BRITISH CHEMICAL ABSTRACTS
B.—APPLIED CHEMISTRY
DEC. 8 and 15, 1933 *
I.— G EN E R A L; P LA N T; MACHINERY.
E lectrically heated stea m generators for process in dustries. S. Z. Ow e n (Ind. Eng. Chem., 1933, 25, 1078—1079).—The conditions favourable for the use of electrically heated steam generators (which have efficiencies of 95%) arc discussed. D. K. M.
G lass-lin ed steel equipm ent in chem ical in
d u stry. P. S. Ba r n e s (Ind. Eng. Chem., 1933, 25, 1080—1083).—Borosilicatc enamels, m.p. 98‘2° approx., are resistant to all acids except IiF , but must be used with caution against caustic alkalis. The conditions of service should always be specified. For the steel shells 0 2-C 2H 2 butt-welds should be used. After sand
blasting, the cast Fe or low-C steel is coated (<£ 2 coats) with enamel by applying either hot dust enamel to the steel after withdrawal from a furnace a t 1010° or wet spray enamel cold prior to entering the furnace. The finished surface may be tested with a low-voltage current passing through a brush with Cu b ristles;
arcing indicates defects. Oil-jacketed vessels may be used up to 316° approx. Localised over-heating or over
cooling, mechanical abuse, or too great a strain a t clamped or flanged joints resulting from the use of unsuitable gaskets may cause failure. Generally glass- lined steel equipment may be reconditioned. D. K. M.
D rying of so lid s. VI. D iffusion equations for the period of constant drying rate. E. R. Gi l l i l a n d and T. K. Sh e r w o o d (Ind. Eng. Chem., 1933, 25, 113-1—1136; cf. B., 1933, 347).—An equation is derived and a graph given for the determination of the moisture distribution at any instant in a solid slab drying a t a const, rate. The graph is used to calculate crit. moisture content at the junction of the const, and falling-rate periods. Experimental verification lias been
obtained. D. K. M.
G rinding and grinding m achinery. P. Ro s i n
and E. Ram m lkr (Chem. Fabr., 1933, 6 , 395—399, 403— 405).—For most powders which have undergone fine grinding th e relation between R, the residue loft on a sieve, and the grain size («) is of the type R — lOOe-^”, b and n being cousts. This enables the curve between R and n to be obtained from 2 determined points and the sp. surface of the powder to be calc. This is not the case with coarse-grinding. Relations of capital and power costs to the fineness of grinding in various cases are shown by curves. Curves showing the relationship between speed of revolution and fineness of product of centrifugal mills and roller mills are also given. Drum mills have an optimum degree of filling for which through
put is a max. Ball mills have a crit. speed of rotation at which the balls revolve evenly with the walls. The
optimum speed is some fraction of this, depending on the filling ; in some cases there are two optimum speeds.
H20 content of material to be dried is often im portant ; coal is best dried while being ground. I t is very un
economical in power to run a mill a t reduced through
put, and the power consumption is also affected by the efficiency of the screens or other devices for removing
fines. C. I.
Concentration by flotation. M olecular forces.
A. Fu r i a (Chimica, 1933, 1, 195—197).—The theory of surface tension and flotation effects is reviewed. E. L.
M echanical an alysis for technical purposes.
J . St i n y (Geol. u. Bauwesen, 1931, No. 4 ; Proc.
Internat. Sôc. Soil Sci., 1933,8, 113).—The construction and use of a special sedimentation tube arc described.
A. G. P.
N ephelom etry as an aid to industrial an alysis and control. .T. G r a n t (Ind. Chem., 1933,9, 317—319, 353—355).—Apparatus and technique are described, and applications to analysis of I i 20 , oils, org. solvents, metals,-foods, biological materials, smokes, and fumes are
discussed. E. S. H.
Instrum ent for rapid determ ination of m oisture content of hygroscopic m aterials [e.jf., tobacco], A. Pf e i f f e r (Chem. Fabr., 1933, 6 , 406—407).—The sample is placed in a small »»pen box over which fits a capillary hygrometer, the total vol. enclosed being 100 c.c. The v.p. is thus measured relative to th a t of the air over pure H 20 and results are independent of temp. It is most conveniently applicable where it is desired to bring a material to a const. H 20 content.
If II 20 content in wt.-% is desired the apparatus is not so suitable as it must be calibrated for each type of
substance tested. C. I.
Efficiency o f rectifying apparatus. E. Kmscn- baum (Chem. Fabr., 1933, 6 , 431— 436).—A lecture describing the influence of many factors, espeeially composition of liquid, foaming, and velocity of vapour.
In the systems examined max. efficiency was attained at a vapour velocity of about 0-2 m./sec. E. S. H.
Flow of sim p le fluids through porous m a te ria ls.
G. H. F a n c h e r and J . A. Lew is (Ind. Eng. Chem., 1933, 25, 1139— 1147).—D ata relating to the flow of oil, H 20 , and air through tubes filled with Pb shot and different sands, and through sandstone and ceramic blocks, are given, together with friction-factor charts. The flow resembles th a t through pipes in th a t there is a definite change from viscous to turbulent flow as velocities
increase. D. K. M.
P la sto m eter.—See XIV. R otary vac. filtration.
Im m ersion refractom eter.—See XVII.
a
* T h e re m a in d e r of th is se t of A b s tra c ts will a p p e a r in n e x t w eek’s issue.
991
B r i t i s h C h e m ic a l A b s t r a c t s — B .
9 9 2 Cl. f . — Ge n e r a l ; L'l a n t ; Ma c h i n e r y.
Pa t e n t s.
A utom atic kiln-drying apparatus. f. Mu r p h y, and
Ba n d o n Mi l l in g & El e c t r i c Li g h t i n g Co., Lt d. ( B . P .
398,628, 25.7.32).—A kiln (for grain etc.) having a single floor is provided with rotating rakes which move the material outwardly, then circumferentially, to discharge
apertures in the floor. B. M. V.
H eat-exchange devices in w hich liquids are heated in the liquid phase. 0 . D. Lu c a s, and
Wh e s s o f. Fo u n d r y & Eng. Co., L td . (B.P. 399,186, 24.12.31).—-Liquid is heated in helical elements (I I ) and pipe coils (P) while preferably flowing through part of II remote from the fire, then through P surrounding the fire, and finally through / / in the lower p art of the stack which forms a cylindrical casing around //. H are constructed by slitting, dishing, and twisting annular discs of metal, which are then welded together in pairs.
B. M. V.
H eat-transm itting m aterials. N. V. De Ba t a a f- s c h e Pe t r o l e u m Ma a t s. ( B . P . 399,441,18.5.33. IIoll., 22.6.32).—Fluids suitable for use in heating mineral oils prior to distillation or for the concn. of NaOII lyes etc.
include high-boiling alkylated aromatic compounds, e.g., triiVopropyl- or disec.'-butyl-naphthalene, or their
hydrogenation products. L. A. C.
H eat-transfer m ed ia. Ge s. f. Dr u c k t r a n s f o p.m- a t o r b n ( Ko e n e m a n n- Tr a n s f o r m a t o r f.n) G.m.b.H. (B.P.
399,757, 29.5.33. Austr., 30.5.32).—The use is claimed of mixtures of ZnCl2 with other anhyd. metal chlorides, e.g., a mixture, m.p. 180°, of ZnCl„ 75, NaCl 10, and
KC115%. " L. A. C.
Cooling d rum s for cooling of liquid and m olten su b stan ces. A. Ge r s t e n b e r g (B.P. 399,252, 6.5.32).—
In, e.g., a margarine cooler operated with liquefied gases the oil chamber in the stuffing box on the trunnion is so situated th a t any oil creeping towards the interior of the drum m ust run against the outflowing cooling gas ; within the drum, oil th a t may be entrained from the compressor is caught on a perforated lining before it can reach the heat-transm itting surface. B. M. V.
G rinding m ills. H. Barthelmess (B.P. 398,914, 29.3.32).—In a disc grinder, preferably with vertical axis, the fixed disc is resiliently supported and to it is attached a downwardly extending conical trough (T ) to catch the ground material ; a smaller cone attached to the rotating disc is placed within T, the combination causing a down
ward current of air in the annular space and an upward one within the cone back to the feeding zone. Fines may be removed through perforations in the trough.
B. M. V.
Separating separate kinds from a m ixture of solid bodies of different specific g ra v ity . II.
I Ie i d e n r e i c h (B.P. 399,294, 11.7.32. Ger., 11.7.31).—
The material is subjected to a jigging action assisted, if desired, by steady upward currents of hydraulic or pneumatic fluid. The jigging is produced by the rise and fall of alternate grate bars. [Stat. ref.] B. M. V.
Sedim entation apparatus. Do r r Co., In c. (B.P.
399,297, 23.7.32. U.S., 23.2.32).—In a thickener the raking mechanism is supported and driven entirely from
an untrussed central column within which are also situated the uprising feed pipe and control valve.
B. M. V.
A pparatus for separating and recovering solid m atter [e .g ., long w ood fibres] from liquid su spen
sion . C. B. Th o r n e (B.P. 398,980,6.7.32. Can., 3.12.31).
—A continuous moving screen, preferably a rotating cylinder, is formed with apertures large enough to pass the short fibres and wood flour while retaining the long fibres. In the earlier parts, reciprocating paddles are provided to agitate the liquid ; in the later parts, sprays are provided to wash the long fibre backwards into dis
charge means. B. M. V.
Purification of solu tion s. W. C. Gr a h a m, Assr.
to Gi l c h r i s t & Co. (U.S.P. 1,903,215, 28.3.33. Appl., 13.2.25).—In, e.g., the separation of colloids from sugar solutions by neutralisation, a large body of liquid is kept in const, circulation and agitation sufficient to keep all floes in suspension (but insufficient to prevent the formation of large floes) and to disseminate the gradually added reagent almost instantaneously throughout the liquid. Then, under the batch system of working, the pH remains uniform throughout the bulk, although changing gradually ; under the continuous system, the pu of the bulk is held const, while raw liquid and reagent are added simultaneously a t different points, and treated liquid and floes are removed from another
point. B. M. V.
P u m p s for filter-p resses and the lik e. H. H.
Da v i s, and S. H. Jo h n s o n & Co., Lt d. (B.P. 398,684, 28.11,32).—A single-acting steam piston lifts a single- acting pump ram and attached wt. on the suction stroke, the discharge being by gravity only. A suitable valve
motion is described. B. M. V.
Vacuum d istillation . E. H. Pa y n e, Assr. to
St a n d a r d Oi l Co. ( U . S . P . 1,899,916, 28.2.33. Appl., 18.12.29).—An apparatus in which oil (e.g.) is distilled in a moving thin layer and the vapours are in stan t
aneously condensed comprises a spiral trough surrounding a vertical heater which itself is surrounded by a H20 - cooled surface. The bottom of the trough is level (in diametral cross-section) so th a t the oil forms a uniformly thin layer; the metal of the trough is thick but tapered, so th a t the heat conducted from the heater is uniformly
spread. B . M. V.
M eans for filtering liq u id s. Br y c e, Lt d., and A. A. Si d n e y (B.P. 399,207, 31.3.32).—A filter, particu
larly for liquid fuels, in which the medium is in the form of a deeply-fluted column, is described. B. M. V.
D istillation p rocess. W. Sc h u i.t z e (U.S.P.
1,903,573, 11.4.33. Appl., 23.10.29. Ger., 10.10.28).—
To distil wood rosin, fatty acids from fats, crude oil, etc.
a suitable quantity of the material is preheated to approx. 200° and then allowed to flow on to a surface a t 225—255°/ ]> 1 mm. in a thin stream so th a t it forms a layer 3— 4 mm. thick ; the non-volatile portion is led
away continuously. S. M.
E m u lsifyin g apparatus and the like. W. M.
Me lm o r e, and Fl u i d Pr e s s u r e Pu m p s, Lt d. ( B . P .
399,014, 15.9.32).—A hand-operated pump has the outlet constricted by two adjacent cones or m ulti-start
Cl. I f . — I-’u e l ; G a s ; 'X’a r ; M i n e r a l O i l s . B r i t i s h C h e m ic a l A b s t r a c t s — B .
993
th re a d s ; the cylinder oscillates together w ith the supply reservoir, which is thereby agitated. B. M. V.
Separation of solid particles held in suspension in gaseous fluids. E. C. St. - Ja c q u e s (B.P. 398,779,
12.5.33. Fr., 13.5. and 20.7.32).—The gas is passed outwards through a polygonal centrifugal rotor the centre portions of the flat sides of which are perforated for the exit of clean gas, the passage of solid particles being prevented by the high speed. The solids collect in the angles and may be removed downwards by jarring
or a H 20 flush. B. Mi V.
Apparatus for m ix in g gases w ith liquids. Be l i. Br o s. (Ma n c h e s t e r, 1927), Lt d., C. G. Be n s o n, and
A . M . Mi t c h e l l ( B . P . 398,491, 7.12.31).—A valve for the gas is closed by the pressure of the gas on a diaphragm and opened by the pressure of the liquid on a larger diaphragm on the same stem. A spring with screw adjustm ent is provided, for the fine regulation of the opening or closing pressure. B . M . V.
T ransferring liquefied g ases from one v essel or container to another. N. Y. Ma c h i n e r i e e n- kn Ap p a r a x e n- Fa b r i e k e n (B.P. 399,112, 4.4.33. Ger., 12.5.32).—Liquefied gas is transferred from a transport container (T) to a container for use ({/) by means of a pump which partly evacuates an intermediate con
tainer (/) which then quickly receives the liquid from T while the gas produced is pumped (through a cooler if necessary) to an em pty container (E, preferably another transport container). When T is emptied or when the pressure in E has risen sufficiently high the connexions of the pump are reversed and gas is blown from E to I and liquid from I to U. A simpler scheme in which I and U are combined in one vessel is also
described. B. M. V.
D ecom position of g a s m ix tu res w ith low evapor
ation point. Ma p a g Ma s c h i n e n f a b r. Au g s b u r c- Pl a t t- l i n g A.-G., and M . Fr a x k l (B.P. 399,405, 11.3.33).—
In, e.g., the resolution of air the evaporation of 0 2 in the lower part of the rectifier is effected only by the sensible heat of the low-pressure air after expansion without liquefaction. The wash liquid (air) is produced by cooling of high-pressure air by the leaving N2
followed by expansion. B. M . V.
C la s s if ie r s . Dorr Co., Inc. (B.P. 398,579, 25.4.32.
U.S., 29.5.31).—See U.S.P. 1,881,875; B „ 1933, 688.
A pparatus [centrifugal fan] for circulating gases or vapours in tunnel ovens and like plant. S. R.
Hi n d and B. Ai.a m s (B.P. 399,436, 11.5.33).
Pulp and dirt separator. Paper stuff hydrator.
—See V. Pptn. apparatus for g a se s.—See XI.
D ehydration of vegetables etc.—See X IX . D ust- count apparatus.—See X X I. T reating hard H „0.
—See X X III.
II.— F U E L ; G A S ; T A R ; MINERAL OILS.
P h ysical and chem ical properties of coal in relation to classification. II. F. Ya n c e y and K. A.
Jo h n s o n (Trans. Amer. Inst. Min. Met. Eng., 1932, 1 0 1 ,
171—200).—Friability, slacking characteristics, yield of products from low-temp. assay, and agglutinating vals.
of 100 coals (lignite -y anthracite) have been plotted against B.Th.U., fixed C, and ultim ate analysis. Class
ification on the basis of fixed C and the use of analyses on the as-received basis is preferred. Ch. Ab s.
M oisture determ ination for coal classification . E. St a n s f i e l d and K. C. Gi l b a r t (Trans. Amer. Inst.
Min. Met. Eng., 1932, 1 0 1 , 125—147).—Low-rank coals should be classified by analysis on the moist-coal basis.
A rapid procedure for determining the true II 20 of coal in the seam is described. I l 20 -holding charac
teristics of Alberta coals are given. Methods for partial drying or air-drying of coal, and for determining residual 11,0 in coal, are discussed. Ch. Ab s.
Proposed m ethod for determ ining the oxidation tem perature of anthracite. J. L. My e r (Trans.
Amer. Inst. Min. Met. Eng., 1933, 1 0 1 , 215—223).—
Powdered anthracite is gradually heated electrically in a current of N2 or 0 2. At 300—400° with 0 2 there is a sharp break in the tem p.-resistancc curve, and the temp, rises rapidly. In 2—3 min. the coal temp, is several hundred degrees > the furnace temp., then slowly falls, and when only ash is left the bridge can no longer be balanced. The N2 curve is smooth. Ch. Abs.
B ase exchange of coal ash . H. Mo n n ig (Angew.
Cliem., 1933, 4 6 , 631—634).—The silicates occurring in coal which are capable of exhibiting base exchange are identical with those in arable soil, and it is probable th at to this fact the fertilising action of coal ash may be in part ascribed. The exchange of Ca is considerable and th at of Jig relatively small, but both vary very appreci
ably with the type of coal. II. F. G.
Coke form ation. IX . Softening and sw ellin g of coal in relation to p la sticity . R. G. D a v i e s and R. A. Mott (Fuel, 1933, 12 , 330—340; cf. B., 1933, 899).—The plastic stage of a coking coal undergoing carbonisation has been studied by examining the stru ct
ure of the coke obtained by heating samples of the coal to successively higher temp, in the Sheffield laboratory coking apparatus. The temp, of initial gas evolution rises with the C content of the c o a l; in general, the softening point also rises with the C content but the correlation in this case is less regular. The softening point (temp, of initial contraction) is little affected by increasing the load up to 50 lb./sq. in., but falls as the load is further increased to 200 lb./sq. in., again remaining const, up to loads of 600 lb./sq. in. The min. softening temp. (S°) so produced corresponds approx. with Holroyd and Wheeler’s “ active decomp, tem p.” (B., 1929, 116).
T hat S° is th a t temp, at which active decomp, of the ulmins occurs is confirmed by the sharp rise in reactivity towards alkaline K M n 0 4 (cf. Heathcoat, B., 1933, 256) of coals preheated to just above th a t temp. The temp, of initial expansion ('1'°) of a column of particles is, for a given rate of heating, unaltered by the application of external pressure. The mechanism of the changes occur
ring in the coal up to 2’° is discussed in detail. Just above S° each individual coal particle begins to swell (stage of local plasticity), whereas a t T° pore formation begins in the mass as a whole and the cake of loosely- bonded particles becomes a single mass of more or less
homogeneous structure. A. B. M.
a 2
B r i t i s h C h e m ic a l A b s t r a c t s — B .
994 Cl. I I .— Fu e l ; Gas ; Ta r ; Mi n e r a l Oi l s.
D eterm ination of the degree of gasification (Aus- gasungsgrad) of cokes. W. Lu d e w i g (Gas- u. Wasser- facli, 1933, 76, 733—736).—1 g. of coke was heated rapidly to 1000° in a tube connected to a vessel of 3-2 litres capacity which had been evacuated to an initial pressure of 5 ram. Hg. H eating was continued for 60 min., when the vol. of gas evolved was measured (after adjusting to atm . pressure), a correction being made for the residual air in the collecting vessel. The gases consisted principally of CO and 1I2, with smaller quantities of C 02 and N2, and occasional traces of CII4.
The yields varied from 21-6 to 43-8 c.c./g. (2-01—
5-14 wt.-%) for a series of gas cokes, and from 21-4 to 29 -8 c.c./g. (2 • 13—2 • 54 wt.-%) for a series of 4 metall
urgical cokes. The influence of tim e of heating and of initial pressure has been studied and the results are compared with those of a previous investigation (B., 1932, 374). Drying the coke a t 110° had no influence on the results. A coke is regarded as completely carbonised when a sample tested as above yields >■ 30 c.c. of gas per g. The method has been applied to show th a t a fall in the gas yield (expressed in therms) from certain retorts was due to incomplete carbonisation and not to leakage
losses. A. B. M.
Carbon dioxide content of com bustion g a ses as a chem ical index figure in g a s technology. P.
D olch (Brcnnstoff-Chem., 1933, 14, 361—364).—The max. CO., content (M) of the combustion gases from a fuel gas burning in air is related in a simple manner to the C and “ available ” H contents of the fuel gas. For fuel gases obtained by the complete gasification of coal the val. of M gives an insight into the processes occurring during the production of the gas. M may be calc, from the composition of the fuel gas, or determined directly by experiment. Some applications of the relationships
involved are discussed. A. B. M.
T estin g the thread-draw ing pow er as a technical m ethod of investigation in the bitum en industry.
W. R odiger (Kolloid-Z., 1933, 65, 11—20).—Two methods for determining thread-drawing power (I) are described. The variation of this property with temp., origin, and composition of some bitum ens has been determined. In a series of asp h alt-tar mixtures, (I) decreases with decreasing dispersity. E. 8 . IT.
R ecent p rogress applied to extraction and pur
ification of benzol. E. Ba r r e t (Chim. et Ind., 1933, 29, Spec. No., 515—522).—Modern plant for the extrac
tion and continuous rectification of benzol is described.
E. S.
Active-charcoal and w ash -oil benzols. H.
Heckei, (Gas- u. Wasserfach, 1933, 76 , 645—649).—A criticism of Engelhardt and Ruping’s remarks (cf. B., 1933, 611). The benzols produced by both processes can be compared only if the adsorption takes place in both cases before or after 8 removal. Figures for gum formation in a wush-oil benzol are given in support of
this. ' R. X. B.
[A ctive-charcoal and w ash-oil benzols.] A.
K ngei.hardt and H. R u m o (Gas- u. Wasserfach, 1933, 76, 649).—A reply to Heckel’s criticism (cf. preceding
abstract). R. x. B.
A cetylm ethylcarb inol and diacetyl in pyro- ligneous acid. J. P r i t z k e r (Chem.-Ztg., 1933, 57, 793—794).—To determine Ac2 (I) in pyroligneous acid 10 c.c. are diluted to 50 c.c., neutralised w ith NaOH, and 20 c.c. distilled into a mixture of N H 20H,HC1, NaOAc, and NiCl2 [wt. of Ni dimethylglyoxime (III)
X 0-5962 = wt. of (I)]. To determine CHAcMe*OH (II) the process is repeated with the addition of 50 c.c.
of 30% aq. FeCl3 to the distillation flask. After deduc
tion of (III) S ( I ) , the remainder X 0-610 = wt. of (II).
A. R. P.
D esign of plant for recovery of gasolin e from natural g a s. N. Ma y e r (Petroleum, 1933, 29, No.
38, 1—5).—The methods of recovery of gasoline, viz., by absorption in oil, by compression, or by adsorption on active charcoal, are briefly described, and some of the theoretical principles and calculations underlying the design of suitable plant are discussed. A. B. M .
R ecovery and treatm ent of natural g a s for p ro
duction of g a so lin e. C. Be r t h e l o t (Chim. et Ind., 1933, 29, Spec. No., 511—514).—An account is given of the recovery of natural gas in Europe and the process of extracting gasoline therefrom by means of active C.
E. S.
D etonation of narrow cu ts of paraffin-base ga so lin e. R. A. Vi r a b y a n and Y. Y. Go v a k o v (Grozn.
Neft., 1932, 2, No. 11—12, 52—60).—Elimination of fractions to improve the anti-knock properties of Grozni gasoline is too expensive, but compounding with Baku gasoline rich in naphtlienes is feasible. Ch. Ab s.
G um sta b ility of g a so lin es. I I . O bserved and true oxygen -b om b induction periods. J. \V.
Ra m s a y and II. S. Da v i s (Ind. Eng. Chem., 1933, 25, 934— 936 ; cf. B., 1932, 584).—The 0 2-bomb induction period in accelerated gum tests is affected by the rate of rise of temp, of the gasoline while heating up the bomb. A correction is given so th a t induction periods corresponding to raising the gasoline instantaneously to the test-bath. temp, may be calc. D . K. M.
A bsorption spectra of gaseou s charges in a gasoline engine. L. Wi t h r o w and G. M. Ra s s w e i l e r
(Ind. Eng. Chem., 1933. 25, 923—931).—Photographs of the spectra of the gases in an internal-combustion engine producing power, using C6H6, C0Me2, MeOH, gasoline, tso-C8IIjS (I), and mixtures of (I) with gasoline, E t20 , and with C7II16 us fuel and of the absorption spectra of some of these fuels, together with descriptions of the apparatus by which these were obtained, are given.
Chemical reactions have been detected in the non
inflamed fuel-air mixtures under certain conditions. As the conditions under which knocking occurs are approached the chemical changes in the knocking zone ahead of the flame either increase in degree or change in nature. The observations support the theory th a t knock is due to spontaneous ignition ahead of the flame front preceded by relatively slow reactions in the non
inflamed gases, D. K. M.
T heoretical and practical aspects of the [oil-]
cracking p rocess. An o n. (Chem.-Ztg., 1933, 57, 762—764).—Various cracking processes are briefly de
scribed. I t is concluded th a t future developments will lie along the lines of hydrogenation-cracking. A. B. M.
C l . I I .— F u e l ; G a s ; T a b ; M i n e r a l O i l s . B r i t i s h C h e m ic a l A b s t r a c t s — B .
995
Fractionation of petroleum into its constituent hydrocarbons. E. W . Wa s h b u r n (Ind. Eng. Chem., 1933, 25, 891—894).—A description of tlie methods URed and a list of the hydrocarbons separated are given.
D. K. M.
M ethods for ap p roxim atin g critical and therm al properties of petroleum fractions. K. M. Wa t s o n
and E. F. Ne l s o n (Ind. Eng. Chem., 1933,25,880—887).
—Using the Engler distillation curve and d, curves and/or formulœ are given for determining the molal average b.p. and a characteristic factor, and these are used for the determ ination of approx. mol. \vt., sp. heats (in liquid and vapour states), crit. temp, and pressure, heat of vaporisation, and heat content (at. diSerent pressures) of petroleum fractions. D. K. M.
E valuation of kerosene. W. Jakubowicz (Przemyst N aft., 1933, 8 , 284— 288).—Kerosene of high photo
metric quality contains a min. amount of naphthenic acids and S compounds. The optimum quantity of aromatic compounds is 10—20%. The b.-p. range of kerosene from diSerent sources is not a measure of its illuminating qualities. Ch. Ab s.
U ral (Perm ) crude oil. D. M. Ma u k o and I. I.
La p k i n (Bull. inst. res. biol. Perm, 1932, 8 ,145— 149).—
Crude oil from wells 1 and la- contains gasoline 25, S >> 5, asphaltenes 6, resins 8, and paraffin wax 1-5%.
The kerosene (9%) is unsuitable for illumination owing to the high content of aromatic compounds. The bottoms (56'7% ) are suitable for cracking and the
production of asphalt. Ch. Ab s.
D eterm ination of the yield of oil from oil sands under laboratory conditions. B. Mi k h a i l o v (Grozn.
Neft., 1932, 2 , No. 7—8, 61—65).—The yield depends on the original pressure in the sands and the original gas pressure, the physico-chemical condition of the crude oil and gas or dissolved gas, the physical nature of the subterranean reservoir, the rate of production, the area of the deposit, and the diam. of the wells.
Ch. Ab s.
M ethyl alcohol as addendum to liquid fuel.
A. W. Sc h m i d t (Erdöl u. Teer, 1933, 9 , 74—77 ; Chem.
Zentr., 1933, i, 2896).—MeOH (used with E tO H and C6I I 6) as an addendum to petrol has good anti-knock properties. The performance of such mixtures is
discussed. A. A. E.
Knocking characteristics of naphthene hydro
carbons. W. G. Lo v e l l, J . M. Ca m p b e l l, and T. A.
Boyd (Ind. Eng. Chem., 1933, 25, 1107—1110).—The relative tendency to knock in a single-cylinder variable- compression engine has been measured for 69 cyclic hydrocarbons ; the measurements were made on the hydrocarbons in admixture with gasoline and the results have been expressed by using the antiknock eSect of N H 2Ph as a standard of comparison. The relation between structure and tendency to knock appears to be quite consistent and comparable with previous relations found for the paraffin and aliphatic olefine hydrocarbons (B., 1931, 328, 661). ' H. S. G.
V apour-liquid equilibria of hydrocarbon m ix tu res. E. C. Br o m i l e y and D. Qu i g g l e (Ind. Eng.
Chem., 1933, 25, 1136— 1138).—D ata are given for the
following m ix tu res: n-C7II]8 (I)-PhMe (II), (II)- h-C8H 18 (III),moC8II18-(III), (l)-methylc!/ck>hexane (IV), (IM IV )-(II), (I)-(IV)-COMe2. II. S. G.
Lubricating o ils in contact w ith cla y s. Effect of tim e a t elevated tem peratures. V . A. Ka l i c h- e v s k y and J . W. Ra m s a y (Ind. Eng. Chem., 1933, 2 5 ,
941—943).—When decolorising oil by contact with clay air has a deleterious effect. W ith acid-treated clays (I) the colour improves as the time of contact is increased to a max., beyond which the colour remains const. W ith natural clay (II) a t 371° the colour improves as the time of contact increases to 20—30 min. ; it then darkens for the next 30 min., after wnich it improves and remains const. With (I) the colour showed an improve
ment with raised contacting temp. (II) reaches its max.
decolorising power a t a lower contacting temp, th an (I).
The relationship between quantity of clay and colour intensity a t equilibrium m ay in some cases be repre
sented by a Freundlich adsorption isotherm.
D. K. M.
Flow of fluids through porous m a teria ls.—See I.
EtOH from C2H 4. P olym erisation of propylene.
E xtracting phenols.—See III. R efractory cem en ts for coke ovens.—See V III. A ction of m otor fuels on A l.—See X.
Pa t e n t s.
Coking retort ovens. Ko p p e r s Co. o f De l a w a r e,
Assees. of J. Va n Ac k e r e n (B.P. 398,610, 8.6.32. U.S., 8.6.31).—Vertical ducts are provided in the partitions between adjacent flame flues through which a p art of the combustion gases is returned to dil. the combustible m ixture and so lengthen the combustion flame to give more uniform heating. The upper end of the duct is connected to the tops of the adjoining flame flues ; the lower end is connected to the inlet port for gas and air, which is designed with a restricted orifice so th a t the combustible mixture has an injector effect, thereby effecting the desired recirculation of the combustion gases.
A. B. M.
(a) Coking, (b) apparatus for carbonisation, of coal. E. W. Th i e l e, Assr. to St a n d a r d Oi l Co. (U.S.P.
1,899,887—8, 28.2.33. Appl., [a] 14.5.28, [b] 27.7.29).
—The coal, preheated to about 360°, is charged into a vertical coking chamber wherein it is mixed with coke which has been preheated to a sufficiently high tem p., e.g., 1100°, to effect the desired carbonisation of the coal.
The coke is preheated by partial combustion in air in a separate coke heater, and the gases from the latter are burned with secondary air and utilised to preheat the coal, preferably in a rotary kiln. A. B. M.
Coking of (a) [solid], [b] so lid , carbonisable m aterial, (a, b) L. Ke r n, (b) F. C. Ke r n (U.S.P.
1,899,808—9, 28.2.33. Appl., [a] 23.2.29, [b] 18.6.30).
—(a) Coal etc. is finely crushed and mixed with a plasticising agent, e.g., an acid, acid sludge, oxychloride, or Cl2, etc., which reacts w ith the inorg. constituents of the coal, with the evolution of C 02 and S compounds, to form a plastic binding material. The mass is then briquetted and carbonised, (b) When the inorg. con
stituents (gangue) of the coal are high in S i02 an alkaline plasticising agent, e.g., aq. NaOH or N a2C03, is used.
A. B. M.
B r i ti s h C h e m ic a l A b s t r a c t s — B .
9 9 6 Cl. I I . — Fu e l ; Ga s ; Ta r ; Mi n e r a l Oi l s.
Manufacture of porous siliceou s carbon. L. Ke r n
(U.S.P. 1,899,810, 28.2.33. Appl., 18.6.30).—Carbon
iferous S i02 materials are carbonised a t low temp., e.g., 250°, pulverised, treated with a hot mineral acid, preferably I I 2S 0 4, and the product is washed and dried.
A. B. M.
Separation of acetylene [from g a s m ix tu res].
F. J. Me t z g e r, Assr.' to Ai r Re d u c t i o n Co., In c. (U.S.P.
1,900,655, 7.3.33. Appl., 11.2.32).—The gas is absorbed a t >• room temp, and under pressure (P) in an alkyl carbonate, e.g., E t2C03, and is expelled by heat and reduction of P ; the process is repeated if desired, or P may be reduced or the temp, raised in stages to obtain C2II2 of increasing purity. L. A. C.
R em oval of [w ater-soluble] im p u rities from crude petroleum . L. L. Da v i s, A. He n r i k s e n, and .i. J. Al l i n s o n, Assrs. to Co n t i n e n t a l Oi l Co. (U.S.P.
1,901,228, 14.3.33. Appl., 5.7.28).—H 20 is added, to a petroleum oil containing I I 20-sol. inorg. compounds and the mixture heated to below its b.p. under sufficient pressure to prevent substantial evaporation and with sufficient incidental agitation to rupture the asphaltic films surrounding the impurities. The heated mixture is then passed through a filter bed of granular material and the brine and oil are separated by settling.
II. S. G.
T reatm ent of petroleum o ils. M. S. Da r r o w
and L. S. Sweeney (U.S.P. 1,903,094, 28.3.33. Appl., 3.5.28).—The oil stock, after H 2S 0 4 treatm ent and sludge removal, is passed through a filter bed comprising an ntim ate mixture in a comminuted state of fuller’s earth 18-7, solid NaOH 28-7, and PbO 22-6 wt.-% , to effect neutralisation and clarification. H. S. G.
T reatm ent of hydrocarbon oil. E . R . Bi r k h i m e r,
Assr. to At l a n t i c Re f i n i n g Co. (U.S.P. 1,904,402, 18.4.33. Appl., 15.5.31).—An aromatic aldehyde, e.g., PhCHO (¿1), is added to a viscous oil containing paraffinic and naphthenic hydrocarbons and the mixture heated to effect complete dissolution. On cooling, a solution richer in naphthenic hydrocarbons separates from the oil and is removed, and the remaining oil is re-treated with A. A is removed from both portions by distillation, thereby yielding fractions richer respectively in paraffinic and naphthenic hydrocaroons. II. S. G.
D ew axing of o ils. A. He n r i k s e x, Assr. to Co n t i n e n t a l Oi lCo. (U.S.P. 1,901,240,14.3.33. Appl., 18.1.30).
—To a wax-containing oil is added a suitable solvent and a mixture of a colloidal asphaltite, e.g., grahamite.
and petrolatum. The resultant mixture is chilled and
centrifuged. I I . S. G.
Conversion of gaseou s paraffin or olefine hydro
carbon into liquid arom atic hydrocarbons. A. S.
Ra m a g e, Assr. to M. Wi i.e y and 0 . L. Sm i t h (U.S.P.
1,900,997, 14.3.33. Appl., 21.5.30).—Wild natural gas
oline is separated into a stable liquid portion (A ) and a highly volatile portion, which latter is admixed with steam (2—5%) and heated a t 327—482° by contact with a hot mass of Fe20 3, and then brought into contact with more Fe20 3 a t 538—593°. Further steam is added to the resulting vapours to bring the total am ount up to 15%
and the mixture is brought into contact with an extended surface of metallic Fe a t 641—704° and the resulting
gases are subjected to partial condensation. The con
densate is mixed with A and the uncondensed gases are bubbled through the mixture. II. S. G.
T reatm en t of low -b oilin g hydrocarbons. H.
Ro s t i n(U.S.P. 1,904,172,18.4.33. Appl., 2.3.29).—Low- boiling hydrocarbons, with or without the addition of I I 2, a t 220—300° are conducted over a porous ore, e.g., minette, which has been freshly reduced in an atm . con
taining free H 2. II. S. G.
Purification of naphtha sto ck s. I). E. Da y (U.S.P.
1,902,221, 21.3.33. Appl., 5.12.31).—Cracked gasoline stocks are mixed w ith a conc. aq. solution of a caustic alkali and passed through a heating zone a t 177—260°
under sufficient pressure to prevent substantial evapor
ation and for a period of tim e sufficient to polymerise unstable hydrocarbons. The pressure is then released and air introduced into the mixture, which is passed to a vaporising zone (A) from which the purified vapours are removed for fractionation, condensation, and separation from the II20 . Sufficient H 2Q is introduced into A to replace th a t evaporated, and the products of reaction and introduced I I 20 containing the caustic alkali are continuously withdrawn. H. S. G.
Production of sp ir its, o ils, and the like from coal or sim ila r m aterials. T. R . Dix o n (B.P. 398,601, 17.5. and 7.6.32).—Coal or other carbonaceous material is treated with an org. acid produced by bacterial action, e.g., lactic acid, and/or with fungi or enzymes developed a t a later stage of the process, and the liquor produced
is fractionated. A. B. M.
Production of m otor-d rivin g sp irits. H. Ka f f e r
(U.S.P. 1,904,830, 18.4.33. Appl., 27.3.30. Ger., 29.10.26).—Crude benzine from the low-temperature distillation of coal (500 kg.) is mixed w ith finely-divided active C (100 kg.) and autoclaved in an atm . of II 2 for 3 hr. a t approx. 350°/110 atm . ; the contents of the autoclave are subsequently blown with steam.
H. S. G.
M anufacture of [liquid] fuel. L. Ke r n (U.S.P.
1,899,811, 28.2.33. Appl., 18.6.30).—Coal or other solid carbonaceous material is finely ground, e.g., to 200- mesh, and mixed with H 20 to form a loose but plastic cohesive mass, which is then carbonised by being rapidly heated to about 550°. The porous, highly voluminous product is ground and mixed w ith a fuel oil, with which it forms a stable suspension suitable for use as a liquid fuel. If the initial material is rich in S it is preferable to use dil. HC1 or aq. MgCL instead of the II 20 in the plastic
ising operation. A. B. M.
M anufacture of gu m -inhibited m otor fuels.
Gu l f Re f i n i n g C o ., A s s e e s . o f E. Ay r e s (B.P. 399,733, 26.8.32. U.S., 26.10.31. A d d n . t o B.P. 394,511 ; B.,
1933, 695).—0-0005—0-01% o f t h e p r o d u c t s m e n t i o n e d i n t h e p r i o r p a t e n t a r e a d d e d t o a m o t o r f u e l a s g u m
i n h i b i t o r s . II. S. G .
Preparation of crude oil for distillation into lubricating o ils. A. E. Pew, ju n ., Assr. to Sun Oi l
Co. (U.S.P. 1,903,407, 4.4.33. Appl., 28.2.28).—A residual oil containing lubricating fractions is separated from a crude oil by partial evaporation and fractionation a t a temp. <[ th at of substantial cracking, and is mixed
B r i t i s h C h e m ic a l A b s t r a c t s — B .
Cl. I II.—OncA.Nic I n te r m e d ia te s .
with ¡in alkali solution. The mixture is subjected, while distributed over a large area, to a pressure sufficient to effect simultaneously, a t the temp, of the oil, the evaporation of the solvent of the alkali and a lighter
fraction of the oil. H. S. 0 .
M anufacture of v iscou s oil by polym erisation of cracking products. N. V. De Ba t a a f s c h e Pe t r o l e u m Ma a t s. ( B . P . 399,646, 23.9.32. Holl., 16.11.31).—
Prior to the polymerisation process, the cracked products are refined with dil. H 2S 0 4 followed by an alkali wash and, if desirable, fractionation. H. S. G.
M anufacture of hydrocarbon products. J. Y.
Jonxsox. From T. G. Fa r b e n i n r. A.-G. (B.P. 399,527, 4.3. and 28.5.32).—Addition of > 10% of a polymeris
ation product of wobutylene having mol. wt. 1000 to a hydrocarbon product, e.g., lubricating oil, grease, wax, benzine, or illuminating oil, gre’atly improves the viscosity characteristics, electrical properties, etc.
of the products. H. S. G.
H eat-transm itting m aterials [for oils]. Filtering liquids. Vac. d istillation .—See I. O il-sol. co m pounds from acid refining of o ils. Fatty acids [from paraffin w a x ]. K etones from im pure v o l
atile a cid s.—See III. N aH S and Na„S. Producing oxygenated org. com pounds. H 2 + CO.—See VII.
A sphaltic com p osition s. Road surfaces.—See IX.
Coating of b itum inous surfaces.—See XIII.
III.— ORGANIC INTERM EDIATES.
A cetic acid from p in ew ood . E. IIagglu.vd (Svensk Pappers-Tidn., 1932, 35, 749—750 : Chem. Zentr., 1933, i, 2761).—Sawdust was treated with 2-5% I I 2S 0 4 by Schorger’s method ; the AcOII formed and extracted with E t20 amounted to 1-27%. The acid contained 24 • 8% H C 02IT ; hence the % of easily hydrolysable AcOH in pinewood is 0-9. Reheating the residue with IIoSO, afforded only a very small quantity of volatile
acid. ' A. A. F,
Preparation of alcohol from ethylene obtained from cracked g a s. M . A. Da l i n and V . S. Gu t u i r y a
(Azerbaid. Neft. Choz., 1933, No. 3, 66—75).—The gas was passed over CaCl2, adsorbent C', quartz + II2S 0 4, and through a hydrolyser for separation of EtO H from E tH S 0 4. The yield of EtO H (90%) is 5 • 5—6-2% .
Ch. Ab s.
C atalytic polym erisation of propylene. F. Hi
Ga y e r (Ind. Eng. Chem., 1933, 25, 1122—1127).—
D ehydrated “ floridin ” (I) polymerises C3IIG a t 340- • 350°/l atm. to a highly unsaturated liquid th a t gives on steam-distiUation 90% of an almost gum-free motor fuel of CgII18 no. 87. The fraction b.p. <C 150° contains homologous C5—C9 olefines (much C6) and some paraffins.
The activity of (I) is improved by treatm ent with conc.
HC1 (which removes much Fe), washing, and renewed dehydration, and still further by further action of 5%
aq. NaOH and conc. HC1. A trace of free HC1 in the gas acts as promoter. This is conveniently supplied by an alkyl chloride, e.g., Pr^Cl, which gives C3H G and HC1 (this reaction is reversed a t <[ 200°). A synthetic catalyst (II) from pptd. S i0 2,xH.,0 and A12(S 04)3 has approx. 20 times the activity of (I) (polymerisation) and
•similar properties, but is a poor catalyst for addition of
11C1 to C3H6 ; replacement of A1 by Fe or Mg does not give a catalyst. Both (I) and (II) are readily poisoned by alkalis, 0 2, and much H 20 , but not by S ; (I) is improved by a trace of H 20 , but (TI) is poisoned. Active A120 3,0-2II20 from Na aluminate and deficit of acid or from A l-Hg is an excellent catalyst for combination of C3I I 6 and HC1; Fe20 3 on S i0 2 has also some activity.
H. A. P . ' D irect sulphonation of natural substances con
taining higher alcoh ols. M. Ga l l o t t i and A. Moooi (L’Ind. Chimica, 1933, 8 , 1226).—This process may be carried out. by dissolving the oil or wax in dry C2HCl.j and adding ClS0 3II. The reaction product is cooled with ice and treated with milk-of-CaO. After removing the solvent, the aq. solution of the Ca salt is treated with Na2C03. In this way spermaceti yields Na cetylsul- phonate, with, in the ppt., Ca palmitate, from which fairly pure palmitic acid is isolated. The sulphonated products obtained by this method have similar proper
ties to those derived from the pure alcohols. E. W. \Y.
E xtraction of phenols from caustic [soda] so lu tions. II. E. B. Ke s t f.r (Ind. Eng. Chem., 1933, 25, 1148—1150; cf. B., 1932, 1113).—The extraction of PhOH, o-, m-, and y-cresols, 1 : 3 : 2 - and 1 : 3 : 5 - C6H3Sle2'OH, thymol, and guaiacol from 2-5Ar-aq.
solutions of their Na derivatives indicates th a t the rate of extraction is increased by dilution, rise of temp., and increase of vol. of solvent. P r820 is inferior to E t20 for a given temp, on a vol. basis, but almost equal on a mol. basis, b u t a t its b.p. is comparable (vol.) with E t2G a t its b.p. The method is applicable to the ta r acids from high- and low-temp. carbonisation of coal, and could probably be used in fractionation. Use of by-product alcohols, b.p. 133—147°, from MeOIl synthesis fails as they extract the phenoxides and not
the free phenols. H. A. P.
Friedel Crafts reaction. Effect of size of a lu m inium chloride p articles in preparation of keto- acids. P. II. Gr o g g i n s and R. H. Na g e l (Ind. Eng.
Chem., 1933,25,1083—1085).—W ith good agitation the size of A1C13 particles used in the prep, of 4'-chloro-o- benzoylbenzoic acid (I) is immaterial up to the size of a pea, but beyond this they tend to become coated with an impervious layer of AlCl3-keto-aeid complex which prevents complete reaction of the A1C13. In a ball mill, as would be expected, particle size is of no account.
Yields of the order of 90—93% are obtained, the losses being incurred during isolation. The solubility of (I) in IlgO a t 20—100° is determined. H. A. P.
A u toxid ation of tetralin. L. Pi a t t i(Angew. Chem., 1933, 46, 638—639).—Repeated heating (to 160°) and cooling of tetralin (I) in a current of air for 14 days, under conditions such th a t compounds of low b.p. are not lost, causes increases of d (about 8%), 75 (14%), and b.p. (27°). The oxidised (I) is dark yellow and contains acids of high b.p. which attack Fe and Cu. II. F. G.
CHAcMe-OIl and A c2 in pyroligneous a c id .-- See II. E sters of laevulic acid and su cro se.—See XVII.
Pa t e n t s.
H ydrogenation of hydrocarbons. W. S. Ca l c o t t,
A. S. Ca r t e r, and F. B. Do w n i n g, Assrs. to E. I. Du
B r i ti s h C h e m ic a l A b s t r a c t s— B .
im Cl. I I I . — O r g a n i c I n t e r m e d i a t e s .
Po n t d e Ne m o u r s & Co. (U.S.P. 1,903,501, 11.4.33.
Appl., 24.3.30).—Polymerisable, non-benzenoid polymer- ides of C2H2, e.g., CH^CH-C-CH, (CH2:CH-C:)2, C8H 8, and their polymerides, are partly or completely hydro
genated by standard methods. H. A. P .
Manufacture of products [derivatives of higher hydrocarbons] containing nitrogen. I. G. Fa r b- e n i n d. A.-G., and A. Ca r p m a e l (B.P. 398,510, 14.3.32.
Addn. to B.P. 339,962; B., 1931, 195).—Halogen- containing bases of the prior patent are heated a t 200—
300° in presence or absence of C u catalyst, an acid- binding agent, and/or a diluent, at <£ 1 atm . The unsaturated bases so obtained are wetting agents etc., and improve the fastness of direct dyeings to hot H ,0
and acid. C. H
M anufacture of acetic acid. S . R . Me r l e y and 0 . Sp r i n g, Assrs. to Do h e r t y Re s e a r c h Co. (U.S.P.
1,904,160, 18.4.33. Appl., 31.1.31).—C2H 4 and S 0 3 arc made to interact a t 95—115° in a tower, and the carbyl sulphate (I) formed is hydrolysed w ith H 20 ; the solution is neutralised with NaOH, some N a2S 0 4 separated by cooling, and the resulting 0H -C H 2'CH2'S 0 3Na heated with some Ca(OH)2 and excess NaOH a t 150°. NaOAc thus formed is acidified [with hydrolysed (I) liquors]
and fractionally distilled. An apparatus is claimed.
H. A. P.
Preservation of eth yl ether. H. L. Cox and P. S.
Gr e e r, Assrs. to Ca r b i d e & Ca r b o n Ch e m i c a l s Co r p.
(U.S.P. 1,903,642, 11.4.33. Appl., 26.2.32).—Presence of Cr, Ni, or an Fe-C r-N i alloy (7 4 :1 8 :8 ) prevents deterioration of E t20 in closed containers. H. A. P.
Manufacture of [aliphatic] a m in es. Ro h m &
Ha a s Co. (B.P. 399,201, 30.3.32. U.S., 2.4.31).—An alcohol vapour is led with NH 3 or a primary or sec.
amine over a catalyst containing P, e.g., a phosphoric acid, P 20 6, an N H 4 or At phosphate, preferably on a carrier, a t 300—400°. The prep, of N H 2Me, NPhMe2, NHMcj, and NMe3, P r and Bu amines, is described.
C. H.
Production of ethanolam ines. E. W . Re i d and 1). C . Le w i s, Assrs. to Ca r b i d e & Ca r b o n Ch e m i c a l s Co r p. (U.S.P. 1,904,013, 18.4.33. Appl., 18.8.27).—An apparatus is claimed in which C2H 40 (? 1-5—2-4 equiv.) is passed through porous tubes into aq. NH3 which is continuously circulated through a heat exchanger in order to m aintain a temp, of 0— 100°
(40—50°). Excess of NH3 and H 20 are then, distilled, leaving N ^ IL 'C H j/O H ^ [containing 25—35% of
NH(CH2-CH2-0H )2]. H. A. P.
Preparation of ethylidene chloride. G. H. Co l e m a n, Assr. to Dow Ch e m. Co. (U.S.P. 1,900,276, 7.3.33.
Appl., 27.7.28).--An equimol. mixture of CH2!CHC1 and HC1 (from thermal decomp, of C2H 4C12) is passed over A1C13 a t 25—150° (125°). A 20—40% conversion into ClIMeCl, containing little or 110 CH2C1-CH2C1 is
obtained. H. A. P.
Preparation of chlorohydrins. L. W. Cook, Assr.
t o Te x a s Co. (U.S.P. 1,904,677,18.4.33. Appl., 25.9.28).
—Liquid defines th a t give I I 20-insol. chlorohydrins (octylene) are treated with <£ 0 -7 5 % aq. HOC1 (from NallCOg and Cl2), which when exhausted is removed from contact with the olefine, regenerated in a separ
ate vessel, and returned to the process, this being repeated until chlorohydrin formation is complete.
Formation of dichloride is thus avoided. H. A. P.
M anufacture of m aleic acid. J . W . Li v i n g s t o n,
Assr. to Mo n s a n t o Ch e m. Wo r k s (U.S.P. 1,901,914, 21.3.33. Appl., 8.5.31).—Aq. maleic acid is distilled under the lowest pressures compatible w ith a fluid state (at one stage solid separates and the temp., and therefore the pressure, has to be raised for a while). Maleic anhy
dride distils with the final fraction. H. A. P.
P urification of crude m aleic acid. H. W . Wi t z e l,
Assr. to Se l d e n Co. (U.S.P. 1,900,680, 7.3.33. Appl., 21.7. 31).—Fe and coloured impurities are removed from the crude acid by pptn. with a cyanide or ferrocyanide
in aq. solution. H. A. P.
Purification of crude dicarboxylic acid s. A. O.
Ja e g e r, Assr. to Se l d e n Co. ( U . S . P . 1,900,649, 7.3.33.
Appl., 20.7.31).—Crude polycarboxylic acids (maleic acid) are crystallised from an ester of the acid, hydrogen
ated polymiclear hydrocarbon (tetralin), or a mixture of the two, w ith addition of a non-solvent (C8H6, PhMe)
if desired. H. A. P.
Preparation of fatty acid s. R. T. Ha s l a m, A s s r . t o St a n d a r d Oi l De v e l o p m e n t C o . ( U . S . P . 1,904,452, 18.4.33. Appl., 14.8.30).—Hydrocarbon oils containing solid paraffins (petroleum) are hydrogenated (350— 440°/
200 atm .), whereby the solid content is increased, and then oxidised by air-blowing in the normal way (190°/1 atm.). The paraffin wax is preferentially oxidised.
H. A. P.
R ecovery of oil-solu b le sulphonic com pounds form ed in acid-refining of m ineral o ils. G. Vo o g t,
Assr. to Sh e l l De v e l o p m e n t Co. (U.S.P. 1,901,383, 14.3.33. Appl., 25.3.31. Ger., 31.3.30).—The lower layer of the alkaline alcoholic extract from the acid- refining process is salted out (NaCl) and the pptd. soaps are purified by dissolution in 96% EtOH, and filtration and evaporation of the solution. H. A. P.
Production and d istillation of aqueous sulphuric acid solutions of se c .- and teri.-a lco h o ls. B. T.
Br o o k s, Assr. to St a n d a r d Al c o h o l Co. (U.S.P.
1,904,200, 18.4.33. Appl., 30.6.31).—The solutions of alkyl sulphates, e.g., from cracked hydrocarbon gases and H 2S 0 4, are first hydrolysed if necessary by heating from 50° to the b.p. of the alcohol in a vessel of vitreous material (e.g., glass, glazed earthenware), and then passed downwards through a stripping column, also of vitreous material, in countercurrent to steam. The use of vitreous instead of metal equipment is claimed to prevent
dehydration to defines. H. A. P.
D irect m anufacture of ketones from im pure volatile acid s. J. G. Ma u g e r, Assr. to Ma is o n Ca m u s- Du c h e m i n So c. Anon. (U.S.P. 1,904,495,1S.4.33. Appl..
10.5.30. Fr., 13.5.29).—The acid, e.g., crude pyrdigne- ous acid, is freed from tarry m atters and catalyst poisons by passage over active (wood-)charcoal a t 425° before contact w ith the ketone catalyst. The charcoal is regenerated by heating a t 500—550° in a stream of air
or other gas. H. A. P.
Reduction of furfural [furfurylidene]acetone and furan d erivatives. F. N. Pe t e r s, JU N ., A s s r . t o
