Systems for selective removal of contaminants from a composition and methods of regenerating the same

• US 8,017,796 B2
• Filed: 08/13/2009
• Issued: 09/13/2011
• Est. Priority Date: 02/13/2007
• Status: Active Grant

• Current Assignee: Mcneff Research Consultants, Inc.
• Original Assignee: Mcneff Research Consultants, Inc.
• Inventors: Yan, Bingwen, McNeff, Larry C., McNeff, Clayton V.
• Primary Examiner(s): Caldarola; Glenn A
• Assistant Examiner(s): Stein; Michelle L
• Application Number:
  US12/540,568
• Publication Number:
  US 20100147771A1
• Time in Patent Office: 761 Days
• Field of Search: 208/263, 210/690, 554/175, 554/178, 502/20
• US Class Current: 554/193
• CPC Class Codes: B01D 15/00 Separating processes involving the treatment of liquids with solid sorbents using liquid sorbents B01D11/00; ion exchange processes or materials, sorbent materials in general B01J, e.g. sorbents for chromatography B01J20/281; for investigating or analysing materials G01N30/00; Apparatus therefor
• CPC Class Codes: B01J 20/0211 Compounds of Ti, Zr, Hf
• CPC Class Codes: B01J 20/06 comprising oxides or hydroxides of metals not provided for in group B01J20/04
• CPC Class Codes: B01J 20/08 comprising aluminium oxide or hydroxide; comprising bauxite
• CPC Class Codes: B01J 20/3433 of sorbents or filter aids other than those covered by B01J20/3408 - B01J20/3425
• CPC Class Codes: B01J 20/3475 in the liquid phase
• CPC Class Codes: C10G 25/00 Refining of hydrocarbon oils in the absence of hydrogen, with solid sorbents
• CPC Class Codes: C10L 1/026 for compression ignition
• CPC Class Codes: C11B 3/10 by adsorption
• CPC Class Codes: C11C 3/003 by esterification of fatty acids with alcohols C11C3/02 takes precedence

Abstract

The present invention relates to devices and methods for selectively removing contaminants from a crude product mixture. In an embodiment the invention includes a method for removing organic acids from a crude product mixture including contacting the crude product mixture with a metal oxide substrate, wherein free organic acids in the crude product mixture bind to the metal oxide substrate, thereby removing free organic acids and forming a refined product mixture; separating the refined product mixture from the metal oxide substrate; and removing the organic acids bound to the metal oxide substrate by contacting the metal oxide substrate with an alkyl ester composition at a temperature of greater than about 100 degrees Celsius. Other embodiments are also described herein.

Claims

1. A method for removing organic acids from a crude product mixture comprising:

contacting the crude product mixture with a metal oxide substrate, wherein free organic acids in the crude product mixture bind to the metal oxide substrate, thereby removing free organic acids and forming a refined product mixture;

separating the refined product mixture from the metal oxide substrate;

removing the organic acids bound to the metal oxide substrate by contacting the metal oxide substrate with fatty acid alkyl ester composition at a temperature of greater than about 100 degrees Celsius.

2. The method of claim 1, comprising removing the organic acids bound to the metal oxide substrate by contacting the metal oxide substrate with an alkyl ester composition at a temperature of greater than about 150 degrees Celsius.

3. The method of claim 1, the metal oxide substrate comprising Lewis acid sites and Lewis base sites sufficient to bond with free organic acids.

4. The method of claim 1, the metal oxide substrate comprising Bronsted base sites sufficient to bond with free organic acids.

5. The method of claim 1, the metal oxide substrate comprising Bronsted acid sites sufficient to bond with free organic acids.

6. The method of claim 1, the crude product mixture comprising fatty acid alkyl ester composition.

7. The method of claim 1, the crude product mixture comprising an organic acid containing material selected from the group consisting of rapeseed oil, soybean oil, canola oil, cottonseed oil, grape seed oil, mustard seed oil, corn oil, linseed oil, safflower oil, sunflower oil, poppy-seed oil, pecan oil, walnut oil, oat oil, peanut oil, rice bran oil, camellia oil, castor oil, and olive oil, palm oil, coconut oil, rice oil, algae oil, seaweed oil, and Chinese Tallow tree oil.

8. The method of claim 1, wherein at least about 95% of the free organic acids in the crude product mixture bind to the metal oxide substrate.

9. The method of claim 1, the metal oxide comprising a porous metal oxide.

10. The method of claim 1, wherein the metal oxide is selected from the group consisting of zirconia, alumina, hafnia and titania.

11. The method of claim 10, the metal oxide comprising zirconia.

12. The method of claim 1, the metal oxide substrate comprising a particulate metal oxide, the particulate metal oxide comprising an average particle size of about 0.2 microns to about 1 millimeter.

13. The method of claim 1, the metal oxide substrate disposed within a housing, the operation of contacting the crude product mixture with a metal oxide substrate comprising pumping the crude product mixture into the housing.

14. The method of claim 1, wherein the step of contacting the crude product mixture with a metal oxide substrate is performed at a temperature less than about 100 degrees Celsius.

17. The method of claim 1, further comprising heating the metal oxide media up from a lower temperature to a temperature of greater than about 100 degrees Celsius after the step of separating the refined product mixture from the metal oxide substrate.

15. A method of regenerating a free fatty acid removal apparatus comprising

contacting saturated metal oxides disposed within the free fatty acid removal apparatus with a fatty acid alkyl ester composition at a temperature of greater than about 100 degrees Celsius, thereby releasing bound fatty acids from saturated metal oxides into the fatty acid alkyl ester composition.

16. The method of claim 15, contacting saturated metal oxides disposed within the free fatty acid removal apparatus with a fatty acid alkyl ester composition at a temperature of greater than about 150 degrees Celsius.