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Chemical Engineering Research at The B. F. Goodrich Company *
A. B. JAPS T H E ,E. F. QOODRICH COMPANY, AKRON, OHIO
C h e m i c a l engineering research a t The B. F. Goodrich Company embraces t w o m a i n branches: preliminary development and evaluation of new products and processes on a small p i l o t p l a n t scale; and t h e conception and development of fundamentally new techniques for carryi n g o u t unit operations and processes. The m a i n laboratories occupy roughly one third of t h e three-story Engineering Research building, t h e largest of t h e five buildings comprising t h e new B. F. Goodrich Center a t Brecksville, Ohio. The arrangement of t h e space allotted t o chemical engineering research (60 X 100 feet and t h r e e stories high) was determined m a i n l y by six factors: t h e general architecture of t h e building; safety; flexibility of layout and adaptation t o f u t u r e needs; general nature of anticipated experimental work; determination of necessary auxiliary service facilities and t h e i r location in other parts of t h e building; and appearance. To accommodate p i l o t p l a n t
u n i t s w i t h different heights, t h e second floor has been omitted in some areas, and b o t h second and,third floors in other areas. All of t h e building columns in high areas are constructed t o p e r m i t t h e f u t u r e spanning of any bay w i t h steel f o r t h e support of floors or platforms a t almost any level. For work of a hazardous nature, a separate explosion-proof area of four bays has been constructed w i t h t i l e fire walls and explosion-relief windows, W i t h t h e exception of t h i s small area, t h e laboratories are windowless, air-conditioned, and artificially illuminated w i t h fluorescent lights. In addition t o i t s m a i n laboratories, t h e Department of Chemical Engineering Research i s responsi ble for t h e operation and maintenance of t w o smaller structures, t h e Hi-Vent b u i l d i n g and t h e Hi-Pressure building, which have been especially designed t o secure comparative safety in experiments w i t h highly toxic chemicals and h i g h pressure,equipment, respectively.
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a few pounds to a few hundred pounds, t o determine its usefulness more fully than is possible ordinarily with a few ounces resulting from laboratory investigations. These preparations, made in the simplest possible assembly of equipment, serve t o acquaint the research chemical engineer with the engineering problems involved and yield a basis for the preparation of very preliminary raw material or production cost estimates. If testing and evaluation of the product result in continued interest, and if cost estimates appear favorable, a research pilot unit, batch, or continuous, as the circumstances justify, is designed from the best information available. Parts are then assembled on as small a scale as practicable for investigating the equipment and conditions necessary for carrying out the unit operations involved. Engineering experimentation, accompanied by frequent alterations of equipment, reveals the effects of such process variables as agitation, time and temperature, catalysis, flow rates, prmsure, methods. of purification, and materials of construction of equipment, as well as product quality and yields attainable. As the work progresses, its course is charted and altered in the light of frequent analysis of the accumulated data and discussion with key laboratory research men and production technicians. When a project reaches a stage of apparent practicability and is accepted for development by the manufacturing division of our organization, all data together with preliminary estimates of production costs and recommendations based on pilot plant results are submitted formally for study and further development in semi-works installations such as that of the Chemical Company a t Avon Lake, Ohio ( I ) . A number of chemical engineering research studies, often a s many as eight or ten, may be under simultaneous investigation in as many different setups requiring widely divergent types of
N LBRGE industrial concerns, the term pilot plant has been
used broadly to designate the building and equipment employed for the small or medium scale evaluation and development of new products and processes. However, pilot plants may be used not only for the purpose which gives them their name, but also for fundamental research in engineering problems. At The B. F. Goodrich Company, the Department of Chemical Engineering Research employs pilot plants as part of its equipment for the performance of its main functions, which are: small scale evaluation of new products and processes, including adaptation of the processes to types of equipment to be employed in subsequent semi-works development; and chemical engineering research, involving the conception and development of fundamentally new techniques and equipment for carrying out the unit operations and processes in the field of chemical engineering. The first of these functions may be regarded principally as service to research, rather than as true research, though i t may often lead to valuable new discoveries and the conception of new research projects. FUNCTIONAL ORGANIZATION
To carry out these functions, a staff of trained chemical engineers, picked especially for their ability in research, work in close cooperation with the research chemists of the laboratory. These engineers, by applying basic chemical engineering knowlege to a new synthesis, determine, for example, the basic unit operations required and try to diseover and develop through engineering experimentation the simplest and most suitable process and equipment for conducting these operations. A new project undertaken by the Chemical Engineering Research Department usually begins with a request for the production of a quantity of the new product; this may vary from
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equipment and facilitate cleaning. Pressure and temperature ranges of utilizatron are extended as far as economically justifiable. Interchangeable agitators and variable speed agitation are usually employed a b far as possible. Since engineering information, and not the quantity of a chemical product, is the primary objective generally, the capacities of the principal units of an assembly are maintained as small as possible t o obtain significant results. The smaller the equipment the simpler is its assembly into pilot plants. Also a larger range of variables can be investigated in a given period of time with less expenditure of man power and space for handling raw materials and finished products. On the other hand, accurate data on flow measurement and control and significant material balances become increasingly difficult to obtain as the scale is reduced. Figure 1. Identical Small Pressure Reactors Designed for A series of four small identical pressure reactors Investigating Emulsion Polymerizations especially designed and constructed for investigating the emulsion polymerization of such monomers as butadiene and styrene are illustrated in Figure 1. These reactors have proved successful in obtaining informaequipment and producing vastly different products. A process might be one for synthesizing a new gaseous polymerization tion capable of being extrapolated to larger production vessels. They are constructed of glass-lined steel to withstand 200 monomer, a crystalline accelerator, or a liquid age-resister for use in rubber compounding, or it might be one for producing a new pounds per square inch pressure. They have variable speed agitation and temperatures are Controlled accurately by film plastic or a new synthetic rubber. T h e product might be either cooling. organic or inorganic i n nature. Consequently, both flexibility Figure 2 shows a group of three special chemical reactors of of operation and a wide variety of versatile experimental equipstainless steel and glass-lined steel construction varying in cament are required. pacity from 25 to 75 gallons. These vessels serve as central units EQUIPMENT around which other more portable equipment is assembled. T o this end, a rather extensive stock of generally useful pilot I n the interests of flexibility, the only items of equipment more plant equipment has been accumulated over a number of years; or less permanently fixed are some of these special reactors and certain niachiiies for operations such as drying, grinding, washnew equipment is added as the occasions arise. Many of the milling, and screening; these are generally discontinuous with the items, such as pumps, agitators, heat exchangers, dryers, filters, preceding and succeeding stcps of any process. Most other crushers, grinders, vacuum equipment, flow meters, and tempilot plant equipment is kept portable as far as possible, even t o perature recorders and controllers are fairly standard pilot plant thp extent of mounting on wheels or casters, so that it can be pieces. However, a goodly number of items (as reactors and stills) moved up readily and connected into a n assembly. Portable have been designed and especially constructed to permit flexibility pieces containing motors have their own motor controls and proin investigating as wide a range of variables as possible. Extection built as part of the assembly and are fitted with flexible tensive use is made of stainless steel and glass-lined steel as plug-in electrical leads. materials of construction. Openings are designed sufficiently Portability even prevails in such auxiliary units as refriglarge and numerous to permit attachment of predictable auxiliary erating and heating equipment. A portable refrigeration unit capable of giving 2 tons of indirect refrigeration a t -10" F. is shonn in
Figure 2.
Special Chemical Reactors Varying in Capacity f r o m 25 t o 75 Gallons
Figure 3. Portable Refrigeration Unit w i t h Capacity of 2 Tons of Indirect Refrigeration a t -10" F.
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Figure 4.
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Portable Filtration Units
(Left) Plate and frame press; (center) variable speed centrifuge; (rlght) vaouum d r u m filter
Figure 3. This unit on casters contains a 10-h.p. Freon compressor, a pump and heat exchanger for circulating and cooling alcohol, and all refrigeration and electrical controls. Connections of power and water supply, as well as refrigeration connections to pilot plant equipment, are made easily and quickly at the panels built into the ends of the unit. Three types of portable filtration units, also mounted on wheels, are shown in Figure 4. These include a stainless steel 12-inch plate and frame press with pump, a stainless steel variable speed centrifuge with 12-inch diameter basket, and a 12 X 12 inch vacuum drum filter. Figure 5 shows the arrangement and size of equipment used in t h e initial small scale investigation of a typical distillation operation whereas Figure 6 illustrates the same operation being performed at a subsequent time in a more truly pilot plant unit. Both units are composed entirely of glass or glass-lined steel because of the corrosive nature of the materials being handled. Figure 7 is illustrative of another small scale assembly involving several unit operations and presented to show the general size and nature of some of the equipment used by the research chemical engineer in carrying on engineering investigations. The research engineers are assisted ordinarily in the assembly, rearrangement, maintenance, and experimental operation of the pilot plant by a specially trained group of nontechnical salaried employees, called research mechanics. This versatile group of men is distributed among the various projects as the needs direct. Experience has shown that the time of one such mechanic for each technical man is efficiently utilized in this type of work.
Figure 5. Equipment for Preliminary S m a l l Scale Investigation of Typical Distillation Operation
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T H E B. F. G O O D R I C H RESEARCH C E N T E R The activities and equipment described above are housed in a large area in the Engineering Resear& buildirlg of the nelv B. F. C;oodrich Research Center a t Brecksville, Ohio. This new research center, just now being completed, is situated on a 260-
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acre tract of land overlooking the beautiful Cuyahoga Valley and lies midway b e h e e n The B. F. Goodrioh Company in Akron and T h e B. F. Goodrich Chemical Company in Cleveland. The Center at present consists of five modern well ,equipped arid functionally designed laboratory buildings with complete facilities for carrying on fundamental technical and engineering research studies a t one centralized location. I t s remoteness from congested industrial and resident'ial areas affords complete froodoin from their accompanying dirt, noisc, and vibration. The main research building (at the left in Figure 8) contains 81 laboratory modules 10 X 26 feet designed for great flexibility of arrangement of space, utilities, and equipment for conducting basic chemical and physical research. In addition, the main research building houses the largest, technical library in the rubber industry, a st'reamlined cafekria, a n audi toriuin, arid conference and first-aid rooms, as well as the administrative offices. The second large building, called the Enyineering Research building, contains the chemical engineering research laboratories, physical testing and evaluation laboratories for rubber and plastics, the boiler room, the various maintenance and construction shops, bulky airconditioning equipment, receiving and storage Figure 6. Larger Equipment for Pilot P l a n t Investigation of facilit'ies, and various other necessary services. Distillation Operation Shown in Figure 5
Figure 7.
Small Scale Equipment Involving Several U n i t Operations
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T h e need for auxiliary service facilities and their location in other parts of the building. Appearance and neatness of layouts. T o preserve architectural harmony in this building and with other buildings the outer confines of the area and the distance between floor levels had t o be rigidly maintained. A cross-sectional elevation of the Chemical Engineering Research Laboratories is shown in Figure 9. Since more height frequently has been found necessary in engineering setups than was available between the standard floors, the concrete floors in certain bays were omitted to provide several levels of headroom. To allow so' im' installation of columns, towers, and barometric legs, a n area with 40 feet of headroom is provided by leaving the end row of these bays completely open to the roof slab and by excavating most of this area to a depth of 8 feet below the ground floor level. This low level excavation has become known as the pit. T h e high area is spanned by a 2-ton electrically operated traveling crane. At t h e ground floor level an 8-foot wide platform covered with removable subway grating projects over the pit into the high area. This platform was designed t o support several of the larger reactors and still pots, thus permitting the grouping of portable equipment about and below them and the erection of tall columns overhead. A similar platform, but only 4 feet wide, is cantilevered into the high bays at the third floor level. Besides facilitating support. of equipment, these platforms permit the crane to land heavy or bulky objects onto these two floors from trucks entering the building through a large door in the high area.
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Figure 8 Both of these large connected three-story fireproof buildings a r e windowless, air-conditioned, and artificially lighted. Behind the main buildings lie two smaller structures, the HiVent and the Hi-Pressure buildings, which have been designed respectively for carrying out investigations with highly toxic ahemicals and engineering studies in high pressure equipment under conditions of comparative safety. The small building in the foreground is a solvent storage building, and the structure opposite in the background is a water cooling tower which rests on a 300,000-gallon underground storage tank, The Center is powered with gas-fired boilers. Water is obtained from Lake Erie through the Cleveland municipal supply, a n d electricity is delivered to the substation a t 33,000 volts direct from two stations of the Cleveland Electric Illuminating Company. C H E M I C A L E N G I N E E R I N G RESEARCH LABORATORIES
The areas in the Center under the jurisdiction of the Department of Chemical Engineering Research include: the Chemical Engineering Research Laboratories in the Engineering Research building; the Hi-Vent building; and the Hi-Prcssure building. The Engineering Research building, like the others, is constructed of steel frames, concrete floors, and brick walls. Exposed steel columns are spaced on 20-foot center lines to standardize the steel framing. Floor to floor height is fixed a t 11 feet 6 inches to give a clear working height of approximately 10 feet beneath the exposedesteel beams. Interior walls and permanent partitions are made of structural glazed tile, low in maintenance expense. Adaptability in the use of experimental space has been gained by subdividing some of the larger areas and forming corridors with partitions composed of interchangeable flushtype standard industrial steel panels which can be rearranged easily. T h e Chemical Engineering Research Laboratories are contained in the full three stories of a n area 60 X 100 feet in the northeast portion of this building-that is a space three bays wide by five bays long, or approximately one third of the area of the whole building. Within this area the arrangement of experimental space was determined by consideration of six principal factors, a s follows: The general architecture of the building. Safet considerations. Flexifility of t h e layout and ease of adaptation t o future needs. The general nature of the anticipated experimental work based on previous experience.
Figure 9
By omitting the second floor in the six bays adjoining the high area, considerable useful space of clear heights of 21 feet 6 inches on the ground floor and 10 feet on the third floor levels was obtained for pilot plants requiring intermediate and relatively low heights. I n all of the area where floors have been omitted the steel framing was designed with sufficient strength to support floors if ever i t is desirable to install them. All of the building columns in high areas are constructed with continuous vertical fins which carry 0.75-inch perforations every 3 inches, thus enabling the spanning of any bay with steel and the support of floors or platforms at almost any desired level. The arrangements of space on the various floor levels are shown in Figure 10. The hazardous nature of a substantial portion of the experimental work, particularly t h a t involving polymerizations or reactions of flammable monomers, such as butadiene and vinyl chloride, made i t necessary t o provide a n area which could be maintained entirely explosion-proof to meet the requirements of the insurance and building codes. Such a n area was obtained by partitioning the northwest block of four bays through all three
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pair of explosion-proof cold rooms capable of being maintained at, 0" and -25" C., respectively, for storage of volatile and unstable chemicals. Bulk quantities of such polymerization monomers as butadiene and vinyl chloride are stored in 200-gallon refrigerated glass-lined tanks housed in a penthouse over the cold rooms. A typical chemical laboratory for control tests of pilot plant operations is shown adjacent to the cold rooms. An engineering design room accommodating drafting tables, blueprint and catalog files, and a large conference table as n-ell as the departmental director's office and stenographic space were provided by installing movable industrial-type steel partitions in two bays of the general work space. Although no additional office space has been provided, each individual research engineer has his own desk placed in the immediate vicinity of his work. All office and laboratory furniture throughout aro of steel construction.
GENERAL WORK PREP
EXPLOSN- PROOF AREA
THIRD FLOOR PLAN
CSNTROL LA6
CHEVIChL ENCINEERING RESEARCH EXPLOSION
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SERVICES AND U T I L I T I E S
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DRYING, GRINDING AND SCREENING AREA
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SECOND FLOOR PLAN
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Figure 10
Boors from the general pilot plant areas by 8-inch thick tile fire walls and installing explosion-relief windows in the outside walls. Double door vestibules allow communication between the two types of area. To facilitate the erection of setups up to 20 feet high in the explosion-proof area, the second floor was constructed entirely of removable sections of subway grating instead of concrete. A section of concrete slab 4 feet square adjacent to the center column was omitted in the third floor t o permit future columns as high as 30 feet t o be set up. This opening is now covered with checker plate to facilitate air-conditioning. The batch preparation laboratory (Figure 10) is designed and equipped for the preparation (for preliminary evaluation) of batches of chemicals in ceramic potd or laboratory glassware. A special 5-fOOt wide by 12-foot long completely enclosed walk-in hood was constructed here for venting the disagreeable odors which often accompany this type of preparation. On the second floor a space has been provided and specially ventilated for carrying out the ordinarily dusty operations of drying, crushing, dry-grinding, screening, and sampling. The explosion-proof area on the third floor is now being utilized for polymerization development and contains the four experimental polymerizers shown in Figure 1. This area opens into a
All confined experimental areas have a t least two means of exit, usually located on opposite sides of the area. Also in the interests of safety, overhead emergency showers are located near most, exits. Concrete and tile staircases across the corridor from the experimental areas afford general communication between floors. Eight-foot, wide corridors and double swinging doors allow access to a truck-loading ramp and a &ton freight' elevator for convenient movement of materials and equipment. They also communicate directly with the auxiliary service rooms for the Center (housed in t'he building); most of these are necessary to our chemical engineering research work. I n the service areas are stock and storage rooms; well equipped maintenance and construction shops for pipe fitting, metal working, welding, woodworking and painting; an instrument shop for instrument repair and storage; storage rooms for ice and dry ice; and locker and shower rooms. The absence of windoxs in the building (except in the explosionproof area and in the power plant) created a number of problems in adequately ventilating and lighting the experimental spaces, particularly the large high areas. These problems all havc been solved successfully, and their solution has given the windowless laboratories several distinct advantages over laboratories wit,h windows. The problem of making the windowless laboratories comfortable during occupancy was solved by air-conditioning the space with approximately 16,500 cubic feet of filtered, cooled, arid tempered air each minute. However, in order t o ventilate experimental areas adequat,ely during periods of operation when chemical fumes or excessive heat might be present, i t was necessary to install seven different exhaust systems, each system capable of being operated independently and containing a number of functionally spotted and dampered ' openings. Flexible tubes when connected to the openings provide approximately 3000 cubic feet per minute of local exhaust from almost any spot in t>hework areas. When all systems are being operated simultaneously approximately 45,000 cubic feet of tempered auxiliary air is supplied to and xvithdrawn from the portion of the building each minute. Lighting is accomplished with fluorescent lights in all spacer except the explosion-proof areas where Class 1, Group D incandescent fixtures are installed. An illumination intensity of 30 to 35 foot-candles is attained in all experimental areas, while 50 to 70 foot-candles are available in the offices and chemical laboratory. Good lighting and constant temperature assist matwially iii the running of a number of experiments (particularly thoso involving continuous operation) and afford uniformly good u-orlcing conditions, whet,her i t be day or night, slimmer or winter. The absence of windows also allows greater flexibilit,y in tho utilization of space and in t,he distribution of services hcaust.
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INDUSTRIAL AND ENGINEERING CHEMISTRY
almost all wall space can be utilized with equal efficiency. Generally throughout this building and the Hi-Vent building, the services (150-pound steam, 90-pound compressed air, process vater, natural gas, and 440- and 220-110-volt three-phase electric power) are distributed in bands around the walls a t a minimum height of 7 feet from the floor, with convenient outlets spaced approximately every 10 feet. Some of the utilities are available also a t the central columns, hence only relatively short piping runs have t o be made in connecting and arranging portable equipment. Process waste removal is accomplished by means of 8-inch wide grating-covered trenches set into the concrete floors along the perimeters of the working areas, and the floors are well pitched t o the trenches to secure proper drainage. Certain special utilities such as vacuum, distilled, demineralized, and zeolite-softened waters, and hot liquid Dowtherm are piped from certain permanent installations to some of the areas for convenience.
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waste disposal is particularly useful when toxic chemicals are accidentally spilled during operations. HI-PRESSU R E BU I L D I N G
The Hi-Pressure building, a building 20 feet wide, 50 feet long, with a 14-foot ceiling, was built for investigating reactions carried out under pressure. It contains spaces for housing experimental setups, each barricaded a t the front and two sides from floor to ceiling with 12-inch thick r e i n f o r c e d concrete walls. Figure 12 shows a plan view of the building and cross-sectional elevation through one of the barricaded enclosures.
HI-VENT BUILDING
The Hi-Vent building (Figure 11) was constructed for investigating reactions involving very toxic chemicals such as hydrogen cyanide or phosgene. This building, measuring 20 by 30 feet with a working height of 16 feet, is designed as a large walk-in hood in which the air is capable of being changed a t rates of once or twice a minute during periods of operation. This is accomplished by blowing either 10,000 or 20,000 cubic feet per minute of fresh air, heated when necessary by two large unit heaters, into the plenum chamber above the suspended ceiling and through a perforated cenhal portion of it. The air flows down and across the room and is withdrawn through 12inch wide slots in the floor into a second plenum chamber under the entire floor which is connected with a 30foot masonry stack. A two-speed fan in the stack, electrically interconnected n-ith the supply fans, equalizes the pressure in the room. The exhaust floor slots are covered with removable 18inch s e c t i o n s of subway grating and checker plate whose arrangement, together with the arr a n g e m e n t of a number of special suspended movable CROSS SECTIONAL ELEVATION baffles which terHI -VENT BUILDING minate 7 feet above the floor, caused the Figure 11 air to be directed down and across the investigator as he operates a n experimental setup placed anywhere along the walls. This building has windows with sills 8 feet above t h e floor; these can be opened to provide natural ventilation during settingup periods. The exhaust floor slots serve also as drains for process waste. The plenum chamber underneath is constructed to serve as a collecting basin with central drain to sewer. This method of
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HI -PRESSURE FLOOR PLAN
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CROSS SECTIONAL ELEVATION Figure 12
The back or open side faces explosion-relief windows, and the roof over the enclosure is loosely attached so as t o blow open rather than damage the building proper in the event of equipment rupture. Doorways through the side barricades and aisles between the enclosures allow two means of access to each. Dual sets of peep slots set through the face of each barricade a t a 45-degree angle permit indirect vision of the equipment, and a number of pipe sleeves afford connection with the general utilities, which are carried in a band across the front faces of the barricades. Wall ventilating fans operate a t the rear of each space. To utilize efficiently the space and equipment in this building, all of ~e work 'done, which includes the maintenance and installation of equipment, the running of batch pressure reactions a s ' a service for the laboratory researchers, and the small pilot plant development of continuous pressure processes is conducted under the supervision of a n experienced chemical engineer. The chemical engineering research facilities at The B. F. Goodrich Research Center are new. Operations are just now getting under way at this location. Consequently, a number of the special features described have not been fully tested. Nevertheless, they embody the best ideas gathered from a large number of engineers and key research men engaged in chemical process development in leading industrial, university, and government laboratories. The company has sought to combine greater versatility and attractiveness of facilities with maximum safety for personnel in a n industrial laboratory for small scale process development in a widely diversified program.
LITERATURE CITED (1) Schoenfeld, F. K., Chem. I n d s . , 60,958 (1947). RECEIVED April 26, 1948.
