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Патент USA US2406097

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Patented Aug. 20, 1946
2,406,097
2,406,097‘ .
METHOD; Eon‘rnontromawmm: :
‘ sonwmnosnmms .7 '
AveryrAi Morton,i Watertown; Mass:
‘
'7
7' ‘NoDl-awin'g. Application January 21,, 1942,
'
Serial'No.'427;679"-.
‘
I
is :Glaiinsa (01. 2605-105) .
1,
t
.
_
methodifor producingithersame;
'
More'sparticularly itisrelatesi :to :the producing
and‘ isolating-of‘ alkali meta-l:rosinateswhichihavei
the-:‘peculiar :characteristics- that they are white;
and also th‘atittheyiare': freeifrom‘ certain’: objec~
tionablelifeaturesi hitherto ‘acon‘sidered' :typical- of.
v
»
2
c
trially“ usefulfforva‘ll purposesifor which ‘the cus-r
tomary‘ ‘rosinatesi heretofore known can“ bet ape
This "invention ' relates :rto's odium'ro sinatesvan d1‘
plied,‘ ‘lacking no-useful functions- by area'sonjo? the
absence ofaTthe dark‘rrosinategbutibeing-xfree from
I‘ the“ burdens --‘h'itherto< attending, :rosin‘ates." The
process - of ‘segregation ‘ includes a step which utl‘él
lizes the preferential ia?iriity oi as rosin»,:soluti‘ém'sv
rosinates;
I
- The invention: issherein ' i'll'listrativ'e'ly- described:
for “the 1 dark, rosinate.
withrreferencefvto its bearing ion‘lthe soap aindus-; 10''
for uses to which @theyi'arerappropriatei '
try; because’ of: its vpromoting:“rosin :to-thestatus
of ihaving-amarket and‘ cooperativeiutili'ty among;
materiallyforimaking-s?i'st class-isoap: The ‘high
The closest approaches of prior art, known to‘
me», arefound vamong methodsiproposedr'for light
valuei'ofi'the rosin'ate offithe:invention-*inwthis re-Y'
The vdark;rosinate, sand‘
re'senes and!‘ esters; can-‘be: separately irecovereds
‘
'
ening th’ecolorrof ‘Irosin‘ or irosi-natessbutanone-sofi
those; nor» any ‘of Ithoseewh'ichi separate 5the resin‘;
spectfcomes iiromiitherlfactrthatfit enables white 15" intq'?componentsi or crystallize ‘it as @abletic acid;
soap 7' to‘ have‘ the; advantages» ‘which u atten'dfi' the1
use- of "rosin; andilyeti'be- free from defectshan'df
disabilities,» » hitherto 1 considered 1
inseparable,»
which’: haveiexcl'uded rosin. Iromi s'oapiof: that
class." But the: utility is not llimited'ff-to:v ‘soap: ‘20
has eresultedi in: furnishing‘ white =»rosinate='for ‘the
soap‘ - maker.
This" is - so =universal>ly~ recognized’
that the-iexpressions “rosin soap” and “yellow;
soap’! areiipracti‘ca‘lly- synonomous.
Among these prior proposals,~ that» sh‘owniin
Many or- ‘a‘llk industries usingvrosinates =' or I rosi-nr
United States PatentsNos; 2,08551511 -and¥2',1085;152l
may' bene?t; and" with“ the ‘aidioF-this I-invention'
issued ‘to Georgi ‘would’treat va ‘solution? 'of abi'eti‘ci-v
acid orrresin; preferably a ten ' per cent-solution»;
in a solvent which ‘is a non-solvent ot'thesalkfalif
the vintroduction of i-‘rosinz products rinto?-‘stillll'otherr
?eld'svmayib'e expected;
'
- Hitherto rosinchas<depreciatedisoap b'yiiimpartm 25 and of the‘ abietate, with alkali “su?lcient ‘to “sub
mg to - it‘ a» ‘disapproved ' characteristic; iyellowishi
brown color. Bars of white soapwemibodyiing the‘
white .rosinate?of Ith'e: invention have beeni found’
stantially; neutralize -‘ the~~ abi'eti‘ci'r acid» present?"
The 'product 1 ‘of this-‘Itreat-ment fis' -stat‘ed“fto’-‘be=
“alkali abietate in rather purg-form;-. that‘ii'sgi free“;
not r'losing I theiriwhiteness as=they age \iundéreorji
from-1resenes'~‘or'the likef’ iandlthese-ipatents also
Andith‘ere are improvements vlniuoth'er ' respects;
bodies"; but Jtests' showlthat _ color; bodies are-
say their product is “substantially tree-KI-riom-Y ‘color’
overzlrosin as~1heretoifore-iusediv
I‘ have demonstrated: vthat"; from 1theig“sodi'um'=
present in ‘appreciable; quantity. Theepatentito
Kesler---No-. ‘1,633,’? 64 veproposed?to» precipitateithei
alkali acid’ salt-while‘ anew-mg thes'resenes “col-ree
rosinate?" of: ordinary‘-3 useithere 'can-fb'e epro'dueed»
twodistinguishable ?substancesabothr of ‘which are} 3 1 main in solutione,l~to makeia-"product whichsd'oes
not become ‘moist and isticky, ands‘ffrom which‘ 'is=v
rosinates. As hitherto knowmthese are; soiith‘orw
obtainable “abietic acid free‘ of impurities?"
oughly- intei'mingrled‘;v are‘sso: much alike-“and; in
Howev'en‘it removeson‘lythe ~resenes andwhat-mixture, are so dominated byl 'tlleucharacten of:
ever of ‘the-color:bodies'are:present-initheiresenesr
one of ‘them that the bene?ts o?thelotheriof them
have notrf'b‘efore» been {available-ion ‘ even-- known; 401 The product still- ' contains =the-colored-' salts-Let"
so ' fair 1as II 1 am 1 aware:
Whatever "the chemical‘
distinction: that may-rultimatelydbe found‘ between"
these 'two,'-» the present-'1 speci?cation -»di’scloses- a;
way of producirigrthem 1‘separately from the ‘cus-i
tomary -"‘ro'sinatea"
rosin- acids. In‘the; processe of1’Frencl-1'~-- 'N'er
2,01'2;1-25 for‘ highly’ purifying rosin‘; an aqueous
petroleum suspension of rosinat'evisedelliyclratedi
by- hot ‘petroleum'so‘that*thealkalrresinate'sepa
It'l-‘is-@suf?cientlys ' distinctive:~ 45; rates-from theso'lution. The “crystals-crime»new»
for ‘purposes he-r-eot ~to ~-desig~nate>i thesewrespec~
tively “dark resinate-i’ andwwhiteirosinate? " My:
discovery» of i‘the-whit‘érosinate;andfiofil‘a waycto:
segregate-it; contributes-to industrywrosinates"of- '
product’! are, according to thewpatent; “readilyl
amenable. to washingiior -iotherzpuri?cation1treat=~
men‘ -.”~ ‘Th'ewproduct-obviously was :not whiten
‘None: of‘. these method'sifor»y=improvingithe ‘color
sod-hint (another alkali?thatlappearitoibe lindus-v‘ 50'? makes a1rosinateiusablelinswhiteisoaps ‘Mere're-Q
2,406,09‘?
.
,
,moval of the resenes and such color bodies as are
3part of the resenes, i. e. unsaponi?able matter, is
inate is present than can be dissolved withthe
given amount of rosin, the dark rosinate will be
{not su?icient.
a
I The inherent inability of prior procedures to
taken and held preferentially, leaving more or
less of White'rosinates in a solid form which can
‘separate whiterosinates from dark is perhaps the
' be recovered by ?ltration.
As an illustration of
this theory, 40 g. of a powdered dry sodium ros
inate, made from WG rosin and therefore con
‘reason why white rosinate has, so far as I am
aware, remained unknown until my discovery.
The discovery has shown ‘further that the ob- ' ‘ ' .taining a quantity of dark sodium rosinate, can _'
lvjectionable features'of rosin in soap are not asso
ciated with all rosinates, but are more particu
larly attributes of the substances which the in
vention eliminates.
be added to 190 cc.,of kerosene, and the mixture
10 heated to 140° C. with stirring, without there be
ing any appreciable dissolving of the rosinate.‘
However, upon adding 40 g. of rosin, and repeat
ing thefprocess of heatingand stirring over a
period of-two hours, most of» the rosinate be
I show that there is a di?er
‘ence of solubility,‘ aspwell as of color, between the
dark an‘dhthe‘ light; and further that all of the
substances having offensive color characteristics,
comes dissolved. When the whole process is re
:normally found in the mix after treating rosin . peated using 80 g. instead of 40 g. of dried’s‘o- V '
1with a base, can be held, preferentially overthe . dium rosinate a large portion of the rosinate re
,white rosinates, in a solution herein' described.
‘The described procedure is successful without
,. -mains undissolved. ‘ When recovered by ?ltration
' fthis material is found to be white.
‘needing an exact theory as‘ to how or.‘ whyljthis .
> Another-.method for demonstrating the theory
‘is so.
which underlies this invention is to add a lim
,
To understand my attainment’
a ‘product’;
ited quantity of sodium carbonate to a petroleum_
having the whiteness which is demanded'in"soapsw ' H solution of rosin. As the carbonate reacts with
of high, quality one may- bear in mind the fact
the‘rosin'iandrforms sodium rosinate, the latter
that rosin contains some oxidized or colored 25 goes into solution. Theaddition and reaction of
more and‘ more carbonate eventually produces
acids; that-salts of those'acids are .dark; that
the: process herein‘ to ,be disclosed applies the
more rosinate than the solutionican hold. The
principle of preferential solubility, by’ propor
white sodium rosinate then comes out of solu
ftions, controls and adjustments, so as to separate
tion as a precipitate and the dark colored rosinate,
is held preferentially. By adjusting empirically.
those dark salts from other salts which are white;
andrthat theordinary sodium rosinate, hitherto
.ja'so'ap material ofv low esteem, always possesses
theseunwanted characteristics because there is
always. some of the dark rosinate present'in it,
‘however highly puri?ed or “light colored” it may
w
the quantities of alkali,; rosinand'hydrocarbon
solvent-it is possiblev to produce a highly desirable
3 condition for operation of the process. As a spe
ci?c illustration of this second; method of show
35; ing the solubility. of sodium rosinate-in a p'etro-g
leum solution containing ; rosin,.and also as a
The process comprises a treating of rosin with '
a base,‘ and 1a separating of, thepproduct into two
parts; ,one ofwhiehghas the‘ white sodium» rosin-j
§ates.;:,~ 1The:otherjparl11is a solution containing all
,of-theicolored substances, including darksodium
demonstration 91.10118 method of practicing this
inventiomthree cases are herejgiven: First, (a)
usejof- alkali in what may,<for this purpose, be
called a ‘flow’? ratio (of, alkali makes sodium ros
inate that will remainin solution, gbecauseof the
solubility of allysodiumrosinates in a solvent 7
‘rosinates, resene's, rosin esters, and‘some unneu-.
jtralized rosin.‘ This solution is amenable to fur-_. ‘ which-also. iholds .unneutralized rosin in solution.
ther separation if .desired. vThe preferential sol-I
Itis assumed in each'of these, illustrations that
‘ubilitylofthe dark‘ substances depends upon the 45 the-process. is run as long as the sodium rosinate
continues to be formed at a reasonable rate.
‘solution holding also a suihcient-concentration of
Second, (1)) whatmay be calledv a,“moderate”
rosin. ~ Thegreater the concentration of-rosin in
the solution, the more surely will the dark rosin a ratio of alkali makes more?sodium rosinate, than I
the solution can hold; thefraction that precipi-v
fates beheld in solution,
', p
_
V
_
~_
i. For greatest economic efficiency, the quantity 50' tates out is a white rosinate;. and whatever dark
‘of, solvent and the concentration of rosintherein
rosinate. is, present continuesin solution” But
mustbe selectedor adjusted. so thatthe rosin-~
(0), with a ratio’ of alkali so. 1“large” that mostv
ateedissolvingcapacity,
made by the concentra 1 .of the rosin acids becomes neutralized,,,the power
_
‘tion of_._ rosin,.is._su?icient_to take up all of the v
of the solventto ‘hold the dark sodium rosinate
drops sharply, vandthe precipitate,‘ is a mixture.
' darkrosinates, in addition to the resenes, esters
and other colored components; and yet is limit
of the white anddark sodium rosinate, and there--,
fore is not white. Thusgby,selecting-the'proporq.
;ed so that the solution will become saturated when
, Zall of those have been taken up, so that no con-_ .
lsiderable quantity of the white‘ rosinates will be
taken"up._ This- saturated, condition is>what
> _‘ should be prevailing'at rthe'stagerwhe’n'the white
tion of alkali which is introduced fOr- the. reac
tion, whiteness vof precipitate "can. be’ obtained,
60, care being taken-that the concentrationof rosin.
does'not become too much reduced.
irosinates are beingseparated- fronrthe solution: ‘
Before that stage the concentration of rosin pres‘ent, will preferably be great"enough so that it can
goingcasesfollowu 1'
action; and-yet becorrect in‘amount to produce
time and temper-;
V 4, tlledesired saturation, iat the
' i ..,;'I-‘o1demonstrate-the
rosinate isinsoluble in kerosene.’ If,_ however,
rosin in 1suf?cient quantity is added tothe kerosene the sodium. rosinate *bothgwhite and dark;
fore-I
r
sene to make a ‘total volume of approximately
1750 cc., which makes the concentration of rosinv ~
theory which underlies ‘this’
, invention one may ,obseryeithat dry sodium
-
(a) The addition at 110110., with stirring, of
40 g; of anhydrous sodiumcarbonate to 'asolutionf
*of 480g; of WG rosin,jdissolved in enough kero-,
undergo diminution with the progress of the re
ature ofeiiltration. _
,
. Quantitative examples illustrative. of the
70
*be about 36% in the-tqtalweight of solution, if
the kerosene has a; speci?c gravity of 0.73, causes‘
the described reaction,;which can. proceed. to a;
conclusion in about one vand one-half hOurs with-'
, ‘will .dissolve.-._ If,.,on the other hand,,.rosin, is
out the temperature-having risen ;ab,ove-133°.,C_-.;
However, the sodium saltwhichjias; been pro,
present .in insu?icient.-quantity,_~i_. e., if ‘more gross;
ducedremains largely dissolved ill-the reaction,
5
6
mixture,‘- even" when‘ the kerosene solutioneiséal
it shouldilb e1 understood ‘that =the ‘pre-de‘termirlai
tionloflthe adjustment ‘of-factors to: housed in any
lowedtocooltoroomtemperature:
'
~
,
practicing ‘ or the‘ process industrially‘ * can {if
‘ ~Irr~case~'(b'); where theY-ratio-lof carbonateie'to
necessaryif always-'4 bee-approached? empirically ‘by
allowingLsodiiimlcarbonate' iorioth‘er suitablee‘alka‘li
rosiniisy say 2 Jtol --l2 ‘instead of‘ 11‘-v to'll2j'» and " the
heatingandwtirring ‘is'~‘carried-~out until 'reae~
tionfhas been-effected'at a; ?naliltemperature?of
to react with rosin, in a-e'solvent'lihavingys; high
concentration of rosinyandithe' progression-‘reac
tion ‘withiprecipitationlofsodium rosinateibe ob‘
145°‘ Ci; av precipitate *is produced-‘which white
orvso- near’, tol-whiteethat; after“ separation" from
the solution ‘and fr'om‘adhering liquidgi‘it' is suit
served until= ‘ the ' obtainable -~quanti1ty- = of’ ‘white
able —for use in "white- soap; ' or for useeas a'high 10
quality of ‘size‘for paper-,"or-ror any useefor which
afwhite- sodium rosinate may be’desi-red;
‘
.
‘
sodium‘ rosinate has-lbeen formed; and? adjusti
mentsv ‘made Iof11rosin; ‘concentration, alkali, tern‘
perature; and durationd‘as-‘mayabe- desired.‘
The; proportion 1of" ‘rosin ~in~ lthecsolvent-J is»: the
Butv (0)1- when‘ the’* ratio’ ‘of ‘carbonate "to'rosin
isv ‘made 43 ate -12‘the1color~ of 5the precipitate~has
most ‘ important’ of ‘the factors-‘mentioned 5~above-,
been lfound'to‘ fall into~~the~range \of-"grayishwhite 15 for ‘if i the 1- initial 1~concentration- of rosin- is *sui?’;
c'iently hig'hlthe concentration existing‘ at theeen‘d
‘or tan; If ‘a still‘4'higheriproportion ‘of-l alkali is
otithe reaction willl not ‘ have 'fallen‘so low ‘was’ to
used the "color becomes brown;
The foregoing'examples respectively show; ?rst; , fail to hold- in ‘solution the-undesired-rosinate‘and
the» other»v undesired isubstancesé Although-'~ the
all? v"sodium 'rosinates icausedi‘toi dissolve‘ ‘in ‘a"-hy"
drocarbon‘ solvent’ by~the-»presence>1of‘~rosin;‘ ‘sec 20 having of ith'e concentration "adequate=at‘1the*-time
of separation‘ of- lthe whiterrosinate is’ of ultimate
ond, dark?‘ rosinate~~kept ~ in“ the solution ~‘prefer=
importance;=- it ‘Tis'1m0St Lpractical land ‘informato-ry
entially, while the-precipitate i5~ entirely white
rosinate; and;v third-,i darkI rosinates precipitated
to *- state the concentration- of: rosin- ~in-=~ termseof
the‘: amount at the A beginni'ngaof-vv reaction; aegis
to some ‘extent’ when», th‘ere-v comes *to :be-'~st-ill“less
’
rosinpresent in the-solutions These also‘ show 25 done inthe-eXam-ples here given; - 1 _
‘ However, in; any instancei' the} concentration
that practice 'of ‘this inventionv'rmayJ requirerad
‘of’ - rosin existingiat- theltir'neeof *?'ltrationiicarrlbe
justment of a numberot factors;
.
found (by 7 analysis; Concentrationsvsoo-found-ein
The I principal :variables ‘in the =processware', (A)
concentration'of rosin in the-solverit; which is
best kept-as high as =possible, for 'it'rdiminis'hes
aseri'esrof trial-operations1on~samples can be used '
continuously throughout 1a reaction ‘in: which rose
be employed in afmain operation 1on<1~any ipartic'u's
as 1a guide to» select" ‘the! initial;lconcentrationeto
larilotcof I'OSil'li- In;vari'ouselots-ethelcontentsiof
mate‘ is being produced,» and» yet lsh'ould'i at; the
darkl r0sinate:-may¢--di?er; J Iffiit iis-desired toaattain
enclof reaction be- ‘such‘ thatithei colored rosinate
the i highestwpracticableayieldt oi vwl'i'iiie'r11rosina-te;
and- alliother rcolor-ing; matter is: surely held/1 in
solutioniin the .motheri'liquor; .(B) adjustment‘of 35 with a minimum of attendant costs, the concern
trationv of resin‘ for dealing with'i any ip'articular
the ratioof: alkali present forlthe reaction-1(0)
lotv should
i-suohi as »Will»_';-make- the- saturation
selective control of the temperature; which'must
point for» ‘rosinatessoccur when¢all ofi‘theida-rk
be 'high'renough? to effect reaction; and? at»- times
rosinate has been dissolved, and approximately
high enough ‘to. increase the-“solubility: so» as -1 to
prevent precipitation of :dark rosinate, rbut'ypref 40 all of the whiterosinate rem‘ains'rundissolveds By
a; series ot Jlaborator-y ‘ tests applying: the‘; process
erably will'be 'hel‘dltod moderate ‘limit-s,‘ iniorder
that‘ crackingioii the, rosin-acids shall be avoided;
tonsamplesx from a particular-lot withE diminishing
concentrations-.iofh rosin, in successive samples
(D) suitable:agitatiom-themoregvigorousithe bet
ter, tos-make good contactibetweenithesolid'alhali
‘until ;one;is ifound "whose isolated rosinate product _
and i the. rosin acids, and' .to ‘promote prompt es; i
cape §o£ral1~ volatileaproducts; (E) ‘adjustment; vas
to the duration timeysince sthe ros'inatea?rst'pre:
is not-white: it lcan'lbe learned ‘which initiati'ros-in
concentration‘ value-will‘; be?) commensurateiwitha
rosinate=dissolvingr'capacityLof'ithe rosin solution
that is. limited; so: that :the solution ibecomes. satu
rated with rosinate zcoincidentlyi'iwit'h‘ theicomp'le;
cipitated- will be ‘ whitepbut ?ahat precipitated later
may be dark1,;as when thepr'ocessgoesztocomple
tion; and’ the ireduction" of 1 concentrations of the 50 tion'; of the .‘ dissolving of ' all; 1 dark; ros-inatevthat
rosin ‘in ‘the’ solutiom. andithe .icurrentl conditions
exists: imthe particular: lot{tome-"treated, Lomthat
as tolquantityvof 'alkaliyztemperature:onother fac
tor! may be;v or imayaco'mel to be; suchithatstoward
is- produced itfromu itz, Inizthatt case; the; rosinate
the .end darkx'bodi'esi ares‘ precipitated; .(F)' rprefer;
will have been fractioned so'zthat:theiundissolved
rosinate will be all of the white rosinate that is
ably; ‘that the source ‘material! ichosen ‘should the
available, a modicum bein'vgalready‘"dissolved;L
cleaned crude gum, or elsefb'e;:lightvcoloredmosirr;
and (G) for the best commercial success, that
the solvent and the alkali be of inexpensive kinds‘, ~
for which at present'kerosene and'sodium'car;
bonate are satisfactory.
_
-
An1 analysis ‘maybe-made by shaking the ?ltrate
of the sample operation, viz, the mother liquor
which has passed through the ?lter, with water
to take out isodium rosinate equivalent to what
60 was in solution at the time of ?ltering; then ex
Theinvention ‘can vbe ‘practiced with wide var
iation of these‘ conditions. Herein ‘will <?rst
tracting-the rosinthereof'with sodium carbonate;
given observations pertaining when there is a
to recoverresenes and esters. 'I'hisseriesciopen
relatively high concentration of rosin, which
anions-(provides dataaby, which concentration of
and after that distilling awayithe mother liquor
mighti'be called a preterredi=region for operating 65 ‘combined and I uncombined rosin .i acids, and- or
_ the process. In thisithe above mentioned varia
1 other constituents ‘may: be: calculated: "‘Tl’IB'QllQII-ié
tity of solvent... may‘; be: assumed“ notitolhave
bles can be ichangediwithiniwide limits without
greatlyaffecting the result. Second, thecasewill , ‘changed appreciably- during the reaction; but» if
be stated where the conditions are in a region
I any. is known to have been lostror added?due
whichocantbe vdescribed-as critical,- in that the 70 allowance can’be made; ‘Thewei'ght of ‘combined
factors '~ are *so inter-dependent that ‘if anyone
of-themevaries too 'far from its normal or advisable
value'the'control or adjustment ‘of others becomes
very-important. 1 The- conditions’ for-“successful
‘
rosin is'obtainablepby‘acid treatment offthe rose
inates‘found in'the‘residue ‘and those ‘foundfin
the ?ltrate. Thetotal ‘of combined ‘andj’unconie
bined rosin, plus the smalleamou'nt of resenesand
operationwill'be illustrated; ‘in‘addition' to which 75 esters; found by this’ analysis, is comparable ‘with
2,406,092
,
V
8
7
the :various percentages of rosin mentioned in the ‘
particularly if the mass starts to gel.‘ The petro
leum may advantageously contain some low boil-7
ingyfraction, which byits own volatilization ‘will
tables which follow; and-the optimum concentra_
tion of‘ rosin required to be provided in therosim ‘
1' solution, ‘for-the ?ltration step, in producing white %
rosinatefrom the particular-lot of'ijosin thus sam
pled, canthu's be known. -. I - I
facilitate the removal of the small amount of wa
ter' that is formed by the neutralization of the
rosin.‘ Removal of this small amount of ‘water
'
. The. best form of the, process‘, in brief, involves ‘
1 the making of anoneaqueous mixtureof ‘alkali;
} withaninert'solvent holding in solution a very
helps to prevent gelling. A little additional pee ‘
troleum may be added to compensate for any loss
by volatilization, or to facilitate the stirring if the
' high concentration of rosin acids,-_although'not 19 mixture becomes extremely thick. - Stirring is
too high for agitation to be effected, about 45 to .
50% by weight if petroleum with a speci?c grav- ‘
‘ ity of._0.73 is used ;rheating,stirring vand maintain- I
, ingm?uidity,v in the thick, mixture while reaction
. producingrosinatercontinues at restricted tem 116
continued while the mixtureis held at 140°= C. to
150? C. during the last hour, vwithout the tem
perature rising materiallyabove the limit indi
cated, until, the reaction is, substantially complete,
shown by cessation of escape of water or of car
‘ peratureifractioning the soluteby precipitating ;
bon dioxide set free by the-reaction. The mix
1 the. white rosinate from solution while themother
j liquor» has sufficient concentration of-rosin to re
ture isthen allowed to cool to about 120‘? 0., where
it is ?lteredito separate the precipitate, more of
' tain in solution all rosinates and other substances .
‘ which comes out of solution as the mixture cools.
5 having color; separating thejprecipitate from the 20 Filtration can be carriedout at 90° or even lower
1 solution by ?ltration; and, if desired, washing the
but the mixture is correspondingly thicker and .
i separated matter clean of themotherliquor, to ;
harder to ?lter. The precipitate is found to be
snow white sodium rosinate. ’All color, bodies,
j make .the ?nal product, Details will appear .
: hereinafterof steps andrestrictions that may be
i appliedgfor controlling the source material, the
solution and the ?uidityof‘the mixture, the reac
particularly the dark colored sodium rosinates,
pass through the ?lter because the rosin is still
125. sufficiently
concentrated to hold them in solu
§ 7 tion, and the fractioning of the solute. These may '
f vary,;considerably, relative to each other, while ‘
tion in the mother liquor, in which the white so
dium rosinate is relatively insoluble, so that it is
retained by the ~?lter. The ?ltration can be ef
i still-givingran, optimumof whiteness.‘ Also they
; may vary among themselves according to the 30 fected by any of the'recognized varieties of ap
gradenof ‘?nal product which is wanted, in case > paratus, including the centrifuge.
, The centrifuge will ordinarily leave the precipi
1 it is adjudged admissiblethat the extremely white
1 bevslightly shaded by containing a. modicum of
tate'sui?ciently clear of the mother liquor, but, if
1 lower grade mixed- with it, for lower cost or greater ’
desired, the whiteprecipitate maybe washed with‘ 7
§yie1d._‘1
I
.
'
35 small quantities of kerosene or other petroleum,
1 ; qThetermfr'osin” as used herein may be .con
to remove the mother liquor from it, untilthe liq? _ _
Q sidered to include any material'whose acid come’ ‘
uid coming away is colorless; Low boiling petrO:
'1, ponent has the composition. of approximately
'leum can be employed to remove higher boiling .
T
j
wash liquid; and the low boiling petroleumf can
In, TableI are illustrative examples in which, 40 be cleared away by promoting, its evaporation.
CzoHsoOz.
'
'
-
-
1 at the beginning, rosin was concentrated in kero- 1 I
- 1 sene in the high ratioof about 1 g. of rosin to 1.1 ‘
~
‘ If itis desired to, separate the unreacted excess
3 g. of petroleumsolvent, a concentration. of about 3
of alkali, that was'retained by the ?lter with‘, the ».
rosinate, this canbe cleared from the rosinate by '
50%. ~A;result of this high concentration is that
dissolving them both inwater, and then salting "
atthegend- of the process, notwithstanding the -‘ out the rosinate, or in any other known manner.
; diminution of rosin which has occurred, the rosin ‘
If ‘the White rosinate is to be used in soap thisstep
‘ concentration :islstill great enough .tohold the 3 7 can be postponed and the result attained at'the
. color, bodies in solution,'even when the poorest
‘grade of. rosin is used, whilelthe white‘sodium ‘
rosinate-is precipitated.,_ Formation of ‘sodium
corresponding stage of’ the soap making.
,
.
The completing of ?ltration is considered to
water. begin at a temperature onlyailittle above I,
end the process of the‘invention, the white rosin'-.'
atebeing then isolatedfromthe dark rosinates.
The free alkali-thatimayg be present with it is in-Vv
100.‘? Ci,faccording to the equation:
consequential; This would be some of the alkali
' rosinategand evolution-70f... carbon dioxide! and ‘
'
z‘csHacob?seNa'zéow ‘
:~
7
v
_,
'_
'
‘I
‘
Q
.
V
B02111!
J ’
"
"
~
\
-
.
.
V _
»2C19I;I2,9COONa+COz+HzO
‘
No.
_
' ‘that was introduced for the reaction but became
55 covered by precipitated rosinate and thereby was.
-
.l
'
~H‘I1Y.TABLEIVI
-
l
V
>
_
-
,
u
i
-
7
So].
Na-zgo" ..vol.,
e
cc.
'39,‘ ‘- ‘285 v
.48
.31..
Mesa
.280'
~31
; 285
35
< 285
"Anhydrous sodium carbonate having been intro
,duced into the solution of rosin in kerosene at or
1 below 110° C., heatingis continued so that .in an
hour thetemperaturehas risen .to about 14030.
Percent
_
-
to 1.1531111
.vpement’
~
.
.
-
-
-.
‘
Concentra-
‘a
:IGrade
,
‘
prevented from reacting.
V
l
"
‘
'
.
tion ofrosm
a
'Max.
‘
,percve’utby'
°O.
'
, 32.5)
49
150
2.5‘
,_
_ 40:
25.9
50
49
150
v~25
2.5
25.9
49
.150, '
______ __
.7152
-
-
insolution, temp., Time’
213%‘; 7
,P
Color ’
'
so‘ snqjw white. "
s1
so
,
, Do.
1.5
13v
Do.
1.3
70.
Do.
?rInl Example 5 the rosin was ?rstrdissolved in
800 cc. of ligroin, ?ltered while cold, concentrated-,; '
and then diluted to a volume of 285 ccrby addi:
tion of kerosene. . These operations renjlovedcol-v
lThe mixture usually'becomes ‘very 'thick,§and
cred-material which was insoluble inepetroleum
1 stirring rjlmiust be f_ vigorousfjto maintain ?uidity’, 75 andwould have contaminated the product. The‘
2.40am’?
:93?
10
.
exaclzwpercentagesaare?inot‘l-knowng in thisuexam
plewbecause thecquantity'ro?petroleum-insoluble
careraatothe ratio of alkali to: rosin,_ themaking
oiwradj-ustment ‘of the ratio of alkalimeans that
the-Quantity of :alkal-i'whichwill give the desired
material, which was separated before-carrying
out the process,..reduced thevajctual. weight g'of
result should be determined-empirically, and that
the. quantity used, in proportion» .to sthe ‘other
--,'Simi1ar= operations usine'zwas sourcev material 5 substancesv present, be limited» accordingly. The
crudepgumn ~of;>a.1.kind whicha-would ordinarily
secondg-rex-ample- above l-giventgof the --th,eor_y;:un
rosin used.
;
-
'
z
‘
produce WG rosin; give; parallel: results,; as ‘shown
.derlying. the; process». shows how; the. quantity i .of
in.'.l?able;1I.v
alkalircan be. adjusted empiricallyvso. thatm Pmde
'
f
5
No
v
-
>
'
L‘
I
'
.
I, ~g.II
‘alkali.
I 3,120";
I
'
"Percent
1.
‘Theta-II
‘Rosinin‘
I‘
Gum, NazOOg,
’ "5
- l n
"
esolutionr
,
weight
v
"
I
:tTlme, jrYien. .
.--to'rosi_n,.1:»¢pencent by?‘
y'\II._,percent,.
' ‘
0 C " .,.hrs.,
_
‘
6 ------- --
156
31
285
26
49
146
7 _______ __
152
39
285
33
50
150
'_
2-5?
2.5,
'
"
-
.
'
s30;
I
'
Color
.perzcent
'
I
'
so
Snow white.
Do. I
As the crude gum source material‘ waslaboutv 20 not of suitable‘whi'teness is'ob'tain'ed. “The sensi-‘
four-?fths rosin and one-?fth turpentine, the;
basis
concentration
of 80% rosin
of content
rosin was..':i,calculatedj
i'n'lthe gum_' ,onf'thIe,
,
._.tivity;.is callsedffbythmdanger that within the
‘customary time vperiodzlso 'much- rosinfwill beare
moved‘Nas-roS'ina-te, from; the solution that the
In the above examples,_in_ Tables I andII, that .... vdesiredWretention of; the, dark colored, rosinate in
source material ranged from, crude! gum through}, 25
WG rosin to FF Wood rosin. . The rosinateproda _
solution may not be realized.
.I
Y
,
Elia some :.of the dark; sodium rosinate ceases. to
uct in each of these cases wasqsnowi white. That. ‘I \
from the FF wood rosin‘wasnnot 1S0; beautifully I.
be “held inn-solution:theiteniperature of reaction
maydoe raised, in order to::assure that thejdark
snow white as the others, yet:even._in this case if:
rosfinate shall stay infgsoluti'on. Irrithese lcases'a
the product, when dissolved in. watenandprecipb' 30 drop-in temperaturez?tol 1110f’ C. orwlowenbefore
tated byv addition of saltnlgavena-product which,
?ltration' will cause glprzeciiiitationcgof moss-‘like
in soap would have been satisfactory- 1
.
'
aggregates-bf dark’ so‘diumK-rosinater; and. .these
These examples illustrate the-merit of having,
contaminate the product so as to ‘renderitun
high concentration of rosin in the solvent, the
suitab'lefonwhite soap. “To increase the solu
limit being. reached. only- when - the vvmixture "be 3,5 bility-oi the‘dark' lro'sinate the temperature» of .
comes toothick to~stir~ori?lteru ‘First, thelcol
?ltration: must also- be---raised;I land’ the-?ltration
ored. material‘. (the colored- rosinates as~welllas
process‘ itself mds?be-asurabid as‘, possible 1"(-for
the v{colored ‘resenes) ‘#is thereby-readily held ‘in
example, a ?ltrationibyvcentrifugingl) inlorder'to
solution. Second, it/is' possibleito obtainhgood '
complete the =separating»_before- the'dark-rosi‘nate
yield of ---high quality material in-a single'opera-- .40 will“ have begun to. precipitate. “Theymore'the
tion without the/necessity of=recyclin'g. "IJ'hird,
itoren'ders ‘ unnecessary many details of manipu
lation-which becomes advisable when] the strength
of certain of’the-va-riables‘liesiin-a more-‘critical
zone, -as~indicated hereinafter. ~'And-a~fourth I,
advantage ‘is that very cheap lgradesiof rosin, '
su‘ch-as'FF-wood; can‘beempl'oyed.
alkali‘ becomesconsumed, ri.;e."the further the
progress toward‘ ‘neutralization ofea‘ll rosin acids
present, within the time allotted for reactionfth'e
greater-is the (“dangerv of / precipitation?pfif'dark
rosinatefaoccurringa; and-rtheegreater isiltheccare .
requiredtoeavoi?vithatduring'?ltration.
'
I
‘ Whenlloperationsaredwithin ‘the-critical zone
‘
' If, asl-in the above examples lot/preferred ~prac
tice,-‘-there'--=is- so much rosin‘dn the solvent ‘that
its weightappro'aches-or about equals lthewei’ght I
of the‘solvent, this ‘may vbis-‘considerednormal in "
thesense that the process will work comfortably
even though- the quantity of alkali, thetem-Iper'a'e
ture; or the grade -of-- rosin,gor-'all of‘ these,--lie in
zones which under other conditions mightbe con
sidered not so good. But’ if'the-ros'in is only
about- half as» much 'as'l'the solvent,~by weight, ‘or
less,’v the» ‘conditions'lof alkali,~‘temperature vand
thelgrade - of ‘resin selected for the starting
material; -is~~- of considerable: importance. Light
‘colored \rosins ‘Whi$h'~"COn?taln a 'minimum' of
colored material are muchbetter than‘ the darker
grades'of‘ rosin. ‘One ‘of the;best grades for~pro
duction of white rosinate is crude gum; becauseiof
the) smallness of ‘ the proportion of’, colored acids
present.
'
"-
"
The tabular‘ ‘showings-‘of test examplesiwhich
follow illustrate the, varying'le?ectsobtained with
the di?ering‘ relations of materials, proporti ng,
gradev require} critical consideration ~ andilr‘estric
temperatures, kinds, etc, therein shown.
tion,v lest "theis'odiume rosinate obtained‘fail of
I 'In‘ Iable?I‘IIf-the color of‘the-roIsin'ate obtained,
having ‘the characteristic white, ' or'jnear 'white_
' 5'“
ranging irom'snowwhite to tan,- in'all ‘cases was
ness, of the invention, -or_ ‘ be not‘free' ‘from ‘I un
betterthfanthe sodium rosinatepreparedl-by gon
saponi?able matter.
ventionalEn'iethods. ' The. temperature ‘at ‘which
sodium" rosin'ate was recovéred‘by ?ltration-was
’
'1
I
'
'
‘Practice ‘of this invention Tin such-1a" less con
centrated-solution isvwhatv was'referred to herein .
belowY-lllo" 'Cffor‘t-he‘ betterigrad‘es of vproduct.
before as having conditions inac'riticar Zone. ‘55 Where thIeIgyield was high, however, higher vtexn- .
Considerable variation of some (of these condi-I
peratures- were employed. even up to 160°, in order
tions can still be allowed but such :factors‘as the
quantity of alkali, thetemperature of ?ltration,
and thegrade -of "rosin'niust be considered much
'towhich
reduce
is aptjto'
precipitationoccurIat
of this
darkjsodiuin
co'ncentrafro on‘rof
resin in the 501mm; The temperatures; I_
more ‘carefully than’ is the ‘case 'withj'theIf-very 70 the, maximum, and were those ‘reached I, abo
concentrated solutions. Observations “follow as
to ' adjustment of ‘alkali, , then of ‘the temperature,
and next of the grade'of‘ resin) to be selected‘as
a=sourcematerialii
I
I
.
,
I
,'
~?‘If‘ the processis‘to-ib'e practiced-‘withIneed‘for ‘
will“! Sets‘) in‘. 1.3.1115? about 11.076.
.carbo?ate.wesi‘offten ad
.ne‘ratllreseiqrtxemple;
‘Agitation was continued
' .iati.
'
V
.
ll‘
12
,
high'in some of the experiments, the presence
of alkali reduces the tendency for the rosin to
decompose by’ cracking.’
;
-
I
> i‘
.
of course readily separated from the ros’inateby
warming in a vacuum, or by otherwise allowing it
steadily. Although the ?nal temperature is rather ‘
to‘Mixtures
evaporate.
of solvents
» a
can
V " be used.~
i 'Y
w
Dried sodium rosinate may be added to a solu
tion of rosin in petroleum/as mentioned in-the
?rst'illustration of the theory of the process. 1 Also
The various tables show that, at these low con
centrations of rosin in kerosene, the yield of white
I rosinates is less. In general, they show that the
partially neutralized rosinate can be used‘;
1~
These and many other variations can lbef used
better‘ results‘ attend the greater; ratios of excess 1
rosin in solution, the lower ratios of carbonate 1
to rosin, the lower temperatures, and the shorter 10 withoutdeparting from the fundamental nature
of the process, these being. merely adaptations
reaction times. However, in all cases, dark
colored sodium rosinates have been removed, as v . such aspersons skilled in chemical processes
‘
can be shownzby retrieving the remaining acids I 4I would apply at convenience.: , L
The invention can be practiced’
as the sodium salts and comparing their color‘ '
1
alkalilin
with that of the material separated in the process. {.15. aqueousisolutibn; if the, PmPQrtifms 0f rQSin, ros
TABLE III
-
I
Y
WG rosin and NG2CO3 in kerosene
'
,
‘1
Naoob
,.
.
. 2 g‘ .
T 11 SW“;
$3,695 .
ght
cc.’
inysolution,
'00F1,150
' .
85
1,150
Bit’ml
'
'
alkali
tow tema‘-.
1
' msm’f 10;.’ ’
I
'l
Time,
Yield,
hrs‘ . Percent
.
percent‘as
Peres
111.71
‘ , 156
34
11.1
‘159
2.25
'
2.25
.
18
1,150
22
25.6
‘112
2.5
15
1,150
3
22
25
‘182
2.
_ 80
1,150
,
22
26.5
r2112
26.5
54
'00
1,150
1,150
100
1,150
100
1,150
160
1.150
15
22
1
-
21
' a0.
,189
110
119
I ;'
-
sv 01
" a
4.25
3
'
°. 11”‘
color '
5
‘41
Suowwhlte;
I
41,
'
'59
09
021
14
-
1..
rosinate
’Do.
60 ,White.
I
I
1a
15
’
"
,
Gray white.
,
'Do._
Do.
Do.‘ . 5' .
‘185
119
2.25
3.4
33.1
.184
a
19
Cream white.
22
33.3
182
2.25
82
Light tan." ,
28
. i0 .
192
3 . '
s2
Tan.
Y "
'
Shady white.
, Do.
_. '
inate, and solvent atthe end of the process ‘are
‘ '
In computing’ the concentrations of rosin'the *35
suchas to permit retention of, the dark rosinate
speci?'c-gravity of kerosene; is taken as 0.73.
in solution. But asidejfrom possibly; aiding rapid-‘
In Nos. Sand 9 lowratios of alkali to rosin are
ity of neutralization of the ‘rosin acids,:and a more
seen to go with snow white rosinate.
In Nos; 10-19 higher ratios of alkali to, rosin,‘ ‘ complete utilization, of thegalkali,~inclusion of
water contributes little otevalue, and- the intro-,1
higher temperatures, and longer times of reaction,
' are seen to go with reducedperfection of whitee 1
duced water must later be removed.
rosinate.
'
1
>
'
,
~
,
As the quantity of water is increased the dim-'
ness, 1. e., lesscomplete separation of dark colored
. cultyof its removal becomes-greater;More.s01;
'
. ; The practice of the invention seen in the fore- j I
vent must be used, so that evaporation of the hy
goingillustrations is capable of many modi?c'ae 1
drocarbon solvent 5 will facilitate the removal of
tions without departingfrom the essential prin
the water. The rosinate is very apt to form a gel,
which makes stirring more and more di?icult,» and
~
3 ,ciple of'retaining dark rosinates saturating a'sol- ,
vent‘ for rosinates so that white rosinates‘ do not
requires stillmore solvent tov thin the mixture: to
asuitable- consistency. The temperature must be
dissolve. Among such variations that~Iwi1l---be
raised higher and higher, in order to drive out the
water, with result that above 180° C. the danger
of cracking the rosin, or causing other undesirable
mentioned below are routine-modifications which
‘may beintroduced during commercial adaptation, r
.theIintroduction of water, changes in the. solvent, ‘
andchanges in the alkali.
I
I ,.
changes,ris increased. In the end the extra sol
I V
vent must be distilled from thelmixture,_vuntil the
rosinI concentration is suitable for holding-5 the
to ‘many modi?cations of ‘the way in which the ‘
process- is practiced. For example, thecarbonate 1 55 dark rosinates in solutionwhile the-white rosinate
material separates. The use of much water makes
may be added ?rst tothe petroleum, followed by
it necessary to recirculate or add petroleum until
theIrosin, without the operation of the invention I
at theend of the process the, operator maywell
' Practical considerations and utilities may lead,
being affected. -
_
'
2
' In cases- where there is a tendency of dark
haveused four,_?ve, or even as much as ten times
rosinate. to precipitate before ?ltration, ,fuIrther
60 the amount of solvent necessary, all of which must
‘rosin may be added at the end of the reaction‘
in order to hold this dark rosinate in solution,
H
v, be distilled from the reaction'mixture with con- '
sequent danger of injuring the product.
Thepetroleum solution can ‘be forti?edlwithl
, _-The method above described for arrivingatthe
’Ifresh rosin, and re-used-a number of times, be- '
preferred state employs anhydrous materials and
jorethe dark material need be separated from it 1 65 adds more alkali than is necessary to neutralize
the rosin, sometimes an excess of 50% or, more,
i and the petroleum recovered by distillation. . The
better thegrade of rosin employed, the more
‘étimesthepetroleum can vberecycled.
'
but this practice seems as good asif not better
thang'one which, by' introducing water, requires
»
I ,When can; rosinate shows a tendency to come‘:
outduring the ?ltration, and the product is to be
washed, the initial washings can be made with a
i 'warmtoh'ot solution- of kerosene containing-a lit
, excessively large apparatus, distillation of much .
solvent, generally higher temperatures; additional‘
expense, and also raises thedanger of having the '
reaction mixture setI.to-a= gelfor » ifI injuring the
tle, rosin; then with .warm petroleum ;' nex'txwith:
product by employing high. temperature, any of_
{I .withIZlIow-Iboiling petroleum. 111e, 111121 solvent is 15
.cess of dry alkali,:_a_nd vigorousastirring, are used
petroleum at room temperature; and then finally
which'might nullify the commercialIvalue.,_-;Ex- .
2,406,097
. snowwhite product
57%‘.
_
.
_
..
.
_.
16v
obtained;the yield being
.
A
‘
tinguishing visual characteristic that-the solid is
V
'TABLE'VI‘
7 white.
.7,
,
" ' 'Pale'crude'gum, which would ‘produce 'WG'ifOSiYl, and NazCOa in'kerosene
'
i
R
No.
.
" b
°sm - Y
Na 00
calculation,
V
I g_
25;...“
’
2."
'r tl
"-8
tijonctmi" ‘ ‘Ram'
°“‘’ “5” alkali to
—1n1x
~bywelghtln1
g.
-
M
,
‘85.
1,750
->2s-.----_
473
1a_
1,750
27____ -_
470'
474
120 ' 1,750
Time
.
o0. '
vas
>
8*
temp.
assixg?f,
'
,
rosinate
percent
'l8.'7' ' '- 149 ' " 2.2
as
as
s di
°. “"1
Yield
'~
chrsn.
‘
I" V
57
Snowwhite.
21.9
_ 190
3.0
70
White.
20.0
r 188
2.3
,66
“ Woodrosin,v particularly‘ the FF grade, is gen
1
Do.
I 'I-Iaving. the detergentv properties that char
erally considered to be all-inferior variety, by
acterize all rosinates it can be mixed with the
‘ reason‘ 'of the large number and variety of color
. bodies present. Illustrations have been givenlin
V salts'of other fatty acids in the manufacture of _ I
soap, ‘and its standing as a rosinate which has
Tablelof'the use of these materials in jhig?he'per 20 properties, distinctive from those, of other _ros-_
' cent rosin solution. ~Tab1e'VII shows the appli
inates as above indicated constitutes the product}
cation me .zone of more critical concentration.
an improvement inv rosin soaps in which, the
In'all cases. colored rosinates are»removed,.but
rosin. present cooperates benignly with the other
therdegree of whiteness is not as high‘ as that
ingredients, without the depreciating e?ect here
~ givenrin vTable I. In thecase ofFF wood rosin,
tofore experienced.
after the vrosinl'wasdissolved in the kerosene, the
solution was preliminarily ?ltered to remove the
considerableequantity of matter insolubleqinethe '
kerosene, and than was treated as-‘described.
Successful results from very poor grades of rosin .30
are partlyaffected byv-theinsolubility of its, ex
‘ traneous matter in the solvent. As theponcen
;
I
>
I
I
V
v;
»
_
Y _ In the appended claims, the'term“‘inert,”Aap-_
plied to the liquid solvent,- indicates only itsvla'ck
of reactivity with the substancesthatlmay ‘be
present, 1. e. alkali, water, Yunneutralized rosin
acids, . rosinates, resenes, esters and whatever
other products remainl after rosin-has been
treated with-a-base; “rosin,” unless'contextin
' tration of rosin in‘ thekerosene solution dimin-vv
dicates otherwise, signi?es a body whose ‘acid _
ishes, more of this insoluble matter is found pree,
component is unneutralizedrosin acids; ,“concen
'cipitated with the precipitation" of rosinate.
35 tration offrosin’v’rin the solutionmwns- the ratio
,
; i2;
.‘
‘I
-
a
,V'QTA’BLEVIIQ,
>Wood rosin=a1td NazC-‘Os. in kerosene’ '
,-..»_ g
'_'No.'
:2
r
Rosin'gf
.
'i"t.1
7 mp0,,
.
- g-.
.
Ft‘ weed 400.-
29;.
_
»
M
1°n;° Wit“- alkali to
'5
a‘-
r
Time,
di
Yield, 2
‘1111153531,. Joslmtr W56?" 'hrs.. ‘percent
e
28.;
so
"éJoncentra-J frRatio
' H-
V
-
e 50
:
percent
L750‘
FFwood 303--
s5~*1,75o
Kwood 537---
so
71,750
'
‘
‘
percen
28
12.5
122 i
e
.
37;
,
I
I
e
2.5 v
' 22 only white.
21.1
160
2.5
,
14.9
142
71.5
Y Abietic acid is the product of isomerization of
4e
> 34
Lightbrowrn
I
-
‘Snow white.
of rosin to the total of resin
therosin acids under'acid influence. The com
~
mggllgse'. > '
a
160
’
°. ‘1m
its‘solventgby »
weight; “rosinate” refers to the,’ heterogeneous
mixture of, rosinates producedby neutralization
mercial product containSthe dark rosin acids i
which make this material degrading when used
of the various .acids that may be present in rosin,
and includes the rosinate of'any one 'of'ithos'e .
infso'aplj Practice ofvthe'present invention on
this product‘led to isolation of a white sodium
acids in a/pure form'of thev acid; e. g. ab'ietic ‘
' abietate: Commercial abietic acid, 120 g., was. . .acid; and white rosinate is considered to‘be
dissolved in enough kerosene to make a volume‘ ' “isolated? when it is separated from other ros
of v285 cc._ The mixture was then he'ated't‘o" 125°‘ ~
inates, and substances contained in or derived
from rosin, as rosin is known in‘commerce; re-:
Cvat which temperature 36 g. of anhydrous s05
dium carbonate was added. The mixture. was
gardless that non-resinous substances, e. g. alkali ' '
mechanically stirred, as in the other cases, was
or petroleum, may‘. be mixed with it’ or'adhering ~
heated to 149° C. during the course of an hour, 60 to it.
' '
and-was maintained at between 149° C. and~152° '
"Iclaim as myinvention:
C. for- one hour longer.
?ltration and washing, snow
By. white
the 'usual
sodium
cooling,
abiee
tatewas recovered.
,
V
.,
,
,
These numerous illustrations show the wide
, range'of condition's‘eunder which the invention
can be practiced and the great variety of starting:
~
j
' "
'
1. A process for dividing white alkali metalf~ '
rosinate from dark alkali metal rosinate char-y
acterized by the step "of, subjecting a hetero;
geneous mixture of alkali metal rosinates to “the
solvent action'of a solution of rosinin kerosene,
in whi'ch'the rosin-‘kerosene solution “holds in;
solution all dark rosinate ofthe mixturabyits
materialswhich' can be employed; ', From‘any of ’
1' (such the‘ process of the invention-can‘ produce ' a?‘i’nity'for dark rosinate in preference to "white
‘ f a rosinateithat ‘is white, isolated from’ all dark
rosinates as well as from'all resenesesters'and
all other‘ dark'or unsaponi?able ‘substances.
.
-The white rosinate thus isolated can be de
rosinate; white rosinate that was in the said mix; 7
ture and not taken into the rosin-kerosene so1u~
tion
2. being
The art
left of
in solid
separating
form. whitei
7
alkali?
" e
metal
scribed as‘the' sodium orlpotassium salts of rosin . -; rosinate from other alkali metal rosinates,» char; I
acids'which, when insolid "state,lhave the dis-1
V acterized by the ‘step that'all of the saidrosinate's’ I
.
2,406,097
.
.
17
are immersed in a solution of rosin in kerosene
which solution has a saturation point for dis
present, which capacity is commensurate with a
dissolving of all dark rosinate thatv is present but
not all white rosinate that is present, by preferen
tial a?inity of the rosin-organic solvent solution
to dissolve dark rosinate before it dissolves white
rosinate; followed by ?ltering out the undissolved
matter.
6. A process for producing alkali metal white
rosinate apart from other rosinates; following a,
kerosene solution commensurate with that re
quired for dissolving the quantity of dark rosinate
reaction in which a salt of an alkali metal is re
which is present.
3. A process for dividing white alkali metal
rosinate from dark alkali metal rosinate charac
terized by the step of subjecting a, heterogeneous
mixture of alkali metal rosinates to the solvent I
action of a solution of rosin in a petroleum sol
vent, in which the rosin-petroleum solution holds '
in solution all dark rosinate of the mixture, by ,
rosinate, while some white rosinate of the said
7
rosinates, determined by the quantity of rosin
solving rosinates that is high enough to permit
of all dark rosinates present being dissolved and
low enough to leave some white rosinate undis
solved; the rosin-kerosene solution holding dark
rosinate in solution in preference to white ros
inate; and the said saturation point being ?xed
by having the concentration of rosin in the rosin
its affinity for dark rosinate in preference to white
l8
solvent solution has a dissolving capacity for
v
acted with rosin that is in solution in a liquid
organic solvent, which said organic solvent by it
self alone is not a solvent for rosinate and is
chemically inert to rosin and to rosinate and to
water and is immiscible with water, thereby pro
ducing heterogeneous rosinates, in which process,
after the said reaction, the concentration of rosin
and the saturation point of the rosin-organic sol
v20 vent solution for'dissolving rosinates, determined
by that concentration of rosin, are made com
mensurate with a dissolving of all dark but not all
4. A process for dividing white alkali metal
white rosinate that is present, determinable by
rosinate from dark alkali metal rosinate charac
sampling and testing, by preferential a?inity of
terized by the step of subjecting a heterogeneous 25 the rosin-organic solvent solution to dissolve dark
mixture of alkali metal rosinates to the solvent
rosinate before it dissolves white rosinate.
'
action of arsolution of rosin in a liquid organic
7. A process for producing alkali metal white
solvent, which said organic solvent by itself alone
rosinate apart from other rosinates, as in claim 6,
is not a solvent for rosinate, is chemically inert
characterized in that during the said reaction and
to rosin, to rosinate, and to water, and is immis+ 30 process the concentration of rosin varies from an
mixture remains undissolved.
cible with water, in which step the rosin-organic
initial high proportion, approximating equality
solvent solution holds in solution all dark rosinate
with the weight of the organic solvent, down to a
of the mixture, by its ai?nity for dark rosinate in
?nal lower proportion sufficient to hold‘dissolved
preference to white rosinate; and some white
all dark rosinate that is present after the reac
35 tion but not sufficient to dissolve all white rosin
rosinate of the mixture stands undissolved.
5. A process for segregating alkali metal white
ate then present; fluidity of the mix during re
rosinate from other rosinates in a mixture of
action being maintained by heating and stirring.
rosinates by holding the mixture immersed in a
8. A process for producing alkali metal white ‘
solution of rosin in a liquid organic solvent, which ,
rosinate apart from other rosinates as in claim 6,
said organic solvent by itself alone is not a solvent
in which, during the reaction, the liquid body in
for rosinate and is chemically inert to rosin and
which the reaction is occurring is maintained free
to rosinate and to water and is immiscible with
water, in which said solution a concentration of
rosin is maintained such that the rosin-organic
from water.
'
‘
AVERY A. MORTON.
'
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