Purification of biodiesel with adsorbent materials

• US 7,635,398 B2
• Filed: 10/01/2004
• Issued: 12/22/2009
• Est. Priority Date: 10/09/2003
• Status: Active Grant

• Current Assignee: The Dallas Group of America Incorporated
• Original Assignee: The Dallas Group of America Incorporated
• Inventors: Abrams, Christopher, Bertram, Bryan, Cooke, Brian S.
• Primary Examiner(s): McAvoy; Ellen M
• Application Number:
  US10/956,856
• Publication Number:
  US 20050081436A1
• Time in Patent Office: 1,908 Days
• Field of Search: 554/191, 554/192, 446/05, 443/20
• US Class Current: 44/605
• 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 20/10 comprising silica or silicate
• CPC Class Codes: B01J 20/28004 Sorbent size or size distribution, e.g. particle size
• CPC Class Codes: B01J 20/28011 Other properties, e.g. density, crush strength
• CPC Class Codes: B01J 20/28057 Surface area, e.g. B.E.T specific surface area
• CPC Class Codes: C07C 67/56 by solid-liquid treatment; by chemisorption
• CPC Class Codes: C07C 69/24 esterified with monohydroxylic compounds
• CPC Class Codes: C07C 69/52 Esters of acyclic unsaturated carboxylic acids having the esterified carboxyl group bound to an acyclic carbon atom
• CPC Class Codes: C10L 1/026 for compression ignition
• CPC Class Codes: C11C 1/08 Refining
• CPC Class Codes: Y02E 50/10 Biofuels, e.g. bio-diesel

Abstract

A method of purifying a biodiesel fuel by contacting the biodiesel fuel with at least one adsorbent material, such as magnesium silicate. Such method removes impurities, such as soap, formed during the production of biodiesel fuels.

Claims

1. A method of purifying a crude biodiesel fuel, comprising:

contacting said crude biodiesel fuel with at least one adsorbent material, wherein said at least one adsorbent material comprises magnesium silicate, and wherein said biodiesel fuel is a product of reacting triglycerides with an alcohol, thereby providing a purified biodiesel fuel which includes at least one monoalkyl fatty acid ester.

2. The method of claim 1 wherein said magnesium silicate has magnesium silicate has surface area of at least 300 square meters per gram.

3. The method of claim 2 wherein said magnesium silicate has a surface area of at least 400 to about 700 square meters per gram.

4. The method of claim 2 wherein said magnesium silicate has a particle size of from about 20 microns to about 175 microns.

5. The method of claim 2 wherein said magnesium silicate has a bulk density of from about 15 to about 35 pounds per cubic foot.

6. The method of claim 1 wherein said magnesium silicate is an amorphous hydrous precipitated synthetic magnesium silicate, said magnesium silicate having been treated to reduce the pH thereof to less than about 9.0.

7. The method of claim 6 wherein said magnesium silicate has a pH in a 5% slurry of from about 8.2 to about 8.9.

8. The method of claim 7 wherein said magnesium silicate has a pH in a 5% slurry of from about 8.5 to about 8.8.

9. The method of claim 1 wherein said magnesium silicate has a surface area of no more than 150 square meters per gram.

10. The method of claim 9 wherein said magnesium silicate has a surface area of from about 50 square meters per gram to about 150 square meters per gram.

11. The method of claim 10 wherein said magnesium silicate has a mole ratio of MgO to SiO₂ of from about 1:

3.0 to about 1;

3.8 and a pH in a 5% water suspension of from about 9.5 to about 10.5.

12. The method of claim 1 wherein said magnesium silicate has a pH of from about 9.0 to about 9.5.

13. The method of claim 1 wherein said crude biodiesel fuel is contacted with said magnesium silicate in an amount of from about 0.01 wt.% to about 20.0 wt.%, based on the weight of said biodiesel fuel.

14. The method of claim 13 wherein said crude biodiesel fuel is contacted with said magnesium silicate in an amount of from about 0.5 wt.% to about 4.0 wt.%, based on the weight of said biodiesel fuel.

15. The method of claim 1 wherein free fatty acids are removed from said crude biodiesel fuel.

16. The method of claim 1 wherein chlorophyll is removed from said crude biodiesel fuel.

17. The method of claim 1 wherein methanol is removed from said crude biodiesel fuel.

18. The method of claim 17 wherein said methanol is trace methanol.

19. The method of claim 1 wherein glycerin is removed from said crude biodiesel fuel.

20. The method of claim 1 wherein unreacted catalyst is removed from said crude biodiesel fuel.

21. A method for treating a crude biodiesel fuel, said biodiesel fuel including a fatty acid methyl ester, said fatty acid methyl ester having been prepared by reacting methanol with triglycerides in the presence of a catalyst, said method comprising:

treating said crude biodiesel fuel with magnesium silicate to remove one or more of soap, unreacted catalyst, sulfur, phosphorus, calcium, iron, monoglycerides, diglycerides, polymeric triglycerides, acidic compounds, glycerin, chlorophyll, water, sediment, and remaining methanol.

22. The method of claim 21 wherein said magnesium silicate has a surface area of at least 300 square meters per gram.

23. The method of claim 22 wherein said magnesium silicate has a particle size of from about 20 microns to about 175 microns.

24. The method of claim 21 wherein said magnesium silicate is an amorphous hydrous precipitated synthetic magnesium silicate, said magnesium silicate having been treated to reduce the pH thereof to less than about 9.0.

25. The method of claim 21 wherein said crude biodiesel fuel is contacted with said magnesium silicate in an amount of from about 0.01 wt. % to about 20.0 wt. %, based on the weight of said biodiesel fuel.

26. The method of claim 25 wherein said crude biodiesel fuel is contacted with said magnesium silicate in an amount of from about 0.5 wt. % to about 4.0 wt. %, based on the weight of said biodiesel fuel.

27. A method of purifying a crude biodiesel fuel, wherein said crude biodiesel fuel is produced by reacting triglycerides with an alcohol in the presence of an alkali catalyst, thereby producing a crude biodiesel fuel including at least one monoalkyl fatty acid ester and at least one impurity including soap, said method comprising:

contacting said crude biodiesel fuel with at least one adsorbent material, wherein said at least one adsorbent material comprises magnesium silicate, thereby removing soap from said crude biodiesel fuel.

28. The method of claim 27 wherein said contacting of said crude biodiesel fuel with said at least one adsorbent material further removes at least one of unreacted catalyst, sulfur, phosphorus, calcium, iron, monoglycerides, diglycerides, polymeric triglycerides, acidic compounds, glycerin, chlorophyll, water, sediment, and remaining methanol from said crude biodiesel fuel.

29. The method of claim 28 wherein chlorophyll is removed from said crude biodiesel fuel.

30. The method of claim 28 wherein remaining methanol is removed from said crude biodiesel fuel.

31. The method of claim 28 wherein glycerin is removed from said crude biodiesel fuel.

32. The method of claim 28 wherein unreacted catalyst is removed from said crude biodiesel fuel.

39. The method of claim 27 wherein said magnesium silicate has a surface area of at least 300 square meters per gram.

40. The method of claim 27, wherein said magnesium silicate has a particle size of from about 20 microns to about 175 microns.

41. The method of claim 27, wherein said magnesium silicate is an amorphous, hydrous, precipitated magnesium silicate, said magnesium silicate having been treated to reduce the pH thereof to less than about 9.0.

42. The method of claim 27, wherein said crude biodiesel fuel is contacted with said magnesium silicate in an amount of from about 0.01 wt.% to about 20.0 wt.%, based on the weight of said biodiesel fuel.

43. The method of claim 42, wherein said crude biodiesel fuel is contacted with said magnesium silicate in an amount of from about 0.5 wt.% to about 4.0 wt.%, based on the weight of said biodiesel fuel.

33. A method of purifying a crude biodiesel fuel, said biodiesel fuel including a monoalkyl fatty acid ester, said monoalkyl fatty acid ester having been prepared by reacting triglycerides with an alcohol, said method comprising:

contacting said crude biodiesel fuel with at least one adsorbent material, wherein said at least one adsorbent material comprises magnesium silicate, and wherein during said purifying of said crude biodiesel fuel, said crude biodiesel fuel is not contacted with water.

34. The method of claim 33 wherein one or more of soap, unreacted catalyst, sulfur, phosphorus, calcium, iron, monoglycerides, diglycerides, polymeric triglycerides, acidic compounds, glycerin, chlorophyll, water, sediment, and remaining methanol is removed from said crude biodiesel fuel.

35. The method of claim 34 wherein soap is removed from said crude biodiesel fuel.

36. The method of claim 34 wherein chlorophyll is removed from said crude biodiesel fuel.

37. The method of claim 34 wherein remaining methanol is removed from said crude biodiesel fuel.

38. The method of claim 34 wherein glycerin is removed from said biodiesel fuel.

44. The method of claim 33 wherein said magnesium silicate has a surface area of at least 300 square meters per gram.

45. The method of claim 33, wherein said magnesium silicate has a particle size of from about 20 microns to about 175 microns.

46. The method of claim 33, wherein said magnesium silicate is an amorphous hydrous, precipitated magnesium silicate, said magnesium silicate having been treated to reduce the pH thereof to less than about 9.0.

47. The method of claim 33, wherein said crude biodiesel fuel is contacted with said magnesium silicate in an amount of from about 0.01 wt.% to about 20.0 wt.%, based on the weight of said biodiesel fuel.

48. The method of claim 47, wherein said crude biodiesel fuel is contacted with said magnesium silicate in an amount of from about 0.5 wt.% to about 4.0 wt.%, based on the weight of said biodiesel fuel.