PERICIN MEDAL..
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Awarded to Walter S. Landis for work on cyanamide and its derivatives and on fertilizers (particularly ammonium phosphate), for the first commercial production. of argon., and for contributions to the explosives industry
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HE Perkin Medal for 1939 was presented to Walter S. Landis, vice president of the American Cyanamid Company, on January 6, 1939, a t a joint meeting of the American Section of the Society of Chemical Industry and of the New York Section of the AMERICANCHEMICAL SOCIETY, a t The Chemists’ Club, New York. Victor G. Bartram, president of the Society of Chemical Industry, presided over the meeting. Wallace P.Cohoe, chairman of the American Section, opened the program with a commemoration of former medalists. After a talk on Landis, the man, by Floyd Parsons, and a discussion of his scientific accomplishmentsby C. M. A. Stine, the medal was presented by Marston T. Bogert, of Columbia University. Then Dr. Landis gave his medal address on the subject of argon. Dr. Landis was born in Pottstown, Pa., in 1881, and received his elementary education there and in Orlando, Fla. WALTERS. LANDIS He received the metallurgical engineering degree in 1902, the degree of master of science in 1906, and the honorary degree of doctor of science in 1922, all from Lehigh University. He held various teaching positions a t Lehigh,mainly in the field of metallurgy, and then became chief technologist of the American Cyanamid Company in 1912. He has been vice president execution or publication, or whether it became valuable in of that company from 1922 to date. His accomplishments in subsequent development of the industry. The medalist is industry include processes for the production of cyanamide, chosen by a committee representing this society, the AMERIof cyanide from cyanamide, and of urea; he was the first to CAN CHEMICAL SOCIETY, the Electrochemical Society, the oxidize ammonia commercially in the United States, the American Institute of Chemical Engineers, and the Soci6t6 originator of the Ammo-Phos process, the first commercial de Chimie Industrielle. producer of argon; and he has made contributions to the The list of medalists from the date of founding to the present explosives industry, electric furnace studies, etc. is as follows : Dr. Landis was president of the Electrochemical Society in 1920, chairman of the New York Section of the AMEBICAN 1924 Frederiok M. Becket 1906 Sir William H. Perkin CHEMICAL SOCIETY in 1931, and Joseph W. Richards Memo1925 Hugh K. Moore 1908 J. B. F. Herreshoff rial Lecturer of the Electrochemical Society in 1934. He is a 1926 R. B. Moore 1909 Arno Behr 1927 John E. Teeple 1910 E. G. Acheson member of the AMERICAN CHEMICAL SOCIETY, Electrochemical 1928 Irving Langmuir 1911 Chailes M. Hall Society, American Institute of Chemical Engineers, American 1929 E. C. Sullivan 1912 Herman Frasch Institute of Mining and Metallurgical Engineers, Tau Beta 1930 Herbert H. Dow 1913 James Gayley Pi, Sigma Xi, and Epsilon Chi. He has published many ar1931 Arthur D. Little 1914 John W. Hyatt 1932 Charles F. Burgess 1915 Edward Weston ticles and textbooks, and has been granted many patents in the 1933 George Oenslager 1916 Leo H. Baekeland United States and foreign countries. 1934 Colin G. Fink 1917 Ernst Twitchell The Perkin Medal was founded in 1906 in commemoration 1935 George 0. Curme, Jr. 1918 Auguste J. Rossi of the fiftieth anniversary of the coal-tar color industry, the 1936 Warren K. Lewis 1919 Fa G. Cottrell 1937 Thomas Midgley, Jr. 1920 Charles F. Chandler first medal being awarded to Sir William H. Perkin, discoverer 1938 Frank J. Tone 1921 Willis R. Whitney of aniline dyes. The medal may be awarded annually by the 1939 Walter S. Landis 1922 William M. Burton American Section of the Society of Chemical Industry for the 1923 Milton C. Whitaker most valuable work in applied chemistry. The award may be made to any chemist residing in the United States of (For list of achievements of each medalist up to 1934, see America for work which he has done a t any time during his IND.ENG.CHEM.,February, 1933, page 229.) career, whether this work proved successful a t the time of
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240
An Early Chapter in Argon Production W. S. LANDIS American Cyanamid Company, New York, N. Y
S
INCE this occasion is really a memorial to past achievement, it should properly be one of retrospect. I shall have no quarrel with those who question the choice of the medalist, nor with those who place accident and occasion as responsible for much of his work. Progress in our science is difficult of exact measurement, and even more obscure is the determination of the exact contribution of the individual. The records of the Patent Office attest to this latter fact. Very often we chemists have been neglectful of recording the milestones of progress in our industry. We have been poor advertisers in years gone by. We had an inferiority complex, not deserved. Today all this is corrected, but that does not take care of the past. So we are going back nearly a quarter of a century and at this late date record a bit of chemical history that could long ago have been added to the literature. On November 14, 1914, the American Cyanamid Company accepted an order from the National Lamp Works of the General Electric Company to deliver 5,000 cubic feet of argon a t the rate of 100 to 200 cubic feet per day, the concentration of argon in the mixture shipped to be more than 20 per cent. Deliveries actually started in December, 1914, and continued through to May, 1915, totaling in all nearly 8,000 cubic feet of argon. The major part was shipped to Cleveland, but considerable quantities were exported to Europe. It is the
equipped itself with this apparatus and begun the supply of a similar mixture from one of their plants in this country. In December, 1913, Dr. Willis R. Whitney of Schenectady wrote to ask if we could assist them in obtaining a small quantity of argon for experimental work. He stated that he had been operating a small liquid air unit for some time but that the production of argon was almost nil. I frankly discussed with Dr. Whitney a t that time the position of the Cyanamid Company process with respect to its possibility of serving him, and both of us agreed that the process as ordinarily conducted offered very little hope of solving his problem, for the following reasons.
Operations in 1913 The cyanamide process as developed in Europe had choice of two methods of producing the relatively pure nitrogen gas required. One method we shall call the “copper process” and the second method, the “liquid air” process. In the copper process, air is passed over heated copper which fixes the oxygen as copper oxide and delivers the nitrogen with the other inert gases of the atmosphere to a purification system where accidental impurities such as carbon dioxide, water vapor, and the like are removed. The copper oxide is then regenerated by the use of any reducing gas, and the cycle begins again.
ORIQINALCYANAMIDE PLANTAT NIAGARA FALLS,CANADA,IN 1909
In the liquid air process, air is compressed and liquefied in part, and with the assistance of a rectification column, nitrogen is recovered from the top and oxygen with the major part of the argon removed from the base of the column. It is not necessary to go into further details of the complicated apparatus used to make this separation. Now it happens that the atmosphere around a cyanamide plant is very apt to contain small quantities of acetylene. This acetylene accumulates in the column in the form of solid crystal floating in the liquid oxygen in the lower part of the apparatus. This is an extremely hazardous combination, and in those early days there had been several rather disastrous explosions in the liquid air units in foreign plants.
story of performance under this contract that will be told here. As far as we know, it was the first commercial contract for this gas made anywhere in the world. There were rumors that the Linde Company of Germany had supplied small experimental lots of argon to European lamp companies, but we were never able to confirm whether these deliveries were regular or not, and with the advent of the war all further traces of production seem t o have been lost. It is well known, however, that the Linde Company had developed fractionating apparatus which would place them in a position to supply argon in the form of a mixture containing 40 per cent argon, 40 per cent oxygen, and 20 per cent nitrogen. It is also known that in the spring of 1915 the Linde Company in America had 241
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Therefore, it was decided to install the copper process a t Niagara Falls, on the Canadian side where supplies of natural gas were available for regeneration of the copper. We are now speaking of conditions as they existed in 1908 a t the time of the design of the first Niagara Falls unit. For the production of cyanamide the Niagara ovens were of the usual cylindrical type closed by a removable cover. The carbide was charged into a perforated metal basket, and the basket lined with paper to prevent sifting. A tube of paper was placed axially before the basket was filled with carbide, and this made space for the insertion of the carbon resistor rod which served as a heater for starting the reaction. The reaction itself is strongly exothermic so that the amount of heat supplied is relatively small, even to the point of merely raising a thin skin of adjacent carbide to redness from which the reaction will proceed automatically to completion; naturally it is assumed that the oven is thoroughly insulated against heat losses and that there is a plentiful supply of pure nitrogen. Back in those early days the carbide charged to such an oven was about 900 pounds, and the complete cycle from start to finish lasted about 40 hours, of which 24 hours represented an active period of nitrification. The nitrogen retorts were of steel plate, riveted and welded; each plate was 3 feet 4 inches in diameter and 9 feet high. They were filled with a briquetted mixture of copper roll scale, kaolin, and asbestos, and carried 5 per cent metallic copper. The retorts themselves were built into a furnace structure that permitted heating for starting-up purposes and gave some rough control of temperature either by supplying combustion gas or by circulating air around the shells. Behind each retort was a smaller apparatus which we called a “purifier.” The purifier was made of 12-inch pipe about 9 feet high, and was filled with the same copper mass. Provision was made for externally heating these purifiers by burning gas around them, Assuming the units in operation, the approximate cycle of operations was to pass air slowly through the retorts
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over a period of about 4 hours; the amount of air was roughly 1,000 cubic feet per hour. The bulk of the oxygen was absorbed in the main retort, but to ensure complete absorption the exit gases were passed through the heated purifier. In the regeneration cycle, gas was passed through the purifier t o secure complete reduction and thence to the main retort. Something under 1,000 cubic feet of gas per cycle were required for reduction. The nitrogen produced by this system was contaminated with carbon dioxide. The retorts even a t the low temperature a t which they were operated would crack the hydrocarbon gas and deposit soot in the copper mass. This would be burned during the air phase. The nitrogen gas, therefore, was scrubbed with sodium hydroxide solution, dried by refrigeration, and then passed through lime tanks. The argon passed through the retorts unchanged. In the cyanamide ovens a t that time we were able to utilize only about 50 per cent of the nitrogen led into them, and this was by no means uniform throughout the 40-hour nitrification period. During the starting-up period the ovens were flushed with nitrogen before the heater unit was turned on. Again the ovens were cooled under nitrogen. Consequently both the beginning and the end periods showed rather low nitrogen absorption, whereas in the more active portion of the cycle there were undoubtedly times at which up to 80 per cent of the nitrogen was going into the carbide. These ovens floated on the nitrogen line, and regulation was accomplished by manipulation of a vent in the cover of the oven. During nitrification a number of side reactions took place. The paper liner and tube distilled. Residual water vapor and decomposition products of carbide both produced foreign gas. Consequently the vent gases were not pure nitrogen and argon, but a very complex mixture; for example, taking the most active period of nitrification, about 20 hours after starting, the percentage composition of the mixture was: argon, 6; hydrogen, 24.7; oxygen, 3.2. Nitrogen and undetermined constituents made up the balance. These com-
CYANAMIDE OVENS
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plex waste gases from the cyanamide oven make complications in argon recovery.
Nature of the Problem In the preliminary discussion with Dr. Whitney it was pointed out that the mere collection of the waste gases from the vents of the cyanamide ovens would be of little help in the solution of his problem. Air carries approximately 0.9 per cent argon. After removal of the oxygen, the concentration is increased to 1.2 per cent. The ovens as a whole extracted about 50 per cent of the nitrogen, which would give a maximum concentration of around 2.5 per cent argon. But actually because of the introduction of foreign gases the argon concentration will be less than this figure. Therefore, in the regular cyanamide practice as of that time, argon concentration was hardly worth consideration. It was recognized, however, that during the most active period of nitrification, some 18 to 25 hours after the start of the ovens, there should be a much higher concentration of argon in the vent gases; samples were actually obtained from individual ovens showing as high as 6 per cent of this desired gas. One great difficulty was our lack of a quick and effective means of determining argon concentration. For a long time we were forced to ship gas samples to Schenectady for analysis, and the delay occasioned by this procedure greatly slowed up progress in the development of the most promising method of approach to a solution of the problem. It was not
until December, 1914, that we obtained from Schenectady an apparatus that enabled us to make rapid and reasonably precise determinations. Naturally it occurred to us that we might improve this concentration by connecting cyanamide ovens in series, passing the vent gases from one to the next. Strange to say this did not yield improved results. The gas current picked up large volumes of foreign gases which reduced the nitrogen concentration to a point where it was difficult to maintain temperatures in the ovens because of slowing up of the reaction. We improved this condition, however, by starting nitrification in an adjacent bank of ovens. When they had reached the active period and were at full temperature, we would pick them up and drop them into the series-connected ovens; in this way the heat stored in the hot mass of carbide and cyanamide was utilized to carry on fixation at lower nitrogen concentrations, but even then we had difficulty in obtaining much above 10 per cent argon, calculated to argonnitrogen mixture. The next modification was to break the connections in our series of ovens and insert in the line a small copper purifier such as was used in the nitrogen plant. This was a piece of 12-inch pipe about 6 feet long and filled with copper mass. It was built into a furnace structure and could be heated externally by gas flame. The final arrangement consisted of four ovens in series, then the purifier with its scrubbing equipment, and two additional ovens in series with a second purifier and a scrubbing and drying equipment. We kept
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these purifiers oxidized so that most of the copper was in the form of copper oxide. This would burn the hydrocarbons to carbon dioxide and water vapor, which were removed by caustic scrubbers and lime dryers. With this system we began to approach a 20 per cent argon-nitrogen mixture, but beyond that point we could not go with the cyanamide
ovens. Although the contract called for a gas containing 20 per cent argon minimum, pressure was brought to bear to increase this concentration as high as possible. An additional absorption unit was constructed consisting of a horizontal pipe built into a furnace, into which we charged carbide. This was externally heated by gas and enabled us to continue nitrogen absorption independent of the heat generated by the reaction. We also studied the possibility of catalysts in thc carbide, and finally determined that a mixture of calcium fluoride and calcium chloride did have a beneficial effect when added to the extent of about 10 per cent of the carbide charged into the final absorber. The apparatus, however, proved quite impractical on large-scale continuous operation.
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Solution of the Problem Sitting in the lunch room at Niagara Falls one day, I had a sudden hunch as to a more effective piece of apparatus for final absorption of nitrogen. I picked up a heavy stoneware saucer, such as is ordinarily found in plant lunchrooms, sent it to a local foundry, and had a large number of castings made Kith this saucer as a pattern. A hole was drilled in the center, and we strung these castings on a long iron rod, spacing them with ordinary pipe nipples. Four of these units were assembled. A furnace was built into which four steel pipes were set vertically and arranged for gas heating. These pipes were connected together in series. In operation the crane would pick up the “Christmas tree,” as our string of saucers was called, and lower it slowly into the pipe from the top. A funnel charged with carbide would fill these saucers as they were lowered into the pipe. The caps were replaced, and the unit was put into operation. It required only a few minutes to load such a furnace. This, then, became the tail end of our absorption system, and we
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found we could run the argon content up to 90 per cent and above without difficulty. When the carbide was exhausted, it was a simple matter to lift the saucers from the pipe; the spent carbide was discharged merely by laying the saucers on their sides on the ground and rapping them with a hammer, when they were ready for replacement. This final absorption apparatus was also followed by a copper purifier with its caustic scrubber and lime dryer. Next the gases were sent to the compressor which filled them into the steel bottles in which they were shipped to the lamp company. The plant actually commenced operation and shipment in December, 1914. By March we were producing better than 2,000 cubic feet of argon per month. All told, we shipped a little under 8,000 cubic feet of argon, most of which was better than 80 per cent concentration. From the commercial standpoint we spent about $2,500 for labor and materials in assembling the unit. This included expenditures for alterations during an experimental period and before signing the contract. In addition we borrowed from the storeroom meters and blowers; considerable stocks of this equipment were carried, since they were standard in the nitrogen plant. There was little or no wear and tear upon them during this short period of operation. We received $1.25 per cubic foot for the argon under the contract, and as nearly as the accountants could determine, the operation just about broke even when it was wound up in May, 1915. It has been mentioned that in the discussion with Dr.
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Whitney we did not believe the cyanamide process could offer any solution to this argon problem. The contribution of the routine oven operation as noted was only to double the argon content, hardly enough to make it of moment. From that point 'onward it called for special manipulation, all of which interfered to some degree with cyanamide production. For example, the transfer of a hot can of carbide from one oven to another involved oxidation and consequent loss of efficiency. This amounted only t o 2-3 per cent, but it was nevertheless an item to be considered. Of much greater moment, however, was the fact that the copper process of producing nitrogen had become obsolete by this time. Improvements in the liquid air machinery and a better knowledge of safe operation about a cyanamide plant spelled the end of the copper retort, for the liquid air process could be operated to produce a higher quality nitrogen at about one third the cost of that by the copper process as it was set up a t Niagara Falls. There was under construction a t Kiagara Falls in 1913, a liquid air plant, and as fast as equipment could be installed the copper units were being closed. In the liquid air plant some SO per cent of the argon is discharged with the oxygen; in order to obtain high-purity nitrogen, a cut was made so that the oxygen carried about 10 per cent nitrogen, which rendered it of no value for bottling. It was therefore wasted a t Nagara Falls, along with most of the argon content of the air entering the apparatus. We were all fully aware of this shift in process when we made this agreement to supply argon, and fortunately in the late spring of 1915 the oxygen producers had equipped themselves with auxiliary apparatus to supply argon from the Linde plants. It is probably also true that the quality of argon furnished by the liquid air plant was superior ng that could be produced in the cyanamide plant, since there is no contamination by the miscellaneous lot of hydrocarbons that we picked up in our chain of apparatus. It is a simple matter to remove the oxygen from this liquid air product by burning it with hydrogen to give an argon concentration of a t least 80 per cent after such simple treatment. Fortunately, therefore, since we were desirous of dropping this small operation, other sources of supply were available immediately; probably our greatest contribution was the quickness with which we produced argon and made available sufficient gas to carry on lamp development on a reasonable sized scale. From the technical and scientific aspects this argon venture was not of any great significance. It probably merits attention only as a historical record. Many will probably wonder why such a minor subject should be chosen for this address, But to me there is another angle which has not been touched upon so far.
Early Research Methods
NITROGENRETORT
Up to the signing of that argon contract, the development of the fundamentals in the operating plant had been very slow. There was no great driving force behind it, and when one considers that the gas samples had to be shipped 300 miles to Schenectady for analysis, one can understand the
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period of rapid production of new processes and new products. I believe that that type of association was responsiblefor more of our performance than any other item. Unfortunately two of these men have passed to the great beyond. Now let us contrast this situation with developments years afterward. Many of us have visited the great modern laboratories and marveled at the wonderful equipment, the staff of technicians, engineers, and chemists, and have admired the organization and the way in which it functions. Yet I am quite certain that many of these institutions work much less efficiently from the standpoint of production than we did in the old days with but an infinitesimal fraction of the facilities now available. It is not that they are not producing, for their output is probably, in the aggregate, far greater than anything dreamed of in the old days, but the production seems to be far less efficient when measured in terms of man-hours. What would have happened had Berzelius, or Wohler, or Davy, or Robert Hare been put in charge of one of these modern laboratories? Would he have produced anything like the amount that he did with his meager equipment and facilities available at the time he was most productive? I believe not. I think the same thing would have happened as has often , taken place in some of our institutions where the man who should be turning out constructive work a t the desk or table is so wrapped up in the red tape of an operating organization that his productiveness has been considerably lessened. Fifty per cent of the great chemist's time would have been spent on the telephone answeringabsurd questions from people who were incompetent to ask them and could make no effective use of the knowledge after receipt. Another 25 per cent would have been spent acting as a traffic cop for a multitude of office correspondence that starts somewhere and gets nowhere. And the other 25 per cent with worrying about the detail of a slip-up in storeroom routine when three 5-cent bolts were charged to the wrong job.
AUXILIARY NITROGEN ABSORPTIONEQUIPMENT
Need for Less Formal Research Units relatively slow progress in these early stages. But when two commercial men had signed a contract to produce something that neither knew very much about and under specifications far beyond anything that had yet been attained in the unorganized exploratory work, there was an entirely new aspect. It was a strong moral, if not a legal, obligation t o make good. But even at this point the argon venture was only an incident, for two much more important problems had to be solved at the same time, both resulting in large operating units to be completed and put into operation before the summer of 1915, and both concerning entirely different materials. The war in Europe was forcing performance on a record scale and at a record pace. The technical staff responsible for this pioneer work was composed actually of only four men, an experienced operator, a construction engineer, a designing engineer, and myself. We could draw some assistance from the control laboratory at the plant for simple chemical work, mainly analytical. The plant could, of course, supply mechanics, millwrights, and 8ome shop facilities. I believe our great success, however, was due entirely to the fact that there were only four of us working without the burden of formal organization. There was no red tape, We were not concerned with burdensome reports for the education of uninformed executives, in fact with anything outside of production of sketches, of building the units, and of putting those units into operation. As soon as they turned over, we moved to the next problem. We all used the same office room, we were frequently using the same desk, and I might almost say we lived together during this
I have gone through many of these laboratories and found the best chemists and most productive minds so entirely devoted to matters of office routine and corporate red tape that little time was left to chemical production. That detail needs to be left largely to the younger and less experienced individuals. Kow do not mistake me and think I am critical of all organization, but I have seen many examples of just exactly the situation set forth here. The remedy would be to turn the laboratory upside down, put the youngsters in the front office, and let experience retire to the rear rooms without telephone and without messenger service. They might not produce more, measured in quantity, but I believe it would be better quality, with much less expenditure in man-power, both of which mean quicker results. It is not a problem that is difficult of solution, and some of our large institutions have gone a long way towards creating a less formal research unit, more nearly approaching the seminar of our old school days. Get the creative chemists somewhere near the bench, and leave the front to the nontechnical men entirely. I recognize that control of large institutions with their enormous annual expenditure is quite necessary. I also believe that in many cases we have placed that policing too much in the hands of our best technical men and have diverted their attention far from the lines of their most productive work, As individuals we have become slaves to the diagrammatic picture of control and have bowed down to the idol of the little square block towards the top of the list because we thought it carried a more imposing title than those towards the end of the row where the titles are frequently missing. Our best chemists, to whom we should pay the highest commensu-
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rate salaries, should not be burdened with responsibility for details of the conduct of the institution. That should be left entirely to nontechnical men and to the younger technicians, who could, in turn, graduate from the front office into the working quarters; with each graduation they should be relieved of more and more of the routine of operation. My ideal would be that the top men who have attained their position in such an institution would be found together in the same room somewhere on the rear top story of the laboratory, so surrounded by buffers that it would be a real task to disturb them. I would not make reception clerks, guides, and information clerks out of them; they probably would have irregular time clock records, for they would be encouraged to make outside contacts of their own selection and to feel perfectly free to bring into their shop friends of their own choosing. In brief, turn the laboratory upside down. Years ago I had this brought to my attention forcibly by one of our greatest industrial leaders now unfortunately about
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to retire. On taking over a large institution that had run down badly at the heels, he practically reassigned the entire directing staff, taking men from the drafting tables and shops and putting them into executive positions, and vice versa, always with the remark that the trouble with the institution was too much overhead which is unproductive. Some of the best superintendents were doing clerical work in the office, and some of the best office men were in the shops. That is the situation we sometimes face in our own work of a grossly overbalanced organization of highly paid desk workers when what we really need is a much higher grade of man at the laboratory bench.
Nationalized Research An interesting situation is now confronting the world. One of the great European nations has nationalized research. This country is about to try it. In general, when politics come into the picture, the politician occupies the fro& office and 'the technical worker the back office. One should expect from such an organization, if my thesis is correct, some rather effective work. As a matter of fact, there has been a great deal of effective work turned out from these institutions; if measured by the expenditure in man-hours, or preferably in man-hourdollars, I am not certain that it will not outrank many of our private research laboratories. We must remember that many of these state institutions are handicapped by maximum salary limits and other considerations that give them poor chance in competition with the private laboratory. Some time just check up production of the technical worker on the basis of man-hourdollars in a state institution. I still believe that this nationalized research, if organized along the classic political pattern, is something to be reckoned with, for the bench worker will have nothing but bench work to do if he is chosen under the civil service merit system, and under the unusual conditions that exist today in our country, some of our laboratories will have to bow to nationalized institutions. I really do believe that the small informal organization that carried us through the early days of the war,.when we were called upon to turn out process after process to make products formerly imported, was the ideal setup. I am quite certain that the lack of any elaborate laboratory facilities forced us to intense analysis of our problem; this carefully engineered process had to bear the scrutiny of a construction engineer and an experienced operating man as to every step (I might say almost from nail and bolt), which certainly worked for speed of accomplishment. Under the unusual conditions then existing, when every emphasis was laid upon early production and not so much upon cost, this type of organization could not be excelled. Under the more highly competitive postwar conditions we should probably have taken advantage of slightly more laboratory work in many of our ventures. Nevertheless a number of them are still working today, among which, however, is not the argon project, for the very good reasons stated. R ~ C E I Y BDecember D 28, 1938.
