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nice conronn'rron, or sennnncrnnr, new YORK, a conronarron or new"

EXTRACTION AND PURIFICATKON 0F INULINQ

No Drawing. Application ?led November 16', 1920, Serial No. dQIlAlW. Renewed. tlctoher i, rose,
The present invention relates to the re preferably to about 75 G, or even less, until I
covery of inulin from juices containing it, alarge part ofthe impurities become 00-
as for instance the juices obtalned from agulated and vexamination showsthat?ltra 55
_ dnhlia- bulbs and similar sources. . tion will 'be'successlul. The impurities thus
5 'Iihe juices referred to are obtained by coagulated settle out in a form easily re
comminuting the inulin-containing material moved by ?ltration. in some instances, the
and expressing the sap therefrom or by com liquid will now have become faintly acid
minuting and extracting, or by otherwise but in general it will be preferable to. add W,
obtaining from the vegetable material, a a little more of the clarity %_ solution after
lo liquor containing the inulin in a more or the mixture is heated, or w I; is it is being -
less soluble form or in the form of a colloid heated in order to make it slightly alkaline
associated or combined with im urities. In to methyl red paper, but excessive alkalinity
my process such juice is ?rst su ]e_cted to a must be carefully avoided, in order to prevent dd
clarifying operation havin for 1ts ob]ect the formation of slimy products by the by
' 15 to increase the purity and 'nal yield of-the, drolysis of the albuminous and similar con
inulin and to convert the impurlties into stituents of the sludge. ' ,
such term that their subsequent removal by , After removal of the separated impurities
?ltration is rendered somewhat easier. After in this ?rst stage or the clarifying process
?ltration, the ?ltrate is subjected to a de the ?ltrate is treated with more of the clari
so colorising operation, su plemented in some tying solution until a faint alkaline reaction
instances by the remove of additional small to methyl red paper is obtained in the heated
uantities oi organic impurities present in liquid, whereupon a further coagulation of
t e clarifying juice, Finally, the clear so impurities takes place and these are removed 75
lution obtained is concentrated to promote by a second ?ltration.
an the separation of inulin therefrom, and this The liquid is now quite clear and free from
process is aided preferably by the addition impurities ot: a gummy or albuminous na
of inulin to the liquid either in owdered tune, but still contains substances which give
form or in suspension in water-t e added it more or less color. I prefer to treat the
inulin acting as seed to accelerate the sep liquid, therefore, with boneblack' or a like de
so oration oi? the inulin contained in the s0lu~ colorizing agent of a character which'will
tion. Subsequently, the mixture,_containing adsorb coloring substances of the hind pres
the precipitated inulin is ?ltered and the in ent in, a liquid, whereupon a considerable
ulin obtained from the ?ltration is thorough portion or the coloring substances will be re 85:
1y washed with one water until the washings moved, including some impurities which
so are colorless. urther purification of the inn would, it left in the solution, have a tend
ulin may be e?'ected by redissolving it, again ency to be adsorbed by the inulin which sep=
clarifying, decolorizing, seeding, separating arates out from the solution in a later stage
and washing, as will hereinafter more fully of the process, dd
a car, . if desired, 1 may, at this sta e of the
no the practice of the invention, in its pre process, alter the addition of the ioneblack
ferred form, the initial clari?cation oi the or like decolorizing' agent, add a sodium
inulin-containin _ juice is e?ected by adding carbonate solution to the clari?ed juice until
to the juice su stantially equivalent quan the juice is alkaline to phenol phthalein,
ties of calcium hydroxide andcal'cium chlo thereby precipitating the calcium present ' '
45 ride, the addition being made carefully in in the form otmcalcium carbonate which car
the cold until the thoroughly stirred mix ries down with it further small quantities
ture is just alhalineyto methyl red. paper. of organic impurities, which may then be
The clarif ing solution referred to is pref; removed by ?ltration. The solution, in this Mill)
erably ma e by grinding calcium hydroxide case, can then he brought back nearly to
to with a solution of calcium chloride so as to the neutral point as indicated by methyl red
make a smooth cream. The mixture of the indicator by adding acid capable of neutral
clarifying solution and juice is then heated, izing sodium carbonate'for that purpose, '
 2 noisier '

The clear solution obtained by the treat and any base may be substituted for the cal- Y
ment with boneblaclr, or the clear solution cium hydroxide which can neutralize the
obtained by the further addition of sodium acid thus produced Without decomposing or
carbonate and Which is then brou ht back precipitating the inulin or causincr the pre
nearly to the neutral point by dddlng acid, cipitated impurities to- become glimy and 70
is then evaporated until the concentration difficult to remove by ?ltration. Also the
of inulin is about 10%, or even'more. The said salt and said base may be added alter
solution is then allowed to cool and acetic nately in relatively small amounts.
acid is added to promote the separation of Instead of calcium chloride and calcium
10 the iuulin until the acetic acid concentration hydroxide for the puri?cation mixture 1
is about .Olll. A small amount of powdered may use such combinations-as aluminum
inulin, or a suspension of inulin in Water chloride and aluminum hydroxide, magne
is then added to act as seed, and the liquid sium sulphate and magnesium hydroxide;
is allowed to stand quietly, or "with slow agi In these combinations I prefer to use as a
15 tation until separation of the inulin is prac
basic substance the hydroxide of the metal tit)
,tically complete, which requires 16 to 48' corresponding to the neutral salt used, but
hours. The mixture is then stirred until I may use other basic substances, such as
it assumes the consistency of smooth cream sodium hydroxide, sodium acetate, sodium
when it is ?ltered in any approved manner phosphate. For neutral salts I may use such
and the inulin is washed thoroughly With salts of the heavy metals, the alkaline earth 85
pure Water until the washings are color metals andrare earth metals as conform to
less. 7 f the requirements already mentioned.
~ The inulin thus obtained, although al Whatl claim is:
most tree from impurities, can be subjected 1. In the recovery of .inulin from juices
25 to a further puri?cation, it" desired, by re containing it, the method of clarifying the 90
dissolving it in hot waterjwhich, to prevent juice which comprises subjecting it to the
hydrolysis, should contain a very small action of a mixture of calcium hydroxide
quantity of sodium carbonate. By the use and calcium chloride; substantially as de
oi diatomaceous earth and decolorizing car= scribed.
-30 bon, separately or jointly the solution is 2. In the recovery of inulin from juices
clari?ed and decolorized; The ?ltered clear containing it, the method of clarifying the
liquor is then cooled and made .OlN acid by juice which comprises subjecting to the ac
the addition ct acetic acid, seeded, and the tion of a mixture of calcium hydroxide and
inulin separated and Washed as hereinbetoro calcium chloride in substantially equivalent
described. ' amounts; substantially as described.
It been found that there is particular 3. In the recovery of inulin "for uices con
adr-iantage in adding the clarit1 ing agent taining it, the method of clarifying the juice
(consisting of calcium hydroxile and cal which comprises subjecting it to the action
cium chloride) in two stages so that the of a mixture of calcium hydroxide and cal
major portion of the impurities may be sep
cium chloride in an initial step of the op I105
arated out and removed in the ?rst stage eration and thereby separating out a large
andythe residual impurities separated out part of the impurities, removing the impuri~
and removed trom the ?ltered product or the ties thus separated, and subjecting the ?l
?rst stage, So also, as hereinbe'fore noted trate, in a second step oi the operation, to
15 it is desirable to restrict the amount of clari the action of an additional quantity of the 110
, lying agent added to an amount which will clarifying mixture; substantially as dc~
produce only slight- alkalinity to methyl scribed. I
red, so as to avoid the production of slimy thin the operation described in claim 3,
substances which would tend to increase the adding the mixture of calcium hydroxide
ditliculty of ?ltering the liquid. in refer and calcium chloride to the juice in the cold; 1115
ring, in the foregoing description, to the use substantially as described.
of equivhlent amounts of calcium hydroxide 5. In the operation described in claim 3
and calcium chloride it is intended to indi addino' the mixture of calcium hydroxide
cate-that the practice in most cases will be and calcium chloride to the juice, in the ?rst
to use these two substances in amounts sub stage of the clari?cation, in the cold and
stantially proportional to their equivalent then heating the mixture up to the point
Weights. 'lt ~will, of course, be understood Where the impurities to be removed during
that there may substituted for the calcium the ?rst step become coagulated and settle out
hydroxide and calcium chloride, their chem~ in a form adapted for removal by filtration;
ical equivalents in the reactions which they substantially as described. 125
bring about. Thus any salt may be substi 6. in the recovery of inulin from juices
tuted for the calcium chloride "which has the containing it, c?ecting the preliminary co
power when used alone of precipitating some agulation of impurities therein by subjecting
of the impurities and simultaneously caus-~ the juice to the action of a mixture of cal
ing an increase in the acidity of the liquor cium hydroxide and calcium chloride, and
 1,616,167
then decolorizing the clari?ed juice and re evaporation and separating out the inulin
moving further impurities therefrom, by -frormthe concentrated solution by seeding.
subjecting it to the action of an adsorbing 10. In the recovery of inulin from juices 30
. decolorizlng agent; substantially as de containing it Without freezing the juice, the
5 scribed. steps of neutralizing the alkalinity of a clari
7. In the recovery of inulin from juices ?ed solution containing inulin, concentrating
containing it, effecting the preliminary co the solution by evaporation, and acidifying
agulation of impurities therein by subject the concentrated clari?ed solution to separate 35
invithe juice to the action of a mixture of out inulin.
10 _ ca cium hydroxide and calcium chloride, 11.. In the recovery of inulin from juices
then decolorizing the clari?ed juice and re containing it without freezing the juice, the '
moving ,further impurities therefrom, by steps of neutralizing the alkalinity of a clari
subjecting it to the action of an adsorbing tied solution containing inulin, concentrating 40
, decolorizin agent, and adding a solution of the solution by evaporation and treating the
sodium car onate to precipitate the calcium concentrated clari?ed solution with acetic
as carbonate; substantially as described. acid to separate out the inulin. '
I 8.'In the recovery of inulin from juices 12. In the recovery of inulin from juices
containing it without freezing the. juice, the containing it without freezing the juice, the
steps of neutralizing the alkalinity of a clari steps of neutralizing the alkalinity of a clari~
20 tied solution containing inulin, concentrat ?ed solution until the solution is neutral to
ing by evaporation and treating the concen a methyl red indicator, concentrating the so
trated, neutralized, clari?ed solution to sep lution by evaporation and treating the neu
arate out inulin. ' 'tralized, concentrated, clari?ed solution to '
9. In the recovery of inulin from juices separate out inulin.
" containing it without freezing the juice, the In testimony whereof I a?ix my signa~
step of neutralizing a clari?ed solution of ture. I
the juices, concentrating the inulin therein by WILLIAM C. ARSEM.