IP Library Granted Patent US 12,146,110
Granted Patent B2
US 12,146,110 · App. 18/237,691 · Granted Nov 19, 2024

Method of manufacturing renewable diesel from biological feedstock

Inventors: Thomas Bass (Mandeville, LA); James Rolston (Friendswood, TX); Terry Sparkman (Beaumont, TX)
Assignee: Green Carbon Development, LLC
C10G3/46C10G3/50C11B3/006C11C1/04C11C1/10C11C3/12C10G2300/1011C10G2300/202C10G2300/4006C10G2300/4081C10G2300/708C10G2400/04
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Quick Facts
Patent No.
US 12,146,110
App. No.
18/237,691
Granted
Nov 19, 2024
Kind
B2
Abstract

A method for producing renewable diesel includes introducing a primary feedstock comprising biologically-derived triglycerides with catalyst poisons into a first reaction chamber and hydrolyzing the primary feedstock within the first reaction and liquid-liquid extraction chamber for at least an hour such that the reacted triglycerides are separated into an aqueous solution comprising glycerol and catalyst poisons, and an intermediate feedstock comprising free fatty acids and catalyst poisons. The method also includes distilling the intermediate feedstock to separate the intermediate feedstock into a purified intermediate stream and a lower volume bottom stream containing unreacted triglyceride, diglyceride, monoglyceride, FFA and catalyst poisons. The method also includes combining the purified intermediate feedstock with a hydrogen stream and converting, in a second reaction chamber comprising a metallic catalyst bed, the purified intermediate feedstock into a product comprising long-chain alkanes. The method also includes hydrotreating the purified intermediate feedstock into a renewable diesel product.

Claims (33)

1. A system for producing a renewable fuel comprising C10-C18 alkanes, the system comprising:

a first reaction chamber configured to:

receive a primary feedstock and up to 50% water under counter-current flow conditions, the primary feedstock comprising biologically-derived triglycerides and catalyst poisons;

hydrolyze the primary feedstock for at least an hour to form a hydrolysis effluent comprising (i) an aqueous solution comprising glycerol and a first portion of the catalyst poisons and (ii) an intermediate feedstock comprising free fatty acids and a second portion of the catalyst poisons, wherein the first reaction chamber is maintained at a temperature between 250° C. and 270° C. and a pressure between 700 psig and 900 psig; and

separate the intermediate feedstock and the aqueous solution;

a distillation column configured to:

receive the intermediate feedstock; and

distill the intermediate feedstock at an absolute pressure under 700 mm Hg to obtain a purified intermediate feedstock comprising free fatty acids and a bottom stream containing unreacted triglycerides, diglyceride, monoglyceride, free fatty acids, and at least a portion of the second portion of the catalyst poisons;

a second reaction chamber comprising a metallic catalyst and configured to hydrotreat the purified intermediate feedstock by contacting the purified intermediate feedstock with hydrogen to produce the renewable fuel comprising C10-C18 alkanes, wherein the hydrotreating is carried out at a temperature between 200° C. and 350° C. and a pressure between 300 and 1000 psig;

a purification unit configured to:

remove the at least the portion of the second portion of the catalyst poisons from the bottom stream to form a recycle stream containing unreacted triglycerides, diglyceride, monoglyceride, and free fatty acids; and

direct the recycle stream to the first reaction chamber.

2. The system of claim 1 , wherein, while hydrolyzing the triglycerides, the first reaction chamber is configured to be maintained under conditions sufficient to yield liquid-liquid extraction of the first portion of the catalyst poisons into the aqueous solution.

3. The system of claim 2 , wherein the first reaction chamber comprises internal components effective to yield a contacting surface area per volume of the first reaction chamber of not less than about 150 m 2 /m 3 .

4. The system of claim 2 , wherein the first reaction chamber comprises internal components effective to yield a contacting surface area per volume of the first reaction chamber of not less than about 200 m 2 /m 3 .

5. The system of claim 2 , wherein the first reaction chamber comprises internal components effective to yield a contacting surface area per volume of the first reaction chamber of not less than about 250 m 2 /m 3 .

6. The system of claim 2 , wherein the first reaction chamber comprises internal components effective to yield at least about 93% voidage.

7. The system of claim 2 , wherein the first reaction chamber comprises internal components effective to yield at least about 95% voidage.

8. The system of claim 2 , wherein the first reaction chamber comprises a plurality of stages.

9. The system of claim 2 , wherein the first reaction chamber comprises at least 4 stages.

10. The system of claim 1 , wherein the first reaction chamber is configured to hydrolyze the primary feedstock to produce a glycerol yield at least 95% of theoretical glycerol yield.

11. The system of claim 1 , further comprising a glycerol refinement stage.

12. The system of claim 11 , wherein the glycerol refinement stage is configured to:

separate the aqueous solution into a glycerol stream and water; and

return the water back into the first reaction chamber.

13. The system of claim 12 , wherein the glycerol refinement stage is configured to separate the aqueous solution into the glycerol stream and water by distillation.

14. The system of claim 1 , wherein the metallic catalyst comprises molybdenum, aluminum, nickel, cobalt, or a combination thereof.

15. The system of claim 1 , wherein the second reaction chamber is configured to hydrotreat the purified intermediate feedstock to produce a combined carbon dioxide yield of no more than 80% of a combined carbon dioxide yield than would be produced in the same reaction chamber during a hydrotreatment except with a triglyceride feedstock that was pretreated with bleaching earth.

16. The system of claim 1 , wherein the second reaction chamber is configured to receive the hydrogen at a throughput volume of no more than 80% of a hydrogen throughput volume than would be consumed in the same reaction chamber during hydrotreatment except with a triglyceride feedstock that was pretreated with bleaching earth.

17. The system of claim 1 , wherein the intermediate feedstock comprises less than 2 parts per million by weight (“ppmw”) phosphorous, 20 ppmw sulfur, and 30 ppmw nitrogen.

18. The system of claim 1 , wherein the renewable fuel comprising C10-C18 alkanes comprises at least 20% more even numbered straight-chain alkanes of length C14 or greater than would be produced in the same reaction chamber during hydrotreatment except with a triglyceride feedstock that was pretreated with bleaching earth.

19. The system of claim 1 , wherein the second reaction chamber is smaller in size than a reaction chamber as would be required to operate the same hydrotreating step except with a triglyceride feedstock pretreated with bleaching earth.

20. The system of claim 1 , wherein purification unit is configured to remove at least the portion of the second portion of the catalyst poisons from the bottom stream by subjecting the bottom stream to ion exchange, activated carbon, solvent extraction, centrifugation, chromatography, electrodeionization, zeolite, or combinations thereof.

Assignments (2)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Feb 24, 2024
From: BASS, THOMAS; SPARKMAN, TERRY; ROLSTON, JAMES
To: GREEN CARBON HOLDINGS, LLC
Reel/Frame 066552/0669 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Feb 24, 2024
From: GREEN CARBON HOLDINGS, LLC
To: GREEN CARBON DEVELOPMENT, LLC
Reel/Frame 066552/0678 →
Continuity (5)
Continuation 17856707 · Jul 1, 2022
Continuation In Part 17557329 · Dec 21, 2021
Provisional Application 63282804 · Nov 24, 2021
Provisional Application 63128526 · Dec 21, 2020
Related Publication 20230407185A1 · Dec 21, 2023