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Patented Feb. 14,v 1950'
orrics ‘
Carl S. Carlson, Elizabeth, and Howard E fllahlley,
.11 ersey (City, N. 3., assignors to Standard (iii llBe=
veiopment @empany, a coration of Deiaware
g. Appiica?on Ant 23.. 1946,
Seriai No. 692,708
2 Claims. (Ci. 26%657)
soluble or insoluble foam-inducing substances
are removed to enable the system to operate at
troi of foaming.
normal capacity. It is contemplated in this in
Foaming of solutions in reactors, evamrators,
vention to provide means in such a system where
and the like, is the cause of decreased equip
y be allowed to foam over and
ment capacity, as it requires equipment having CR by the system
whereby foam may be removed from the system.
greater volume, etc. Foaming in distillation
It is contemplated that the system may be op
systems results in a loss of emciency in the sys
erated until the foaming-over occurs and the
tem and usually in decreased capacity.
foam is removed from the system or that ‘a sur
An object of this invention is to remove foam
inducing impurities from a system prone to foam. 10 face active material which induces foaming may
be added to the system at any time after op
smother object of this invention is to permit
eration has started and after the foam-inducing
a small amount of foaming-=over in a system
substances in the system have accumulated.
whereby foamsinducing impurities in the system
whereby substantial foaming is induced and re
are substantially removed.
Still another object of this invention is to pro~ 15 sults in foam‘ being carried out of the system.
It is also contemplated in this invention that
mote a small amount of foaming-over in a sys
a surface active material may be added to a
tem prone to foam by the addition of a surface
system which is prone to foam in order that
active material, thereby removing foam-induc
foam may be inhibited until the foam-inducing
ing impurities.
Another and further object of this invention 20 substances, which are produced in the system,
have reached such a concentration that it is de
is to prevent foaming in a system prone to foam
sirable that they be removed. At this point, an
by the addition of a small amount of a surface
additional amount of surface active material.
active agent, whereby foaming is inhibited, un
large enough to induce foaming, may be added
til foam-inducing impurities are accumulated to
in order that foaming-over may occur and the
a troublesome degree, and then to promote foam
foam-inducing impurities be removed from the
ing-over by the addition of a larger amount of
This invention relates to a process for the con
surface active material whereby foam-inducing
Surface active materials, in general, may be
materials are removed from the system.
used in the practice of this invention; the fol
Other objects and a fuller understanding of
the invention may be had by referring to the 30 lowing have been found particularly advantage
ous: petroleum sulfonatcs, salts of alkyl aromatic
following description and claims.
' sulfonic acids, sodium sulfosuccinic esters, qua
It has been discovered that by removing a sub
ternary amine salts, polyethers, and long-chain
stantial amount of the foam from a system which
shows a tendency to foam during the course of
The amount of surface active vmaterial which
its operation, that foaming in such a system'is
is added to a system to inhibit foaming is with
inhibited and ceases to be a troublesome feature
in the range of from 5 to 25 parts per million of
and a deterrent to e?icient operation of the sys
‘the liquid in the system. The amount of sur
tem at normal capacity. Foaming in a system
face active material which is added to induce
which is prone to foam occurs ordinarily after
foaming'is within the range of from 100 to 500
an initial period in which foaming is not a major
parts per million of the liquid in the system.
problem; this is probably due to the formation
The amount of liquid in the system removed
during the initial period, of foam-inducing sub
as foam by allowing or inducing foaming-over is
stances. Foam-inducing substances may be
within the range of from 1 to 10% of the total
soluble or insoluble materials such as polymers
and so forth, which are generally large molecules 45 volume of the liquid in the system; the preferred
amount is within the range of from 1 to 5%.
and which upon continuous operation of the
The practice of this invention is not to be re
system, particularly when the system is heated.
stricted to any particular means of removing foam
may be carbonized to result in ?nely divided in
from a system in which foaming causes di?icul
soluble particles which are highly conducent to
ties; the foam may be drawn oil‘ from the sys
foaming. When these insoluble or soluble par
tem at any level at which the foam is present
ticles which induce foam have accumulated in
but it is preferred to draw off the foam at the
the system to an appreciable amount, foaming
top of the foam level by letting the foam ?ow out
results which is so serious that the capacity of
of the system through some such means as an
equipment is reduced. By removing at this point,
a substantial amount of the foam, enough of the 65 over?ow pipe or conduit. The foam which is
drops of lauryl sulfate were added to the solu
tion and this induced foaming to such an ex
tent that foam came over the top of the gradu
removed from the system may be allowed to settle
and the clear liquid free from any insoluble par
ticles may be returned to the system, however,
any other means such as ?ltration may be used
ate. Foaming then subsided in the graduate to
to separate the liquid from any insoluble foam
a point where it was negligible.
inducing particles.
From the above exemplary material and de
scription of the invention it will be seen that ‘by
the practice of this invention the dii?culties en
countered as a result of foaming in a system i
prone to foam are obviated and operation of such
a system may then be conducted without encoun
tering the di?iculties resulting from excessive
foaming and at the normal capacity of the sys
The practice of this invention is applicable to
any system which is prone to foam and is par
ticularly applicable to the system in which alkyl
chlorides are synthesized from hydrogen chloride
and an aliphatic alcohol in the presence of an
aqueous metal chloride catalyst‘ or an aqueous
mixture of metal chlorides and particularly an
tem equipment.
aqueous metal chloride catalyst such as zinc chlo
As many apparently, widely different embodi
ride or zinc chloride in combination with other 15
ments of this invention may be made without
metal chlorides such as those of the alkali and
departing from the spirit and scope thereof, it is
alkaline earth metals, e. g., calcium chloride, po
to be understood that the invention is not to be
tassium chloride, bismuth chloride, also antimony
limited to the speci?c embodiment thereof, in
chloride, stannic chloride and lead chloride. It is
also particularly applicable to the system in which 20 .the nature of examples, except as de?ned in the
appended claims.
a butadiene-cuprous ammonium acetate complex
What is claimed is:
solution is heated to produce butadiene, which
1. A process for controlling spontaneous foam
has been concentrated by means of the cuprous
ing in a continuously reacting aqueous liquid
salt. It may also be used in similar concentra
phase system, wherein an alkyl chloride is pre
tion of_ other conjugated dienes, such as isoprene,
pared from hydrogen chloride and an aliphatic
the piperylenes, the conjugated hexadienes, etc.,
by means of cuprous salt complexes.
alcohol in the presence of a metal chloride cata
lyst in aqueous solution during which reaction
Example I
foam-inducing substances are continuously
Three per cent by volume of the liquid contents 30 formed and built up, which comprises an' initial
was removed, as foam, from a reaction zone in
step of adding lauryl sulfate to the system in a
which methyl alcohol-and hydrogen chloride were >~small amount su?lcient to suppress foam forma
contacted with aqueous zinc chloride at 150° C.
tion, whereby foaming is inhibited, followed by
for the production of methyl chloride and in
a second step during which period the reaction is
which foaming was so bad that the system could 35 allowed to proceed and foam-inducing substances
not be operated at normal capacity because of
continuously form and build up to an undesir
the high level of the foam. Foam was allowed to
able concentration within the aqueous liquid
go out of the reaction zone through an opening
phase reacting ‘system, and a third step of subse
at the top of the reaction chamber which led to
quently adding lauryl sulfate to the system in an
a receptacle in which the foam was caught. 70 40 amount su?lcient to positively produce foam
cc. of liquid was removed as foam from the re
therein, and thereafter removing said foam so
actor and 2100 cc. remained in the reactor. The
produced from said system leaving behind a rela
liquid remaining in the reactor was clear and
tively foam-free aqueous liquid phase in which
substantially free from suspended particles or
the preparation of the alkyl chloride is continued.
sediment. The level of the foam in the reactor
2. A process according to claim 1, in which 6 to
was then ‘low and caused no di?iculty in oper
25 parts per million of lauryl sulfate are added
ating the system at normal capacity.
to the reacting system in the initial step and 100
to 500 parts per million of lauryl sulfate are added
Example II
to the system in the third step.
Two liters of 60% zinc chloride solution was 50
withdrawn from a reactor in which the reaction
described in Example I was being conducted and
was agitated in the two liter graduate at room
temperature with nitrogen. A foam level of 3 to 4
inches was observed.
One drop of lauryl sul- -
fate was added to the graduate which reduced the
foam level to a point where it was negligible.
Thirty drops of lauryl sulfate were then added
to the graduate and this induced foaming to the
point where the foam was carried out of the grade
uate. Although agitation of the liquid remain
ing in the graduate was continued with nitro
gen, foaming then subsided in the graduate to
The following references are of record in the'
?le of this patent:
a point where it was negligible'
Example III
Frei _____________ __ Dec. 9, 1930
Dole et a1. ______ .._ June 13, 1939
Miles ___________ .._ Mar. 28, 1944
Bennett et a1. _____- Dec. 11, 1945
Arnold __________ __ Feb. 26,
Cone ___________ __ May 14,
Showalter _______ .._ May 14,
Monson __________ __ Oct. 1,
Two liters of 60% zinc chloride solution which
had been withdrawn from a reactor in which the
reaction described in Example I was being run
Ross et 111., “Industrial and Engineering Chem
was agitated in a two liter graduate at room tem 70 istry,” vol. 36, pages 570-573 (1944).
perature with nitrogen. The foam level was 3 to
Atlas Powder Co., “Surface Active Agents,"
4 inches above the level of the solution. Thirty
pages 42-3 (1948).
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