Document a47aBjnNpB7314bEwv9oGmzX
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DATE___ js2jL_lj-f_.lg.2i------------TEST CONCLUSION NO. TA-C- 7 2-261
OrrtClAL PRODUCT NAME 2-Chloro-4-Nitroaniline (OCPNA) PRODUCT CODE NO. 14? 1 60,POUNDS PRODUCT ACTUAL . AP.prqg,,.,,5C0-----------------------------------------------------a r e a "Ponsol"______________________________b u il d in g n a me Bldg. 743 - "Ponsol" Dryer Mo,__2
t it i e Spray Drying Feasibility___________________________
------------------------------------------------------7t t 7-------------------------------;----------'----------------PREPARED r v : R. C. Frankiin, A. C. Stein:-------------------------------------------------------------------------------------------
PURPOSE OF TEST: To demonstrate the feasibility of spray drying OCPNA wet cake
in the new Proctor & Schwartz dryer. A Whirlpool hopper will be used to
prepare the feed slurry since TA-C-70-901 was unsuccessful due to poor homogenization of the feed slurry and subsequent plugging of piping and
nozzles. RESULTS OF TEST: spray drying of OCPNA (Chg. 1) was carried out in the Proctor
& Schwartz dryer using an internal mix P&S paste nozzle in April,1972,according to the procedures of this TA. Slurries prepared in the Whirlpool hopper were pumped satisfactorily to the dryer, but problems were encountered with some plastering on the walls and build-up at the discharge valve. About 500 lb., of marginal quality OCPNA was collected before discontinuing the experiment. Attempts to vary drying conditions were not successful in eliminating the problems.
Data on the feed slurry and product are attached.
*
RECOMMENDATIONS:
.
Carry out further studies on spray drying OCPNA in "Ponsol" Dryer No. 1, and with different types of nozzles in No. 2 (i.e., pressure, 2 fluid, 3 fluid).
DISTRIBUTIONS
F. Laucius
F. Stalzer
^ ' ----
J. Slentz-- R. J. Pohl ' '
H. Terss
Jackson Lab. Files Co H. Lake T. E. Lewis
M. S. Moores
J. A. Moffett
D. 0. Miller (3) G. L. Porter
D. Putnam (3) R. C. Franklin A. C. Stein J. J. Meyer M. L. Reinhart
TC-C-72-261
OCPNA Slurry from Whirlpool Hopper Solids - 22% Wet screen tests - 0.45%* retained on 20 mesh - 1.14%* retained on 40 mesh
* Based on 100% OCPNA.
Product collected (approx. 500 lb.)
Appearance - brownish yellow powder (normally bright yellow).
Moisture - nil
Freezing point - 107'. 0C (Specif. 106.8C)
Purity
- 99.8% (Spec. 99.0%)
Diazo insolubles - 1.14% vs. 0.58% on a control sample.
Material Collected from Walls Appearance - reddish brown, slightly tacky Moisture - nil Freezing point - 107.0C Purity - 99.1% Diazo insolubles - not determined because of tackiness.
7/15/74 /grg
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FOR COMPANY USE ONLY
Ptk P'1
DATE------- Apr J-1 3 r--1.9,? 2..^
d TEST AUTHORIZATION NO. TA-C. 72-261
OFFICIAL PRODUCT NAME_______2-Chloro-4-nitroaniline--(OCP.NA).,
PRODUCT CODE NO142 160POUNDS PRODUCT PROPOSED UP to 5,000 _lbs .
ar ea
" Ponsol11_______________________ BUILDING ma mf Bldg.743 - "Ponsol" Dryer No.2
TITLE Spray drying feasibility.
PREPARED BY:
L. C. Hale d^Cfj--
RESPONSIBLE FOR TEST AND TEST CONCLUSION:__k
t
PURPOSE OF TEST: To demonstrate the feasibility of spray drying OCFNA wet cake in the new Proctor & Schwartz dryer. A Whirlpool hopper will be used to prepare the feed slurry since TA-C-70-901 was unsuccessful due to poor homo
genization of the feed slurry and subsequent plugging of piping and nozzles.
DURATION OF TEST:
One to three charges.
s t an d ar d in v o l v ed : ANALYTICAL CONTROL:
Chambers Works process for 2-Chloro-4-nitroaniline dated
May 23, 1966.
change
Change described under Test Details
TECHNICAL BASIS FOR CHANGE: TA-C-70-901 dated January 13, 1972.
TEST DETAILS: See attached. (Include Safety and Waste Disposal)
Safety; No unusual safety hazards are expected. Refer to TA-C-70-901 for dust explosion properties of OCPNA. No explosion hazard exists. o OCPNA is an aromatic amine that may cause cyanosis. Avoid contact with the skin or inhalation of the dust.
Waste Disposal; . 1. Dust Emission - A negligible amount of dry product (~ .004 Ib./lOO lb. of produced product) is expected to be released to the artiffosphere as a
yellow dust.
2. Liquid Wastes - Two streams are involved: (a) Dust scrubber liquor - This stream will contain approximately 0.4 lb. of OCPNA/100 lb. dry product produced + 3000 lbs. of water. (b) .Wash water used to clean tanks, dryer, dust collector. Whirlpool hopper, etc.
DISTRIBUTION:
J.Blackwell R.J.Pohl
A. ln/5:
R. C. Franklin.
J.Meyer )In
J. L. F i le s
J. F.Froning
C.J.Slentz)Turn
H.P.Landerl
R. T.Gilsdorf R.T,McNally)In .
A. S.Brookes,Jr. L. C.Hale
D.M.Dietz )Turn
J.E.Cole,Jr.(3) R. H.Kasch
D.O.Miller
J .H .DeYoung_________D. B.Kirk
J.A.Moffett________
APPROVED BY:
i'1' c?,! i.' ? Pa -ft
CHIEF SUPVR., OPERATIONS
i?
7*-
DATE
CH. SUPVR., TECH. OR PLT. ASSIST.
M. S.Moores G.L.Porter D.Putnam(3) R.B.Root R.F.Stalzer A.C.Stein
R.H.Terss
R.Wiederhorn
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dt^c. P*tr* t
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dat e
SUPERINTENDENT, ANALYTICAL (When Bequif-sd)
AUTHORIzm.BYp;
d- >L h*1 2 * * *
S.UPERINTepfpENTi MANUFACTURING, lOr Delegates)
DATE
SUPERINTENDENT, OYE DUALITY CON TROL (When Req'dl DATE /
j ///,^
v/v/}r ?
s u p e r in t e n d e n t ,nve Modernization /
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Page 2 TA-C-72-261 2-Chloro-4-nitroaniline (OCPNA)
Test Details:
1. The dryer feed slurry will be prepared in a Whirlpool hopper by Dye Modernization - Facilities personnel. Depending upon the solids content of the wet material, a sufficient quantity of water to produce a' 20-25% solids slurry should be added to the hopper. This will yield a slurry with a viscosity of -v 10,000 cp. The mass will be deagglomerated by high pressure drop (~ 80 psig) pumping across a valve such that 100% of the slurry will pass through a 20 mesh screen.
2. The OCPNA slurry will be pumped from the hopper by a Moyno
pump and be fed through a 15 mesh riddle.
j
Note:
This riddle will be unnecessary when a dis integration system is available. Its primary purpose is to screen tramp material and agglomerates.
3. Spray dry the charge in D-10 using the paste nozzle consisting of a 1" diameter slurry tube and a 1/2" nozzle diameter at the following initial conditions:
Steam pressure = 70 psig
_ ,.
... / lb.steam/hr. 'N
nn
Ratio setting (2 gpm'siurry FlO'V = '9
Outlet temperature = 175F. (80C.) FN-11 damper setting = 50%
A satisfactory product {> 99% purity, < 0.1% moisture) was obtained in the Azo dryer under TA-C-70-901 at 482F . (250C .) inlet and0^5F. (80C.) outlet tempera
tures.
4. "Adjust the outlet temperatures to maintain product moisture below 0.5%.
Any of the initial conditions should be adjusted at the discretion of spray dryer supervision.
5. Send a one-pint composite sample of each 10 drums or of each significant change in drying conditions to G.A.L. for determina tion of product moisture, purity and freezing point. Label samples "TOXIC". Send a similar sampia_.tp R. C. Franklin, Azo Laboratory for evaluation of diazotization properties.6 *
6. Toward the last hour of the run, rinse the feed tank walls with water and dry the resultant dilute slurry.
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Page 3 TA-C-72-261 2-Chloro-4-nitroaniline (QCPNA)
7. Clean and shut down the system per spray dryer supervision's instructions.
8. Weigh and label drums:
OCPNA Spray Dried TA-C-72-261 Toxic
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