USRE19749E - Method of extracting rosin from - Google Patents

Description

Reissued Nov. v 12, 1935' UNITED STATES warrior) or nxmc'rnro nosmmom ruzsmous woen Leavitt N. Bent, Holly on. M, assignor m ner- Wilmington,

cules Powder Company,

corporation of Delaware No Drawing Original No. 1,sas,oz5, dated November 15, 1932, Serial No. 254,622, February Application for reissue September 8,

1934, Serial No. 743,185

ISCIiI-lilil.

My invention relates toa method for extracting rosin from wood. I

As is well known,"a principal source of rosin is in stumps and down wood 01' the long lea! pine 5 harvested i'rom cut over lands and subjected in a comminuted state to treatment tor the removal oi turpentine and pine oil and then to extractionwith gasoline, which acts to dissolve out rosin. 10 In accordance with prior practice the stumps and down wood are comminuted to a suitable size and loaded into retorts or extractors in which the turpentine and part or the pine oil are removed by the use of live steam. The Wood is then is subjected to extraction with a solvent, as a low boiling, petroleum hydrocarbon, which acts to dissolve out the remaining pine oil and the rosin.

"30 final steaming of the wood to effect separation of the solvent from the spent wood must be continually-rejected from the system. Heretoiore, petroleum-naphtha; or gasoline, has been considered the most satisfactory solvent, but such v is found to be open to a number oi! objections chief among which are that it is capable 01' extractlng in the cold only about 75% of the resinous materialpresent in the wood, and that when heated it constitutes a fire risk and re-;

4 quires a particulalr type of apparatus @101 its Now, in, accordance with my invention, I

eflect the extraction 0! the resinous material 45 from wood by the use of a cold, water'miscible mixed with; acertain 'amountiori water, the concentrationoi the solvent being'sudhthat it will dissolve out all were resinous from the vwood andattheflsame time of; a cbncen' "tration such that wheng't irther diluted, y -moisture' in th 'e'wood, it may in substantially its concentration bydistillation trom'a -simplestil1.

5;; Assolvents, the use or which I contemplate-in solvent, and moreparticularly, 5 such a solvent the foregoing, example.

accordance with my invention, may be mentioned, for example, acetone, alcohol, methanol and the like, and the treatment of the wood with one or another of the water miscible solvents in accordance with my invention may be in accordance 5 with the usual practice at atmospheric or increased pressure and withthe use oi any ordinary .or desirable form of apparatus; The solvent when used will, as has been indicated, be mixed withwater to aconcentratlon enabling its recovery at substantially its original concentration by distillation from asimple still anddepending upon. the particular solvent selected may be mixed with water to a concentration of solvent within, for example, about the range 65%-90%. More specifically, acetone may be desirably used at a concentration of about 75%, alcohol at about Y80% and methanol at about 80%.

As aspecific example of the carrying out of the'me'thod in accordance with my invention wood chips, which normally contain about 15% 18% of moisture, are steamed in the usual manner for distillation ofl oi. turpentine, and

after steaming will contain about 20% of moisture. The wood chips after steaming are ex- 25 tracted with, 'for example, acetone mixed with water to a concentration of about 75%. The acetone during the process of extraction and solvent recovery will pick up suillcient moisture-from the wood chips to reduce its concentration from to about 70% and may be completely re-. covered as acetone by rimning it through a simple still in which the solvent will be separated from the rosin extracted.

As a further example of the carrying out of the 35 method in accordance with my invention, pounds of pine wood, suitabLv chipped; is extracted with say 232 pounds of asolution oi. acetone in water of a concentration of say, for I example,'86% acetone. During the extraction heat may be applied, through it will be understoodthat the application of. heat is not necessary. The extraction may be carried out at atmospheric pressure. After a suitable period the acetone "solution, -.together with extracted 4 rosin, is drained from the wood and the woodmay be, re-extracted with say 235 pounds of 86% acetone solution, which in turn'isdrained Iromthe' wood and. ii desired, third, fourth and even firth my extractions may" be eflected. Extraction with) 86% acetone solution, using say five extractions,

will be iound to remove from. 99% to 100% or the-aoetonesoluble'rosin, or about 23 pounds in the like,j than heretofore.

As an alternative method there may be added to the dilute acetone solution of rosin sufiicient butane, pentane, or other water immiscible low boiling petroleum hydrocarbon, which is not miscible with the solvent, as'acetone, used for extracting the wood, and which ,has a greater sol-vent power on the rosin than has the solvent used for extraction of the wood in a closed vessel to prevent the volatilizing of the butane, to extract from this dilute acetone solution of rosin the rosin content. Butaneand dilute acetonebeing substantially immiscible, two layers will be formed on settlement, the upper layer being a butane solution of rosin, the lower being a dilute acetone solution containing dark colored resinous bodies. The lower layer is drawn oi! and distilled to rid it oi' the excess water picked up from the wood chips, and for the recovery of dark colored r'osin and other extracted materials which are soluble in acetone but not soluble in butane. The upper' duce an acetone of 74% concentration or approxi-.

mately of the same concentration as the original acetone and available for re-use in extraction.

As will be obvious the water miscible solvent, such as alcohol, acetone, etc., is not a good solvent for turpentine but is agood solvent for pine oil as well as for rosin. Consequently where a resinous wood containing turpentine and pine oil, 1. e., wood from which turpentine has not been removed, for example, by steaming, is extracted,

the turpentine will largely remain and will be separated from the wood by steaming, for example, in connection with recovery of. solvent from the wood, and may be readily refined by distillation. Pine oil contained by the wood will be largely dissolved out with the rosin and will .be readily separated from the rosin and solvents by distillation. v

The method according to my. invention, and more especially the use of a water miscible solvent, will enable the extraction of substantially all the resinous matter from wood chips and while the rosin recovered will be found to-be darker than that obtained by prior methods, it maybe readily purified to a common or superior grade of rosin by distillation, by treatment with'selective solvents, by treatment with decolorizing earths or charcoal .or by other known methods. Further, due to the high percentage extraction of rosin, the spent wood chips will be found more suitable for use, for example, in'the manufacture of paper pulp, and

It will be understood that the figures given in theabove example may vary considerably in practice for variousreasons, such as the moisture content of the wood chips treated, the quality of steam used, the of the extractor, etc., and it will within limits enabling recovery of the solvent as described.

in; :wm .be understood am out the according to my inventiom-I contemplate orother form of apparatus. v

. of asimple still for the recoveryof I vent. b the continuous evmq er on the rosin and which is immiscible and non-' reactive with the first mentioned solvent, to the solution of rosin obtained, separating the low boill0 .ing petroleum hydrocarbon anti dissolved rosin from the original solvent and distilling of! the low boiling hydrocarbon for the recovery of rosin.

2. The method of extracting rosin from resinous wood, which includes extracting the wood with an alcohol solvent for the rosin, adding a low boiling petroleum hydrocarbon, which has a selective sol-. vent power on the rosin, to the solution of rosin obtained, separating the low boiling petroleum hydrocarbon and dissolved rosin from the alcohol and distilling oil the low boiling hydrocarbon for the recovery of rosin.

3. The method of extracting rosin from resinous wood, which includes extracting the wood with a monohydric alcohol a solvent for the rosin, adding a low boiling petroleum hydrocarbon, which has a selective solvent power on the rosin, to the solution of rosin obtained, separating the low boiling petroleum hydrocarbon and dissolved rosin from the monohydric alcohol and distilling oil? the low boiling hydrocarbon for the recovery of rosin.

4. The method of extracting rosin from resinous wood, which includes extracting the wood with methyl alcohol a solvent for the rosin, adding a low boiling petroleum hydrocarbon, which has a 35 selective solvent power on the rosin, to the solution of rosinobtained. separating the low boiling petroleum hydrocarbon and dissolved rosin from the monohydric alcohol and distilling off the low boiling hydrocarbon for the recovery of rosin. 4o

5. The method of extracting rosin from pine wood which includes extracting the wood with a water miscible organic aliphatic solvent diluted with water to a concentration within the range 15570-9070, extracting rosin from the solution ob- 45 tained with a low boiling petroleum hydrocarbon which is immiscible and non-reactive with the solvent, separating the low boiling petroleum hydrocarbon and extracted rosin from the original solvent and distilling oil the low boiling hydro- 5 carbon for the recovery of rosin. v

. 6. The method of extracting rosin from pine wood which includes extracting the wood with a water miscible organic aliphatic solvent diluted with water to a concentration within the range 66 %-90%. extracting rosin from the solution'ob Y tained with a lbw boiling petroleumhydrocarbon which is immiscible and non-reactive with the solvent, separating the low boiling petroleumhydrocarbon and extracted rosin from the original 00 solvent, distilling oil the low boiling hydrocarbon for the recovery of rosin and distilling the original solvent. Y v

"l. The method of extracting rosin from pine wood which includes extracting the wood with 66 an alcohol diluted with water, extracting rosin from the solution obtained with a low boiling petroleum hydrocarbon which is immiscible with, the diluted alcohol, separating the low boilingi petroleum hydrocarbon and extracted rosin from 70 the original solvent and distilling on the low boiling hydrocarbon for the recovery of rosin.

8. The method of extracting rosin from-pine wood which includes extracting the wood with Amethyl alcohol diluted with water, .entrsat1n rosin from the solution obtained with a low boiling petroleum hydrocarbon which is immiscible with the diluted methyl alcohol, separating the low boiling petroleum hydrocarbon and extracted rosin from the original solvent and distilling oil the low-boiling hydrocarbon for the'recovery' oi the rosin. x

9. The method of extracting rosin from pine wood which includes extracting the wood with an alcohol diluted with water to a concentration of about 80% extracting rosin from the solution obtained with a low boiling petroleum hydrocarbon which is immiscible with the diluted alcohol separating the low boiling .petroleum hydrocarbon and extracted rosin from the original solvent and distilling oil the low boiling hydrocarbon ion the recovery or rosin.

10. The method of extracting rosin from pine wood which includes extracting the wood with an organic solvent for the rosin which is miscible with water, adding a low boiling petroleum hydrocarbon, which has greater solvent power on the rosin and which is immiscible with the solvent used, to the solution of rosin obtained, separating the low boiling petroleum hydrocarbon and dissolved rosin from the original solvent and distilling on the low boiling hydrocarbon for the recovery of rosin.

11. The method 01' extracting rosin from pine wood which includes extracting the wood with a water miscible organic aliphatic solvent for the rosin diluted with water, extracting rosin from the solution obtained with a low boiling petroleum hydrocarbon which is immiscible and non-reactive with the solvent used and separating the low boiling petroleum hydrocarbon and extracted rosini'rom the original solvent and distilling of! the low boiling hydrocarbonior the recovery oi.

12. The method of extracting rosin from pine wood which includes extracting the wood with acetone diluted with water, extracting rosin from distilling oil the low boiling hydrocarbon for the 5 recovery 01' rosin.

13. The method of extracting rodn from pine wood which includes extracting the wood with acetone diluted with water, extracting rosin from the solution obtained with butane, separating the butane and extracted rosin from the acetone and I distilling oi! the butane ior therecovery of the rosin.

14. The method of extracting rosin from resinous wood, whichvincludes extracting the wood 16 with an organic aliphatic solvent for the rosin which is miscible with water, adding a low boiling petroleum hydrocarbon, which has selective solvent power on the rosin and which is immiscible and non-reactive with the first-mentioned sol- 20 vent, to the solution of rosin obtained, separating the low boiling petroleum hydrocarbon and dissolved rosin irom the original solvent, distilling ofl the low boiling hydrocarbon for the recovery 0! rosin and heating the wood to a temperature such as to remove organic water-miscible solvent therefrom.

15. The method of extracting resin from resinous wood, which includes extracting the wood with an organic aliphatic solvent for the rosin which is miscible with water, adding a low boiling petroleum hydrocarbon, which has selective solvent power on the rosin and which is immiscible and non-reactive with the first mentioned solvent, to the solution of rosin obtained, separating the low boiling petroleum hydrocarbon and dissolved rosin from the original solvent, distilling oi! the low boiling hydrocarbon for the recovery of rosin and steaming the wood for theremoval 0! organic water-miscible'solvent therefrom. 0

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