PURIFICATION METHODS OF ROSINS
Presently described are methods for performing rosin purification. The methods described herein utilize a unique solvent precipitation process that surprisingly and unexpectedly reduces the color of rosin and the sulfur and unsaponifiable contents in the rosin. The described methods are also applicable to rosin derivatives such as rosin esters and amides. Utilizing this purified rosin as raw material, rosin derivatives with much improved characteristics (color, softening point and sulfur content) can be made that would otherwise be difficult to make.
1 . A method for purification of a rosin comprising the steps of
a. admixing a rosin-containing composition and at least one first solvent;
b. heating the mixture to form a solution;
c. combining the solution with at least one second solvent;
d. cooling the solution from step (c); and
e. isolating a purified rosin precipitate,
wherein the purified rosin has at least one of: a Gardener color from about 1 to about 4 as measured according to ASTM D1544-04; a sulfur content of about 50 to about 500 ppm as measured according to X-ray fluorescence; an acid number equal to or greater than about 178 mg KOH/g according to ASTM D664, or a combination thereof.
2 . The method of claim 1 , wherein the first solvent is a rosin-favorable solvent, and the second solvent that is a rosin-unfavorable solvent.
3 . The method of claim 1 , wherein the first solvent to rosin-containing composition ratio is about 10:1 to about 1:1 by weight.
4 . The method of claim 2 , wherein the rosin-favorable solvent is at least one of an alcohol, chloroform, toluene, acetone, or a combination thereof.
5 . The method of claim 2 , wherein the rosin-unfavorable solvent is at least one of hexanes, petroleum ether, acetonitrile, benzonitrile, acrylonitrile, heptane, petroleum ether, or a combination thereof.
6 . The method of claim 1 , wherein the cooling step comprises cooling the mixture to a temperature of from about 30° C. to about −10° C.
7 . The method of claim 1 , wherein the yield of purified rosin is greater than 60%.
8 . The method of claim 1 , further comprising a drying step comprising air drying, oven drying, or a combination thereof.
9 . The method of claim 1 , wherein the purified rosin has at least one of: an acid content of from about 96 to about 100% as determined by gel permeation chromatography, a softening point of greater than about 85° C. according to ASTM 6090, or a combination thereof.
10 . The method of claim 1 , wherein the purified rosin has a percentage of palustric acid, a percentage of abietic acid, and a percentage of neoabietic acid, wherein the combined total of the percentages of palustric acid, abietic acid, and neoabietic acid is from about 50 to about 75% as determined by gas chromatography-mass spectroscopy.
11 . The method of claim 1 , wherein the purified rosin has a percentage of dehydroabietic acid of less than about 25% as determined by gas chromatography-mass spectroscopy.
12 . The method of claim 1 , wherein the purified rosin has a ratio of abietic acid to dehydroabietic acid of greater than about 1.5 as determined by gas chromatography-mass spectroscopy.
13 . A method for purification of a rosin using recycled solvent comprising the steps of
a. admixing a rosin-containing composition and a recycled solvent;
b. heating the mixture to form a solution;
c. cooling the solution from step (b); and
d. isolating a purified rosin precipitate,
wherein the purified rosin has at least one of: a Gardener color from about 1 to about 4 as measured according to ASTM D1544-04; a sulfur content of about 50 to about 500 ppm as measured by X-ray fluorescence; an acid number of equal to or greater than about 178 mg KOH/g according to ASTM D664, or a combination thereof.
14 . The method of claim 13 , wherein the recycled solvent is a mixture of a first rosin-favorable solvent and a second rosin-unfavorable solvent.
15 . The method of claim 14 , wherein the rosin-favorable solvent is at least one of an alcohol, chloroform, toluene, acetone, or a combination thereof.
16 . The method of claim 14 , wherein the rosin-unfavorable solvent is at least one of hexanes, petroleum ether, acetonitrile, benzonitrile, acrylonitrile, heptane, petroleum ether, water, or a combination thereof.
17 . The method of claim 13 , wherein the purified rosin has at least one of: an acid content of about 96 to about 100% as determined by gel permeation chromatography; or a softening point of greater than about 85° C. according to ASTM 6090.
18 . The method of claim 13 , wherein the purified rosin has a percentage of palustric acid, abietic acid, and neoabietic acid, wherein the combined total of the percentages of palustric acid, abietic acid, and neoabietic acid are from about 50 to about 75% as determined by gas chromatography-mass spectroscopy.
19 . The method of claim 13 , wherein the purified rosin has a percentage of dehydroabietic acid of less than about 25% as determined by gas chromatography-mass spectroscopy.
20 . The method of claim 13 , further comprising a drying step comprising air drying, oven drying, or a combination thereof.