U.S. patent number 3,881,949 [Application Number 05/336,223] was granted by the patent office on 1975-05-06 for vapor degreaser process employing trichlorotrifluoroethane and ethanol.
This patent grant is currently assigned to E. I. du Pont de Nemours & Company. Invention is credited to Carl Martin Brock.
United States Patent |
3,881,949 |
Brock |
May 6, 1975 |
Vapor degreaser process employing trichlorotrifluoroethane and
ethanol
Abstract
Articles are cleaned in a vapor degreaser open to the atmosphere
utilizing mixtures of 1,1,2-trichloro-1,2,2-trifluoroethane and
ethanol as the boil sump liquid; the concentration of ethanol
exceeding its azeotropic value. The vapors of the boil sump liquid
are maintained in a nonflammable condition by: A. employing a boil
sump liquid consisting essentially of 35-85 weight percent of
1,1,2-trichloro-1,2,2-trifluoroethane and 15-65 weight percent of
ethanol; B. employing a rinse sump liquid consisting essentially of
88-100 weight percent of 1,1,2-trichloro-1,2,2-trifluoroethane and
0-12 weight percent of ethanol; C. adding to maintain the liquid
volume of the system a make-up liquid mixture consisting
essentially of 90-97 weight percent of
1,1,2-trichloro-1,2,2-trifluorethane and 3-10 weight percent of
ethanol in such amount that the volume of the boil sump liquid is
at least the volume calculated from the equation v.sub.m = v.sub.i
/100 [(1.44 c.sub.b + 2.30 c.sub.r - 22.1)] Wherein v.sub.m =
minimum permissible volume of boil sump liquid, v.sub.i = initial
volume of boil sump liquid, c.sub.b = initial weight percent
concentration of ethanol in the boil sump liquid and c.sub.r =
initial weight percent concentration of ethanol in the rinse sump
liquid; and D. maintaining the liquid volume in the rinse sump and
condensate diverting means at least equal to the initial liquid
volume in the boil sump.
Inventors: |
Brock; Carl Martin (Wilmington,
DE) |
Assignee: |
E. I. du Pont de Nemours &
Company (Wilmington, DE)
|
Family
ID: |
23315106 |
Appl.
No.: |
05/336,223 |
Filed: |
February 27, 1973 |
Current U.S.
Class: |
134/31;
134/40 |
Current CPC
Class: |
C23G
5/02 (20130101) |
Current International
Class: |
C23G
5/00 (20060101); C23G 5/02 (20060101); B08b
005/00 () |
Field of
Search: |
;134/11,12,31,40,105,109
;252/364 ;202/17D |
References Cited
[Referenced By]
U.S. Patent Documents
Foreign Patent Documents
Primary Examiner: Bashore; S. Leon
Assistant Examiner: Caroff; Marc L.
Claims
I claim:
1. In a method of cleaning articles in a vapor degreaser which is
open to the atmosphere and comprises:
a. a boil sump containing a boil sump liquid;
b. at least one rinse sump which contains a rinse sump liquid and
has an overflow means so that overflow rinse sump liquid
gravitationally flows into the boil sump;
c. a means for condensing vapors of the boil sump liquid;
d. a means for diverting condensed vapors to the rinse sump;
and
e. a vapor space between the condensing means and the boil and
rinse sumps,
said boil and rinse sump liquid consisting essentially of
1,1,2-trichloro-1,2,2-trifluoroethane and ethanol and said method
comprising:
a. boiling the boil sump liquid;
b. introducing articles to be cleaned into the degreaser and
passing the articles through at least the vapor space of the
degreaser;
c. condensing the vapors of the boil sump liquid;
d. adding 1,1,2-trichloro-1,2,2-trifluoroethane and ethanol as
necessary to maintain the liquid volume of the system; and
e. removing the articles from the degreaser,
the improvement whereby the vapors of the boil sump liquid are
maintained in a nonflammable condition by:
a. employing a boil sump liquid consisting essentially of 35-85
weight percent of 1,1,2-trichloro-1,2,2-trifluoroethane and 15-65
weight percent of ethanol;
b. employing a rinse sump liquid consisting essentially of 88-100
weight percent of 1,1,2-trichloro-1,2,2-trifluoroethane and 0-12
weight percent of ethanol;
c. adding to maintain the liquid volume of the system a make-up
liquid mixture consisting essentially of 90-97 weight percent of
1,1,2-trichloro-1,2,2-trifluoroethane and 3-10 weight percent of
ethanol in such amount that the volume of the boil sump liquid is
at least the volume calculated from the equation ##EQU3## wherein
v.sub.m = minimum permissible volume of boil sump liquid,
v.sub.i = initial volume of boil sump liquid,
c.sub.b = initial weight percent concentration of ethanol in the
boil sump liquid, and
c.sub.r = initial weight percent concentration of ethanol in the
rinse sump liquid; and
d. maintaining the liquid volume in the rinse sump and condensate
diverting means at least equal to the initial liquid volume in the
boil sump.
2. The process of claim 1 wherein the boil sump liquid contains
about 35 weight percent of ethanol and the rinse sump liquid and
the make-up liquid each contains about 4 weight percent of ethanol.
Description
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to a method for cleaning articles,
especially electrical articles, in a vapor degreaser employing
trichlorotrifluoroethane and ethanol.
2. Description of the Prior Art
Prior art vapor degreasers usually comprise an open top enclosure
having at least one sump, containing a boiling solvent (boil sump
liquid), and condenser means. The enclosure and condenser provide
means for containing and condensing the normally heavier-than-air
vapors generated by the boiling solvent. There is provided within
the enclosure a vapor space above the boil sump liquid, a vapor-air
interface in the region of the condensing means and a region of
quiescent air above the vapor-air interface. Characteristic of
prior art vapor degreasing processes, as opposed to other solvent
degreasing processes, is the condensation of solvent vapors on the
article being cleaned.
Most prior art degreasers comprise also at least one normally
unheated rinse sump; the condensate from the condenser is directed
to the rinse sump to maintain the rinse sump full with distilled
solvent (rinse sump liquid). Flow of rinse sump liquid over a weir
separating the boil sump from the rinse sump returns the excess
rinse sump liquid to the boil sump. In degreasers of this kind
articles to be cleaned are normally passed through the boil sump
liquid and thereafter through the rinse sump liquid. The rinse sump
liquid not only rinses the article but it cools the article so that
on removal from the liquid, vapors in the vapor space condense on
the article surfaces to provide a final rinse with freshly
distilled solvent. The condensing vapors reheat the article so that
on removal to the region of quiescent air above the interface, the
article quickly dries; the bulk of the vapors generated during such
drying return, by virtue of their normally greater-than-air
density, to the vapor space.
Some prior art degreasers comprise an external condensate system;
condensate from the condenser is diverted in part to a hold tank
fitted with a normally flexible tube communicating with a nozzle,
ordinarily hand held, for spraying articles in the vapor space. A
pump for propelling the condensate is usually provided. The sprayed
condensate may perform the functions of a rinse sump liquid or it
may supplement the functions of that liquid.
Many commercial degreasers are fitted with automatic safety and
convenience devices. Such devices include float-actuated switches
which function to maintain the boil sump liquid volume constant by
adding make-up liquid from a reservoir as needed. Some devices
include float-actuated switches which operate to shut off heat
provided to the boil sump if the volume of the boil sump liquid
falls so low as to risk overheating the residue of the sump.
Vapor degreasing is often employed for the removal of flux from
soldered circuit boards. A typical circuit board consists of a thin
plate normally of epoxy resin reinforced with glass fibers and
carrying electrical connectors, usually on only one side,
consisting of thin strips of copper. Electronic components are
normally placed on the side opposite the connectors and, by means
of leads passing through holes in the board, are attached to the
connectors by crimping and the like, followed by soldering.
Soldering is carried out by first coating the connector side of the
board with a flux and then passing that side of the board over the
surface of molten solder. The fluxes employed in this use consist
for the most part of rosin. Increasingly popular in the trade are
rosin fluxes which are activated by the addition of ionic materials
such as oxalic acid derivatives and amine hydrochlorides, typically
trimethylamine hydrochloride. The activators ensure better solder
bonds, especially on slightly corroded connectors and leads.
The choice of a solvent for the removal of the flux is restricted
by the requirement that the solvent not attack the board or the
various materials of construction of the electronic components.
Alcohols have been used; however, their use is limited because of
the severe danger of fire. The known nonflammable azeotropic
mixture of 1,1,2-trichloro-1,2,2-trifluoroethane, a mild
nonflammable solvent, and 4 weight percent of ethanol has been
widely used. Being azeotropic, the mixture does not separate
distillatively into its components and there is no danger of
accumulation in the boil sump of flammable mixtures containing high
concentrations of ethanol. The mixture may be undesirable if, due
to the materials in the activated flux used, it leaves a white
residue on the board and on the components. The mixture of
1,1,2-trichloro-1,2,2-trifluoroethane and 35 weight percent ethanol
has been used in cold defluxing operations wherein the boards are
dipped in the mixture at room temperature and then allowed to dry.
Attempts to use such a mixture in the degreaser mode of operation
have led to the formation of mixtures having high concentrations of
ethanol in the boil sump and to the formation of flammable vapors
in the vapor space.
OBJECTS AND SUMMARY OF THE INVENTION
It is an object of this invention to provide a process permitting
the safe use in a vapor degreaser of boil sump liquids which
initially comprise 1,1,2-trichloro-1,2,2-trifluoroethane and
ethanol, the latter in excess of the azeotropic amount. A further
object is to provide a vapor degreaser process for the defluxing of
circuit boards, said process employing boil sump liquids comprising
1,1,2-trichloro-1,2,2-trifluoroethane and ethanol, the latter in
excess of the azeotropic concentration. Another object is to
provide such a process whereby improved defluxing, particularly
with respect to the removal of the white residue hereinbefore
described, is realized without formation of flammable vapors in the
vapor space.
In summary, the invention herein resides in an improvement in the
prior art method of cleaning articles in a vapor degreaser which is
open to the atmosphere and comprises:
a. a boil sump containing a boil sump liquid;
b. at least one rinse sump which contains a rinse sump liquid and
has an overflow means so that overflow rinse sump liquid
gravitationally flows into the boil sump;
c. a means for condensing vapors of the boil sump liquid;
d. a means for diverting condensed vapors to the rinse sump;
and
e. a vapor space between the condensing means and the boil and
rinse sumps,
said boil and rinse sump liquid consisting essentially of
1,1,2-trichloro-1,2,2-trifluoroethane and ethanol and said method
comprising:
a. boiling the boil sump liquid;
b. introducing articles to be cleaned into the degreaser and
passing the articles through at least the vapor space of the
degreaser;
c. condensing the vapors of the boil sump liquid;
d. adding 1,1,2-trichloro-1,2,2-trifluoroethane and ethanol as
necessary to maintain the liquid volume of the system; and
e. removing the articles from the degreaser.
In the improved process of this invention the vapors of the boil
sump liquid are maintained in a nonflammable condition by:
a. employing a boil sump liquid consisting essentially of 35-85
weight percent of 1,1,2-trichloro-1,2,2-trifluoroethane and 15-65
weight percent of ethanol;
b. employing a rinse sump liquid consisting essentially of 88-100
weight percent of 1,1,2-trichloro-1,2,2-trifluoroethane and 0-12
weight percent of ethanol;
c. adding to maintain the liquid volume of the system a make-up
liquid mixture consisting essentially of 90-97 weight percent of
1,1,2-trichloro-1,2,2-trifluoroethane and 3-10 weight percent of
ethanol in such amount that the volume of the boil sump liquid is
at least the volume calculated from the equation ##EQU1## wherein
v.sub.m = minimum permissible volume of boil sump liquid,
v.sub.i = initial volume of boil sump liquid,
c.sub.b = initial weight percent concentration of ethanol in the
boil sump liquid and
c.sub.r = initial weight percent concentration of ethanol in the
rinse sump liquid; and
d. maintaining the liquid volume in the rinse sump and condensate
diverting means at least equal to the initial liquid volume in the
boil sump.
If the volume of the boil sump liquid is allowed to decrease below
the volume determined (as a range) by the aforesaid equation, the
vapors in the vapor space will become flammable.
It is to be understood that the ethanol employed in the process of
this invention can be pure ethanol or the commonly used denatured
ethanols which are readily available. It is to be further
understood that the articles being passed through the degreaser may
be conveyed in any manner known in the art.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 shows a conventional 2-sump vapor degreaser.
FIG. 2 is a graph relating boil sump liquid volume to time in an
experiment wherein make-up liquid was added intermittently to the
boil sump.
FIG. 3 is a graph relating the concentration of ethanol in the boil
sump liquid to time during an 8-day experiment wherein the volume
of the boil sump liquid was maintained essentially constant.
DETAILED DESCRIPTION OF THE INVENTION
The invention herein resides in the discovery that vapor degreasers
can be operated effectively and safely employing mixtures of
1,1,2-trichloro-1,2,2-trifluoroethane and greater than azeotropic
amounts (that is, greater than 4 weight percent) of ethanol
provided there is adherence to the aforesaid improved process
conditions.
Although it is not preferred, rinse sump liquids containing
concentrations of ethanol above the limit defined above can be
charged and flammability still can be minimized if the boil sump
liquid has a sufficiently low concentration of ethanol. Shortly
after start-up the concentration of ethanol increases in the boil
sump liquid and decreases in the rinse sump liquid, thus placing
both concentrations within the defined limits for the initial
concentrations of ethanol in the two liquids. Thereafter, the
concentration of ethanol in each sump liquid may or may not change
substantially during use depending on the manner in which the
invention process is carried out, but in any event, the
concentration of ethanol in the boil sump liquid remains higher
than the concentration of ethanol in the rinse sump. For this
reason and because it is only the boil sump liquid which is boiled,
it is the concentration of ethanol in the boil sump liquid which is
controlling as to the flammability of the vapors in the vapor
space.
The principal functions of the rinse sump, as already stated, are
to cool the articles (which are warmed by the boil sump liquid) so
that the vapors in the vapor space condense thereon in the next
step and to rinse the bulk of the relatively dirty boil sump liquid
from the articles. As to these functions, the ethanol concentration
in the rinse sump liquid is unimportant. Similar considerations
apply to condensate which may be diverted to a hold tank and
employed as a spray liquid. The invention criteria are mainly
directed to the maintenance of boil sump liquid compositions which
cannot produce flammable vapors in the vapor space; the
concentration of ethanol in the rinse sump liquid is allowed to
equilibrate or to approach equilibrium with the boil sump
liquid.
In the normal operation of a degreaser losses of liquid occur by
various routes. The best recognized are diffusion across the
vapor-air interface (which seems to be the principal route when the
degreaser is idling) and drag out (which is the liquid carried out
by the degreaser on the articles). In well designed degreasers,
when 1,1,2-trichloro-1,2,2-trifluoroethane liquids are employed,
these losses amount to about 0.2 lb./hr.-ft..sup.2 of vapor-air
interface while the degreaser is idling and about 0.5
lb./hr.-ft..sup.2 when the degreaser is working, that is, when
articles are being passed through the degreaser. Naturally, the
magnitude of the working losses vary according to the type of
article being treated. Losses from degreasers are reflected in a
lowering of the volume of the boil sump liquid. In processes
employing mixtures comprising 1,1,2-trichloro-1,2,2-trifluoroethane
and greater than 4 weight percent of ethanol, such losses cause the
concentration of ethanol to rise in the boil and rinse sump
liquids. It is usual in the operation of vapor degreasers employing
conventional liquids to add make-up liquid to one of the sumps to
compensate for losses. In carrying out the instant invention, two
criticalities must be observed. The first of these pertains to the
volume of the boil sump liquid, the other pertains to the maximum
permissible concentration of ethanol in the make-up liquid. In
order to avoid eventual flammability of the vapors in the vapor
space, it has been found that the concentration of ethanol in the
make-up liquid must not exceed about 10 weight percent. As it is
desired to maintain a sufficient concentration of ethanol in the
boil sump liquid to ensure adequate defluxing, this being the
principal utility of the invention, a concentration of ethanol of
not less than about 3 weight percent in the make-up liquid is
necessary.
It is preferred to maintain the volume of the boil sump liquid
essentially constant to minimize fluctuations in the concentration
of ethanol in the boil sump liquid. Although make-up liquids
containing any concentration of ethanol within the defined limits
can be used, it is preferred to employ ethanol concentrations given
by the equation
C.sub.m = 4.19 + 2.51 .times. 10.sup.-.sup.5 c.sub.b.sup.3
wherein
c.sub.m = the weight percent concentration of ethanol in the
make-up liquid and
c.sub.b = initial weight percent concentration of ethanol in the
boil sump liquid.
By employing this equation to determine the concentration of
ethanol in the make-up liquid, the concentration of ethanol in the
boil sump liquid is maintained more nearly constant.
In a nonpreferred embodiment, if the ethanol concentration which is
employed in the make-up liquid is greater than c.sub.m, but not
greater than 10 weight percent, then the value used for c.sub.b to
determine the volume of the boil sump liquid by the equation given
earlier above no longer is applicable, in which case a new value of
c.sub.b must be determined and the volume of boil sump liquid must
be recalculated.
Although it is possible to operate the process of this invention
with safety at concentrations of ethanol as high as 65 weight
percent in the boil sump liquid, it is preferred to employ a
concentration of about 35 weight percent of ethanol in this liquid.
Moreover, because of the higher cost of pure ethanol, it is
preferred to prepare the liquids required by this invention from
denatured ethanol. The denaturants commonly used are present in low
concentrations and do not affect the essential properties of
ethanol as they pertain to the invention. The preferred denatured
ethanol contains about 9 weight percent of methanol and this type
of ethanol has been employed in the following examples.
FIG. 1 shows a conventional prior art degreaser. An open-top
housing 1 encloses the components of the device. A boil sump 2
containing boil sump liquid 3 and rinse sump 4 containing rinse
sump liquid 5 are provided. Heating means 6, normally of the
electrical resistance type, is provided to effect boiling of boil
sump liquid 3. Vapors from boil sump liquid 3 fill vapor space 7
and are condensed on condenser 8. Condensate from condenser 8 is
collected in trough 9 and directed to rinse sump 4. Water separator
conduits (not shown) sometimes of substantial volume and intended
for the removal of co-condensed water, may be employed at the exit
end of trough 9. A vapor-air interface (not shown) is maintained by
condenser 8 in the region of condenser 8 between the vapors in the
vapor space and quiescent air layer 10. Overflow of rinse sump
liquid 5 from rinse sump 4 passes over weir 11 into boil sump
2.
In the following examples and in FIG. 2 reference is made to the
minimum safe volume of the boil sump liquid in terms of a
percentage of the initial volume of boil sump liquid. It is to be
understood that such a percentage, expressed as v.sub.%, is
calculated by the equation ##EQU2## wherein v.sub.m and v.sub.i are
as already defined. The prior equation for v.sub.m can thus be
written in terms of v.sub.% as
v.sub.% = (1.44 c.sub.b + 2.30 c.sub.r - 24.1) .+-. 2
wherein c.sub.b and c.sub.r are as already defined.
EXAMPLE 1
In this example make-up liquid was added intermittently instead of
continuously as is preferred. Between additions the volume of the
boil sump liquid decreased as a result of normal idling and working
losses. Simultaneously, the concentration of ethanol rose in the
boil sump liquid. Except for one instance, as explained below, the
vapors generated by the boil sump liquid remained nonflammable. The
process was carried out in a laboratory size degreaser having a
rinse sump volume of 5.4 liters; the sump was filled with a mixture
of 1,1,2-trichloro-1,2,2-trifluoroethane and 4 weight percent of
ethanol. The boil sump was charged with an equal volume of a
mixture of 1,1,2-trichloro-1,2,2-trifluoroethane and 35.2 weight
percent of ethanol. The boil sump liquid was boiled in the normal
manner for a total of about 58 hours (the running time) during 8
working days. The degreaser was covered during nonrunning hours.
Total loss rates of liquid of between 0.4 and 0.7 lb./hr.-ft..sup.2
were realized by passing the following articles through the sumps:
during the first 4.5 days of the running time paper towels were
used to simulate the treatment of absorbent articles; thereafter,
an endless chain was used to simulate the treatment of nonabsorbent
articles. The boil sump liquid was replenished four times during
the running time. The volume of the boil sump liquid and the
concentration of the ethanol therein passed through four and
one-half cycles. During the first cycle the volume of the boil sump
liquid was allowed to fall to 36.2 percent of the initial volume,
that is, within the range (35.8 .+-. 2 percent) calculated for
v.sub.% by the aforesaid equation. The vapors in the vapor space
were found at this point to be marginally flammable. It is to be
understood that the minimum volume of boil sump liquid v.sub.m
should not be allowed to decrease below the low end of the range
calculated from either of the aforesaid equations for v.sub.m and
v.sub.%. When the minimum volume is allowed to decrease to within
said range, the vapors may or may not be flammable. It is to be
further understood that the range recited in either equation is
required primarily because of the mathematical difficulties
encountered in characterizing the system with such simplified
equations, or in other words, in order to avoid recitation of a
range a much more detailed and sophisticated equation would have to
be derived.
Addition of make-up liquid consisting of
1,1,2-trichloro-1,2,2-trifluoroethane and 4 weight percent of
ethanol restored the vapors in the vapor space to a nonflammable
condition. During the remainder of the running time, wherein all
criteria of the invention were met, the vapors in the vapor space
were maintained in a nonflammable condition by maintenance of the
boil sump liquid volume at a value greater than 35.8 .+-. 2 percent
of the initial volume by addition of the aforesaid make-up liquid.
From the original concentration of 4 weight percent the
concentration of ethanol in the rinse sump (determined by density)
increased with decreasing boil sump liquid volume during the first
cycle to about 12.7 weight percent; on addition of make-up liquid
it decreased to about 6 weight percent. Thereafter, the
concentration fluctuated, with variation in the boil sump liquid
volume, between about 6.0 weight percent and about 9.9 weight
percent. FIG. 2 shows graphically the relationship of boil sump
liquid volume (as percent of initial volume) to running time.
Dashed lines represent additions of make-up liquid. The slope of
the lines during each cycle is proportional to the rate of liquid
loss.
EXAMPLE 2
This example demonstrates the operation of a degreaser containing a
boil sump liquid having an initial concentration of ethanol at the
maximum permissible level. The experiment was carried out as in
Example 1 except that the initial charge to the boil sump consisted
of a mixture of 1,1,2-trichloro-1,2,2-trifluoroethane and 65 weight
percent of ethanol and the initial charge to the rinse sump
consisted of a mixture of 1,1,2-trichloro-1,2,2-trifluoroethane and
12.1 weight percent of ethanol. Because of the high concentration
of ethanol there is much less latitude in the regulation of the
volume of the boil sump liquid. In other words, from the equations
previously given, it can be calculated that the boil sump liquid
volume must be maintained at at least 97.3 .+-. 2 percent of the
initial volume. For this reason the volume of the boil sump liquid
was maintained essentially constant by means of a feeder device
which operated on demand to add (to the boil sump) make-up liquid
consisting of 1,1,2-trichloro-1,2,2-trifluoroethane and 11 weight
percent of ethanol. During 29 hours running time, carried out over
4 working days, the volume of the boil sump liquid was maintained
by the regulating device, according to measurement of the depth of
the liquid, at between 96.3 and 103.7 percent of the initial
volume. There was a brief increase to 111.1 percent on the first
day due to malfunction of the regulator and a brief decrease to
92.6 percent on the third day. Paper towels, simulating the
treatment of absorbent materials, were passed through the sumps at
a daily liquid loss rate of about 0.30 to 0.46 lb./hr.-ft..sup.2.
The vapors in the vapor space were found to be nonflammable on the
second day when the measured volume of the boil sump liquid was
96.3 percent of the initial volume; a burning match, when thrust
into the vapor space, was extinguished. The boil sump liquid was
shown to be nonflammable at the end of the test.
EXAMPLE 3
This example demonstrates a preferred embodiment of the process
wherein the following parameters were selected:
1. the initial concentration of ethanol in the boil sump liquid was
35 weight percent;
2. the initial concentration of ethanol in the rinse sump liquid
and in the make-up liquid was 4 weight percent; and
3. the volume of the boil sump liquid was maintained essentially
constant by continuous (rather than intermittent as in Example 1)
addition of make-up liquid.
The mixture of 1,1,2-trichloro-1,2,2-trifluoroethane and 4 weight
percent of ethanol is preferred as initial rinse sump liquid and
make-up liquid for reasons of convenience since it represents a
known azeotrope. The preferred ethanol concentration for the
make-up liquid is 76.1 percent of the permissible concentration
calculated from the equation given above for c.sub.m. Surprisingly,
the concentration of ethanol in the boil sump liquid remained
remarkably constant for an extended period equal to or greater than
the usual useful life of the liquids. FIG. 3 shows the
concentration of ethanol in the boil sump liquid as a function of
time. Also shown is the cumulative, added make-up liquid (in terms
of volume percent) as a function of the boil sump liquid
volume.
More specific to the above, in this example the degreaser was
charged with boil and rinse sump liquids as already described. The
boil sump liquid was boiled in the normal manner for about 61 hours
over a period of 8 working days. The degreaser was covered during
nonworking hours. An endless chain was passed through the sumps and
to the outside of the degreaser for a sufficient fraction of the
running time each day to effect losses of 0.63 to 0.70
lb./hr.-ft..sup.2, losses which are at least as high as is normal
in industrial practice. On the sixth day 74 grams of activated
rosin flux, such as is used in the soldering of circuit boards,
were added to the boil sump liquid. From time to time samples were
taken from the sumps and assayed for ethanol by hydrometer density
measurement at standard temperature. It was established that the
presence of flux does not affect the accuracy of the assay within
the precision herein reported. The concentration of ethanol in the
boil sump liquid as a function of time is shown graphically in FIG.
3. Extrapolation of the results of the figure suggests that the
concentration of ethanol in the boil sump liquid would remain
within the 30 to 35 weight percent range indefinitely. The vapors
of the vapor space were never flammable during the 8 days of the
experiment. After equilibrium, which occurred in the first two
hours of running time, the concentration of ethanol in the rinse
sump liquid remained between 6.2 and 7.2 weight percent.
EXAMPLE 4
This example demonstrates a preferred embodiment carried out in a
commercial size degreaser. The degreaser was of the 2-sump type
such as shown in FIG. 1 and included an external condensate system
not shown in that figure. The rinse sump in horizontal dimensions
was 30 inches square and 16 inches deep. The boil sump had the same
horizontal dimensions. The boil sump was provided with two
float-actuated switches. The first of these operated to open a
solenoid valve to admit make-up liquid to the rinse sump from a
reservoir as required to maintain the volume of the boil sump
liquid essentially constant. The second float-actuated switch was
adjusted, as a safety measure, to shut off the electrical heating
of the sump if the volume of the boil sump liquid decreased to a
predetermined level (below the volume prescribed by either of the
aforesaid equations). Since the volume of the boil sump liquid was
maintained essentially constant during the course of this
experiment, the second switch was never actuated. The rinse sump
and the external condensate system were charged with a mixture of
1,1,2-trichloro-1,2,2-trifluoroethane and 4 weight percent of
ethanol. The rinse sump required 81.8 gallons; the external
condensate system, 10 gallons. The boil sump was charged to a
liquid depth of 16 inches with 62.3 gallons of a mixture of
1,1,2-trichloro-1,2,2-trifluoroethane and 35 weight percent of
ethanol. The make-up liquid reservoir serving the boil sump was
charged with the 1,1,2-trichloro-1,2,2-trifluoroethane/ethanol
azeotrope. The boil sump liquid was boiled for 63.5 hours over a
period of 10 days. The degreaser stood idle on the sixth day.
During the course of the experiment, 17 circuit boards were
defluxed. The boards were prepared, as is customary in the trade,
by coating the circuit side of cleaned boards having wired
connections with flux and passing that side of the boards for 5
.+-. 0.2 seconds over the wiped surface of molten 50:50 Pb:Sn
solder held at 464.degree.F. Of the 17 boards of the experiment, 13
were coated with highly activated flux and four were coated with
mildly activated flux. Three modes of defluxing were employed. All
boards were submerged in the boil sump liquid for 4 minutes. One
board coated with highly activated flux was not further liquid
rinsed. All other boards were submerged for 15 seconds in the rinse
sump liquid. All but one board (coated with highly activated flux)
were thereafter sprayed for 15 seconds with condensate in the vapor
space. All boards were held 15 seconds in the vapor space. All
boards regardless of the defluxing treatment were completely clean.
No trace of white residue was visible. The overall liquid loss rate
was 0.40 lb./hr.-ft..sup.2. During the entire period of the
experiment the concentration of ethanol in the boil sump liquid was
between 36.0 and 33.5 weight percent. The vapors in the vapor space
were nonflammable.
* * * * *