I
C.
H.
STOCKMAN and R. E.
LYNN, Jr.
Research Center, 6. F. Goodrich
Co., Brecksville, Ohio
8
Equipment for Miniature Pilot Plants Is Available
Om
THE MOST important operations in miniature pilot plants is the pumping of liquids. Low volume streams can be pumped with the proportioning pumps manufactured by Propcktioneers and Milton Roy, but these are somewhat large and cumbersome for miniature pilot plants. HOWever, many small pumps are available, some of which have no packing glands or stuffing boxes.
Flowmeters
Measurement of fluid streams is important in most pilot plant operations and for clear liquids and gases, rotameters are convenient. When the fluid properties are known, calibrations can be calculated for the Tri-Flat rotameters recently developed by the Fischer and Porter Corp. A kit containing several of these rotameters o f ' different sizes is available for about $100. Rotameters are also manufactured by Brooks Rotameter Go., Lansville, Pa., and by Schutte and Koerting, Cornwells Heights, Pa. Distillation Equipment
Packed columns, vacuum-jacketed and silvered-glass, are usually used for distillation on the miniature pilot-plant scale. Useful packing includes l/c-inch ptrcelain Berl saddles available from U. S. Stoneware Co. in Akron, Ohio, Fenske single-turn helices in stainless steel or glass from Scientific Development Co., State College, Pa., and Cannon stainless-steel protruded packing, also available from Scientific Development Co. The still pots used with these columns are usually glass flasks containing thermocouple or thermometer wells. They are heated electrically with heating mantles controlled by autotransformers such as the Variac or Powerstat. The reflux ratio can be controlled by any of several reflux dividing heads available from the laboratory glassware supply houses. These are usually magnetic devices which operate with intermittent take-off. The reflux ratio is set and controlled by repeat cycle timers such as the Eagle Flexipulse timer available from the Eagle Signal Co., Moline, Ill. The vacuum-jacketed and silvered columns are available from many laboratory supply houses at prices ranging from
about $60 to $120. The magnetic reflux dividers cost about $40 to $100 and timers cost about $100 apiece. The vacuum-jacketed and silvered columns are available in standard sizes up to about 37 mm. in internal diameter and heating mantles and glass still pots are available in sizes up to 12 liters. Complete laboratory distillation units are available from Podbielniak in Chicago and from Fisher Scientific Co. A complete Fisher unitized distillation assembly containing three columns, four sizes of still pots, and all necessary items such as reflux dividers, product collectors, and timers to carry out two simultaneous distillations costs $2680. Prices of Podbielniak distillation units start at about $1700. For slightly larger operations, 2-gallon glassed-steel kettles along with. glassedsteel columns and condensers are available from Pfaudler and from Glasscote in models usable at pressures up to 150 p.s.i. For kmaller scale distillations at pressures substantially above atmospheric, the column may be constructed of pipe and a solenoid valve used as a reflux divider. The still pot may be a pipe, or it may be constructed of an army-surplus oxygen container of the type available from several surplus houses, some of which advertise regularly in Chemical and Engineering News.
large for miniature pilot plants. A much smaller machine is the Eriez Hi-Vi manufactured by the Eriez Mfg. Co., Erie, Pa. This is a small vibratory feeder which can feed from 0 to 500 lb. per hour and which can be supplied with a variety of feeder trays. Reactors
Occasionally in miniature pilot plant work it is desirable to see what is happening inside a reactor operating at a pressure substantially above atmospheric. The Sutherland glass reactor is available for this purpose (7). Piping
In miniature pilot plants it is frequently necessary to connect glassware to piping. For this purpose both spherical joints and taper joints may be purchased in stainless steel, Monel, or brass. They are available from Ace Glass or Kontes glass, both in Vineland, N. J., at from $7 to $60 a unit depending on size and material. The nylon Zytel fitting made by the Jaco Manufacturing Co. of Cleveland, Ohio, may also be used to connect glass tubing to metal tubing. Also, borosilicate glass pipe is available in '/d-inch size. High-pressure Equipment
Extraction
For solvent extraction work packed columns similar to those used for distillation are applicable. In general, these need not be vacuum-jacketed and silvered. Interface control for liquidliquid extraction in packed glass columns may be by means of a balance leg or an electromechanical device such as the Thermocap capacitance relay available from Niagara Electron Laboratories, Andover, N. Y. The sensing element of this relay is actuated by changes in the interface level, and the relay controls a solenoid valve.
Extensive lines of small-scale highpressure equipment are available from American Instrument Co., Silver Spring, Md., Autoclave Engineers, Erie, Pa., Pressure Products Industries, Hatboro, Pa., and High Pressure Equipment Co., Erie, Pa. A top-stirred high-pressure autoclave of l-liter capacity costing about $1500 and obtained from High Pressure Equipment Co. is illustrated along with a high-pressure pilot plant for reacting a gas and a liquid, which is enclosed in a reinforced concrete bunker. This particular unit was purchased from Autoclave Engineers for about $20,000.
Powder Feeders
Feeding powders on a small scale is frequently difficult. The Omega Powder Feeder manufactured by the Omega Machine Co., Providence, R. I., works well although the machine is rather
literature Cited (1) Sutherland, J. D., McKenzie, J. P., IND.END.CHEM.48, 17-19 (1956).
Received for review December 4, 1957 Accepted December 9, 1957
See following pages for Equipment lists and illustrations VOL. 50, NO. 4
APRIL 1958
585
Here Is Some of the Equipment Available Manufacturer
Item, Type
Price, Material
Description
Pumps Minipump
Carpenter 20, $270
3-3200 ml. clear liquid/hr. ; 1000 p.s.i.
Constametric Minipump
$1010
Continuous discharge ; 2 liquid ends with common suction and discharge manifolds; driven by cams 180a out of phase
cow on-Cerveny
Microbellows
Smallest model, 15750 ml./hr.; stainless steel, $129
Models to deliver 15-6000 rnl./hr. ; no packing glands or stuffing boxes; bellows and check valves may b e surrounded by heating jacket; stainless steel, Monel, glass, or Teflon
Lapp Insulator Co., New York, N. Y.
Microflow Pulsafeeder
Carpenter 20 stainless steel, Kel-F diaphragm, motor,
0-0.395 ml./stroke normally at 44 strokes/min. ; liquid driven
Milton Roy Co., Philadelphia, Pa.
by diaphragm actuated by piston in oil; without packing glands or stuffing boxes
$295
Sigmamotor Inc., Middleport, N. Y.
Sigmamotor
Technicon Chromatography Chauncey, N. Y.
Technicon
Corp.,
Eco Engineering Co., Newark, N. J.
Vanton Pump and Equipment Corp., New York, N. Y.
Without motor and variable speed drive, $60
.....
Propel liquids by squeezing flexible tube of rubber, Tygon, or other material; tube dia. or speed of pump varies delivery rates Similar to Sigmamotor
Eco All Chem Housing, Carpenter rotary 20; $185 displacement
31/2 gal./min.; impeller, neoprene, Hypalon, Teflon, or phenolic
Eco Minilab rotary
Carpenter 20
0.05-1.5
Vanton Flexiliner
Body of stainless steel or several plastics,
'/3-20 gal./min.; clear liquids and slurries compatible with rubber liner
resin gal./min.; impeller, carbon or Teflon
$35-395
Jabsco Pump Co., Burbank, Calif.
Jabsco
Models from $12.75 to $275
Smallest model, 0.7 gal./min. at 500 r.p.m.; clear liquids and slurries ; neoprene impeller; bronze or stainless steel housing
Robbins and Myers Inc., Springfield, Ohio
Moyno
Glass, $225 ; stainless steel, $325
Slurries and clear liquids; nonpulsating flow; valveless, positive displacement; helical screw rotor turns in stator with double internal helical thread
% Proportioneers, Inc. %,
Microfeeder
With variable speed drive, $1500
0.1-10 ml./min. ; 200 p.s.i. ; high accuracy; hypodermic syringe principle ; cylinder capacity, 800 ml.
$700; drive gears, $5 1 pr .
Capacity, 100 ml. ; constant speed drive ; delivery rate controlled by changing drive gears; feed rates, 1.67-22 ml./hr.
Providence, R. I.
Hills-McCanna Co., Chicago 18, Ill.
McCannameter
Distillers Co., Ltd., Great Burgh, Epsom, Surrey, England
Micro pumps
Ruska Instrument Corp., Houston, Tex.
..... Stainless steel, $125 UP
M pump Volumetric proportioning
. . . . e
..,..
Similar to Microfeeder;
0-0.82 gal./hr.
Sizes from 7 to 1500 ml./hr.; flow rate varied by micrometer adjustment of plunger stroke; press., a few p.s.i. 2400 p.s.i.; in sizes having max. capacities, 0.16-8.23
gal./hr. Cylinder vol., 100-1000 cc., press., 4000-50,000 p.s.i. ; stainless steel lab. valves and fittings for 25,000 p.s.i.
Flowmeters Potter Aeronautical Corp., Union, N. J. Minneapolis-Honeywell Regulator Co., Minneapolis, Minn. American Meter Co., Inc., Philadelphia, Pa. Precision Scientific Co., Chicago, Ill. American Meter Co., Inc., Philadelphia, Pa.
...
... ..
Stainless steel $475$2000
Liq. flow, 0.08-5200 gal./min.; gas flow, 5 ft./sec. to sonic; sizes, l / g 8 in.; turbine-type rotor floating in axial position i n steam; indicates both rate and integrated flow
Stainless steel $130
Wet test meters for integrated flow of gases not highly corrosive or soluble
$80
Dry gas meters for integrated flow of noncorrosive gases ; accuracy, 2% ; bellows type ; models suitable for benchscale work have larger observation dials reading 0.1 or 1 cu. ft./rev.
Extraction Equipment Allis-Chalmers Mfg. Co., Milwaukee, Wis.
Liquid-solid, continuous
With glass column ; Total submergence, countercurrent; 3-in. dia. col. contains metal parts of Type several plates with hole and scraper; solids fall through liquid; continuous drag drains and discharges solids from 316 stainless steel, $2475 bottom of col. (Continued on page 590)
586
INDUSTRIAL AND ENGINEERING CHEMISTRY
Wet test and (above)
dry
gas meters
Distillation apparatus (right)
VOL. 50,
NO. 4
0
APRIL 1958
587
An Eriez Hi-Vi feeder can handle 0 to 500 pounds of powder per hour /
/
In the Allis-Chalmers extractor, solids fall through the liquid
The Tolhurst laboratory centrifuge i s compact and develops forces up to 750 times gravity
The Sparkler filter has a filtering area of 1 square foot and a cake capacity of 0.073 cubic foot
588
INDUSTRIAL AND ENGINEERING CHEMISTRY
Niagara laboratory filter. Leaves are covered with filter cloths of stainless steel, cotton, nylon, Vinyon, saran, glass, or wool
With the Sutherland reactor, what happens inside the reactor can be seen
Speed of the Fawcett air-driven mixer can b e varied from 0 to 2000 r.p.m.
Typical miniature pilot plant made from metal and glass (above)
This BakerAPerkins Sigma-blade mixer i s useful for high viscosity liquids, Here, a rubber composition i s being mixed
Top stirred high pressure autoclave (right)
For reactions of gas and liquid at high pressure. Right, the controls outside the bunker
Above, the pilot plant.
VOL. 50, NO. 4
APRIL 1958
589
Here Is Some of the Equipment Available (Continued) Manufacturer
Item, Type
Price, Material
Description
Extraction Equipment (Continued) The Gas Machinery Co., Cleveland, Ohio
Liquid- or solid-liquid
Turbo-Mixer Div., General American Transport Corp., Chicago 90, Ill.
R.D.C. Column
Podbielniak Inc., Chicago, Ill.
Centrifugal
.....
.....
Vertical, multistage, mix and settle ; continuous counter-current (Donahue) 6.0 X 8.0 in. col. ; other equipment built to specification
With 2 8-gal. feed tanks and table, $4500
Holdup, 65 ml.; separation equivalent to 8-12 theoretical stages; cap. to 500 ml./min. for combined streams
Centrifuges Tolhurst Centrifugals, East Moline, Ill. Bird Machine Co., South Walpole, Mass.
...
...
Stainless steel, $1650 Basket type; 12-in. center slung; force, to 750 X gravity; cake thickness, l 7 / 8 in. ; ring cap., 290 cu. in. ; total cap., 5 5 1 cu. in.
.....
12-in. basket type; interchangeable solid and perforated baskets
Filters American Machine & Metals, Inc., Niagara Filter Div., East Moline, Ill. Sparkler Mfg. Co., Mundelein, Wis.
...
...
Stainless steel, $500; with borosilicate glass cylinder, $535
Vertical pressure-leaf-type ; 7-in. dia. tank cylinder; 3 type 316 stainless steel leaves provide 100-sq.-in.-filter a r e a ; cake cap., 62.5 cu. in.; press., 50 p.s.i. with glass shell or 100 p.s.i. with stainless steel
Type 304 stainless Horizontal plate; filter area, 1 sq. ft.; cake cap., 0.073 cu. ft.; i n steel, $1000 carbon steel, rubber-lined carbon steel, and all grades of stainless steel, pure nickel, Monel, or bronze
Reactors Sutherland Reactors, Baton Rouge, La.
Marco Development Co., Wilmington, Del.
Girdler Process Equipment Division, Louisville, Ky.
...
e . .
...
Explosion proof light-bulb protection globe ; metal parts, stainWith agitator and drive, cooling or less steel; press., 200 p.s.i. heating coils, 1/2 gal., $525; 1-gal., $785 Continuous, $6800
Several chambers each containing 2 impellers and baffie disk. Over-all heat transfer coefficient for water, 350 B.t.u./hr./ sq. ft./O F. and surface, 165 sq. in.; holdup, 0.2 gal.; normal flow, 0.05-50 gal./hr.; temp., 650' F.; press,, 1000 p.s.i.
Votator, continuous, stainless steel; $3000
Material processed in annular space between heat transfer surface and mutator shaft carrying scraper blades; over-all heat transfer coefficients for thin liquids, 400-700 B.t.u./hr./sq. f t . / O F. ; for viscous liquids, 15,000-50,000 cp., 100-200; temp., 15O0-7OO0 F.; press., 500 p.s.i.; heat transfer surface, 0.7 sq. ft.
Mixers M. F. Fawcett Co., Macedonia, Ohio
Mixing Equipment Co., Inc., Rochester, N. Y. Ace Glass Inc., Vineland, N.J. Baker, Perkins Inc., Saginaw, Mich.
Atlantic Research Corp., Alexandria, Va.
590
...
... ... ...
...
INDUSTRIAL AND ENGINEERING CHEMISTRY
Air-driven, hp., $55; 12-in. stainless steel shaft, $1.90; 3-in. dia. stainless steel impeller, $3.75 . . . e .
Ace Trubore, $18
Speed, 0-2000 r.p.m. ; press, 30-90 p.s.i. ; '/a, I / * , and '/z hp. ; Jacobs chucks fit l/s-in. shafts; rods for mounting on vertical rod with standard clamp
Complete line of mounted and portable mixers and impellers Usable in flasks under vacuum with any suitable drive unit
Sigma-blade, stainless For very viscous materials; model sizes, 2 cu. in. up; jacket for steel ; 6 cu. in., heating and cooling; may be sealed for operation under $1400 vacuum or controlled atmospheres V-blade ; somewhat more expensive than similar mixers
Similar to Sigma-blade mixer ; disassembled readily for cleaning
