The J o u rn a l of In d u strial and Engineering Ghemistry
P u b l i s h e d b y T H E A M E R I C A N C H E M I C A L S O C I E T Y
Volume Y FEBRUARY, 1913 No. 2
B O A R D O F E D I T O R S
Editor: M . C. W h i t a k e r
Associate Editors: G. P. Adam son, E . G. B ailey, H. E . Barnard, G. E . B arton, A . V . Bleininger, Wm. Brady, C. A . Brow ne, F. K . Cam eron, F . B. Carpenter, C. E . Caspari, V . Coblentz, W . C. Geer, W. F. Hillebrand, W . D. Iiorn e, T . K am oi, A. D. L ittle , C. E . L ucke, P. C. M cllh iney, W m . M cM urtrie, J. M. Matthews, T. J. P arker, J. D. Pennock, W. D. R ichardson, G. C. Stone, E . T w itchell, R . W ahl, W. H. Walker, W . R. W h itn ey, A. M. W right.
Contributions an d c o m m u n ic a t io n s s h o u ld b e a d d r e s s e d to th e E d ito r, M. C. W h ita k e r, C o lu m b ia U n iv e r s it y , N e w Y o rk C ity P u b lish e d m o n th ly . S u b s c rip tio n p ric e t o n o n -m e m b e rs of th e A m e ric a n C h em ica l S o c ie ty , $ 6 .0 0 y e a rly .
F o re ig n p o s ta g e , sev e n ty -fiv e c e n ts , C a n a d a , C u b a a n d M exico e x c e p te d .
E n tered a s S e c o n d -c la ss M a tt e r D e ce m b e r 19, 1903, a t th e P ost-O ffice a t E a s to n , P a ., u n d e r th e A c t o f M arch 3, 1879.
Es c h e n b a c h Pr i n t i n g Co m p a n y, Ea s t o n, Pa.
TABLE OF CONTENTS Ed it o r ia l s:
Cooperation am ong Chemists and M anufacturers . . . . The Present State of the A rt of Industrial M anagem ent Or ig in a l Pa p e r s:
The Hydrogenation of Oils. B y Carleton E l l i s ...
Boron: Its Properties and Preparation. B y E . W ein- tra u b ...
Acetylene Solvents. B y Joseph H. J a m e s ...
Tests on the O pacity and H iding Pow er of Pigm ents.
By G. W. Thom pson...
An Application of the E lectric R esistance Furnace to the Determination of O xygen in Iron and Steel.
By R. H. M cM illcn...
The Volumetric Determ ination of Manganese in R ock, Slags, Ores and Spiegels. B y F. J. M etzger and L.
E. M arrs...
Antiseptic Tests of W ood Preserving Oils. B y A . L.
Dean and C. R . D ow ns...
The Oxygen Absorption T est for Linseed Oil. B y Hans M annhardt...
A Rapid and A ccurate G ravim etric Method for D eter
mining M ilk-Fat in E vaporated Milk and Milk orders. B y E. P. H arding and G u y P a rk in ...
rv7 C ^ e Reaction of N itrous Acid and Urea in dilute Solutions. B y W . D. Bonner and E. S.
Bishop... ..
The Influence of a Preceding Crop on N itrification in boil. B y T. L yttleto n L yo n and James A . B izzell. . SOII?Par‘son ° f Some Q ualitative and Q uantitative .Methods for Carbonates in Soils. B y E. W . G aither Contribution to Our Methods of Determ ining N itro- Pres'11 ^ umus' B ir Charles B . Lipm an and H . F.
La bo ra t o ry a n d Pl a n t:
The Manufacture and Properties of Sublim ed W hite A v c y John A - S ch aeffer...
x> C'» V?rm L aboratory E xtractio n A pparatus.
By A. E. Perkins... ... ...
r u ' lcc Controlling Sm all E lectric Furnaces. B y C h iles Burton T h w in g ...
aj’ ubble and W ashing Tube for Com bustion Ap- A B>'H- E‘ Sm!th... ■
Nider Extraction A pparatu s. B y G. M. Mac- Add
4
sRsJ ‘X ^ n s e r . ' ' B y S. W . W i l e y .'.' .' ! an ,° isti!latio" ' n ^ lc United S tates— General Devel-P ent and R ecent Progress. B y R . P . P erry . . . . 92
9 3
9 5
106 115
123
125 126 129
131
>34 136 138
143
144 148 149 150 150 151
151
Disposal of Sewage w ith R ecovery of Elem ents of P lan t Food for Use in A griculture. B y W illiam
M cM urtric... 156
M anufacture and Uses of Cyanam id. B y E. J. Pranke 159 Cu r r en t In d u str ia l Ne w s: United States S tatistics for 1 9 1 2 ... j6i The ChemicaL A ctivities of B e lg iu m ... 161
The Increased Use of Charcoal I r o n ... 161
Gilled T u b in g ... 161
The T o xicity of W h ite L e a d ... 161
T antalu m as a Substitute lor P latinu m ... 162
Sulfur in Illum inating G a s ... 162
T he Use of Gases for F ire E xtin ction on Board Sh ip . . 162
A New T im ber Preserving P ro cess... 163
T h e B illiter Alkali-Chlorine C e lls ... 163
W ater Purification in the In d u strie s... 163-
T he Slate-B ed T reatm ent of S e w a g e ... 163
T h e M anufacture of Swedish F ilter P a p e r ... 164
T h e Minim ization of Fire R isks in the Case of Inflam mable L iqu id s... 164
The British Starch In d u s tr y ... 165
The Sulfite W aste Liquor P r o b le m ... 166
“ Sacchulosc” ... 166
No t es a n d Co r r e sp o n d e n c e: A Standard Viscosim eter and Standard Methods for Determ ining Viscosities— W h y not ?... 167
The U se of a L ig h t F ilter Cell in Polarizing H igh Grade ^ S u g a r s ... 167
The A nalysis o f Unsweetened E vaporated M ilk 168 T he Determ ination of “ V olatile” in C o a l... .. 169
N ew Chief of Bureau of C h em istry... 170
E lectrolytic Copper Refining in N o rw ay... 171
Growing Use of Am m onium Sulfate in C h in a ... 171
Am erican Chemical Society Spring M eeting... 171
“ The Progressive A g e ” becom es “ T h e Gas A g e ” 171 O b itu ary— Alfred B ellam y A u b e r t... 171
Book Re v ie w s: A H andbook of Sugar A nalysis; Com parative Fuel Values of Gasoline and Denatured Alcohol in In ternal Combustion Engines; T extb o o k of Chemical Tech nology and M etallurgy; Die Synthese des K a u t schuks; Soil F ertility and Fertilizers; Das H ydrosul fit; T h e A nalysis of P ain t and Varnish P ro d u c ts .. . 172
Ne w Pu b l ic a t i o n s... 175
Re c e n t In v e n t io n s... 176
Ma r k e t Re p o r t... 178
92 T H E J O U R N A L O F I N D U S T R I A L A N D E N G I N E E R I N G C H E M I S T R Y F e b ., 1913
EDITORIALS
COOPERATION AMONG CHEMISTS AND MANUFACTURERS Men in a calling which has so m an y ram ifications as has chem istry in its various applications to all modern activities, m ust cooperate if the profession, as a whole, is to advan ce sym m etrically and uniform ly.
Before such cooperation can be effective, m utual understanding betw een the profession and the m an
u factu rer m ust be achieved. I t is true th at m any of the chem ical m anufacturers still follow the old rule of th um b m ethods w ith ou t them selves having a n y notion of the underlying principles w hich are unchangeable and inexorable. These m anufacturers must be brought to see the actual existence of such principles and to realize th a t an understanding, as well as strict com pli
ance therew ith, is necessary for the attaining of th a t m easure of success w hich is necessary in order to m ain
ta in uniform q u a lity and m axim um output of finished product.
T h e organizers of the E igh th International Congress of A pplied Chem istry, which recently m et in N ew Y o rk , endeavored to bring about some such m utual under
standing betw een the m anufacturers on the one hand, and the educators and those who practice chem istry as a profession on the other. T o this end more than tw o hundred cham bers of commerce and eight th ou sand m anufacturers in the U nited States, as w ell as over tw o hundred and fifty educational institutions were appealed to in special bulletin setting forth the points in w hich cooperation between these three rep
resen tative divisions w ould be valuable and helpful.
T h e com m ercial side, as represented b y the cham bers of com m erce and m anufacturers, was informed, in effect, th at our educational institutions felt th a t the com plaints, so frequen tly made b y those engaged in com m ercial pursuits, of the lack of intellectual equip
m ent possessed b y youn g chem ical graduates, were due in a large measure to the p olicy of secretiveness fol
low ed b y our chem ical m anufacturers. T h ey were ap pealed to to break down this p olicy of secrecy and to cooperate w ith our educational institutions, so th at th e record of The E igh th International Congress, as reported in its proceedings, w ould disclose to our foreign visitors a h earty cooperation betw een the edu
cational and m an ufacturing institutions of pin; country.
On the other hand, the d u ty of cooperation w ith the m anufacturer w as urged upon the educational insti
tutions.
T h e results have shown th at neither the m an ufac
turers nor th e educators responded to the suggestions of the organizers of th e Congress. This is to be re
gretted , for it is not lik ely th a t such another oppor
tu n ity will be offered in this co u n try for fifty years or more. H ow ever, the seed has been sow n; the idea and its need still exist. L et us all w ork togeth er to the end th a t it m ay not be v e ry m an y years before such cooperation w ill become an accom plished fact.
The A m erican Chem ical Society, w ith its m em ber
ship of more than six thousand, represents to-d ay the
greatest, the strongest, the m ost active, and the most virile association of chem ists in th e world. I t . is through the members of the A m erican Chemical Society, associated as th e y are in fo r ty or more sec
tional units, th a t such cooperation seems m ost likely to be finally accomplished.
In N ew Y o r k C ity, the chem ist who is to be appointed to the M unicipal B oard on Com bustibles and Ex
plosives is selected b y the M ayor from am ong three nam es subm itted to him for th a t purpose b y the New Y o r k Section of the A m erican Chem ical Society. Ef
forts are now being m ade to obtain sim ilar coopera
tion in other departm ents of the C ity of N ew York governm ent. Chem ists have cooperated in the pur
chasing bureau of the city, and in less th an three years the savings effected b y them run into tens of thousands of dollars annually.
Sim ilar efforts a t m unicipal cooperation are like
wise successful in Boston and Philadelphia. These facts brought to you r attention now m ay a ct as a seed- crystal around which you r own efforts m ay crystallize.
T h e efforts m ade b y those in charge of the Eighth International Congress of Applied Chem istry, and the N ew Y o r k Section of the Am erican Chem ical Society, show th a t m aking converts to th e cause of cordial cooperation is a slow and laborious proceeding, par
ticu larly in chem istry, because, w hile th e w ork of the chem ist is fundam ental and essential, th a t fundamental and essential character is not alw ays obvious to the la y mind. T h a t is the reason w h y, in m aking converts, yo u w ill m eet w ith v e ry m eager and slow results at the start. W hile it m ay tak e y o u years to g et the Govern
m ent and the m anufacturers to w ork w ith the chemist, the value of the result should spur y o u on to greater effort rather than cause yo u to lose heart.
Probably the broadest opportun ity to raise the stand
ard of the chem ical profession in the U n ited States, to bring about better understanding betw een manu
facturers on the one hand and the chem ists on the other, to prom ote acquaintance, personal, social, and otherwise am ong those who practice chem ical pur
suits, is in an institution like the Chem ists ’ Club of New Y o r k C ity. W hile this club is located in N ew York C ity, it is not alone for the chem ists of N ew Y ork, but it is devoted to the interests of th e chem ical profession of the entire U nited States. I t know s no state, no sectional boundary. Its field ranges over the entire domain of chem istry; those w ith whom it seeks to co
operate and those whom it seeks to benefit, are those of us who teach, practice, or a p p ly chem istry any
where in the U nited States. T h e C h em ists’ Club is organized on the broadest lines conceivable.
Y o u ask w hat the C hem ists’ Club can do for those in the south and west. A chem ist residing a t a dis
tance greater than tw en ty-five miles from the Build
ing in N ew Y o r k C ity, and not regu larly doing business in the city, is entitled to non-resident membership f°r
$10.00 per year. N ow w h a t do non-resident mem
Feb., 1913 T H E J O U R N A L O F I N D U S T R I A L A N D E N G I N E E R I N G C H E M I S T R Y 93 bers get for th at $10.00? The C h em ists’ Club has its
home in the C h em ists’ B uilding, w hich is the only building in the w orld erected for th e p articu lar and p e
culiar benefit of the chem ical profession. I t has la b oratories from the top floor dow n to th e six th ; it has two floors of sleeping room s; it has a good restauran t and a good social roo m ; it has a good lib rary. A non
resident member com ing to N ew Y o r k can p u t up a t the Chemists’ Club as he w ould a t a hotel, and if he finds that he needs a lab orato ry for a w eek or ten days or a month or six m onths, he can h ave it. T h e Club has three laboratories for rent to transients.
You may come to N ew Y o r k to sell a prod u ct or a process, and it m ay be necessary to m ake a lab orato ry demonstration. Y o u cannot w alk into so m eb o d y’s else laboratory, and g e t the necessary accom m odation and the necessary p rivacy. Y o u m ay be a m an w ith out a country and a stranger w ith ou t a home, b u t y o u need not be either if y o u are a non-resident m em ber of the Chemists’ Club. Y o u m ay live, h ave e very lab oratory facility and en jo y the use of a m ost valu able chemical library in this b uilding in the center of the city. You cannot do th a t in a n y other c ity in the world.
No technical organization in a n y co u n try offers so much to its non-resident m em bers as does the Chem ists’ Club in N ew Y o r k C ity.
Many of you have been in a position where y o u have wanted a certain volum e of the Berichle, the Annalen, or any one of a num ber of other journals or a te x t
book, or have w anted a translation into E n glish of some French, Germ an, or Ita lia n reference. N on-res
ident members of the Club telegraph or w rite to the Club librarian and receive th a t p articu lar volum e b y return mail; if the book is not in duplicate, tran s
cripts will be made of the portions th a t y o u w an t and will be mailed to y o u ; a t the end of th e m onth y o u w ill get your bill for services w hich w ill be m ade a t cost since the Club is not run for profit.
Some of you m ay not need literature, b u t it is ju st possible that you m ay w a n t some chem ical th a t is not stocked by any of the chem ical dealers in the U nited States. If the plans of those in charge of th e Chem ists ’ Club do not m iscarry it w ill be o n ly a short tim e when by telegraphing or w riting to th e Chem ists ’ Club th ey will be able to take ou t of th eir m useum an original package of the chem ical th a t yo u w a n t b u t cann ot b u y m the United States, and m ail it to y o u ; y o u in turn will order from the m aker, a t y o u r convenience, an exact duplicate of the original p ack age to replace the one loaned you b y the C h em ists’ Club. W h a t have you gained? Y o u have saved th e expense of a cable, consequent delay, and a fuss a t the custom s house, e American chem ist, n e xt to m em bership in the merican Chemical Society, has never been offered a etter opportunity for cooperation th an m em ber
ship ra the Chem ists’ Club.
The development of the Club L ib ra ry is an exam ple cooperation. Mr. H erm an F rasch has m ost gen- rous y donated $10,000, the incom e from w hich is to Ch °Ji Purc^ase ° f new books. Prof. Chas. F.
j.an ®r’ New Y o r k C ity, has donated p ractica lly of his private lib rary, and Prof. John W . M allett,
of the U n iversity of V irginia, donated p rac tica lly all of his lib ra ry; th e A m erican Chem ical S o ciety and the N ew Y o r k Section of the S o ciety of Chem ical In d u stry h ave given th eir b o o k s; w e also h ave th e benefit of the S ir W illiam H en ry P erk in L ib ra ry Fund, and the Charles Frederick Chandler L ib ra ry Fund. N um erous m em bers have donated p arts or all of th eir w orking libraries, and the libraries of several of our deceased m em bers h ave passed into the possession of the Club.
T h e aim of th e C h em ists’ Club is to g e t togeth er the m ost com plete set of books on chem ical su bjects in existence, and fu rth e r to h ave as m an y as possible of them in duplicate, so th a t w e m ay h ave a circulatin g lib ra ry of immense proportions.
Those of y o u who are m em bers of the C h em ists’
Club, or the A m erican Chem ical Society, or both, will find th a t the best and the m ost useful resting place for such of th e books in you r lib ra ry for w hich yo u y o u r
self h ave no fu rth er use, w ill be in the cu sto d y of the C h em ists’ Club.
T h e C h em ists’ Club fu rth er maintains, an em p loy
m ent bureau for the use of chem ists, w hether m em bers or not, w ho are o ut of a position; this bureau does not seek to aid those a lread y in a position to b etter th em selves ; all it does is to g iv e a m an a start, and once he has th a t he m ust m ake or break himself. B y n o tify ing the em ploym ent bureau of the C h em ists’ Club of vacancies in y o u r d istrict or b y sending, to it nam es and addresses of w o rth y chem ists who are ou t of positions, y o u w ill be adding g re a tly to the effectiveness of th a t bureau w hich has fo r m an y years p ast helped hundreds of men an n u ally in obtaining good positions and in enabling m an y m anufacturers to g et suitab le chem ical assistance w ith little delay.
W e have pointed out o n ly a few of the opportuni
ties for cooperation, and dilated upon th e benefits th a t th e C hem ists’ Club w ill confer upon the individual chem ist and upon the chem ical profession as a whole.
T h e field of cooperation is too b ig to do more th an m erely to scratch the surface and com m end it to y o u r serious consideration and to solicit y o u r earnest sup-
p o rt- B . C. He s s e
TH E PR ESEN T STATE OF TH E A R T OF IN DUSTRIAL MANAGEMENT
T h e A m erican S o ciety of M echanical Engineers h ave made, through a sub-com m ittee of th a t organ
ization, a m ost careful stu d y and an elaborate report on th e present statu s of the efficien cy m ovem ent in industrial w ork. T h e y h ave carefu lly an alyzed th e problem and classified th eir conclusions in b y fa r the m ost im portan t contribution so fa r subm itted on this subject. W e h ave carefu lly sum m arized their w ork in the follow ing ab stract:
D uring th e p a st few years a num ber of strikin g phenom ena, in connection w ith industrial m anage
m ent, m ust h ave becom e evid en t even to the m ost superficial observer. T h e more im portan t are:
(a) T h e w ide-spread, p opular interest in th e su b ject w hich had its rise in a statem en t m ade before the In te rsta te Com m erce Commission, in a hearing on the m atter of proposed advan ces in freigh t rates, th a t b y
9 4 T H E J O U R N A L O F I N D U S T R I A L A N D E N G I N E E R I N G C H E M I S T R Y F e b ., 1913 the application of new ly discovered principles of
m anagem ent “ in the railroad operation of this cou ntry an econom y of $1,000,000 a d ay is possible.” This p opular interest is shown b y the great num ber of a rti
cles published in the d aily papers and popular m aga
zines, m edium s th a t g ive b u t scant attention to tech nical subjects excep t of the m ost striking nature.
(b) T h e suddenly intensified interest in the subject on the p art of em ployers and business executives in m an y lines of a c tiv ity , shown b y lectures, addresses, professional papers and reports presented to their as
sociations.
(c) The opposition of labor unions to the newer m ethods of m anagem ent, shown b y statem ents of labor leaders, in a few instances b y strikes, and b y an a t
tem p t to prohibit b y law the use of some of these m ethods in G overnm ent shops.
(d) G overnm ent recognition of the m atter shown b y the appointm ent of a special com m ittee of the House to investigate system s of m anagem ent in G ov
ernm ent arsenals and shops, which reported in March, 19x2; b y the appointm ent of a civilian board b y the Secretary of the N a v y to investigate m anagem ent in the n a v y yards, which reported in July, 19 11; and b y a Senate bill, S 6172, now in com m ittee, which is in
tended to prohibit tim e stu d y and the paym en t of prem ium s or bonus on Governm ent work.
(e) The rap id ity w ith which literature on the sub
je c t has accum ulated. One directory of books on business m anagem ent lists 500 titles, and states th at 75 per cent, of them have been w ritten w ithin five years.
C/) T h e form ation of two societies having as an aim th e furtherance of the applications of the principles of m anagem ent.
(g) T h e separation of persons interested in the m at
te r into tw o cam ps, one of enthusiastic advocates, the other of vigorous opponents of w h at is called the new elem ent in m anagem ent.
(h) The unquestionable proof of the advance th at can be m ade in unskilled w ork, as shoveling m aterial, and in ancient trades, as bricklaying, b y the applica
tion of the principles of m anagem ent. This is the m ost .striking phenom enon of all.
Before defining the elem ent in the art of m anage
m ent th a t has given rise to these phenomena, it is necessary to review briefly the beginnings of modern industry. T h is gives a historical setting from w hich the present can be more tru ly judged.
Modern ind u stry w as brought about b y the change from handicraft to m anufacture, and early B ritish econom ists held th at the application of the principle of division of labor w as the basis of m anufacture.
I t appears, however, th a t another principle is the basic one in the rise of industry. I t is the transference of skill. The transference of skill from the inventor or designer to the pow er-driven mechanism brought ab out the industrial revolution fjrom handicraft to m anufacture.
N o b etter single illustration of the application of th is principle can be found than in the invention of th e lathe slide rest b y H enry M audsley, in 1794. So
com plete has been this transference of skill that to
d ay hand tooling is a vanished a rt in Am erican ma
chine shops. V ery few lath e hands can chase a thread w ith hand tools, y e t all can cu t good threads on an engine lathe, thanks to the slide rest.
Methods of analyzing and recording operations were early developed. A d am Sm ith recorded the divi
sions of the w ork of m anufacturing pins, listing all operations. Charles B abbage g a v e a tab le from a French investigator showing the num ber of opera
tions, tim e for each, cost of each, and expense of tools and m aterial for m aking pins in F ran ce in 1760.
T hus we see the application of the principle of transference of skill a t the basis of the development of the industry, and an early application of the value of the detailed stu d y of operations in m aking that transference more com plete. B u t the machine was the view point. I t w as looked upon as the producing unit. The subsequent developm ent has had the ef
fect of advancing still further the division of labor, and beginning the division of thought. T h e drafting room presents the first exam ple of this trend, in its collection of engineering data, in its prediction of re
sults and the form ation of staff organization. The a rt of m achine design has been g re a tly developed.
T he last half of the last cen tury saw a tremendous in
crease in inventions, a trem endous furtherance of the application of transference of skill to machine and tools. The skeleton of an industrial organization of this period, one th a t was too large for a single execu
tive to manage, consisted of a designing department and a production departm ent, each w ith a head re
sponsible to the manager.
The first of these, the one th a t w as the means of em bodying skill in the m achinery and tools of pro
duction, was highly developed and organized. Ex
periment, research and detailed stu d y were constantly resorted to, to aid in reaching the desired result.
The work was highly specialized and the employees highly paid. N ot infrequently the m anager or chief executive devoted much of his ow n tim e to this part of the business.
The production departm ent presented a contrast
ing condition. The workm en were g iven the tools and machines designed in the drawing-room and using their own unaided skill were expected to pro
duce w ork of the desired q u ality and q u an tity. Ex
cept in rare instances, no effort was m ade to transfer the skill of the m anagem ent to the production depart
m ent and to the em ployees, or to undertake the divi
sio n of executive thought. V e ry little consideration was given to the workm en a s a producing unit.
W ithin the past 20 or 25 years certain changes have taken place in the attitu d e of m an y production man*
agers tow ard the problem s th a t th ey face and the forces and means th a t th ey control. A n early evi
dence was the developm ent of profit-sharing, p r e m iu m
and bonus system s to reward increased effort and out
put. There followed welfare w ork, industrial better
m ent m ovem ents, the adoption of safeguards and regu
lations to minimize industrial accidents, the s u b s ti
t u t i o n of the principle of accident c o m p e n s a t i o n f°r
employers' liability and an im provem ent in the physical surroundings and conditions of factories.
All of these tendencies have been fostered and to a great extent initiated b y em ployers. B u t even to day these are b y no m eans generally adopted.
Another tendency, less pronounced in character, has as its object the im provem ent of the personal relations between the em ployees them selves and be
tween the employee and the em ployer. It is the effort to establish the best of fa cto ry w orking conditions in those things not p h ysical in nature, to develop and maintain a shop atm osphere free from all harassing and hindering influences. I t is an a ttem p t to m ake use of the results of experim ental p sych o logy in im proving working conditions.
But the most im portant change and one th a t com prehends the others, is in the m ental a ttitu d e tow ard the problems of production. T he tenden cy is tow ard an attitude of questioning, of research, of careful investigation of everyth in g affecting the problem s in hand, of seeking for ex a ct know ledge and then shaping action on the discovered facts. It has de
veloped the use of tim e stu d y and m otion stu d y as instruments for investigation, and the planning de
partment as an agency to p u t into p ractice the con
clusions drawn from the results of research, and m eth
ods of wage paym en t w hich stim ulate cooperation.
All of these changes h ave affected the production department much more than the designing d ep art
ment. The effect is to extend the principle of trans
Feb., 1913 T H E J O U R N A L O F I N D U S T R I A L
THE HYDROGENATION OF OILS’
B y Ca r l b t o n El l i s
I he treatment of unsaturated oily bodies w ith hydrogen to obtain saturated d erivatives is of great scientific and technical interest. In the fa t ind u stry a most fascinating problem has been th a t of th e con
version of oleic acid or olein into stearic acid or the corresponding glyceride.
Oleic acid and hydrogen com bine, m olecule for molecule, to yield stearic acid according to the reaction:
c 18h 31o 2 + h 2 = C lgH 380 2
Ihus 282 pounds of oleic acid require 2 pounds (or about 0.7 per cent.) of hydrogen for the production
°f 284 pounds of stearic acid, and sim ilarly the tran s
formation of olein into stearine requires the use of about 0.68 per cent, hydrogen.
One thousand cubic feet of hydrogen w eigh ap p roxi
mately 5.5 pounds, hence a pound of olein calls for a little over 0.1 of an ounce of hydrogen equivalen t to approximately 2500 cubic feet of hydrogen per ton 2000 pounds) of olein. T hus b y w eight only a.v elatlvW sma^ q u a n tity of hydrogen is needed, '• ■ c by volume the am ount required, of course, is considerable.
•lany attempts to hydrogen ate oleic acid have been
t_ . !!-si''Ued before th e N ew Y o rk S e c tio n of th e S o ciety of C hem ical
ustry. November 22,. 1912.
ference of skill to production, so th a t it com p letely em braces every'- a c tiv ity in m anufacture. T h e skill of m anagem ent is consciously transferred to all of the operations of the factory. T h is extension is expressed b y these phases; the drawing-room is the planning de
p artm ent of design, and the planning departm ent is.
the drawing-room of production.,
T o obtain inform ation on present conditions, the com m ittee w rote to the recognized experts, to execu tives of p lan ts in m any lines of industry, to students of industrial problem s, and it has had m an y inter
view s w ith men in these various fields. The responses to the requests were in the m ain m ost generous, and the replies co n vey the ideas of a conscious effort to ascertain and stu d y facts and sy stem atically to a p p ly them to instructing the w orkm en and in controlling e v e ry departm ent of industry. S etting these against the underlying principle of the transference of skill, th e y conceive the prom inent elem ent in present-dayr industrial m anagem ent to be: the mental attitude that consciously applies the transference of skill to all the activities of industry.
H ere em phasis is placed upon the w ord all, for the restricted application of this principle to m achines and tools has been highly developed for a long period. B u t its conscious application in a broad w a y to the produc
tion departm ents, and p a rticu larly to the workm en, w e believe has been m ade during the last q u arter century.
A N D E N G I N E E R I N G C H E M I S T R Y 95
m ade. R eview in g this su bject in 18971 Lew kow itsch refers to the ease w ith w hich the low er m em bers of the oleic series are converted into saturated acids and states th a t “ oleic acid itself resists all attem p ts at h ydrogen ization ,” fu rth er rem arking th a t he had
“ carried out a large num ber of experim ents in this direction under m ost varied conditions, b u t hitherto all of these g a v e n egative results.”
Prior to this, how ever, Goldschm idt, in 1875/
had reduced oleic acid b y means of hydriodic acid and am orphous phosphorus a t 200-210° C. This pre
su m ably led to the attem p ted com m ercial d evelop
m ent of a process b y de W ild e and R eych ler3 in volvin g heating oleic acid to 280° C. w ith 1 per cent, of iodine, adding and m elting therein a certain q u a n tity of tallow soap, and then boiling w ith acidulated w'ater. The product w as then distilled and the iodine, in part, recovered from the pitch. T h e yield of stearic acid or satu rated fa t i s ' stated to be ap p roxim ately 70 per cent, of the theoretical. O nly ab out tw o-thirds of the iodine could be recovered so the process ap p ar
e n tly did not find technical use.-t Should the much lauded m ethod of treatin g kelp, prim arily for o b tain ing potash salts, com e into use, a cheap supply of iodine
1 J . S . C. I ., 389 (1897).
2 S ite . b. d. W ie n e r A k a d . d. IV issii 72, 366.
3 B u ll. Soc. C him ., [3] 1, 295 (1889).
* Chem. Ztg.. 1889, 595.
ORIGINAL PAPERS
96 T H E J O U R N A L O F I N D U S T R I A L A N D E N G I N E E R I N G C H E M I S T R Y F e b ., 1913 w ould be availab le w hich m ight then m ake the W ilde
and R eych ler process of some technical interest.
Chlorine in lieu of iodine has been tried, but great difficulty has been experienced in securing an a u to cla ve of resistant m aterial. Im b ert1 recommends using quantities of chlorine and alkali e x a ctly calcu
lated on the iodine num ber of the fa tty acid and oper
atin g a t a tem perature of 120° to 150° C. and pressure of ab out five atm ospheres for a period of six hours.
Zurrer2 chlorinates the fa tty acid and then heats w ith w ater in the presence of a finely divided m etal as zinc or iron. L ew kow itsch alleges th at the tre at
m ent of m onochlor-stearic acid in this manner causes a reversion to oleic acid.
Tissier, in 1897,2 lays claim to a process for the re
duction of oleic acid b y nascent hydrogen. Pow dered m etallic zinc is placed in an autoclave, w ater and the fa tty m aterial containing olein introduced and treated under pressure.
U nder the circum stances the glyceride is hydro
lyzed to fa tty acid and glycerine, and according to Tissier nascent hydrogen is evolved b y virtue of the finely divided m etal and reduces the oleic to stearic acid. Freundlich and R osauer4 claim the Tissier process to be inoperative.
T h e conversion of oleic acid into palm itic and acetic acids b y means of caustic potash in accordance w ith the V aren trap p .reactions has not proved to be of much com m ercial significance, although it appears th at certain firms have been m aking use of the process in a lim ited w ay.
T he Schm idt zinc chloride process6 involves heating oleic acid and zinc chloride a t e x a ctly 185° C. w hile interaction is takin g place. “ D eviation from this p oint leads to an increase of liquid substance. U n
fo rtu n ately the solid candle m aterial m ust be dis
tilled and the considerable proportion of /?-hydroxy- stearic acid (m elting point 82° C.) in the crude product is seriously dim inished b y the partial conversion of this acid into oleic and iso-oleic acids. Thus, from a candle-m aker’s point of view , a substance of high m elting point is rendered p ractically valueless.
S ch m id t’s process was tried on the large scale in an A u strian candle works. T he q u a n tity of liquid tinsaponifiable substance obtained was, however, so large th a t com m ercial success was out of the question.”
M any processes have been proposed based on the w ell-know n action of sulfuric acid on oleic acid.
H yd ro xy-stearic acid is obtained b y steam ing the product. I t w ould lead us too far from the present su b ject to enter into a n y further discussion of these reactions.
P R O C E S S E S IN V O L V I N G A P P L IC A T IO N O F E L E C T R IC IT Y
In 1886, W eineck? called atten tion to the possi
b ility of • electrolytic addition of hydrogen to oleic
' U . S. P a t e n t N o. 901.905. of O ct. 20, 190S; sec also B u ll. Soc. C him ., 1899, 695. 707.
- G e rm a n P a te n t N o. 62,407, of A ug. 8. 1891.
3 F rc n c h P a te n t N o. 263,158, of J a n . 16, 1897.
4 Chem. ZtQ., 1900, 566.
3 J . S . C. A, 98 (1883), 200 (1884).
0 L ew kow itsch, "O ils, F a ts a n d W ax e s,” p. 664.
7 Osterr. P r iv il., 10, 400 (J u ly 19. 1886).
acid. K u ess1 later attem pted to a p p ly the electric current in the steam distillation of f a t t y acids.
In patents taken o ut b y M agnier, B ragnier and Tissier,2 the fa tty m aterial is acidified w ith sulfuric acid, whereupon the acidified m ass is m ixed with 5 to 6 tim es its w eight of w ater and then under a pressure of 5 atm ospheres is subjected to the action of an electric current, w hich generates hydrogen in a nascent state.
A n interesting m ethod of converting oleic into stearic acid is th a t com prised in the Hemptinne electric discharge process. T h e m ethod is carried out b y interposing a thin layer of the oil in the path of an electric discharge, w hile bringing hydrogen into contact w ith the oil.*
Fig. 1 shows the arrangem ent of apparatus for this purpose. The conversion is effected in a chamber having an inlet pipe, H, furnishing hydrogen under constant pressure. Oleic acid is supplied b y a pipe, O, to a sprinkling device which discharges the acid onto a system of parallel plates consisting of the glass
plates G and altern ately the m etal plates M, N. The m etal plates M are connected to one pole, the others, N, being connected w ith the other pole of a source of electricity. A s the oil passes over the plates the electrical discharge causes conversion of some oleic acid into stearic acid, and analogous compounds having m elting points in the neighborhood of 69° C.
H em ptinne prefers to w ork a t pressures less than atm ospheric. The yield is low er a t atmospheric pressure. B y treatm ent in this m anner it is not difficult to secure a yield of 20 p er cent, of stearic acid. R epeated treatm ent perm its even up to about 40 per cent, yield. Here, as so often elsewhere, the effect of mass action becom es m anifest and as the content of stearic acid increases the speed of reaction g rea tly decreases. Much better results are obtained b y saturating to the exten t of ab out 20 per cent., rem oving the stearic acid b y pressing, w hen the oil of reduced stearic acid content is again subjected to the electric discharge, and a further 20 per cent, yield obtained. The oleic residue contains liquid condensation products am ounting to about 40 per cent, of the total w eight. I t is stated th a t the presence of these bodies
1 Chem. ZtQ., 1896, 618.
2 E n g . P a te n t N o. 3,363, 1900; G e rm a n P a te n t N o. 126,446. of Oct.
3. 1899, a n d a d d itio n a l G erm an P a te n t N o. 132,223.
3 U. S. P a te n t N o. 797,112, of A ug. 15, 1905.
Feb., 1913 T H E J O U R N A L O F I N D U S T R I A L A N D E N G I N E E R I N G C H E M I S T R Y ' 97 does not impair the m arket valu e of w h at some one
has termed “ electrocuted” oleic acid.
“J. Petersen1 also endeavored to reduce oleic acid to stearic acid b y allow ing an electric curren t to act between nickel electrodes on an alcoholic oleic acid solution, slightly acid u lated w ith sulfuric acid or p ref
erably with hydrochloric acid. B u t the y ie ld of stearic acid was sm all, even under th e m ost fa v o r
able conditions, and did not exceed 15 to 20 per c e n t.”
Petersen also endeavored to reduce sodium oleate in aqueous or alcoholic solution to the stearate. No satisfactory results were obtained.
C. F. Bohringer and Sohne3 obtained b y the same method much better results when using as cathodes, metallic electrodes, w hich were covered w ith a spongy layer of the sam e m etal. T h e y recom m end as cathodes platinized platinum , and also palladium electrodes covered w ith a sp on gy lay e r of palladium - black. Nickel electrodes are not as effective.
Kolbe* in 1871 states th a t S a ytzeff reduced nitroben- zol to aniline b y passing the vapors of the, former, mingled with hydrogen, over palladium -black.
About tw enty-five years later Sabatier and Sen- derens began their classic stu d y of nickel and other metallic catalyzers.
The work of Sabatier and Senderens laid the founda
tion for the present processes of hydrogenation of oils. Their work is so w ell know n th a t it is needless to discuss it here.
Fig. 2 shows app aratus used b y these investigators m the hydrogenation of bodies capable of vap o riza tion. In this apparatus, 1 is a hydrogen generator;
2 and 3 are wash bottles and 4 is a vaporizer containing
e substance to be converted into a vapor. 5 is a rogen chamber containing nickel ca taly ze r and 6~ ec! by an oil bath. 6 is a condenser.
hile a good deal of w ork has been done on the } rogenation of fa tty oils, the literature on the sub- wh" h Ver'r mca" re mdeed and only through the patents j- ,1C ^ave been issued can w e gath er from a n y pub- e records much th a t is enlightening as to develop-
°nts in this industry. T h e p atents concerned w ith
2 r ® el,lr°chemie, 1905, 549.
3 r '" !'P.atCnts N os- 187,788, 189,332, 1906.
iro *1- CA«n ., [2] 4, 418 (1871).
the m atter have, m oreover, been subjected to a great deal of scru tin y because of the alleged basic ch aracter of certain of them . F or these reasons the follow ing discussion pertain s v e ry largely to processes which h ave been covered b y p aten ts in this co u n try or abroad.
( No t e.— The illustration s herein are largely derived
from the draw ings of p a te n t records or h ave been prepared from w ritten descriptions. A ll details deemed unnecessary .in the p o rtraya l of th e essential features of these processes h ave been om itted. T h e original records should, of course, be consulted for details.—
Au t h o r.)
A G erm an P aten t, No. 139,457, of J u ly 26, 1901, to J. B. Senderens, is p rob ab ly the first p a te n t record h avin g to do w ith the reduction of organic bodies b y hydrogen in the presence of nickel catalyzers. T h is p a te n t is for the production of aniline from nitro- benzol and involves passing the latter b o d y in th e form of a vap o r over heated nickel, copper, cob alt, iron, or palladium in the presence of hydrogen. T h e hydrogen m ay be in the pure state or in the form of water-gas.
The first disclosure of the possib ility of hydrogena
tion of oils in a liquid state ap p aren tly com es from L e Prince and S iv e k e .1 In E n glan d a corresponding p a te n t (No. 1515, of 1903) was issued to N orm ann1 and the latter p a te n t has becom e w id ely know n because of its alleged fundam ental character.
N orm ann states th a t he m ay ca rry ou t the h ydro
genation of oils b y treatm en t either in the form of vapors or as liquids. In the form er case the fa tty acid vapors together w ith hydrogen m ay be caused to pass over ca ta ly tic m aterial carried b y a pum ice stone support. T his m ay be represented b y Fig. 3
F i g . 3
in .w hich A is a bed containing granular pum ice coated w ith a m etal catalyzer. O is an inlet for oil vapors and H is an inlet for hydrogen. The m ixtu re passes through the tub e A and the converted m aterial is w ithdraw n a t B. Norm ann notes, how ever, th at it is sufficient to expose the fa t or fa tty acid in a liquid condition to the action of hydrogen and the ca ta ly tic substance. H e states, for instance, if fine nickel pow der obtained b y the reduction of nickel oxide in a curren t of hydrogen is added to oleic acid, the latter heated over an oil b ath and a strong current
1 G e rm a n P a te n t N o. 141,029, of A ug. 14, 1902, H e rfo rd e r M asch in en - f e t t u n d O el F a b rik .
2 T h is E n g lish P a t e n t is o w ned b y a larg e so ap m a n u fa c tu rin g h o u se in E n g la n d a n d i t is r e p o rte d th e y allege th e p a t e n t in t h a t c o u n try t o b e fu n d a m e n ta l a n d co n tro llin g fo r th e h y d ro g e n a tio n of f a t t y oils g e n e ra lly . T h e y a re offering re w a rd s fo r in fo rm a tio n as t o th e s e c re t a n d u n a u th o riz e d u se of th e process a n d i t is said a lre a d y t o h a v e s ta r te d litig a tio n .
98 T H E J O U R N A L O F I N D U S T R I A L A N D E N G I N E E R I N G C H E M I S T R Y F e b ., 1913 of hydrogen caused to pass through it for a consider
able tim e, th at the oleic acid m ay be com pletely con
verted into stearic acid.
Fig. 4 shows v e ry simple apparatus, such as m ight h ave been used b y N orm ann to this end. A is a vessel containing oil, 0 , in which fine particles of nickel are
suspended w hile a strong current of hydrogen from the pipe H affords the hydrogen requisite for re
duction of the oil. B y this means N orm ann treated the fa tty acid of tallow having an iodine num ber of 35 and m elting a t about 46, thereby converting it into a body of im proved color h aving an
F ig . -1 iodine num ber of about
10 and a m elting point of about 58. Normann also states th at com m ercial gas m ixtures, such as water- gas, m ay be used in lieu of pure hydrogen.
The disclosures of the Normann patent are, however, rather m eagre and hardly can be considered to com p rehen sively traverse the difficulties encountered in the p ractical hydrogenation of oils in a liquid state.
Dr. D avid T . D ay, of W ashington, has brought out a process1 in which he treats, not fa tty oils, but h ydrocarbon oils, w ith hydrogen in the presence of w h at he term s a porous absorptive substance, men
tioning palladium -black, platinum sponge, zinc dust, fu lle r’s earth and other clays. Fig. 5 shows one m ethod proposed b y D a y to this end.
The upper cham ber A is filled w ith hydrocarbon oil, and porous absorptive m aterial such as palladium - b lack is introduced in the interm ediate cham ber C
Fi g. 5 Fi g. 6
b y w a y of the plugged orifice D. A n y air present in C m ay be expelled b y flushing out w ith hydrogen or an indifferent gas. H ydrogen is then adm itted b y th e pipe H until the porous m aterial has absorbed
> U . S. P a te n t N o. 826,089. of J u l y 17. 1906.
its full quota. The hydrogen gas m ay be admitted under a pressure of 100 pounds or more to the square inch. W hen the porous m aterial in C has become properly charged w ith hydrogen, the oil is allowed to run from the cham ber A through the cham ber C into the collecting cham ber E, hydrogen being intro
duced as required b y the pipe H.
In the place of hydrogen, D a y states th a t ethylene or other hydrogen carrying gas or vap o r m ay be em
ployed. B y this treatm ent the disagreeable odor of hydrocarbon oil is' in great part rem oved and the burning qualities of the oil im proved. W hen palladium black is used it is recomm ended th a t a proportion of one-half ounce to the gallon of oil be taken.
Fig. 6 shows a m odification of D a y 's process. A is an oil still, in the low er p art of w hich the perforated pipe H serves for the admission of hydrogen. Palla
dium -black or other porous absorptive m aterial forms a layer, C, on a screen above the hydrogen inlet.
0 shows the charge of oil. In operating this ap
p aratus the layer of m aterial C is first charged with hydrogen and then oil run into the still. Distillation is carried out while hydrogen gas is being forced through the absorptive m aterial and oil.
A peculiar m anner of treatm ent has been shown b y Schwoerer,1 which w ill be m ade clear b y Fig. 7.
The receptacle A , which is heated b y the steam jacket S, is provided w ith w h at Schwoerer calls a helical
pan, shown at B. The underside of the pan carries a layer of nickelized asbestos. 0 is an inlet for oil and hydrogen, and D an outlet for the treated material.
Schwoerer states th at he first m ixes fa tty acid and hydrogen b y atom izing the oil w ith a je t of super
heated steam in the presence of hydrogen and con
ducts this m ixture through the pipe O, into the cham ber A. The tem perature m aintained in the apparatus is from 250 to 270° C. V apors of oleic acid come in contact w ith the layer of catalyzer on the underside of the helical pan and are converted into stearic acid. The product collects, more or less, in the gu tter of the helical pan and is rem oved at D.
The repeated caution given b y Sabatier to bring ifl contact w ith the ca talyzer only the vapors of the
1 U. S. P a te n t N o. 902.177, of O ct. 27, 1908.
Feb., 1913 T H E J O U R N A L O F I N D U S T R I A L A N D E N G I N E E R I N G C H E M I S T R Y 99 material, doubtless led Schw oerer to devise this
form of apparatus.1
Bedford, presum ably w ith the same caution of Sabatier in mind, discloses, in U. S. P ate n t No.
949,954, of Feb. 22, 1910, a process w hich also has to do with vaporization of the oily m aterial. F ig. 8 shows the Bedford apparatus. A still or tow er, A , carries two beds of catalyzer, C and C '. This is said to be preferably nickelized pum ice. B y m eans of hydrogen under pressure, oleic acid is sprayed from the pipe 0 , onto the ca talyzer bed C '. H ydrogen is admitted through the pipe H. A tem perature of about 200° C. and a dim inished pressure of about 50 to 100 mm. is m aintained in the still or tow er A.
The vapors of oleic acid m ingled w ith hydrogen pass through the second ca taly ze r bed C, where more or less conversion occurs, then pass to the condenser D, and finally collect in the receptacle E . F is a connec
tion to a vacuum pum p.
Neither this process nor th a t of Schw oerer is broadly applicable to the treatm ent of glycerides as these cannot be vaporized w ith ou t undue decom position.
Erdmann has taken out a Germ an P a te n t No.
21 r,669, of Jan. 19, 1907, involvin g passing an oil as spray or m ist into a cham ber containing nickel catalyzer supported on pum ice and the like. Fig. 9 probably indicates one form suggested b y Erdm ann, who, by the w ay, does n ot show an y draw ings in the
f i g . 9 F i g . 1 0
patent. The cham ber A has a rotatab le cylinder, B. which is coated w ith nickel catalyzer. In the bottom of the receptacle is a q u a n tity of nickelized pum ice.
u,i enters at 0 and is atom ized b y hydrogen entering at H. The atom ized m ixtu re im pinges upon the ro-
335 ,.^a^a*‘er and Senderens, A n n a tes de Chimxe el de P h ysiq u e, [8 ] 4, cessif d ■ Sta*e ^ l a t " ^ e !n<‘,l-a ' ne s° i t ja in a is m o u illi p a r u n afflux ex- de | l U <lue 1'o n tra ite , o u a la 's u ite d 'u n a b a iss e m e n t a c c id e n te l cyclohCmPeratUre t u k e ‘” T h e y f u r th e r s a y t h a t in th e p re p a ra tio n of but V i T 01 'ln^ ' ts hom ologues fro m p h en o l o r cresol a t a te m p e ra tu re cond 1 ak ° ve ^ u' boiling p o in ts of th e l a t t e r b odies, so m etim es b y th e ir a lm o -t^ l°^ ' n >ckel becom es m o iste n e d a n d im m e d ia te ly becom es , lnactlve, due, no d o u b t, to th e su rfa c e b eco m in g p e rm a n e n tly ch an g ed
^ a cter by c o n ta ct w ith th e liq u id p h en o l o r cresol.
tatin g cylin der B , then passes through the bed C, the oil being draw n off a t D. T h e excess of hydrogen is presum ably ven ted in the upper part of th e apparatus.
A second m odification (Fig. io) involves a tow er, A , filled w ith ca talyzer C, w hich m ay be in the form of nickel supported on coarse fragm en ts of pum ice.
B y the pipe O, oil is adm itted to the cham ber in an atom ized or finely divided state. H ydrogen enters b y the pipe H. E rdm ann states th a t the tem pera
ture of treatm ent should be from 170 to 180° C.
T h e treated oil is draw n off a t D w hile the excess of hydrogen passes a w a y at B.
In a supplem ental patent, No. 221,890, of Jan. 19, 1907, E rdm ann recom m ends the steam distillation from the reaction cham ber of the satu rated product under dim inished pressure.
V ereinigte Chem ische W erke A . G .1 m ake use of palladium ca taly ze r p recipitated on an indifferent b o d y as a carrier and recom m end as carriers finely divided m etals w hich do not h ave an ti-ca taly tic properties, also m etal oxides and carbonates. U nder these circum stances it is stated th a t one p art of p a lla dium is sufficient to co n vert in a few hours xoo.ooo parts of oily m aterial to a firm mass. T h e y recom m end the use of a hydrogen pressure of tw o to three atm ospheres and a tem perature som ew hat ab o ve the solidification point of the satu rated fat. T h e y caution against arsenic, hydrogen phosphide and sulfide, liquid h yd ro carbons and carbon bisulfide, chloroform , acetone and free m ineral acids as being destructive to the a c tiv ity of the catalyzer.
K a y s e r3 describes a process of treating oil w ith m etal
lic ca taly zer consisting in m echanically a gitatin g the oil and ca taly zer in the presence of hydrogen, p referably under pressure. One form of the ap p aratus indicated b y K a y s e r for thispurpose isd iagram m atically represented b y Fig. x 1.
H ere A is a closed horizontal cylin d rical vessel in w h ic h ,is a paddle w heel, D, m ade up of blades carryin g wire gauze. T h e paddle wheel is rotated
Fi g. 11 Fig. 12
b y a drivin g gear a t B. In the upper p a rt of the tan k is an inlet for charging oil an d p resu m ab ly also ca talyzer, the oil being adm itted to the ta n k in an am ount sufficient to fill to perhaps one-fourth or one-fifth the entire cap acity. H ydrogen is adm itted a t H and passes, b y the th ree-w ay cock I, to the com pres
sion pum p J, going from there to the treatin g re
ceptacle. A t the opposite end of the tan k is an e x h aust pipe, L , carryin g a blow -off valve, M, for the
1 G e rm a n P a t e n t N o 236,488, of A ug. 6. 1910; also E n g lish P a te n t N o. 18,642, of 1911.
2 U . S. P a t e n t N o. 1,004,035, o f S e p t. 26, 1911,
T H E J O U R N A L O F I N D U S T R I A L A N D E N G I N E E R I N G C H E M I S T R Y F eb ., 1913 purpose of venting the unabsorbed, hydrogen. The
tem perature of treatm ent is stated to be about 150 to 160° C. A lth ou gh the claim s call for the use of hydrogen under pressure, no w orking pressures are specified. F ig. 12 shows diagram m atically one form of construction of the screen-covered paddle wheel used b y K ayser.
In another U. S. P aten t (No. 1,008,474, of N ov. 14, 19 11), K a y s e r sets forth the use of an inert pulverulent m aterial such as kieselguhr as a carrier for the nickel catalyzer, he ap p aren tly h aving determ ined, as did Sabatier and others, th a t hydrogenation is more rapid or com plete when a carrier for the catalyzer is used;
and he claim s the process of hydrogenating oil in v o lv
ing agitation of a m etallized inert pulverulent carrier w ith a fa tty oil in the presence of hydrogen. It is com m only understood th a t the K a yser process is in operation on the large scale in this country.
T w o p atents relating to the spraying of oil into a cham ber containing compressed hydrogen have a t
tracted some atten tion abroad. One of these is English P aten t No. 7,726, of 1910, to T estrup and the other is to W ilbuschew itch which finds its counter
p a rt here in U. S. P aten t No. 1,024,758, of A pril 30, 1912. Fig. 13 shows the elem ents of the T estrup process.
Oil and ca talyzer are pum ped through the pipe 0 , into the tan k A , and hydrogen is adm itted b y the
Fi g. 13 Fi g. 14
pipe H, to furnish a gas pressure of say 15 atmospheres.
The tubes B are heated b y steam and the stirrer C circulates the oil and ca talyzer in the tank A , until the oil has becom e heated and presum ably som ewhat hydrogenated. T h e oil is allowed to pass into the adjacen t tan k E , entering this tan k b y the spray nozzle F. H ydrogen gas is adm itted to the tan k E, from the tan k A, so as to afford a pressure of, say, 12 atm ospheres in the tan k E . A series of tanks m ay be arranged w ith a con stan tly decreasing pressure so th a t the differential pressure enables the spraying of the oil from tan k to tank. T estrup states th a t sp ray
ing the m aterial ten or fifteen tim es is sufficient to bring an oil of an iodine num ber of n o down to an iodine num ber of 50.
A s catalyzer, T estrup recommends finely divided palladium or preferably nickel, the latter being tw o to three per cent, b y w eight of the oil. A s a
treatin g tem perature 160 to 170° C. is mentioned.
T he W ilbuschew itch p aten t itself details a rather com plicated system and Fig. 14 shows o n ly w hat ap
pears to be the essential features of the treating ap
paratus. Several tanks or autoclaves are connected as shown a t A and A ', oil entering the top of the tank A b y the pipe 0 , to form a sp ray w hich in descending m eets an upward current of hydrogen entering by the pipe H. The oil is drawn off through the pipe O ', and sprayed into the tan k A '. T h is tim e it meets a current of hydrogen represented b y the excess of hydrogen com ing from the tan k A. T h e treated oil is drawn off and m ay be centrifuged to rem ove the catalyzer. A pressure of nine atm ospheres is recom
mended and the pressures m ay be varied in the differ
ent tanks.
Of the W ilbuschew itch process G oldschm idt1 states th a t the high hydrogen pressures em ployed enable the reaction to take place q u ick ly a t temperatures betw een 100 and 160° C., so th a t the fa t is not likely to be injured b y the tem perature to w hich it is sub
jected. I t should be stated th a t several years previous to the date of the W ilbuschew itch p atent, Ipatiew had noted and carefully studied the action of increased pressure.3
Bedford and W illiam s3 have brought ou t an inter
esting process represented b y U. S. P aten t No.
1,026,339, of M ay 14, 1912. Fig. 15 shows the appara
tus indicated b y Bedford and W illiam s for carrying out the process. Oil is placed in the receptacle A,
Fi g. 15 Fi g. 16
which is heated b y a steam coil, S. M etallic oxide catalyzer is added, about 1 percen t, being recommended, and hydrogen and oxygen or air is introduced by the pipe H. A s a catalyzer, nickel oxide (previously used b y Ipatiew ) is recomm ended and instead of the cus
tom ary hydrogenating tem perature of 150 to i7o°C., a tem perature of about 250° C. is em ployed. While hydrogen alone m ay be used for the purpose, the in
ventors recommend and claim treatm en t of the oil 1 Chem, ZiQ.. 1912, 945.
2 R u m o r h as it th a t th e processes o f T e s tru p a n d W ilbuschem tdi w ere so m u ch alike t h a t d u rin g th e p ro se cu tio n of th e ir p a t e n t applications before th e E nglish P a te n t Office, th e y co n clu d ed t o u n ite interests aad th a t su b se q u e n tly th e y sold th e rig h ts in E n g la n d t o a so ap manufacturer
■who, i t is alleged, proposes to c o n te s t th e claim s o f th e p re s e n t owners of th e N o rm an n p a te n t as to th e alleged b asic n a tu re o f th e la tte r.
3 I t is re p o rte d th a t in E n g la n d som e o f th e in d e p e n d e n t soap manu- fa c tu re rs h a v e ta k e n o v e r th is p a te n t of B e d fo rd a n d W illiam s and also tic E rd m a n n rig h ts. T h e B ed fo rd a n d W illiam s pro cess d o cs n o t seem dcs- tin e d to be of g re a t service in co n n ectio n w ith th e m a n u fa c tu re of edible fa ts , in p a r t ow ing to th e hig h te m p e ra tu re em p lo y ed . I t is questionable w h e th er o r n o t w orking w ith a m ix tu re o f h y d ro g e n a n d oxygen in the p resence of a c a ta ly z e r m ig h t n o t a t tim e s a ffo rd c o n d itio n s leading to explosions.
