BRITISH CHEMICAL ABSTRACTS
B.—APPLIED CHEMISTRY
F E B R U A R Y 18. 1927.
I.—GENERAL; PLANT; MACHINERY.
Catalytic pow er of [anim al] charcoal. V. Po d r o u-
z e k (Chem. Listy, 1926, 2 0 , 553—555).—The catalytic activity of animal charcoal depends on its iron con ten t;
extraction of the charcoal with hydrochloric acid reduces its activity practically to zero when all the iron has been removed. Absolutely pure carbon, whether in coarse particles or in colloidal solution, shows no sign of catalytic
activity. A. R. Po w e l l.
Pa t e n t s.
[Jaw] crushing m achines. E. 0 . St u b b i n g s (E.P.
261,211, 1.1.26).—As shown in the figure, a single eccentric, 7, reciprocates the upper part, 4, of the jaw
directly, and gives an exaggerated motion to the lower part, 3, of the jaw by means of the toggles, 9,10, and 12.
A sliding wedge piece, 18, is provided to take up wear.
B. M. Ve n a b l e s.
[Fine] grinding m ill. J. Ee r h a r d t (E.P. 261,322, S.9.26).—An apparatus for fine grinding comprises a
disc rotating preferably on a vertical shaft, against the edge of which a number of blocks are individually pressed by a weighted lever and screw. Entrance for the feed material is provided by passages formed in the blocks, emerging near the leading edge, and the ground material falls away between the blocks. By setting the axes of the blocks a t an angle to their respective radii a larger proportion of the edge of the
disc is rendered effective. B. M. Ve n a b l e s.
Regenerative heat-exchanging apparatus. E. H., and E. P. Ki g n e l l (E.P. 249,152, 12.3.26. Conv., 14.3.25).—A heat exchanger for two or more fluids is arranged so th a t the conduit for one fluid forms the container for the heat-transferring substance, which has passages left in it for the flow of the fluids. The other fluid or fluids enter and leave through the side of the
main conduit, and all the fluids are distributed to the various passages of the regenerator in turn by continu
ously rotating valves. B. M. Ve n a b l e s.
R efrigerating p rocesses. R. W. Da v e n p o r t ( E .P .
249,097, 25.2.26. Conv., 12.3.25).—The refrigerant is circulated continuously in a closed cycle, and comprises a condensible component, such as carbon tetrachloride, and a non-condensible component insoluble in and inert to the condensate, such as air. The latter promotes normal boiling, i.e., without superheating. The cycle includes compression of the gas and vapour together, cooling of the compressed mixture to condense part of the vapour, expansion of the gas and vapour in thermal contact with the liquid, and heating of the liquid to vaporise it in contact with the gas. The non-condensible component is of sufficient volume to produce a total pressure on the liquid substantially exceeding its own vapour pressure, and such volume is determined in accordance with the tem perature desired in the refrige
rating zone. The total pressures of the high and low sides of the cycle remain constant, and the ratio of the partial pressure of the non-condensible component to the total pressure is kept constant. H . Ho l m e s.
Evaporating apparatus. D. A. Bl a i r, and Bl a i r, Ca m p b e l l & McLe a n Lt d. (E.P. 262,608, 30.12.25).—A system of evaporation (especially suitable for tannin extracts) comprises a film evaporator combined with at least two other evaporators which contain a good bulk of liquid. The film evaporator does the bulk of the evaporation continuously, and the somewhat irregular product from it is collected in one of the bulk evaporators while the other bulk evaporator is finishing a batch.
B . M . Ve n a b l e s.
P ro c e ss of evaporation. W. L. Ba d g e r, Assr. to
Sw e n s o n Ev a p o r a t o r Co. (U.S.P. 1,609,853, 7.12.26.
Appl., 9.8.23).—A crystallisable liquid is boiled in an evaporating chamber, and small quantities are with
drawn and superheated. The superheated liquid is re-introduced into the chamber, where it flashes, producing seed crystals which promote the crystallisation.
H . Ho l m e s.
Apparatus for drying granular m aterials. F . M . Pa r k e r ( E . P . 261,517, 3.10.25).—The material is sub
jected to a countercurrent of furnace or other hot gases as it slides down a zigzag passage constituted by super
posed compartments carried by a connecting frame, the movement of the material being produced by impart
ing a swinging motion to the frame. The compartments may be inclined tubes communicating a t their ends, and partitioned longitudinally to provide different passages for different grades of material. Alternatively, a casing carried by the frame may be divided into compartments by trays attached alternately to the opposite end walls,
95 a
B r itis h C hem ical A b stra c ts— J3.
96 C l. n . —F u e l ; Gas ; D e stk o o tiy i D is tilla t io n ; M in eral Oils.
each tray sloping downwards from the point of attach
ment and terminating at a distance from the other end wall. The dryer may be enclosed to conserve heat radiated from the top of the furnace, and the receiving end of the discharge shoot for the material may be mounted within the furnace. H . Ho l m e s.
M ixing process and apparatus. J. W. Sm i t h
(E.P. 261.135, 4.9.25).—Flowable materials are mixed by passing them through a conduit which is provided with a number of deflecting devices, each comprising a ring of tapered fingers or blades extending from the circumference inwardly and inclined. The blades are preferably twisted to a helicoidal shape so as to give a whirling motion to the liquid, which is reversed at alternate mixing devices. B. M. Ve n a b l e s.
Centrifugal m ix in g or em u lsifyin g apparatus.
F. Gr i m b l e, M. N. Ca i e d, and E. Co o m b s(E.P. 261,904, 7.11.25).—The apparatus comprises a number of specially-shaped discs assembled on a hollow shaft or driver which forms the feed passage. The outlet spaces between the discs are segmental (i.e., not complete annuli), and are narrower at the outer circumference. Corru
gated material may also be placed between the discs with the corrugations substantially radial.
B. M. Ve n a b l e s.
Separation of the constituents of gaseou s m ix tu res. Liquefaction and separation of gaseous m ix tu res. C. C. Va n Nu y s, Assr. to Ai r Re d u c t io n
Co., In c. (U.S.P. 1,607,320—1, 16.11.26. Appl. [a]
2.8.21; [b] 31.1.23).—(a) A constituent not readily liquefiable is separated by subjecting the mixture to selective backward-return condensation, first with previously liquefied portions evaporating a t a lower pressure, and afterwards with an extraneous liquid evaporating a t a lower temperature, thus liquefying selectively substantially all bu t the desired constituent.
(b) A portion of the mixture is partially expanded.
Another portion is liquefied by indirect contact with a liquid enriched in the less volatile constituent, and the liquefied mixture is rectified by direct contact with the partially-expanded gaseous portion. The gases resulting from the rectification are subjected to selective lique
faction with backward return to supplement the liquid enriched in the less volatile constituent produced by the
rectification. H . Ho l m e s.
Liquefaction of g a ses. C . C. Va n Nu y s and J . L.
Sc h l i t t, Assrs. to Ai r Re d u c t io n Co., In c. (U.S.P.
1,607,322, 16.11.26. Appl., 10.1.25).—The gas is com
pressed, cooled, partially expanded, and further cooled to the liquefaction tem perature corresponding to the expansion pressure. I t is then subjected to backward return condensation by therm al contact with previously liquefied portions. H . Ho l m e s.
Separation of the constituents of gaseou s m ix tures. C. C. Va n Nu y s, Assr. to A ir Re d u c t io n Co.,
In c. (U.S.P. 1,607,708, 23.11.26. Appl., 22.10.24).—
The mixture is subjected to a primary rectification to produce a gas impoverished in one constituent. This gas is withdrawn, recompressed, and liquefied, and the liquid is subjected to an auxiliary rectification to separate another constituent in substantial purity. The low temperature of the auxiliary rectification is maintained
by application of refrigeration from the primary recti
fication. H . Ho l m e s.
Liquefaction and rectification of ga ses. C. C.
Va n Nu y s, A s s r . to Ai r Re d u c t io n Co., In c. (U.S.P.
1,609,450, 7.12.26. Appl., 2.12.19).—A gaseous mixture is liquefied to separate a portion of one constituent as a residual gas which is withdrawn, expanded, and caused to travel in indirect contact with the mixture to be liquefied. The liquid is rectified to produce a liquid comprising one constituent in substantial purity, and an effluent having substantially the composition of the original gaseous mixture. The liquid is vaporised, and the vapour is withdrawn separately from the effluent.
H . Ho l m e s.
Method and m eans for determ ining or com paring the viscosities of flu id s. Kn o w Mi l l Pr i n t i n g C o., Lt d., and T. L . Mo r t ( E .P . 262,539, 18.9.25).—The apparatus comprises a handle provided a t the end with a depression or cup accurately ground to fit a ball. The distance between the ball and the cup is regulated by means of a screw within the handle terminating in three small feet a t the centre of the cup. To operate, the ball is pressed into the cup when both are below the surface of the liquid to be tested, and the time taken for the ball to fall away under its own weight is noted when the gap is set a t a standard thickness; or the gap may be adjusted till the ball falls away in standard time.
B. M. Ve n a b l e s.
V iscosity m eters. C. M. La r s o n and C. L . Kn o p f ( E .P . 262,652, 17.5.26).—Two similar tubes, each con
taining a ball or other solid particle, the one filled with a standard liquid (which may be sealed) and the other filled with the liquid to be tested, are tilted together and the time noted for the ball to run down. A form of the apparatus suitable for direct attachm ent to the crank-case of an engine is described. B. M. Ve n a b l e s.
Filters for air and g a ses. D. Ha l l, J. H . Ka y, and
Ha l l & Ka y Lt d. (E.P. 261,897, 26.10.25).—The filter medium, which may be flannel or other fabric, is backed by wire netting or similar material stretched over the open frames. B. M . Ve n a b l e s.
Preparation of diatom aceous earth. R. C . Wi l l i a m s, Assr. to Th e Dia t o m In s u l a t io n C o . (U.S.P.
1,606,281, 9.11.26. Appl., 15.7.25).—Raw diatomaceous earth is mixed with a large quantity of water and deflocculatcd by the addition of a suitable substance, the mixture is then flocculated by the addition of another substance and allowed to settle, the broken skeletal frames and impurities being decanted off with the water from the heavier whole skeletal frames.
B. M . Ve n a b l e s.
Lubricant. E . M . Ho n a n and J. R. To w n s e n d,
Assrs. to We s t e r n El e c t r i c Co., In c. (U.S.P. 1,606,788, 16.11.26. Appl., 17.12.24).—Spermaceti wax and petro
latum are dissolved in a readily volatile vehicle.
H . Ro y a l- Da w s o n.
II.-FUEL; GAS; DESTRUCTIVE DISTILLATION;
MINERAL OILS.
Coking process and path of travel of g a ses in the coke oven. T. Sc h m id t (Fuel, 1926,5, 486—509).—
In a partially carbonised coke-oven charge there exists
B r itis h C h em ica l A b s tr a c ts— B .
Cl. I I . — Fu e l; Ga s; De s t r u c t i v e Di s t i l l a t i o n; Mi n e r a l Oi l s. sn
a zone of uncarbonised coal separated from a zone of semi-coke by a layer of coal in the plastic state. As heat penetrates the charge the plastic layer is trans
formed into semi-coke and a new plastic layer is formed in the succeeding layer of coal. Immediately after charging an oven a considerable positive pressure, increasing towards the sole, exists in all planes of the charge. As the plastic layer advances from the oven wall the pressure within the semi-coke zone formed falls to a slight vacuum, which is fairly uniform through
out the height of the oven. The positive pressure exists, however, on the cooler side of the plastic layer so long as any uncoked coal remains. The temperature in the semi-coke rises from 500° to 1000° according to the duration of its heating. The uncoked coal remains a t 100° so long as it contains any moisture, which in the case of the coal a t the centre of a 21-in. oven is not driven oS until 18 hours after charging. The plastic layer, therefore, is divisional between a zone of high pressure and low temperature, and one of low pressure and high temperature. Depending upon the nature of coal in the plastic state, the carbonisation in coke ovens is more or less a two-stage process.
Samples of a coal which was being carbonised in ovens on the large scale were distilled up to 500° in the labora
tory, and the nature and the distribution of the products were determined. A sample of freshly-formed semi
coke was taken from one of the ovens and distilled to 1000°, its products being determined and examined.
The formation of ta r ceases with the plastic state, and no ta r was formed by distillation of the semi-coke.
The permanent gas is equally distributed, by weight, between the high- and the low-temperature stages, but the relative densities and, therefore, volumes in the two cases are very different. Samples of gas from the uncoked coal 1 hr. and 12 hrs., respectively, after charging were both precisely similar to the gas obtained from the low-temperature distillation of the coal in the laboratory, indicating th a t little or no gas passes from the semi-coke through the plastic layer, which is to be expected from the rise in pressure across the plastic layer in th a t direction. Some of the low-temperature products pass from the plastic layer into the coke, as indicated by the presence of ta r in samples of gas from the coke zone, and also by the high methane and low hydrogen content of the gas passing through the coke as compared with the gas distilled from freshly-formed semi-coke. I t is calculated th a t with a lean gas coal 20 26% by volume of the permanent gas, 80% of the tar, and 10% of the ammonia produced pass through the uncoked coal. Ammonia is confined essentially to the coke zone, and is not subject to the influence of the large proportion of moisture in the coal as carbonised
in coke ovens. S . Pe x t o n.
Relative ignition tem peratures of solid fuels.
K. Na k a m u r a and A. Sh im o m u r a (Mem. Coll. S c i.
Kyoto, 1926, A 10, 89—94).—The relative ignition temperatures of 22 kinds of solid fuel, including various types of Japanese coal, a semi-coke, a metallurgical coke, and wood charcoal, have been determined by Wheeler’s method (B., 1924, 896). The method was slightly modified by the introduction of a paraffin bath surrounding the tube containing the coal, and secondarily
heated by the electrically-heated sand bath. In general, the greater the oxygen content or the volatile-matter content, or the lower the ash content of a coal, the lower is its relative ignition temperature. The rule relating to the oxygen content, however, does not apply to lignites. A. B. Ma n n i n g,
Specific gra vity of lig n ites and of the cokes therefrom . M. Do l o h (Z. angew. Chem., 1926, 39, 1518—1521).—The sp. gr. of a large number of brown coals and lignites rich in volatile m atter from Central Germany is about 1 ■ 00, but for more ligneous brown coal it is generally lower. The desiccation of the coal with air lowers the sp. gr. of the lignites very considerably, but not th a t of the more pronounced ligneous coals, whilst more amorphous coals give irregular results. German brown coals shrink much less when dried in nitrogen than by air drying. The sp. gr. of the coke from various types of coal is also subject to the same variations, and here also the presence of oxygen in the drying gives a smaller coke volume with brown coal, bu t this is not found with coke from the more ligneous coals. The sp. gr. of coke from brown coal is about 0-50, cokes from ligneous coals are as low as 0 -15, whilst cokes from more amorphous coals occupy an intermediate position.
W. G. Ca r e y.
Wood as ga s-m ak in g m aterial. O. F. St a f f o r d
(Ind. Eng. Chem., 1926, 18, 1318—1320).—Distillation of dry Douglas fir mill-waste in the generator of a water- gas plant used as an internally heated retort gave, per ton of wood, 18,000 cub. ft. of a gas of heating power 480 B.Th.U. and no tar. Substitution of wood for coal in a blue water-gas plant gave a gas very similar to th a t obtained when coal is used, and a little tar. Under certain conditions it appears possible to make a producer- gas of low heating power more cheaply from wood th an from coal. Low-temperature distillation of wood yields relatively small amounts of a gas which is chiefly carbon dioxide, bu t this could be converted into a product resembling water-gas by passing it through a bed of incandescent charcoal. Soft woods are most suitable
for gas-making. R. Cu t u i l l.
Influence of the variable com position of coke- oven g as on its econom ical com bustion. Sa u e r m a n n
(Gas- u. Wasserfach, 1926, 69, 1135—1141).—The com
position of coke-oven gas depends on the pressure maintained in the oven, the external wind pressure and direction, the coal used, the coking temperature, and other factors, and is therefore subject to considerable variation. Analyses, calorific values, densities, volumes of products of combustion, volumes of air required for combustion, theoretical flame temperatures, etc. are tabulated for 20 samples of gas taken from a coke-oven plant a t various times during the course of six months’
working. No simple relation exists between the calorific values and densities of the gases. The volume of air required for combustion and the total volume of combus
tion products are approximately linear functions of the gross calorific value. The carbon dioxide content of the flue gases bears no relation to the calorific value, and gives no accurate measure of the excess air. The influence of the am ount of excess air on the flame temperature and the heat losses, and the variation of these when a burner is supplied with gas of varying
a 2
B r itis h C h em ica l A b s tr a c ts—B.
98 Cr.. I L— F u e l ; Ga s; D e s t r u c t i v e D i s t i l l a t i o n ; M i n e r a l O i l s .
pressure and composition, are discussed. For economical combustion good" pressure regulation is necessary. A t constant pressure, fluctuations in the gas supply may occur owing to variations in the density, and even a t constant density the excess air in the flue gases may vary owing to the varying air requirements of the coke oven gas. For the gases tabulated, the maximum variation due to these causes is not greater than th a t due to a pressure difference of 25 mm. of water. Similar calcula
tions have been made for two series of gases of varying composition, b u t of constant calorific value and constant density, respectively. Comparison of these shows the latter to have the advantage, gases of the same calorific value being capable of greater variation in their behaviour on combustion th an gases of the same density.
In evaluating a gas the density and carbon dioxide content, as well as the calorific value, must be taken in to consideration. A. B. Ma n n i n g.
Cracking of ozokerite. E. To p o r e s c u (Bui. Soc.
R om ani Stiinte, 1926, 2 9 , 3—5).—The cracking of ozokerite in presence of 5% of anhydrous aluminium chloride as catalyst yields products distilling a t about 160°, and containing about 6% of benzine and 19% of petroleum oil. W ith 15% of catalyst the distillation commences a t 122—125°, the distillate containing 30% of benzine and 5% of petroleum oil, and with 25% of catalyst the distillate, which first comes over a t 110°, contains 7% of benzine and 2% of petroleum oil. In the last two cases large quantities of gas were evolved, and in all cases unsaturated hydrocarbons were
produced. S. K. Tw e e d y.
A rtificial ageing of m ineral o ils. F. Ev e r sand R.
Sc h m id t (Wiss. Veroff. Sicmens-Konz., 1926, 5, 210—
228).—When a transformer oil is heated a t 150° in an atmosphere of oxygen changes take place similar to those occurring over the course of years of use. These changes may be accelerated by dispersing the oil on silica gel previously impregnated with an oxide catalyst.
The rate of oxidation of the oil is dependent on the chemical and physical nature of the catalyst, the most efficient being colloidal oxides of m ultivalent metals such as vanadium, molybdenum, or tungsten in combination with ferric oxide. The relative stabilities of various oils may be compared by determining the rate of oxidation under standard conditions, e.g., heating for 2 hrs. a t 150°, followed by a determination of the acid value of the oxidised oil. The rate of oxidation is usually very great during the first 5 min. heating, b u t subsequently it decreases rapidly, finally becoming stationary in 1—2 hrs.
During the oxidation small amounts of carbon dioxide, carbon monoxide, methane, and hydrogen are formed, together with acids and dark-coloured solids of great complexity similar to those occurring in the gelatinous deposit formed in transformers. A. R. Po w e l l.
Exam ination of so m e transform er o ils kept for long periods in the dark. H . v o n d e r He y d e n and K. Ty p k e (Petroleum, 1927,23,15).—The increase in the tar-forming values of a number of transformer oils
■which have been kept in the dark for periods of one year or longer have been determined. Most of the oils were kept in metal containers, but some were in
glass b o ttle s; the vessels were not completely filled.
The majority of the oils, and in particular one American non-sludging oil, show considerable deterioration. Of a number of Russian oils examined, those which had been subjected to the least refining showed the least deterioration on keeping. A. B. Ma n n i n g.
Volum etric determ ination of arom atic hexahydro- hydrocarbons in petroleum and tar d istillates.
N. Da n a il a and V. St o e n e s c u (Bui. Soc. Romana Stiinte, 1926, 2 9 , 23—41).—The olefinic hydrocarbons are first determined in the manner previously described (B., 1924, 857 ; 1925, 835). The washed and dried residue is then dehydrogenated a t 300—310° in presence of platinised asbestos (Zelinsky and Pawlow, B., 1923, 797). The unsaturated hydrocarbons are determined in the product as above, and again after a second dehydrogenation, and so on, until the amount of unsaturated hydrocarbons is constant. The saturated aromatic hydrocarbons are then determined. From these quantities the amount of aromatic hexahydro- hydrocarbons is calculated. S . K . Tw e e d y.
M oore ignition m eter. W. R. Or m a n d y and E. C.
Cr a v e n (J. Inst. Petrol. Tech., 1926, 1 2 , 650—654).—
The meter used was similar to th a t described by Moore (cf. B., 1917, 109 ; 1924, 700), except th a t the explosion chamber had a slightly larger volume. Gas heating was used for moderate temperatures, and the block was heated to high temperatures by means of a nichrome wire winding. The spontaneous ignition temperature (S.I.T.) of heptane, previously given as 245°, has since been found to be 253°, great care being taken to remove all traces of hydrogen from the oxygen. Although successive readings of the S.I.T. can be obtained to within 1°, slight alterations of conditions may have an appreciable effect. No certain effect upon the S.I.T.
was obtained by focussing the crater of an arc into the explosion cham ber; by. bringing the arc within a few inches of the chamber cover ; by raising the potential of the block to 200 volts or by other attem pts a t ionisation; or by intensive drying of the liquid and the oxygen. The substitution of vapour for liquid raised the S.I.T. by about 5°. The S.I.T. are given of a number of compounds, and their significance is discussed.
L. A. Co l e s.
D eterm ination of benzene in alcohol solution.
Or m a n d y and Cr a v e n.—See III.
Pa t e n t s.
Coal w ash eries. A. Ro b in s o n, and Sim o n- Ca r v e s, Lt d. (E.P. 261,490, 1.9.25).—lit coal-washing processes such as described in E.P. 22,189/13 (B., 1914, 410) and E.P. 110,994 (B., 1917, 1266), the slurry passes from the settling tank to a washing box of the air-pulsation or Baum type, the heavier and dirtier slimes are removed, and the lighter constituents of the slurry pass for drainage to inclined fixed and horizontal vibrating sieves.
A. C . Mo n k h o u s e.
M anufacture of fuel agglom erates and their binders. F. M. Cr o s s m a n (E.P. 244,053, 12.9.25.
Conv., 5.12.24).—A binder is preferably made by mixing 100 lb. of starch with cold water and adding 1 lb. of sodium nitrate or other oxidising agent. The solution
B r itls h C h em ica l A b e tr a c ts—B .
C l . II.— F u e l ; G a s ; D e s t r u c t i v e D i s t i l l a t i o n ; M i n é r a l O i l s . 99
is heated so as to gelatinise the starch, and 500 lb. of sulphite cellulose liquor (d 1 ■ 26) are added to enhance the cohesive properties of the binder. To the boiling mixture 400 lb. of oil residuum are added as a water
proofing agent. The binder thus prepared is admixed with powdered coal, preferably of low volatile content, in the proportion of 4—6% of binder. The agglomerate is pressed to shape and dried at 100—200°.
S . Pe x t o n.
Coke m anufacture. R . F . F. Fabry (E.P. 259,869, 8.6.26).—Coal is preheated to 100° by means of waste products of combustion and charged by a centrifugal fan into a small insulated service bunker. The preheating reduces the subsequent time of carbonisation, diminishes the water content of the distillation gases, and dispenses with coal-stamping and charging machines ; a larger, denser, and harder coke is obtained.
A. C. Mo n k h o u s e.
Coking and d istillation of carbonaceous m ate- x'ials. J. F. L. Mo e l l e r (E.P. 260,020, 25.6.25).—
The material is subjected to a preliminary drying and cleaning, if necessary, and then preheated by hot air or by waste gases cooled to the desired temperature with air. The retort used may be of any type, and is supplied with steam superheated to a temperature at or above th at of the fuel, viz., 260—400° for peat and 450—600° for coal. The steam is generated a t high pressure and, after superheating, fed to the retorts at low pressure, the retorts being maintained a t a pressure slightly lower than atmospheric. For stationary retorts a channel covered with perforated plates is used, the holes being protected by flaps. For rotary retorts a perforated central tube is used from which hollow perforated arms project which act also as stirrers.
A . C. MONKHOUSE.
Carbonising p rocesses. W. E. Tr e n t (E.P.
261,954, 8.2.26).—Pressed mixtures of coal and fuel oil of desired shape are fed into trays and slowly conveyed through a chamber for preliminary heat treatm ent at a low temperature (230—300°) in an atmosphere con
taining oxygen. The heating is conducted by hot elements temporarily fixed in eacli tray and on which the briquettes rest. The heating elements are replaced by other hot elements after each passage through the carbonising chamber. The briquettes, case-hardened by this treatment, are eonveyed to a second retort and carbonised a t 600—650° in an atmosphere free from oxygen.^ The product is of the same shape and size as the original briquettes. S. Pe x t o n.
Carbonising or cracking fuels. In t e r n a t io n a l Co m b u s t io n En g i n e e r i n g Co r p., Assees. of W. Ru n g e
(E.P. 253,499, 18.5.26. Conv., 12.6.25).—Finely divided fuel, e.g., pulverised coal or atomised oil, is sprayed into a vertical retort, heated internally by ascending gases.
The top of the retort is cooled to below 150° either by a water jacket or by cold gases entering above the car
bonising zone ; the hydrocarbons of higher b.p. are con
densed and run back into the lower portion of the retort maintained a t 570°, where they are carbonised.
A. C . Mo n k h o u s e.
Treating carbonaceous m aterials. W. E. Tr e n t
(E.P. 259,795, 3.12.25).—Dry pulverised coal or such coal in oil suspension, after mixing with a fluxing agent,
e.g., calcium or iron oxides or sodium carbonate, is carried in suspension in a stream of oil or air into a combustion chamber. Distillation takes place without fusion of the carbon particles. Carbonisation proceed, a t 450° in a coil heated by gases passing down a refractory chamber in its centre. The products, oil, coke, and slags are separated by gravity, or water may be injected and the resulting emulsion subsequently treated.
A. C. Mo n k h o u s e.
Production of liquid fuel m ixtu res. T. H. Bu t l e r,
F. J. W. Po p h a m, J. C. Ma n n, and II. W. Ro b in s o n
(E.P. 261,907, 17.11.25).—Coal ta r pitch is blended with petroleum fuel oil by heating the former above its m.p.
and gradually adding the oil during continuous agitation of the mixture. The fuel is burnt while still hot. The exact temperature a t which mixing must take place is found by laboratory experim ent; too low a temperature leads to a dull grainy mixture owing to separation of
bitumen. W. N. I Io y t e.
Burning powdered or liquid fuel in furnaces.
E . S . Su f f e r n ( E .P . 261,807, 29.5.25).—The fuel and
“ primary a i r ” (about half th a t quantity required for complete combustion) are projected into the primary combustion chamber where the stream is deflected and diffused. W ithout extinction of the flame the stream passes to the secondary chamber where admixture with further air causes complete combustion. The burning fuel in the primary chamber is subjected to the radiant heat from the secondary chamber.
W. N. Ho y t e.
Gas producers. A. Wi n k l e r (E.P. 247,565,10.2.26.
Conv., 11.2.25).—Steam or atomised water is sprayed into the fuel bed of gas producers through passages in the walls above the grate. The tubes for injection are continuous and arranged in recesses protected by fire
brick a t such a height above the grate as to prevent the formation of arches of clinker and the adherence of clinker to the walls. Various applications are described, in some of which the slope of the producer grate is adjustable, and an automatic extractor is provided a t the end of the grate for the removal of ash and clinker.
A. C. Mo n k h o u s e.
D istillin g or coking b itum inous substances.
Ko h l e n v e r e d l u n g Ge s.h.b. H ., and C. Ge i s s e n (E.P.
261,290^ 27.5.26).—In horizontal or vertical retorts in which a thin moving layer of fuel is carbonised by heat applied a t one side, a wall is provided a t the side of or above the fuel on the opposite side to the heating zone.
This wall contains a number of channels to enable the products of distillation to be rapidly removed from the hot zone, the wall acting as an insulating medium pre
venting decomposition of the gases. A. C. Mo n k h o u s e.
Apparatus for the d istillation of granulated and like com bu stib les. II. Wi e d e m a n n (E.P. 261,156, 9.10.25).—The retort used is of a beehive type enclosed in a furnace of similar shape heated a t 400—600° by gas burners. The material is fed on to the bottom flat circular plate of the retort by means of a shoot with a flange to prevent the material passing to the coke con
veyor. The charge is stirred by a vertical shaft fitted with flanged stirring arms which conveys the material round to the coke conveyor situate a t the opposite
B r itis h C h em ica l A b s tr a c ts—B .
1 0 0 Cl. I I I . — Ta b a n d Ta b Pr o d u c t s.
side to the gas offtake. The coke finally passes from the conveyor to a generator of inverted pear shape contain
ing a similarly shaped core, fitted with spur-like projec
tions, which can be rotated. Air and steam for the generator are supplied through channels in the casing
walls. A. C. Mo n k h o u s e.
Combined process for carbonising coal and cracking oil. W. E. Tr e n t (E.P. 262,302, 15.2.26).—
Pulverised coal, passing 100 mesh, mixed with water, is fed to an agglomerater, where it is mixed with petro
leum residuum in the proportion of about 5 pts. by weight of coal to 1 pt. of hydrocarbon. The soft agglomerate is dried, formed into briquette shapes, and passed through a baking oven maintained a t about 350°
by hot flue gases, where the briquettes harden ; they are then discharged. The vapours evolved from the oven pass to a compressor where they are compressed to about 100 lb./sq. in. ; their temperature thereby rises to about 450°, cracking takes place, and the compressed vapours and liquid pass to a heat interchanger and thence to a pressure distillate storage. -Fresh petroleum is also fed to the heat interchanger, the vapours evolved from the heating of this petroleum also pass to the above- mentioned compressor for cracking, and the unvaporised portion is stored and fed as required to the agglomerator.
The compressor is actuated by steam, the flue gases from the boiler are utilised as a source of heat in the baking
oven. W. N. Ho y t e.
Converting m ethane g a s into hydrocarbons of higher carbon content. Le Pé t r o l e Sy n t h e t i q u e
Soc. An o n., and A. Fo l l i e t (E.P. 261,267, 29.4.26).—
Methane is slowly raised to 950° by passage between two refractory walls, 1 mm. or more apart, arranged by having a central core of refractory material inside a hollow tube.
The gaseous products are then suddenly cooled to atmos
pheric temperature by means of a water cooler. The apparatus is maintained under a reduced pressure of 20 mm. of mercury by a pump. Using a natural gas containing 80% CH4, 6% H 2, 2*5% C 02, 2- 6% C3H 8. etc., 80% of the methane is converted into ethylene and olefines without the formation of naphthalene and tar.
A. C. Mo n k h o u s e.
Com plete gasification of bitum inous fuels in alternately-operated gen erators. H. St r a c h e(U.S.P.
1,611,842, 21.12.26. Appl., 6.8.21. Conv., 28.6.16).—
See E.P. 117,083; B„ 1920, 439.
D estructive d istillation of v in a sses. G. P. Guig
n a r d (U.S.P. 1,609,712, 7.12.26. Appl. 6.11.24. Conv., 9.11.23).—See G.P. 421,787; B., 1926, 304.
M ethod and apparatus for cracking and d is
tillin g o ils. M o t o r Fuel C o r p ., Assees. of C . F.
R i c h e y a n d P. Y. D u f f e e (E.P. 235,564,16.6.24. C o n v .,
9.6.25).—See U.S.P. 1,530,091 ; B., 1925, 492.
Apparatus for treating hydrocarbon o ils. J. P.
PERSCH,Assr. to M. E. Peksch(U.S.P.1.611,669,21.12.26.
A ppl., 22.11.20).—See E .P . 181,034 ; B., 1922, 580.
Apparatus for petroleum refining. C. Je f f e r s o n,
Assr. to Gr is c o m- Ru s s e l l Co. (U.S.P. 1,609,822, 7.12.26.
Appl., 25.1.21).—See E.P. 174,569 ; B., 1923, M0.
P rocess and apparatus for converting high- boiling oils or hydrocarbons into stable low -
boiling oils or hydrocarbons. D. L. Th o m a s (U.S.P.
1,611,615, 21.12.26. Appl., 24.4.19. Renewed 15.5.26).
—See U.S.P. 1,585,573; B., 1926, 623.
Charging horizontal gas retorts. F. G. Ma t t h e w s
and J. G. W . Al d r id g e (E.P. 262,625, 29.1.26).
Gas burners. Ra d ia t io n Lt d., H . J. Ya t e s, a n d
M. Ho w l e t t & Co. Lt d. (E.P. 262,659, 4.6.26).
Producing am m onium sulphate [from coal gas]
(E.P. 262,320).—See VII.
V iscosity m eter for testing the v isco sity of liquids [lubricating oils] (E.P. 262,652).—See I.
IH.—TAR AND TAR PRODUCTS.
Safety precautions in tar d istillation .—Rie h m
(Z. angew. Chem., 1927, 39, 1597—1599).—An account of the precautions usually observed against risks of fire and explosion in the distillation of ta r from pot-stills.
C. Ir w i n.
Determ ination of benzene in alcohol solution.
W . R. Or m a n d yand E. C. Cr a v e n (J. Inst. Petrol. Tech., 1926, 12, 636—649).—A rapid method has been devised for the determination of benzene in solution in alcohol of 95% strength and upwards, accurate to about 2%
of the benzene present. A mixture of 50 c.c. of the solution with 5 c.c. of petrol, previously shaken with sulphuric acid to remove aromatic compounds, is shaken first with 150 c.c., then with 25 c.c. of 20% sodium chloride solution or with water, the aqueous layer being run off in each case. The percentage of benzene in the alcohol is approximately proportional to the difference between the refractive index of the residual hydrocarbons and those from a blank test using alcohol free from benzene. Preliminary notes are given on the application of the method for the determination of petrol in alcohol, and methods are discussed for the deter
mination of the water content of alcohol-benzene mix
tures. L . A. Co l e s.
R em oval of tar from producer and coke-oven gas b y electrostatic precipitation. We y l.—S e e II.
Volum etric determ ination of arom atic hexa- hydro-hydrocarbons in tar d istillates. Da nAi l a a n d St o e n e s c u.—S e e II.
Pa t e n t s.
M anufacture of asphalt or like su bstan ces in finely-divided condition. N.V. d e Ba t a a f s c h e Pe t r o l e u m Ma a t s c h a p p i j, and F. R. Mo s e r (E.P.
245,418, 26.10.25. Conv., 2.1.25).—A stable “ asphalt gel ” proof against further coagulation is prepared by adding finely-divided substances to an emulsion of asphalt, tar, or pitch. These substances may be coagulating agents or, alternatively, an electrolyte is added simultaneously with the finely-divided material.
Thus 1000 kg. of petroleum asphalt are emulsified so th a t the emulsion contains 50% of water ; it is then mixed with 5 kg. of caustic soda and stirred into 1000 litres of a solution containing 5 kg. of crystalline aluminium chloride. Coagulation takes place, and the viscous gel is easily separated from excess water. The asphalt thus prepared is homogeneous and finely divided, and can be stored without further coagulation. S. Pe x t o n.
B r itis h C h em ica l A b s tr a c ts—B .
Cl. I V . — Dy e s t u f f s a n d In t e r m e d i a t e s. 1 0 1
Production of liquid fuel m ixtu res (E.P. 261,907).—
See II.
IV.—DYESTUFFS AND INTERMEDIATES.
M icroscopical tests for certain naphthalenesul- phonic acids. W. Ga r n e r (J. Soc. Dyers and Col., 1927, 43, 12—13).—Two drops of a 40% solution of sulphate or chloride of zinc, magnesium, nickel, copper, iron, or manganese are mixed on a microscope slide with 3—4 drops of a 50% solution of the sulphonic acid, the solvent is allowed to evaporate, and the resulting crystalline mass examined. Characteristic structures are given for Schaffer’s, naphthionic, Koch, and 2S
acids, whilst S, H, and J acids yield no useful results.
B . P . Ri d g e.
Sensitisation of photographic plates. Le s z y n s k i.
—See X X I.
Pa t e n t s.
Azo dyestuffs. Br i t i s h Dy e s t u f f s Co r p., Lt d., M . Me n d o z a, and K. H. Sa u n d e r s (E.P. 262,243, 13.11.25).—The substituted 2 : 4-diaminodiphenylsul- phones obtained from salicylic acid (or its homologues or substituted derivatives) according to E.P. 245,865
( B ., 1926; 233), especially 2 : 4-diamino-4'-hydroxy- diphenylsulphone-5'-carboxylic acid and its 3'-methyl- and 3'-chloro-derivatives, m aybe used as end components in the manufacture of dyestuffs. Examples are given of the preparation of the following derivatives of the first- mentioned sulphone : benzenesulphonic acid-i-azo-2 : 4- diamino-i'-liydroxydiphenylsulphone-b'-carboxylic acid; the benzenesulphonic acid-3-azo-compound; the naphthalene-l- sidphonic acid-i-azo-compound; the 3-nitrobenzenes-ulphonic acid-l-azo-compound ; the benzmesidplionic acid-2 : 5-di- (azo-compound) ; and the diphenyl-3 : 3'-dimlphonic acid- 4 : 4'-di-(azo-compound). The dyestuffs deepen from yellow towards blue with increasing complexity. The shades yielded on wool from an acid bath change on chroming, becoming a t the same time fast to milling etc.
Printed on cotton with a chrome mordant they yield shades fast to warm soap. B . Pu l l m a n.
Polyazo dyes and process of m ak ing sam e. E .P .
Hi t c h and F. H . Sm i t h, Assrs. to E. I. d u Po n t d e Ne m o u r s & Co. (U.S.P. 1,610,946, 14.12.26. Appl., 10.10.23).—Two mols. of tetrazotised benzidine are coupled with 1 mol. of 1 : 8-aminonaphthol - 3 : 6 - disulphonic acid, the product is then coupled with 1 mol.
of another component, and the remaining amino-group converted into a stable inorganic group. A. J . Ha l l.
Manufacture of dinitrotoluene. Br i t i s h Dy e- s t u f f s Co r p., Lt d., E . H. Ro d d, and R . W . Ev e r a t t ( E .P . 263,018, 12.5.26).—Mixtures of dinitrotoluenes which remain liquid below 20° are prepared by nitrating mixtures of nitrotoluenes containing less than 45% of the »t-compound, crystallising the liquid product a t a suitable temperature, and removing the solid matter.
E.g., 685 pts. of nitrotoluene containing 33% m-, 32% p-, and 35% o-compound are nitrated during 3—4 hrs. at 40—50° with a mixed acid composed of H 20 5-7% , H N 0 3 24 • 3%, and H 2SO,j 70%. After stirring for 3 hrs.
longer a t 55—60°, the dinitrotoluene is separated in the usual way, washed free from acid, and dried by heating a t 80° for a few hours. I t is then crystallised by stirring
a t 18—20° for 24 hrs. The product is filtered or centri
fuged, and thus yields 380—430 pts. of an oil of setting- point below- 0° and 450—490 pts. of a solid of setting- point 54—60°. If the crystallisation is carried out a t 25°
for 24#hrs., 500 pts. of an oil of setting-point 18—20°
are obtained, and the solid melts a t 56—58°. (C f. E.P.
17,128/13 ; B ., 1914, 890.) A. Da v id s o n.
M anufacture of nitro-derivatives of arom atic am in es. J. W. Le i t c h & Co., Lt d., and A. E . Ev e r e s t
(E.P. 261,459, 13.8.25).—Dinitro-derivatives of o- and p-toluidines, p-chloroaniline, and aniline are prepared by treatm ent of the arylsulphonyl derivatives of these amines, or their mononitro-derivatives, with dilute nitric acid in excess, followed by hydrolysis of the products with sulphuric acid. E.g., 70 g. of water, 26-1 g. of p-toluenesulpho-o-toluidide. and 25" 2 g. of nitric acid (100% = 4 mols.) are mixed and heated slowly, with stirring, to 85°. The reaction which occurs further raises the temperature, which is then kept a t 100° for several hours, the final product being a greenish-yellow flocculent mass. After cooling, this is filtered off and washed. By heating this with sulphuric acid (2 pts.) followed by dilution with water, p-toluenesulphonic acid is split off and 3 : 5-dinitro-o-toluidine is obtained.
A . Da v i d s o n.
M aking aniline and other a rylam in es. W. J.
Ha l e and J. W. Br i t t o n, Assrs. to Dow Ch e m ic a l Co.
(U.S.P. 1,607,824,23.11.26. Appl., 5.2.25).—Aryl halides react with ammonia in the presence of a copper compound and metallic copper. B . Fu l l m a n.
Producing n itriles of the benzanthrone series.
Ka l l e & Co., A.-G. (E.P. 243,026, 17.11.25. Conv., 17.11.24).—Halogenated benzanthrones are acted on by cuprous cyanide. E.g., a mixture of 8 pts. of bromo- benzanthrone (E.P. 20,837/06 ; B., 1907,756) and 2 - 6 pts.
of cuprous cyanide is heated a t about 200—210° for some hours. The powdered melt is extracted with hot nitrobenzene, from which, on cooling, cyanobcnzant krone, m.p. 243—244°, crystallises. Fusion of the nitrile with caustic alkali or sodamide produces dark bluish-violet
vat dyes. A. Da v id s o n.
Manufacture of vat dyestuffs of the isodibenz- anthrone series. Ba d i s c h e An i l i n- u. So d a- Fa b r.
(E.P. 242,620, 26.10.25. Conv., 7.11.24).—Benzanthrone- 3-thio-ethers (alkyl or aryl, the latter including antlira- quinonyl, benzanthronyl, and the like) containing a free 4-position are acted on by alkaline condensing agents in the presence or absence of inert diluents.
E.g., to a melt of 80 pts. of potassium hydroxide and 80 pts. of alcohol, previously heated to 135°, while distilling off excess of alcohol, 20 pts. of benzanthrone- 3-y-thiocresyl ether are added while keeping the tem perature a t 135—140°. After stirring for 1 hr. more at 140—145°, the melt is diluted with water, and air is passed to precipitate the dye, which is i’sodibenzaiithrone practically free from dibenzanthrone. The same pro
duct can also be obtained from benzanthronyl-3:3 -
sulphide. A. Da v id s o n.
Manufacture of isodibenzanthrones. J. ^
s o n. From Ba d i s c h e An i l i n u. So d a Fa b r. (E.P. [a j
261,888 and [b] 262,030, 9.10.25).—(a) ife-Halogenc^
benzanthrones containing a free 4-position are convert«;
B r itis h C h e m ic a l A b s tr a c t*—B .
102 Cl. V.— F i b r e s ; T e x t i l e s ; C e l l u l o s e ; P a p e r .
a t comparatively low temperatures into isodibenzan- thrones by the use of mixtures of caustic alkalis and alkali alkoxides in presence of inert diluents.
Instead of alcohols, substances such as benzaldphyde capable of forming alcohols by the action of caustic alkali may be used. Air should be excluded during the condensation. E.g., 30 pts. of isopropyl alcohol are added to a stirred mixture a t 10—15° of 200 pts. of benzene, 70 pts. of potassium hydroxide, and 10 pts. of pure Z?z-chlorobenzanthrone, air being excluded. The ben
zene and alcohol are expelled by steam and the residue is vatted a t the boil with hyposulphite. The v at is filtered and the dye precipitated by a current of air.
(b) As condensing agents for the same purpose, metal compounds of aromatic amines in presence of an inert diluent may also be used. E.g., to a solution a t 15°
of 8 pts. of sodium in 400 pts. of aniline are added all a t once 40 pts. of chlorobenzanthrone (E.P. 20,837/06 ; B., 1907, 756). The temperature rises to about 25°, and stirring is continued a t this point for 1—2 lirs.
The dye is isolated, e.g., by pouring the mass into dilute acid and filtering. I t dyes vegetable fibres reddish- violet. The sodium may be replaced by other metals such as calcium, magnesium, or potassium. jBz-halo- genobenzanthrones containing, in addition, halogen atoms in other positions may also be used, such as the dichlorobenzanthrones made by chlorinating (in the Zfe-nucleus) 8- and 10-chlorobenzanthrones.
A. Da v id s o n.
Interm ediates, dyes, and d yeing. J. E. G. Ha r r i s,
B. Wy l a m, J. Th o m a s, and Sc o t t is h Dy e s, Lt d. (E.P.
261,139, 1.5.25).—The process of E.P. 247,787, 251,491, and 260,638 (B., 1926,403, 625 ; 1927, 39) is extended to quinones in general, so as to yield quinone derivatives soluble in water, and capable of conversion into the original quinones by treatm ent with acid oxidising agents.
When applied in particular to a number of anthraquinone derivatives which have hitherto been regarded as inter
mediates for, bu t not in themselves, dyestuffs, the derivatives so obtained may be used for dyeing or impregnating fibres, on which by treatm ent with .acid oxidising agents the parent anthraquinone derivatives are then regenerated. Examples are given of the preparation of derivatives from anthraquinone, 1 :4 - di-p-tolylaminoanthraquinone, 1-methylaminoanthra- quinone, 1 : 4-dimethyldiaminoanthraquinone, etc.
A. Da v id s o n.
Manufacture of interm ediate products [2 : 3 - hydroxynaphthoic arylides] suitable for the pre
paration of azo d yestuffs. Br i t i s h Sy n t h e t i c s, Lt d., and E. B . Hi g g i n s (E.P. 262,958, 28.12.25).—
The reaction between 2 :3-hyclroxynaphthoyl chloride and an aromatic amine containing no electronegative sub
stituent can be made practically quantitative as regards both amine and chloride by vigorously mixing the two substances in presence of water and a slight excess of weak alkali. The mixing of the components may be done in varying order, and the acid chloride m aybe used in solid form or in solution in an indifferent solvent.
E.g., to a paste of 93 g. of aniline with 100 g. of sodium bicarbonate and 50 g. of water a suspension or solution of 206-5 g. of 2 : 3-hydroxynaphthoyl chloride in 200 g.
of' benzene is slowly added with efficient stirring or
grinding, the temperature not exceeding 60°. After stirring for J hr. more, 100 g. of water are slowly added and the benzene is driven off by steam. The mass is then neutralised to phenolphthalein by adding hydro
chloric acid, and the anilide washed and dried. The yield is 97% or more. Alternatively, the chloride may be added to a mixture of the amine and alkali, followed by water, or a mixture of the chloride and the amine is added to the alkali and water. A. Da v id s o n.
Production of vat dyestuffs. D . G. Ro g e r s, Assr.
to Na t. An i l i n e & Ch e m i c a l Co., In c. (U.S.P. 1,609,965, 7.12.26. Appl., 17.6.21. C f. G.P. 331,283; B., 1921, 294).—iV-Dihydro-l: 2 ': 2: l'-anthraquinoneazine is pre
pared by gradually adding about 30 kg. of potassium hydroxide to a mixture of about 200 litres of mineral oil and 40 kg. of p-aminoanthraquinone a t about 220—
225°, raising the temperature to about 230°, and allowing the water vapour evolved to escape. A. Da v id s o n.
Dibenzanthronyl product. D yestuffs and inter
m ediates. R. E. Th o m s o n and J. Th o m a s, Assrs.
to Sc o t t is h Dy e s, Lt d. (U.S.P. 1,607,491—2, 16.11.26.
Appl., 20.2.26. Conv., 21.10.24).—See E.P. 251.313;
B., 1926, 576.
V.—FIBRES; TEXTILES; CELLULOSE; PAPER.
Am idated cotton. P. Ka r r e r and W . We h r l i (Z.
angew. Chem., 1926, 39, 1509—1514).—Cotton and other cellulose materials, when treated with ammonia, yield a fibre containing 1—3% N , the reaction either being the substitution of an amino-group for a hydroxyl group, or partial oxidation of the cellulose, and such amidated yarns are dyed directly with acid dyes. A so- called “ immune ” yarn is prepared by the partial esterification of cotton with ^-toluenesulphochloride, it has considerable immunity to substantive dyestuffs, and can be treated with ammonia to form amidated yarn.
Instead of ammonia, organic basic nitrogen compounds can be used for the treatm ent of cotton or “ immune ” y a rn s ; e.g., aliphatic amines such as ethylamine or dimethylamine in aqueous solution give a yarn which can be dyed with tartrazine, cyanol, etc. Benzylamine gives a yarn with strong affinity for acid d y e s; molten urea, phenylhydrazine, piperidine, and also tertiary amines are applicable. The essential quality of amidated yarns is their smooth dyeing power with acid dyes, which is not shared by “ immune ” or ordinary cotton.
A list of suitable dyestuffs is given. W. G. Ca r e y.
Changes in the tenacity and elongation of artificial silk in the norm al and w et conditions. II. Y.
Ka m i (Cellulose Ind., Tokyo, 1926,2, 39—40).—The loss of tenacity of artificial silk is greater in boiling water than in water a t normal temperature, and the lossincreases as the time of boiling is prolonged. This increased loss is partly attributable to the expansion of occluded gas and the consequent disruption of the cohesive forces of the cellulose molecules ; the mechanical disturbance due to ebullition also plays a part. The elongation, with a few exceptions, is diminished in the same manner.
Drying the boiled silk a t a high tem perature has an injurious effect on tenacity and elongation, but if the m aterial be dried out in the air, not above 35°, the physi
cal characteristics are substantially restored to the original
