# US 10,501,698 B1 · Countercurrent and cross current high pressure extraction techniques for biodiesel fuel > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 10,501,698 B1 - Document ID: US10501698B1 - Status: Granted - Kind: B1 - Application number: 15/782,178 - Filed: 2017-10-12 - Granted: 2019-12-10 - Earliest claimed: 2016-10-12 - Assignees: University of South Florida - Applicants: James Cameron Walker - Inventors: James Cameron Walker - Web page: https://patentgrep.com/patent/US10501698B1 ## CPC - C10L 1/026: {for compression ignition} - B01D 11/0426: {Counter-current multistage extraction towers in a vertical or sloping position} - B01D 11/0488: {Flow sheets} - B01D 11/0492: {Applications, solvents used} - C11B 3/006: {by extraction} - C12P 7/649: Biodiesel, i.e. fatty acid alkyl esters - C10L 2290/544: Extraction for separating fractions, components or impurities during preparation or upgrading of a fuel - Y02E 50/10: Biofuels, e.g. bio-diesel - C10L: FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G OR C10K; LIQUIFIED PETROLEUM GAS; USE OF ADDITIVES TO FUELS OR FIRES; FIRE-LIGHTERS - B01D: SEPARATION (separating solids from solids by wet methods B03B, B03D; by pneumatic jigs or tables B03B; by other dry methods B07; magnetic or electrostatic separation of solid materials from solid materials or fluids, separation by high-voltage electric fields B03C; centrifuges, vortex apparatus B04; presses per se for squeezing-out liquid from liquid-containing material B30B9/02; treatment of water C02F, e.g. softening by ion-exchange C02F1/42; {arrangements of air intake cleaners in gas turbine plants F02C7/05} ; arrangements or mounting of filters in air-conditioning, air-humidification or ventilation F24F13/28) - C11B: PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES (drying-oils C09F) - C12P: FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE {(brewing of beer C12C; producing vinegar C12J; producing specific peptides or proteins C07K; producing enzymes C12N9/00; DNA or RNA concerning genetic engineering, vectors, e.g. plasmids, or their isolation, preparation or purification C12N15/00; measuring or testing processes involving enzymes or microorganisms C12Q; measuring or testing processes involving nucleic acid amplification reactions C12Q1/6844; fermentation processes to form a food composition, A21 or A23; compounds in general, see the relevant compound class, e.g. C01, C07)} - Y02E: REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION ## Abstract Methods of extracting biodiesel from a mixture of biodiesel and alcohol are provided. The methods can include contacting the mixture of biodiesel and alcohol with a petrodiesel to form a two-phase system including a polar phase and a nonpolar phase, wherein the alcohol preferentially partitions into the polar phase and the petrodiesel and biodiesel preferentially partition into the nonpolar phase, and separating the nonpolar phase from the polar phase to extract the biodiesel. The methods can include using a multi-stage extraction apparatus, for example in countercurrent or crosscurrent extraction arrangement. Methods of making a biodiesel blend are also provided. The methods can include making a biodiesel blend with a biodiesel content from about B2 to about B25. ## Claims ### Claim 1 A method of extracting biodiesel from a mixture of biodiesel and alcohol, the method comprising pumping the mixture into a first stage of a multi-stage liquid-liquid extraction apparatus having from 4 to 12 stages configured in a countercurrent or crosscurrent extraction arrangement with an operating pressure of about 80 bar to 140 bar and a pressure difference of from 0.5 bar to 5 bar applied across each stage, pumping a petrodiesel into a last stage of the multi-stage liquid-liquid extraction apparatus, removing a polar phase from the last stage of the multi-stage liquid-liquid extraction apparatus, wherein the polar phase comprises the alcohol, and removing a nonpolar phase from the first stage of the multi-stage liquid-liquid extraction apparatus, wherein the nonpolar phase comprises the petrodiesel and the biodiesel. ### Claim 2 (depends on 1) The method of claim 1, wherein the multi-stage liquid-liquid extraction apparatus comprises a plurality of stages configured in a crosscurrent extraction arrangement, wherein the method comprises pumping petrodiesel into each of the stages, wherein a two-phase system is formed in each stage, wherein the two-phase system includes a polar phase and a nonpolar phase, wherein the alcohol preferentially partitions into the polar phase and the petrodiesel and biodiesel preferentially partition into the nonpolar phase in each stage, wherein the method further comprises pumping the polar phase from each stage and into a next stage until exiting the last stage, and wherein the method further comprises removing the nonpolar phase from each stage to extract the biodiesel. ### Claim 3 (depends on 2) The method of claim 2, wherein the concentration of biodiesel in the mixture prior to the separation is about 2 mol % to about 20 mol %. ### Claim 4 (depends on 3) The method of claim 3, wherein the concentration of the biodiesel extracted in the nonpolar phase is about 5 mol % to about 30 mol % after the extraction. ### Claim 5 (depends on 4) The method of any claim 4, wherein the concentration of the biodiesel in the alcohol is about 500 ppm or less after the extraction. ### Claim 6 (depends on 2) The method of any claim 2, wherein the alcohol is selected from the group consisting of methanol, ethanol, 1-propanol, 2-propanol, 1-butanol, 2-ethoxyethanol, and a combination thereof. ### Claim 7 (depends on 1) The method of claim 1, wherein the multi-stage liquid-liquid extraction apparatus comprises a plurality of stages configured in a countercurrent extraction arrangement, wherein a two-phase system is formed in each stage, wherein the two-phase system includes a polar phase and a nonpolar phase, wherein the alcohol preferentially partitions into the polar phase and the petrodiesel and biodiesel preferentially partition into the nonpolar phase in each stage, wherein the method further comprises pumping the polar phase from each stage and into a next stage until exiting the last stage, and wherein the method further comprises pumping the nonpolar phase from each stage and into a preceding stage until exiting from the first stage to extract the biodiesel. ### Claim 8 (depends on 7) The method of claim 7, wherein the method is performed at a temperature from about 10° C. to about 150° C. ### Claim 9 (depends on 8) The method of claim 8, wherein the concentration of biodiesel in the mixture prior to the separation is about 2 mol % to about 20 mol %. ### Claim 10 (depends on 9) The method of claim 9, wherein the concentration of the biodiesel extracted in the nonpolar phase is about 5 mol % to about 30 mol % after the extraction. ### Claim 11 (depends on 10) The method of any claim 10, wherein the concentration of the biodiesel in the alcohol is about 500 ppm or less after the extraction. ### Claim 12 (depends on 7) The method of any claim 7, wherein the alcohol is selected from the group consisting of methanol, ethanol, 1-propanol, 2-propanol, 1-butanol, 2-ethoxyethanol, and a combination thereof. ### Claim 13 (depends on 1) A method of making a biodiesel blend, the method comprising extracting biodiesel from a mixture of biodiesel and alcohol using a petrodiesel, wherein the method is performed according to claim 1, and wherein the biodiesel blend has a biodiesel content from about B2 to about B25.