IP Library › Granted Patent US 9,181,144
Granted Patent B2
US 9,181,144 · App. 13/763,829 · Granted Nov 10, 2015

Diesel and jet fuels based on the oligomerization of butene

Inventors: Michael E. Wright (Tremonton, UT); Benjamin G. Harvey (Ridgecrest, CA); Roxanne L. Quintana (Ridgecrest, CA)
Assignee: The United States of America as Represented by the Secretary of the Navy
C07C2/08B01J31/143B01J31/189B01J31/2295C10G45/00C10G50/00C10G69/126C10L1/08B01J2231/20B01J2231/645B01J2531/46B01J2531/48B01J2531/49C10G2300/1011C10G2300/1092C10G2300/302C10G2300/308C10G2300/44C10G2300/703C10G2400/04C10G2400/22Y02E50/13
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Quick Facts
Patent No.
US 9,181,144
App. No.
13/763,829
Granted
Nov 10, 2015
Kind
B2
Abstract

A renewable biofuel based on a highly efficient batch catalysis methodology for conversion of 1-butene to a new class of potential jet fuel blends. By tuning the catalyst and then using the dimer produced, the carbon use is about 95% or greater. This latter point will be particularly important in the future, where the source of raw materials (i.e., biomass/biofeedstock) is limited.

Claims (41)

1. A process, comprising:

activating a Group 4 metallocene pre-catalyst with methylaluminoxane in a suitable solvent to produce an activated catalyst;

removing said solvent from said activated catalyst;

mixing at least one aromatic solvent, without heteroatoms, with activated catalyst to form a solution;

adding dried 1-butene to said solution;

allowing contact of said activated catalyst with 1-butene in a gas tight vessel to form a first mixture of butene oligomers;

removing by distillation C8 dimers to produce a second mixture of butene oligomers;

contacting of said second mixture of butene oligomers with a hydrogenation catalyst and hydrogen gas to create a third mixture of butene oligomers; and

fractional distilling of said third mixture of butene oligomers to afford a turbine and diesel fuel having a high flash point of >60° C. and a viscosity at −20° C. from about 6.0 cSt to about 12.5 cSt and a density from about 0.75 g/ml to about 0.80 g/ml.

2. The process according to claim 1 , wherein said C8 dimers are placed in contact with concentrated sulfuric acid to form a heterogenous fourth mixture;

stirring said fourth mixture to allow contact of reactants at ambient temperature until reaction is complete to form a reaction fifth mixture comprising an organic phase and an aqueous phase;

separating the organic phase from the aqueous phase of said fifth mixture; and

isolating butene C 16 oligomers from said organic phase.

3. The process according to claim 1 , wherein said C8 dimers are placed in contact with concentrated sulfuric acid to form a heterogenous fourth mixture;

stirring said fourth mixture to allow contact of reactants at temperatures from about 0-60° C. until reaction is complete to form a reaction fifth mixture comprising an organic phase and an aqueous phase;

separating the organic phase from the aqueous phase of said fifth mixture; and

isolating butene C 16 oligomers from said organic phase.

4. The process according to claim 1 , wherein said Group 4 metallocene catalyst is selected from the group consisting of at least one metal from titanium, zirconium, or hafnium.

5. The process according to claim 1 , wherein said at least one aromatic solvent is used having one aromatic ring and from 9 to 16 carbon atoms.

6. The process according to claim 1 , wherein said hydrogenation catalyst used has at least one metal taken from Group 10 of the periodic table.

7. The process according to claim 1 , wherein the pressure of said hydrogen gas is from about 10 psig to about 2000 psig.

8. The process according to claim 2 , further comprising contacting said C16 oligomers with a hydrogenation catalyst and hydrogen pressure to produce a mixture of C16 oligomers that are fully saturated with hydrogen.

9. A process, comprising:

activating a Group 4 metallocene pre-catalyst with methylaluminoxane in a suitable solvent to produce an activated catalyst;

removing said solvent from said activated catalyst;

mixing at least one aromatic solvent, without heteroatoms, with activated catalyst to form a solution;

adding dried 1-butene to the solution;

contacting of said activated catalyst with 1-butene in a gas tight vessel to form a first mixture of butene oligomers;

removing by distillation C8 dimers to produce a second mixture of butene oligomers;

contacting of said second mixture of butene oligomers with a hydrogenation catalyst and hydrogen gas to create a third mixture of butene oligomers;

contacting said C16 oligomers with a hydrogenation catalyst and hydrogen pressure to produce a fourth mixture of saturated C16 oligomers;

adding a mixture of saturated C16 oligomers to the third mixture of butene oligomers to create a forth mixture of butene oligomers; and

fractional distilling of the fourth mixture of butene oligomers to afford a turbine and diesel fuel having a high flash point of >60° C. and a viscosity at −20° C. from about 6.0 cSt to about 12.5 cSt and a density from about 0.75 g/ml to about 0.80 g/ml.

10. The process according to claim 9 , wherein said Group 4 metallocene catalyst is selected from the group consisting of at least one metal from titanium, zirconium, or hafnium.

11. The process according to claim 9 , wherein said at least one aromatic solvent is used having one aromatic ring and from 9 to 16 carbon atoms.

12. The process according to claim 9 , wherein said hydrogenation catalyst used has at least one metal taken from Group 10 of the periodic table.

13. The process according to claim 9 , wherein the pressure of said hydrogen gas is from about 10 psig to about 2000 psig.

14. The process according to claim 9 , wherein said C8 dimers are placed in contact with concentrated sulfuric acid to form a heterogenous fourth mixture;

stirring said fourth mixture to allow contact of reactants at temperatures from about 0-60° C. until reaction is complete to form a reaction fifth mixture comprising an organic phase and an aqueous phase;

separating the organic phase from the aqueous phase of said fifth mixture; and

isolating butene C 16 oligomers from said organic phase.

Assignments (1)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Feb 11, 2013
From: WRIGHT, MICHAEL E; HARVEY, BENJAMIN G; QUINTANA, ROXANNE
To: UNITED STATES OF AMERICA AS REPRESENTED BY THE SECRETARY OF THE NAVY
Reel/Frame 029787/0586 →
Continuity (2)
Continuation In Part 12511796 · Jul 29, 2009
Related Publication 20140051898A1 · Feb 20, 2014