Method for Separating Components in Natural Oil

Abstract

Different components of natural oils are separated by forming solid complexes of components of the natural oil with a solvent, and then separating the solid complexes from the remaining liquids. The natural oil is cooled in the presence of a solvent, and at least one component of the oil forms the solid complex with the solvent. This solid complex is separated from the remaining liquid portion of the oil solution, which also contains the solvent. Additional options concentration steps can further concentrate the components left in the liquid phase.

1 . A method of concentrating minor components present in crude natural oil comprising:
 (a) combining the crude natural oil and a solvent and cooling the resulting mixture to at a first cooling rate of greater than 1 degree Centigrade per minute and a second cooling rate of less than 1 degree Centigrade per minute to form a primarily amorphous solid complex of the oil and solvent in a liquid oil solution;   (b) separating the solid complex from the liquid oil solution to form a concentrated minor component oil separate from the solid complex;   (c) performing a chemical extraction on the concentrated minor component oil, wherein said chemical extraction is selected from the group consisting of a saponification or an esterification reaction; and   wherein the concentrated minor component oil comprises at least (i) 22% tocols and (ii) 7% b-carotene by weight after a final drying step.   
     
     
         2 . The method of  claim 1  where step (a) further comprises dissolving the crude natural oil in the solvent to form the oil solution; and batch cooling the oil solution. 
     
     
         3 . The method of  claim 1  where step (a) further comprises dissolving the crude natural oil in a limited quantity of solvent to form a concentrated oil solution; preparing a cold solvent bath comprising the solvent; and adding the concentrated oil solution to the cold solvent bath at a gradual rate to produce the solid complex. 
     
     
         4 . The method of  claim 1  where step (a) further comprises preparing a cold solvent bath comprising the solvent; and adding the crude natural oil in an undiluted state to the cold solvent bath at a gradual rate to form the solid complex. 
     
     
         5 . The method of  claim 1  further comprising further concentrating the minor components in the concentrated minor component oil after step (b). 
     
     
         6 . The method of  claim 5  further comprising adding a base to the concentrated minor component oil to form a fatty acid metal salt; adding water to the concentrated minor component oil to dissolve the fatty acid metal salts in a water phase; and splitting the water phase from an oil phase to further concentrate the minor components in the concentrated minor component oil. 
     
     
         7 . The method of  claim 6  further comprising esterification of the concentrated minor component oil to convert remaining natural oil triglycerides to separate fatty acid esters; and distillation of the concentrated minor component oil to separate the fatty acid esters from the minor components and thereby further concentrate the minor components in the concentrated minor component oil. 
     
     
         8 . The method of  claim 5  further comprising evaporation of solvent from the concentrated minor component oil to further concentrate the minor components in the concentrated minor component oil. 
     
     
         9 . The method of  claim 1  where step (b) further comprises filtering the oil mixture to separate the solid complex from the liquid solution and form the liquid concentrated minor component oil. 
     
     
         10 . The method of  claim 1  where step (b) further comprises centrifuging the oil mixture to separate the solid complex from the liquid solution and forming the liquid concentrated minor component oil. 
     
     
         11 . The method of  claim 1  where the solvent has a dielectric constant at 25 degrees centigrade of between about 6 and 30. 
     
     
         12 . The method of  claim 1  where the solvent is selected from the group consisting of an organic alcohol containing 1 to 10 carbons, acetone, ethyl acetate, water, and any mixture thereof. 
     
     
         13 . The method of  claim 1  where the solvent comprises ethanol. 
     
     
         14 . The method of  claim 1  where the crude natural oil comprises crude palm oil. 
     
     
         15 . The method of  claim 1  where the minor components are concentrated by at least a factor of 10. 
     
     
         16 . A method for separating different components from a crude natural oil comprising:
 (a) cooling crude natural oil in a solvent to at least at a rate of greater than 1 degree Centigrade per minute to form a primarily amorphous solid complex of the oil and solvent in a liquid oil solution, where the oil solution comprises the natural oil and the solvent;   (b) separating the solid complex from the liquid oil solution; and   (c) collecting the solid complex; and   (d) performing a chemical extraction on the liquid oil solution, wherein said chemical extraction is selected from the group consisting of a saponification or an esterification reaction;   wherein the liquid oil solution comprises at least 7% b-carotene by weight after a final drying step.   
     
     
         17 . The method of  claim 16  where the crude natural oil comprises a first component and a second component, where the first component forms a first solid complex with the solvent and the second component forms a second solid complex with the solvent, and where the method further comprises separating the first and second solid complexes from each other. 
     
     
         18 . The method of  claim 17  where steps (a) and (b) further comprises:
 cooling the oil solution to below a first solid complex formation temperature to form a first solid complex; then 
 separating the first solid complex from the liquid oil solution; and then 
 cooling the oil solution to below a second solid complex formation temperature lower than the first solid complex formation temperature to form the second solid complex. 
 
     
     
         19 . The method of  claim 16  further comprising
 (d) heating the collected solid complex to a temperature above a second solid complex formation temperature and below a first solid complex formation temperature after step (c), so the second solid complex becomes liquid; and 
 (e) separating the remaining solid complex from the liquids after step (d). 
 
     
     
         20 . The method of  claim 16  where the crude natural oil is crude palm oil comprising a first component and a second component, and where the first component comprises stearin oil and the second component comprises olein oil. 
     
     
         21 . The method of  claim 16  further comprising the step of separating the solvent from the solid complex. 
     
     
         22 . The method of  claim 16  where step (a) further comprises dissolving the natural oil in the solvent to form the oil solution; and batch cooling the oil solution. 
     
     
         23 . The method of  claim 16  where step (a) further comprises dissolving the crude natural oil in a limited quantity of solvent to form a concentrated oil solution; preparing a cold solvent bath comprising a solvent; and adding the concentrated oil solution to the cold solvent bath at a gradual rate to produce the solid complex. 
     
     
         24 . The method of  claim 16  where step (a) further comprises preparing a cold solvent bath comprising a solvent; and adding the natural oil in an undiluted state to the cold solvent bath at a gradual rate to form the solid complex. 
     
     
         25 . The method of  claim 16  where step (b) further comprises filtering the oil solution to separate the solid complex from the liquid oil solution. 
     
     
         26 . The method of  claim 16  where step (b) further comprises centrifuging the oil solution to separate the solid complex from the liquid oil solution. 
     
     
         27 . The method of  claim 16  where the solvent comprises a protic solvent. 
     
     
         28 . The method of  claim 16  where the solvent comprises ethanol. 
     
     
         29 . The method of  claim 16  wherein step (a) comprises cooling the crude natural oil and solvent solution to at least −40 degrees Centigrade. 
     
     
         30 . The method of  claim 16  liquid oil solution less than 50% free fatty acids by weight after the final drying step. 
     
     
         31 . The method of  claim 30  wherein the liquid oil solution comprises at least one of the following: 8% phytosterol, 3% lutein, 15% squalene or 0.5% co-enzyme Q10 after the final drying step. 
     
     
         32 . A concentrated minor component oil composition comprising minor components present in crude natural oil prepared a process comprising the steps of:
 (a) combining the crude natural oil and a solvent and cooling the resulting mixture to at a first cooling rate of greater than 1 degree Centigrade per minute and a second cooling rate of less than 1 degree Centigrade per minute to form a primarily amorphous solid complex of the oil and solvent in a liquid oil solution;   (b) separating the solid complex from the liquid oil solution to form the concentrated minor component oil separate from the solid complex;   (c) performing a chemical extraction on the concentrated minor component oil, wherein said chemical extraction is selected from the group consisting of a saponification or an esterification reaction; and   wherein the concentrated minor component oil comprises at least (i) 22% tocols and (ii) 7% b-carotene by weight after a final drying step.   
     
     
         33 . The concentrated minor component oil composition of  claim 32  further comprising less than 50% free fatty acids by weight after the final drying step. 
     
     
         34 . The concentrated minor component oil composition of  claim 35  further comprising at least one of the following: 8% phytosterol, 3% lutein, 15% squalene or 0.5% co-enzyme Q10 after the final drying step. 
     
     
         35 . The concentrated minor component oil composition of  claim 32  where step (a) of the process further comprises: dissolving the crude natural oil in the solvent to form the oil solution; and batch cooling the oil solution. 
     
     
         36 . The concentrated minor component oil composition of  claim 32  where step (a) further comprises dissolving the crude natural oil in a limited quantity of solvent to form a concentrated oil solution preparing a cold solvent bath comprising the solvent; and adding the concentrated oil solution to the cold solvent bath at a gradual rate to produce the solid complex. 
     
     
         37 . The concentrated minor component oil composition of  claim 32  where step (a) further comprises preparing a cold solvent bath comprising the solvent; and adding the crude natural oil in an undiluted state to the cold solvent bath at a gradual rate to form the solid complex. 
     
     
         38 . The concentrated minor component oil composition of  claim 32  where the process further comprises concentrating the minor components in the concentrated minor component oil after step (b). 
     
     
         39 . The concentrated minor component oil composition of  claim 38  where the process further comprises: adding a base to the concentrated minor component oil to form a fatty acid metal salt; adding water to the concentrated minor component oil to dissolve the fatty acid metal salts in a water phase; and splitting the water phase from an oil phase to further concentrate the minor components in the concentrated minor component oil. 
     
     
         40 . The concentrated minor component oil composition of  claim 39  where the process further comprises: esterification of the concentrated minor component oil to convert remaining natural oil triglycerides to separate fatty acid esters; and distillation of the concentrated minor component oil to separate the fatty acid esters from the minor components and thereby further concentrate the minor components in the concentrated minor component oil. 
     
     
         41 . The concentrated minor component oil composition of  claim 40  where the process further comprises: evaporation of solvent from the concentrated minor component oil to further concentrate the minor components in the concentrated minor component oil. 
     
     
         42 . The concentrated minor component oil composition of  claim 32  where the solvent used in the process has a dielectric constant at 25 degrees centigrade of between about 6 and 30. 
     
     
         43 . The concentrated minor component oil composition of  claim 42  where the solvent is selected from the group consisting of an organic alcohol containing 1 to 10 carbons, acetone, ethyl acetate, water, and any mixture thereof. 
     
     
         44 . The concentrated minor component oil composition of  claim 42  where the solvent comprises ethanol. 
     
     
         45 . The concentrated minor component oil composition of  claim 42  where the crude natural oil comprises crude palm oil.