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Nov. 19, 1946.
'
F. c. MITCHELL ET'AL
2,411,453v
APPARATUS FOR MAKING ALKYL LEAD COMPOUNDS '
'
Filed July 23, 1942
2 Sheets—She|et 1
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'
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ATTDRNEY
Nov. 19, 1946.
F. c. MITCHELL z-rrm.
2,411,453 _
APPARATUS FOR MAKING ALKYL LEAD COMPOUNDS
Filed July 23', 1942
I
2 Sheets-Sheet 2
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JOJEBII L. 6720951?
BY
Patented Nov. 19, 1946
2,411,453 .
UNITED
Tea PAT-s;
FFICE
2,411,453
APPARATUS FOR
G ALKYL LEAD
COMPOUNDS
Frederick Charlton Mitchell, Wilmington, DeL,
James Cuthbert Lawrence, Moylan, Pa., and
\ Joseph Ludwig Stecher, WllmingtomDeL, as
signors to E. I. du Pont de Nemours & Com
pany, Wilmington, bet, a corporation of Dela
ware
Application July 23, 1942, Serlai No. 452,106
9 Us. (Cl. 23-260)
- 1
This invention relates to a process and appa
ratus for making alkyl lead compounds and for
carrying out similar chemical processes whereby
such processes may be carriedout more rapidly
and successfully than has been possible hereto
fore.
'
'
.
2
V
iced tank so as to reduce the pressures,v to some
extent.
>
,
.
With the process and apparatus of Patent‘
2,091,112, the rate of addition of the ethyl chloride
to the autoclave was strictly limited. The neces-‘
sary tube restrictions in the condenser cause a
In the commercial production of tetra ethyl
pressure drop across the condenser, decreasing _
lead, lead-mono-sodium alloy is placed in an
the available head for feeding the ethyl chloride.
autoclave and ethyl chloride is added to it as
When the ethyl chloride feed valve was progres
rapidly as possible while still maintaining control
sively opened, more vaporization occurred, the
over the reaction. As is well-known in the art.
pressure drop throughthecondenser increased
the reaction is exothermic and large quantities
and only a low feed rate of ethyl chloride was
of heat must be removed to prevent development
obtained. When the tank was vented to remove
of excess temperatures andpressures, which may
accumulated noncondensibles, the feeding head
cause rupture of the equipment with explosive M on the ethyl chloride was further reduced. Also,
violence. One of the most emcient means oi heat
unless large and uneconomical feed tanks were
‘removal .has involved the use'oi a condenser to
employed, the permanent gases in the system
condense the vaporized ethyl chloride and the
upset the ethylchloridepressure-temperature re
return of the condensate'to the source of supply
lationships. Furthermore, when the reaction
of the ethyl chloride. Prior to the present inven
slowed down, there was a de?nite tendency for the
tion, tetra ethyl lead was produced commercially
condenser to become vapor locked because the
by the method of U. S. Patent No. 2,091,112,
velocity of the gases through the condenser was
issued to Amick, ~I-‘armelee and Stecher. In ac
insumcient to sweep out the non-condensibles.
cordance with such process, vaporized ethyl
Another objectionable feature of the process 01'
chloride was condensed in a condenser and the
material from the condenser was led into the ethyl
chloride storage tank and the condensed ethyl
chloride fed back into the autoclave along with
the fresh ethyl chloride at a controlled rate.
Patent 2,091,112 was that, as the feed valve was
opened to a large extent, increased vaporization
and condensation of ethyl chloride occurred,
more condensate was returned to the feed tank
and the net disappearance of ethyl chloride from
‘ While the process of Patent 2,091,112 has been 30 the feed tank remained substantially constant and
very satisfactory in practice, it had certain fea
was not increased by further opening of the feed
tures which de?nitely limited the time required
. valve.
for completing the process and presented prob
The use of tetra ethyl lead. has greatly increased
lems in successfully carrying out the process.
requiring increased production. For the reasons
These problems are due to the fact that, in the 35. outlined hereinbefore, no further economically.
course of the reaction between ethyl chloride
feasible reductions in time and increaseiri pro
, and lead sodium alloy, some ethane, ethylene and
‘ duction could be made by employing the process
butane are formed. Both ‘ethane and ethylene
and apparatus of Patent 2,091,112. Applicants
are non-condenslble at the temperatures and
have discovered a new process and apparatus
pressures of the reaction and, unless some provi- 40 whereby the manufacture of tetra ethyl lead can
sion is made for their control, they tend to vapor
be carried out more successfully in a much shorter
lock the condenser, cause unduly high pressures
period of time, thereby materially increasing pro
and upset the pressure-temperature relationships
of the ethyl chloride. In the process and appa
ratus of Patent 2,091,112, provision was made to
control the effect of the non-c‘ondensible~ gases
to some extent. In this patent, the condenser
tubes were restricted to such a degree that the
velocity of the gases would be su?lcient to carry
ductlon. Applicants’ new process and apparatus
overcomes the objections and problems inherent
in ‘the process and apparatus of Patent2,991,112.
An object of the present invention is to provide
a method and apparatus for manufacturing alkyl
lead compounds and particularly tetra ethyl lead
more economically than has heretofore been pos
the non-condensibles through the condenser and 50 sible by decreasing the manufacturing time cycle.
into the‘ ethyl chloride feed tank. The ethyl
Another object is to provide a method and‘ appa
chloride feed tank was made overlarge so as‘ to
hold these gases without obtaining a large rise
ratus which will permit a more rapid additionvoi
ethyl chloride and the‘ like to lead¢sodium alloy
in pressure. Provision was also made to vent
while still maintaining adequate control over the
' the hydrocarbon gases from the ethyl chloride 55 reaction. A further object is to provide a method
2,411,403
and apparatus for accurate automatic, control of
the reaction and the pressures obtained therein
by venting non-condensibles from the autoclave
equipment automatically‘ in conjunction with
automatic ‘control of the flow of cooling media to
the condenser and the autoclave. A still further
object is to provide a process and apparatus which
will allow maximum removal of heat from the
4
for the reaction are obtained. The temperature
and pressure tend to rise still further, but, when
the optimum conditions are obtained, the ?ow‘ of
cooling ?uid in the jacket of the autoclave and
-in the condenser is started and increased to '
prevent the temperature and pressure from ris- '
ing materially above the optimum temperature '
and ' pressure.
When cooling ?uid > is passed
through the condenser the ethyl chloride there
reaction by the use of full ?ow of cooling media to
the condenser and the autoclave, as it is needed, 10 in is condensed and the rest'of the ethyl chloride,
as it is vaporized, passes upwardly through con
and maintaining all of the surface of the con
‘duit 20 and cone 24 into the condenser 22. The
denser available for condensation and preventing
condensed ethyl chloride ?ows into the cone 24
vapor lock. Other objects are to advance the
where a body of liquid ethyl chloride accumulates
art. Still other objects will appear hereinafter.
The above and other objects may be accom 15 causing the cone to act as a liquid gas separator.
The , condensate further ?ows downwardly
plished in accordance with our invention, which
through conduit 26 to the autoclave where it ab
will be explained in detail hereinafter, reference
sorbs heat from the reaction due to its di?erence
being made to the accompanying _ drawings
in temperature and due to at least partial re
wherein_
Fig. 1 is a somewhat diagrammatic drawing of 20 evaporation. The ?ow of ethyl chloride from
the tank I 4 into the‘autoclave is regulated so that
one type of apparatus which is suitable for car
it is_ at the maximum rate which will maintain
rying out our invention;
the temperature and pressure at the maximum
Fig. 2 is a representation, with parts broken
‘ away for clearness of illustration, of a preferred.
while employing the maximum cooling in the
form of apparatus for carrying out our process. 25 condenser and autoclave which can be obtained
Referring'nrst to Fig. l, the apparatus com
prises a conventional liquid cooled jacketed au
toclave l0, provided’ with the usual charging pipe
l2 for the lead-sodium alloy and which is her
with the particular equipment.
When the trap or liquid seal 28 is provided,
be supported on a scale [,as is usual.
smoother ?ow of condensate from the condenser
and ‘the cone 24 is rendered more efficient as a
the condensed ethyl chloride flows into the trap
to provide the desired liquid seal preventing va
pors
from ?owing upwardly through the conduit
metically closed by a suitable valve or cap not 30
26 to the cone 24. Thereby there is provided a
shown. The ethyl chloride storage tank i4-rnay
Ethyl chlo
ride is fed to the autoclave from the tank i4
through pipe l6 controlled by valve [8. Conduit
liquid-gas ‘separator. The condenser is placed
20 is provided for conducting vapors from the 85 at a sufficient height above the autoclave and'the
trap to allow for a head of liquid between the
cone 24 and the autoclave greater than the pres
sure di?erential between these points caused by
the pressure drop in the condenser. The dis-‘
and the condensate passes from the condenser
autoclave to the condenser 22 through a cone 24
positioned at the bottom of the condenser. In
this case, the condenser 22 is of the re?ux type
duit 2B is provided a trap or other type of liquid ’
tance between the cone 24 and the trap 28 must
also be su?lcient to provide a head of liquid great
enough to cause the condensate to ?ow through
sealing means<28 which will permit downward
the- trap.
into the cone 2t and then through the return
conduit 26 directly to the autoclave. In the con
.
As the process proceeds, non-condensible gases
?ow of condensate, but will greatly restrict or
prevent the flow of vapors. upwardly through 45 accumulate in the top of the condenser and they
_ would ordinarily upset the desired pressure-tem
conduit 26 from the autoclave to the condenser.
perature relationships. As the non-condensibles
The trap or liquid seal 28 is not absolutely essen-‘
accumulate to an'undesirable and objectionable
tial to the successful operation of the apparatus
extent, they are vented off through vent pipe 30.
or process, but is generally desirable in order to
obtain smoother and. more rapid operation of 50 This permits maintenance of the desired pres-'
sure-temperature relationships and overcomes
the process.
‘
one of the main objectionable features of Patent
A vent pipe 3!! controlled by valve 32 is provided 7
2,091,112. Also, by venting the non-condensibles
at the top of the condenser for the controlled
from the top of the condenser in this manner, the
venting of non-condensible gases. The con
- venting of large amounts of vethyl chloride with
denser is also provided with the usual inlet pipe
the non-condensibles, as was obtained in the
34 and outlet pipe 36 for circulation of cooling
media.
~
,
The autoclave is also provided with a vent pipe
38 controlled by valve lit for the release of pres
process and apparatus of Patent 2,091,112, is
avoided.
-
-
By this arrangement and process, more effi
sure and removal of excess ethyl chloride when 60 cient control of the temperature and pressure in
the autoclave is readily maintained. Also, larger
the reaction is completed. A pressure equalizing
amounts of ethyl chloride are introduced into the
line 42 controlled by valve 44 is shown between
autoclave over a unit period of time and from
the vent pipe and ethyl chloride storage tank.
two sources, the ethyl chloride storage tank and
If desired, this equalizing line may lead of! from
the autoclave or the charging pipe l2 if desired. 65 ‘the ' .condenser. Thus, the manufacturing time ‘
cycle is very materially reduced and/ the reaction
In the operation of the process, employing the
is carried out more smoothly and successfully
apparatus of Fig. 1, the lead-sodium alloy is
whereby greatly increased production is obtained.
charged into the autoclave and the ethyl chloride
Fig. 2 discloses an apparatus which is‘similar
is placed in the tank i4 and the system is closed.
The ethyl chloride is fed from ‘the tank I4 into 70 in structure and operates on substantially the
same ‘principles as that ‘of Fig. 1, but which is
the autoclave at a predetermined gradual rate.
slightly different in certain details and illustrates
As the reaction starts, large amounts of heat are
a preferred form of the invention. In Fig. 2, generated and part of the ethyl chloride is vapor
the numeral iii designates the jacketed autoclave
ized. The temperature and pressure are per
mitted to build-up until the optimum conditions 75 provided with the charging-pipe I2 closed by ;‘
‘9.411.455
valve n. In this modiil ‘tion or the apparatus. . sure of the ethyl chloride at the temperature or
the ethyl chloride feed line it, leading from the‘
the reaction As the pressure and temperature
ethyl chloride storage tank i4 and controlled by
approaches that temperature and pressure'which
valve l8 leads directly into the autoclave rather
. has been determined to be the optimum for the
than into the charging pipe l2. The'scale sup‘
porting-the ethyl chloride storage tank is indi
cated at 16. The ethyl chloride vapor line 20
leads into the top 01 the condenser 22, which is
structurally similar to the condenser disclosed
.reaction, usually from about 65,‘ C. to about 75° .
C. and from about 50 to about 65 pounds per.
square inch gauge pressure, the. controller “will .
operate valves ill and ill to cause cooling media
to ?ow through the autoclave jacket and, the
in Patent 2,091,112. The return pipe 28 for re 10 condenser, respectively. Usually, ‘the controller
turning the condensed ethyl chloride to the auto
will be caused to start opening the valves ‘I and
clave is provided with a U-bend 28 which serves
80 when the pressure in the system reaches about
the same purpose as the trap 28 in the apparatus
45 to about 60 pounds per square inch.
illustrated in Fig. 1.
‘By the time that the controller 83 starts to
In the modification illustrated in Fig. 2, the 15 open the valves 60 and 40, the autoclave, con
liquid-gas separator is separated from the con
denser, liquid-gas separator and connecting pipes
denser and is in the form of a cyclone separator .
are ?lled with the vapors of ethyl chloride. The
ethyl chloride in-the condenser is now condensed
and’ the condensate ?ows through ,the return
ior 24 so as to direct the gases ?owing through 20 conduit 26, ?lls'the U-bend or trap 28\and ?nally
into
the
liquid-gas
separator
in
a
tangential
t
?ows back to the autoclave. Condensation of the
24., The conduit 21 leads oil‘ from the return
conduit 26 and leads into the liquid-gas separa
direction. The vent pipe 30, controlled by‘the
valve 32, leads oil from the top of the liquid-gas
separator.
_
ethyl chloride in the condenser causes a de
creased pressure in the condenser drawing more
vapors through the vapor line 20 from the auto
clave. The U-bend or trap 28 provides a liquid
seal which prevents return of the vapors through
this section, but permits free ?ow oi’ the con
densed ethyl chloride to the autoclave. The non
condensible gases pass into the liquid-gas separa
In the modi?cation shown in Fig. 2, the inlet
pipe 34 for the cooling media for the condenser
enters at the bottom and the outlet pipe 36 leads
‘of! from the top of the condenser. Also, the
equalizing line 42 connects the ethyl chloride
storage tank with the ethyl chloride vapor line 30 tor 25 mainly through the pipe 21 and, since they
20 instead of a separate vent pipe. Furthermore,
enter the cylindrical liquid-gas separator 241 in
there is shown in Fig. 2, the inlet pipe 46 and the
a tangential direction, any entrained ethyl chlo
outlet pipe 48 for the cooling media employed
ride is separated fromthe non-condensibie gases
in the jacket of the autoclave. ,Still further, a
by centrifugal action. The separated ethyl chlo
motor 52 is shown for operating the usual agi
ride then ?ows downwardly into the_ conduit 26,
tator, not shown, in the autoclave.
>
trap 28 and autoclave iii. The condenser and the
In the feed line 46, there is provided an air
liquid-gas separator are placed above the auto
operated diaphragm valve 50, together with a by
clave at a sumcient height to provide a head of,
pass line 54 and conventional auxiliary hand
,liquid between the separator and the autoclave
operated valves. Also, the valve 32 is an air op 4.0 greater than the pressure differential between
erated diaphragm'vaive and has associated with
these points caused by the pressure drop through
it the conventional by-pass 58 and auxiliary
the condenser.
hand-operateduvalves. Similarly, the inlet pipe
As more ethyl chloride is added to the auto
34 for the condenser is also provided with an air
clave and the reaction progresses, the pressure
operated diaphragm valve 60, by-pass 'line 58 and 45 and temperature in the system continues to rise.
auxiliary hand-operated valves. Line 62 is the
With such rise in pressure, the controller 86
air supply line for operating these diaphragm
causes the valves 50 and B0 to be opened further
valves. Valve 32 is operated through the pres
and ?nally, when the pressure which is most con
sure actuated controller 64 and'line 68. Con
ducive to the production of high yields of tetra .
troller at is responsive to the pressures in the top 50 ethyl lead is obtained, full ?ow of the cooling
of the condenser and is suitably connected there
media to the condenser and the autoclave jacket
to byline ‘it. The valves 50 and to are operated
is obtained. During this time, the feed of ethyl
through line ‘i2 ‘connected with the pressure actu
chloride from the tank id to the autoclave is,.reg
ated controller ‘6t. Controller 66 is also con
ulated through valve is to cause the pressure and
nected to the top of the condenser through line 55 temperature to rise rapidly. to the desired opti
14 and is responsive to the pressures‘ in the con-.
mum.
denser.‘
‘
Control of the operation, as has been just de
The process, as applied for instance to th
scribed, would be sumcient were it ‘not for the
preparation of tetra ethyl‘lead by the present
tact that considerable quantities of non-con
improved method and employing the apparatus 60 densible gases are formed as the result of, side
Just described and illustrated in Fig. 2, may be
reactions. It is essential that these gases be
illustrated as follows:
'
properly vented from the system without, at the
A weighted amount of lead-mono-sodium alloy
same time, venting large quantities of ethyl chlo
is introduced into the autoclave Iii‘ through the
ride and without upsetting the pressure-temper
autoclave feed chute 12', the valve it is closed
ature relationships desired. For‘ this purpose, the
and the autoclave agitator motor 52 is started.
controller 64 is set to open valve 32 at pressures
The ethyl chloride scale tank it, having been
slightly above that at which controller 66 fully
?lled previously with the required amount or
opens valves 50 and 60. In other words, after
ethyl chloride, the valve is is opened and the
the optimum conditions of temperature and pres;
70
ethyl chloride is allowed to flow into the auto-_
sure have been obtained and the valves 59 and
clave continuously at a controlled rate, the
G0 are fully opened so that the process is being
amount being read from the scale dial ‘it. As
operated at maximum speed, the pressure tends to
the reaction between the ethyl chloride and the
rise, without corresponding increase in tempera
alloy begins, heat is evolved and the pressure
ture, due to the non-condensible gases in the sys
of the system begins to rise due to the vapor pres-Y 75 tem. when. the pressure rises slightly above
1 2,411,453:
.
such'optimum conditions, the controller .64 starts
in the usual manner to recoverthe tetraethyl '
to operate valve 32 tovent non-condensible. gases ‘
lead','..
inch above the optimum pressure. The optimum
pressure will usually be, at from about 60 to about
75 pounds per square inch. Generally, the pres
Maximum‘use of the condenser and the'autoclave
jacket, as the means of heat removal, is accom
plished by allowing full flow of cooling media to
sures in the system should not be permitted to rise
'
.‘.
maximumiuse of» the means of heat removal and;
therefore',*allows for the most rapid feed rate of
ethyl chloride possible with any given equipment.
troller M will start-;,to open the valve 32 at pres
sures from about 1"‘to about 5 pounds per square
above 80 pounds per square inch.
V.
vIt wlll'be'seen that our invention provides for
from the liquid-gas separator. Usually, the con
10 these points as soon as a pressure rise- indicates
The pressure, at which the vent valve 32 is
opened, is important. If the- valve is opened at
too low pressures, considerable quantities of ethyl
a corresponding temperature rise, and by main
cumstances, the vented gases are low in ethyl
with no increase in operating labor or super
vision. The higher rate of addition of the ethyl.
taining the condenser free of non-condensible
gases, thus insuring that all condenser surface
is available for heat removal, and that‘no vapor
chloride will be removed along with the non-con
_densible gases, the yield of tetraethyl lead will 15 locking occurs. Full ?ow of cooling media to
the condenser and autoclave jacket is retained
be lower and full bene?t of cooling means will
even whileventing non-condensible gasesfrom
not'be obtained. Ii‘, on the other hand, the vent
the system, because the controller is so arranged
- ingpressure' is too high, the non-condensible
that venting shall occur only when full flow of
gases will build-up in the condenser tending to '
cause it to vapor lock and the reaction may get 20 cooling media to these points is in eiiect.
' Our invention has several important advan
out of control because of decreased cooling. Also,
tages over the system of Patent 2,091,112 which .
the liquid-gas separator is small relative to the‘
has been employed previously. By the use of our
ethyl chloride feed tank of Patent 2,091,112. It
invention, we can add the ethyl chloride to the
should be as small as possible while still being
of asize such as will conveniently handle the 25 lead-sodium alloy at a rate of 2.5 times that
quantity of gases passing therethrough; Due to ‘which has been possible heretofore. Thus, the
use of our invention in commercial operations
this structure, the non-condensible gases in the
has permitted‘ the addition of the ethyl chlo
liquid-gas separators are in contact with only
ride to be completed in less than half the time
a small body of ethyl chloride which is substan
tially saturated with the gases. Under these cir at required with greatly increased production and.
chloride and minimum losses of ethyl chloride
chloride appears to favor the formation of tetra
ethyl lead with fewer side reactions. In addi
' tion, the automatic venting and cooling arrange
iscontrolled so that the ethyl chloride is added
ment provides the most economical and eiiicient
as rapidly as is possible and as the particular
heat removal. With the. total elimination of
equipment employed will permit. The maximum
rate is easily determined experimentally and a‘ . vapor lock in the condenser, full condenser sur
face is at all times available for cooling and full
standard set up. - Also, observation of the amount .
of venting can serve as a criterion for control of 40 ?ow of the'cooling media to the condenser and
the autoclave jacket is obtained whenever high
‘the feed. Knowing the quantity of non-con
in the vented gases-are thus assured.
' The feed of the ethyl chloride to the autoclave
pressures indicate high temperatures and the
need for rapid. heat removal. Only through
densible gases usually generated in the system,
more than'norm'al rate of vent indicates the re
maximum condenser ei?ciency' can the most
moval of excessive quantities of ethyl chloride.
This, in turn. shows that the condenser is unable 45 rapid addition of ethyl chloride be obtained, and
our invention insures that such ef?ciency will be
to condense all of the ethyl chloride vaporized
realized. These effects are obtained by venting
and the feed rate must be lower. Conversely, a
the non-condensible gases from the system at a
low rate of vent indicates that more rapid addition
point in the system where such venting will not
of ethyl chloride is desirable. The temperature
' pressure relationshipis also a criterion for con 60 affect the rate of feed of the ethyl chloride to
trolling the rate of feed of ethyl chloride. When > the autoclave. Also, by returning‘the condensed
ethy1 chloride directly, to the autoclave instead
the temperatures obtained are higher than the op
of the ethyl chloride feed tank, a greater amount
timum for the desired pressure, the feed of‘ ethyl
I ‘chloride should be decreased.
of ethyl chloride is fed into the autoclave in a
Conversely, low
temperatures indicate the desirability of more 55 unit of time, thereby obtaining greatly increasedv
cooling and feed of ethyl chloride.
rapid addition of the ethyl chloride. The rate
Although we have described our invention
of addition of the ethyl chloride should be such
with‘ particular reference to the manufacture‘ of
as to raise the temperatures and pressures up to
tetraethyl lead, it will be understood that such
the optimum as rapidly as possible. If the pres
sures tend to rise as high as 80 pounds per square 60 description, is for illustrative purposes only. Our
invention has been successfully employed in the
inch or above, the rate of feed of the ethyl chlo
preparation of other alkyl lead compounds, and
ride should be decreased.’ While the valve IB,.
particularly ‘in the manufacture of mixed tetra
for controlling the feed of ethyl chloride, is shown
methyl-ethyl lead compounds, prepared by the
as hand operated, it may be automatically con
trolled by'the temperatures or pressures in the 65 action of a-mixture of methyl chloride and'ethyl
system in accordance with the principles herein , '
chloride on lead mono-sodium alloy.
set forth.
vention is particularly useful in the prepara- .~
.
,
When the addition‘of ethyl, chloride is com
plete, the pressure of .the system will fall off
rather rapidly. When the pressure has decreased
to approximately 50. pounds per square inch, the
?ow'ofthe cooling media will be stopped and the
reaction permitted to go to_ completion. When
w
Our in- .
tion of tetraalkyl lead compounds in which each
alkyl group contains from 1 to 4 carbon atoms.
Our invention is also applicable to the prepara
tion of corresponding alkyl compounds of other
metals such as tin and the like.
Also, while we
have indicated particular conditions of tem
perature, pressure and the like, it will be
the reaction is completed, the excess ethyl chlo
- ride is removed and the reaction mass is treated 75 understood that such conditions may be varied
9,411,458
without departing from our invention. The par
ticular conditions‘ are those which have been
found to be most desirable with the particular
equipment employed in one particular case. It
will be understood that the equipment may be
I modi?ed in various ways and as it is so modi
?ed and as more or less emcient cooling means
are employed, the particular conditions employed
will necessarily vary.
‘
I
We claim:
1. An apparatus, adapted for preparing alkyl
lead compounds from alkyl halides and lead
sodium alloys, which comprises a reaction vessel,
'
l0
-
the reaction vessel, a conduit connecting the
reaction vessel to the condenser for conveying
gaseous products to the condenser, a liquid con
densate return conduit connecting the condenser
to the reaction vessel independently of the alkyl
halide storage tank for conducting condensed
alkyl halide to the reaction vessel without pass
ing it through the storage tank, a liquid-gas sep
arator connected to the return conduit below the
10 condenser so that liquid condensate lily-passes
vthe separator‘ and uncondensed gases pass into
the separator to be separated from entrained
condensate, a controllable gas vent connected to
an alkyl halide storage tank, means for con
the liquid-gas separator for controlled venting
tinuously feeding alkyl halide from the storage 15 of separated non-condensible gases only irom the
tank to the reaction vessel, a condenser above
liquid-gas separator, and a liquid seal in the
the reaction vessel, a conduit connecting the re
> return conduit below the condenser and liquid
action vessel to the condenser for conveying
gas separator preventing gaseous products from
gaseous products to the condenser, a liquid con
?owing upwardly through the conduit while per-'
densate return conduit connecting the condenser 20 mitting liquid condensate to pass to the reaction
to the reaction vessel independently of the alkyl
vessel, the condenser and the liquid-gas separa
halide storage tank for conducting condensed
tor being placed above the liquid seat a sure ‘
alkyl halide to the reaction vessel without'pass
?cient distance to provide a head of liquid con
ing it through the storage tank, a liquid-gas
derisate ,su?lcient to start a pressure greater than
separator associated with the condenser for sepa 25 the pressure drop through the condenser so as to
rating non-condensible gases from the liquid
cause the liquid condensate to ?ow through the
condensate, and a controllable gas vent asso
liquid seal and into the reaction vessel.
ciated with the liquid-gas separator for con
4. An apparatus, adapted for preparing alkyl
trolled venting of separated non-condenslble
lead compounds from alkyl halides and lead so
gases only from the apparatus and sealing means 30 dium alloys, which comprises a reaction vessel,
associated with the return conduit below the
an alkyl halide storage tank, means for con
condenser preventing gaseous products from
tinuously'feeding alkyl halide from the storage
flowing upwardly through the conduit while per
tank to the reaction vessel, a condenser above
mitting liquid condensate to pass to the reaction
the reaction vessel, a conduit connecting the re-,
action vessel to the condenser for conveying gase
2. An apparatus, adapted for preparing alkyl
ous products to the condenser, a liquid condensate
lead compounds for ‘alkyl halides and lead
return conduit connecting the condenser to the
‘ sodium alloys, which comprises ‘a reaction vessel,
reaction vessel independently of the alkyl halide
an alkyl halide storage tank, means for con
storage tank for conducting condensed alkyl
tinuously feeding allwl halide from the storage 40 halide to the reaction vessel without passing it
tank to the reaction vessel, a condenser above
through the storage tank, a liquid-gas separa
the reaction vessel, a conduit connecting the
tor connected ‘to the return conduit below the
reaction vessel to the condenser for conveying
condenser so that liq'uid condensate by-passes
gaseous products to the condenser, a liquid con
the separator and uncondensed gases pass into
densate return conduit connecting the condenser 45 the separator to be separated from entrained
to the reaction'vessel independently of the allwl
condensate, a controllable gas vent connected to
halide storage tank for conducting condensed
the liquid-gas separator for controlled venting of
alkyl halide to the reaction vessel without pass
separated non-condensible gases only from the
ing it through the storage tank, a liquid-gas
liquid-gas separator, and a U-bend in the return
separator connected to the return conduit 50 conduit below the condenser and liquid-gas sep-=
below the condenser so that liquid condensate
arator to provide a liquid seal preventing gaseous
by-passes the" separator and uncondensed gases
products from ?owing upwardly through the con
pass into the separator to be separated from en
duit while permitting liquid condensate to pass
trained condensate, and a controllable gas vent
to the reaction vessel, the condenser and the
associated‘with the liquid-gas separator for con 55 liquid-gas separator being placed above the liquid
trolled venting of separated non-condensible
seal a su?icient distance to provide a head of liq
gases only from the apparatus, and sealing means
uid condensate sufficient to exert a pressure
associated with the return conduit below the
greater than the pressure drop through the con
vessel.
.
.
-
condenser and liquid-gas separator preventing
denser so as to cause the liquid condensate to
gaseous products from ?owing upwardly through 60 ?ow through the liquid seal and into the reaction
the conduit while permitting liquid condensate
vessel.
> to pass to the reaction vessel, the condenser and
'
'
5. An apparatus, adapted for preparing alkyl
the liquid-gas separator being placed above the
lead compounds from alkyl halides and lead
sealing means a su?cient distance’ to provide a
sodium alloys, which comprises a jacketed reac
head. of liquid condensate'sumcient to exert a 05 tion vessel, means circulating a cooling ?uid
pressure greater than the pressure drop through
through the jacket of the reaction vessel, an alkyl
the condenser so as to cause the liquid con
halide storage tank, means for continuously feed
densate to how through the sealing means and
ing alkyl halide from the storage‘ tank to the‘
into the reaction vessel.
reaction vessel, a condenser above the reaction
3. An apparatus, adapted for preparing alkyi 70 vessel, means circulating a cooling ?uid through
lead compounds from alkyl halides and lead
the condenser, automatic control means respon-'
sodium alloys. which comprises a reaction vessel,
sive to the pressure in the apparatus automati
an alkyl halide storage tank, means for con
cally regulating the circulation of the cooling
tinuously feeding alkyl halide from the storage
?uid through the condenser and through the
a tank to the reaction vessel, a condenser above 75 Jacket of the reaction vessel, a conduit connect
2,411,453
.
l2
’
ing the reaction vessel to the condenser for con
action vessel, a'conduit connecting the reaction
.veying gaseous products to the condensena liq
uid condensate return conduit'yconnecting the
products to'the condenser, a‘ liquid condensate
condenser to the reaction vessel independently
of the alkyl halide storage tank for conducting
condensed alkyl halide to the reaction ‘vessel
without passing it through the storage tank, a
liquid-gas separator connected to the return con- ,
vessel to the condenser ‘for/conveying gaseous
return conduit connecting the condenser to the
reaction vessel independently of the alkyl halide ' ’
storage tank for conducting condensed alkyl halide
to the reaction vessel without passing it through
the storage tank, a liquid-gas separator connect
. ed to the return conduit below the condenser so
duit below the condenser so that liquid conden
sate by-passes the separator and uncondensed '14) that liquid condensate by-passes the separator
and uncondensed gases pass into the separator _
gases pass into the separator to be separated
from entrained condensate, a controllable gas
vent connected to the liquid-gas separator for
controlled venting of separated non-condensible
gases only from the liquid-gas separator, and
sealing means associated with ,the return vcon
duit below the condenser and liquid-gas separa
to be separated from entrained condensate, a con
trollable gas vent connected to the liquid-gas sep
aratur for controlled venting of separated non
condensible gases only from theliquid-gas sep
arator, automatic vent controlling means respon
sive to pressures in the apparatus slightly‘higher
than those which cause the greatest ?ow of cool
tor preventing gaseous products from ?owing up
ing ?uid through the condenser, and sealing
wardly through the conduit while permitting liq;
uid condensate to pass to the reaction vessel, 20 means associatedwith the return conduit below
the condenser and liquid-gas separator prevent
the condenser and the liquid-gas separator being
ing gaseous products from ?owing upwardly
placed above the sealing means a su?lcient dis‘
through the conduit while permitting liquid con
tance to provide a head ‘of liquid condensate
densate to pass to the reaction vessel, the con
sufficient to exert a pressure greater‘ than the
pressure drop through the condenser so as to 25 denser and the liquld-gasseparator' being placed
above the sealing means a sumcient distance to
cause the liquid condensate to ?ow through the
provide a head of'liquid condensate sufficient to
sealing means and into the reaction vessel.
exert apressure greater than the pressure drop
6. An apparatus, adapted for preparing alkyl
through the condenser so as to cause the liquid
lead compounds from alkyl halides and lead so
dium alloys, which comprises a reaction vessel, 80 condensate to ?ow through the sealing means
an alkyl halide storage tank, means for con
~ and into the reaction vessel.
8. An apparatus, adapted for preparing alkyl
lead
compounds from alkyl halides and lead so
tank to the reaction vessel, a condenser above
dium alloys, which comprises a jacketed reaction
the reaction vessel, a conduit connecting the re
' action vessel to the condenser for conveying gase 36 vessel, vmeans circulating a cooling ?uid through
the jacket of the reaction vessel, an alkyl halide
ous products to the condenser, a liq'uidconden
storage tank, means for continuously ieeding al- 1
sate return conduit connecting the condenser to
kyl halide from the storage, tank to the reaction
the‘ reaction vessel independently of the alkyl
vessel, a condenser above the reaction vessel,
halide storage tank for ‘conducting condensed
alkyl halide to the reaction vessel without pass 40 means circulating a cooling ?uid through the
ing it through the storage tank, a liquid-gas sep- - condenser, automatic control means responsive
to the pressure in the apparatus automatically
airator connected to the return conduit below
the condenser so that liquid condensate by-passes ‘, regulating the circulation of the cooling ?uid
through the condenser and through the jacket
the separator and uncondensed gasespass into
the separator to be separated from entrained 45 of the reaction vessel, a conduit connecting the
tinuously feeding alkyl halide from the storage
condensate, a controllable gas vent connected
‘ to the liquid-gas separator for controlled venting
of separated non-condensible gases only from the
liquid-gas separator, automatic vent controlling
means responsive to the pressure in the apparatus,
and sealing means associated with the return
conduitbelowthe condenser and liquid-gas separa
tor preventing gaseous products from ?owing up
wardly through the conduit while permitting liq-'
‘ reaction vessel to the condenser for conveying
gaseous products to the condenser,'a liquid con
densate return conduit connecting the condenser
to the reaction vessel independently of the alkyl
halide storage tank 'for conducting condensed al
kyl halide to the reaction vessel without passing
it through the storage tank, a liquid-gas separa
tor connected to the return conduit below the
condenser so that liquid condensate by-passes
uid condensate to pass to‘ the reaction 'vessel, - the separator and uncondensed gases pass into
the condenser and the liquid-gas separator being I the separator to be separated from entrained con
densate, a controllable gas vent connected to the
placed above the sealing means a suf?cient dis
liquid-gas separator for-‘controlled venting 01 sep
tance to provide a head oi liquid condensate suf
arated-non-condensible gases only from the liq
?cient to exert a pr'essure'greater than‘ the pres
sure dropfthrough the condenser so as to cause 60 uid-gas separator, automatic vent‘ controlling
means responsive to pressures in the apparatus
the liquid condensate to ?ow through the sealing
slightly higher than those which cause the great
means and into the reaction vessel.
" _
est ?ow of cooling ?uid through the condenser,
- 7..An apparatus, adapted for preparing alkyl
and a U-bend in the returnconduitbelow the
lead compounds from alkyl halides and lead so
dium alloys, which comprises a jacketed reaction 65 condenser and liquid-gas separator to provide a ,
liquid seal preventing gaseous, products from ?ow
vessel, means circulating a cooling ?uid through
ing upwardly through the conduit while permit
the Jacket of the reaction vessel, an alkyl halide
ting liquid condensate to pass to the reaction
storage tank, means for continuously feeding a1
kyl halide from the storage tank to the reaction ' vessel, the condenser and the liquid-gas separator
being placed‘ above the liquid seal a su?icient
vessel,- a condenser above the reaction vessel,
distance to provide a head of liquid condensate‘
means circulating a cooling ?uid through the
condenser, automatic control means responsive to " su?icient to exert a pressure greater than the
pressure drop through the condenser so as to
the pressure in the apparatus automatically reg
cause the liquid condensate to ?ow through the
ulating the circulation of the cooling ?uid through
the condenser and through the jacket of the re 76 liquid seal and into the reaction vessel.
2,411,453
9. An apparatus, adapted for preparing alkyl
lead compounds from alkyl halides and lead so
dium alloys, which comprises 1a reaction vessel,
an alkyl halide storage tank, means ‘for con
tinuously feeding alkyl halide from the storage
tank to the reaction vessel, a pressure equalizing
line between the reaction vessel and the alkyl
14
densate, a controllable gas vent connected to the
liquid-gas separator for controlled venting of sep
arated non-condensible gases only from the liquid
gas separator, and sealing means associated with
the return conduit below the condenser and liq
‘uid-gas separator preventing gaseous products
from ?owing upwardly through the conduit while
permitting liquid condensate to pass to the re
action vessel, the condenser and the liquid-gas
action vessel, a conduit connecting the reaction
separator being placed above the sealing means
10
vessel to. the condenser for conveying gaseous
a su?icient distance to provide a head of liquid
products to the condenser, a liquid condensate
condensate sufficient to exert a pressure greater
return conduit connecting the condenser to the
vthan
the pressure drop through the condenser
reaction vessel independently of the alkyl halide
so as to cause the liquid condensate to ‘?ow
storage tank for conducting condensed alkyl hal
ide to the‘, reaction vessel without passing it 15 through the sealing means and into the reaction
vessel.
'
through the storage tank, a liquid-gas separator
FREDERICK C. MITCHELL.
connected to the return conduit below the con
JAMES C. LAWRENCE.
denser so that liquid condensate by-passes the
JOSEPH L. STECHER.
separator and uncondensed gases pass into the
separator to be‘ separated from entrained con 2o,
halide storage tank, a condenser above the re
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