June 1 , 1926.

'

1,586,732

E. I. CLAPP
ABSOLUTE ALCOHOL PROCESS

Filed Nov. 18, 1924

anwmtoz

W c9 . QQW
$3M? .

Patented J uneil , 1926,

' UNITED STATES

' 1,535,732

PATENT OFFICE.

EL'woon' 1'. cLArzor BALTIMORE, MARYLAND, Assreuourro' U. s. INDUSTRIAL

. 1

ALCOHOL 00., A CORPORATION ouwEsr VIRGINIA. .

ABSOLUTE-ALCOHOL PROCESS.
Application ?led November 18} 1924. Serial 110,750,519. _

This invention relates to an absolute alco

hol process, and more particularly to one
5

binary mixture of alcohol and'benzolin the

middlevof the column, while absolute ethyl

wherein alcohol is dehydrated completely by alcohol will be'found at- the bottom~ of the
distilling therefrom constant boiling mix column, and during the progress of this op

tures containing the water present in they eration this'ethyl alcohol will bewit'hdrawn,
.
at approximately the rate atwhich it is pro
The invention has as an object a process of duced, through a pipe 7 to a suitable storage

original alcohol.

60

dehydrating alcohol to remove substantial

ly all of the water therefrom by means of a
The distillation in the column produces
10 distillation process, in which benzol or its on the top plate, where thetemperat-ure is
vessel.

'

'

equivalent is employed to form constant boil maintained {at approximately 65 (1., the as
ing mixtures with the water and alcohol, in constant. boiling ternaryjiniXture of ethyl '
order to separate the water from the alcohol alcohol, ben'zol, and water, "or as near this

which remains in the distilling column. It theoretical-amountas the design of the appa
is also an'object of the invention to regulate ratus- will permit. This mixture passes
the ratio of the benzol or its'equivalent to; the through a'vap'or pipe 8-into a dephlegmator.

15

water, so'tha't there'gulation, operation,- and 9, which condenses part?of the yapors and re
control of the' dehydration process will be turns the, condensate .a-s .re?u'xv through a
.inade'vmy- simple, and so that they product pipe 10 to the top plate of the column..-'_ The
produced by} such process .vwill be uniform ' remaining yapor'is: now condensed in a'con- '
and of high quality. ' Other advantages and denser 11, which also'cools the condensed objects of the invention will be more fully liquid, The. latter: isrdrawn oil" through a
set forth in the'following speci?cation,~in ,valve 12 and flow box 13, andfp'asses through

. which aipreferr-ed embodiment of the inven--' a conduit 14 to a separator15l Any surplus

2 as 'tion'is fully described.

'
held backby the"valve_12 passes through a
'- The said preferred embodiment of an ap# pipe 16_,to the top. plate of the column 5.

paratu's forjuse with my invention (is illus-_

80

The condenser 11 isw'ented to the-air. The '

trated-inj the accompanying'drawings which vwater-supplied 1to the dephlegniator and,

form; part lot the: speci?cation, and V in condenser i's'regulated in-any sui'tableway,

30

and the steam that enters the" heater 6 is

which1 -

_ . The ?gure shows, in ~diag_1_"ammatic"form,f

preferably'regulated- in'a-ny suitable manner

lanlapparatus for carrying out the process to maintain a; de?nite pressure therein. - .

of dehydration'witli the aidof _-a third liquid

'Upon entering the separator 15, the liquid

separates intotwo '-layers,'the top layer 0011-"
3'5. For the purpose of illustration, it will-be sistingchie?y of ben'zol and the-bottom layer
7' assumed that commercial ethyl alcohol con consisting chiefly of aqueous ~alcohol. The 90
such as .benzol.

'-

'

taining 95% by yolume-purealcoliol vis- to be ' approximate~ proportions in these two layers- '

areas follows : iThe benzoll layer comprises

less strength may be .used for- this purpose, bj?weight85;6% _.ben'zol, 11.6% alcohol and
.if desired.-- Thealcohol' is supplied from a 2.8% water. The lower layer comprises by .

v ' dehydrated, although alcohol of, greater or

40

suitable tank 1,.and theben-zol sufficient-to, 1weigh't8.1%_' benZol, 151.3% alcoholkand

charge the: apparatus, 5 is; supplied from a. 40.6%=water; The upper benzol layer ?ows
tank 2. -' The liquidsfare mixed- prior to enter-s " back intov the column ~5__ jthrougli the pipe 4:,
_- ~ing'a?oW'boX-3, and thence pass through vwhich alsoseryes, as preyiously's'tated, as the
45,- pipe flinto-a dehydrating column" 5._ The entrance-pipe for the mixture of 95%. alcolatter is heatedJat-its loWereI-Idby means of -l_io'_l and benzol. _ Thebottomj'layr makesits

ailsuitab'le steam "heater, 6, and. the- mixture vexitthrough a pipe 18, which acts as a-leyel. regulating .dev'ice', and;thence passes into al

. _ in'. 'the column is recti?edv until the- ingredi

50

_ ents areiproperly' distributed throughout the scrubber-19 wherein it" is'w'a'shed by means
column; .' When, equilibrium conditions are .._of water entering through atpipe, 20,- Ass '.
obtained, .a constant boilingternary mixture

resultv the remainingfybenzol is separated J05

comprising approximately by Weight 118.5% 'froml the mixture and ?ows back froi'nxthe
ethyl alcohol, .74.14-%-benzo1_,1_and 7.4% water top of the scrubber by means hf apipe 21' to, will appear at

topv of. the column, and a the aforesaid pipe 4,,tlius reentering _the'_'dis-.- '

1,586,782
regulated in such a. manner as to maintain
tilling column 5. Substantially all of the the
proper temperature at the top plate of
benzol used thus is returned to be used again

being accom
in the distilling process in the column 5. the column, this feed regulation
plished by operating a valve 31 in the alco- '

The washing in this scrubber 19 produces _a 1101 feed pipe, the operator being guided by
wash water containing by volume approxi the reading of the thermometer 30 in adjust
mately 0.1% benzol, 25% alcohol, and 74.9% ing the valve. The valve 31- will be so oper
water. The aqueous alcohol thus produced
as to maintain the ternary constant boil
is removed through a pipe 22 which delivers ated
ing
composition
on the top plate of the col
it to an alcohol recti?cation column 23,
wherein the alcohol is recti?ed'in the usual
manner to recover 95% ethyl alcohol, the
water being discharged at the bottom of the
column. The vapors from the column pass
through a dephlegmator 24 and a condenser
25 and the condensate issues from the same
by a ?ow box 26. From this flow box the

10

70

umn. Since substantially all of the benzol

originally admitted is continually recovered

an

returned to the distilling column 5,

there will be no occasion to admit further

benzol from the tank 2 except to replace

losses, and when doing this the benzol is
admitted until the proper temperature is
indicated by the thermometer at the side. of
condensed liquid may be passed back again the
column. The regulation of the admis
through the pipe 4: into the ?rst distilling sion
of alcohol fixes the ratio of benzol to
column 5. As in the case of the column 5,
in the mixture entering the column
suitable pipes 27 and 28 are. provided for water
through
the pipe 4, since the water is of
supplying the top plate of the column with course obtained
from the incoming alcohol.

15

20

80

liquid.

35

40

,
A suitable thermometer 29 is provided as It has been found that this ratio of benzol
shown on the column 5; to indicate the tem to water may be approximately 17 :1. How 90
perature in the column at the point where ever, this ratio will diminish and reach a
there is alcohol containing a slight trace of ratio of about 10: 1, or, in practice, any ratio
benzol and where the temperature is nor from 10.521 to 95:1, as an approximate
limit, when thecolumn is operating
mally 79 C. If the temperature there in lower
creases above that point, this indicates a loss with nearly the exact constant boiling ter 95
of benzol by leakage, and loss due to use of nary mixture on the top plate.
second method of regulating the proc
wash water, etc., and some further benzol essThe
is
to
hold the feed constant and regulate
should then be added .from the tank 2. As
re?ux by means of the valve 12 in such
already pointed out, the alcohol reaches the the
bottom of-the column in a pure form while a manner as to maintain the required _tem~ mo
the water issues from the top in the form perature on the top plate of. the column
of a ternary constant boiling mixture, which This method of regulation need not be fur
is suitably treated as described, to remove ther described, as it would be analogous to
?rst-mentioned method of regulation.
the water and return the benzol and alcohol 1theAn
advantage of the rocess just described
to the column. The number of plates re is the close
regulation w rich may be obtained 105
quired for the recti?cation will vary with

and the resulting purity of the product.

the design of the apparatus and will depend The
uniform manner in which the process

principallyr upon the e?iciency of each plate.

45

It shou d be noted that in this embodi may be conducted requires lesslabor and also ' ment the feed of 95% alcohol and benzol has the advantage of consuming a minimum 110
amount of benzol. It will be understood
from the tanks 1 and 2 may- be mixed with

' benzol and alcohol obtained from the con

that in this process benzol may be replaced

or wholly, by equivalent li uids, such,

stant boiling mixture, prior to their admis-' partly
sion to the distilling column 5. The number for example, as the petroleum hydrocarbons,
of plates above the pipe 4: should of course ethyl acetate, chlorinated hydrocarbons or

be su?icient to produce a constant boiling any dehydrator which is not miscible with
water and which will form a constant boil
ternary mixture at the top plate, and the ing
ternary mixture with alcohol and water
before
stated,
' temperature at this point, as
in_
such
a manne r as to remove the water
should be approximately 65 0., a. suitable
the alcohol.
thermometer 30 being placed there to indi from
'As many apparently widely different em
55 cate the temperature.
of this invention may be made
The operation of the process will to a cer bodiments
without
departing
from the s irit thereof,
tain extent be clear from the preceding de it is to be understood
that I 0 not intend

60

60

scription of the apparatus, but it is desired to limit myself to any speci?c embodiment
to state that either of two methods of oper
ating the apparatus may be used. Assum thereof, except as indicated in the appended
'
ing the steam pressure in the heater to be claims.
I
claim
2*
held constant, the amount of re?ux back tov 1. In the manufacture of absolute ethyl
the column 5 maybe held constant, as, for alcohol by fractional distillation of a mix
example, at a ratio of 3 parts returned to
1 part drawn off, and the feed may then be ture of alcohol, water and low boiling hydro

120

126

'

1,586,732
carbon in a columnv still, the process which re?uxing to the said still a portion of the
comprises supplying said still with a mix ultimate condensate obtained therefrom.
ture of the three substances wherein the ratio

40

6. In the manufacture of absolute ethyl _

of the low boiling hydrocarbon to water is alcohol by fractional distillation of a mix

between a point above 10.5 : 1 and 17: 1.

10

ture of alcohol, water and benzol in a column

2. In the manufacture of absolute ethyl still, the process which comprises supplying
alcohol b fractional distillation of a mix said stillwith a. mixture of the three sub
ture of a cohol, water and benzol in a col stances wherein the ratio" of the benzol to
umn" still, the process which comprises sup water is between a point above 10.5:1 and
plying said still with a mixture of the three 17: _1, and re?uxing to the said still a por
substances wherein the ratio of the benzol to tion of the ultimate condensate obtained

wzater is between a point above 10.5:1 and

1

:1.

therefrom-

'

60

7. In the manufacture of absolute ethyl

3. In the manufacture of absolute ethyl alcohol by fractional distillation of a mix~

alcohol by- fractional distillation of a mix ture of alcohol water and low boiling hy
ture of alcohol, water and low boiling hydro drocarbon in a column still, the process
carbon in a column still, the process which which comprises supplying said still with a 55
comprises supplying said still with a mix mixture of the three substances which is
ture of the three substances which is made made outside of the, column wherein the ratio
outside of the column wherein the ratio of of the low boiling hydrocarbon to water is
the low boiling hydrocarbon to water is be between a point above 10.5 : 1 and 17 :1, and
tween a point above 10.5 : 1 and 17: 1.
re?exing to the said still a portion of the 00
4. In the manufacture of absolute ethyl ultimate condensate obtained therefrom.
8. In the manufacture of absolute ethyl
alcohol by fractional distillation of a mix
ture of alcohol, water and benzol in a column alcohol by fractional distillation of a mix

25

still, the process which comprises supplying ture of alcohol, water and benzol in a column
still, the process which comprises supplying

said still with a mixture of the three sub

30

stances which is made outside of the column

wherein the ratio of the benzol to water is
between a point above 10.5 : 1 and 17: 1.
5. In the manufacture of absolute ethyl

' alcohol by fractional distillation of a mix

ture of alcohol, water and low boiling hydro

35

45

In testimony that I claim the foregoing,

carbon in a column still, the process which
comprises supplying said still with a mixture I have hereunto set my hand this 6 day of
of the three substances wherein the ratio of November, 1924.
the low boiling hydrocarbon to water is be-_
tween a point above 10.5:1 and 17 :1, and

05

said still with a mixture of the three sub

stances which is made outside of the column
wherein the ratio of the benzol to water is be
tween a point above 10.5 :'1 and 17:1, and re
?uxing to the said still a portion of the ulti 70
mate condensate obtained therefrom.

ELWOOD I. CLAPP.