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Y -:}_.&#39; Preliminary Operating Manual -Ha
Tacture er Adipic 1p1e1§§_.; g.. - _ _. _:&#39; &#39;
&#39;Introd
nt10n: _ " _  - &#39; . Y <:-_ i;§§§§
f,
&#39; e l - This mangel cover: the operating detaili for the =£§§§$%{: »
_mun§aeture or p
re adipic acid frem 
exalin. The procedure_7i; &#39;
1ecovered in rive eectione as tollowez _. -l-,§ {Q"
1. Vapor phase OXIDATION orHexalin. *
22. Refining of cycle hexanone from vapor phase Ox1da-";1,
 ~ Ptlnu
1-. .<.--. __a 1:;-L -__.&#39;
_ _ 5. Liquid phase Oxidation or Cyclohezanone to 1¢1p1e Ti}§"
.Ac1d. - H   .3-&#39;4? 
44. Purification of Adipib acidv-from liquid phase -5..
 e xidaticn
Q  I :5 0 R6 covery or Lcetlececid and Ldipic acid and from &#39;
7 purge liquor» &#39; W" &#39; 3». ..
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Hateriale Per. Day Quanities .
. per moth , :i"¢»¢ ; i - -- &#39; e 0 .eJ&#39;9&#39; _ e~.-,- ,_ J J, »<:
gf; §:}nmP7 of Process §ateria1s :!.&#39;J _&#39;"%Ti&#39;
2  &#39; - _ . - &#39; -_ -. . .&#39; .-
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Peri! e
.j?.= ;T*;&#39;_1&#39;-_ "_, &#39;.
uhdipio acid ------ -- vvs # --- ---- --.-- 21,000 i --------250,000#_
Acetic acid ------- 145 # ------ -------- 4,000 # ----- ---4e&#39;,000 §
"-»_,__:_,-. . -.
h Cyclohexanone ----- 91 gals. ----7------2,500 gals.--~--$0,000 gal .
__ _Bexa1in --------116 gals. - ------ ---3, 200 gala.-----58,000 b?
Hanganeee Acetate --l.7# --------47 # ----560 # &#39;
Darco ----J---17 # &#39; ----- ------470# ----7---5,
&#39; Acetic acid make -up will be required at this rate,coo! -
once the system is completely tilled. Approximatel§ 5,000 lbs}
of Acetic acid will be required when first starting the process.
At least tour teed mixes will be made before any recovered .
Acetic acid is available.
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->- to Cyclohexanone. &#39; &#39; &#39; a JQ
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.fr.f 5- l 1. Hexalin and Cyclohexanone are inflammable attt§i¥T?
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Part l."Vapor Phase Oxidation of exalin _i: *i- jg?
.1"_. 1--
Discussion or Safety Precautions: ~ v;-~ t_,,+g?l --. .3-"EL ..,.. *
-q--"U -t . -aale. Explosion proof motors and lamps are used, There shoubd}}.&#39;
not be smoking or open flames in Fhis area. Also avoid bringing
these materials in contact with the skin; .-. -HH. . H. ._ .-. &#39; --&#39;.-&#39; is .
Outline of Process: ~ t &#39; 
Vapor phase oxidation is accomplished by passing
Hexalin vapor and air over silver gauze Catalyst, which operates
at about 550 C. Although the reaction is slightly exothermic &#39;
-  -_. __the converter is not self sustaining. External heat must be EH
applied. The off vapors are condensed and decanted into a A
water saturated Cyclohexanone layer and a Cycloheaanone saturated. -
water layer.The err gases are cooled and vented toaatmosphere 
A flow diagram or the process is attached   Figure 1!. eff
. -.---v-&#39;-.-
Detailed 0perating;Instructions 2  -
 A! Starting the process
Q1-$2-  &#39; - _
1. Since the freezing poi nt of Hexalin is approx-&#39;
-imately as c. the hexalin storage and =11 lines through which &#39;
Hezalin passes must be steam heated and lagged. The temperature -
is
on Hexalin reed tank No. 3-A must be held between 30 and 35 C.
Turn steam on teed tank Ho. 3-A and all steam traced lines. .
.. _2. Fill Hexalin reed No.5-A untrm-erases.-J atnmniznet" -- . . I . - . - ,t .-
Irom the tank rdrm.&#39; _  . ." ~?§§p5" &#39;
t. _- --r.- . &#39; . .
}:;- 3. Tnnn water on converter H0. 4-A. . ;"-i§§§i
- 4. Check decanter No.5 and see thatv valves are set
to put.oil layer to No.7 storage and water layer to No. 6 storage
.5. Turn rull steam on vaporizer_No. 5-B. §;:.&#39;_"jl
1- u. - Ais 1...; w e-r Is 1-I.* "" &#39; *- _ __, _____,, _._.... .. ._ ,_. .. . ,__.._ . -----q:-w.--&#39; -~ &#39; *1 , .,--. - H .,_ N _.___....,_:._ .-.&#39;.-~-- -.-_-.- .. -.-----,-~.-- n -- . -: . &#39; 9" - __ _ - ._ -:

lQ!&#39;!"""~ ""&#39;T""- """&#39;T""&#39;=- "M "-"*Y"#.&#39;.&#39;-1--"::w::&#39;,g-!E
E._ ._ ......_.__..._.._.._.:.-..-._-._ _ __ __, _._._4-A-as--~44-i _I
u" 6. Start air compressor &#39; _ M
!-. - 7. Start Hexalin teed pump Ho. 3-D. &#39; ; 3-. =~5- --
- hi 3. Turn heat on converter Ho. 3 -C and heat to 5Obhé.?iF
;f
. - &#39; $2
A 9. Start flow or Hezalin of 3 to 4 G.P.H. to vapor1zsr,?
v £:E;B.8tart very small tlov of air to vaporizer .  lot more3-0&#39;-»__ _ . ......-..~»3-- &#39;,i+:l-7,14,-;="_-F  ?.,...|.___;,.;.-----. -,92 ._- .4... _ _
92.. , +
-,4 ._-
_ then 2 to 3 cu. tt. per. min.!  .- 1
ll . Ls reection&#39;lights Qif92 gradually increase air flow
to hold converter between 500 and 650 C. -s
12. Gradually raise Hexalin feed to 5 or 6 G.P. H.nnd
 increase air flow to correspond. - _
.f 1 13. Check condenser No.4-A to be sure it is operating. &#39;
14. If at any time the Hexalin flow is stopped, turn off
.; ,- all flow immediately. - - - _
,&#39; Shutting Down the Process. .
. _. __ Pip it» e  e****- - .
.&#39; 1. Stop air flow to converter. -
&#39; é- 2. B&#39;tpp Hexalin Ilow to vaporizer.
&#39; 3, Hexalin feed pump NO. 3- A.
- _4. Turn heat off condenser. . I
_ 5. Turn steam oft vaporizer. _
, 6. Turn cooling water oft condenser. _ - _ ~
.r 4 4. r.-
.some time, condenser and water lines should be drained!. §E£:
1  -"- - I i . - .. W! r::?:_ H T U C51 *  £ I &#39; &#39; - -  2
: - -C."Control not Process _ gg __
I* &#39;..- 4-  -" 3-:
_}&#39; &#39; &#39; -- no control is required tor the vapor phase
v &#39; oxidation beyond maintenanoe_oQ;uni£orm flows of air and.¢
_ exalin being fed. Operating temperature of the converterLéyi *_. Ho. 4-A  cautiona In freezing weather leave b. u 5%}.
I small flow of water on condenser, it shut down is to be*tor
u
- - - &#39;_._&#39;.--"|,~.:&#39;92&#39;_92.. _. -, _-  &#39;_ ,-,_;,-_?_
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;-. -_.;._.

5--H. ;.-..- -~: 1 ,~<:_;»l¢&#39;~- __&#39;_il" . -- .-_._ .._ ___ - - 92 -1-:-..»-;~-»-;-A--»=~»--n_;:_,;_ ___/ _, T - A--5 -,-q_,,:--&#39; ----92._.¢~"~ -;u~_&#39;_ -__~ *4. _;;__:._.. .7-. @_ , _ ,. _V I , cont. from Page II.  :    "___  -   &#39;7 y -must be between 500 and 550 C. It is no sary to supply_{;"
l some external heat to the converter ,_&#39;. ~ * "  ;>_
__ V As a general check on convertlton and performance -oI_i:;-4;
- =@;~:» __the unit the laboratory should analyze thee crude productfiipi
, 92.. ._.
by precession distillation. Occasional analyses should be ?x§~
made of the off gas, to check the loss of material as C0 -_
and C_O§-- - . _ -| . .. .
Part 12. Refining of Cyclohexanone 
Outline of Process  1 _
The crude Cyclohexanone produced in the vaporizphsse ..
~  oxidéation is refined in a 200 gallon vacuum still. The process
consists or drying the charge by refluxing through adccanter, .
producing a refined ketone fraction, aAsemi-refined ketone
. fraction, and a hexalin residue which is returned to hexalin 
E? _
storage.
Distillation Procedure: , f
See Fig. &#39;2 tor flow diagram. ; d ~
A. Productbcn or Refined Cyclohexanone from vapor,/
phase Oxidation. -&#39; -
1. Chargp still H0. l0-d.to approximately one _ " _
inch from top or sight glass with crude Cyclohexanone from Q?r
IO. 7 tank. I  
2,. Turn water on ketone still condenser No..lO-_.
. 8. Be euro that still is vented through valvel.&#39;l. 192
at base of&#39; l0-H. &#39; u._;5  &#39; "&#39;§;j; &#39;~
::f~*&#39;- 4. Turn full steam on coils to H0210 -A kettleT?1f?. .. . I
=and heat to about 80 C. Reduce steam tie; to about-10Q 1e§§§§§ *
&#39; &#39; per. hour and bring still to reflux. _ 3 &#39;1&#39; ;"T=;
. _ . 5 5. Bet valve so that make passed to decanter.Noll1O4D
- water layer to water storage ale. 6 and pil layer returned to
_x: .. -&#39; 1-. -,.. -.,,. . ...._, ,_.,__.., .._ . ._. ,._. ,..._._,... -._ i. - --... ~_ W... ----»-»-.-- --- ---_--- --1----- -.-92-re ----1-fp.-eq-1331-~r--v---qr--I-~»---P-92~»-;¢fT=&#39;!;-3-q-r--f -¢ --W __ .|&#39; . t  .-&#39;- &#39;~g. v .   .. s  -:.,.¢

F.
3..-. 1 .. .- .s . . ., . - i 1- .._ .....a.92.-s-._ &#39; ...._..-_-,,-_.s. ,-- ~~¢»_e,~,;_e;,e4a ..._1- -----L ;_.__.-l. --- &#39; ; a ..  ~* ~a~e_."- -r ...&#39;. _1_l_ _.
. &#39; 6. Decent water eggtinuous y st spp:>nimate1y 2.1 1
. . _
~ .... ._;_-... _ . &#39; T1, _-_-__  _still kett e. . - -h. f - &#39; -  &#39;_ :_    lbw1   4: O  _v - y
1p reilux ratio. The proper draw off is that which gives the 
-4 . 
maximum water removal. &#39; _ ;;-:- - -.h?=¢e.». 1&#39;4 -, .-
0?, 7. When head temperature reaches 100 C. and no»nere&#39;
water will separate turn oft steam to kettle. - ."m3¢if$;-*=.. _. ,E,¢L4é__ _
8. Bloee valve to decanter Ho 10-D and prepare still- "f1&#39;.§._.
for vacuum operation. - - 1-.r--;Ȥ L
9. Close valve on oil return to kettle.
10. Start vacuum pump as instruced below and gradu-
-ally reduce pressure on system .  At such a rate the normal-e
boil up is maintained to 2.0 inches H. 3. _
ll. The tollowingkreuts are made:
at 15.6 C. at
3. Ho. 7.
121
at 2:1 reflux
at 4:1 refluxLe :.- _92..- 3  &#39;atQr Q1112 t° R01 "&#39; 10 .1 -
a 4:1 reflux ratio - to crude ketone storage &#39;-
B. Prom R.
ratio to refined
C. From R.I
ratio to refinedI. equals 1.452 to 1.453 at 15.6
ketone storage No.12 &#39;-
equals 15530 to 1.4540 at 15660
ketone storage Ho. 12. . Z
D. From R.I. equals 1.4540 to a head temper-
-ature of 88 to Q 0 C.  at 2inch Hg.! at 4:1 reflux ratio to
crude ketone storage No.1. " -1. .&#39;;-
1B. The still residue is pumped   Ho. 9 pump!
to crude hexalin storage at the hydrogenation plant. L @_
- Q1 &#39; 12. The actual distillation procedure made , v.9§*Z3£I
. . ~_ . _gevhat from the above depending upon the quality of the erude_&#39; .._|a_ _
- s  -
cyclohexanone charge. For low grades of crude ketone it will
.- he necessary to take a semi - refined ketone out to be fed in
a semi- refined storage No. ll for redistillation 32_§~-
1 &#39; , . t . H-..
,__ ___ ,- ._.,-., _,_.,,.._ T.,_._..,_,,_..___..._.__._|.».--.-..-----.. -..-3.-".11-......-P v--1---q. -14* ~--tr -.-~ ......» 7-. -.-_-_-&#39;:"-1v----,._&#39;!__::"&#39;f__" r &#39;

 "* ~ * &#39;__... - .1 -. -- -&#39;4_~;:-~1--.$~&#39;- --=7-1&#39; ..._.¢._.;_-. .,_...._... . ._. i-._ . _._._4-........n...;._....-_-_._. _ _ _. _l.~__- --T-.  -- -- _&#39; . _ - . . _
&#39; - - _- ,__ --. r . = 1 5 ~
EB. Seetthat .11 valves i=
Figure J gves the boiling point pressure curves for cycl-
-ohexanone and hexalin. ! &#39; "w t _
-,&#39; Fig. 4 gives a pivot distillation of crude cyclohexanone;r.~
as produced by vapor phase oxidatio. s e _ ._..27¢.
&#39; Recovery of oil from Cyclohexanone water layer. Ire;
l. Charge still No. 10-A approximately li-inch below ,..
the top of sight glass with eater layer Ho. 6 tank. --
ndenser Ho. 10 C __ &#39; 2. Turn water on ketone still co _
. I &#39;  ..
33. Turn steam on kettle and establish reflux.
4. Pass draw off through decanter returning water
layer to still kettle and oil layer to crude ketone storage &#39;M
ximum removal : No.7. The rate of draw off is set to give the ma
or oil. &#39; _
5. When all oil has been removed shut down and discharge
I
water inn kettle to sewer. ~ _
6 .
Vacuum Pump Operation. __
I  _
1. See that the oil is at the proper level in the oil. _
separator tank. The proper oil is Opalube S.A.E 20 tor winter
operation and Opaluba 8.5.3.30 tor summer operation.
2. To start tacuum Pump. .j_ ,
_ A.-Start small flew water to water Jacket. t *"y_
n oil seal line are closed
-f &#39; and remain closed untill pump is running. §_+_
2 5*-&#39; . C. Turn on power and start pump running. t
J"5; D. Open wide plug cock in oil seal line. k
e-half turns the valves allowing
oil to flow into bearings, at each end of crank shaft.E. Open one and on
._i _-.-,_.....- -.,.,..,_.._.._...-..-s. ..., __.......-... ...__-_,.,,.._-q -&#39;.._--_..-,-.._...... _ ...-,..-» -_- --  --- --_~ _""T92_ --_-_- 1---_ S mg 1.;-,.--92--; .~.-.- »7---_-¢.-:.&#39;~_-3..-.7-1--_¢_;-. g-_,-_.--92 ._ Q...92 92

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foreign materials and should be perfectly tight j &#39; I; p jzfI F. Suc%ion lines should he absolutiii iree or allcit H@lL}{9
_ Shutting down Pump. __ _ - &#39; -
H IV d. Close plug, cock in oil seal line. - -L t&#39;lE§%%§§tf
B. Allow pump to run thirty seconds to tree itself of oil. J
&#39; "&#39; -C. Shut oft power.  1 - &#39; "= #"w¥"*
D. Stop flow of cooling water to jacket. _ e
Part 3. Liquor Phase Oxidation of Cyclohexanone to Adipic Acid.
q_~"_-|n_   __;-all 7
Outline of Process: . &#39; _ .
Adipic acid is made from cyclohexanone by e
liquid phase oxidation. Air and cyclohexanone in an acetic acid
-92 .
medium are upaseaddco-current through unpacked towers in series.
The towers are maintained at 80 C. by Inter circulation.
&#39; The adipic acid solution formed is collected in a _
hold up tank for subsequent purification. The spent air is _
first water cooled and then passed through a refrigerated i.
condenser to remove acetic acid and cyclohexanone. The condo?
&#39; -nsate is returned to the oxidizers with the feed.
A1 flow diagram is attached . Fig.5.
_ r
$
. 92.
4
r - L. L,92_
F 4*!
I
.,__.,...._.._...-__.,....._92........,..-.;,__-... r -. _._ ., ,, _. _- -.-...._..._._-.,,7-......-.l.,,,- _.-.-<,_.....___..... -. . ..=.._-..__--_-.-I-.. V.-
- t . .. - ;; ~~_. us... __-  . .-A ._.

4&#39;
*7F".&#39;T&#39;7-""&#39;*&#39;-""?_&#39; "{."""&#39;§""~"&#39;1l&#39;FW l&#39;92Y"W-§I92"I*92&#39;I&#39;;-&#39;F§ 1--_-uv~-Q».L
F1V~ ,_, _&#39; r. .- _. -_ ,_- .,_ .- _ _,ii..L_ _. . ___ . __ - ,_ - -  . - -- -- . __T.<¢i,~-e~ i - -7- --_. __ ..-_:-=h.a 1._ . ; __h_,____ .__ . ,__ __-  _. 1. IQ. - ,._g wan . I .3 i _ gl gfé ._;. /.0S artin the Process. &#39;   &#39;6 . I . 1
. 1. Aceticcacid Storage: The $00 gallon aluinu tank Ho.1§
" &#39; - . .- . . a.....,___;:-._.,§ . _
is provided for acetic acid stora~e. Since its only source o1&#39; a _ 3- ~..-... - 5- ;-.&#39;-+:;-&#39;- 1. - , _ e f-.... - _
acetic acid is from the acid recovery still, this tank will beg
 enPtY» ihen first startin8 the Process. H &#39; W 92&#39; tv uJ%?$?&#39;
_.--1-..
2. Acid mother Liquor Storage; This storage No. 34 tank f{_
will also be empty when first starting the prpceas. Its source _o
. . _ _ K
of acid liquor is from the centrifuge. &#39; &#39; - - &#39; &#39;-&#39; ;,,
3. Refined Ketone Storage: The refined ketone storage io.l2 1
should contain at least 50 gallons of refined ketone as produg @ -
-ced in Section 2. above. . p _ ___ _H&#39; -g
4. Content of Oxidizers: It oxiddzers are empty add to No.20-1
&#39;oxidizer, about 65 gallons of pure acetic acid from carboys. __
This is done as follows: d &#39; so
1"" __ -
A. Pump 75 gallons acetic acid from cartoge g-ough &#39;
pup No. 18-B to teed tank No.20-C. ___ ;__;_ _
B. Pup acid from feed tank through pump H0.2OD:tO _ »
oxidizers. If oxidizers are full from some previous shut-doin
they can usually be started without any charge. __» *_
;§.;Preparation of the Fi1l:L
The teed is mixed in weigh tank No.18 and is suff-
_ - icient to last for twelve hours. The normal teed mix consists
£ . ..&#39;  . ..- . &#39;-. J &#39; :"Z&#39; &#39;.7- *-&#39;of the following: " "
A. Pure acetic acid from No.15 tank equals 335#._:
&#39; &#39; &#39; &#39; " 2*-. ...
B . Refined ketone from 210.12 tank &#39;*" _seo#&#39;"&#39;"
.&#39;..¢-, _,.
1 C. Acid mother liquor from No.34 tank &#39; _800#._
-Ll. _ . ,
f " -  Approx.l74gals!
. Catalyst equals Blbs. manganese acetate dissolved &#39;
in tcetic acid, per batch. &#39; V _ 2;
-..--. ~-.-..-.-.  .-;-.-.-. - .:_.._-...__ , -5.... 7,. -_ .. __,-.___,,_.,,.,._._.,,. .._..............._ V -.. 2.. .-- , ... ..._ __..._ -.,,.,,.,q,, ,....z ,a.,,__,.,,.,,,,....,n....,,.-.,,_;.__:_  ,,_g _,_
 1 - &#39; " - &#39; &#39; , &#39;  ~ I &#39; -

wr WI w a-s~§q,-.7:w_ W -rr -sqw Turzfqw. F:-Q-"192&#39;Yi
"%~i1y;_ h _ 11. Start teed pump No.20-D. _ sh; <_H. ,,;§.;5,_$_£$_392 -..92 ..- -._ .-....-.-..--.-..-~...L_ _,&#39;.;-..i Q_._ ... _ -.....__1_~-- - ~43-A&#39; -_-. --__-»_.=A-e ";I _ I _ .::_.; . in ,i_i-. e. .. i .~..- ..__._._..,..,;:_x_,;n7_.____ ______ _
_- - . _ ,. .. -- .._--=. _. -< __ .92- -__?,.-.-.T- _-_.__- 7 _ r _  -. _ _&#39; _ _
Since it id:;eceesary to add approxima{:ly 85 lbs of make- ii,
- -up acetic acid every 12 hours, the catalyst is disso1ved.1n the
;~ . .
&#39; 5 .&#39;i:~ quanity of acid inua carboy ahd pumped to the Ieigh tank. The.:-  .. _._ _.._-.~ _ sud- ~ - - . .. .. _._. ,3. ;,§""&#39;1_,-&#39;i__., _-, ..-remaining acetic acid required, 35!lbs. is run in from the;§@&#39;
 -- - ...:,_ --..-.. _.
ascetic acid storage. __&#39; l ;7 £;*§+
~ »- -qaY;a?--
&#39; Ihen first starting the process there will be no acetic acid -
. . -_. .92
in No.15 tank and no acid mother liquor in No.34 tank. The . _
composition of these mixes will be as_tolloes: -&#39;
_ r
 Pure Acetic acid from carboys equal ll55# &#39;-in
Refined Cyclohexanone from No.12 tank equals 560# _ f -
 Total 1495§ *&#39;
.Catalyst equals B# maganese acetdte dissolved in 85 lbs. ~~
of acetic acid. all of the acid and catalyst from the first
HF#; mixes is pumped directly from carbcys.to the weigh tank. Rubber-,
&#39;4 gloves and goggles should be used during this operetion.- q _:@_ii-1-. e .
&#39;Y 6. than the teed mix has been completed, circulate mix th-&#39;
--rough pump No.18-B to top of No.18 tank tor two hours. . --.
I . 4 .-
P 7. Pumptteed tbrfeedttagks
et
-6. A &#39;1 A
1, ;_i1&#39;; **:~, T4 . ,_
B . Iater Circulating system.Fill water hold up tank No.20-B with filteredweater 1 -
I
 and circulate water through oxidizers. .. 
~ - 9. Turn water on cooler No.20-F. _
_ -10. Turn ammonia on refrigeratedscolpmh No.20-H. - __§*-
.&#39;.&#39;..
&#39; |
*.:&#39;7 12. Start air compressor and set flow at 2? cu. It.per. nun.
. L &#39;_ .
-,; to oxidizers. _ &#39; &#39;1 »;3¬i&;,;
 &#39; .&#39; ,. . x.._ 0- > -"2 7-S--.&#39;.-. . &#39;"&#39;11s. Turn small steam flow on, feed preheater 110.20-14. -
i ~ &#39; §}l4.-Start feed of about 6 G.P.H to oxidizers. * IZ&#39;:i&#39;
§§§?jf ". ..&#39;... , - -.
9 15. Adjust eater circulating system to hold oxidizers at BO 0. .
16. When teed has settled out at G.P.B. gradually raise-to ~_ Q -
. __ -a
14 GQPQHI .  &#39; &#39;=;:| . , __,__ - ..
.-- . - -r- _ f_.. A. r-. ._.¢q----. ...-.-e-. --.--=-.."-..--~~.- -7.--_-c-.,. -.. _.w...--;-.92--..-- -~ - - - ----¢ ,---I --..--_-_-u--Q .v-1-".?1?&#39;¬&#39;I."".q"_3-$?_Vf&#39;¢"QSII": -..-~; . 1, - -1-. 15-,» y
. _  _ - I i . . . -  y .1; ,;. - - &#39; . ". - . Ia _ , - _ a . . . . _j
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t_. ._. .. ._ .;,._.. , . , -_ ._ __..._. l- ~_;&#39;__- _.-=A<__--_-.__--.~~., -- -- -- - _.~ -_-._._...-.-s--._._-1.... -..--»...-- . -- -4- - -- &#39;"as.-. -..___,. ,, ..., . . - . ,. - ,__ --. . , ,- ,
.. ,-&#39;l7. Check £I:Y or recycle condensate :££:!.5§r.£$r&#39;n5l§o-s /;%9
and 2066. Leave rotameters wide open so that full tics returns
B  .
etc oxidizers. - _ - >;~. c." %£.¬a.T
_  _ I. _ ¢ _ I . . - V _ ,_ . . : &#39;_&#39;- &#39; . ,- . . __-_ _:&%,Aii:;  __  
, ~18. Be sure that steam is on coil or hold up tank 80.20-I.1end
all steam traced lines in this system. These lines should:slIa§s
_ 92 _ .- . -._i:!_,__._ ,1
be heated unless system is flushed and completely drainedJ{5@5?i*"
19. Control of process consists of maintainlngeconstant f1OIl~
ofliquid feed and air and holding the oxidizer at B0 C. kf M
Shutting down the Process. -
1. Out off teed to oxidizers. .
2. Stop air flow to oxidizers, and shut down air comprel sor
if not needed for vapor phase oxidation or isobutyl PPOp6hQ&t6_. &#39;
. 4 .
&#39; 3. Shut down teed pup No.20-D. . - l 7
4. Out steam off preheater N_o. 20-N. "__;
5. Stop cooling rater to cover No.20-L and start a small &#39;
steam flow to the water circulattng system, or completely drained&#39;
to hold up tank No. 20-J. It the shut down is to be tor some - ~-
tlme the oxidizers should be drained. _
. 6. Turn water ctr spent air cooler No. 20-F.  Oaution:t"
Leave small flow of water on this condenser in freezing weather
or drain completely!. =&#39;
-w . 7. Turn ammonia off refrigerated spent air cooler. . .__~.._~-_;-,_._ .
YOU WILL FIND ANALYTICAL IETHODS ON SEPARATE SHEETS.
_&#39;.. A-.. - -,, , . _ . _.
.. __ . &#39; . h ..
-fa Part 4. Purification of adipic acid from liquid phase_ _.i-,&#39;_.""- . ..-_ ._ 1 .,_
_o1idation.: - _ 2"
_ -1&#39;  &#39;.- .
.. - &#39;" Outline of Process: _ &#39;
; _ - The effluent from the mother phase oxidizers
is cooled in batch crystallizer and the adipic acid which crystal-
, _ _ ._ __.92.
M 1  W-lites is centriisbd. f_1.°1_i=_h° _I91! °11*=.=_19¢!$1= "Id. ¥9=.P2__¢f;_.&#39;
. _ I  . _ . I. _ . - --

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I_.. _-4-_s&#39;92_.-l.J_4.,-,.,,¢,sA-_-  l_~ ..._ _ _ _ _ ,,_ ._,,_,__....._..,.._..__i.......-...-...-._-_s.....,..,.. _ 4,- __.._....._..~_-.._..__.-.-_-._.._-._~..._-=-_-l.- s. ....----- -1 1-» - - - a
3-r1
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- 2 .
j.The crude {_;hed crystals are dissolveQn distilled water V
and recycled mother liquor with a proportionate amount at _
second crude crystals and treated with Darco. Ihe hot liquor
.. , . .. ..;..;:.,-_ ,_. _.-. a-.
is filtered free or Darco and slowly cooleddin a second_bstch:§;j.
| - _p;=.-
. crystalliser. The adipic acid crystals obtained are oentrifuf_
éged from the mother liquor washed-and dried. The Mother liquor
from this step is divided into tio portions. One portion is.
held in the water solution tank for dissolving additional adi-
-ic acid. The other portion purged to a recovery evaporator, .&#39;-
where water and acetic acid are removed and adipic acid is f
recovered from the residue as second crude crystals.
A flow diagram is attached Fig. 6. e
Summary of Operating Instructions. V
_ J
- A. Separation of first Srade crude crystals from a
- acid mother liquor. N &#39;I
&#39; 1. Be sure that all lines from hold up tank llo."20-J .
to cryetallizer No.50 are heated.
2. Fill water jacket of Ho.3O Crystalliser and heat &#39;
to so c. with steam.  &#39;
3. Check distilled water supply,at least 50 gallons
should be on hand. -  _|w
4. Pump acid solution from No.20-J to Io.3O _ »
crystallizer. Charge should be 250 to 300 gallons.&#39;t ¥" t"
5. Btart slow speed stirrer in No.30  --__ 4 w???
. _;1- -  6. Start flows of cooling rater to No.30 jackets
_"_, . . _»....... u _ -,_>_.,.
Adjust cooling water rate to give cooling or approximately 1;
.- cc.&#39; - - - e -pg -._.&#39; 10 C per hour. &#39;3 .F 
7. when the acid liquor in No.30 has crystallised.
&#39; and celled to 20 0., Check centrifuge No.51 to be sure it Iill .
-operate profrlis . 1 .- -
_,_..q-- i,--I-1.-..,.,,,,_,._-..-, .,..-.-..-.-..~...-.-._- --.  __;;_. ,. .._. . ,2-._-:_ .w-v--11¢-I--+-"~r: p-|=<._?-<|,-_&#39;_;-|- --.---;=-.v-- --if-, ,_--W -92_,-=92"-y.-.--1-P-I-11-gin:-_&#39;»g-"1. PW" . - . . - _ _ . _ , . .- , _ .

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Place crude adipic acid crystal reciver under centrifuge _j
discharge. _-&#39; . . -.&#39; - &#39; ." .3 ., _  - _ .  _ &#39;s_.92.d_ ,_ . .
:1 &#39;- &#39; .;, _; _ ~. _ -  - -.1 ~ ._..._..»..;-.;._.._ -
;H.- 81 The centrifuging is done on the following eycle:_;§:§g;<;i_ - w-I. _"&#39; _&#39;  ...-.~e92- .--"&#39;~  - .;  I-5. Bet liquor valves to acid mother liquor .¢$£.g§fno$§{Qf
-i*_&#39; " B. Start centrifuge on slow speed and charge from Io.§0,g
. , . 7-. _;-&#39;&_--a-&#39;.&#39;r_...-- .-. -. -
crystallized. Ihen cake begins to build up near the top of ths&#39;r
basket, stop flow :1-em No.50 &#39; .. -. ._ . .- 1:1:lQ;:5§lfgQI1I§§§§f§.§.&#39;§lLL
- ~ - _" .r.v---&#39;-
O. Put centrifuge on high speed for one minute. ;*
;"
D. Put centrifuge on slot speed. - »[-.*.i3L§§j:§j3g g.-- "&#39;92..-_
E. Set liquor valves to water mother liquor storage No.64.
F. ash crystals with three gallons of distilled water.
G. Put centrifuges on high speed for one minute. &#39;_Q»g
H. Put centrifuge on low speed and discharge basket to;Q"
crude crystal recetvrr. * -=- ~==. 1- .. .__-_. -* _r ,
-  2. . -
,&#39; - .
Repeat the above cycle as many times as it is nec- #-
eseary to empty No.30 crystallizer. A 300 gallon charge to No.50 &#39;
should be handeled in about eight loads to the centrifuge.uf£&#39;f?&@
9. when charge has been centrifuged, cash centrifuge Itth .
five gallons of distilled water. Ran wash cater to Io.54 tank.
. ._ --- -. >__§ -
B. Purification and Drying of first grade crude crystals.
I |_ 4-I 1I-an I -_- .|s___-,_ _ -_v _
. l. Besure steam is on heating element in water e v
.. ..-  __;.1-2; ;.&#39;.*&#39;-:&#39;1&#39;- "&#39;._-92..-r,..&#39; .-solution tank No.41 and all steam traced lines. __q.Li ".&#39; Y .
Yshould be on hand.
&#39;. .;,-&#39;
": &#39; 3. TO H0041. 1 ... . ,- . - 92
1&#39;and 50 gallons of water
agitator and heat to 80
* 4. see see2. Check distilled water supply, at least 150 gallons
_ _ &#39; . r, .";q_a ,&#39;;"!-_.&#39; -.. ...&#39; -j . 7.; &#39;. _ &#39;&#39; -.-_.:&#39; . .. fr 1&#39;;-~ &#39; -&#39; Q., . .
tank add 45 gallons of distilled rater
- - _&#39; &#39;-.&#39;»*".-.- .&#39;;&#39;.
mother liquor from No.54 tank. Start"
O. .f . =- e -
__ . L. &#39;_ -1»-_.e.
lbs. of first grade crude crystals and .
BO lbs. of residue crystals and dissolved, = ~ 7&#39;¢;§r,~.
".1 ._ -- .--_._.-... ¢--,.__ -,,,....,-,._-----~ .....- -.- -.. ....-K. ____-..-,-»:-._-- 1-._~ -n--. -=>;- ---H av-_ fr * -1-"*_--3 &#39;..:.- ._*-- --I . ..  _ ..A_,..&#39; [A _. .-. ~K: 1"o&#39;-*- :j&#39;riA;;:ji_1q;i§=:g_3:22:29
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.- ._  k I 5. Add Q lbs of Darco and  half!  W
6. In essethere are no residue crystals the batch is com-
-pleted with first grade crystals. - r g-» 7- ,=;:;J.~,%@..l¢
. <-é,~_- §-&#39;.&#39; &#39; f. . 1 * l 2   ~__ -; r- ~.;~~- ;~;="-{;- -
-1fqw§n , "Distilled water is used when there is a storage nt_jeter&#39;.
**&#39; "  .1 &#39; ".- . . 1 F_?2@§m3..
_ Imther.1tquor. &#39;  &#39;1 _. . ~- <§atq" 
-=&#39; : . - -K -. -- -1&#39; .._ ¢2f"-1,;~.-&#39;?;-- -~ &#39; -- -&#39;~-;,- z.---~  :17. Check filter press Ho es be sure that 1: is m operating
condition. eteam should be on all trace lines and heating elements
- . . . . .. . .- -_- . _ . __ _. -.. _. . .. -__, -..__..__7. ,.-U-.. -_- _. ._~ - - .._ - .... ->- ._ .¢.-- ._ _ .
in press. . , - .H .._ .H
8 . Start circulating pup No.46 A. and circulate water ~
&#39; solution through filter press No.46 to top of 10.41 t&nk.l,f1Q &#39;
. Continue clrculatio untillall Daren has been removed 5;-,
from the solution. - " . . .,-r_t;y§@g2-
9. Fill jacket to crysetallizer No.50 with water and T . _
heat to 80 C. _ - 7__ 1 L ,
10. Turn steam on tracer system from filter press Ho.J50a__
crystalliser, these lines remain heated unless flushed and drained .
&#39; l 1. When water solution is tree of Daroo pump to.crystg
. .. _ .
-allizer No.50. - &#39; &#39; -
12. Stop agitator on No.41 and No.46-A. pump. " &#39;
. Caution: Do not turn steam oft of heating system _=.
unless flushed end draines. &#39; &#39;i
13. Start slow speed stirrer in crystalizer 80.50 and
starts cooling waterto Jacket. Cool charge at the of 10 C per. hr.
. .  . .. .";_
cool to 20 C. Care must be taken to avoid sudden cooling since
. "
rate of cooling governs crystals size. It may be necessary_to_;-_
.- -.&#39;hi§2seed&#39; the batch to start crystallization. This is done bi¬§$;V_
Tlntroductngnseveral crystals or pure adipic acid to the §¥§.£.11=.r
92 Z. &#39; -&#39; .._ . l -z ,. . . . _ >. ,5._-_-_- - _Aiiiah-t l 14. vhen the solution in crystallizer No.50 has been
, .
evolved to 20 C. and crystallized it is rea
y for centrifuging.
&#39; 15. Place refined adipic acid crystals reciever under
. &#39; r .* .- . . . -~ . _ .--.- _ _-. -&#39; 7, __ . , v 1 3 " _centrifuge discharge. . v&#39;l. d &#39;:&#39; - y :- ="{fl&#39;T[ . -~ 92-----n-- -  - - -  » - - -v - -._- ~- ~ .--. *~*-4&#39; - ,-sq:---v *"Il~C&#39;92&#39;*-"&#39;92~PV_ "-  92&#39;..- -I-92-e-1--E-!. _A"Df_&#39;I:1Vl"92.~-44&#39;;-Q -$5, 1,,-7"£.!7&#39;.  V , ; &#39; - _--. -&#39; r
K

T}&#39;i&#39;"-JTT 1&#39;!-T_ _ . _ ____ _ i____A _ ___.___-; __ ____,,_  _ _ i ___ ___  ._.,a___._l.&#39;...-.._;......,..e._..-rc_.. --=-e -- 4-s --- - - U-V, _, ,,_ ___,-.._.._......_._._n-i ,....,. -__. in g _ -- _ A 7- _ _ _ _ J ____:___ _ .1, _ 7
, -  ~~1.- P"...-*~< - -- * ~ e -~- -- -  -&#39; &#39;  -" ~"- *;&#39;.""  -~ 2"&#39;t&#39;.1=;:f-:_-*.r&#39;¥.--&#39; "?&#39;:-L;-"-:Il,;-&#39; ;;&#39;.&#39;;i~.  IM u   I   l L       e W
, 16. C -..:.&#39;;rituging is done eon the I62; owing =cyole"i_§-¢;&#39;5;_<*¢1._-.&#39;
. . _ &#39;__"&#39;92"-_,_--7 _. _. _____-___ &#39;.____:&#39;_~&#39;£.a"-.*.::_.ef:"_--" .1-.__ A
".1,_ _- T. &#39;   A-Q_ Set liquor valves to waters:other&#39;1iquor_1!torage A-
&#39;- .  -  J - _{ .- - . -- I _ _ &#39; V __:;_-  &#39; _;&#39;_ . in. - . -» - * - .- :&#39; .._ . . :4... --- . » - =  &#39; 3 . &#39;__. - -.--.-~ ~. &#39;--&#39;-"I ~-_-- &#39;92" ?&#39; - I . ;- .. .3- % -. . 0.54. - . . -- .- -. . - - l in >. __ _ ___ _, ,_ , _____ _ _ __ _ . , ,,_ .._, . ..-. -. . --- ~ -...&#39;.- I-~_--~ ¢--L-1; 1  QB-~--v-&#39;-_ 4 I- - - - . -- -~ ---- - iu ~  __ _ __ _ _ _ __* _1 _ _ . _ -. .. , --.,._- , 1:. ..-;_»---. .,.,-ta. ~ 4.8,: "P: $f"&#39;u-;_*!_=-*-"~~-yr.1-,} _.-_.---. -~. - ._,- , _. _..,,p.-.-- l _ - _ ; A . . _ I I --3?-_§q_-.___92: - 74%.-. - - ,- _ . .. - .
!..~ P.>..  B! Btartoentriruge on slow speed me charge"1riim&#39;-ff.:§".==".--.*- - J V I _   _ _. -."z:.f1-Lists:-.;Ei"_Ilo,{_&#39;5Q crystallizer. when cake begins to buildup near -the~ 1 ._?" _:_ i _ . . . - _ _ &#39; . _ _ _"__=__ ____T __ f " " &#39;-~o£ "the basket stop tlos from 110.50 crystelliser. ..i-1 i_&#39;T-J. f.;&#39;f&#39;i-",.;1?&#39;,i_,l_-&#39;~-I
-. e.
.... -
f_
in
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&#39;;l;..;._92P;-=_.~. - ._.
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Q- - -* &#39; QCOOPut centrifuge on high speed for one sai.nutliJ&#39;l&#39;,""5l7. _ ..--.-_92.,, _ .. . . - - _ . ...._.-.-._. _ ___  ,. ..;-.-..._.,-.-  DO Put centrifuge on slow speed and washYcake -with L,
three gallons oi water-distilled. 7 V _&#39;  -. I
p _- _ i.__-,,._2_
 sq Put-centrifuge "on high speed for one minute. 3
- - - . _- - . .. &#39;1&#39; &#39;.-__   {P} Put centrifuge on I1OI.1&#39;lp6Bd and discharge I
&#39; -§ --,;=.;&#39;...w .2-.--» -<§_&#39;=--1"crystals to refined adipic acid crystals recsiver.&#39;. ~;§:l,.&#39;L__&#39;1--,7-f._j
_ _ _.92,.. __ r.__- _. . &#39;_ The above cycle is followed untill crystalliser
5 , _  " Tc".
No.50 is empty. A full charge of approximately 300 gallons  _
No.50 should be handeled in light loads in the .epzr1ruge.f;??i%Z>&#39;
- - __.__ ._-.. ,.a_.. . _- - " " &#39; - ". -- &#39; - &#39; . . &#39; * - -&#39;=- -= &#39; -.-&#39;-&#39;. :5--"£"?"i"-4&#39;- - &#39; &#39; &#39; . .: -&#39;  " -&#39;*1.
L7.p;;1n5 er adipic acid. &#39;  &#39;~ a &#39;  ¥=""ff5§ gT¬i*§¢f?
The drier No.56 provideefor this operaticnzgis a counter-
~ y . _ ,I:.__._- ____J__-P :-
-. ,. _ _.__ :.. ,3
P coils, is drained through the drier in one direction and edipic
 _ _. , .. . y,acid is fed in at the other end. _ .    -
b  Dry refined Adipic acid crystals are discharged
the other end. &#39;
&#39; Thedrier is or sufficient capacity to handle a twenty?
__  ,  : .- 2.:-L.-.&#39;_-.1. st eel-
 &#39;- - -1  -&#39;92-...-....I "&#39;performance -or drier and rats oi throughput smst be sdjusted_.b§
&#39; * -- &#39;- * 1 -  .3 "i 
l
irf ~I d V _ _ &#39;  &#39; " :&#39; 4, _-,_&#39;  V &#39; - ~ _.=;_:. __,_i&#39;..:i-;&#39;;92§,"&#39;:¢_-nig£::1:_j_é;l&#39;:u-_92._
, . - -."»~*u»-.. .-.,. ¬ 
g-&#39;0. Recovery Kvapoator: . , .  ._  - &#39;92 1&#39;... -» .  . &#39; -_,.,.
.current rotary drier. Air heated -to 140 C. by passing over steam
tourihour mks of refined wet crystals in sex hours. The actus.1~-._=--3
I
-2* .1.  -
 .. -..é:-;;.~1.-e =~_t<.j. .-=--.1-L-",.":. 92   &#39;  &#39;- &#39; &#39; _   &#39; i V . &#39;  N  &#39; .: | _ _ - 1 __-92- w ~ - a - - - 1. . , __ -." " ; - &#39; 3. " .;&#39;* &#39;
The portion oi water mother liquor in No.54 tank &#39;
Ihiohis not needed for dissolving crude adipic acid is pimped J!
. 3.1. , .  -..;~ ,- -P - . &#39; ~i&#39;u &#39; &#39; -_ - 1. - Lto recovery evaporator Iio.6O. __  -.  I ._ .~_  &#39; &#39;1:-.~= ,+.~.-3~=_-...i_ -
_ ;..- _ __._.._ ..___ .. 2,.» .-_-.¢-&#39;.-- ~_..,- --- -~ "&#39;-- - -&#39;"&#39; "1-!""&#39; &#39; *- :"""":-&#39;" *--" "&#39;r--f-&#39;:_" -"""""- _ ."""*""&#39; &#39;-"-&#39;- . ;- "1   "
I - &#39; &#39; l  &#39; t &#39;. -* e _-:. I. &#39;- .
_kI92

u
r-... _- __ _. n  Q h __ __. ___ _,._..... To-; -_-....-  ..1
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.., n.__.._, 4.. _ -.92. ... - -
? ..
-- 1
P-3&#39;:--IT .,
.&#39;-L - 7&#39;1.-,4... -1-_ _
n&#39;-.s.- .-Q. .-..._ A. . I
!]ga..-&#39;v.:--- -.92-.v- .1" V - .&#39;.-.1-.r ,. -I-.;;_-.2 -r. --
.
Rib,_, ..
.-.._92_ .-.:;__ . _- .
e... . -_:5.-.-&#39;._. _
.7eE=" &#39;,. ,. .1...» ..
:,.__r_ ._,_ _
:s&#39;..; ._". &#39;-, , _: ._ , _ ., -r , -,_.._ ;.. ._. -._ ."92_,92 ...~;_ __; .~ " . . -   _ 1.9. .;-._&#39;_. P &#39;5" &#39; &#39;2-&#39;:"1"":";._..".92-*&#39;*&#39;.. ._...
-= .  .. - - .  &#39; ". .  _ , .4» _ .  . -- .-.&#39; 1 I . ~ -
- , - .  &#39; _ &#39;_ .~ -_&#39; . ....-.-, ~--_, , - ¢__w g _- ., -. &#39;» ,_ . - ._ ..- _. . -- - 92  ~ -. }o- .- .-., - . i. r... - - 3&#39; .__
fhehawstet and acetic acid are &#39;_eva&#39;porsted to  ~
through the vent. The eitent to which the evsporationis carried ,..- -F"-5-T I;-T-" - - &#39; - &#39; ~-   &#39;*  &#39;      " 1 "-::"&#39;-"_""** ;&#39;*:.:i-%--f&#39;-E:¢&#39;:-:&#39;T -&#39;:-"2- -should be determined by cooling a sample oi hot liquor  .I_1012{:I1§. :.A.___T_, J? , . . . , ._ _.-_.--&#39; ,;&#39;g.:§§.E_,,i.._."_.&#39;_92:,
the crystallization occurs at 20 to.25 C. , the evaporation ;is.~.3:;- -;
stopped and the hot liquor disc ged through s heated 3.ine_,*to;;§i>_&#39;~;f5;_.. T _._ ._,§_|...:_..-e erystalliser Ho. 30. The erysta isationend centrifuging  __&#39; &#39; - - &#39;: ."~ &#39;:r.=L&#39;3..&#39;..&#39; " - - - 1 &#39;~ -_ - ~ ~ 92  - ~ . -.-. -. -. .- g. - -W... -1 -.1...-. .__~.-._~-:1&#39;q,yv:§?l.=_. ..4 . - 1- -dbl in 11.11.» i. ~31- I&#39;¢=°"1°f1 551?!-0 edid is the s me as in Part B. above -...kl _. . - . _ &#39;7&#39;-&#39;-I -"&#39; ~- 4 ---- ~_ . . .,  _.._._. ,:. . .___... ;___ _ _ __ .&#39;- _  . - . &#39; ~ _ --;-  _-_-92-, -;|- -~.:-2-3;-__ ~: 
M=a1r1=1==1 Pr<><=~dw-==  -. i-  F  ,. .~.f-.LL¥.{
-. The pure adipic acid can be analyzed by dissolving- - - - .. -- -  ;-~&#39;.&#39;-s.-- ~. _ _ ,_ I4! ,__".-.-1.E-&#39;-:»|_» .- _.- . . 7 -_ , - .--,..
§.- 
._  92_
1-. -
.
1-E"»I=?8;.
:-.".-"-- - . ...:1 < vi--&#39; 1_&#39;E.~r&#39;fT&#39;t-
- -»_.. I} 0. .._ ..>15-.-.&#39; J -..+. .q¢..;.-. L3:5 . _
. . - -
kl-: _.;*l&#39; I A - .-
::i - -
=i*?"j- -f
s-ii~&#39;1:1s_.1 . .. >-!!&#39;g..--I. _ #-.J&#39;:.. , 4 -&#39;
vu __ |
>- - _._
an v ,# _rs--"."&#39; &#39;-,5_.,,..,_ ,.-.5,, .
0
.1- -u._,
5_l&#39;n-;&#39;r,.- -- .- .
.1 _.
. .- . 2 , .:=,.»?-1.1:. . &#39;s-,.:a:.?._..-.
- 4
-1a 1000 gram sample in methanol and tetrating with 0.511 caustio""&#39;i1&#39;- Q = - &#39; -&#39;_"&#39;__&#39;__.  A  3-1 5-T.-..::--._.*"~I&#39;._",*__§.5,f§_-T->-.7"-i-&#39;
in methanol solution to the phenol-phthalein end-point.?=*=5§*i:&#39;;j:=i;;" - . _.-i.-.. _ . ..;...__  :.:. -&#39; &#39; 5 Adipio acid equals cc. 1! base .ovs 100 -_ .-;:._;._.;___. .  . . ii 7 7 7 7 i 7 _ i _ 4  _<-=&#39;   _?~: .,3Z__ ; &#39;-
 . &#39; - Il1=- sample j 1&#39; ."i :j::.&#39;r.  -.=.*= --EL *~_ - .   ._..-:_.;_*_&#39;_: - L-
tor each determination. " - - __ -. » .__;..:_h_.;__A._:-,__.;é._..,,kg
I Part £5 . ligcoveryot Acetic acid
andildipie -ia
cid .._-f
the Purge Liquor. &#39;7 .  . l
 . " _: 4; , . r .&#39; V &#39; .&#39; &#39; ~ .; &#39;-&#39; -g A .- --ID, I &#39;7»: ;_..: _L..&#39;. nOutline of Process: __ r -  "_  jr_",_"i;*":".-&#39;."-17" "&#39;»- I -~ .1:~&#39;,~&#39;-. ., - V - _ - . -- - .~ s .1 ;- - 9 -_»-._._..n-I-5;: ... 4.- . 1.; -Y. .v&#39; Lactone acids are formed as by-products in the &#39;liquid____
phase oxidation. these are soluble in the solvent"mediu"i,92..J I  . .. .._ .- . ~-. .&#39; ~:...*&#39;- .. . ..- .-__&#39; -are purged from the system to prevent building up. &#39;1&#39;he_part-or l - _»..
. I-5 &#39; . -.92*..~ . - - &#39; 41. ~
&#39;- _ . . . . .|_-- - . .. . ..--. .= .-..- l _, . -4 , _-. .-.-._.,-1....: recovery still. dcetic acid and ketone are recovered at &#39;the_;;+&#39;.- &#39;_ _ _ _ ,&#39;._ ..  _ _ _. _ ,._&#39; &#39;...;.-_.
f§§;.."§&#39;-  ,  Jshead of the Lstill. Laetone acids are removed lhen adipic iscid?"_;_.-&#39;j;1".i";ZT&#39;i
. | >.
. ».<,.. -"...&#39; &#39;
-.a_|
1 -.&#39;- --&#39;,-1 -I&#39;,&#39;,&#39;-"""-g :5 vT~{ z
~"-~--.&#39;*. -:. 3". ~- "-".ts;f.~"-&#39;* 1&#39; *-3 ~ ~ s 
|:_ I ..:-. . - , ,. - 3 --1"-8; ...&#39; ..-13  . . .. . ,--  . 1 -- ::....~-1..-~ -. .L- 1&#39; "&#39; " " - - &#39; 4.-. ~4-1:- -&#39; -&#39;»&#39;*~r .-. &#39;. .&#39; 1 *r vi, -. 4 -. _ 3--5:: ft,-.¢92:.i..» - H  :1; centrifuged from the: residue 1 quor.   {J-_;&#39; __-___.-;_.;_~__A; ._-.._s~&#39;~.
V.  2  A flow diagram is attached, figure B.»  -  :j.§.-.-.-__~_.._--_._&#39;--_j,;._*f.j.;__.1 . ._ .  &#39;. _ , . &#39; . _ . .&#39;-.:- - - _,.-,.-=__"...,&#39;;_&#39; .~......&#39;~_ _"&#39;__. - . _ * -~92, &#39; _ _. 5 &#39; . "- . &#39; &#39; . a .. r92, . J... 2- : - __ z _ . 1 u &#39;- .,. -.. ... &#39; - >1 ._. . . .4 I . 92_. » . . 1- - 1. .. _. &#39; I¢" &#39;-4"--&#39; 4. --.-- -1 - r- -" 92 &#39; .  ..- . . . -. _ . .. .. 1 .1 . M . ._- ,... . ,.  > - . ._ ._4._..&#39;_. - _ . _ . 1-&#39; . - , .. - - .- ._, 1. v .._~ _ _ _ ~_ ,h_ ,_.v _ _&#39;__, _i. &#39; , . _ _.1 ., .,.,. 4&#39;- _ -IA. -. _ _ ,- .. _ . . _..... _. .1 ......-.... .. .4» Q. .....,~.-....A_..._. ..-. .. - -. - . -.,- . ._ --.., , __ _4,._._..,,§,, -- _ .....H. . -., - 92 - -. 4 1 -2-
"&#39; ..- -. _,-.. ...< .-. r ,_ -|- &#39; .. - : » -._&#39; __&#39;,.._ . . .92_ ." t .. _ ,.. ._p_ &#39;~.&#39; ;_... .1.-. {E __ -- ._&#39; _ 1 92- _ ___J 1- 3 I v I _+_-  92___,_ rt.-
_, , 0- J &#39;-| ,~-. .r_"~-:&#39; _, -»- -ug" - -.- -.- _ . _.. :,lAI- .. "..:. &#39;-- -&#39;- &#39;--" &#39;..- -  " - ~-;~T " -&#39;: 151- .3-Y  1"-.-=*.&#39;>» r" &#39;- ..&#39;!w -s 1.!-r&#39;.":.-L .. "-&#39;"__._r ... .... _ .. ._ - ...._. .__,,__., P7... . _ .,_-- ._.. ,-,....._..,,_:.;_,T_V ,._,..., ,,..,__-&#39; -..&#39; ..._ - &#39; 4.:»-A»-_. -..... ..|...--&#39;..¢--e---l-A-_ -.- -- -  a:_; I .._-.1. L:- ., --- - - r -- ~ ~ -&#39; -1" -- ;- ¢ &#39;..-J22 - . &#39;--. P&#39;_a-Fl -. &#39;_ r..- J1 :-Q-off?» &#39;-&#39;0-&#39;  -. - -. -    .  :=.~».: -*:1-* . -&#39;" I  .&#39;- -&#39; 1 - - &#39;-1:; 920&#39;1", ~-I -r *" .+_-1 .§,.. -.-.~ 1... -_ Y! _ 1-A-.v_!:"&#39;:-:5 1 u-;;-_,..u-- -v _§1"r;-&#39; r . -.. i v _ ... _ *4 - L u Y&#39;92Y 1-
A tjtration of-.=thc base against }.5  should be run"
acid notherfliquor which is not rgycled is charged to the _scid__.-=__-;.K

*1
.
"F""&#39;I" §&#39;?.&#39;I&#39;FT$""T"""9F&#39; 1"- &#39; 8l92"&#39;-5&#39;r&#39;  Z,-1&#39;3 - &#39;; "1 t -  I      ;_§.-&#39;_;f.=jI.&#39;   0" &#39; Operating Pro :-ure: &#39;  _ _ "I  -- &#39;   L  _ W
F92.
s!-,.. . n*f *j§@§i*.¢=w- g &#39; -~ "-
&#39; ---- ~ 1 - ~ -A - -..-----. -.-.,.__ _ _ _ . ._ _ _,¢@_d;__.__@.*~__-1:a-n;4u1m-i.;____@__J_i.__¢.4~A-a.@»a*__~» .-_L-__. .92...-.5..- L--: __.. . . - &#39; " ~ -  - - &#39; .. . &#39;." . ~ . *_,.-r ¢- .
-
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&#39; A. Acid 3iRecovery Still. &#39;_  7 &#39; -    - - _. I _ - ~;..:r...- - -  V  __ _ __ _ ,_|1 &#39; -1;. - ~_ _ - ---_-. __. -,_.__:_.-a .|-- .
_;..-;-.~_.:_._- " - 1- 9118-1&#39;59 acid recovery etill kettle Io.§5-_-_A
-apaprcizimately one inch from the top of the eight 31...
acid mother 1iquor_from No.32 tank. &#39; .5--..;~ i§i;§aqg;~;c
2. Turn rater on condenser No.53-G. ."-&#39; _ .. -.  &#39;1 :55" -&#39;
- .&#39;.1~-.92_
- 8. Turn steam on coils to lIo.33A. The full eteam
flow may be applied intiw the baee of the column begine to warn
up. Then reduce eteam flow to about 100 pounds per. hour and -_
&#39; 1
establish reflux. - - _ _  ___ _ _ _
. " 1. Turn steam on tracer to discharge line lio.33A " "
&#39;  t._ .,
to hold-up tank No.54 and heating coil in Ho.34. Leave heat o I;
this system at all times unless completely drained. M " &#39; 
- 5. - The following cute are made: if _    .--~* ~
A. Ketone, water cut at 5:,1 reflux ratio to .}.{
ketone water layer storage lio.6_  approx. 4 gale.! _   "
6. B. Weak acid cut at 1011 refluat ratio. This
is drained 1rom_the receiver to a oarboy to be discarded;  _  ~
 app:-ox15 gal! u &#39; -A " &#39;  A
C, Btrong acid out at 1:1 reflux ratio to --1. - &#39;
receivers 33-E and 53-F and then dropped to pure acetic acid 
etorage No.13  a&#39;pprox.l56 gals.! _   _
D. the residue ie diecharged to No.34 hold-up - _
tankdaprox. 34 gale! -  M "  &#39;1  &#39;
1 1 v ._ 6. Ihen the required strong acid has been removed
|92 _.- no. _. -5-~.-.4 ..-W. Ywf;.@@ er: steam and discharge not residue to No.54 eanx._;;§%;;;.
ue.ss.c. cauei§H{if §-24. ..-:._, . - _».- -H _&#39;=- .: -_.__u&#39;-- -
Leave small flow oi rater on this condenser in freezing weather &#39;
. &#39;_-A _ -
or drained °°mp1,g;,1y!_ Since acetic acid freezes; at 160. care .
- &#39; c*;&#39;:7-1:"-m-3 :.-1&#39;.-e&#39;~o.1,q _;a .»2:>sP.:;¬=;:1g .
must be taken to avoid plugging the oondeneer and draw-ctr linee.
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&#39;- . &#39;7 . Turn water oft condenser
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lines should be completely drained during shut-downs when&#39;the;§;
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-
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