triglyceride fraction separated in said second oil seed extraction material separation zone to a third oil seed extraction material separation zone;

b) maintaining said amount of oil seed extraction material in said amount of supercritical carbon dioxide having said phosphatid fraction separated in said first oil seed extraction material separation zone and said triglyceride fraction separated in said second oil seed extraction material separation zone at a temperature of between about 40°

C. and about 70°

C.;

c) adjusting pressure of said amount of oil seed extraction material in said amount of supercritical carbon dioxide having said phosphatid fraction separated in said first oil seed extraction material separation zone and said triglyceride fraction separated in said second oil seed extraction material separation zone to between about 75 bar and about 100 bar to achieve a density of said supercritical fluid of between about 0.10 g/mL and about 0.30 g/mL; and

d) separating an free fatty acid fraction from said oil seed extraction material in said amount of supercritical carbon dioxide having said phosphatid fraction separated in said first oil seed extraction material separation zone and said triglyceride fraction separated in said second oil seed extraction material separation zone.

4. The method of fractionating oil seed extraction material as described in claim 3, wherein said step of maintaining said amount of oil seed extraction material in said amount of supercritical carbon dioxide in said first oil seed extraction material separation zone at a temperature of between about 60°

C. and about 110°

C. comprises the step of maintaining said amount of oil seed extraction material in said amount of supercritical carbon dioxide in said first oil seed extraction material separation zone at a temperature of between about 70°

C. and about 90°

C.

5. The method of fractionating oil seed extraction material as described in claim 4, wherein said step of adjusting pressure of said amount of oil seed extraction material in said amount of supercritical carbon dioxide in said first oil seed extraction material separation zone to between about 200 bar and about 400 bar to achieve a density of said supercritical fluid of between about 0.75 g/mL and about 0.85 g/mL comprises the step of adjusting pressure of said amount of oil seed extraction material in said amount of supercritical carbon dioxide in said first oil seed extraction material separation zone to between about 250 bar and about 350 bar to achieve a density of said supercritical fluid of between about 0.75 g/mL and about 0.85 g/mL.

6. The method of fractionating oil seed extraction material as described in claim 5, wherein said step of maintaining said amount of oil seed extraction material in said amount of supercritical carbon dioxide having said phosphatid fraction separated in said first oil seed extraction material separation zone at a temperature of between about 60°

C. and about 100°

C. comprises the step of maintaining said amount of oil seed extraction material in said amount of supercritical carbon dioxide having said phosphatid fraction separated in said first oil seed extraction material separation zone at a temperature of between about 70°

C. and about 90°

C.

7. The method of fractionating oil seed extraction material as described in claim 6, wherein said step of adjusting pressure of said amount of oil seed extraction material in said amount of supercritical carbon dioxide having said phosphatid fraction separated in said first oil seed extraction material separation zone to between about 150 bar and about 300 bar to achieve a density of said supercritical fluid of between about 0.65 g/mL and about 0.75 g/mL comprises the step of adjusting pressure of said amount of oil seed extraction material in said amount of supercritical carbon dioxide having said phosphatid fraction separated in said first oil seed extraction material separation zone to between about 175 bar and about 250 bar to achieve a density of said supercritical fluid of between about 0.65 g/mL and about 0.75 g/mL.

8. The method of fractionating oil seed extraction material as described in claim 7, wherein said step of maintaining said amount of oil seed extraction material in said amount of supercritical carbon dioxide having said phosphatid fraction separated in said first oil seed extraction material separation zone and said triglyceride fraction separated in said second oil seed extraction material separation zone at a temperature of between about 40°

C. and about 70°

C. comprises the step of maintaining said amount of oil seed extraction material in said amount of supercritical carbon dioxide having said phosphatid fraction separated in said first oil seed extraction material separation zone and said triglyceride fraction separated in said second oil seed extraction material separation zone at a temperature of between about 45°

C. and about 65°

C.

9. The method of fractionating oil seed extraction material as described in claim 8, wherein said step of adjusting pressure of said amount of oil seed extraction material in said amount of supercritical carbon dioxide having said phosphatid fraction separated in said first oil seed extraction material separation zone and said triglyceride fraction separated in said second oil seed extraction material separation zone to between about 75 bar and about 100 bar to achieve a density of said supercritical fluid of between about 0.10 g/mL and about 0.30 g/mL comprises the step of adjusting pressure of said amount of oil seed extraction material in said amount of supercritical carbon dioxide having said phosphatid fraction separated in said first oil seed extraction material separation zone and said triglyceride fraction separated in said second oil seed extraction material separation zone to between about 80 bar and about 95 bar to achieve a density of said supercritical fluid of between about 0.10 g/mL and about 0.30 g/mL.

10. The method of fractionating oil seed extraction material as described in claim 9, wherein said step of maintaining said amount of oil seed extraction material in said amount of supercritical carbon dioxide in said first oil seed extraction material separation zone at a temperature of between about 70°

C. and about 90°

C. comprises the step of maintaining said amount of oil seed extraction material in said amount of supercritical carbon dioxide in said first oil seed extraction material separation zone at a temperature of between about 75°

C. and about 85°

C.

11. The method of fractionating oil seed extraction material as described in claim 10, wherein said step of adjusting pressure of said amount of oil seed extraction material in said amount of supercritical carbon dioxide in said first oil seed extraction material separation zone to between about 250 bar and about 350 bar to achieve a density of said supercritical fluid of between about 0.75 g/mL and about 0.85 g/mL comprises the step of adjusting pressure of said amount of oil seed extraction material in said amount of supercritical carbon dioxide in said first oil seed extraction material separation zone to between about 275 bar and about 325 bar to achieve a density of said supercritical fluid of between about 0.75 g/mL and about 0.85 g/mL.

12. The method of fractionating oil seed extraction material as described in claim 11, wherein said step of maintaining said amount of oil seed extraction material in said amount of supercritical carbon dioxide having said phosphatid fraction separated in said first oil seed extraction material separation zone at a temperature of between about 70°

C. and about 90°

C. comprises the step of maintaining said amount of oil seed extraction material in said amount of supercritical carbon dioxide having said phosphatid fraction separated in said first oil seed extraction material separation zone at a temperature of between about 75°

C. and about 85°

C.

13. The method of fractionating oil seed extraction material as described in claim 12, wherein said step of adjusting pressure of said amount of oil seed extraction material in said amount of supercritical carbon dioxide having said phosphatid fraction separated in said first oil seed extraction material separation zone to between about 175 bar and about 250 bar to achieve a density of said supercritical fluid of between about 0.65 g/mL and about 0.75 g/mL comprises the step of adjusting pressure of said amount of oil seed extraction material in said amount of supercritical carbon dioxide having said phosphatid fraction separated in said first oil seed extraction material separation zone to between about 195 bar and about 230 bar to achieve a density of said supercritical fluid of between about 0.65 g/mL and about 0.75 g/mL.

14. The method of fractionating oil seed extraction material as described in claim 13, wherein said step of maintaining said amount of oil seed extraction material in said amount of supercritical carbon dioxide having said phosphatid fraction separated in said first oil seed extraction material separation zone and said triglyceride fraction separated in said second oil seed extraction material separation zone at a temperature of between about 45°

C. and about 65°

C. comprises the step of maintaining said amount of oil seed extraction material in said amount of supercritical carbon dioxide having said phosphatid fraction separated in said first oil seed extraction material separation zone and said triglyceride fraction separated in said second oil seed extraction material separation zone at a temperature of between about 50°

C. and about 60°

C.

15. The method of fractionating oil seed extraction material as described in claim 14,wherein said step of adjusting pressure of said amount of oil seed extraction material in said amount of supercritical carbon dioxide having said phosphatid fraction separated in said first oil seed extraction material separation zone and said triglyceride fraction separated in said second oil seed extraction material separation zone to between about 80 bar and about 95 bar to achieve a density of said supercritical fluid of between about 0.10 g/mL and about 0.30 g/mL comprises the step of adjusting pressure of said amount of oil seed extraction material in said amount of supercritical carbon dioxide having said phosphatid fraction separated in said first oil seed extraction material separation zone and said triglyceride fraction separated in said second oil seed extraction material separation zone to between about 80 bar and about 90 bar to achieve a density of said supercritical fluid of between about 0.10 g/mL and about 0.30 g/mL.

16. The method of fractionating oil seed extraction material as described in claim 15, wherein oil seed extraction material comprises corn germ extraction material.