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Патент USA US2110899

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March 15, 1938.
W. WOELFLIN
2,110,899 `
ELECTRICAL METHOD FOR MANUFACTURING SULPHONATED OILS
Original Filed Dec. 26, 1933
HTTo/efwsy
2,110,899
Patented Mar. 15, 1.938 l
UNITED STATES PATENT OFFICE
ELECTRICAL LIETHOD ‘ FOR IHANUF'ACTUR'e
ING SULPHONATED‘ OILS
wmnm woemin, 'ung Beach, oeuf., assigner zu
Petroleum Rectifying Company of California,
Los Angeles, Calif., a corporation of California
Application December 26, 1933,\Serlal No. 703,945
Renewed June 5, 1937
19 Claims.
My invention relates to an improved electrical
process and apparatus for the manufacture of
` , sulphonated oils such as textile oils, leather oils,
chemical emulsifying and demulsifying agents
the fatty raw material employed in making sul
pho-fatty bodies is a mixture of fatty acids and
Vglycerides prepared by splitting or partially split- .
ting triglycerides by means >of acids or splitting
and the like, such as are used in the textile, leath- l agents like Twitchell reagents.
erv or other industries.
l
The presently described process is also appli
-
In general the problem of manufacturing sul
phonated oils and sulphonated fatty materials is
not new. Oils, fats, and the fatty acids occurring
therein have previously vbeen reacted with lsul
cable to the preparation of such materials as
-Twitchell reagents, whichl .are the products of
sulphonation of a fatty body and an aromatic
body by means of sulphuric acid or a derivative
phuric acid, oleum, chlorosulphonic acid, etc.,
thereof, this material to be sulphonated being in- -
and the resulting products of such reactions have
found utility in the textile, leather, and other
industries, especially in a partially or completely
ble of reaction with sulphuric acid or a derivative.l
neutralized state, these products being sulpho
cluded within the term “organic fatty body capa
thereof”.
_
'
,
\
-
The presentprocess is then, in general, appli 15
cable to sulphonation reactions in which the
principalingredient is an organic fatty body cap
fatty bodie‘sand containing in some cases acid
sulphates, and in others ~true sulphonic acids.
More recently the higher alcohols, e. g., cetyl al
cohol, have been employed as ingredients in sim
ilar processes to produce sulpho-bodies of some-‘
present, in addition to‘these primary ingredients,
what similar properties.
various other reactive or inert ingredients, such
Y
able 'of reaction with sulphuric acid or a deriva
tive thereof, as herein defined. There may be
The present process relates to an'improved 1 as petroleum distillates, aromatic bodies, like ben- `
process and apparatus for vthemanufacture of
such sulpho-fatty »materials and particularl to
Va sulphonation process using sulphuric aci
as
a. reaction agent. . I shall hereinafter employ the
term “organic fatty body capable of reaction with _
sulphuric acid or a derivative thereof" for the
material preliminarily- treated in the manufac
ture of such products. By4 the‘word “derivative”
in this term, I have reference to a derivative
zol or naphthalene or phenol, carbon tetrachlo- ‘
ride', etc.‘
‘
~
.
'
'I'he process of this invention is applicable in
the preparation 'of sulphonated fatty derivatives
containing large percentages ,ofi sulpho-com
pounds, as well as in the preparation of sulpho
natedffatty bodies in which the percentage of
sulpho-compounds is small, i. e., in which the 30
amount of organically combined sulphur trioxide
which is an equivalent of the sulphuric acid. In _ present is very small.
-The products of such sulphonation processes I
this term are included fatty bodies such as gly-v
cerides, animal andy vegetable oils, fats, waxes and
shall refer to as sulpho-fatty bodies, or sulphof
the fatty acids occurring therein, ’as well as thel
fatty derivatives, it being distinctlyunderstood 35
that in these terms I include not only sulpho
the oils, fats, and waxes in physical appearance .nated oils and sulphonated fatty acids, but also
and in many of their properties. Of these higher- sulpho-alcohols and sulpho-.aromatic fatty bodies.
alcohols, I include specifically those having more The sulpho-bodies referred to herein may be
than eight carbon atoms `inwthe molecule, of either true sulphonic bodies, containing the sul
phonic group, or they may be acid sulphate bodies
which group cetyl alcohol, octädecyl alcohol, me
higher aliphatic-alcohols, which latter resemble
lissyl alcoholï and ceryl alcohol may be named
containing the sulphate group.
The present method of manufacturing such
The fatty bodies referred to above includes the l sulpho-fatty materialsl consists usually of the fol
'unsaturated' oils, fats,- and fatty acids commonly lowing general steps: (l) Mixing a sulphonat
_employed in preparing sulphonated fatty deriva-V > ing agent in the form of sulphuricV acid or a suit' as
examples. _
tives.
>
40
.
.
They also include otherY fatty. materials,
e. g., hydroxystearic acid, which owe their re
able derivative thereof with an organic fatty body4
capable of reaction with such sulphur acid, either
alone or with the addition of suitable solvents,`
diluents, or other ingredients, `allowing the fr_e
activity, in the presence of sulphuric acid or its
derivatives, to -the existence of areactive group,
like the hydroxyl group, in the molecule. The , action to proceed for a desired length of time and'
more common members of this group of organic at a desired temperature. (2) Washing the acidic
.fatty bodies-capable of reactionwith' sulphuric -reaction massv with a suitable amount of an
acid are oli’ve'oil, castor oil, fish oils, sperm oil, aqueous washing medium which may be water
i whale oi1,`oxeic acid (red ou), etc. In sqmecases, Q1.’ other suitable aqueous solution. _ By wash
.
2, 110,899
2 .
ing, I mean mixing or contacting, more or_less
color the product or be detrimental to the ap
intimately; the acidic reaction mass and the suit
pearance or quality thereof.
able aqueous medium. In most cases, mixing is
continued `until a4 homogeneous mixture is pro
duced, which may separate more or less slowly.
(3) Allowing the mixture to stand in a quiescentI
state until it separates into two layers. The
excess sulphonating agent and the Washing me
dium, with possibly -some Water-soluble organic
.matten like glycerin, comprise the lower aqueous
10 layer, leaving an oily supernatant layer in the
upper part of the settling zone. (4) Withdraw
ing the lower aqueous layer. (5) Partially or
completely neutralizing the oily supernatant lay
15 er consisting of sulphonated, sulphated, or oth
erwise altered’fatty matterial, this neutralizing
action being effected by adding a suitable neu
tralizing agent, usually one of the common al
`
In the present process the above-mentioned
defects' are'overcome and a superior product is
obtained by utilizing electrical means for assist
ing in performing either or both separating steps.
Thus, the acidic >reaction mass, together with the "
water or other aqueous medium mixed there
with, may be subjected tothe action of an elec
tric field which quickly coalesces the excess of
water or aqueous medium and sulphonating agent
into masses of suñlcient size to be easily and
rapidly removed byA gravitational or centrifugal
methods.
The same -method can be used in
separating the neutralized or partly neutralized
material.
'
»
Among the important objects of the present
invention is the provision of a method and ap
_kali metal bases, caustic soda, `caustic potash, _ paratus- for forming such sulphonated' products
20
anhydrous or aqueous ammonia, etc., or one of
the alkali ‘carbonates or bicarbonates, `or other
bases like those of the alkaline earth metals.
(6) Allowing the neutralized or partially neu
tralized mass to stand in a quiescent state to
permit settling therein of the small amount of
aqueous solution remaining after the first set
tling period and the neutralizing step, as well as
to allow a settling of more or less of the water
which may have been added With'the neutral
so
izing agent.
'
.
~.
produce an improved andv superior product- of in
creased effectiveness.
l It is a further object of the invention to pro
vide a novel step in the process of producing
sulphonated fatty derivatives, Whereina mixture
of an acidic reaction mass and a washing me-`l
dium is subjected to the action of an electric
field.
_'
The length of time required for. these separa
tory steps is quite large,
which effects not only a distinct saving of time, 20
apparatus and materials in the manufacture of
these products, but which has' been found to
.
»
»
30
>A further object lies in the subjection of a
The ñrst such step, ,finished or Áa semi-finished product consisting of
a partially or completely neutralized sulphonated
wherein the lower /aqueous layer is"formed`after
washing the acidic reaction mass, frequently re
35 quires from eight to thirty-six hours, depending
on the temperatures employed in washing, the
nature of the ingredients, the reaction tempera
turek employed, and other factors. The.- second
separatory step also requiresa prolonged time
of settling to remove the Water or aqueous solu
tion. In some' cases separation of aqueous ma
fatty derivative to the action of an electric ñeld.
A'I further advantage of the present process is 35
that a saving is effected in the amount of neu
tralizing agent needed to neutralize the material .
to a desired point, as compared with the amount
needed whe/n prolonged gravitational settling is
resorted to, and it is a further object of the in_
40
vention to/'pròvide a process and apparatus which- _
vaccomplishes súch a saving in the amount of
îterial continues for as long as a month, and
products behaving in .this fashion cannot be y. materials required. ’
It is not necessary to thepresent process. that
safely marketed untilf substantially all traces of
l
.
;
an
“anhydrous product be obtained.-> The sul
this material are removed. Centrifugal methplds
>are commonly ineffectual in that they fail ma'. .plioiiiated fatty derivatives prepared in accord
terially to accelerate and facilitate the separa-¿f ance with the present process may sometimes still
contain considerable amounts of water, though in
tion and stratification of the constituents;
`
Not only do either or both of these settling steps many instances the process results in the pro
result in a great waste of time and necessitate duction of a product containingonly traces of
much additional equipment which would- other
wisc be unnecessary, but my, experiments have
shown that> it- is .very undesirable to maintain
such water or aqueous solutions in contactwith
the fsulphonated
products.
i
water.
'
It has sometimes been found desirable to util
ize an electric field of special‘oscillatory charac,
ter, andl it is another object of the present in
I have yfound that__ vention to use one or more electric fields of this 55
prolonged contact between these materials pro
duces undesirable side reactions which material
ly decrease the effectiveness of the finished prod
uct. Among these side reactions may be cited
60 hydrolytic and polymerizing reactions which vare
quite detrimental to the ñnished product.
Furthermore,- incomplete and imperfect sepa
ration of .the aqueous material before neutral
ization results `in the retention of excessive
amounts of the sulphonatin'g agent by the oily ‘
acidic mass _after washing and settling.
causes the- amount of vneutralizing agent required
.to be excessive, which in turn results in higher
costs and, if _the neutralizing base be employed
This .
character in the removal-of excess water or other
aqueous constituents from a sulphonated fatty
derivative.
.
.
Other objects and advantages of the invention
60
will be made apparent hereinafter.
The said organic fatty body capable of reaction
with sulphuric acid or a derivative thereof is ñrst
mixed with the sulphuric acid or other suitable
sulphonating agent in a reaction or mixing cham
ber of any common or desired form, with or with
65.
out the addition of diluents, solvents, reactive or
inert aromatics, etc. In the annexed drawing,
I have diagrammatically shown a tank III into
which these organic fatty materials, etc., and the
sulphonating agent are respectively introduced
in aqueous solution, also results in undesirable
as through pipes I I and I2.
dilution lof the product. Other disadvantages
are, lfor example, the inclusion of large amounts
be stirred by any suitable agitator means, not
shown, _or by a Wooden paddle. The result is"
of mineral sulphates which may separate on
standing, or which may cloud or otherwise dis
the formation of an acidic reaction mass.
These materials may
When the‘reaction has proceeded for the de
2,1 10,899
3
transference to a‘vsecond vessel. Thus, in the
ration of theaqueous layer. In some cases, the
rod and electrode may be so mounted or moved
that a constant distance is maintained between
the electrode and the constantly rising surface
latter-process, the aqueous washing medium in
the form of water or other suitable aqueous me
dium commonly employed to remove the excess
be constantly raised as separation proceeds under
the influence of the process.`
sired length of time, the acidic reaction mass
may be transferred to arwashing chamber or it
may be washed in the same tank I0 without
of thesaid aqueous layer, i. e., the electrodel ‘may
In other instances the electrode structure may
be retained in a ñxed position in the tank 2| so
that as the level indicated by the dotted line
2l ris'es the field between this level and the screen
electrode 25 will increase in intensity.
Any suitable means may be utilized for`build
ing a. potential between the rod 24 and the tank
reaction mass by any suitable agitator positioned _ 2|. Best results are-obtained if an altern-ating 15
or pulsating current is utilized. In manyin
in the tank I0 or by manual means.
stances it is possible to secure entirely satisfactory
If desired, the mixture may be allowed pre
liminarily to settle in the tank Ill to permit the treatment by'connecting the high tension wind
in_g of a transformer between the tank 2| and
bulk of the aqueous medium, consisting of wash
„in'g medium, excess sulphonating agent, and any the rod 24, this transformer being one which 20
other ingredients of the acidic reaction mass ' builds a high voltage therebetween. Potentials
such- as glycerol, which may be preferentially less than 10,000 volts in magnitude are ordinarily
sulphonating agent from such mass, such as so
dium chloride, or sodium sulphate solution, is in
troduced into the tank Il) by any suitable means.
Diagrammatically, I have illustrated a pipe I3
for introducing this aqueous washing medium
into the lower end of the tank I0. This washing
medium is intimately admixed with the acidic
soluble in water, to separate naturally by gravity,
reserving theapplication of the electrical treat
ment for the removal of the last traces of re
movable aqueous material. If this is done the
' material which gravitationally separates can be
removed through a pipe I4, allowing the remain
der of the material to move through a pipe i5
to the electric treater 2|).ä Generally, however,
the process of this invention is_most advan
tageously employed by quickly subjecting the
very satisfactory,` though usually the potentials
employed should be above 1,000 volts. Very sat
isfactory'results will thus accrue if a 5500-volt
transformer is utilized thereby making -an aver
age gradient of 1,000 volts per inch. These limits
are, however, not exclusive, for in some instances
it is possible to use potentials higher or lower ‘
than those above mentioned. ' The limits set
forth are illustrative, and I do not limit myself
thereto. With such a system the alternating po
whole mixture ol' acidic reaction mass and wash
ing medium to the action of an electric field to
separate the "removable aqueous material as rap
tential can be continuously applied or can be
idly and completely as possible, for reasons pre
viously recited herein. In this instance the en
tire mass of material is moved through the pipe
one-half cycle if desired, or may be of such length f
as to include more than one-half cycle or several
complete cycles if desired.
i
In some instances it has been found desirable
|5‘and into the treater 20.
_
As diagrammatically illustrated, this treater 20
40 mayinclude a tank 2| comprising an outer
4 vgrounded electrode on which insulators 22 are
periodically interrupted to form a series of im
pulses. Such impulses may be of a duration of
to utilize the circuit shown in the accompany
40
ing drawing, especially when treating masses of ~
an especially conducting nature. In the form/
These insulators, of any desired shown, I have illustrated a transformer 3|]v in
cluding a high voltage winding 3|, one terminal
'mounts a rod 24, which latter_` element may„in of which is grounded and connected tothe tank.
2|. The other terminal is connected to the rod
some instances, in itself comprise an inner elec
trode. In the exemplary form shown, a screen 24 through a spark gap 33. It is usually prefer
electrode 25 is retained at the lower end of the able,V though not always necessary, to place a
rod 24. As treatment progresses, there is formed condenser 34 across the high tension winding 3|,
supported.
number, carry a cross bar 23 which adjustably
in the bottom of the tank I2| an aqueous layer
the level of which slowly rises until` the mixture
ì has been substantially completely separated.
I
as shown.
The transformer 30 includes a low 50
tension winding 35 which is connected to va suit
able commercial-frequency,supply line through -a
'
'
have -indicated the' ultimate uppermost surface choke‘coil 352 .
When a treater thus connected i‘s placed in‘
4of this lo'wer aqueous layer by the dotted line 2l,
and have found it preferable to> position’the operation, the current flow throughl .the treat
screen electrode -25 a slight distance above this ing space will be limited by the choke'coil 36.. At
surface 21. If, then, a potential difference is- the same time, by properadjustment of the spari;y
maintained between the tank 2| and the rod 24, gap 33, this gap will periodically break down asv
treatment will take' place not only in the space the potential thereacross builds up. _Thus, as the '
around the rod, i. e., between this rod and the potential across the electrodes is building up?the
tank 2|, but will also take place between the condenser 34 will be charged, and when a, suf
screen electrode 25 and the tank 2|. In addition, ficiently high_,potential is attained, the spark
gap 33 will break down. vAtkthis, instant, a low
treatment will take place between the screen elec
trode 25 and the surface of the aqueous lower resistance -path is formed across thejterminals
layer which -is of a conducting nature. _The of theI spark -gap and cu'rrent can flow there
electrode 25 and the rod 24 should not at any Athrough to the electrodes. During this break
time be submerged below the upper level ofV this down period, the condenser 34 discharges to. the
lower -aqueous layer, since short-circuiting would electrodes. "This discharge is an oscillatory one
and is usually of high frequency, this frequency
be caused.l
.
v
^
‘
being determined by the-electrical characteristics Til
It is to be distinctly understood that the posi
tion of the rod and electrode in relation to the
surface ‘of the lower aqueous layer vis not to be
regarded as necessarily fixed. Different reaction
masses may require different adjustments of the
rod and electrode to -attain most efficient sepa
of the condenser 34 and theY remainder of the
circuit. However, any current flowing to ~the
electrodes decreases the potential across' the
winding 3|, especially when a choke coil 36 is
being used. Thus, the potential is reduced to such
y2,110,899
4
an extent that the arc will not persist'across the ~
ized products to the electrical separation process
spark gap- 33, thus stopping a major portion of
the current flow to the electrodes. The cycle is
repeated when the potential across the trans
former winding 3| again builds up. Other types
of high frequency systems producing an oscil
latory potential may also be _used to advantage.
Further, by using a rectiñer with spark gap and
condenser, direct-current impulses can be ob
tained. These may also be used to advantage in
of the invention is that a »product of superior
`homogeneity can frequently be so prepared. For
certain
instances.
_
_
-
After such electrical treatment the lower aque
ous layer may be withdrawn from the tank 2|
through a pipe 4D including a valve 4l. There
after the=oily acidic mass remaining in the treater
may be neutralized therein, or it may be removed
from the treater to another container in- which
_ this neutralization takes place. _In the form il
lustrated the electrode structure is so formed as
to be easily removable from the insulators 22,
thus permitting the neutralization step to take
place inthe tank 2 |-. The neutralizing agent may
I be added by any suitable means, as by a pipe 42. '
This- neutralizing agent is in the form of a
suitable ‘basa The common neutralizing agents
are sodium, potassium, and ammonium hydrox
example, sulpho-fatty materials that have been;
neutralized only slightly past the point where all
the strong acidic hydrogen has been neutralized
are sometimes marketed in this form and ñnd
particular utility in certain. commercial processes
over products which are neutralized to a greater
If the separation is allowed to take place 10
degree.
by gravitational means, such relatively under
neutralized _products exhibit the very undesirable
property of settling water or other aqueous s_olu
tion over an extended period of time.
If, there
fore, such products are marketed immediately
15
upon completion of manufacture, the separation
of such _aqueous material in the container pro
du‘ces an unfavorable reaction on the purchaser.
Thus, regardless of whether partial or complete
neutralization is effected, it is usually vdesirable 20
to subject the neutralized or partially neutralized
mass to the action of an electric field.
This can
be accomplished by reinserting the electrode'
structure in the tank 2| and establishing the
fields therein so as to coalesce and quickly remove
the water or other vaqueous solution. A superior
ides, although any other base may be employed « product is produced if such foreign substances
as desired. For example, alkaline earth metal
bases may be used, or the carbonate or bicarbon
30 ate of any desired metal or metal equivalent may
be used in this capacity. The neutralizing agent
is suitably mixed with the reaction mass, as by
being stirred or otherwise agitated either manu
are removed in a short period of time, as herein
before mentioned.
'I'he electric field utilized in
conjunction with the neutralizing step may be
of an alternating or pulsating type, as previously
described. ' With certain materials it is desirable
to use the oscillatory system illustrated, though
ally or mechanically by meansnot shown.
Insome‘instances it is possible to neutralize to
it will be understood that the utility of the process
is not dependent upon the use of su'ch a field ofv 35
the desired -degree in a single s_tep. In this in
high frequency oscillating potential.
stance the inorganic and the organic acids pres- _
If a poly-stepneutralizing process is utilizedv
this electric treating step can be performed either
ent are neutralized to the desired point by the
addition of the proper amount o‘f neutralizing
40 agent. In this instance the resulting product may
be removed through the pipe 40 or _it may be
allowed to settle for a time in the tank 2 I. Usual
ly, however, it is desirable -again to subject the
' v neutralized or partially neutralized mass to the
action of an electric ñeld as will be hereinafter
described.
'
A
-
In other instances it is desirable to vary this
procedure, and, instead of‘neutralizing the olly
acidic mass to its ñnal degree in one operation
as is -performed in the common process of manu
facturing sulphonated oils, to conduct the neu
between the time that the respective neutralizing
steps are taken or afte? the desired degree of
neutralization has been obtained by this poly- _
step neutralizing process.
It should be understood that I am not limited
to the particular apparatus shown. If desired
the tank l0 can be dispensed with and the sul
phonating agent and washing. medium added di
rectly to the tank 2| during the time that the '
electrode is not positioned therein. So also it is
possible to perform the neutralizing step in a
container separate from the tank 2|. So also, if 50
desired, the electrical treatment of the neutral
tralization in two or more steps. For example, ized or partially neutralized product can be ei- it may be desirable to neutralize in the ñrst step » fected by the use of an entirely separate- electric only the strong acidic hydrogen that is due to the treater similar to that indicated by the numeral
20. Furthermore, while it is usually desirable to
Cil :A sulphuric acid and the organic sulpho-bodies
present in the mass. Such a procedure would utilize the invention in conjunction with a batch
thus permit the settling of mineral sulphates. ‘ process, it will be apparent that my process is
water andA other similar aqueous or water-soluble equally applicable to the preparation of sulpho
material before completing the neutralization in fatty bodies by continuous processes and the use
of the word "mass” in the appended claims is not
60 one or more subsequent steps., In this Way the
presence of rexcessive amounts of such inert and to beconstrued as limiting same to a batch proc
frequently undesirable substances can be avoided.
ess.
-
' The subsequent neutralizing step or steps would
I claim as my invention:
_be used for the purpose of neutralizing the prod- .
1. An improvement in the process of manu
uct to any desired degree, e. g., _until a water
facturing sulpho-fatty bodies, which improve
_soluble oil is obtained.
The product can be car- - ment includes the steps of: intimately contacting
ried to the point of complete neutralization if de
the reaction organic fattybody to be sulpl'ionated
sired, or neutralization may _stop short thereof,
depending upon the product to be produced. If
and a. sulphonating agent to form an acidic reac
tion'mass; mixing said acidic reaction mass with
an aqueous washing medium; separatingat least
out, it has been found very desirable to subject the . a part of said aqueous Washing medium by ap
semi-finished product to the action of an electric plying to the'mixture an electricñeld; Withdraw
iield, thus. greatly decreasing the time `necessary ' ing the separated aqueous layer; at least partially
to separate the removable material. An advan
neutralizing the remaining oily acidic mass ;.. and
such a poly-step neutralizing process is carried
tage accruing from subjecting such semi-neutral
subjecting said partially neutralized mass to the 75
5 ,
2,110,899
‘ action of an ‘electric field to separate aqueous- reaction with sulphuric acid or a derivative there
material therefrom.
of to'form an acidic reaction mass. which im
_
provement includes the steps of: mixing said
acidic reaction mass with an aqueous washing
medium; separating at least a portion of the
aqueous washing medium to leave an oily acidic
2. An improvement in the process of manu
facturing sulpho-fatty bodies by adding a sul
phonating agent to an organic fatty body capable
of reaction with‘sulphuric acid or a derivative
thereof to form an acidic- reaction mass, >which
mass; partially but not completely neutralizing
said oily acidic mass; subjecting theresultant
product to the action of\ an electric ñeld of high
improvement includes the steps of: mixing said
acidic reaction mass with an aqueous washing
. intensity to -coalesce at least a part of the aque
10 medium; and then subjecting the resulting mix
field to quickly separate the oily portion of the
acidic reaction mass from the aqueous washing
layer.
medium and substances associated therewith,>
preventing prolonged contact rwhich
V15 thereby
would set up deleterious side reactions.
10
ous -material removable therefrom; allowing the
electrically treated material to settle to form
an aqueous layer; and removing said aqueous
ture ’to the action of a high-intensity electric
`
8. An improvement in the process of manufac
‘ -turing sulpho-fatty bodies by adding a sulphonat
ing agent to an organic fatty body capable of
‘3. An improvement in the process of manu
facturing sulpho-fatty bodies by adding a sul
phonating agent to an organic fatty body ca
20 pable of .reaction with sulphuric acid or a deriv
reaction with sulphuric acid or a derivative
thereof to-fo-rm an acidic reaction mass, which
improvement includes the steps of: mixing said 20
acidic reaction mass with an aqueous washing
ative thereof to `form an acidic reaction mass.
medium; separating at least a portion of the
aqueous Washing medium to leave an oily acidic
which improvement includes the steps of: mixing
said acidic reaction mass with an aqueous wash
mass; partially neutralizing said oily acidic mass;
subjecting the resultant product to the action of
an electric field of high intensity; and subse
quently further neutralizing the material treated
ing medium; 'subjecting the washed acidic re
action mass to the action >of a high-intensity
electric field to coalesce`at least a part of the
aqueous material; settling said coalesced material
to form an aqueous layer; withdrawing the ma
terial in said aqueous layer; and separately with
'
by's‘aid
‘
4. An improvement in the process of manu
-
reaction `with sulphuric acid or a derivative
thereof to form an acidic reaction mass, which
-i'acturing sulpho-fatty bodies by adding a sul
phonatlng agent to an organic fatty .body ca
pable of reaction with sulphuric‘acid or a deriv
ative thereof to form an acidic’reaction> mass,
which improvement includes the steps of: mixing
improvement includes the steps of: mixing said
acidic reaction mass with an aqueous Washing
medium; separating at least a portion of the
aqueous washing mediumA to leave an oily acidic
mass; at least partially neutralizing said oily
acidic mass; subjecting the resultant product to
-said acidic reaction mass with an aqueous wash
ing medium; immediately subjecting the mixture
to the action of a high-intensity electric ñeld to
coalesce at least a partfefl the aqueous material;
'the action of an electric ñeld of high intensity l40
to coalesce at least a part of the aqueous ma
and` relatively> quickly separating said aqueous
5. An improvement in the process of manu
.
turing sulpho-fatty bodies by adding a sulphonat
ing _agent to an organic fatty body capable of
drawing the remainder of the reaction mass.
material thus coalesced from the remainder -of
the mass to prevent prolonged contact-which
would set up deleterious side reactions;`
electric field.
9. An improvement in the process of manufac
terial therein; removing said coalesced material;
and further neutralizing the product remaining
after removal of said coalesced material.
«
~ 10. An improvement in the process of manu
facturing sulpho-fatty bodies byr adding a sul
facturing sulpho-fatty bodies as described in
phonating agent to an organic fatty body ca
pable of reaction with sulphuric acid or a deriv
ative thereof to form an acidic reaction mass,
ñéld is of high frequency character.
which improvement includesgthe steps of : mixing
said lacidic reaction mass with an aqueous wash
ing medium; allowing the mixture to stand in a
quiescent state until a portion of the washing
medium and other material preferentially soluble
in water have separated; and thereafter separat
ing the only portion of said washing-medium` and
45
claim 2, in which said high-intensity electric ’
1l. An improvement in the process of manu
facturing sulpho-fattyvbodies by adding a sul
phonating agent to an organic fatty body capa
50
ble of reaction with sulphuric acid or a deriva
tive thereoff to form an acidic reaction mass.
which-improvement includes the steps of : period
ically discharging a condenser in circuit with a
pair of electrodes bounding a treating space to
the remainder of said reaction mass by sub- ' establish an electric stress in `said treating space;
jection to the action of a high-intensity electric
field.
60
Y
.
‘
'
6. An improvement in the process of manufac
turing sulpho-fatty bodies by adding a sulphonat
ing agent to an organic fatty body capable of
`reaction with sulphuric acid or a derivative there
of to form an acidic reaction mass, which im
63
provement includes the steps of: mixing said
mixing said acidicY reaction mass with an aque
ous washing medium; and subjecting the mixture
. to the action of said electric stress.
‘ 60
12. An improvement in the process of manu
facturing sulpho-fatty bodies by ladding a sul
phonating agent to an organic fatty body ‘capa
ble of reaction with sulphuric acid or a deriva
tive thereof to form an acidic reaction mass,
which improvement includes the steps of : es
acidic VVreaction mass with an `aqueous washing
medium; separating- at least a» portion of ‘the ` tablishing an oscillatory electric field; mixing
aqueous washing 'medium to leave an,_ oily acidic
mass; « at least partially `neutralizing. said oily
acidic mass: and subjecting the resultant prod
uct to the action of an electric field` of high in
tensity.
,
¢
H
7. An improvement ,in the process of manufacf
turing sulpho-fatty bodies by adding a sulphonat
ing agent to an organic fatty body capable of
i
said acidic reaction mass with an aqueous wash
ing medium; and subjecting- the mixture to the
action 'of said oscillatory electric ileld.
13. FAn improvement in the process of manu
facturing sulpho-fatty bodies as described in
claim 2, in which said high-intensity electric
field is established by impressing an alternating
/
2,110,8'99
6
potential of commercial frequency across a pair
washed maß by adding a base in insuilicient `
quantities to completely neutralize same; then
separating at least a part of the aqueous material
facturing sulpho-fatty bodies as described in - from the partlyAneutralized mass; thereafter
-claim 2, in which said high-intensity electric'ñeld ' adding additional quantities of a base; and sube.
of electrodes.
14. An improvement in the process of manu
is established by impressing analternating po
jecting the product- resulting‘from the second
tential across a pair of electrodes-fand including
neutralizing step tothe action of a high-intensity `
the step Ioi’ ’periodically impressing an oscilla
tory potential of high frequency across said elec
-.
10~ trodes.
15. An improvement in the process of manu
electric
ileld.
`
v
,
'
-
418. A process asdeiined in claim 17 in which
'said separation step performed between said 10=
neutralization steps is performed by subjecting
facturing sulpho-fatty bodies as described in "the mass to the action of an electric- ileld after
claim 2, in which said high-'intensity electric 'the first addition of said base and prior> to the
subsequent neutralization to separate a vportion
field is established by impressing a potential be
15 tween a pair of electrodes, and periodically inter--k of the first-added base prior to the subsequentA 16
rupting said potential.
neutralization.
16.` An improvement in the process of manu
facturing sulpho-fatty bodies as described in
'
`
19. An improvement in the process of manu- -
facturing -sulpho-fatty bodies by `adding a sul
claim 2,-in which said high-intensity electric , phonating agent to an organic fatty body capable
20 field is established by impressing an alternating
potential between a pair of electrodes, and pe
' riodically interruptinglsaid alternating potential.
17. An- improvement _in the process of manu?
facturing sulpho-fatty bodies by adding a‘sul
25 phonating agent to `an organic fatty body capa
ble of reaction with sulphuric acid or a deriva
tive thereof to form a reaction mass, which irn
provement includes the steps of: mixing said
>reaction mass with an aqueous washing medium;
of reaction with sulphuric acid or a derivative 20
thereof to form an acidic reaction mass, which
.improvement includes the steps of t mixing said
acidic reaction mass fwith an- aqueous washing
medium; subjecting the washed acidic reaction
mass to the action of an electric ñeld to separate 25
at least a part of the aqueous material; at least _
partially> neutralizing the resulting oily reac-=
tion mass; and subjecting the resulting product
to the action of an electric field of high intensity.
30 separating at :least »a portion- of said aqueous
so
WILLIAM WoELFuN.
washing medium; then partly neutralizing the
CERTIFICATE V0F coRaEcTIoN.r
Patent No.' 2,110,899.
March 15, 1958-. I
WILL IAM WOELFLIN .
It is hereby certified -that error appears in the printed specification
of the above numbered patent requiring correction as follows: IPage. 2, first_ column, line 16, for "matterial" read naterial; page 5, first column, ~line56, claim 5, for "only" read oily; and that the said Letters Patent should
be readwith these corre ations' therein, that theA vsame may conform to the record
of the case in the Patent Office..
Signed' and sealed this 10th day of l'iay, A._ D. 1958..
(Seal.)
~
Henry Van Arsdale,.-
_
y
Acting Commissioner of Patents.
/
2,110,8'99
6
potential of commercial frequency across a pair
washed maß by adding a base in insuilicient `
quantities to completely neutralize same; then
separating at least a part of the aqueous material
facturing sulpho-fatty bodies as described in - from the partlyAneutralized mass; thereafter
-claim 2, in which said high-intensity electric'ñeld ' adding additional quantities of a base; and sube.
of electrodes.
14. An improvement in the process of manu
is established by impressing analternating po
jecting the product- resulting‘from the second
tential across a pair of electrodes-fand including
neutralizing step tothe action of a high-intensity `
the step Ioi’ ’periodically impressing an oscilla
tory potential of high frequency across said elec
-.
10~ trodes.
15. An improvement in the process of manu
electric
ileld.
`
v
,
'
-
418. A process asdeiined in claim 17 in which
'said separation step performed between said 10=
neutralization steps is performed by subjecting
facturing sulpho-fatty bodies as described in "the mass to the action of an electric- ileld after
claim 2, in which said high-'intensity electric 'the first addition of said base and prior> to the
subsequent neutralization to separate a vportion
field is established by impressing a potential be
15 tween a pair of electrodes, and periodically inter--k of the first-added base prior to the subsequentA 16
rupting said potential.
neutralization.
16.` An improvement in the process of manu
facturing sulpho-fatty bodies as described in
'
`
19. An improvement in the process of manu- -
facturing -sulpho-fatty bodies by `adding a sul
claim 2,-in which said high-intensity electric , phonating agent to an organic fatty body capable
20 field is established by impressing an alternating
potential between a pair of electrodes, and pe
' riodically interruptinglsaid alternating potential.
17. An- improvement _in the process of manu?
facturing sulpho-fatty bodies by adding a‘sul
25 phonating agent to `an organic fatty body capa
ble of reaction with sulphuric acid or a deriva
tive thereof to form a reaction mass, which irn
provement includes the steps of: mixing said
>reaction mass with an aqueous washing medium;
of reaction with sulphuric acid or a derivative 20
thereof to form an acidic reaction mass, which
.improvement includes the steps of t mixing said
acidic reaction mass fwith an- aqueous washing
medium; subjecting the washed acidic reaction
mass to the action of an electric ñeld to separate 25
at least a part of the aqueous material; at least _
partially> neutralizing the resulting oily reac-=
tion mass; and subjecting the resulting product
to the action of an electric field of high intensity.
30 separating at :least »a portion- of said aqueous
so
WILLIAM WoELFuN.
washing medium; then partly neutralizing the
CERTIFICATE V0F coRaEcTIoN.r
Patent No.' 2,110,899.
March 15, 1958-. I
WILL IAM WOELFLIN .
lïzishereby certified that error appears in the printed specification
dftheabovennmberedpatentrequiringcorrectionasfbllows: Page 2, first
_ column, line 16, for "matterial" read naterial; page 5, first column, .line-
56, claim 5,for“on1y"readoily; and thatthesaid Letters Patent should
be readwith these corre ations' therein, that theA vsame may conform to the record
of the case in the Patent Office..
Signed' and sealed this 10th day of l'iay, A._ D. 1958..
(Seal)
~
Henry Van Arsdale,.-
_
y
Acting Commissioner of Patents.
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