BRITISH CHEMICAL ABSTRACTS
B.—A PPLIED C H EM ISTR Y
J U N E 10, 1927
I.— GENERAL; PLANT; MACHINERY.
K in e tic s o f c a ta ly s e d g a s r e a c tio n s in flow s y s te m s . A. F. Be n t o n (Ind. Eng. Cliem., 1927, 19, 494— 497).— I t is assum ed th a t th e phenomenon of catalysis is a result of adsorption or of th e form ation of a superficial layer of an interm ediate compound. The variation of adsorption w ith pressure is given by s /S = a p K l^ a p ) , where s /S is th e proportion of the area covered. W hen adsorption is sm all i t is therefore proportional to th e pressure. In th e case of two reacting gases i t will be proportional to th e product of their
■ p artial pressures. If of two gases one is strongly adsorbed ApjdX=kxSjpz • ap1 /(1 -bapj) an d th e p artia l pressure of th e product is inversely proportional to th e ra te of passage of the m ixture, or th e yield is independent of this rate.
The divergence from th is result in th e synthesis of am m onia is explained by adsorption of th e product.
From these considerations equations are deduced to cover special cases, th e effective pressure of each gas being tak en to be th e mean of th e pressures in the entering and exit gases. The catalysis of hydrogen and oxygen by silver is a case where oxygen an d w ater are strongly adsorbed, b u t n o t hydrogen. H ere i t is shown th a t the yield should v ary w ith th e square root of th e ra te of flow. I n th e synthesis of am m onia, where neither of th e reacting gases is strongly adsorbed, th e equation is X>y=3Jc1S p l6 a x —h2S, where x is th e volume fraction of am m onia an d v th e ra te of gas flow. In th e case of th e contact sulphuric acid reaction, all three gases are strongly adsorbed. In th e conditions m et w ith in practice th e yield is k^SjaF —J^S/Za where F is the fractional conversion of sulphur dioxide. Experim ental results are in each case com pared w ith these equations.
I t is shown th a t w ith uniform conditions over th e cross- section, th e shape of th e cataly st mass is im m aterial.
C . Ir w i n. C o n d e n s a tio n o f a g a s m i x t u r e to f o r m a n id e a l s o lu tio n . J . H . Sim o n s (Ind. Eng. Chem., 1927, 19, 482— 485).— The q u a n tity relations in th e condensation of a gas m ixture of three or more com ponents can only be calculated on th e assum ption of an ideal solution. This assum ption is nearly tru e for th e liquefaction of air and for th e condensation of members of a homologous series, e.g., petrol vapour. A series of equations is developed by which, th e vapour pressures of th e pure components being known, th e dew p oint and th e p o in t of to ta l con
densation m ay be calculated and th e composition of vapour an d liquid a t these or interm ediate tem peratures ascertained. Composition curves based on calculation are given for th e condensation of oxygen, nitrogen, an d argon between 85-5° Abs. and 82-3° Abs., th e dew
point and p oint of to ta l condensation a t 1-395 atm ., respectively. These show good general agreem ent with the results of experim ent. C. Ir w i n.
A u to m a tic d ev ic e s f o r th e e x tr a c tio n o f p o w d e re d m a te r ia ls . S. Pa l k i n an d H . R. Wa t k i n s (Ind. Eng.
Chem., 1927, 19, 535—537; cf. B., 1925, 566).—-Two types of ex tracto r are described in which th e solvent flows upw ards through th e m aterial to be extracted, thus m aintaining i t in a sta te of loose suspension and ensuring complete extraction. The first ty p e consists of a boiling tu b e connected a t th e to p to a reflux con
denser, an d having near its m id-point a side tu b e bent downwards to connect w ith a flask containing th e solvent. The filtering medium, which m ay be absorbent cotton, is tig h tly sandwiched between th e wall of th e boiling tu b e an d a cylinder of wire gauze, which latter has a folded groove running from th e to p to th e point of entry of th e side tube, to perm it free passage of th e solvent vapour to th e reflux condenser. Down the centre of th e boiling tu b e passes a narrow tube, closed a t th e lower end by a p ad of absorbent cotton and funnel shaped a t th e to p to receive th e condensed solvent.
The> m aterial to be ex tracted is situated in th e annular space betw een th e gauze and th e inner tube. W hen in operation, th e condensed solvent flows down th e central tube, passes upw ards through th e solid m aterial, and after filtering through th e gauze and cotton, overflows into th e heating vessel. In th e second type th e heating flask is provided w ith a long vertical tube sealed through the bottom of a wide boiling tube. Over th e to p of the inner tu b e is inverted a long test-tube, which rests loosely on th e bottom of th e boiling tube, in which is contained th e powdered m aterial suspended in solvent.
Solvent vapour from th e flask passes upwards through the inner tube, and, escaping from the bottom of th e test-tube, m aintains th e solid in constant agitation.
The filtering and overflow devices are substantially the same as in th e first type, and the whole extraction vessel is w ater-jacketed. A. liquid seal inside the heating flask prevents vapour entering th e retu rn pipe.
H . J. Do w d e n. C o n tin u o u s e x tr a c tio n a p p a r a tu s . A. H . Cl a r k
(Ind. Eng. Chem., 1927, 19, 534—535).—The apparatus described is of th e Soxhlet type, capable of dealing w ith large quantities of m aterial. The container consists of a pharm aceutical percolator, th e bottom of which is closed b y a cork and connected to th e flask containing the solvent th rough a straig h t tu b e provided w ith a stop
cock, and having a vertically-directed insertion below th e cock. (A lternatively, th is side tube m ay be replaced by a su itab ly b en t tu b e passing into th e solvent flask).
399 °
B ritish C hem ical A b stra c t» —B.
400 Cl. I.— Gen e r a l; Pl a n t; Machinery.
The to p of th e percolator is closed by a cork or clam ped wooden disc and washer, and is connected to th e usual reflux condenser through a straig h t tube having a side tu b e branching downwards. The two side tubes are connected by rubber tu b in g or a Liebig condenser, which for less volatile solvents, e.g., alcohol, is used as a steam jack et to prev en t undue condensation. W hen in operation th e outflow from the percolator is regulated by th e stop-cock to equal the ra te of condensation in th e reflux. The extraction th en becomes continuous, there is no siphoning, w ith its inherent irregularities, involved, and the operation can be stopped a t any m om ent by closing th e stop-cock. H . J . Do w d e n.
L u b r ic a tin g o ils . L a b o r a to r y te s ts in r e la tio n to p r a c tic a l r e s u l t s . A. G. Ma r s h a l l a n d C. H.
Ba r t o n (J.S.C.I., 1927, 46, 130—138 t).—The validity of a num ber of laboratory tests usually applied to lubri
cating oils was exam ined by m eans of engine trials.
I t was found th a t oiliuess had no practical significance in th e lubrication of internal-com bustion engines.
Oxidation and coking tests of th e ty p es a t present in use were found to give results which enormously exagger
a ted th e difference between different lubricating oils in those cases in which th e y were in line w ith practical results, and in m any cases th e y were found to be blended w ith residual filtered cylinder stock, w ith th e resu lt of
“ im proving ” th eir tests from th e popular specification p oint of view. Such blending, however, increases the danger due to deposits in service. E valuation of an oil by means of th e ra te of change of viscosity w ith te m p eratu re was also found to be misleading.
G la s s w o o l a s in s u la to r . Ba t e s.—See V III.
Pa t e n t s.
M e th o d of f u r n a c in g in th e r m o - c h e m ic a l t r e a t m e n t. C. B. J a c o b s , Assr. to E. I. d u Pontd e N e m o u r s
& Co. (U.S.P. 1,625,610, 19.4.27. Appl., 24.2.21).—
Charges which shriuk during therm o-chem ical synthetic reactions are tre a te d u n til a su b stan tial shrinkage occurs, a further charge is then added before th e completion of th e original batch, and th e augm ented b atch is treated
to completion. W. G. C a r e y .
A p p a r a tu s f o r p r o d u c in g r e f r ig e r a tio n . S to r in g d e v ice f o r g a s a n d liq u id s . F. G. Ke y e s, Assr. to Na t io n a l Re f r i g e r a t i n g Co. (U.S.P. 1,622,519 — 1,622,523,29.3.27. Appl. [a—e], 19.2.20, 11.5.20, 8.6.21, 6.11.23, and 4.12.23).— In a refrigerating system com
prising a still, a condenser, an d refrigerator proper, w ith a cooling means used alternately for th e still an d th e condenser, electrical m eans are used to effect th e change over an d cu t off th e heat from th e still, which m ay be controlled by th e level of liquid in th e condenser or in the refrigerator. Check valves m ay be used in th e pipe connexions between th e still an d th e condenser, and between th e refrigerator an d still, whilst a capillary tu b e m ay be used betw een th e condenser and refrigerator so th a t liquid m ay continually pass to th e refrigerator while th e still is working. In (e) a form of electrically heated still is described. B. M. Ve n a b l e s.
H e a tin g g r a n u l a r m a t e r i a l s . J . Y. Jo h n s o n.' From I. G. Fa r b e n i n d. A.-G. (E .P. 268,599, 21.6.26).—
Granular m aterials such as contact masses, or sulphur and granulated coal for th e production of carbon d i
sulphide, are heated uniform ly in an electric furnace by forcing gases th rough th e m to m aintain constant agitation.
Steam superheated a t 250° th u s agitates coke granulated between 1— 10 mm. in a furnace heated electrically by steel electrodes, and water-gas is produced continuously.
W . G. Ca r e y. A p p a r a tu s f o r d e te c tin g a n d d e te r m in in g i m p u r itie s a n d d is s o lv e d m a t t e r in w a te r a n d o th e r f lu id s . E v e r s h e d & V i g n o l e s , L t d . , and C. E. Perry (E.P. 268,597, 18.6.26).— In apparatus, such as th e “ Dionic W ater Tester ” described in E .P . 23,706 of 1907 an d 12,735 of 1914 (cf. B ., 1908, 1036 ; 1915, 454), in which th e im purities an d dissolved m a tte r contained in w ater are ascertained from a m easurem ent of th e electrical conductivity of th e w ater, the tem perature correction is effected by varying th e effective electrical length of th e column of liquid being tested, a tem perature scale being provided to enable this length to be readily adjusted.
J . S . G . Th o m a s. S e p a r a tio n of c o n s titu e n ts o f t e r n a r y g a s e o u s m i x t u r e s . W . Wi l k i n s o n, Assr. to Ai r Re d u c t io n
Co., In c. (U.S.P. 1,619,909, 8.3.27. Appl., 15.10.25).—
A prim ary liquefaction and rectification separates a liquid rich in th e least volatile constituent and a gas rich in th e m ost volatile constituent. Interm ediate vapours are w ithdraw n to another rectifier n o t in heat com m unication w ith th e prim ary one, b u t th e gaseous product of th e auxiliary is liquefied by h e a t exchange w ith a cold product of th e prim ary rectifier and returned to th e auxiliary rectifier. Tho liquid product from the auxiliary is returned to th e prim ary rectifier.
B. M. Ve n a b l e s. G a s a n a ly s is a p p a r a t u s . R . W . J a m e s . From B r o w n I n s t r u m e n t Co. (E.P. 268,637, 3.9.26).—In gas analysis apparatus of the catharometer type in wThieh the relative thermal conductivities of two gases or gas mixtures are compared electrically, the cells in which the gases are respectively received are formed in a single
‘“'metallic block, e.g., of aluminium, winch may be coated with wax or varnish, the block being contained in a metallic housing provided with gas passages, so that temperature differences in the two gases are minimised.
The gas passages are provided with filters for cleaning and drying the gases during passage to the respective
cells. J . S . G. TnoMAS.
C e n trifu g a l s e p a r a t o r . T . C. Th o m s e n, Assr. to Ko e f o e d, Ha u b e r g, Ma r s t r a n d, & He l w e g Ak t i e s e l s- k a b e t Ti t a n (U.S.P. 1,625,919, 26.4.27. Appl., 9.7.26.
Conv., 8.3.26).—See E .P . 259,514 ; B., 1926, 999.
S e p a r a tin g g a s e o u s m i x t u r e s . J . l e Ro u g e, Assr.
to Soc. l’Ai r Li q u i d e (So c. An o n, p o u r l’Et u d e e t l’Ex p l o i t. d e s Pr o c. G. Cl a u d e (U.S.P. 1,626,345, 26.4.27. Appl., 1.2.23. Conv., 16.3.22).— See E .P . 195,046; B., 1923, 638 a.
[H e a tin g c h a m b e r ] f o r g a s - o r o il-fire d fu rn a c e s . R . F . His l o p (E.P. 268,421, 29.12.25).
B ritish C hem ical A b stra c ts—B .
Cl. I L — Fu e l ; Ga b ; De s t k u o t i v k Di s t i l l a t i o n ; Mi m b r a l 0i l3. 401
II.— FUEL; GAS; DESTRUCTiVE DISTILLATION;
MINERAL OILS.
C o m p o s itio n of c o a l. R e s o lu tio n of co al b y s o lv e n ts . C. Co c k r a m and R. V. Wh e e l e r (J .C .S ., 1927, 700 — 718). — The y-compounds of bituminous coals (compounds soluble in pyridine and chloroform—
6 -9% of coal), on extraction w ith (a) light petroleum, (b) ether, and (c) acetone, are separated into the following percentage fra c tio n s: (a) 33, (b) 37, (c) 12, and (d) residue, 18. From a stu d y of th e destructive distillation, oxida
tion w ith hydrogen peroxide an d n itric acid, and ultim ate analysis th e compositions of th e fractions are (a) satu
rated hydrocarbons, 40% ; un satu rated hydrocarbons, 40% ; resins, 20% ; (b) resinols, resines, and resenes;
(c) and (d) resin-like compounds. The treatm en t of bitum inous coal w ith benzene under pressure a t 200°
gave a n e x tract am ounting to 5 ■ 96% of the coal.
Fractionation of this e x tract w ith th e above solvents gave products sim ilar to those obtained b y th e pyridine- chloroform extraction. A t 285° th e ex tract amounted to 7-3% of th e coal, b u t th e general characters of the resulting fractions were th e same. Tables showing the results obtained from different coals are given.
H . Bu r t o n. D iffe re n tia tio n o f p e a t a n d lig n ite . U. Sp r in g e r
and G. Ab e l e (Brennstoff-Chem., 1927, 8, 117—120).—
Differentiation along geological, botanical, or petro- graphical lines is unreliable, as is also th e physical m ethod of determ ining th e adsorptive power towards a dilute solution of ferric chloride, which varies consider
ably -with th e acidity and th e fineness of th e specimen.
The degree of decomposition of th e cellulose in the m aterial m ay be measured by determ ining the degree of hydrolysis produced by 72% sulphuric acid, b u t the values found for different types of coal often lie very close together. A simpler and more reliable differentia
tion is afforded by th e pentosan content of th e material, which is very rarely less th a n 2% for p eat or greater th a n 1% for lignite, though even-so, interm ediate types are inevitably m et with. W. T. K. Br a u n h o l t z.
P a t h of tr a v e l of th e g a s e s in t h e co k e oven.
I I . a n d I I I . W. E . Da v i e s (Gas W orld, 1927, 86, Coking Sect., 2—5, 12— 16 ; cf. B., 1927, 4).—A further discussion of th e influence of th e plastic layer resistance an d th e variation of th e gas pressure in th e h o t and cool zones on th e flow of gases in th e coke oven. The rate of heating of successive layers of m aterial across th e oven and th e am ount of Assuring occurring in th e coke layer are im p o rtan t factors in determ ining th e pressure gradients. The work of Foxwell and others is criticised in th e light of th e au th o r’s theory of th e mechanism of th e coking process. A num ber of applications of the theory to coke-oven practice are summarised.
A . B . Ma n n i n g. R e a c tiv ity of c o k e . G. Ag d ean d H . Sc h m i t t (Brenn
stoff-Chem., 1927, 8, 121— 123).— The differences in re
activ ity exhibited by different cokes are a ttrib u te d to somewhat other factors th a n those described by Nettlen- busch (cf. B., 1927, 208). The reactiv ity of a coke depends essentially on th e accessibility of its carbon, particularly its am orphous carbon, to carbon dioxide, this being determ ined by th e specific num ber, form, and
diam eter of those pores of which the surface is accessible to th e gas w ithout unduly prolonged diffusion. The two principal factors in deciding this are th e nature of the p aren t coal an d th e degree of decomposition of the ta r coke (the solid decomposition product of non
expelled ta r) corresponding to the carbonising tem pera
ture. W hilst graphite m ay be deposited on coke through decomposition of m ethane, it is also derived from decom
position of th e ta r coke a t high tem peratures. The reactivity of coke, under given experim ental conditions, m ay vary as th e experim ent proceeds, owing either to p artial gasification of th e accessible carbon, or to an increase in th e q u an tity of accessible carbon through changes in shape {e.g., due to fracturing).
W. T. K. Br a u n h o l t z. D e te r m in a tio n of r e la tiv e ig n ita b ilitie s a n d c o m b u s tib ilitie s of d o m e s tic c o k es. T e s ts o n th e p o s s i
b ilitie s o f a “ b r a z ie r a n d w e ig h in g m e t h o d .”
T. F. E. Rh e a d and R . E. Je f f e r s o n (J.S.C.I., 1 9 2 7 , 4 6 , 1 6 6 — 1 7 2 t).— -A m ethod for determ ining th e relative ignitability and com bustibility of cokes for domestic use, b y th e continuous weighing of a coke fire in a brazier, has been p artially investigated and some of th e diffi
culties have been overcome. The apparatus used is briefly described, and results are given showing the effects of grade of coke, size of fire, and grate area on th e rate of combustion.
D e te r m in a tio n of th e p h e n o l c o n te n t of g a s liq u o r [c ru d e a m m o n ia liq u o r] a n d e fflu e n ts f r o m co k e- o v en b y - p r o d u c t p la n ts [a n d g a s w o rk s e tc .].
H . Bachi a n d H . Ut h e ( B r e n n s to f f - C h e m ., 1 9 2 7 , 8 , 1 2 0 — 1 2 1 ).— E x i s t i n g v o l u m e t r i c a n d g r a v i m e t r i c m e t h o d s o f d e t e r m i n i n g p h e n o l i n c r u d e a m m o n i a liq u o r a r e b r ie f ly d is c u s s e d . A n i m p r o v e d m e t h o d , i n w h ic h a ll s u l p h u r c o m p o u n d s w h ic h a r e o x id is e d b y b r o m id e a r e c o m p l e te ly r e m o v e d , is t o a c i d i f y t h e liq u o r ( 1 0 0 c .c .) a n d d i s t i l t w i c e t o v e r y s m a ll b u l k , f i lt e r t h e p h e n o lic d i s t i l l a t e , a n d b o il g e n t l y u n d e r a r e f lu x c o n d e n s e r u n t i l a l l h y d r o g e n s u l p h i d e h a s b e e n e x p e l l e d ( a b o u t
£ h r .) . A b o u t 1 c .c . o f a q u e o u s b a r i u m c h lo r id e a n d tw o d r o p s o f p h e n o l p h t h a l e i n a r e a d d e d , a n d t h e n d i lu t e s o d i u m h y d r o x i d e i n s l i g h t e x c e s s . T h e s o l u t io n is a g a i n b o i le d t o a g g r e g a te t h e p r e c i p i t a t e d b a r i u m s u l p h a t e a n d c a r b o n a t e , a n d f i lt e r e d , t h e p h e n o l i n t h e f i l t r a t e b e in g d e t e r m i n e d w i t h b r o m in e b y K o p p e s c h a a r ’s
m e t h o d . W. T . K . Br a u n h o l t z.
V a p o ris a tio n of p e tr o le u m . E . H. Le s l i e and A . J . Go od (Ind. Eng. Chem., 1 9 2 7 , 1 9 , 4 5 3 — 4 6 0 ) .—
The vaporisation of a paraffin-base petroleum has been studied in an apparatus consisting of a heating coil and an equilibrium cham ber in series, immersed in a con- stan t-tem p eratu re b ath . The liquid was fed a t a con
s ta n t ra te of 10 c.c./m in. into th e heating coil and, on a ttain in g equilibrium , th e liquid and vapour phases were collected separately an d analysed by a m ethod giving th eir tru e b.p. curves. E quilibrium “ single
flash ” vaporisation of th e petroleum was carried out by this m ethod a t 2 5 0 ° , 3 0 0 ° , 3 5 0 ° , etc., up to 6 0 0 ° F.
The vapours all contained high-boiling compounds and th e residues low-boiling compounds. The proportion of th e distillate, i.e., th e condensed vapour, which boiled below th e flash tem perature was approxim ately constant
B ritish C hem ical A b stra c ts —B .
402 Cl. I I .— F u e l ; G a s ; D e s t r u c t i v e D i s t i l l a t i o n ; M i n e r a l O i l s .
and averaged 82 • 3% . In a second series of experim ents the crude oil was first vaporised a t 250°, tlie residue tlien vaporised a t 300°, an d so on up to 600° F . ; this con
stitu tes - successive-flash ” vaporisation. I t is less efficient th a n “ single-flash ” vaporisation in yield and in composition of th e distillate, an d also in h e a t require
m ent. The proportion of distillate boiling below the flash tem perature was 80-61% . The results are dis-^"
cussed w ith regard to th eir application to petroleum distillation practice. A. B. Ma n n i n g.
P e tr o le u m l u b r ic a n ts . C. F. Ma b e r y (Ind. Eng.
Chem., 1927, 1 9 , 526—529 ; cf. B., 1926, 810).—D eter
m inations have been m ade of th e sp. gr., viscosity, proportion distilling below 300° (30 mm.), and th e sp. gr.
and viscosity of th e distillate and residue, of a num ber of lubricants from American petroleum s. The behaviour of the original lubricant, of th e distillate below 300°, and of th e residue, in a C arpenter friction-testing machine, has also been studied. In some instances th e distillate supports a heavier load th a n th e original, an d in others it breaks under a lighter load ; th e residues show similar variations in stability. The residual hydrocarbons obtained after extraction of th e residue above 300°
w ith an alcohol-ether solvent approxim ate to th e series Cnil2n-8 for th e Pennsylvania oils, an d to CnH2„_io and C«H|)„_i2 for th e others. Two oils subjected to heavy use have been exam ined an d found to have undergone little deterioration. There appears to be no direct relation betw een th e viscosity and th e stab ility under load, oils of th e same viscosity showing wide variations in frictional tests. A series of oils of th e same viscosity a t 38° (320 sec.) showed a m axim um difference in vis
cosity of 12 sec. a t 98° and of 27 sec. a t 54-4°.
A. B. Ma n n i n g. A c tio n of “ a n t i k n o c k s .” A. Eg e r t o n and S. F.
Ga t e s (N ature, 1927, 1 1 9 , 427).—A ntiknocks do n o t influence detonation in rapid com bustion m ix tu re s ; th e y function in th e in itial stages of th e combustion as negative catalysts. Those m etals which give effective organo-metallic antiknocks are capable of forming higher oxides. Only those ty p es of purely organic substances are effective as antiknocks which re ta rd th e oxidation, a t th e ordinary tem perature, of certain liquid aldehydes. A. A. El d r i d g e.
D e te r m in a tio n o f [h a rd ] a s p h a ltu m c o n te n t of m in e r a l o ils . J . Ma r c u s s o n (Chem.-Ztg., 1927, 51, 190).— The m ethods used h ith erto for the determ ination of asphaltum are neither concordant nor accurate. I t is now proposed to use an ethereal solution of ferric chloride as th e precipitant. 5 g. of oil are dissolved iu 50 c.c. of eth y l ether an d 5 c.c. of a 5% ethereal solution of ferric chloride added. The precipitate is filtered oft and washed w ith ether, ex tracted w ith boiling ether, and dissolved in warm chloroform. This solution is ag itated first w ith 5 c.c. of dilute hydrochloric acid, then w ith 5 c.c. of w ater, and finally, after evaporation to dryness a t 105°, the residue is weighed.
H . Mo o r e. V a lu a tio n o f c o m m e r c ia l m o to r s p i r i t s b y O s tw a ld ’s in d e x n u m b e r m e th o d . W. Os t w a l d
(Petroleum , 1927, 23, 445— 448).—The au th o r traverses th e criticisms raised b y Kroch (B., 1927, 272), and
m aintains th a t the m ethod gives reliable commercial results, even w ith benzine-benzol m ixtures. I t is of use as indicating th e am o u n t of b.p. depression in
alcohol m ixtures. H . Mo o r e.
P o w d e re d c o a l fo r k iln f ir in g . Ha r t f o r d.—See V III.
L in in g s f o r w a te r - g a s m a n u f a c tu r e . Br a d y.—
See V III.
Pa t e n t s.
C o k in g r e t o r t o v e n . J . v a n Ac k e r e n, Assr. to Ko p p e r s Co. (U.S.P. 1,613,068,4.1.27. A p p l ., 14.2.21).—
Each of th e oven walls contains a series of up-flow and a series of down-flow flues which can be in te r
connected. Two channels com m unicate w ith each series of combustion flues, th e channels being altern ately used to supply fuel gas and air to th e up-burning flues, and to receive th e w aste gases from th e dow n-burning
flues. S. Pe x t o n.
P r o c e s s f o r b r iq u e ttin g c o a l. S. R . Wa g e l, Assr.
to Le h i g h Co a l & Na v ig a t io n Co. (U.S.P. 1,618,029, 15.2.27. Appl., 30.9.24).— Coal is bonded w ith clay, bitum en, and a binding agent which is effective between th e tem perature a t which bitum en loses its binding qualities and th a t a t which th e clay becomes sufficiently baked to consolidate th e whole. S. Pe x t o n.
B in d e r f o r b r iq u e ttin g o r m o u ld in g fu e ls, m in e r a ls , e a r t h s , a n d o th e r fin e ly -d iv id e d s u b s ta n c e s . A. Ta p p i n g (E.P. 263,942, 6.10.25).—An aqueous pulp of starch containing alkali or sodium silicate and a preservative, e.g., cresol or form aldehyde, is mixed w ith pitch or bitum en of fairly high m.p. in a heated cham ber under pressure. The tem p eratu re is m aintained above th e m.p. of th e bitum en and th e m ixture is stirred. The m oisture content of th e product is regulated, after mixing, by allowing th e escape of steam therefrom . The p ro d u ct m ay be used either in th e liquid form, or cooled and th e solid binder m ixed and ground w ith th e m aterials to be bonded.
S. Pe x t o n. M a n u fa c tu re of u s e fu l p r o d u c ts b y o x id is in g c o a l. W . A. Bo n e and R . Qu a r e n d o n, Assrs. to Ga s Li g h t & Co k e Co. (E.P. 268,006, 14.12.25).— Coal, or th e residue obtained after heating coal under pressure w ith benzene, is oxidised, preferably a t raised tem pera
tu re, w ith a solution of caustic alkali, and an alkali m anganate or perm anganate, a t ordinary pressure or in an autoclave. A fter filtration, th e alkali salts of benz- enoid carboxylic acids, e.g., mellitic acid, are separated.
W . G. Ca r e y. M a n u fa c tu re o f liq u id fu e ls . I. G. Fa r b e n i n d. A.-G. (E.P. 252,018, 10.5.26. Conv., 8.5.25. Addn. to E .P . 226,731 ; B., 1925, 163).— In liquid fuels containing iron carbonyl, the q u a n tity of th e la tte r is reduced by adding organic compounds of m etals or metalloids soluble in benzene, e.g., m ethyl or ethyl borate or silicate, silicon or lead tetra e th y l, zinc oleate, etc. The fuel m ay also contain organic halogen compounds such as ethylene chloride, chloroform, carbon tetrachloride, an d /o r organic compounds containing oxygen or nitrogen (cf. E .P . 252,019 ; B., 1927, 357). W . G. Ca r e y.
M a n u fa c tu re o f c o m b u s tib le g a s . W . D . Wil c o x
(U.S.P. 1,624,644, 12.4.27. Appl,. 1.4.21).—A m ixture
B r itis h C h e m ic a l A b ê tr a c ts— B .
C l. I I .— Fu e l ; Ga s ; De s t r u c t i v e Di s t i l l a t i o n ; Mi n e r a l Oi l s. 403
of coal- and water-gas is generated b y passing steam through, c o a l' (contained in two generators) previously raised to incandescence by means of an air blast. The w ater-gas produced is superheated by passage through regenerators (previously heated by the combustion of the blast gases) and th en passes upw ards through a charge of fuel, having a layer of uncarbonised coal, to a gas
outlet. , C. 0 . Ha r v e y.
T r e a t m e n t of g a s c o n ta in in g c a r b o n m o n o x id e.
W. H . Kn i s k e r n, Assr. to At m o s p h e r ic Nit r o g e n Co r p. (U.S.P. 1,614,072, 11.1.27. A p p l., 21.9.23).—
Gas to be purified from carbon monoxide is brought into contact with a cataly st in th e presence of steam.
The h eat of tre a te d gases is passed on to th e incoming u n treated gases, which are th e n brought into contact w ith circulating water, producing steam for the reaction.
S . Pe x t o n. D e s u lp h u r is in g c o a l, w a te r , o r m ix e d g a se s fo r illu m in a tin g o r h e a tin g . E. Ra f f l o e b, Assr. to W. E. Le u c h t e n b e r g (U.S.P. 1,624,625,12.4.27. Appl., 3.1.25).—The gas is blown into a desulphurising chamber along w ith finely-divided m aterial capable of absorbing
sulphur. C. 0 . Ha r v e y.
A p p a r a tu s fo r th e d e s tr u c tiv e d is tilla tio n of oil s h a le . L. R . Ab e r n a t h y (U.S.P. 1,618,038, 15.2.27.
Appl., 1.12.24).— Oil shale is distilled in superheated steam in a reto rt, dome shaped a t th e top. W ithin the dome is a conical hood from th e underside of which the products of distillation are withdrawn. The raw shale entering th e re to rt falls on to th e outside of the hood, where it is preheated and distributed in the
retort. S. Pe x t o n.
D e c o lo ris in g a n d c la rify in g a g e n t [fo r p e tro l
e u m ]. H . S. Ch r i s t o p h e r, Assr. to St a n d a r d Oil
Co. o f Ca l i f o r n i a ( U .S .P . 1,617,476, 15.2.27. Appl., 30.9.22).—Pure h y d rated alum inium silicate having the approxim ate composition Al20 3,12Si02,2H 20 is claimed.
S . Pe x t o n. A p p a r a tu s f o r d is tillin g h y d r o c a r b o n s u n d e r p r e s s u r e a n d a c a ta ly s in g a g e n t. F. M . He s s
(U.S.P. 1,625,467, 19.4.27. Appl., 29.9.22).— The hydro
carbons to be cracked are vaporised in a still and the vapours passed through a prim ary dephlegmator and thence to a secondary dephlegm ator into which a catalys
ing agent is introduced. C. 0 . Ha r v e y. E x tr a c tio n of b itu m in o u s m a te r ia ls . I. G. Fa r b- e n i n d. A.-G., Assees. of E. Re i s s m a n n and A. Ric h t e r
(G.P. 437,010, 8.11.25).— The fraction of mineral oils, tars, etc. which is soluble in liquid sulphur dioxide is used as an extracting a g e n t; higher yields are obtained th a n when benzene is used. A. B. Ma n n in g.
M a n u fa c tu re of a n e m u ls io n . D. Fi n l e y, Assr. to Pa r a f f i n e Co s., In c. (U.S.P. 1 ,6 2 5 ,3 0 4 , 1 9 .4 .2 7 . Appl., 17.1.23).—H o t bitum en is added slowly w ith agitation to lime slaked w ith w ater, w ith which is mixed a hot solution of alum , th e tem perature being maintained.
H . Ro y a l- Da w s o n. T r e a tm e n t o f e m u ls io n s o f h y d r o c a r b o n o ils a n d w a te r . St a n d a r d De v e l o p m e n t Co. From C. F . Pe s t e r (Can. P. 247,810, 25.6.24).— The emulsions are treated w ith | — 5% of the sludge obtained in refining
m ineral lubricating oils w ith fuming or concentrated sulphuric acid, and the m ixture is heated a t about 77°.
A . B . Ma n n i n g. I r o n c a r b o n y l p r e p a r a tio n . Ba d is c h e An i l i n- u. So d a- Fa b r. From A . Mit t a s c h and M . Mü l l e r- Cu n r a d i (Can. P . 262,601, 11.7.25).— Iro n carbonyl is dissolved in a hydrocarbon, the solution containing a t least 20% of th e former. H ydrocarbon substitution products which are in ert to iron carbonyl can also be used as solvents. A . B . Ma n n i n g.
C o n v e rs io n of p e tr o le u m h y d r o c a r b o n s . R. Cr o s s, Assr. to Ga s o l in e Pr o d u c t s Co. (U.S.P. 1,624,778, 12.4.27. Appl., 29.10.23).—The oil accum ulates in a pool in an initial stage, and passes thence through a heating stage to a converter which has open vapour communication w ith th e initial stage, whereby the evolved vapours pass through th e relatively cooler oil and thence to th e dephlegm ator and condenser. The unvaporised oil provides energy for producing a tu rb u len t condition in th e converter and m aintaining th e carbon
in suspension. C. O . Ha r v e y.
P r e p a r a t i o n a n d t r e a t m e n t of o le fin e s. Pe t r o l e u m Ch e m ic a l Co r p., Assees. of II. S. Da v i s and W. J . Mu r r a y ( E .P . 248,375, 24.2.26. Conv., 24.2.25).—
The define m ixtures resulting from th e cracking of petroleum vapours a t a nearly constant tem perature between 600° and 650° are subjected to a physical frac
tionation in suitable p lan t of which a diagram and detailed description are given. Three m ain fractions are col
lected containing : (1) ethylene and propylene, (2) A“- and A M m tylenes and isobutylene, and (3) A“- and Ap-amylenes, isopropylethylene, as-m ethyletliyl- ethylene, and trim ethylethylene, together w ith hexylenes an d higher olefines. The fractions are th en selectively absorbed in diluted sulphuric acids of various strengths or in hydrochloric acid, which effects a further separation of th eir constituents owing to th eir varying reactivity w ith acid. The resulting alkylsulphuric acids or alkyl chlorides, on hydrolysis, yield th e corresponding alcohols.
E.g., from th e cracking of “ gas oil ” (d 0-856) at601°there are obtained per barrel (42 gals.) 2-6 gals, of th e amylene fraction. This is agitated w ith 12-2 lb. of 65% sul
phuric acid a t below 20° for 6 hrs., allowed to settle, and th e lower acid layer separated, neutralised, and distilled, when 0-28 gal. of crude te rtia ry alcohols (chiefly amyl) is obtained, resulting from th e interaction of trim ethylethylene, m ethylethylethylene, and some higher olefines w ith th e acid, and subsequent hydro
lysis. The upper layer of residual olefines, containing th e amylenes and isopropyl ethylene, is distilled up to 60°, yielding 1 ■ 1 gals, of distillate. This is treated w ith 15-3 lb. of 77% sulphuric acid a t 35— 40° for 6 hrs., when th e above olefines are absorbed. After settling, the lower acid layer is diluted w ith w ater so as to reduce th e acid strength below 20% , and distilled to obtain 0-56 gal. of crude secondary am yl alcohols. Similarly, th e butylene fraction (102 cub. ft.) obtained from the gas oil is treated w ith 65% sulphuric acid, which extracts isobutylene etc., and yields, on hydrolysis, 0-28 gal. of tertiary butyl alcohols. The residue, on treatm en t with 77% sul
phuric acid, produces on hydrolysis 0-46 gal. of second
ary alcohols formed from th e butylenes. A. Da v id s o n.
B ritish C hem ical A b stra c ts—B .
404 Cl. I I I . — T a b a n d T a r P r o d u c t s . Cl. IV.— D y e s t u f f s a n d I n t e r m e d i a t e s .
P u lv e r is e d fu e l b u r n e r s . H . A. Pr o c t e r ( E .P . 268,417, 30.1.26).
A p p a r a tu s fo r th e g e n e r a tio n o f g a s f r o m liq u id h y d r o c a r b o n s f o r c o m b u s tio n , lig h tin g , a n d o th e r p u r p o s e s . II. E. Go l d s b r o u g h, an d Go l d s b r o u g h Pa t e n t s Co., Lt d. (E.P. 266,765, 1.9.25).
H e a tin g g r a n u l a r m a t e r i a l s (E.P. 268,599).—
See I.
G a s a n a ly s is a p p a r a t u s (E.P. 268,637).— See I.
M a te r ia l s i m i l a r to c o m p r e s s e d a s p h a lt (E.P.
260,621).—See IX .
B itu m in o u s e m u ls io n s (E.P. 268,411).— See IX . O rg a n ic s u b s ta n c e s f r o m g a s m ix tu r e s (E.P- 262,404).— See X X .
ni.— TAR AND TAR PRODUCTS.
D e te r m in a tio n of p h e n o l. Ba c h a n d Ut h e.—
See II.
Pa t e n t s.
S e p a r a tio n of th e c o m p o n e n ts of lo w - te m p e r a tu r e t a r w ith o u t d is tilla tio n . Z e c h e M . S t i n n e s , an d A.
We i n d e l (G.P. 433,455, 5.9.23).— The crude ta r is tre a te d w ith benzine a t th e ordinary teinperature, and, after separation of th e p recipitated pitch an d rem oval of th e benzine by distillation, th e residual oil is resolved into n eu tral oil and phenols by tre a tm e n t w ith alcohol of less th a n 60% strength. The use of caustic soda being avoided and th e solvents used being recoverable, th e process is economical. A. B. M a n n i n g .
S e p a r a tio n o f th e p h e n o ls a n d n e u t r a l o ils of lo w - te m p e r a tu r e t a r . Ze c h e M. St i n n e s, an d A.
We i n d e l (G.P. 436,444, 22.7.22. Addn. to G.P. 433,268).
— The procedure of th e principal p a te n t is modified by th e use of a m ixture of alcohol and a concentrated solu
tion of am m onia, th e m ixture containing n o t more th a n 60% of alcohol for th e extraction of th e phenols. The solubility of th e phenols in alcohol is increased several tim es b y th e addition of am m onia, so th a t extraction is facilitated, an d th e phenols are recovered directly in a highly pure form. Thus 32% of phenols, p u rity 98—
99% , were recovered by one ex traction from a low- tem p eratu re ta r of which th e to ta l phenol content was 40% . The am m onia an d alcohol are recovered by distillation w ithout appreciable loss.
A . B. Ma n n i n g. A s p h a lt s u b s t i t u t e . J . Dr e s c h e r (Austr. P. 104,402, 4.12.23).—Lignite ta r, heated if necessary, is mixed w ith sulphur, resin, an d a m ineral filler such as sand or b asalt, th e m ixture bro u g h t to 80°, and tre a te d w ith powdered
lime. A. B. Ma n n i n g.
D is tilla tio n o f t a r a n d th e lik e . W. B. Da v id s o n, A. C. Mic h b e, a n d E. W. Mu d d im a n (U.S.P. 1,626,588, 26.4.27. Appl., 23.4.26. Conv., 1.4.25).— See E .P . 255,919 ; B., 1926, 815.
B itu m in o u s e m u ls io n s (E.P. 268,4-11).—See IX . IV.— DYESTUFFS AND INTERMEDIATES.
F o o d d y e . H. Jo h n s o n an d P. St a u b (Ind. Eng.
Chem., 1927, 19, 497— 498).— The green dye known as F a st Green F.C .F., now proposed for admission to the
list of perm itted colours, is form ed by th e condensation of 2 m ob. of ethylbenzylanilinesulplionic acid w ith 1 mol.
of p-hydroxybenzaldehyde-o-sulphonic acid followed by oxidation w ith lead peroxide. The jj-hydroxybenz- aldehydesulphonic acid is prepared from p-nitrotoluene- 0-sulphonic acid by oxidation in alkaline hypochlorite solution to th e corresponding stilbene compound, which is converted into y-nitrobenzaldehyde-o-sulphonic acid by oxidation w ith alkaline perm anganate. The y-nitro- compound is reduced w ith ferrous carbonate, diazotised, and warm ed a t 80—90° w ith dilute sulphuric acid, where
b y p-hydroxybenzaldehyde-o-sulphonic acid results. The dye is superior, both as regards fastness and intensity, to th e dyes a t present in use. H . J . Do w d e n.
Pa t e n t s.
P r e p a r a t i o n of azo d y e s . I . G. F a r b e n i n d . A.-G.
( F . P . 611,004, 12.2.26. Conv., 13.2.25).—Azo dyes for acetate silk and wool are obtained by coupling diazotised to lu id in e - G ) - s u lp h o n ic acids w ith arom atic am ines which contain no sulphonic or carboxylic groups. Exam ples a r e : p-toluidine-w -sulphonic acid — diphenylam ine (yellow), 5-nitro-o-toluidine-6)-sulphonic acid-)«- benzyl- ethylanilinc (red), 3 : 5-dinitro-o-toluidine-co-sulphonic acid—)>-ethyl-ß-naphtkylamine (blue-violet). The dinitro
com pound is obtained by anim ation of 2-chloro-3 :5 - dinitrotoluene-co-sulphonic acid. C. H o l l i n s .
P r e p a r a t i o n o f [azo] d y e s c o n ta in in g c h r o m iu m . Ge s. f ü r Ch e m. In d. i n Ba s l e (F.P. 609,518, 19.1.26.
Conv., 16.2.25).—Azo dyes containing chelate groups are heated w ith a solution of chromic chrom ate. E xam ples are : 4-chloroaniline-3-sulphonic acid —)*- salicyclic acid (greenish-yellow on w o o l); 4-chloro-2-aminophenol-5- sulphonic a c id —)»- l-phenyl-3-m ethyl-5-pyrazolone (re d );
1-amino-2-naphthol-4-sulphonic acid—)>-l-m-nitrophenyl- 3-methyl-5-pyrazolone (bluish-red). C. Ho l l i n s.
P r e p a r a t i o n of v a t d y e s of th e a n th r a c e n e s e r ie s c o n ta in in g n itr o g e n . I . G. Fa r b e n i n d. A.-G., Assees. of M. Ku n z (G.P. 436,537, 17.2.25).—Amino- a n d diam ino-anthraquinones or th eir arylidene deriva
tives, an d su bstitution products of these types, are condensed w ith aldehydoanthraquinones or th e ir deriva
tives to give v a t dyes. V at dyes are th u s obtained from 2-am inoanthraquinone and 2-aldehydoanthraquinone (orange-yellow) or l-chloro-2-aldehydoanthraquinone (yellow) or l-am ino-2-aldehydoanthraquinone (c la re t);
from l-chloro-2-am inoanthraquinone an d l-am ino-2- aldehydoanthraquinone (claret-red) or l-azido-2-alde- hydoanthraquinone (sahnon-pink product, m .p. 331—
333°); from l-chloro-2-benzylideneam inoanthraquinone and 2-aldehydoanthraquinone (orange-yellow ); from 2 : 6-dibenzylidenediam inoanthraquinone an d 2-alde
hydoanthraquinone (yellow), or 1-am ino-2-aldehydo
anthraquinone (claret -product, m .p. over 350°), or l-chloro-2-aldehydoanthraquinone (yellow product, m .p. over 360°); an d from 2-benzylideneamino-3- m ethylanthraquinone and l-am ino-2-aldehydoanthra- quinone (pink product, m.p. above 340°). C. Ho l l i n s.
P r e p a r a t i o n of c o n d e n s a tio n p r o d u c ts of th e a n th r a q u in o n e s e r ie s [ f s o d ib e n z a n th r o n e s ] . I. G.
Fa r b e n i n d. A.-G., Assees. of A. Wo l f r a m (G.P. 436,077, 12.8.24. Addn. to G.P. 426,710. Cf. E .P . 255,277 ; B.,
C l . V.— Fi b r e s; Te x t i l e s; Ce l l u l o s e; Pa p e r.
B ritish C hem ical A b stra c ta —B .
405
1926, 780).—3 : 9-Diaroylperylenes, heated with alumin
ium chloride a t high tem peratures, are converted into
i'sodibenzanthrones. C. Ho l l in s.
P r e p a r a t i o n o f a c id w o o l d y e s of th e a n th ra q u in o n e s e r ie s . I. G. Fa r b e n i n d. A.-G., Assees. of W. Mie g
(G.P. 436,539,15.11.24).— The sulphonated (acridinated) products from dianthraquinonylam ines are reduced, e.g., w itli sodium hydrogen sulphide, probably to dihydro- acridines w ith elim ination of one sulphonic group.
1 : l'-D ianthraquinonylam ine, after disulphonation with 15% oleum a t 95— 100°, is reduced by sodium hydrogen sulphide to a compound, which in th e presence of bisul
phite dyes wool an olive-green, becoming brown on after - chroming. Di-oc-anthraquinonyl-l : 5-diamino- anthraquinone yields a sim ilar dye. F rom 1 : 2-diantlira- quinonylam ine by tre a tm e n t w ith 15% oleum and subsequent reduction w ith alkaline sodium sulphide th ere is obtained a red acid dye ; reduction w ith copper d u st an d sulphuric acid in place of sodium sulphide leads to a yellow-brown acid dye, giving brown shades on after-chrom ing. D i-a-anthraquinonyl-2 : 6-diamino- anthraquinone, from 2 : 6-dichloroanthraquinone and 1- aininoanthraquinone, gives, by tre a tm e n t w ith 10%
oleum a t 95—100° followed by reduction w ith alkaline hyposulphite, a brownish-red acid dye. C. Ho l l in s.
M a n u fa c tu re o f v a t d y e s tu ffs. M. P. Sc h m id t, Assr. to Gr a s s e l l i Dy e s t u f f Co r p. (U.S.P. 1,625,826, 26.4.27. Appl., 20.11.23. Conv., 25.11.22).—See E.P.
207,553 ; B., 1924, 1008.
M a n u fa c tu re o f d y e s tu ffs c o n ta in in g c h ro m iu m . F. St r a u b, Assr. to Soo. Ch e m. In d. i n Ba s l e (U.S.P.
1,626,167— 9, 26.4.27. Appl., 29.1.26. Conv., [a], 14.2.25, [b, c], 16.2.25).— See E .P . 247,556; B ., 1926, 910, and F .P . 609,518, preceding.
V .—FIB R E S; TEXTILES; CELLULOSE; PAPER.
C o n s titu e n ts of c e ll-w a ll o f f la x f ib r e . A. E.
Ca s h m o r b ( J .C .S ., 1927, 718—731).— The “ cellulose- complex ” obtained from flax fibre b y freeing the fibre from extraneous m atter, from pectin by ammonium oxalate treatm en t, and from hemicellulose by washing w ith 4% aqueous sodium hydroxide, h ad an «-cellulose co n ten t of 82—83% . H ydrolysis of th e cellulose-complex w ith 2% barium hydroxide solution a t 100° gave galactose together - w ith sm all am ounts of pentoses.
W ith 5% sulphuric acid a t 100° practically no hydrolysis took place, b u t a t 130—140° dextrose, galactose, fucose, xylose, and traces of “ uronic acid ” were produced.
P a r t of th e dextrose produced is obtained by th e hydro
lysis of th e non-cellulose portion of th e complex.
W ater a t 140— 150° hydrolyses th e complex yielding a hemicellulose (3-5% of w eight of fibre) containing ab o u t 21% of “ uronic anhydride,” probably mainly galacturonic anhydride, 60% of galactose, and 10— 14%
of rhamnose. In addition, th ere is obtained a syrup soluble in 70% alcohol (1% of weight of fibre) containing xylose an d fucose. A t tem peratures above 175° water disintegrates th e fibre. H . Bu r t o n.
D e te r m in a tio n o f c e llu lo s e b y sa c c h a rific a tio n . A. Ki e s e l and N. Se m ig a n o v s k y (Ber., 1927, 60, [B], 333—338).— D ry cellulose is preserved w ith 7—10
tim es its am ount of 80% sulphuric acid for 2 | hrs. a t th e atm ospheric tem perature. W ater is added in the proportion of 15 c.c. for each c.c. of acid used, and the resulting solution is heated for 5 hrs. on th e steam bath.
Cellulose is thereby converted q u antitatively into dex
trose. The presence of proteins (gelatin and casein) is w ithout influence on th e change. Dextrose, mannose, galactose, lsevulose, in v ert sugar, xylose, and arabinose retained 99-7, 97-7, 99-9, 26-0, 66-06, 72-2, and 84-5%
of th eir reducing power after treatm en t w ith acid as above. F o r th e determ ination of cellulose in botanical m aterial, th e substance is subjected to a prelim inary tre a tm e n t w ith 2% hydrochloric acid for 3— 5 hrs. on th e w ater b ath , and saccharification of the residue is accomplished as described above, or, alternatively, the process m ay be applied to th e “ crude fibre ” obtained by one of th e custom ary m ethods. D irect saccharifica
tion leads to correct results only in th e absence of ketoses
and pentoses. H . Wr e n.
S u lp h ite b o ilin g p ro c e s s . M . Ho n ig a n d W . Fu c h s (B e r ., 1927, 6 0 , 782—786).— A v e r y m a r k e d in c r e a s e is o b s e r v e d b e tw e e n t h e c o n s u m p ti o n o f io d in e b y o r ig in a l s u l p h i te l iq u o r s a n d t h o s e w h ic h h a v e b e e n p r e s e r v e d in a b o u t 1% a lk a l in e s o lu tio n . T h e a m o u n t o f lo o s e ly c o m b i n e d s u l p h u r d io x id e is g r e a t e r t h a n t h a t w h ic h c a n b e a c c o u n t e d f o r b y t h e a ld e h y d e s a n d s u g a r s p r e s e n t . F u r t h e r , t h e a m o u n t o f o r g a n ic a l l y c o m b in e d s u l p h u r o u s a c i d i n a n o r ig in a l s u l p h i te liq u o r is i d e n t i c a l w i t h t h a t o f a “ f e r m e n te d ” l iq u o r . T h e s u l p h u r d io x id e m u s t t h e r e f o r e b e c o n s id e r e d t o b e c o m b in e d w i t h t h e lig n i n s u l p h o n i c a c id . T h e p r e s e n c e o f a n a ld e h y d ic g r o u p in t h e l a t t e r is i m p r o b a b l e s in c e t h e c o p p e r n u m b e r o f c a r e f u ll y d i a l y s e d l ig n in s u lp h o n ic a c id is n e g lig ib le . I t is p r o b a b l e t h a t t h e s u l p h u r o u s a c i d is u n i t e d t o t a u t o m e r i c a l l y a c t i v e p h e n o ls . H . Wr e n.
U n s a tu r a te d s u g a r c o m p le x e s in w o o d . W.
Fu c h s (Ber., 1927, 6 0 , 776—782).—The yield of sugars obtainable by th e hydrolysis of wood w ith acids can be considerably increased a t th e expense of th e lignin by suitable p re-treatm en t of th e m aterial with perbenzoic acid, particularly if this has been preceded by th e action of 0 -5 % sulphuric acid a t th e atm ospheric tem perature.
The increase is due to th e more copious presence of ferm entable sugars, presum ably dextrose, in the solutions from th e oxidised wood. The pentosans in the original wood are decomposed to a considerable extent under the conditions of th e hydrolysis, and the pentosan content of all the solutions from th e wood subjected to the varied treatm en ts is small and alm ost equal. The observations lend support to th e hypothesis of the presence of un- satu rated sugar complexes in wood. H . Wr e n.
A c tio n of s o d iu m h y d ro x id e o n c e llu lo se u n d e r h ig h p r e s s u r e . S. Od é n and S. Li n d b e r g (Ind. Eng.
Chem., 1927,19,132—133).—C otton cellulose was treated w ith about 7 tim es its weight of approxim ately 3-5N - caustic soda solution and heated in an autoclave slowly to 372° an d m aintained a t this tem perature for some hours. A fter removal of gaseous reaction products the residual tran sp aren t yellow-brown solution was fraction
ated to recover m ethyl alcohol, acetone, and fight oil, evaporated to dryness, and extracted with ether to
B ritish C hem ical A b stra c ts—B .
406 C l . V.— F i b r e s ; T e x t i l e s ; C e l l u l o s e ; P a p e r .
remove pitch. The residue, consisting of alkali salts of organic acids, was then steam -distilled a t 110—585°, and t i e distillate fractionated under reduced pressure into light and, heavy oils and pitchy m atter. The reaction products resulting from these operations are tab u lated and th eir quantities recalculated on th e basis of 100 g.
of pure ash-free cellulose. U ltim ate analysis of these products reveals losses equivalent to about 3-25% of the original cellulose. The densities and refractive indexes of the oil fractions are recorded ; these oils are highly unsaturated, and are possibly ketonic in character.
D . J . No r m a n. D e te r m in a tio n o f s o d a . Te x t o r and Ho f f m a n.—
See V II.
U s e fo r h y d ro c e llu lo s e . Ga r d n e r.—See X III.
C e llu lo se e s t e r v a r n is h e s . Da b i s c h.— See X III.
Pa t e n t s.
P r o d u c tio n o f s tif f fa b ric s w h ic h s ta n d w a s h in g . A.-G. Cj x a n d e e (E.P. 264,783,1.3.26. Conv., 21.1.26).—
Artificial silk is woven w ith vegetable or anim al fibres and th e resulting fabric exposed for a short tim e, e.g., 15 secs., a t about 15° to th e action of an inorganic acid, e.g., sulphuric acid (d 1-53). The strength of th e acid, th e duration of th e treatm en t, and th e proportion of artificial silk in th e fabric determ ine th e degree of stillness.
D . J . No r m a n. M a n u fa c tu re o f f ib r e b o a r d . R. W . Hi l t o n, Assr. to Ke m p e r- Th o m a s Co. (U.S.P. 1,624,599, 12.4.27. Appl., 1.11.23).—W eather-resistant fibre board is made by thoroughly m ixing fibre pulp in an aqueous solution of soap and adding lead acetate to precipitate insoluble lead soap, th e am ount of soap being sufficient to provide n o t over 3% of insoluble soap in the
fibre. W. G. Ca r e y.
M a n u fa c tu re o f s tr a w b o a r d . M. E. Pe n n i n g t o n
an d A. B. Da v i s (U.S.P. 1,625,090, 19.4.27. Appl., 18.4.25).— The straw board comprises disintegrated new straw which has been disinfected and steam distilled, rendering it inodorous and sterile.
H . Ro y a l- Da w s o n. W a te rp ro o f a n d lik e m a te r ia ls . C. Ha f e l e (E.P.
266,813, 3.12.25).— Two or more webs of fibrous m aterial are com pounded by means of a sulphur-free rubber solution containing approxim ately 10% and 5% , respec
tively, of finely-powdered zinc oxide and barium sulphate.
The composite web is th e n satinised and dried by passing it between rollers a t 140—160°. D . J . No r m a n.
P r o te c tio n o f a n im a l fib r e s a g a in s t a tta c k b y a lk a lin e liq u id s . M. Be r g m a n n (G.P. 437,836,14.10.23).
— Sulphite-cellulose waste liquors in which th e active groups have been oxidised, reduced, or halogenated, or the active constituents of th e liquor after th e y have been subjected to one of these processes, are used for protecting th e fibres during tre a tm e n t w ith alkaline liquids.
L. A . Co l e s. M a n u fa c tu re a n d u s e of a r tif ic ia l s ilk a n d th e lik e . Br i t i s h En k a Ar t i f i c i a l Si l k Co., Lt d., Assees. of N . V. Ne d e r l a n d s c h e Ku n s t z i j d e f a b r. ( E .P . 244,496, 15.12.25. Conv., 15.12.24).— The affinity for dyestuffs of artificial silk consisting of or containing cellulose silk, e.g., viscose, m ay be increased by tre a tm e n t w ith an oxidising agent, to increase th e content of oxycellulose,
or decreased by tre a tm e n t w ith liquids which, w hilst having a solvent action on some or all of th e non-cellulose constituents, have no appreciable action on cellulose.
Eor example, th e affinity for dyestuffs of viscose m ay be increased by exposure for ab o u t 2 hrs. a t th e ordinary tem perature to a solution of sodium hypochlorite con
taining 5% of available chlorine, or decreased b y heating for ab o u t 24 hrs. a t 150 “ w ith glycerin. D . J . No r m a n.
M a n u fa c tu re of a r tif ic ia l th r e a d s o r f ila m e n ts . Soc. POUR LA FaBR. DE LA SoiE “ RhODIASETA ” (E.P.
259,190, 31.8.26. Conv., 1.10.25. Addn. to E .P . 233,384 ; B., 1925, 587).—In a modified process for th e d ry spinning of artificial threads involving th e use of tem perature-controlling elements, as described in th e prior p a te n t, th e controlling elements are connected in parallel, and in order to obtain different tem peratures in different p a rts of a cell more th a n one elem ent m ay be used, th e tem perature-controlling fluid to one of th em being cooled if necessary. B. P. Ri d g e.
T r e a t m e n t of c e llu lo s e a c e ta te o r p r o d u c ts m a d e th e r e w ith . Br i t i s h Ce l a n e s e, Lt d., and G. H . El l i s ( E .P . 266,777, 29.10.25).—P a tte rn or other effects are produced on tex tile fabrics m ade from or containing cellulose acetate threads or yarns b y th e local applica
tion (by printing, stencilling, etc.) to th e fabric of one or more substances which m odify th e delustring action of h o t or boiling aqueous m edia or m oist steam , and after
wards subjecting th e m aterial to such delustring tre a t
m ent, preferably w ith m oist steam . The applied sub
stances m ay be mechanical resists, solvents for cellulose acetates, or substances soluble in cellulose acetate, those of th e last two groups which are n o t sufficiently soluble in w ater being either dissolved in liquids which are non
solvents for cellulose acetate, or dispersed colloidally in aqueous media. The delustring m ay be prevented, retarded, or accelerated b y th e agents used, an d th e effects m ay be fu rth er enhanced b y dyeing th e fabric w ith suitable dyestuffs. B . P . Ri d g e.
N o n -in fla m m a b le p la s tic m a s s e s . Pa t h é Ci n é m a, a n c. Et a b l. Pa t h é Fr è r e s (F.P. 612,414, 30.6.25).—
Cellulose esters or ethers are mixed w ith th e phosphoric esters of halogen-substituted aliphatic alcohols an d th e usual plasticisers and highly chlorinated compounds.
E.g., 1 kg. of nitrocellulose is m ixed w ith 400 g. of tri- trichloroethyl phosphate and 400 g. of a plasticiser (tricresyl phosphate etc.), and th e whole dissolved in a volatile liquid. The m ixtures serve for the production of artificial fibres, plastic masses, films, etc.
B. Fu l l m a n. M a n u fa c tu re of c o a te d la id p a p e r . G. W.
Jo h n s o n. F rom A. M. Co l l i n s Ma n u f a c t u r i n g Co.
(E .P. 267,013, 13.9.26).— O rdinary paper is coated p re
ferably on both sides w ith, e.g., a solution of casein or glue, optionally in adm ixture w ith fillers and colouring agents, an d is th en passed between embossing rollers which impress a laid p a tte rn on th e coating. The lines th u s formed are blended w ith th e m ain coating while th is is still m oist in order to give th e effect of a w ater
m ark in th e body paper. The sheet m ay, if desired, receive a second plain coating, an d is finally rolled to produce an even sm ooth surface suitable for high-grade
printing. D. J . No r m a n.
