BRITISH CHEMICAL ABSTRACTS
B.—A P P L IE D C H EM ISTRY
MAR. 31 and APRIL 7, 1933*
I.— GENERAL; PLANT; MACHINERY.
Interference m ethod of m easuring therm al exp an sion . G. E. Me r r i t t (Bur. Stand. J. Res., 1933, 10, 59—76).—The apparatus and technique are de
scribed. H. J . E.
P o st-w a r d evelopm ents in h igh-pressure boilers.
C. H . Da v y a n d C. H . Sp a r k s(J. Inst. Fuel, 1 9 3 3 , 6 , 16G
—207).
T unnel d ryers.—See V III. Fine-grinding of la c q uers.—Sec X III. Lafeuille rotary crysta llise rs.—
See XVII.
Pa t e n t s.
Furnaces of the m uffle typ e. A. Sm a l lw o o d and J . Fa l l o n(B.P. 387,060,10.11.31).—Tubular combustion chambers are arranged in the form of rectangular frames the joints of which are held together by gravity. The frames are arranged abreast in the work chamber.
B. M. V.
H eat exchanger. G. T. Ja c oc k s and J. L. Kr ik g, Assrs. to Alco Pr o d u c t s, Inc. (U.S.P. 1,S55,552, 26.4.32.
Appl., 20.4.31).—A method of descaling an exchanger of the bundle-of-tubes type is described. B. M. V.
D ry in g of g la ss-m eltin g pots and other articles m ade from plastic m aterial. IIe r z o g e n r a t iik r Gl a s w e r k e Bic h e r o u x & Co., G.m.b.H. (B.P. 386,819, 10.3.32. Ger., 12.3.31).—The drying chamber has walls th a t are slightly permeable to moisture and the atm.
is subjected to definite rises of temp, a t definite intervals ; the R.H . also is kept const, during the first period and lowered slightly a t each subsequent period, until shrink
age has been completed. The temp, of the articles will remain approx. const, during all those periods on account of evaporation. Subsequently the temp, is raised quite rapidly. In an apparatus described, the material is loaded on trucks and conveyed to separate chambers for each period ; definite jets of air (withdrawn from the same chamber) m ay be directed on the insides of pots and other places not easily accessible to convection.
B. M. V.
A pparatus for drying tea or other vegetable, an im al, or m ineral su b stan ces. J. R . Fa r b r id g e
(B.P. 386,646, 9.6.31. Ceylon, 16.8.30).—The tea (etc.) is conveyed in a zig-zag course upon slat conveyors, any fine tea th a t falls through the conveyors being picked up by the forced draught and delivered into side com
partm ents opposite the entry for air, whence it can be removed before i t has become too dry. B. M. V.
H eat-in su latin g coverings. F. W. R. P i l t o n and W. H . L a n e ( B .P . 386,774, 14.12.31).—Comminuted insulating material, e.g., granulated cork, is placed in a tube of canvas, linen, etc. and, after treatm ent with
plastic bituminous or resinous substance, is used as a
rope binding. B. M. V.
R efrigerant. L. K. Wr ig h t (U.S.P. 1,855,659, 26.4.32. Appl., 4.10.27).—The use of trimethylene is
claimed. L. A. C.
E lim ination of tartar in boilers, gen erators, piping, etc. and product therefor. F. Le c o m t e
(B.P. 386,865, 6.6.32. Fr., 5.6.31).—Claim is made for a solution of HC1, CuS04, eucalyptus oil, and vegetable blue decrusting material, preferably used hot. The last-mentioned constituent may consist of indigo and Ba(C103)2. The solution (prep, described) can usefully be applied in the cleaning of fermentation vats.
B. M. V.
P lan etary ball m ills. In t e r n a t. Co m b u s t io n, Lt d., Assees. of J. Cr i t e s (B.P. 386,730, 9.10.31. U.S., 9.10.30).—The mill has a single, fixed, outer grinding ring and the single or double rotating inner ring is spring- m ounted so as to force i t in contact with the balls, the springs taking no p art of the driving strain. The m aterial scoops, rotating w ith the inner rings, are arranged to deliver p a rt of the material back to the grinding zone and p a rt through apertures in the rings into the air current above. B. M . V.
M ixing m achine. T. E. Fo r s t e r (U.S.P. 1,855,548, 26.4.32. Appl., 22.5.31).—The apparatus comprises a conical spreader rotating a t comparatively low speed above an inverted conical sprayer of smaller diam. and rotating a t centrifugal speed. B. M. V.
Continuous filters. Ol i v e r Un i t e d Fi l t e r s, In c. (B.P. 387,044, 13,10.31. U .S ., 13.10.30).—I n a d r u m o r d is c f ilte r, in f la ta b le t u b e s o f s o f t m a t e r i a l a r e u s e d a s d iv is io n s b e tw e e n t h e v a r io u s s e c tio n s ; t h e t u b e s a r e l e f t d e f la te d t h r o u g h o u t t h e c a k e - f o r m in g z o n e so t h a t n o d iv is io n s o r e v e n w a t e r m a r k s a r e f o r m e d i n t h e c a k e , w h ic h is t h e n s u i t a b l e f o r r e m o v a l a s a c o n tin u o u s s h e e t of, e.g., w a llb o a r d . I n t h e w a s h in g , d r y in g , a n d d is e n g a g in g z o n e s t h e s t r i p s a r e in f la te d t o p r e v e n t p r e s s u r e flu id r e a c h in g t h e v a c . z o n e s . B. M. V.
F ilterin g sy ste m and filter tank. W. J. Ca n d l is h
and W . T. Mo r g a n, Assrs. to In t e r s t a t e Co-p a r t n e r s h i pAssoc. (U.S.P. 1,855,280, 26.4.32. Appl., 16.9.29).
—A cylindro-conical tank is provided with a filter membrane over practically the whole of the interior walls and spaced from them. All pipe connexions are formed in one casting attached to the apex of the cone, the connexions b e in g : (a) and (6) suction and back-flow from and to the annular space between the filter and wall of the tank, (c) from the annular space to the similar space of the next ta n k either way of a series—
this may be “ teed ” off from (a), (d) upturned pipe
a
* T h e re m a in d e r of th is s e t of A b s tr a c ts w ill a p p e a r in n e x t w eek ’s issu e . 255
B r it is h C h em ica l A b s t r a c t s —B.
2 ö ü Cl. I I . — F ii b l; Ga s; Ta r ; Mi n e r a l Oi l s.
into the pulp space for filling and/or agitation, (e) large aperture directly downwards for discharge of thickened
pulp or cake. B. M. V.
Centrifugal treatm ent of liq u id s. Ak t i e b. Se p a r a t o r (B.P. 387,298, 20.10.32. Swed., 11.11.31).—
Forms of outlet for the continuous discharge of solid m atter are described. Auxiliary liquid is adm itted in excess to au annular space between two bowl-walls each having alined outlet jets, the excess liquid being discharged over a weir a t a radius > th a t for the lighter liquid. The apertures for discharge of slime are pref
erably smaller in the inner than in the outer bowl.
B. M. V.
E vaporators. K . Vy k l u p il (B.P. 3 8 7 ,2 4 1 , 1 8 .7 .3 2 ).
—A calandria is formed of double-concentric tubes, the steam being adm itted to the inner tubes and the liquor on its first pass to the annular sp aces; the separating chamber for the first pass is somewhat elevated and the liquor is passed out through a float-operated valve into the shell surrounding the bundle of tubes, where i t is again evaporated by heat transm itted through the liquor of the first pass. B. M. V .
G as filters. A. Wi l k in s o n and A. T. El l is (B.P.
387,006, 29.7.31).—A filter for insertion in a gas main is described ; two stages of straining are employed and a space is provided for the settlem ent of coarse material.
B. M. V.
C atalytic treatm ent of organ ic and inorganic su b stan ces. W. T. R. Bi n d l e y ( B .P . 386,982,18.4.31).
—The catalyst and a suitable adhesive medium, e.g., metallic oxides and Si ester, is painted on supporting surfaces which preferably are in the form of nested cones.
The apparatus m ay be used for the hydrogenation of coal suspended in oil and of mineral or edible oils.
B. M. V.
A scertain in g the m o istu re content of a m aterial or su b stan ce. S . and J . St a n w o r t ii (B.P. 386,767, 8,12.31).—A closed vessel in which the pressure of gas generated by the action of H 20 on, e.g., CaC2 is measured is provided with a filter between the m aterial com part
m ent and gauge, and w ith a safety valve. B. M, V.
M anufacture of friction m a teria l. A. L. Moot.
From Ra y b e s t o s Co. (B.P. 387,124, 1.2.32).—In a material comprising an asbestos base saturated with oxidisable binder which is liable to form an impermeable skin and prevent the complete curing of thick material, a no. of holes arc pierced after drying (but before curing) so th a t no part of the m aterial is in. from a vent or the external surface. B. M. V.
F riction m a teria ls. Soc. An o n. Fr a n? , d u Fe r o d o (B.P. 386,718, 19.9.31. F r . , 3.10.30).—Claim is made for compositions, not bound by rubber, contain
ing PbO which remains as such in the finished material.
Other ingredients are, e.g., resin, pitch, asbestos, and
graphite. B. M. V.
T em p , control in k iln s.— See V III. P p tn . of particles from g a se s.—See X I.
II.— FU EL; G A S ; T A R ; MINERAL OILS.
T en d en cy of coal to spontaneous ign ition . X.
D. J. W. Kr e u l e n [with P. v a n d e r Gr a a f f] (Chem.
Weekblad, 1933, 30, 103—10S; cf. B., 1933, 4).—A
3-dimensional model showing the relation between
“ volatile C ” content, tem p., and humic acid production is described and discussed. D ata given previously relating to 34 different types of coal are tabulated, with, in addition, the heats of combustion and activity a t 600° of the coke formed a t 900—950°, as indicated by the q u an tity of C 02 fonned per sq. cm. of surface in 5 min. in an air stream of 20 litres per hr. The factor hh0/T m ! where h and h0 are the quantities of humic acid produced a t 240° and respectively, serves as a guide to the ease of coking of a coal ; for almost all coals which undergo coking i t falls between the limits 3-4 and 32, irrespective of the volatile content of the
coal. H. F. G.
R eactivity of coal ; the “ perm anganate n u m b e r .” F. He a t h c o a t (Fuel, 1933, 12, 4— 9).—Five coals were heated with alkaline K M n04 a t 100° under standard conditions and the excess K M n04 was deter
mined after various intervals of time. After a prelim
inary period rapid oxidation occurred a t a rate which was greater the lower the rank of the coal. Ultim ately a const, to tal am ount of oxidation was reached with each coal ; these vais., however, could only be correlated roughly with the rank of the coal. The method of determining the “ permanganate no.” described pre
viously (B., 1932, 630) has been modified in th a t the coal (60/120-mesh) is first extracted with C5H SN, fines < 120- mesh are then removed, a wetting agent (10 c.c. of a 1%
solution of “ perminol ” ) is added to the dry coal before treatm ent w ith the oxidising solution, and the results are expressed in term s of vol. of A7-K M n04 used up. The perm anganate no. affords a rapid method of gauging the rank of a coal. The decomp. temp, of a coal can be determined by heating samples of the coal to success
ively higher temp, in vacuo and plotting perm anganate no. of the preheated coal against temp, of heating ; a sharp change occurs in the direction of the curve a t the decomp. temp. The perm anganate nos. of the vitrain and durain from the same coal differed consider
ably although the oxidisabilities before extraction w ith CglljN were very close. A. B. M.
O xidation of coal. R eaction of stea m w ith incandescent coke. M. Do l c h and J . Ko l l w it z
(Braunkohle, 1932, 31, 607—610, 628—632, 645—649;
Cliem. Zentr., 1932, ii, 2129).— In the interaction of steam and incandescent coke, the nature of the gaseous products depends on the time of contact as well as on the kind of coal concerned. Coke from bitum in
ous coal reacts chiefly thus : C + H aO = CO -f- U 2, whilst th a t from brown coal reacts chiefly thus : C -f- 2H 20 — C 0 2 -f 2H a. W ith coke from coal of interm ediate type, the effects are superposed. The gaseous products depend on the oxidisability of the coal
a t room tem p. A. A. E.
M odern m eth od s of low -tem p eratu re carbon
isa tio n and the preparation of artificial anthracite.
C. Be r t h e l o t (Chim. et Ind., 1933, 29, 18—44).—The principles underlying low-temp. carbonisation are dis
cussed and a no. of typical carbonisation plants are
described. A . B . M.
C arbonisation w ith 103-in. vertical retorts.
F. A. Rh e a d (Gas J., 1933,201, 316—318).—The retorts
B r it is h C h em ica l A b s t r a c t s B.
Cl. I I . — Fu e l; Ga s; Ta b; Mi n e r a l Oi l s. 2 5 7
are heated by external producers using high proportions of breeze (l-in. m esh ); with 50, 70, and 80% of breeze, the am ount of fuel needed was 15-6, 15-83, and 13-9 wt.-% of the coal carbonised. There are no recuperators or regenerators in the setting. The retorts are left out for scurfing for 48 hr. every 23 days, the flues being cleaned every second scurfing period. During this period, the combustion flues are p u t under a pressure or v a c .; the burning of producer gas in the retorts or the presence of air in the flues will indicate leaks if present in the reto rt walls, which are then patched by spraying.
Working results for 6 months, using a coal containing 7 • 1% of inerts and 35-5% of volatile m atter a t a daily throughput of 8-98 tons with 13-45% steaming, gave 83-56 therm s/ton of coal, the gas having a calorific val. of 471 B.Th.U./cu. f t . ; coke and breeze for sale was 10-2 cw t./ton of coal. The ta r (5-1% moisture) and liquor (7 -25-oz. concns.) yields were 17-4 and 30-3 gals.,
respectively. R. N. B.
N ew view s on the coking process of bitum inous coals. G. La m b r is (Gas- u. Wasserfach, 1933, 76, 1—3 ; cf. B., 1931, 660).—Slight oxidation of a bitum inous coal reduces its expansive pressure to zero without appreciably affecting its swelling or caking pow ers; the latter properties are lost in succession on further oxida
tion. Similar effects are produced by heating the coal with S, or metallic oxides or sulphides. Loss of expan
sive pressure is also brought about by heating the coal with caustic alkalis or H3B 0 3. Addition of 0-5% of H3BO3 reduced the expansive pressure of a “ fat ”, coal to zero. Addition of < 2% also reduced the yield of lo w-temp. ta r from the coal from 5% of a brownish-black viscous tai- to 3-25% of a yellowish-brown, mobile tar, lower in phenols and benzine-insol. constituents.
Addition of H3B 0 3 had no effect on the softening point, but diminished the plasticity of the coal. I t is concluded th a t H 3B 0 3 forms a complex with some of the coal constituents, probably by attachm ent to the OH groups.
H„BO, had no effect on the yield of ta r from a dull coal.
3 A .B .M .
A ctive carbon and its industrial applications.
A. Godel (Chem. et. Ind., 1933, 29, 3—17).—A resume, is given of the properties, manufacture, and applications
of active C. A. B. M.
W ater-gas production in the coke oven. G.
Lo r e nzen (Stahl u. Eisen, 1933,53,33—40).—Water-gas m ay be produced advantageously in the coke oven to increase the yield of gas and its II 2 content and to control its calorific val. Various devices for the introduction of steam into the almost completely coked oven charge are described. In a satisfactory method (Otto process) steam is injected from a jet directed away from the ascension pipe and fixed in the cover of the charging hole nearest this pipe. Temp, measurements distri
buted over the whole oven indicate the uniform flow of steam over the greater part of the coke and absence of excessive cooling of the oven walls. The calorific val. of the gas may be further controlled by spraying ta r oils into the oven with the steam. I t is shown th a t increased yields of satisfactory gas m ay be obtained by this process w ithout increased throughput of coal in the
oven. II. E. B.
D eterm ination of hydrocyanic acid in coke-oven and sim ila r g a se s. W. K le jip t and W. R iese (Brennstoff-Chem., 1933, 14, 21—25).—In Drehschmidt and Feld’s method up to 30% of the HCN absorbed by the F e (0 H )2 suspension may be converted into thio- cyanate, which is not reconverted into HCN in the subsequent distillation and p art of which m ay be com
pletely lost by volatilisation as IICNS. The formation of thiocyanate is attributed to the presence of 0 2 in the gas which liberates S by oxidising the FeS formed from the H 2S in the gas, the S then combining with the HCN. Accurate results were obtained by this method when the gas contained < 0-5% 0 2. F urther study of Gluud and K lem pt’s method (cf. Gluud, “ Handbuch dor Kokerei,” 11,85; Voituret, B., 1932, 824) has shown th a t boiling with tartaric acid does n o t completely decompose the thiosulphate in the solution. The method has therefore been modified. The solution is boiled to remove N II3 and I12S, filtered, an aliquot p a rt of the filtrate is acidified with H 2S 0 4 or H N 0 3 (3 c.c. of 5V-acid to 100 c.c.), the solution is boiled gently for 15—20 min., and after being cooled its thiocyanate content is deter
mined by titratio n w ith 0-lA r-AgN03 in the usual m an
ner. The error due to the formation of thiocyanate by interaction of the CS2 in the gas with the N H 4 poly- sulphide in the solution is negligible. A. B. M.
D eterm ination o f the nitric oxid e in coke-oven g a s. H. Tr a.mm and W. Gr im m e (Brennstoff-Chem., 1933, 14, 25—29).—The curve given by Schuftan (B., 1932, 488) to correct for the incomplete conversion of NO into N 0 2 when using his method of determination is considerably in error and a revised curve is given.
Other sources of error are discussed and the following improved procedure is suggested. A measured vol. of the gas is mixed with an equal vol. of 0 2 and the N 0 2 formed is absorbed in aq. NaOH ; the vessel is shaken a t frequent intervals and sufficient time of contact is given, e.g., 3 days, to ensure complete conversion of the NO into N 0 2 ; the n itrite formed is determined color- imetrically with Lunge and Ilosvay’s reagent (sulphanilic acid-a-C10H7‘N H 2). The method has been applied to determine the distribution of the NO in the fractions of a coke-oven gas separated by the Concordia-Linde-Bronn
low-temp. process. A. B. M.
O xidation of m ethane by m etallic o x id es. B.
Ne u m a n nand II. Wa n g (Angew. Chem., 1933, 46, 57—
61).—CuO and CII4 begin to react a t 350°, and a t 725°
C02 and H 20 are formed quantitatively. Fe20 3 is completely reduced to Fe30 4 a t 680°, with production of C 02 and H 20 . Fe30 4 a t 720° oxidises only about 40% of the CH4 present, and of this quantity 66% of the H appears as H 20 , 28% of the C as C 02, and 7% of the C as CO ; part of the 0 is liberated in the free state.
FeO and CH4 begin to react a t about 750°; a t 880°
70% of the gas is oxidised : 62% to C 02 and H 20 and 8% to CO and H 2. S n 0 2 does not react below 800°, i.e., until an appreciable fraction of the CH4 is dis
sociated ; a t 972° the reaction is 73% complete, C 02 and H 20 being the main products. ZnO begins to react a t 800°, but even a t 1000° only 50% oxidation occurs, and the products are CO and H 2, with traces of C. Impure CH4 m ay be completely freed from H 2 by
a 2
B r i t i s h C h em ica l A b s t r a c t s —B .
2 5 8 Cl. I I . — Fu e l; Ga s; Ta r; Mi n e r a l Oi l s.
passage over C11O a t 250° or over M n02 a t 175° ; traces only of C 02 are formed a t these tem p. H. F. G.
B eneficial effect of oxid ation on the lubricating properties of o il. R. 0 . Kin g (Proc. R oy. Soc., 1933, A, 139, 447—459).—Experiments carried out under conditions promoting oxidation of the lubricant and a t const, speed and load show th a t boundary conditions in journal-bearing lubrication are not, as is generally assumed, “ hypothetical.” Effective lubrication with very low friction, depending on such conditions, can prevail a t temp, greatly above those possible when lubrication depends on a fluid film of oil m aintained by the relative motion of the surfaces. W ith mineral oils the boundary conditions required for effective lubrica
tion are induced by oxidation. I t is suggested th a t the active (polar) mols. formed during the early stage of oxidation build up to an appreciable thickness on the adsorbed layer, and the friction observed is th a t on the surface of the built-up layer ; the surface diminishes in rigidity in the direction of motion as the thickness of the boundary layer increases, and friction approaches zero as a surface of complete slip tends to be reached.
L. L. B.
H ydrogenation of cresols etc.—See I II. S i 0 2 coke-oven brick. G raphite as refractory.—See VIII.
Pa t e n t s.
W ater-gas producer for com p lete gasification of fu els. B. Sp i t z e r (B.P. 386,195, 2.5.32).—F or bitum in
ous fuels, especially caking and swelling coals, the producer is so designed th a t the fresh fuel is distributed Upon the glowing and carbonised fuel bed as a shallow layer (20—80 cm. in depth) the surface of which is raked over during the operation by a rotary rake. During the blow the gases leave the producer through slots in the walls situated ju st below the fresh fuel la y e r; during the run the gases pass through tliis layer and carbonise it. On the rotary grate is a central extension which projects into the fuel bed and prevents the formation of a core therein. Carburetting agents m ay be introduced with the superheated steam or other gasifying agent or
heat carrier used. A. B. M.
D ryin g of fuel g a se s. J . W. Na p i e r, and Ne w t o n, Ch a m b e r s & Co., Lt d. (B.P. 385,908, 26.8.32).—The gases are passed horizontally through a washer con
sisting of a series of vertical washing chambers having louvred walls which perm it the passage of the gases and a t the same time support the contact m aterial with which the chambers are filled. A hygroscopic liquid, e.g., aq. CaCl2, is supplied to the top of each chamber, and after passing down over the contact m aterial, collects in a reservoir provided w ith cooling coils. The reservoirs are separated by intercalating troughs into which the liquid passes from the reservoirs on either side, and from which it is pumped to the top of the following washing chamber. The plant includes a stock tank, also provided w ith cooling coils, and an evaporator for reconcent rating the solution. A. B. M.
Gas ca lo rim etry . El l io t t B ros. (Lo n d o n), Lt d., and L . G. Sa lm o n (B.P. 385,712, 13.11.31).—Electrical resistance thermometers for recording the temp, of the H 20 current a t the inlet and outlet, respectively, of a
gas calorimeter form two arms of a W heatstone bridge, the out-of-balance current of which indicates the differ
ence in temp, between the two thermometers and operates an instrum ent for recording the calorific val.
of the gas. Another resistance therm om eter in the I I 20 inlet is connected to a second W heatstone bridge, the out-of-balance of which is used to correct the reading of the instrum ent for variations in the inlct-ILO tem p.
A. B. M.
G as-an alysin g apparatus. A. Ha w k y a r d (B.P.
385,765, 28.1.32).—The apparatus comprises a container (A) for measuring a predetermined quantity of the gas to be analysed, a chamber containing an absorbent (B) for one of the constituents of the gas, a receiver (C) for the residual gas after absorption, pressure gauges (D ), etc. A pum p acts during its pressure stroke to drive the measured vol. of gas from A, through B, into C, and during its suction stroke to discharge C. The reduction in pressure due to absorption is measured.
A device for protecting D from cyclic pressure fluctua
tions is provided. A. B. M.
T ar-d istillation and lik e s t ills . 0. L., C. H., and C. II. L. Benn (B.P. 385,754, 16.1.32).—A method of forming corrugations in dome-shaped still bottoms, in order to give them additional strength and heating
surface, is described. A. B. M.
D istilla tio n of tar o il. 11. Wo l f (B.P. 385,904, 19.8.32. Ger., 19.8.31. Addn. to B.P. 297,829).—Tar is heated under pressure and then allowed to expand through a valve, such as th a t described in the prior patent, into a condensing apparatus wherein the heated products are fractionated. A medium oil is fed into the chamber surrounding the valve so as to mix with the heated products and thus protect the valve apparatus
against incrustation. A. B. M.
T reatm en t of hydrocarbon g a se s. An g l o-Pe r s u n Oil Co., Lt d., A . E. Du n s t a n, and E. N. Ha g u e (B.P.
385,981, 9.4.31).—-Residual gases from oil-cracking stills or other hydrocarbon gases are subm itted to therm al treatm ent in two stages, in the first of which the paraffins are converted into olefines, e.g., a t 650—800°/atm., and in the second the olefines are polymerised and condensed, e.g., a t 350—550° under pressures of 200—
2000 lb./sq. in. To minimise the production of C the apparatus is constructed of or lined with Cu, A l, or stainless steel, etc. The first stages m ay be effected a t higher tem p., e.g., 800— 1050°, whereby arom atic hydro
carbons as well as olefines are produced. The products form anti-knock fuels suitable for internal-combustion
engines. A . B. II.
R em oval of undesired low -b oilin g com ponents from naphtha b y fractional d istilla tio n . St a n d a r d Oi l De v e l o p m e n t Co., Assees. of J . R . Sc h o n b e r g and W. E. Ro b in s o n ( B .P . 386,075, 9.11.31. U .S ., 10.11.30).
—The hot product from a hydrocarbon oil heating and/or cracking zone is passed into the lower half of a fraction
ating zone wherein heavy oils are separated as liquid and crude naphtha as vapour. The naphtha vapours are passed into a second fractionating zone (4 ) from which a liquid fraction is withdrawn containing relatively high-boiling co n stitu en ts; the light ends are stripped
B r it is h C h em ica l A b s t r a c t s —B .
Cl. I I I . — Or g a n i c In t e r m e d i a t e s. 259
from this liquid fraction and returned to A . The vapours withdrawn from the latter are fractionally condensed, under increased pressure if desired, to form a stabilised light naphtha fraction. A. B. M.
T reatm ent of hydrocarbon o ils [to separate acid slu d ge]. D. D. St a r k, Assr. to Ass o c ia t e d
O il Co. (U.S.P. 1,856,141, 3.5.32. Appl., 22.9.28).—
The sludge obtained by treating the oil with 1I2S 0 4 is separated by passing the liquid through vertical porous plates, e.g., of alundum. Periodically the plates are back-flushed with a portion of the filtrate. D. K. M.
T reatm ent [purification] of hydrocarbon o il.
J. A. Shaw (U.S.P. 1,859,262, 17.5.32. Appl., 6.11.28).
—Hydrocarbon oil after treatm ent with H 2S 0 4 and removal of sludge is treated with such quantity of aq.
NaOII containing ta r acids, e.g., PhOH, th a t the aq.
layer is slightly acid. After separation, a further quan
tity of the reagent is added to complete neutralisation and the ta r acids liberated in the first treatm ent are reabsorbed by the aq. liquid. D. K. M.
T reatm ent of petroleum em u lsion s. J . M.
Ev a n s (U.S.P. 1,856,156, 3.5.32. Appl., 19.4.24. Re
newed 24.8.31).—Petroleum -H 20 emulsions arc cut by treatm ent with sulphonated or nitrated derivatives of naphthenes or naphthenic acids, or salts or esters of
such acids. D. K. M.
Coking of heavy petroleum residues or the like and cracking of petroleum vapours. W. W. Tr i g g s. From Br a s s e r t-Tid e w a t e r De v e l o p m e n t Co r p. (B.P.
385,610,22.6.31).—Heavy oils are coked in an oven cham
ber (A) heated from below by horizontal flues. The oils arc sprayed into A together with part of the hot com
bustion gases from the flues, which serve to heat the volatile constituents to the cracking temp. The gases introduced into A m ay contain 0 2 in sufficient quantity to raise the hydrocarbons to the required temp, by effecting partial combustion thereof. The volatile cracked products are withdrawn through an offtake and passed to a condensing system. A. B . M.
[Refining of] insulating o il. J. G. Fo r d, Assr. to We s t in g h o u s f. El e c t r ic & Ma n u f g. Co. (U.S.P.
1,856,700, 3.5.32. Appl., 12.4,28).—The oil is treated with 95—98% H 2S 0 4 (15—50 vol.-%) for £—2 hr., separated, neutralised, washed, and dried. I t is then treated w ith absorbent material (0-5%), e.g., S i0 2 gel, fuller’s earth. The purified oil contains O' 1— 6% of arom atic resinous compounds which act as antioxidising agents. I f these are deficient the oil may be blended, or the product (0-1—5%) obtained by treating turpen
tine with H 2S 0 4, separating, neutralising, and washing
may be added. D. K. M.
R efining of lubricating o il. J . O. St a f f o r d, Assr. to Sin c l a ir Re f i n i n g Co. (U.S.P. 1,856,934, 3.5.32. Appl., 16.6.28).—A non-oxidising, preferably a reducing, gas, e.g., H 2, C 02, N2, tail gas from cracking operations, is bubbled through lubricating oil mixed with fuller’s earth (1— 15%) a t 260—326° for 2—5 min.
D. K. M.
Cracking o f [petroleum ] o il. L. C. H u ff, Assr. to Un iv e r s a l Oi l Pr o d u c t sCo. (U.S.P. 1,839,031,29.12.31.
Appl., 14.4.23. Renewed 1.10.28).
Cracking of o ils. C. P . Du b b s, Assr. to Un iv e r s a l Oi l Pr o d u c t s Co. ( U .S .P . 1,839,017, 29.12.31. Appl., 18.10.20. Renewed 15.8.27).
Catalytic treatm ent [of coal etc.]. Gas filters.—
See I. O xidation of o rg . com pounds.—See III.
O il-sol. d y e s.—Sec IV. A ctivation of alkaline sulphide solu tion s. Crude NH 3 liquor. P urifi
cation of g a se s. P urifying S . Crude I [from oil-field w ater].—See VIL Preservation of w ood.—
See IX . In sulating com p osition s.—See X I. D eter
gent.—See X II. Protecting o il containers. In tag
lio ink.—See X III.
III.— ORGANIC INTERMEDIATES.
C atalysts for sy n th e sis of aliphatic alcohols : characteristics of their action and relations betw een their com p osition and activity. M. St r a d a (Giorn.
Chim. Ind. Appl., 1932, 14, 601—607).—The action of K salts of fa tty acids and of smithsonite impregnated with H C 02K and E tC 0 2K as catalysts in the synthesis of alcohols higher th an MeOH from CO and H 2 is examined. The effects of adding inorg. bases to the catalysts are also recorded. The composition of the mixed products depends on the nature of the fa tty acid salt and, still more, on the % of alkali metal in the catalyst. The higher alcohols are formed by a process of reduction and reconstruction—by the H 2 and CO—
of the fa tty acid salts. After long use, catalysts initially different tend towards equality in composition.
T. H. P.
Sulphonated higher alcohols : new detergents.
D. H. Ki l l e f f e r (Ind. Eng. Chem., 1933,25,138—140).
—An account is given of the reduction of the higher
»-aliphatic acids to the corresponding alcohols by H 2 and a base-metal catalyst a t 300—420°/200 atm . (the process is very sensitive to temp, conditions, which vary somewhat with the nature of the c a ta ly st; a t too high a temp, hydrocarbons are formed). These are converted by H 2S 0 4 and Ac20 , oleum, or C1S03H into alkyl H sulphates which as Na salts have a detergent power superior to th a t of soap and are good dispersing and emulsifying agents. The Na salts are miscible with soap and sol. in soap solutions, and unlike soaps do not become rancid on keeping. Their activity is maintained in acidic and alkaline media, in brine, and in the hardest H 20 , on account of the ready solubility of the H esters themselves and of their Ca and Mg salts. H. A. P.
W axes from the chlorination of naphthalene.
E. E. H a l l s (Ind. Chem., 1933, 9, 58—60).—Chloro- naphthalene waxes have ci15'5 1-5—1-7, m.-p. range 65—130°, and k 4 • 5—5 • 5, according to grade. On oxi
dation HC1 is not split off, b u t on rapid heating the addi
tive C10H 8C14 decomposes into IICl and 1 : 4- C10H 6C12.
Tests show th a t Cu, mild steel, and Cu -}- mild steel in contact do not affect the waxes a t 120—125° in a dry atm . or a t 40—50° in a humid atm ., nor are the metals corroded ; b u t in the presence of H 20 a t 120—
125° Cu is tarnished and HC1 « 0-001%) produced.
The waxes are suitable for electrical insulation pur
poses. D. K. M.
C hloram inę-B . D. N. Po p o v (Khim. Farm . Prom., 1932, 7, 282—283).—P h S 0 2-NClNa,3H20 is a stable
B r it is h C h em ica l A b s t r a c t s — B.
2 0 0 Cl. I I I . — Or g a n i c In t e r m e d i a t e s.
and efficient substitute for chloramine-71; it is recom
mended for the purification of H 20 . Ch. Ab s. H ydrogenation of cresols and dihydric phenols.
C. M. Ca w l e y (Fuel, 1933, 12, 29—35. Cf. B., 1932, 762).—Tlio experiments were carried out in a gas- heated, 2-litre, rotating, mild-steel bomb. At 450° and with an initial H 2 pressure of 100 atm . cresols wore decomposed only to the extent of 6—8% after 2 hrs.’
heating, b u t in presence of a catalyst (charcoal-NH4 molybdatc) they were almost completely reduced to PhMe (40—50%) and methylci/eZohexane (25—35%).
At 500° cleavage of the Me group occurred, both with and without the catalyst. The dihydric phenols were less stable th a n the cresols; a t 450°, with an initial H„
pressure of 100 atm ., and no catalyst, resorcinol was partly, and quinol completely, decomposed to C, pitch and H 20 . The dihydric phenols -were n o t so readily reduced to neutral compounds in the presence of the Mo catalyst as were the monohydric. phenols ; some product was formed which apparently poisoned the catalyst. By the further addition of S, i.e., in the presence of MoSs as catalyst, the dihydric phenols were converted into C6H e (10—20%) and saturated hydrocarbons (40—
50%) mainly naphthenic b u t possibly containing some n-hexane and small am ounts of other neutral
compounds. A. B. M.
C atalytic reduction of arom atic nitro-com - pounds. S. J . Gr e e n (J.S.C.I., 1 933,52,52—56 t).— The catalytic reduction of aromatic N 0 2-compounds is accomplished easily in presence of P t or Pd, b u t only slowly in presence of Ni, unless the H 2 is applied a t an increased pressure. On the other hand, un
saturated esters, which are more difficult to reduce by chemical means than N 0 2-compounds, undergo easy reduction in contact w ith Ni and H 2 a t atm . pressure.
I t is shown th a t this order of reactivity in contact with Ni is completely reversed if N 0 2-compound and unsaturated ester are mixed and hydrogenated. Iu these circumstances, the N 0 2-compound is completely and easily reduced to amine w ith practically no hydro
genation of the oil, this action only starting when the N 0 2-compound has been completely converted.
The unsaturated ester exerts a strong promoting action on the Ni catalyst, comparable with the influence shown by W illstatter to exist in hydrogenations with P t in presence of AcOH. This promoting action is found to be equally strong in the cases of Me oleate and Ble palm itate (carefully freed from unsaturated compounds), so th a t it cannot be associated with the presence of an ethylenic linking, but. rather with th a t of the C 02Me group or the long C chain. The reduction of the mixed nitroxylenes is also investigated, with a view of obtain
ing a selective action, similar to th a t observed by Schroeter (A., 1922, i, 123) in the case of the mixed nitrotetrahydronaphthalenes, which he sharply resolved into 1-nitro- and 2-amino-tetrahydronaphthalenes by simple catalytic reduction. In the case of the nitro
xylenes it is shown th a t th e m-4- and the two o-nitro- xylenes are reduced a t not very different rates, while the symmetrical m-2-nitroxylene is so much more slowly attacked th a t a separation of this isomeride is practicable.
Synthetic cam phor. E . A. Tzo fin and A. T.
R a d u s h k e v i c h (Khim. Farm . Prom., 1932, 50—56, 123— 127).—A review and description of production from turpentine by way of pinene and camphcne.
Ch. Ab s. O xidation o f CH4. U ltra-violet irradiation [of o r g . ch em ica ls].—See X I. Chloroprene p o ly - m e r id e s .— See XIV. B utyric fe rm en ta tio n .—
See X V III.
Pa t e n t s.
M anufacture of halogenated aliphatic hydro
carbons. H. H. Dow, Assr. to Dow Ch e m. Co. (U.S.P.
1,841,279, 12.1.32. Appl... 26.12.28).—C2H 4 and Cl2 are bubbled through heated C2H 4B r2 into the reaction cham ber; combination occurs w ithout explosion risk.
Br m ay also be used as a diluent, whereby C2H 4ClBr is
produced. C. H.
[M anufacture of] chlorinated and brom inated ethinecarbinols [acetylenic alcoh ols]. F. Str au s
and L. R o lle r , Assrs. to W in th ro p Chem. Co., Inc.
(U .S .P . 1,841,768, 19.1.32. Appl., 21.4.30. Ger., 24.11.27).—Acetylenic alcohols, CH:C-CR2-OH, where R = alkyl or CR2 = alicyclvl above C3, are treated with a salt of HOC1 or HOBr, whereby the acetylenic H is replaced by Cl or Br. In the examples, R = E t (Br compound, m.p. 16—18°, b.p. 84— 85°/13—14 mm.), and CRjj = cyciohexyl (Br compound, m.p. 55-5— 56° ; Cl compound, m.p. 51—52°, b.p. 98°/13 mm.). C. H.
M anufacture of p-acetoethyl alcohol [m eth yl fj-hydroxyethyl k eto n e]. I. G. Fa r b e n in d. A.-G.
(B.P. 386,897, 28.7.32, Ger., 13.8.31).—ay-Butylene glycol vapour is led over a dehydrogenating catalyst (Cu on pumice) a t 180—250°/20— 40 mm. C. H.
[M anufacture of] substituted m alon ic e sters.
H. A. Sh o n l e, Assr. to E. Lil l y & Co. ( U .S .P . 1,842,293, 19.1.32. Appl., 2.5.31).—Me, E t, and P r esters of ethyl- and allyl-malonic acids, carrying as second substituent a saturated sec.-alkyl, C5—C7, are prepared, the sec.-alkyl being introduced last. Examples are esters 0 E tR (C 0 2Et)„ and C(C3H 5)R '(C 02Efc),> in which R = CIIMePr" (b.p“. 110— 112 -5°/4 mm.), C H E t2 (b.p. 110—112-5°/4 mm.), cyeZopentyl (b.p. 123—124°/5 mm.), CHMeBu® (b.p. 120— 128°/5-5 nun.), sec.-C7H , 5 (b.p. 127— 133°/10 m m .); R ' = CIIMePr11 (b.p. 95°, J.
mm.). E t allylinalonate has b.p. 114—118°/17 mm.
C .H . Preparation of hydrated citric acid. C. Pf i z e r
& Co. (B.P. 386,705, 19.8.31. U.S., 15.7.31. Addn. to B.P. 380,813 ; B., 1933, 54).—A saturated aq. solution of citric acid is evaporated a t <] 41°/<C 3-2 mm., e.g., aq. acid of 94% purity is evaporated a t 37°/2-5 mm.
to give 75% of the acid as crystals. C. H.
O xidation of organic com pounds. J . Y. Jo h n s o n. From I. G. Fa r b e n in d. A.-G. (B.P. 386,715 and Addn.
B.P. 386,725, [a] 16.9.31, [b] 28.9.31).—(a) As catalyst in the liquid-phase oxidation of paraffin wax etc. there is used 0-05—3% of a mixture of higher carboxylic salts of (a) Li, Na, K, Rb, Cs, Ca, Sr, Ba, Mg, or Al, and (6) Cu, Zn, Cd, Hg, Ti, Zr, Ce, Th, Sn, Pb, V, Sb, Bi, Cr, Mo, W, U, Bln, F e , Co, or Ni, preferably a t 150—170°.
Examples are palm itates of Na and V, or Na, V, and Al.
B r i t i s h C h em ica l A b s t r a c t s — B.
Cl. IV.—Dy k s t c m's. 261
(b) Mixtures of alkali-metal and A1 salts of acids above C5 are used. Examples are : pal nutates of Na and A1;
L i oleate and A1 stearate ; A1 oleate and K salts of acids from oxidised paraffin w ax; K palm itate and
A1 rosinate. C. II.
M anufacture of [sizin g and dressing] assistan ts for the tex tile and related in dustries. J . Y.
Jo h n s o n. From I. G. Fa r b e n in d. A.-G. (B.P. 386,752, 19.11.31).—R ubber and rubber-like products or tlieir degradation products are sulphonated with C1S03H in an org. diluent (E t20) and used in solution or emulsion.
G. H.
M anufacture of [w etting, d isp ersin g, and soften- ing] agents suitable for use as a ssista n ts in the tex tile and allied in dustries. J . Y. Jo h n s o n. From I. G. Fa r b e n in d. A.-G. (B.P. 386,966, 25.6.31).—
Sulphuric esters of hydroxyalkylamines, carrying re
placeable H attached to N, are condensed in presence of alkaline-reacting metal compounds with acyl halides, R -C O X or RO-CO-X. Examples include compounds from : N H 2-CH2-CH2-0-S03H and stearic or oleic or {3-naphthoic acid chloride ; NHBu“-CH2-CIL,-0-S03H and coconut oil acid chlorides, or ClC02Cj8l I 37, or ClC02Ph ; N H 2-CH„-CH2-CHMe-0-S03H and C1C02Bu“ ; NH 2-CH2-CH2-CHMe-0-S03H and lauryl
chloroformate. C. H.
M anufacture of [aralkyl] m ercaptans. J. M. F.
L e a p e r , A s sr. to N a t . A n i l i n e & C hem . Co., I n c . (U.S.P. 1,842,414, 26.1.32. A p p l., 16.1.28).—CII2PhCl is c o n d e n s e d with aq. NaHS a t 75—80°. C. H.
Preparation of am ine hydrohalides. E. C.
Br it t o n, Assr. to Dow Ch e m. Co. (U.S.P. 1,843,705, 2.2.32. Appl., 14.9.29).—H halide is led into the liquid amine (NH2Ph or o-C6H 4Me,N H 2) in a mixing machine below the in.p. of the product. 0. H.
M anufacture of diphenylam ines. J. Fr e i, Assr.
to E. I. D u Po n td e Ne m o u r s & Co. (U.S.P. 1,840,576, 12.1.32. Appl., 22.12.26. Renewed 6.4.29).—N II2Ph and N H 2Ph,HCl are kept boiling a t 300°/20 atm . in an autoclave provided with reflux condenser and an outlet valve for the cooled NH3. a-C10H 7-NH2 is similarly condensed with y-phenetidine in presence of a little sulphanilic acid a t 220°. In both cases boiling is maintained by reducing the pressure as reaction proceeds.
[M anufacture of] diaryl ether derivatives. E. F.
Gr e t h e r, Assr. to Dow Cheji. Co. (U.S.P. 1,842,163, 19.1.32. Appl., 7.10.29).—a-C10H 7-OPh is sulphonated below 100°, and nitrated below 30° to give 2-nitro-l- phenoxynaphthalene-4-sulphonic acid. C. II.
Preparation of 4- and 2-h yd roxy-p -p h en yl-o- benzoylbenzoic acids [4'-o-carboxybenzoyIdi- p h en y ls]. P. II. Gr o g g in s (U.S.P. 1,843,718—9, 2.2.32. Appl., 8.8.29).—(a) 4- and (b) 2-Chloro-4'-o- carboxybenzoyldiphenyls are treated with 4% aq.
NaOH a t 150—220°/6—16 atm. to replace Cl by OH.
The products have m.p. 236— 240° and 183—184°,
respectively. C. II.
M anufacture of triaryl phosphates. W . P. t e r Ho r s t, Assr. to Ru b b e r Se r v ic e La b o r a t o r ie s Co.
(U.S.P. 1,840,335, 12.1.32. A ppl, 26.11.28).—The
reaction between POCl3 and phenols is catalysed by ultra
violet light. C. H.
[M anufacture of com m inuted] anthraquinone product. L. C. Da n i e l s, C. J . Sc h w in d t, and A. 0 . Ja e o e r, Assrs. to Se l d e n Re s. & En g. Co r p. (U .S .P . 1,842,390, 26.1.32. Appl., 22.3.30).—A dustless, com
minuted anthraquinone is obtained by disintegrating needle crystals of anthraquinone. C. H.
M anufacture of anthraquinone derivatives [di- halogenoanthraquinonesulphonic acids]. J. F.
Th o r p e aud A. A. Go l d b e r g (B.P. 386,997, 24.7.31).—
1 : 2-, 1 : 3-, or 1 : 4-Dihalogenoanthraquinones are sul
phonated in absence of catalyst, and the 6- and 7-sul- phonic acids are separated by crystallisation of the Na
salts. C. H.
Preparation of d i-[o-carb oxyp h en ylam in o]- anthraquinones. W. L. Rin t e l m a n and R. J.
Go o d r ic h, Assrs. to E. I. Du Po n t d e Ne m o u r s & Co.
(U .S .P . 1,841,674, 19.1.32. Appl., 11.12.26).— 1 :5- Dichloroanthraquinone is condensed with K anthranil- ate in presence of basic Cu(OAc)2. C. H.
M anufacture of derivatives of the anthraquinone series [pyrim idanthrones]. I. G. Fa r b e n in d. A.-G.
(B.P. 386,861, 2.6.32. Ger., 3.6.31).—An a-amino- anthraquinone is condensed with an alkyliminochloride, R-CCKNR', in which R is aryl or aralkyl aud R ' is alkyl, preferably in presence of org. solvent. The iminochloride may be produced in situ from an acid alkylamide and S0C12. Examples a r e : CPhCKNMe with 4-chloro-l-aminoauthraquinone (m.p. 236—237°), 2 : 4-dichloro-8-amino-6 : 7-phthaloylacridone, 6-amino- 1-methylauthrapyridoue (m.p. 287—288°), 1 : 5-diamino- anthraquinone (m.p. 226°), or l-amino-4-benzamido- anthraquinone (yellow v at d y e ; hydrolysed, m.p.
280—281°); CPhCliNEt with l-amino-5-benzamido- anthraquinone (golden-yellow) ; l-amino-4-benzamido- anthraquinoue with a-C10H,*CCl!NMe (vellow), PhCHiCH-CCKNMe (orange), CH2P h -C C i:N M eo r 2- chloroanthraquinone-3- (green-yellow) or benzanthrone- 2-carboxylmethylimide chloride. C. H.
[M anufacture of] anthraquinone derivatives [phenylbenzanthrones and vat d y es therefrom ].
E. I. Du Po n td e Ne m o u r s& Co. (B .P . 386,989, 22.4.31.
U.S., 2.5.30).—A 2-halogeno- or -liydroxy-phenyl- anthraquinone is heated w ith glycerol, H 2S 0 4, and Cu to give benzanthrones, which m ay be converted into corresponding dibenzanthrones (green-blue to steel-blue vat dyes). The 2-p-chlorophenyl compound yields isomeric benzanthrones, m.p. 131-8— 134-4°, 102-4—
103-6°, and 160—162°, respectively. Compounds from o- and m-chlorophenylanthraquinones are also described.
C. H.
Pure N aO Ac.—See VII. [AcOH from ] sacchar- ification of cellulose. EtOII from w ood .-—See X V II.
BuOH and COMe2 b y ferm entation.—See X V III.
IV.— DYESTUFFS.
Influence of phenols on the violanthrone fusion.
I. Separation of products of fusion. II. P ro p erties of the products. T. Ma k i (J. Soc. Chem. Ind., Japan, 1932, 35, 577—583 b ) . - -Fusion of benzanthrone
B r it is h C h e m ic a l A b s t r a c t s —B.
202 Cl. 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.
with IvOH a t 220° gives 2-hydroxybenzanthrone, m.p.
298—299° (Ac derivative, m.p. 202-7—203-7°) (cf.
Perkin, B., 1920, 623 a) , a substance, m.p. 272°, sol. to a yellowish-orange solution with a green fluorescence in H 2S 0 4, and possibly a dibenznnthronyl (not 2 : 2 '- ; cf. G.P. 407,838), and violanthrone-B (I), a greyish-violet v at dye of unknown composition, in addition to dibenz- anthrone (II) (violanthrone-^4). These are separated in turn by extraction with aq. alkali and then with hot glacial AcOH, and by vattin g the residue a t 55—60°
for 15 min., when the bulk of (I) remains undissolved.
A pure blue solution is given by (I) in conc. I I 2S 0 4 (absorption max. a t X 6360 m jx); it forms with difficulty a violet v at a t 65—70° (Bz derivative of lcuco-dye described). The properties of (II) in a highly purified state arc described; it forms a pure violet solution in conc. HoSO., (absorption max. 5700 mix), and is sensitive to fused KOH a t 250°. The yield of (II) is markedly increased, and th a t of (I) decreased, by addition of PhOH to the melt. All m.p. are corr. H. A. P.
Pa t e n t s.
M anufacture of oil-solu b le d yes. H. E. Buc, Assr. to St a n d a r d Oi l De v e l o p m e n t Co. (U .S .P . 1,841,876, 19.1.32. Appl., 16.5.27).—A basic dye, e.g., Victoria-green, Bismarck-brown, Malachite-green, Me- violet, nigrosine, or Mcthylene-blue, is treated w ith an aq. solution of oil-sol. sulphonated petroleum. C. II.
M anufacture of d yes containing nitrogen [p ig
m en ts, acid and vat d y es]. J. Y. Jo h n s o n. From I. G. Fa r b e n in d. A.-G. (B.P. 387,092, 23.12.31).—
Deeply coloured products are obtained by oxidation, with air or 0 2 a t raised temp, and pressure, e.g., ]>
120°/10—30 atm ., of arylamines in aq. solution or suspension, preferably in presence of acid and of cata
lysts. Examples are : pigments from N H 2Ph,lIC l (black), aminoazobenzene (black), p-nitroaniline (black), k-C]0H 7-NH2,HC1 (brown), S-CJ0IIT-NII2,IIC1 (black), NPhMe2,HCl (black); acid dyes from metanilic (brown), p-phenylenediammesulphonic (brown), benzidine-2 : 2'- disulphonic (brown), 2 : 6 : 8-naphthylammedisulphonic (brown-yellow) acids ; v a t dyes from 1 : 4-, 1 : 5-, and 1 : 8-diaminoanthraquinone hydrochlorides (brown).
C. H.
M anufacture of yello w vat d y es [of the anthra- quinone ser ies]. A. Ca r p m a e l. From I. G. Fa r b e n in d. A.-G. (B.P. 386,733, 13.10.31).—A 1 : 2-dihydroxyan- thraquinone is condensed with a 1 : 2-diha logenoanthra- quinone, preferably in presence of acid-binders and/or org. so lv en t; or the crude products from the condensa
tion of l-halogeno-(or nitro-)2-hydroxyantliraquinones (cf. G.P. 257,832, 265,647, 293,660) are treated with NaOCl before or after extraction of by-products with an org. solvent, b.p. > 80° (AcOH), or before extraction w ith 80—92% HoSO,,. Examples are yellow v at dyes from : alizarin and 1 : 2-dibromo-, 1 : 2-diehloro-, or 1 : 2 : 3-tribromo-anthraquinone ; 1 : 2-dibromoanthra- quinone and 1 : 2 : 7-trihydroxyanthraquinone or 4-
benzamidoalizarin. C. H.
Purification of d ia m in o -a a '[l: 5- and l: 8 ] - d i- hydroxyanthraquinonedisulphonic acid d y es. II. T.
St o w e l l, A s s r. to Na t. An i l i n e & Ch e m. C o., Inc. (U.S.P.
1,840,644, 12.1.32. Appl., 13.2.26).—The crude product from anthrarufin or from chrysazin is treated with 4—5% H 2S 0 4 a t 60—70° to dissolve impurities, cooled
to 15°, and filtered. C. H.
M anufacture of polyazo d y es. I. G. Fa r b e n in d. A.-G. (B.P. 387,222, 17.6.32, Ger., 17.6.31).—Hydroxy- carbazoles are used as end-components in dis- and poly-azo dyes carrying a t least 1 solubilising group.
Examples are : 2 : 4 : 8-naphthylaminedisulphonic acid -> a-C10H 7-N H 2 ->- cresidine -> 4-hydroxycarbazole- 2 : 8-disulphonic acid (grey-blue to blue-black on cotton, viscose, silk, or chrome le a th e r); 2 : 7-naphthylamine- sulphonic acid -> y-xylidine -> 2-ethoxyCleve acid -> 6-amino-4-hydroxycarbazole-2 : 8-disulphonic acid (grey on cotton or viscose); N H 2Ph -> H-acid <- benzidine-> 3-hydroxycarbazole-7-sulphonicacid (green- grey) ; p-nitroaniline -> y-acid, reduced, -> 2 mols.
of 6-amino-4-hydroxycarbazole-2: 8-disulphonic acid
(black). ' C. H.
M anufacture of halogenated indigo and its d erivatives. J . Y. Jo h n s o n. F r o m I . G. Fa r b e n in d. A.-G. (B.P. 387,121, 29.1.32).—Alkyl or alicyclyl H sulphates are used as solvents or dispersing agents in halogenation of indigos, e.g., a t — 10° to 80° a t 1— 10 atm . in presence of a catalyst. C. H.
Preparation of iso cy a n in es containing ¡3-naphtha- quinoline nuclei. Il f o r d, Lt d., and (Miss) F . M.
Ha m e r (B.P. 387,167, 12.8.31. Addn. to B.P. 370,388 ; B., 1932,765).—A3-halogeno- p-naphthaquinoline alkiod- ide is condensed w ith an alkiodide of a JV-ring compound having a y-Me group; e.g., 3-iodo-[i-naphthaquinoline methiodide w ith lepidine ethiodide. . C. II.
P yrim id an th ron es. Phenylbenzanthrone d y es.
—-Sec III.
V.— FIB R ES; TEXTILES; CELLULOSE; PAPER.
W ool sw ellin g and felting in relation to the p a of the w ettin g solu tion . I. S w ellin g of w ool. II.
Felting of w ool. E. Go t t e and W. Kl i n c (Kolloid-Z., 1933, 62, 207—213, 213—215).—I. Apparatus and technique for measuring the swelling of textile fibres are described. A t 20° the swelling max. in the acid region is a t Ph 3-0, there is a min. a t about pn 5-8, and beyond p a 11 the swelling increases rapidly, due to chemical decomp, which leads eventually to complete dispersion.
A t 70° the swelling curve has a min. a t p n 4 • 3.
II. The felting property of wool decreases linearly with increase in alkalinity of the liquor in which it is immersed. This change is attributed to the reduced scaliness of the hair surface. E. S. H.
C h em istry of w ood. IV. W ater-soluble p o ly sa c
charide of eastern larch . L . E . Wi s e, P . L . Ha m e r, and F . C. Pe t e r s o n (Ind. Eng. Chem., 1933, 25, 184—
187 ; cf. B., 1931, 876).—E astern larch (Larix laricina) yields about 4% of a galactan apparently identical with e-galactan from western larch (cf. B., 1930,503). Analysis gives anhydroarabinose 12-0% (as diphenylhydrazone) and 12-6% (by furfuraldehyde method) and anhydro- galactose 82-1% (as mucic a c id ); western larch galactan gave S2-5% of anhydrogalactose. No evidence of OMe or uronic acid groups was obtained. Analysis of known
