# US 8,540,880 B1 · Pretreatment of biodiesel feedstock

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- Number: US 8,540,880 B1
- Document ID: US8540880B1
- Status: Granted
- Kind: B1
- Application number: 13/686,728
- Filed: 2012-11-27
- Granted: 2013-09-24
- Earliest claimed: 2012-11-27
- Assignees: Menlo Energy Management, LLC
- Applicants: Menlo Energy Management, LLC
- Inventors: Gaurav Shah; Sunil Suri
- Web page: https://patentgrep.com/patent/US8540880B1

## CPC

- C10L 1/026: {for compression ignition}
- B01D 15/361: {Ion-exchange}
- 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)
- Y02E: REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION

## Abstract

Process and steps for the production of biodiesel and/or glycerin from feedstock are provided.

## Claims

### Claim 1

A method of purifying a biodiesel feedstock, the method comprising the steps in the order recited:
(a) filtering a biodiesel feedstock, thereby separating from the feedstock solid particles having a diameter up to 2 microns, to provide a filtrate and a retentate;
(b) separating water from the filtrate, to provide a dried filtrate;
(c) distilling the dried filtrate, to provide a distillate and a residue;
(d) distilling the distillate to provide a subsequent distillate and optionally a subsequent residue; and;
(e) passing the subsequent distillate through an ion exchange resin to obtain a purified biodiesel feedstock;
wherein the biodiesel feedstock comprises at least one of edible oils, inedible oils, fats, greases, brown grease, trap grease, used cooking oil, used cooking fat, animal fat, animal grease, and fatty acid distillate; and
wherein the following are substantially separated from the biodiesel fuelstock in steps (a) through (e), as present; sulfur, phosphorus, gums/lipids, sterols, calcium, magnesium, iron, copper, cobalt, manganese, nickel, sodium, potassium, chlorophyll, carotenoids, xanthophylls, proteins, carbohydrates, aldehydes, ketones, carboxylic acids, perchloroethylene, polyaromatic hydrocarbons, polychlorinated hydrocarbons, polymerized triglycerides, pesticides, soaps, detergents, sulfonates, sulfates, phosphatides, phytosterols, sitosterols, cholesterol, and sterol glucosides.

### Claim 2 (depends on 1)

The method of claim 1, wherein the biodiesel feedstock comprises elevated levels at least one of triglycerides, gums, soaps, detergents, unsaponifiables, phosphatides, metals, phosphorus, sulfur, sulfates, sulfonates, sulfides, polyaromatic hydrocarbons, polychlorinated hydrocarbons, polyethylene, plant based sterols, and animal based sterols.

### Claim 3 (depends on 1)

The method of claim 1, wherein the feedstock comprises at least about 40 wt. % free fatty acids.

### Claim 4 (depends on 1)

The method of claim 1, wherein at least about 90 wt. % of the solid particles having a diameter of at least about 2 microns are separated, to provide the filtrate and the retentate.

### Claim 5 (depends on 1)

The method of claim 1, wherein the separating of the solid particles is carried out employing multiple filters, each having a smaller porosity or mesh size relative to a previous filter.

### Claim 6 (depends on 1)

The method of claim 1, wherein the biodiesel feedstock comprises elevated levels of at least one of water, sulfur, phosphorus, gums/lipids, sterols, calcium, magnesium, iron, copper, cobalt, manganese, nickel, sodium, potassium, chlorophyll, carotenoids, xanthophylls, proteins and carbohydrates, aldehydes, ketones, carboxylic acids, perchloroethylene, polyaromatic hydrocarbons, polychlorinated hydrocarbons, polymerized triglycerides, pesticides, soaps, detergents, sulfonates, sulfates, phosphatides, phytosterols, sitosterols, cholesterol, and sterol glucosides.

### Claim 7 (depends on 1)

The method of claim 1, wherein the feedstock comprises up to about 20,000 ppm of at least one of sulfur, sulfates, sulfides, and sulfonates.

### Claim 8 (depends on 1)

The method of claim 1, wherein the feedstock comprises up to about 4000 ppmw phosphorus.

### Claim 9 (depends on 1)

The method of claim 1, wherein the distilling in at least one of steps (c) and (d) is carried out under vacuum.

### Claim 10 (depends on 1)

The method of claim 1, wherein relative to the subsequent distillate, the subsequent residue is enriched in at least one of sulfur, phosphorus, gums/lipids, sterols, calcium, magnesium, iron, copper, cobalt, manganese, nickel, sodium, potassium, chlorophyll, carotenoids, xanthophylls, proteins and carbohydrates, aldehydes, ketones, carboxylic acids, perchloroethylene, polyaromatic hydrocarbons, polychlorinated hydrocarbons, polymerized triglycerides, pesticides, soaps, detergents, sulfonates, sulfates, phosphatides, phytosterols, sitosterols, cholesterol, sterol glucosides, oils, and fats.

### Claim 11 (depends on 1)

The method of claim 1, wherein relative to the subsequent residue, the subsequent distillate is enriched in at least one of triglycerides and free fatty acids.

### Claim 12 (depends on 1)

The method of claim 1, wherein the subsequent distillate comprises up to about 99.995 wt. % triglycerides and free fatty acids.

### Claim 13 (depends on 1)

The method of claim 1, wherein the subsequent distillate comprises at least one of triglycerides and free fatty acids, wherein the at least one of triglycerides and free fatty acids combined comprise less than about 7 ppm phosphorus, less than about 7 ppm sulfur, and less than about 10 ppm of all other metals combined.

### Claim 14 (depends on 1)

The method of claim 1, wherein the subsequent distillate comprises at least one of triglycerides and free fatty acids, wherein the at least one of triglycerides and free fatty acids combined comprise less than about 7 ppm sulfur.

### Claim 15 (depends on 1)

The method of claim 1, wherein a weight of the retentate is up to about 0.2% of a weight of the feedstock.

### Claim 16 (depends on 1)

The method of claim 1, wherein the distilling in at least one of steps (c) and (d) comprises a multi-stage distillation column.

### Claim 17 (depends on 1)

The method of claim 1, wherein up to about 1,000 gallons of biodiesel feedstock is employed in step (a).

### Claim 18 (depends on 1)

The method of claim 1, wherein at least about 100 gallons of the purified biodiesel feedstock is obtained in step (e), within 24 hours.

### Claim 19 (depends on 1)

The method of claim 1, wherein prior to step (a), the biodiesel feedstock is analyzed to determine a qualitative nature of impurities located therein.

### Claim 20 (depends on 1)

The method of claim 1, wherein prior to step (a), the biodiesel feedstock is analyzed to determine a quantitative nature of impurities located therein.

### Claim 21 (depends on 1)

The method of claim 1, wherein none of steps (a)-(e) comprise adding water.

### Claim 22 (depends on 1)

The method of claim 1, wherein the subsequent distillate and the subsequent residue are separated.

### Claim 23 (depends on 1)

The method of claim 1, further comprising repeating at least one of steps (c) and (d), one or more times, by distilling the subsequent distillate, to obtain a final distillate.

### Claim 24 (depends on 1)

The method of claim 1, wherein the feedstock comprises at least one of tallow, pork fat, poultry fat, lard, choice white grease, algae oil, crude vegetable oils, soybean oil, corn oil, coffee oil, hemp oil, linseed oil, rice bran oil, jojoba oil, tall oil, mustard oil, distillers grain oil (DDG corn oil), Jatropha oil, camellia oil, rapeseed oil, canola oil, moring a oil, pongamia oil, sunflower oil, safflower oil, crude palm oil, palm kernel oil, palm fatty acid distillate, palm sludge oil, and coconut oil.

### Claim 25 (depends on 1)

The method of claim 1, wherein the feedstock comprises about 0.2 wt. % to about 100 wt. % free fatty acids.

### Claim 26 (depends on 1)

The method of claim 1, wherein the purified biodiesel feedstock comprises at least one of triglycerides and free fatty acids, wherein the at least one of triglycerides and free fatty acids combined comprise less than about 7 ppm phosphorus, less than about 7 ppm sulfur, and less than about 10 ppm of all other metals combined.

### Claim 27 (depends on 1)

The method of claim 1, wherein the purified biodiesel feedstock comprises at least one of triglycerides and free fatty acids, wherein the at least one of triglycerides and free fatty acids combined comprise less than about 7 ppm sulfur.

### Claim 28 (depends on 1)

The method of claim 1, wherein the ion exchange resin includes a straight, flow-through 2 stage guard bed column reactors in series.

### Claim 29 (depends on 1)

The method of claim 1, wherein steps (a)-(e) are carried out in the absence of a mineral acid.
