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1. E. CRAIG and J. E. DEW Grand River Chemical Division, Deere and Co., Pryor, Okla.
Design for the Future
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A Small High Pressure-Preparations Laboratory What goes into a high pressure laboratory? Here is the story of what one company did to prepare for the future. There is much food for thought in their selection of what they needed, which can help you plot your course as well
PRESENT-DAY emphasis on adequate safety for personnel has resulted in provision of barricaded and isolated areas of some type a t almost all industrial chemical laboratories, regardless of size. T h e need for barricade protection is important in exploratory research a t elevated pressures; it is even important for chemical reactions that are fairly well known. No amount of instrumentation will eliminate all hazards as long as the human factor of operating personnel is involved. T h e need for isolated areas for experimentation and processing with toxic and noxious chemicals, particularly in rather large quantities, is also obvious. T h e Research Laboratories of the Grand River Chemical Division of Deere and Co. were installed in the main office building of the division about 5 years ago. Shortly after the start of experimental work, it became evident that both barricaded and isolated areas were needed. A building to provide both types of areas was designed and constructed. In deciding on the layout and details of construction for the High PressurePreparations Laboratory, numerous publications ( 7- 75) on high pressure laboratory design and operation were consulted. Visits were made to several high pressure laboratories. I t was decided to use what were felt to be the good features of the published designs and of the laboratories visited, with modifications based on personal preferences and results of conversations with operating personnel of these laboratories. The building was then designed with these thaughts in mind:
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ENGINEERING E EA STANDARDS
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GENERAL CONSTRUCTION SPECIFICATIONS
B-1-03
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GENERAL CONDITIONS BUILDING DESCRIPTION: The b u i l d i n g w i l l be one s t o r y and w i l l c o n s i s t o f l a b o r a t o r y room, f o u r t e s t c u b i c l e s , s t o r a g e room, equipment room, and s a n i t a r y f a c i l i t i e s . Foundation w i l l be r e i n f o r c e d c o n c r e t e . F l o o r w i l l b e a t r o w e l f i n i s h e d c o n c r e t e s l a b . E x t e r i o r w a l l s e x c e p t a t t e s t c u b i c l e s w i l l b e 8 i n c h l o a d b e a r i n g masonry w i t h b r i c k e x t e r i o r and S a n i - f i n i s h t i l e i n t e r i o r . B a r r i c a d e w a l l s o f t h e t e s t c u b i c l e s and s t o r a g e room w i l l b e sandwich c o n s t r u c t i o n w i t h s t r u c t u r a l s t e e l frame and wood s t u d s f a c e d on e x t e r i o r w i t h s t e e l p l a t e and on i n t e r i o r w i t h t i m b e r . Space between w i l l be s a n d f i l l e d . P r e s s u r e r e l i e f walls o f t h e t e s t c u b i c l e s and s t o r a g e room w i l l b e t r a n s i t e p a n e l s f a s t e n e d t o s t e e l frame. Roof w i l l be 20-year bonded b u i l t - u p on s t r u c t u r a l s t e e l . C e i l i n g s i n t h e l a b o r a t o r y a r e a and t o i l e t w i l l b e a c o u s t i c a l t i l e . C e i l i n g o f t e s t c u b i c l e s and s t o r a g e room w i l l b e same c o n s t r u c t i o n as walls e x c e p t t h a t t h e roof deck w i l l b e t h e e x t e r i o r f a c i n g and t h e s t e e l p l a t e w i l l be o m i t t e d . T h e r e w i l l b e no c e i l i n g i n t h e equipment room. B u i l d i n g w i l l be h e a t e d by steam. L a b o r a t o r y a r e a and t o i l e t w i l l be a i r c o n d i t i o n e d . Automatic s p r i n k l e r f i r e p r o t e c i t o n w i l l be provided f o r l a b o r a t o r y a r e a and t e s t c u b i c l e s . The f o l l o w i n g o f f s i t e u t i l i t y s e r v i c e l i n e s t o t h o b u i l d i n g w i l l be p r o v i d e d : 50 p s i g s t e a m . d o m e s t i c water. 100 p s i g a i r , t e l e p h o n e , 440 v o l t 3 p h a s e e l e c t r i c a l power. s a n i t a r y s e w e r , and s t o r m s e w e r . B u i l d i n g w i l l be l o c a t e d on Deere P l a n t S i t e a t P r y o r . Oklahoma.
Facilities should be provided for investigations at elevated pressures, investigations with toxic and noxious materials, and small scale preparation work. 0 The barricaded area should provide facilities for carrying out batch-type reactions in autoclaves of 1 liter and smaller. No work is planned with unusually hazardous or high-energy chemicals.
0 Barricades are to protect personnel and equipment from flying objects and debris, not from shock waves. 0 Instrumentation and utilities are to be installed in a manner easily adaptable to variety of investigations. @ T h e building is to be designed SO that it can be increased easily in size. The exterior of the building should conform architecturally to the other plant office buildings. VOL. 51, NO. 10 e
OCTOBER 1959
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Building location and layout
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-1OODI "B"
L A B AREA "E"
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FLOOR PLAN
HIGH PRESSURE LABORATORY
Floor plan of the high pressure-preparations laboratory. The heavy lines are barricade walls of steel-sand-wood sandwich-type construction
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O B S EP R OVRATT I O N BLOW OUT WALL
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VALVE OPERATORS
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E:> S E R V I C E
PIPING
T h e laboratory building is located a t the edge of the plant area, with the blowout wall of the high-pressure section on the side away from the plant. N o barrier has been placed behind this blowout ~vall; the area behind this building is an isolated and uninhabited arra. T h e building is constructed of hollow tile and brick. It is divided into t\vo general areas-a laboratory area and a high prtmurr, barricaded area. Ctilities are supplied from the t:quipment room to all areas by means of piping chases in the floor: Laboratory area A is primarily for use in catalyst preparation, charging and discharging of autoclaves, and processing of rractants or reaction products. Hood .A is the usual laboratorv bench-type hood. Laboratory area B is designed for larger scale preparation \vork. Hood B, a floor-to-ceiling hood, is designed so that electrical outlets and controls and valves for servicc piping are outside the hood. Holes through the walls allow for gases to be brought into the hood from cylinders just outside the building. Vents through the outside \vall make it possible to draw all outside air through the hood. FValk-in hood C provides a hoodrd area, 6 X 10 feet, for still larger scale experimental or preparation Lvork. This walk-in hood is designed so that it can be converted to another high pressure test cubicle by replacement of one door with barricade construction. At present it is equipped with a rack along one side and used for preparation work. T h e barricaded area consists of four test cubicles which are entered by going outside of the building through one of tWo corridors and into the cubicle from the back side. This was done to make it rather difficult to enter the cubicles; weather conditions at this location do not make entry from outside undesirable. Three of the cubicles are 6 X 10 feet in size) rhe fourth is 7 X 10 feet. The building was designed so that an addition could be made a t either end. T h e piping chase arrangement is such that utilities, which are brought into the building in the equipment room, can bc extended easily into an added building in the same manner.
Construction of Barricades
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I CUBICLE SECTION
HIGH PRESSURE LABOR AT ORY
Cross section of a typical cubicle showing details of sandwich construction, valve operator channels, a n d observation port-mirror system
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INDUSTRIAL AND ENGINEERING CHEMISTRY
Barricades are of the sandwich (6,73) tvpe. T h e construction consists of l/4inch steel plate on the outside of the wall, and 2-inch tongue and groove wood siding on the inside wall, with 4 inches of sand filler in between. T h e three barricade sides of each cubicle were prefabricated by welding the steel plate to 4-inch channel iron framework. T h e vertical channel iron members are on 24-inch centers. This framework is
H I O H PRESSURE P R E P A R A T I O N S L A B O R A T O R Y
GRAND RIVER CHEMICAL DIVISION ENGINEERING DEPARTMENT
MATERIAL REQUISITION ~~
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PROJECT
REQUISITION NO.
71-47A
Equipment
ITEM
High Pressure Laboratory
SERVICE QUANTITY
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Positive displacement gas compression pump
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A. Manufacturer Autoclave Engineers, Ino. B. Type - Model M G 1 5 C. Maximum working pressure 15,000 psi
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Stirred autoclave A.
Manufacturer - Autoclave Engineers, Ino.
B. Type - Serial No. AC-1962 C. Capacity - 1-liter
D. Maximum working pressure - 5.000 psi E. Maximum working temper&ture - 650°F F. Material of oonstruction - 316 stainless steel 1
Rocker assembly A.
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Manufacturer Autoolave Engineers, Ino. - for use with 250 and 500 ml reaotors Drive - 1/3 h.p. motor (110 volts) Accessories a. rocker linkage and drive b. combination valve and rupture disc c. swivel joint and oonnector tube Heating element - Glas-col heating mantle, 2,000watts, 220 volt, single phase Reactors - 250 ml., 316 stainless steel, working pressure 12,000 psi at 650'F; 500 ml., 316 stainless steel, working pressure 10,000 psi at 650'F
B. Type C. D.
E.
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Floor-to-ceiling hood showing four sliding doors, air, steam, and water utilities and 110- and 220-volt electrical outlets. The basic equipment rack i s made of five vertical */*-inch pipes. Auxiliary supports are '/s-inch aluminum rods, held by U-bolts
Magne Dash Autoclave Manufacturer - Autoclave Engineers, Ino. - Magne Dash with Model #8 Turner C. Capacity - 100 ml. D. Material of construction - 316 stainless steel (reaotor) E. Working pressure - 5,000 psi F. Working temperature - 650°F G. Reactor - one 250 ml., working pressure 5,000 psi at 650°F A.
B. Type
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anchored to the foundation by I-inch bolts on 12-inch centers, and the three sides are welded a t the corners; 2 X 4 inch wood strips are attached to the upright channel irons and the 2 X 6 inch tongue and groove siding is attached to the wood by lag screws. One of the disadvantages of sandwich construction-leaking out of sand-was overcome by lining the tongue and groove siding with thin polyethylene sheeting. This was accomplished by tacking the polyethylene sheeting to the 2 X 4 inch wood frame prior to installing the siding. The roof of the test cubicles slants upward toward the blowout wall. I t was
felt necessary, because of the location E the building with respect to manufacturing facilities, to employ the sandwich construction over the entire roof area to prevent any projectile from going in any but one direction. T h e wooden interiors of the barricaded cubicles are painted with white fire-retardant paint. T h e part of the building housing the barricaded cubicles is not connected directly with the other part of the building. Side walls, roof, and foundations are separated by expansion ioints. T h e blowout wall is constructed from '/,-inch flat Transite sheets. T h e doors are hinged outward and held shut by
Control panel and barricade wall as seen from the laboratory. Breaker box is convenient to control area. The heater controller-indicator and associated Variac and the gas-control valves are in easy reach of the operator when he i s viewing the autoclave assembly through the observation port. Steam, air, condensate, water, and nitrogen supply to the cubicle can be seen at bottom VOL. 51, NO. 10
OCTOBER 1959
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A Half-liter rocker autoclave as seen from rear of cubicle. Gage i s positioned so that it can b e read from above where the large mirror reflects the image into the mirror of observation port
b Close-up of valve rack and short valve extensions which go through to barricade for operation from the laboratory side
friction catches irhich \ \ o d d allow them to be blown outward easily. T h e remaining panels on the blo\rout ivall are attached by screws and rubber \rashers. the hole in the Transite being larger than the head of the screw. These panels should blow out with a pressure of about 1 pound per square foot. Test Cubicle Details
Service piping is brought into each cubicle from the piping chase through the front cubicle wall just above floor level. Valve handles extend through the wall a t instrument level. T h e instrument panel is attached at right angles to the cubicle wall. Observation port, valve operators, and instruments are located for easy operation and observation. High pressure valves are mounted on a n angle-iron rack on the Xvooden interior of the cubicle. T h e operator fits loosely over the valve handle, thus avoiding difficulties in alignment of valve handle extensions. T h e opcrator is held in place by a packing nut, which also makes a vapor-tight seal, on the fronr of the cubicle wall. A circular plate is welded on the operator handle just inside the cubicle wall to minimize chances that valve operators and handles will be blown into the operating area. There are also valve operators containing a universal joint that will operate valves 5 or 6 feet away from wall and not in a direct line with the valve operator opening. T h e operator openings are plugged on each end with screwed plugs when not in use. Valves are placed on each service just above floor level in the operating area a t the front of the cubicle. Services for each cubicle include 15-p.s.i.g. steam, steam condensate, 150-p.s.i.g. plant com-
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pressed air, sanitary Lvater, and 2UJp.s.i.g. nitrogen. Two spare pipes, capped ar each end, are in place in the wall of each cuticle. T h e observation system consists of a double mirror arrangement. T h e port is protected bj- I, ?-inch sheet steel; 3;/4inch bullet-proof glass installed \rith gaskets makes i t vapor-tight. T h e mirror in the port is about 3 inches square; the mirror in the ceiling of the cubicle is 30 X 30 inchrs. \\-ith appropriate serting of mirrors, nearly the entire interior of the cubicle is visible from the control area. T h e ceiling mirror can be adjusted to bring various areas in view; it can be rcmotrly raised and loirered by a pulley system and a handle through one valve opzrator hole. A small automobile rear vinv-type mirror can be mounted just above part of the port mirror to focus sight on any small specific area \vith sliqlit effect on thc over-all vieiving of the cubicle inrerior. Electrical service rntrrs the instrument panel box through conduit in the floor. .\ breaker panel is located on the laboratory side of the instrument panel box and all circuits \vithin the test cubicle come from this breaker box. Electrical and thermocouple leads are brought into the test cubicle through Class I, Group D (explosion-proof) fittings. Safety Features
Final operating procedures have not been completed. However, the procedures described by Stephens and IValler (74) are being followed, with certain modifications. I t is considered imporrant that the test cubicles are separated from instrument and control areas and the laboratory areas, so that no gases or vapors can be transmitted. All services and leads through the cubicle \\.all are vapor-tight.
INDUSTRIAL AND ENGINEERING CHEMISTRY
T h e blower in each cubicle is sized to provide a complete air change about twke per minute. T h e blower starts when the lights are turned on. ilir is pulled through a 1 X 2 foot expanded metal-covered opening in the bottom of the door in the blowout wall. Thc blower is located in the ceiling near the front wall of the cubicle. This ventilation will minimize the chances for the development of a n explosive gas mixture in the test cubicle. When the lighting and blower system is turned on, a large red sign (DANGER, I N USE) lights on the instrument panel box. At the same time, red lights a t the outside corner above the blowout \Val1 door turn on. Each test cubicle is equipped with an automatic \rater sprinkler system. T h e interior of the cubicle is painted Lvith fire-retardant paint. A r present the instrument panels arc fittcd only with temperature-indicating controllers, an ammeter, and a variablc transformer. A microswitch Lvith red light controls the main power supplythis switch must be on before any po\ver is available in the t a t cubicle; when turned off, it shuts off all po\vcr, including the lights and blower. Microsivitchrs \rith green lights control t h e lighting and blo\rer (controlled by thr same slvitch), 1IO-volt recepraclrs, and 208-volt heating receptacles. :\ 208volt: thrre-phase receptacle is 1)rovidrd in the largest test cubiclr. T h e test cubicles are hcatcd by steam fin tubed hearers moiintc~clo n the criling Hcating is provided for ~ W C X - U [ J protccr i o n , principally; operator comfort is secondary. literature Cited [ I ) Barber, A. T,! ‘I’aylor. .I. €-I.. Inst. .\ierh. h s i s . 1 2 8 , 5 ( 1934 1 . ( 2 1 Bowen, J . C.. .Jenkins. I.
ISIJ.
pp. 241 -9. Kcinhold. Ncw York, 10.51. K w d . F. C:., Fki\vxds, G . C : I I ~ , V . 17, 781 (10251.
. Knt~tllcI,0 . ;I.?l’rtcrs n ,.I. F.. Sharrah, X I . I . . . Ihtd., 48, 840
(1956~. ( 7 1 Glasrbrook. .I.I,.. Rloiitr:otncry, .I. E., Ibid.. 41, 2368 (10401. ( 8 ) Hitcshnc. K. \V.. I b d . 48, 835 ( l O S 6 ~ . ( 9 ) Kiefer, K. I V . . Ib:c/.. 49, 2017 ( 1 9 5 7 r . (101 Killeffer. I). H.. Ibid.. 1 7 , 789 (1925i. ( 1 1 ! XIahly. H. S.! C h ~ r r : ,Eric. .Vezr,J 27, 3860 (19441. 1121 hfiller, J . F., ISD. f 846 (1956). (13) Porter. K. I>.! Lobo. 1’. A , , Slicpcevich, C:, RI.: I bid., 48, 841 (1 956 1. (141 Stephcns. H. K., \j-alkrr; K . I;., Ibid., 49,2022 (lO57). ( 1 5 ) Storch. H. H., Hirst, I,. I,.> I:ishcr, C . H., Sprunk, G . C.. Lr.S. Bur. hlinrs Tech. Paper 622, (1941 I.
RECEIVED for revie\v XIay 28. 1959 ;\CCEPTEII J u n e 6, 1059 Division of Industrial and 1;nginrrrinq Chemistry, 134th Meeting, XCS, Chicaqu, Ill., September 1958.
