IP Library Granted Patent US 8,961,813
Granted Patent B2
US 8,961,813 · App. 13/586,953 · Granted Feb 24, 2015

Hydroxycarboxylic acids and salts

Inventors: Donald E. Kiely (Missoula, MT); Kirk R. Hash (Drummond, MT); Kylie Kramer-Presta (Missoula, MT); Tyler N. Smith (Missoula, MT)
Assignee: The University of Montana
C23F11/126C09K3/185C04B24/06C04B2103/61
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Quick Facts
Patent No.
US 8,961,813
App. No.
13/586,953
Granted
Feb 24, 2015
Kind
B2
Abstract

Compositions which inhibit corrosion and alter the physical properties of concrete (admixtures) are prepared from salt mixtures of hydroxycarboxylic acids, carboxylic acids, and nitric acid. The salt mixtures are prepared by neutralizing acid product mixtures from the oxidation of polyols using nitric acid and oxygen as the oxidizing agents. Nitric acid is removed from the hydroxycarboxylic acids by evaporation and diffusion dialysis.

Claims (51)

1. A method of preparing a deicing composition, the method comprising:

a) preparing an aqueous solution of at least one organic compound suitable for nitric acid oxidation;

b) combining, over time, the aqueous solution of the at least one organic compound and an aqueous solution of nitric acid to oxidize the at least one organic compound to a mixture of organic acids;

c) removing a portion of the nitric acid from the combined aqueous solution through an evaporation process; and

d) making basic with at least one base the solution from which nitric acid has been removed to convert residual nitric acid to inorganic nitrate and to convert the mixture of organic acids to a mixture of organic acid salts;

wherein a deicing agent is combined with the residual inorganic nitrate and the mixture of organic acid salts.

2. The method of claim 1 , wherein the deicing agent is selected from the group consisting of: sodium chloride, magnesium chloride, sodium acetate, potassium acetate, calcium magnesium acetate, and calcium chloride.

3. The method of claim 1 , wherein the organic compound has two or more alcohol hydroxyl groups.

4. The method of claim 3 , wherein the organic compound is glucose, xylose, fructose, glycerol, sorbitol, mannitol, maltose, lactose, cellobiose, maltotriose, maltotetrose, maltotetralose, sucrose, trehalose, stachyose, starch, cellulose, arabinogalactans, xylans, mannans, fructans or hemicelluloses.

5. The method of claim 4 , wherein the organic compound is glucose, xylose, fructose, sucrose, starch or glycerol.

6. The method of claim 1 , wherein at least one organic acid comprises glucaric acid, and the method further comprises the steps of, after step c): adding a potassium base to the solution from which nitric acid has been removed to neutralize residual nitric acid and to convert a portion of the glucaric acid to glucaric acid monopotassium salt; and removing at least some of the glucaric acid monopotassium salt from the at least one organic acid.

7. A method of preparing a deicing composition, the method comprising:

a) preparing an aqueous solution of at least one organic compound suitable for nitric acid oxidation;

b) combining, over time, the aqueous solution of the at least one organic compound and an aqueous solution of nitric acid to oxidize the at least one organic compound to a mixture of organic acids;

c) removing a portion of the nitric acid from the combined aqueous solution through an evaporation process;

d) making basic with at least one base the solution from which nitric acid has been removed to convert residual nitric acid to inorganic nitrate and to convert the mixture of organic acids to a mixture of organic acid salts; and

e) isolating from the mixture of organic acid salts an organic acid salt;

wherein a deicing agent is combined with the isolated organic acid salt or wherein a deicing agent is added to the mixture of organic acid salts and residual inorganic nitrate after isolating from the mixture of organic acid salts an organic acid salt.

8. The method of claim 7 , wherein the isolated organic acid salt is a glucaric acid salt.

9. The method of claim 7 , wherein the deicing agent is selected from the group consisting of: sodium chloride, magnesium chloride, sodium acetate, potassium acetate, calcium magnesium acetate, and calcium chloride.

10. The method of claim 7 , wherein the organic compound has two or more alcohol hydroxyl groups.

11. The method of claim 10 , wherein the organic compound is glucose, xylose, fructose, glycerol, sorbitol, mannitol, maltose, lactose, cellobiose, maltotriose, maltotetrose, maltotetralose, sucrose, trehalose, stachyose, starch, cellulose, arabinogalactans, xylans, mannans, fructans or hemicelluloses.

12. The method of claim 11 , wherein the organic compound is glucose, xylose, fructose, sucrose, starch or glycerol.

13. The method of claim 7 , wherein at least one organic acid comprises glucaric acid, and the method further comprises the steps of, after step c): adding a potassium base to the solution from which nitric acid has been removed to neutralize residual nitric acid and to convert a portion of the glucaric acid to glucaric acid monopotassium salt; and removing at least some of the glucaric acid monopotassium salt from the at least one organic acid.

14. A method of preparing a deicing composition, the method comprising:

a) preparing an aqueous solution of at least one organic compound suitable for nitric acid oxidation;

b) combining, over time, the aqueous solution of the at least one organic compound and an aqueous solution of nitric acid to oxidize the at least one organic compound to a mixture of organic acids;

c) removing a portion of the nitric acid from the combined aqueous solution through an evaporation process;

d) making basic with at least one base the solution from which nitric acid has been removed to convert residual nitric acid to inorganic nitrate and to convert the mixture of organic acids to a mixture of organic acid salts; and

e) isolating the mixture of organic acid salts as an amorphous solid;

wherein a deicing agent is combined with the amorphous solid.

15. The method of claim 14 , wherein the deicing agent is selected from the group consisting of: sodium chloride, magnesium chloride, sodium acetate, potassium acetate, calcium magnesium acetate, and calcium chloride.

16. The method of claim 14 , wherein the organic compound has two or more alcohol hydroxyl groups.

17. The method of claim 16 , wherein the organic compound is glucose, xylose, fructose, glycerol, sorbitol, mannitol, maltose, lactose, cellobiose, maltotriose, maltotetrose, maltotetralose, sucrose, trehalose, stachyose, starch, cellulose, arabinogalactans, xylans, mannans, fructans or hemicelluloses.

18. The method of claim 17 , wherein the organic compound is glucose, xylose, fructose, sucrose, starch or glycerol.

19. The method of claim 14 , wherein at least one organic acid comprises glucaric acid, and the method further comprises the steps of, after step c): adding a potassium base to the solution from which nitric acid has been removed to neutralize residual nitric acid and to convert a portion of the glucaric acid to glucaric acid monopotassium salt; and removing at least some of the glucaric acid monopotassium salt from the at least one organic acid.

20. A method of preparing a deicing composition, the method comprising:

a) preparing an aqueous solution of at least one organic compound suitable for nitric acid oxidation;

b) combining, over time, the aqueous solution of the at least one organic compound and an aqueous solution of nitric acid to oxidize the at least one organic compound to a mixture of organic acids;

c) removing a portion of the nitric acid from the combined aqueous solution through an evaporation process;

d) making basic with at least one base the solution from which nitric acid has been removed to convert residual nitric acid to inorganic nitrate and to convert the mixture of organic acids to a mixture of organic acid salts;

e) isolating the mixture of organic acid salts as an amorphous solid;

f) dissolving at least a portion of the amorphous solid in a solvent;

g) precipitating a solid precipitate from the solvent, the solid precipitate comprising one or more hydroxycarboxylic acid salts; and

h) recovering the solid precipitate;

wherein a deicing agent is combined with the recovered solid precipitate.

21. The method of claim 20 , wherein the deicing agent is selected from the group consisting of: sodium chloride, magnesium chloride, sodium acetate, potassium acetate, calcium magnesium acetate, and calcium chloride.

22. The method of claim 20 , wherein the organic compound has two or more alcohol hydroxyl groups.

23. The method of claim 22 , wherein the organic compound is glucose, xylose, fructose, glycerol, sorbitol, mannitol, maltose, lactose, cellobiose, maltotriose, maltotetrose, maltotetralose, sucrose, trehalose, stachyose, starch, cellulose, arabinogalactans, xylans, mannans, fructans or hemicelluloses.

24. The method of claim 23 , wherein the organic compound is glucose, xylose, fructose, sucrose, starch or glycerol.

25. The method of claim 20 , wherein at least one organic acid comprises glucaric acid, and the method further comprises the steps of, after step c): adding a potassium base to the solution from which nitric acid has been removed to neutralize residual nitric acid and to convert a portion of the glucaric acid to glucaric acid monopotassium salt; and removing at least some of the glucaric acid monopotassium salt from the at least one organic acid.

Assignments (2)
SECURITY INTEREST Recorded Jun 3, 2015
From: RIVERTOP RENEWABLES, INC.
To: SILICON VALLEY BANK
Reel/Frame 035777/0764 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Oct 29, 2014
From: KIELY, DONALD E.; HASH, KIRK R., SR.; KRAMER-PRESTA, KYLIE; SMITH, TYLER N.
To: THE UNIVERSITY OF MONTANA
Reel/Frame 034056/0902 →
Continuity (5)
Division 13277896 · Oct 20, 2011
Division 12422135 · Apr 10, 2009
Continuation In Part 11890760 · Aug 6, 2007
Provisional Application 60836329 · Aug 7, 2006
Related Publication 20120305832A1 · Dec 6, 2012