338
f
T H E J O U R N A L OF I N D U S T R I A L A N D EA'GINEERING C H E M I S T R Y .
May, 1912
ORIGINAL PAPELRS
I believe t h a t we can safely give credit to the steam process people for the possibilities of the turpentine In taking up the subject of wood distillation, I extraction from fat pine wood. I do not remember wish t o sap in the beginning that, like every one else, its production prior to their activities, and certainly I am subject to correction and am anxious to profit not of good quality and in commercial quantities. by the experience of others. I t is only by so doing This steam process with its variation held out many t h a t we accomplish anything. There have been possibilities to us all a t first, but I regret to say that, many improvements in the art of wood distillation from my own observation, it has not proved commersince I first began the work, and I know of no industry cially successful, save in a few cases. Within the last few- years still another process has which, in so short a time, has made such marked strides and which merits so much investigation and been evolved, which, while not new, still, as applied t o the extraction of the products from pine wood, criticism. I n 1904 I prepared a paper for the Scientific A4unerican was novel. I refer to the solvent process, for which Supplement, in which I gave credit for the first com- great things are claimed. mercial work in the distillation of Pine Wood to James By this process the wood to be treated is first Stanley, who built a small commercial plant in %'Tilshredded, or hogged, as it is called, and then subjected mington, N. C., in 1872. This plant was not a suc- to the solvent action of naphtha or some other volatile cess in the hands of Stanley, and was shortly after solvent. The solvent combines with the resinous taken over by two gentlemen of Danish birth, who extracts and the resultant liquid is then drawn off were somewhat familiar with similar work which and subjected t o a fractional distillation. The solwas being carried on in their Motherland. One of vent is recovered and the products are .then refined. these men is still living and is actively engaged in The solvent process is claimed by many to be the the work to-day. I speak of Mr. L. Hanson, who most profitable, and I know t h a t large sums are being is President of the ,Spirittine Chemical Company, of spent for the erection of plants using this process, Wilmington, N. C. I have always held, however, t h a t there is but one I t is rather a striking coincidence t h a t the first, method for the utilization of wood waste in the form and I may say the last plant, has been built in Wil- of fat light wood; and t h a t is to completely utilize mington, and the last one within a few feet of the the raw material. I n no other industry would we former location of James Stanley's plant. This last find such a condition as exists where the steam process plant, which is by my process, I shall describe later. and the solvent process are in operation. The process, as started by Stanley and carried out The taking of a raw material and the extraction by X r , Hanson, was the old crude method of Destruc- of but a proportionately small part of its valuable tive Distillation, which consisted of a series of retorts contents and then throwing the remainder away, with condensers attached, set up in brick work with is a poor proposition, no matter how you look a t it. furnaces beneath. The wood was placed in the retorts I believe t h a t every man who has ever turned his and the doors closed, fires were started in the furnaces attention to this art, has realized from the beginning and kept up until distillation ceased ; the retorts were t h a t the one great essential to be sought was temthen allowed td cool and the charge was withdrawn. perature control during all times of the distillation. No attempt was made to control the temperature Many methods have been tried to solve this question, during distillation and i t was not until years later and I feel reasonably sure that it has a t last been t h a t the possibilities of varying products, depending successfully worked out. on the temperatures, were thought of. By this old I refer now to the plant I have just completed for method, many different degrees of heat existed in the National Wood Distilling Company, of which I the retort at the same time, and i t was a noticeable a m an officer. I n describing this plant and the method fact t h a t the top of the retort myas many degrees used, I ask t h a t I be allowed t o indicate the weak points hotter than the bottom or sides; the loss of heat was in the other processes, as each of these was of assistvery great as i t was necessary to heat up the brick- ance to me in developing the new and successful work before distillation started. There was no at- process we have. tempt a t first to refine or separate these products; Let us take up the old destructive process and see they were pumped into storage tanks and used for how i t bears a rigid analysis: First, for its good the preservation of timber, a creosoting plant having points (and 1 wish to say here t h a t nearly every plant been built nearby, and the creosoting of timber was t h a t has been a financial success has been of this type), a part of the Company's business. the destructive process does utilize the raw material I do not believe t h a t any one, a t this time, even and it does produce far greater yields than any other thought of the possibilities of there being turpentine process, the average production from a cord of good in the products of distillation. I can well recall the wood by the old destructive process being approxitime when such a theory would have been hooted a t . mately twenty gallons of turpentine, ten gallons of Read before the New York Section of the Society of Chemical Industry, light oil and seventy gallons of heavy oil, with a residue March 22. 1912. SOME RECENT DEVELOPMENTS I N WOOD DISTILLATION.' B y THOS.551. PRITCHARD.
May, 1912
T H E J O L R S A L OF I i Y D L - S T R I A L A N D E-YGIAYEERIAYGC H E X I S T R Y .
of twenty-five bushels of charcoal t o the cord. I do not include either alcohol or acetic acid, as their value is slight and varied, and I may say t h a t very few plants distilling resinous woods have found i t of advantage to utilize these products. The first cost of this style of plant is not great in comparison with others, and the expense and difficulty of hogging wood is not a factor. The weak points in this process are, however, serious defects: First, the lack of temperature control in the retort results in the formation of all sorts of compounds which distil with the turpentine and con-
C05lnIERCIAL
3\39
In summing up the good and bad points we may say t h a t the old style destructive process gives us good yields a t comparatively lorn cost, but the products are of inferior quality, the cost of maintenance high and the fire risk great. In addition to this is the factor of time, as it takes very much longer to handle a quantity of wood by this process than by others. In considering the steam process, we must give it credit for the quality of turpentine produced, and for the essential idea in wood distillation, the temperature control. V e must, however, admit t h a t a weak point
FLANT-RETORT.
taminate i t ; and this same lack of heat control results in a large percentage of the heavy products being burned in the retort. Any one who has ever operated a plant of this type will readily recall the deposit of carbonized matter which has t o be cut out of the retort after a short usage. Secondly, the very high temperatures to which the average destructive plant is subject means a comparatively quick wear-out and very heavy up-keep, as well as an enormous waste of fuel. Third, the fire risk in this style of plant is very great, so high in fact, t h a t no insurance company will accept il. plant of this type as a risk.
in this process is the very small proportionate yield of products; secondly, t h a t i t does not utilize the raw material to the fullest extent, as a major part of the products of the wood are not extracted, thus necessitating the use of an enormous quantity of raw material to accomplish any great results. There have been all sorts of claims as to the quantities produced b y this process, but after very careful investigation, based on the report of men who are engaged in this line of work, I am forced t o the conclusion t h a t from six to fifteen gallons of turpentine, and from two to four gallons of pine oil is the minimum
340
.
T H E ' JOL7RA\7AL OF I A - D U S T R I A L A N D E , Y G I S E E R I S G C H E M I S T R Y .
and maximum yield for a cord of fat wood, the variations in quantity being due t o the difference in quality and treatment. The expense of production b y the steam process is high; t h e waste of raw material is enormous a n d without reason. We may, therefore, grant t o the steam process an excellent quality of products, with safety of operation so far as fire is concerned, and a t the same time we must condemn i t for the poor yields, cost of operation and waste of raw material. Within the last few years still another process has been evolved. I refer t o the Solvent Process, for
COMMERCIAL PLANT-SHOWING
which great things are claimed. I am inclined to think from what I can learn t h a t the solvent process possesses considerable advantages over t h e steam process in quantity of production. I also believe t h a t the quality of the turpentine is equally as good, and this process also produces a good yield of rosin. There is still, however, the objectionable feature of a very high fire risk, comparatively high cost of operation and failure t o completely utilize the raw material. The ideal process for the distillation of wood, we may then admit, must possess the following essential features : First, definite control of the temperature during the entire process of distillation; Second, a
May,
1912
maximum yield of products; Third, products must be of good quality; Fourth, cost of operation must be comparatively lorn; and Fifth, the fire risk must be minimized as far as is possible. I a m going t o try to describe a plant which we have recently built in Wilmington, N. C., within a few feet of the original plant of James Stanley. When I first began work on wood distillation, I realized t h a t temperature control was the one great issue. I tried experiment after experiment to achieve this, and a t last discovered t h a t b y utilizing the old chemical process of the oil bath, I could get very
STORACE
TANKCONDENSERS. ETC.
definite temperature control a t comparatively high temperatures. I had great difficulty for a long time in getting a n oil which would stand repeated heating without cracking. I finally found, however, a very high fire-test petroleum cylinder stock, which could by heated t o six or seven hundred degrees F., without trouble, provided air was excluded. With this fact as a starter I developed our present process, which I will now t r y t o describe. I can best do this perhaps, by first describing a miniature plant complete, which I had built last year, and in which I ran continuously ninety-six charges. I n the construction of this small plant, I
usctl tn'o pieces of pipe: the inner shell \\--aseight inchrs in diameter b y txenty-four inches in length ; the outer shell enclosed this, leaving an intermediary space of one-half inch. The ends of this space. of course, were tightly closed. From the inner shell an outlet pipe passed through the space and through the outer shell and connected with an ordinary worm, the condenser. Into the bottom of the outer shell a t one end entered a half-inch pipe, with t h e take-off at the bottom at t h e other end. Connected with this entrance pipe was a small gas hot-water heater, and from the bottom of this hot-mater heater, a pipe led to' a small rotary pump, and from t h e pump t o a small steel storage tank. The outlet pipe from the bottom of the outer shell opposite end of t h e inlet pipe led directly t o the top of this storage tank, which was enclosed. By means of the small rotary pump, t h e bath oil contained in the storage tank was forced through the gas hot-sv::tcr heater, taking the place itpied b y t h e water in t h e t h a t would originally bv PI.same, and from there n.:!lt into the intermediary space entering a t the h,.ttom. and was circulated around the inner retort, f a d i n g its .outlet a t the bottom of the outer shell farthest away from t h e inlet, from there passing back t o the storage tank through the pump around the retort and so on, thus keeping a continual circulation. Between the inlet pipe and outlet pipe I had a pipe of similar size connected with suitable valves, so t h a t t h e oil could be by-passed and the retort circulation completely cut off. I also had a reserve tank filled with cold oil, which allowed me t o introduce cool oil into the circulation a t a n y time. B y means of increasing or decreasing the speed of t h e pump, opening or closing the valves used by passing or introducing cold oil into the circulation, I found i t entirely practicable to control the temperature absolutely. TVe used in this small retort twenty pounds of wood at a charge, and estimating the weight of a cord of good rich wood at four thousand pounds, we had no trouble in getting a pretty accurate approximate average of the production b y this process. I must confess t h a t t h e results of this exj, rimental p1ar.t were far beyond our most sanguinc expectations. We kept a record of every charge and our average for fifty charges was thirty-six and a fraction gallons of water white turpentine, ten gallons of light oil, and one hundred and twenty-five gallons of heavy oil. I have xi-ith me one or two of these record sheets which I shall be glad t o show.. T1-e found t h a t we had no trouble whatsoever in getting complete and uniform carbonization, so complete, in fact, was the heat distribution b y this method t h a t a solid stick of timber eight inches in diameter and of the iength of the inner shell was charred through and through. I n operating this model we discovered t h a t b y varying the temperatures, we could produce varying products. TTe also discovered t h a t b y drawing off t h e liquid contents of the retort after the turpentine had been distilled we could produce large quantities of an excellent grade of rosin. I n fact, one of the main features of this process is its extreme flexibility.
Our commercial plant, which we have just completed and which is now in daily operation, is an exact duplicate of the model, except for the fact t h a t the space for the bath oil is proportionately about three times as great. The large retort has a n outside tiiameter of five feet, with an inner shell of three and a half feet, and a length of twenty-eight feet. This gives LIS nine inches of oil space between the inner and outer shells. For heating the oil bath me use a continuous coil of electrically welded pipe, containing 3 5 0 lineal feet. This pipe is set in a specially constructed furnace so t h a t m-hile not in direct contact with the fire, it yet gets a maximum amount of the heat. The results of this large retort have checked absolutel>- with the model, and we see no reason why i t should not continue t o do so indefinitely. I used the same oil bath in the model for ninety-six continuous charges, and, so far as we are able t o tell? the bath oil is in exactly the condition to-day as when first p u t into service. The low cost of this oil and its long service make i t an ideal menstruum for conveying the heat. I n operating this plant, we run the wood into the inner shell of the retort on cars, the doors are closed, and a steam jet is opened with leads into the inner shell. This is done t o force-out t h e cold air and so hasten the heating. The oil bath is then circulated from the storage tank b y means of a low pressure pump through t h e heating coil, and so t o the retort where i t fills completely the space between the inner and outer shells forming a blanket of hot oil with a uniform temperature, passing out at the bottom of the retort and back to the storage tank. TVe control the temperature so t h a t the inside heat shall not exceed 450 degrees F., until we have distilled off all the turpentine and pine oil ; we then allow the temperature t o slowly rise until we have fractionated the light oil, and it is just at this point t h a t destructive distillation begins and fractional distillation ceases. lye, find t h a t at approximately 480 degrees F. we begin t o get the distillates with the distinctive empyreumatic odors. The temperature is held below 5 2 5 degrees F. until all the light oil is over and then all'Jwed t o increase as fast as possible. TVe find t h a t ;it a maximum temperature of 610 degrees F. in the ;liner shell, we can get complete distillation of all the prcducts, leaving us dry charcoal of excellent quality. At this temperature we find t h a t our bath oil is a t a temperature of 6jo degrees F., which is as high as we generally carry i t , though we have gone as high as 7.50 degrees F., without trouble. I do not hesitate t u say t h a t this process is the most accurate, and the apparatus the most scientific ever evo!veci for this work, and the results prove i t . A t no stage of the process is it not under perfect control and the teniperature can be rnised or lowered a t will. We have found b y actual tests t h a t we can hold t h e temperature of the oil bath a t any given degree as long as may be desired. The time consumed in running a charge by this process is comparatively shorter than b y any other; it takes longer than a steam process plant, b u t when the difference in the
342
T H E JOC‘R-VAL OF I S D L - S T R I A 4 LA4~YD EAYGI.YEERI-YG C H E 3 I I S T R l ’ .
production is taken into account, this comparison is in our favor. We actually begin distillation as soon as the wood goes into the retort, as the oil bath is carried t o about three hundred and fifty before the cars of wood are run in. After the charge is over, instead of having t o wait many hours for the retort t o cool, we mechanically assist the cooling b y pumping cold oil through the heating chamber. The fire risk is also a slight danger b y this process, and I may say right here t h a t an examiner for one of the leading companies in America has classed our plant as a comparatively safe risk, and is willing t o write us a t a very fair rate of insurance. I n regard t o the quantity and quality of the products produced b y this method, let me say t h a t both the turpentine and oils are of a very high grade as the samples I have with me show. The analysis of the turpentine shows i t t o be of remarkable quality. The production is far greater t h a n b y any other process with which I a m familiar. This is best shown b y the records of charges which show not only the yield b u t the temperature a t which each product was distilled. This daily record gives an absolutely accurate record of the varying temperatures, both of the oil bath and the inner shell or distilling space. We also get the exact periods and temperatures a t which the distillates change in nature. We may, therefore, grant t h a t we have accomplished: first, temperature control ; second, the complete utilization of the wood ; third, a maximum amount of products. This being granted, let us see what the quality is, and also consider the cost of production. I n taking up the question of quality, I wish to say t h a t i t is hardly a fair comparison t o consider the products made b y this process against the old destructive ones, as they seem distinctly different. The turpentine as the following analysis shows is very close to the very best gum turpentine, so close, in fact, t h a t b u t for one feature it would be indistinguishable; I refer now t o the pine oil contents which I may say is the one means of classifying wood turpentine as against gum turpentine. The presence of this product, even in very small quantities, raises the average of the boiling points in fractionation. I believe I a m correct when I say t h a t this is the one distinction in even the very best wood turpentine. I a m glad t o say t h a t I a m now working on a method of refining which seems t o promise a n easy and economical method of extracting even the slightest quantity of pine oil from refined turpentine. If this can be accomplished, I do not believe i t will be possible to distinguish good wood turpentine from t h a t distilled from the crude gum turpentines. The following analysis of our unrefined product was made b y J . E. Teeple, of New York City: Color-slightly yellow. Leaves no stain on paper. Specific gravity a t 16O C -0.865. Distillation 5 0 per cent a t 160’ C. Distillation 80 per cent. a t 163 O C. Distillation 8 j per cent. a t 164 O C. Distillation 9 0 per cent. a t 16 j . j O C.
Nay, 1912
Distillation 9 j per cent. a t I 7 2 O C. Non-volatile matter a t I O O O C.-0.03 per cent. Flash-point---108. j O F. Insoluble in sulphuric acid 2 . j per cent. Odor-Contains a noticeable odor foreign t o turpentine and very similar t o creosote. This odor is usually removed by shaking with dilute alkali. The turpentine is slightly acid b u t this acidity is easily removed b y shaking with dilute alkali. Iodine absorption No. 375. I n comparing the oils produced b y this process, I cannot do better than t o show samples of each of t h e distillates, both in crude form and as we refine them. It \vi11 be noticed that the heavy “and light oils are very much brighter in color, and have a much milder odor than the ordinary destructive distillates. This is due in part t o the fact t h a t they are not burned, and are taken from the retort a t their normal distilling temperatures. I have many times seen oils made b y the old destructive process so black in color and so high in odor t h a t they were hardly worth marketing, and this T ~ unquestionably S caused by exposure t o excessive temperatures. I want especially t o call your attention to the samples marked “ X ” , “ X X , ” and “ X X X ” oils, also the one marked “XI,.” These oils are the products of special processes of refining which we have worked out, and they seem to compare very favorably with the better grades of rosin oil. They do not, however, analyze as such. We have had these oils tested out for the commercial purposes t h a t rosin oils are used for, and they seem to serve admirably. They can be produced a t much less cost. The oil marked “XI,” is worthy of notice because of the fact t h a t i t is practically odorless. I n addition to this, it seems to have rather remarkable drying properties, and made into paint shows excellent wear. We have had paint samples in service €or seven months or more, and the results as compared with pure linseed are very favorable indeed. Only the darker shades could be produced, however, as the oil darkens any light pigments. There is n o question but t h a t this oil will be of great value in making up a cheaper grade of paints for such purposes as freight cars and rough work generally. I n speaking of the refining of the oils produced from the distillation of pine woods, I would like t o say t h a t hardly anything has been done. I have perhaps gone as far along this line as any one, and have made, perhaps, as many as seventy-five distillates. I believe t h a t this work alone offers a wonderful field for the research chemist, and i t has always been a matter of wonder to me t h a t some of our men who have the time and means to take this up, have n o t done so. I feel sure t h a t no field before us to-day offers greater opportunities for discovery. The subject is so vast in scope t h a t i t is with great difficulty t h a t I have been able t o limit m y paper to a reasonable time. I feel t h a t I cannot close without saying just a few words relative t o the possibilities of the distillation of pine wood. There are t o d a y millions of cords of wood lying on the ground rotting, and there is a money
May, 1912
T H E JC)LR.\7AL OF IAYDCSTRI.-IL A-1-D E-VGILITEERIA-GC H E L U I S T R Y
value of approximately twenty-five dollars in each and every cord of this wood. There are every day thousands of cords of rich pine wood burned a t sawmills t h a t have an equal money value. The distillation of pine wood is not an industry which requires large capital. Plants may be built for comparatively small amounts t h a t will pay good dividends. There is a n unlimited demand for all the products and a t prices which will pay handsomely. Many plants have failed, i t is true, but every failure can be safely attributed to lack of knowledge of the industry, lack of capital or a poor process. I f a n y men have gone into the business thinking t h a t they could get fancy prices for the products and have been disappointed. X steady sale a t a reasonable profit is all t h a t can be expected. There is, however, a steady demand for all of the distillates now, and this demand is growing dailj-. The question of timber preservation has become a vital one, and when the fact t h a t the heavy wood oil is even more valuable than dead oil of coal tar for this purpose becomes generally known, there will be an unlimited demand for this product. I have had offers from users of timber preservatives for very large quantities of the heavy wood oil, provided i t could be furnished in sufficient quantity and a t a low price. So far this has been out of the question, as one large R. II, P.M.
'. ''
2.00
"
3.00 4.00 4.30
" "
''
I' 1 1 ~
A.M " lL
'I
'( M.
1 . 0 0 P.M. 2.00 " 3.00 4.00 5.00
.
573 605 600
"
5000 543 566
1 1
> 23%ozs.
i1
2;
632 641 j 648 1 677 I 680 670
1
turps.
7 02s. light oil 66 02s. heavy oil
5, 191 1.
2 0 Ibs. wood. Inside.
7.30 5.36 9.00 10.00 11.00 11.55
A.M.
12.57 2.00
P.M.
P i r t started Turps started.
'I
........
Outside.
355 O 41 1
449 474
'I
"
"
546 590
"
3.00 3.35
light oil
598 600 Calculated t o Cord Basis.
"
.....................
72 02s. heavy oil 4 % lbs.
27, 1911.
2 0 Ibs. wood. Inside. Fire started 400' Turps. s t a r t e d . . , , , , , 429 460 492 502 545 562
"
374' 436 476 517 526 540 552 563 600 605 600 Calculated t o Cord Basis.
Charge No. 79-July
................
7 .oo 8.15 9 00 10.00 11.00 12.00
Outside.
Fire s t a r t e d Turps s t a r t e d . . . . . . . .
.................... 28 bushels n off.. . . . . . . . . . . . . . . . 20 gals. Crude turps. . . . . . . . . . . . . . . . . . . . . . 36.71 gals. : . . , . . 1 0 . 9 3 c' . . . . . . 103.12 "
19, 1911.
20 Ibs. wood. Inside. Outside. 7 . 1 5 A.M. Fire s t a r t e d 8.30 " Turps. s t a r t e d . . . . . . . . 376' 485' 9.30 '' 430 520 10.30 " 465 526 20% 02s. 1 1 . 3 0 '' 476 544 turps. 1 2 . 3 0 P.M. 485 541 1.30 " 512 583 } 2.30 '' 550 640 10 02s. 3 . 0 0 (' 550 672 light oil 4.00 596 675 67 02s. 5.00 " 612 674 heavy oil 5.30 " 610 670 J Calculated t o Cord Basis. Charcoal. ....................... 28 bushels Residue.. ....................... 15 gals. Crude light oil.. . . . . . . . . . . . . . . . . . 1 5 . 6 2 gals. 32.03 " Crude t u r p s ..................... Crude heavy oil. 104.68 " Charge No. 47-3tay
9, 1911.
20 Ibs. wood.
Calculated t o Cord Basis.
Charge No. 40-May
1912
Calculated t o Cord Basis. 30 bushels Charcoal., . . . . . . . . . . . . . . . . . . . . . . . Residue drawn off.. . . . . . . . . . . . . . . . 20 gals. Crude t u r p s . . . . . . . . . . . . . . . . . . . . . . 5 0 . 0 0 gals. " light oil .................... 10.93 " " heavy oil . . . . . . . . . . . . . . . . . . . 101 56 ''
13, 1911
20 Ibs. wood. 7 .30 8.45
May,
450'
11
525 565
27% 02s. turps.
596 622 642
J
637
1 6 2 % 02s.
1
1
heavy oil. . . . . . . . . . . . . . . . . . . 112.50
"
Charge No. 82-July
10, 1911. 20 lbs. wood. Inside. Outside.
1
6; 1
Calculated t o Cord Basis. Charcoal.. . . . . . . . . . . . . . . . . . . . . . . Residue drawn off.. . . . . . . . . . . . . . . Crude t u r p s ..................... Crude light oil. . . . . . . . . . . . . . . . . . Crude heavy oil. . . . . . . . . . . . . . . . . . Charge, No. 50-1Iay
'' Outside.
5 % 02s. light oil
heavy oil
25 bushels 40 gals. 4 2 . 9 6 gals 8.59 " 9 i .65 ''
7.10 5.20 9.00 10.00 11.00 11.40 1.00 1.10 2.00 3.00 4.00
31, 1911.
A.>f. "
Fire s t a r t e d Turps. started
1
33 ozs. turps. 551 I 29 02s. water " 560 J I' 593 9 02s. light oil P.M. 630 1 0 % 02s. water 631 " 50 02s. heavy oil " 26 02s. water 579 644 Calculated t o Cord Basis. 30 bushels Charcoal.. ....................... 35 gals. Residue., . . . . . . . . . . . . . . . . . . . . . . . . Crude t u r p s . . . . . . . . . . . . . . . . . . . . . . 51.56 gals. '' light oil . . . . . . . . . . . . . . . . . . . . 14.06 " " heavv oil . . . . . . . . . . . . . . . . . . . 78.12 " "
('
448 477 498 542 546
]
20 Ibs. wood. Inside. 7 . 0 0 A.M. 8 05 "
9.00 " 1 0 . 0 0 '' 11.00 " 1 2 . 0 0 11, 12.20 P . M . 1 .oo " 1 30 '' 2 .oo " 3 .oo 3 30 'I ('
Fire s t a r t e d Turps. s t a r t e d . . ......
388'
425 455 481 501 515 532 543 572 610 614
Charge No. 90-Aug.
Outside.
5r
1
540 ' 571 583 j
32 02s. turps.
;2: )
hgYoil
643 655 684 675
65 02s. heavy oil
1
'1
8.25 10.08 11.00 12.00 1 .oo 2.00 3.00 4.00
5 .oo 5.30
A.M. " "
M.
P.M. " " I'
" "
12, 1911.
20 Ibs. Western wood. Inside. Fire started Turps. s t a r t e d . . . . . . 397' 414 439 459 456 551 606 637 631
Outside.
495 511 562 622 702 652 686
]
Fuse b u r n t o u t 381/4 02s. turps.
1
02s. water 10 02s. light oil 5 % 02s. water
1
27
1 9032
02s. heavy oil 02s.
acid
Charge ?io. 2-Continued. Temuerature
Gals Refined Products. 40 0 W, \\'. turpentine . . . . . . . . . . . . . . . . . . . . . . . . I 5 Second turpentine.. . . . . . . . . . . . . . . . . . . . . . . 10 5 Light oil.. . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3 1 Light product, S o . 1 . . . . . . . . . . . . . . . . . . . . . 2 7 Light product, N o . 2 . . . . . . . . . . . . . . . . . . . . . 87 5 Heavy oil.. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Refined t o e x t r a heavy o i l . . . . . . . . . . . . . . . . . 40 6
Time. 9 . 0 0 A.11. 1 0 . 0 0 '/ 11.00 1 2 . 0 0 \I. 1 2 45 r' >I
........
11 ( 2 s .
Time.
TESTS ON COMMERCIA1 1' .ANT Charge No. I--March I Y . I Y I ; 4653 lbs. wr .:, 'I'cmper,t,~re. I.
Time. 5 . 1 5 A.M. 6.30 " 6 . 4 3 '' 8.00 " 8.00 " 8.17 9.15 " 10 07 '' 10.15 " 11.05 " 1 2 . 0 0 M. I .oo P . M . 2.00 I' 3.00 " 4.00 " 5 . 0 0 c' 5.20 " 6.12 '' 6.30 '' 8.34 " 9.35 " 10.33 " 11.34 " 1 2 . 3 3 A.M. 1.35 " 2.22 3.30 " 3.55 " '(
Changes. Ret,?rt Pumps s t a r t e d . . . . . . . . . . Steam turned in r e t o r t . , . . Oil turned in retort below.
.
,'I1
output.
726" 260
217 Steam cut off, . . . . . . . . . . . . 2 I7 218 225 Cut o u t t a n k . . . . . . . . . . . . . 255 276 309 332 366 380 425 445 480 486 5 02 550 563 575 562 558 559 555 557
27ZL 315 345 393 440 477 520 549 559 587 596 605 63 1 646 649 646 643 643 645 645
33 gals. turps.
20 gals. light oil
'rimc. 7
,
[',
"
s
(10
'(
2 i :O .62
Oil. 576 587 599 604
Charge stopped, leaky pipe 47 , 2 1 gals. pitzh Charge N o 3-11arch
4.31 Ibs.
Gals. ;o 39
Crude turos.. . . . . . . . . . . . light oil.. heavy oil . . . . . . . .
Retort. 504 504 512 504
((
135 9 Calculated to Cord Basis. C h a r c o a l . , . . . . . . . . . . . . . 950 lbs. Residue . . . . . . . . . . . . . . . . 138 "
Changes.
FRERICHS.
Received January 5 , 1912.
Output
33 gals. crude turps.
10 gals. light oil
As a n example of improving an established process of manufacture, I have selected some work which I did about thirty years ago in connection with the manufacture of chloroform. At t h a t time chloroform was made from tax-paid alcohol and bleaching p o ~ der. The acetone process mas then little known but was developed about five years later superseding the alcohol process on account of its greater cheapness. But since we now have tax-free alcohol for manufacturing purposes, the old process has gained interest again, and this is one of the reasons why I have looked u p old records in order to show what can be done with the alcohol process. In the year 1883 I was in charge of a chloroform plant, comprising six cylindrical stills standing on end, each still being 6 feet in diameter and 8 feet high. Each still was connected with a condenser consisting of a lead coil and a receiver t o catch the resulting chloroform. A flat iron box, t o mix the bleaching powder with water, was over each pair of chloroform stills. The general arrangement of the apparatus was as given in Fig. I. Address read a t t h e Annual Meeting of the American I n s t i t u t e of Chemical Engineers, in Washington. D. C . , December, 1911.
