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BRITISH CHEMICAL ABSTRACTS

B.—APPLIED CHEMISTRY

A U G . 3 1 , 1928.

I.— GENERAL; P U N T ; MACHINERY.

Indicating equipment for industrial p H m easure­

m ents. H . C. P a r k e r (Ind. Eng. Chem., 1928, 2 0 ,

676—680).—When the concentration of acid or base exceeds 0-1% conductivity measurements are preferable to pj{ measurement, provided the concentration of salts remains fairly constant. Tables are given for converting voltages into p u values for hydrogen and quinhydrone electrodes at various temperatures. For many industrial purposes, however, the voltage is sufficient. The quin­

hydrone electrode becomes inaccurate above pit 8-5, and above p n 10 the hydrogen electrode should always be used. Three types of complete p H indicators operating either or both of these cells are illustrated. Directions are given for making up the calomel cell and preparing the hydrogen and quinhydrone electrodes. The accuracy aimed a t is 0-05 p u unit. C. I r w i n .

Pfund colour grader. W i l l a m a n . See XVII.

Pa t e n t s.

Shaft furnace, gas producers, etc. S t e t t i n e r C h a m o t t e - F a b r . A.-G. v o r m . D i d i e r , and E. T e r r e s

(B.P. 292,052, 1.3.27).—The steam from the water- jacket of the furnace described in B.P. 284,639 (B., 192S, 352) is superheated by means of the gases from the same furnace, after they have passed through a dust-settling

chamber. B. M. V e n a b l e s .

Device for charging furnaces. W o o d a l l - D u c k i i a m

(1920), L t d . , A. S c o t t , and S . N. W e l l i n g t o n (B.P.

292,278, 28.3.27).—A hopper for charging loose and bulky material to a shaft furnace is caused to rotate, and is provided with a helical vane or flange on its interior surface. B. M. V e n a b l e s .

[Open-hearth] furnace. A. G. Eg l e r (U.S.P.

1,674,167, 19.6.28. Appl., 25.10.26).—A t each end of the hearth is situated a bridge wall which contains a gas port and an air chamber above the bridge w a ll;

the air and gas uptakes are formed within a wall sloping downwardly and outwardly from the above-mentioned

ports. B. M. Ve n a b l e s.

Heat exchanger. M. M a u r a x , Assr. to M a t h i e s o x A l k a l i W o r k s , I n c . (U.S.P. 1,673,918, 19.6.28. Appl., 8.11.24).—Twin spiral passages are formed between double-spiral fins formed on a central body; the outer edges of the passages are closed by spiral ribbons.

B. M. V e n a b i .e s .

Heat exchangers for use in catalytic apparatus.

S y n t h e t i c A m m o n ia & N i t r a t e s , L t d . , a n d F . H.

B r a m w e l l (B.P. 292,404, 27.10.27. A d d n . t o B.P.

241,817 ; B ., 1926, 12).—T h e h e a t e x c h a n g e r o f t h e p r e v io u s p a t e n t , c o m p r is in g d o u b le c o n c e n tr i c t u b e s

wound into a spiral, has the single inner tube replaced by 3, 7, or other number of smaller tubes.

B. M. V e n a b l e s .

Circulating apparatus for heating ga ses. C h e m . T e c h n . G e s .m .b .H . (B.P. 285,475, 19.1.28. G e r.,

18.2.27).—In any apparatus using circulating hot gases, the burner for reheating the circulating gases is com­

bined with the circulating fan. A preferred arrangement is a burner tube concentric in the outlet of the centrifugal fan, in the annular space round the burner tube are dampers to regulate the amount of returned old gases, and the excess old gas is discharged from the fan casing at a point or points behind the burner tube.

B. M. V e n a b l e s .

Drying apparatus for rotary kilns. F . L u t h e r ,

Assr. to G. P o l y s i u s (U.S.P. 1,675,717, 3.7.28. Appl., 26.5.27).—A horizontal, rotary cylinder has wide, internal, longitudinal baffles, the free edges of which are flexible, in order to scatter the material as it falls from these edges. The baffles arc curved both longitudinally and transversely. F. G. C l a r k e .

Rectifying apparatus. W. A. P e t e r s , .tu x ., Assr.

to E. I. d u P o n t d e N e m o u r s & C o. (U.S.P. 1,673,373—4, 12.6.28. Appl., 28.4.23).—(a) The liquid distillate from a condenser, attached to a rectifying column, flows through an adjustable double weir device by which a part of the liquid is run back to the rectifier and part elsewhere. (b) A rectifier is heated by steam at the lower part thermostatically controlled by the temperature higher up the column. A collecting tank for condensate is provided, and increase of the level of liquid in this decreases the supply of feed liquor and vice versa.

B. M: V e n a b l e s .

M achinery for grinding, m ixin g and like opera­

tions. J. H. J. W o o d (B.P. 291,952, 7.6. and 19.8.27).

—A. rotor revolves concentrically within a cylindrical housing. The rotor is formed with deep longitudinal flutes within which are imprisoned loosely grinding bars of various shapes of cross-section. The output and fineness are a function of the width and length of the annular grinding space. B. M. V e x a b l e s .

Pulverisers. C. E. B r a i x a r d (B.P. 288,227,15.11.27.

U.S.,8.4.27).—A cylindrical mill is provided with grinding medium comprising a cylindrical roller subdivided into segments which may or may not fit exactly together.

Feed or discharge is through hollow trunnions and the mill is lined with hard steel on all interior surfaces.

B. M. V e n a b l e s .

Centrifugal m ills for the grinding, m ixin g, em ulsification, and incorporation of solids and liquids, or liquids. C. P. W a l k e r (B.P. 291,957, 13.6.27).—Two discs, one or both rotating, are provided

627 o *

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B r itis h C h em ical A b s tr a c ts —B .

6 2 3 Cl. I I . — Fu e l; Ga s; Ta b; Mi n e k a l Oi l? .

with intercalating pins or blades, and the material is forced through the casing from the circumference imvards, i.e., against centrifugal force. The blades may be sloped to promote, oppose, or be neutral to the passage of the liquid, and a further retarding means such as a valve may be placed 011 the outlet.

B. M. Ve n a b l e s.

Centrifugal m achines. E. Kn u t t e l (B.P. 285,836, 21.2.28. Ger., 22.2.27).—A centrifugal separator, more particularly for finely-divided solids suspended in liquid, has its chamber or chambers formed in lenticular shape with an annular peripheral opening or slot of constant width. The slot is closed by a member which slides axially to the machine and is provided with grooves and projections which mate with the walls of tile chamber in such a manner th a t accumulated solids form a seal. There are preferably two chambers on one driving shaft, the slide being arranged to close oue and open the other. B. M. V e n a b l e s .

Separating or cleaning interm ixed divided m aterials. K. D a v i s (B.P. 292,179, 13.12.26).—A perforated table through which air is blown with velocity decreasing in the direction of flow of the material is divided into zones of which the area is proportioned (a) to the proportion of impurities in any size ra n g e;

(b) to the above proportion plus the proportion th at size range bears to the whole q u a n tity ; or (e) to the above sum plus a further increase, the latter margin being greater in the finer sizes. B. M. V e n a b l e s .

Vacuum air separator. L. L i n d s a y (U.S.P.

1,675,941, 3.7.28. Appl., 14.1.25).—The separator con­

sists of a series of conical separating units connected in series, a grinding apparatus, and a blower, and has means for admitting gas to the upper zone of each separating uuit, and for returning a portion of gas from the last unit to the grinding apparatus.

W, G. C a r e y .

Air classifier. A. H. St e b b i n s (U.S.P. 1,673,848, 19.6.28. Appl., 16.3.27).—An inclined cylindrical vessel is provided with longitudinal lifting blades and is rotated to shower the material within it. A current of air is produced up the incline by means of an external fan, and the air is simultaneously rotated by means of internal, separately driven, longitudinal fan blades having a large clearance between them and the blades on the wall of the rotating cylinder. B. M. V e n a b l e s .

Concentrator. A. H. S t e b b i n s ( U .S .P . 1,673,849, 19.6.28. Appl., 6.5.27).—The flow of pulp is constrained to flow downwards through a narrow annular passage between a container and bulging core. The heavier particles continue along the side walls of the container which then converge to a bottom outlet. The lighter particles flow inwardly away from the walls and are discharged through a central outlet passing through

the core. B. M. V e n a b l e s .

Strainers. A . E . W h i t e . From A n d a l e E n g i ­ n e e r i n g Co. (B.P. 292,236, 15.3.27).—A twin strainer with change-over valves is described. B. M. V e n a b l e s .

Purification of colloidal liquids, em ulsions, etc.

M. G. W. H u m m e l i n c k (B.P. 291,810, 8.12.26).—The liquid is filtered through cloth or wire mesh, the aper­

tures of which are large compared with the colloidal or suspended particles, at a rate which does not exceed 1 • 8 m./hr., arid under such conditions th at the deposit is not disturbed. B. M. V e n a b l e s .

Separation of gases or vapours from gaseous m ixtures. J . Y. J o h n s o n . E r o m I. G. E a r b e n i n d .

A.-G. (B.P. 292,204, 10.12.26).—Two or more adsorbents of different structures, one a t least having hydrophilic properties, and the first preferably having wide pores and successive adsorbents having fine pores, are used in the adsorption, e.g., of benzene from coal gas or of hydrocarbons from hydrogen chloride. Portions of the gaseous mixtures may also be separated by other means before or during adsorption, e.g., by compression, cooling, etc. [Stat. ref.] L. A. C o l e s .

Extinguishing fires. Ex c e l s io r Fe u e r i.o s c h g e r a.t e

A.-G., and 0. T r e i c h e l (B.P. 280,543, 7.11.27. Ger., 15.11.26).—Liquid carbon dioxide and liquid carbon tetrachloride are mixed and the crystallised double compound formed is applied to the fire. W. G. C a r e y .

Refrigerating apparatus of the absorption type.

H. D. F i t z p a t r i c k . From S. K. D. M. v a n Lier (B.P.

293,525—6, 18.5.27).

Refrigerant evaporators. B r i t . T h o j i s o n - H o u s t o n

Co., L t d . From G e n . E l e c t r i c Co. ( B .P . 293,556,22.6.27).

Heat-interchange device. C. R. H o u s e m a n , Assr.

to A i r R e d u c t i o n Co. (U.S.P. 1,677,777,17.7.28. Appl., 23.1.26. U.K., 28.1.25).—See B.P. 251,331; B., 1926, 616.

Producing in a solution the crystallisation of the body dissolved therein. A. D e l a s , Assr. to Soc. d e s C o n d e n s e u r s D e l a s (U.S.P. 1,677,551, 17.7.28. Appl., 25.7.25. Fr., 6.8.24).—See G.P. 412,968 ; B., 1925, 699.

Chemical apparatus (B.P. 293,077).—See X.

II,— FU EL; G A S; TA R ; MINERAL OILS.

Ignition of solid fuels. H. II. G r e g e r (Brennstoff- Chem., 1928,9,232—234 ; cf. B., 1927,864).—Apparatus for the determination of the ignition point of coke etc.

consists of a glass tube (diam. 20 mm.) containing the sample (10—20-mesh), and immersed in an iron crucible full of.sand in such a way th a t a current of air (1 litre/

min.) can be drawn down through the heated sand in the crucible and up through a short column of sand within the tube and finally through the fuel sample. In this way the temperature of the latter can be raised rapidly and regularly by internal heating. The ignition point is shown by a sudden acceleration in the rise of tempera­

ture registered by a thermometer, the bulb of which is immersed in the fuel sample. The ignition points deter­

mined vary from 296° for a wood charcoal to 690° for a metallurgical coke. The influence of some physical factors on the phenomena accompanying ignition is

discussed. A. B. M a n n i n g !

R eactivity of fu els. C. Q u i l l a r d (Compt. rend., 1928, 1 8 7 , 122—124).—I t is suggested that the velocity of luminous combustion in a vertical column of solid fuel may be taken as a measure of its reactivity. The reactivities of various fuels have been determined by burning in a current of oxvgen in a vertical quartz tube.

C. W. G ib b y .

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B ritis h C h em ica l A b s tr a c ts —B .

Cl. I I . — F i r E r . ; G .v s ; T a r ; M i n e r a l O i l s .

Formation of gaseous and liquid hydrocarbons by the action of steam and of alkali on sem i-coke under increased pressure. F. F i s c h e r and EL

P i c h l e r (Brennstoff.-Chem., 1928, 9 , 200—206).—W ien semi-coke, previously freed from tar by heating for 15 lirs. at 520°, is heated at 500° with water, preferably in the ratio 8 :1 , gas is evolved in quantity depending on the source of the so mi-coke; after 3 hrs. the yield may vary from 350 c.c. to 2830 c.c. The composition is, however, practically constant. Besides 33—13%

C 0 2 there are present about 20% H 2 and 40% CII4, the ratio of these constituents corresponding closely with th at calculated by Reinders (cf. B., 1928, 5) for

“ ideal ” water-gas produced at 380° and atmospheric pressure. The use of more water than 12-5% leads to a decreased yield of gas in which the hydrogen and methane contents are respectively increased and diminished. The use of less water also gives a lower yield of gas. When the reaction is continued longer than 3 hrs. the yield of gas is increased, but not proportion­

ally. This is due to a diminution in the reactivity of the semi-coke. The hydrogen and methane contents are, however, decreased and increased, respectively, by longer heating. The reactivity of the semi-coke remains low when the reaction mixture is reheated after removing the gas produced. No appreciable improvement is effected by adding more water or by drying the residual semi-coke in air or at 350° in vacuo before reheating.

Partly used semi-coke rapidly gives a large yield of gas, free from carbon dioxide, when heated with 5iV-potas- sium hydroxide solution. This can be repeated, whereby much gas, richer in methane and poorer in hydrogen, is obtained if more alkali is added, or less gas, poorer in methane and richer in hydrogen, if the residual mixture is merely reheated after removing the gas previously formed. In general, the gas so obtained is rich in hydrogen rather than in metha,ne. The addition of a large excess of solid potassium hydroxide gives a large yield of gas, free from carbon dioxide, and contain­

ing up to 44% of methane and 10% of higher gaseous hydrocarbons. A small yield (3—3-5%) of liquid hydrocarbons free from phenols is also obtained. Rubid­

ium, potassium, and sodium hydroxides in 52V-solution produce effects of the same order of magnitude. Am­

monia and milk of lime have but slight effect in promoting the reaction. Ammonium carbonate, ammonium sul­

phide, and sodium sulphide have no appreciable action ; sodium and potassium carbonate in lOA-solution produce an appreciable yield of gas, but are less effective than the hydroxides. Iron, nickel, ferric oxide, nickel sulphate, cobalt chloride, and nickel and cobalt hydr­

oxides are without influence on the reaction between semi-coke and water. W. S. N o r r i s .

Hydrogenation of coal in presence of catalysts.

B. I I l a v i c a (Brenustoff-Chem., 1 9 2 8 , 9 , 2 2 92 3 1 ).— The effect of the addition of some metallic oxides and chlorides on the hydrogenation (“ berginisation ” ) of coal has been studied, the experiments being carried out in a rotating autoclave of 1-8 litres capacity. The most effective catalysts were the oxides and chlorides of zinc, nickel, cobalt, and copper; compared with ferric oxide, they increased the ta r yield by 3 01 0 0 % , shortened the reaction time to about one third, and improved the

quality of the oil. They did not, however, permit any lowering of the optimum temperature or pressure. Their action affects primarily the splitting up of the coal

“ molecule ” and only secondarily the actual hydrogena­

tion process. A. B. Ma n n in g.

A rsa [Istria] coals. M. G. L e v i and C. P a d o v a n i

(Annali Chim. Appl., 1928, 1 8 , 245—272).—A note on the distillation and berginisation products.

Determ ination of w ater in com bustible m aterials by m eans of m agnesium m eth yl iodide. A.

T a u b m a n n (Z. anal. Chem., 1928, 74, 161—167).—The magnesium methyl iodide method of determining the moisture in combustible materials by measuring the volume of methane evolved on treating the pyridine extract of the sample with the Grignard reagent is shown to give excellent results with coal, coke, bituminous shales, peat, and petroleum products. Several deter­

minations can be carried out in 1 hr. and no heating is

required. A. R . P o w e l l .

Low-temperature carbonisation of lignites and sub-bitum inous coals. J. D . D a v i s and A. E.

G a l l o w a y (Ind. Eng. Chem., 1928, 2 0 , 612—617).—

Comparative assay tests a t low temperature were made on twenty-four American coals and lignites by the oil- shale method (cf. Gavin, B., 1923, 299 a ) , and those of Gray and King (B., 1921, 205 a ) , and of Franz Fischer (Z. angew. Chem., 1920,33,172). The oxygen content of the coals was above 19% and no coherence of the coke was observed. Only 6—20 gals, of tar per ton wore obtained, and though the gas was normal in quantity the quality was poor. Agreement between the assay results obtained by the three methods was not close, and whilst it is believed that all three methods may give reasonably accurate indications in the hands of experi­

enced wo:leers, a preference is shown for the Fischer

method. C. A. K i n g .

Problem s of the brown coal low-tem perature carbonisation process. P. R o s i n (Brennstoff-Chem., 1928, 9 , 182—184).—The problems awaiting solution, such as the increase in the output of the ovens, the carbonisation of finely-divided brown coal, carbonisation by retort or low-temperature carbonisation gas, dis­

posal and utilisation of the coke from brown coal, purification of the effluent liquors, the working-up of the tar with special reference to its dust content, and the use of the gas for long-distance supply systems, are discussed. A. E. M i t c h e l l .

Wood as fuel. L. A. W a n d e r l e y (Bol. Soc. Chim.

Säo Paulo, 1928, 1, 73—77).—Determinations were made of the calorific value and moisture content of the wood of Eucalyptus species and of native Brazilian trees. An attem pt to imitate practical conditions by removing 25% of the moisture before determination of the calorific value gave discordant results. Deter­

minations made on completely dried horizontal sections showed th at all the woods examined had sensibly equal calorific value—about 4700 kg.-cal./kg., independent of source or age. R. K. C a l l o w .

Applications of chem istry in gas-m aking. H.

H o l l i n g s (Gas J., 1928, 182, 924—935).—Examples are given in connexion with the free-carbon content of

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B ritis h C h em ical A b s tr a c ts —B.

030 Cl. II.— Fu e l ; Ga s ; Ta b ; Mi n e r a l Oi l s.

tars from various sources, with the light spirit recovered by stripping coal gas, and with the use of a waste-heat boiler as a meter for waste gases. Recent calculations of leakage from retorts, by use of waste-gas analyses, indicate how serious such losses may be, and further use of gas analyses is made in relation to study of the simultaneous production of coal gas and water-gas in vertical retorts. A relation has been found between the coal gas therm yield and the calorific value of the inert-free coal gas which is expressed in the form of a nomogram or a slide rule, and enables close study to be made of working results. Ammonia recovery is discussed in the light of new data on equilibria between foul gas and liquors of varying strength, and a system of fractional condensation based on these results is described, which reduces the volume of liquor to a minimum. In the manufacture of water-gas an approxi­

mate method for independent calculation of coke and oil figures is illustrated, and results obtained on the efficiency of oil cracking under different conditions are briefly mentioned. R. H. G r i f f i t h .

P ossib ilities of increasing the gas efficiencies in w ater-gas and producer-gas manufacture. J.

G w o s d z (Brennstoff-Chem., 1928, 9, 184—188).—The effect on gas efficiencies, from water-gas and producer- gas generators, of changing the working temperatures and pressures is discussed, with relation to the literature.

The possibility of increasing the reactivity of the coke by use of a suitable catalyst is also considered.

A . E . Mi t c h e l l.

D ust and m oisture control [in gas m a in s]. K. C.

T o m l i n s o n (Gas Age Rec., 1927, 60, 811—814, 817—

818).—Much of the dust in gas distribution lines is due to corrosion. The most corrosive constituent of the gas is hydrogen cyanide. Dehydration of the gas, or coating the pipe with oil, minimises the corrosion.

Ch e m ic a l Ab s t r a c t s.

G lass receiver for determ ination of benzene and benzines by m eans of active charcoal. A. W e i n d e l

(Brennstoff-Chem., 1928, 9, 234).—A U-shaped cali­

brated receiver of improved design is described for collecting the benzene distilled from active charcoal in a current of superheated steam. I t has been designed for use in conjunction with an apparatus for determining benzene in gas (B., 1927, 435). A. B. M a n n i n g .

Action of sulphuric acid on arom atic hydro­

carbons in connexion with their detection in petroleum . M. D . T i l i c h e v and A . I. D u m s k i (Neft.

Clioz., 1927, 13, 647—658).—Benzene, p-disubstituted benzene, and tetrasubstituted benzene are very resistant to sulphuric acid, but all other aromatic compounds present in petroleum are easily sulphonated; 95 • 6%

and 91—92% acid, respectively, are required. Fuming acid reacts with naphthenes. C h e m i c a l A b s t r a c t s .

Properties of sulphonic acids from petroleum products. A . D o b r j a n s k i and B. A n u r o v (Neft.

C’hoz., 1927, 13, 200—204).—Petroleum sulphonic acids are colloids. Salts of first-group metals, except copper, are soluble in w a te r: beryllium, zinc, cadmium, and mercury salts are appreciably soluble in hot water.

Arsenic, antimony, and bismuth do not form precipi­

tates. The acids are easily displaced from their aqueous solutions by salts and mineral acids.

Ch e m ic a l Ab s t r a c t s.

Composition of petroleum and its products.

G . A. B u r r e l l (Ind. Eng. Chem., 1928,20, 602—608).—

A review of the present state of knowledge of the more important phases of petroleum chemistry.

H. Ś. Garlick. Kerosenes from Grozni crude oil. A. I. V o r o n o v

(Neft. Choz., 1928, 14, 52—67).—Aromatic hydrocarbon contents of kerosenes are : Grozni 16, Baku 15, Emba 5, Maikop 29, California 7%. The 200—300° fraction is smaller in Russian than in Californian kerosene.

Ch e m ic a l Ab s t r a c t s.

Comparison of Soviet and foreign lubricating oils. II. S. S. N a m e tk i.\ and B. T. A r k h a n g e l s k !

(Neft. Choz., 1927, 13, 642—646).—Foreign oils are darker, have a higher carbon content, and have f.p.

from — 5° to — 19° compared with — 8° to — 18°

for Soviet oils. The latter are probably less readily oxidised a t high temperatures. C h e m i c a l A b s t r a c t s .

V iscosim etry of lubricating oils. I. Wo. O s t ­ w a l d and A. F o h r e (Kolloid-Z., 1928, 45, 166— 179).—

Measurements of the viscosity of lubricating oils have been made a t various pressures between 7-5 and 103-0 cm. of water. Seventeen different mineral oils, having viscosities both greater and less th an th at of glycerol, were examined a t 25°, and with the exception of two Voltol oils, the Hagen-Poiseuille law was valid for each case. There is very little, if any, structure viscosity in the liquids examined, and the supposed similarity between lubricating oils and colloid systems is not borne out by these experiments. The Voltol oils have a smaller temperature coefficient than the other oils examined. In an examination of the influence of temperature on viscosity, good results were obtained by application of Schwedlielm’s formula, which may be generalised to the form z/G = where z and z' are the viscosities a t temperatures t and G is a constant for all oils and for the particular viscosi- meter employed, and H is a characteristic constant for

each oil. E. S. H e d g e s .

Degree of w etting of silica b y crude petroleum oils. F. E. B a r t e l l and F. L. M i l l e p . (Ind. Eng.

Chem.. 1928, 20, 738—742).—The “ adhesion tensions ” of different crude oils for silica are calculated from the results of experiments on the displacement of the oils from silica bv water (cf. B ., 1928, 1). The factors governing the removal of oil from oil-bearing sand by means of “ water-flooding methods are discussed.

S. S. W o o l f .

Tabulated an alyses of [319] representative crude petroleum s of the United States. N. A. C. Sm i t h

and E. C. Lane (U.S. Bureau of Mines Bull. 291, 1928 ; 69 pp.).

Organic com pounds and am m onia from water- gas. B r u t z k u s . —See III. S olu b ility of lubricating oil in liquid carbon dioxide. Q u i n n .—See VII.

Carbon blacks and rubber. G o o d w i n and P a r k .— See XIV.

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B r itis h C h em ica l A b s tr a c ts —B .

Cl. II.—Fu e l; G as; Ta r; Mi n b u a l Oi l s. 631

Pa t e n t s'.

Manufacture of briquettes. P. Ju n g (U.S.P.

1,675,272, 20.6.28. Appl.,’ 28.7.22. Ger., 24.5.21).—

A uniform mixture of a solid fuel with a small amount of a solid fuel material ground to a colloidal state of fineness is compressed in the form of briquettes.

A . B . Ma n n i n g.

Manufacture of liquid fuel. H. G. C. F a i r w e a t i i e r .

From A m e r . C o a i . i n o i l C o r p . (B.P. 292,673, 22.3.27).—

A solid fuel is finely powdered and the impurities are removed by froth flotation or agglomeration. The oil already admixed with the fuel in the cleaniug process, or, if necessary, additional oil added subse­

quently, is thickened by oxidation with air in order to produce a stable suspension of the fuel.

A. B. M a n n i n g .

Coking retort oven. J. B e c k e p ., Assr. to K o p p e r s

Co. (U.S.P. 1,675,687,3.7.28. Appl., 26.11.20. Renewed 18.6.26).—The regenerators of a coke-oven battery are arranged below and parallel with the coking chambers, and are grouped into pairs crosswise of the battery.

They are connected with the vertical combustion flues of the heating walls. Reversing valve connexions are provided between a producer-gas main and alternate pairs of regenerators, and between the intermediate pairs of regenerators and the outer air. A pair of waste-gas tunnels is located on the same side as the producer-gas main, with valve connexions between one of the tunnels and the regenerators on the pusher side and between the other tunnel and the regenerators on the coke side of the oven. Controlling valves are provided for connecting one of the tunnels to the stack while the other is shut off therefrom.

A. B. M a n n i n g .

Wet process for extinction of coke. Soc. Gén. d e F o u r s à C o k e S y s t è m e s L e c o c q (B.P. 284,721, 3.2.28.

Belg., 5.2.27).—The hot coke is sprayed with water in a closed chamber, and the steam produced is passed through a second chamber wherein a water shower condenses part of it and removes the suspended coke

dust. A. B. M a n n i n g .

Manufacture of high-purity carbon. D. G a r d n e r

(B.P. 292,798, 2.8.27).—Carbonised material, e.g., wood charcoal, is ground to an impalpable powder, and is then washed successively with a hot alkaline solution (OJV-sodium hydroxide) and hot nitric acid (d about 1-33). The washed material is finally heated at 1000—1300°. The alkaline treatm ent may be omitted and the acid treatment then followed by fusion with sodium or potassium bisulphate and subsequently washing with water. Organic solvents also may be introduced into one or other of the washing treatments.

To protect the product against absorption of water it may be incorporated in turpentine, tetrachloroethane,

etc. A. B. M a n n i n g .

Manufacture of activated carbons and decoloris­

ing charcoals. J. v a n L o o n (B.P. 292,213, 10.3.27).—

Activated carbon is prepared by grinding charcoal, or other material containing carbon, a t a raised tempera­

ture, and, if necessary, under pressure, with a wetting agent, e.g., water, alcohol, benzene, etc., which has also

a solvent action on the substances other than carbon in the starting material. A. B. M a n n i n g .

Gas producer. E. G o u t a l and H. H e n n e b u t t e

(B.P. 266,353, 16.2.27. F r„ 16.2.26).—A producer designed for supplying internal-combustion engines has a hearth of relatively small dimensions. The oxida­

tion zone is provided with circularly disposed inlets for the injection of air, and is maintained as small as possible by the use of fuel of uniform character. The gas is enriched by the introduction of heavy oils into the reducing zone, which may be provided with a stack of refractory material to facilitate cracking. Steam may be injected into either or both zones. A. B. M a n n i n g .

Manufacture of coal gas. T. F. C a n n i n g and R. G.

C l a r k (B.P. 292,235, 15.3.27).—A plant for the car­

bonisation of coal comprises a number of horizontal or inclined retorts and a vertical chamber, the upper part of which is directly connected with the discharge ends of the retorts. The retorts and the lower part of the chamber are heated by gas from a separate producer.

The main carbonisation takes place in the retorts, the hot coke being then discharged into the vertical chamber, up which superheated steam is passed. The water-gas so produced passes through the retorts, assisting in the carbonisation of the charge and diminishing the cracking of the volatile products by sweeping them rapidly from the retort. The residual coke, cooled by the steam, is finally discharged from the lower end of the vertical chamber. If desired, oil for enriching the gas may be injccted into the chamber. A. B. M a n n i n g .

L ow-tem perature distillation furnace. J. P l a s s - m a n n (B.P. 275,546, 6.1.27. Ger., 5.8.26).—A large number of minor modifications are introduced into the design of the apparatus described in B.P. 240,800 (B., 1926, 228), including a distributing device for feeding the heating gas uniformly to the separate cells, insulated vertical return shafts for the outflowing heating gases, a staggered arrangement of the filling and discharging devices in the distillation chambers, with corresponding filling shafts fed from a distributing bunker, improved coke discharging and quenching arrangements, etc.

A. B. M a n n i n g .

Gasification of fuel. G. S z i k l a and A. R o z i n k k

(B.P. 274,110, 8.7.27. Ger., 9.7.26. Addn. to B.P.

255,857 ; B., 1927, 180).—The bottom of the gasifying chamber of the prior patent forms with the horizontal an angle smaller than the angle of rest of the incandescent fuel dust, so th a t the latter collects in the form of a crater surrounding the opening through which the air for combustion passes. Adjustable poking devices feed the settled dust towards the opening, which is provided with a slide v alv e; both valve and ¡joking devices may be automatically controlled by the load on the plant, e.g., by the boiler pressure if the plant is used for the production of steam power.

A. B. M a n n i n g .

D istillation of solid carbonaceous m aterial.

M. J. T r u m b l e (U.S.P. 1,674,420, 19.6.28. Appl., 11.9.23).—The material is preheated in a current of steam, then subjected to destructive distillation by passing superheated steam through it under pressure, and finally cooled in a current of saturated steam, the

(6)

B r itis h C h em ical A b s tr a c ts —B .

032 Cl. XI.— F u j t L ; Ga s ; T ab ; Mi n e r a l Oi l s.

l a t t e r b e in g t h e n r a is e d i n t e m p e r a t u r e a n d u t il i s e d in t h e f ir s t s ta g e o f t h e p ro c e s s . A. B. M a n n i n g .

if Separation of coke or half-coke from dry d istil­

lation gases. T r o c k n u n g s - , V e r s c i t w e l u n g s - , u . V e r g a s u n g s - G e s . m .b . H . (B.P. 285,387, 14.2.28. Ger., 14.2.27).—The separation of suspended coke dust from distillation gases, particularly in processes in which powdered coal is carbonised in a current of gas, is brought about by passing the dust-laden gas through a slot of which one wall remains stationary while the other moves. A convenient form of apparatus consists of a flat, cylindrical chamber in which a disc rotates.

The suspended particles are driven towards the stationary wall, where they collect and whence they can be dis­

charged by any suitable means. A. B. M a n n i n g .

Absorbing hydrogen sulphide or hydrogen sulphide and am m onia from ga ses. W . C a r p j i a e l .

From I. G. F a r b e n i n d . A.-G. (B.P. 292,669, 21.3.27).—

Coal gas, coke-oven gas, etc., after complete or partial removal of the ammonia, are scrubbed successively with

t h io s U lp h a te solution containing sulphurous acid and then with t li e polythionate solution obtained thereby mixed with sufficient of the previously recovered ammonia to maintain a neutral or weakly alkaline reaction in the liquor. Methods of working up the products and special applications of the process are described.

L . A . Co l e s.

Desulphurisation of gases. E. R a f f l o e r , Assr.

to W. E. L e u c h t e n b e r g (U.S.P. 1,672,778, 5.6.28.

Appl. ,11.6.26.).—A portion of the gas to be desulphurised is used to blow the powdered purifying agent into a chamber where it meets and mixes with the main current of gas. The mixture passes on to a separator, where the purified gas is freed from solid, e.g., by means of baffles and louvres, the solid being returned to the injector or renewed. C. H o l l i n s .

Production of carbon dioxide. F. H. K e l l i h e r

(U.S.P. 1,675,497, 3.7.28. Appl., 19.6.26).—Finely- divided carbonaceous material is burned, in the presence of sufficient air, to carbon dioxide in a closed furnace.

A pilston pump sucks the gas through a scrubber and settling chamber, and passes it to a separator and gas-receiver. The water removed from the gas in the separator is introduced into the top of the scrubber.

F . G. C l a r k e .

Burning of fuel. E . W. C l a r k e , Assr. to A m e r . 1 'a r P r o d u c t s Co. (U.S.P. 1,660,831, 28.2.28. Appl., 13.10.22).—Pulverised pitch is forced, by means of a blast of air, through a delivery nozzle situated outside the furnace, with such velocity th a t it is maintained in a compact stream at the point of entrance into the furnace, and finally reaches the combustion zone before

becoming adherent. F. R. Ennos.

Combustion apparatus. 0. B r u n l e r (B.P. 292,736, 25.4.27).—In order to prevent the flame travelling backwards within a submerged-flame burner an inter­

changeable reducing piece is inserted between the fuel valve and a bridge piece placed near the mouth of the burner. A. B. M a n n i n g .

Manufacture of liquid hydrocarbons and their derivatives, particularly those of low b.p. from

coal, tars, m ineral oils, etc. I. G. F a r b e n i n d . A.-G.

( B .P . 272,556, 13.6.27. Ger., 14.6.26).—The initial materials are treated with hydrogen a t a high temperature and under pressure, with or without a catalyst, in a current of the gas, preferably in closed circulation, in such large excess th at the partial pressure of the products of low b.p. does not exceed 10% of the total pressure.

A. B . M a n n i n g .

D istillation of em ulsified [mineral] oils. G . Eg-

l o f f and H . P . B e n n e r , Assrs. to U n i v e r s a l O i l P r o d u c t s S o . (U.S.P. 1,674,819, 26.6.28. Appl., 20.8.20. Renewed 24.4.28).—Oil containing emulsified water is distilled by applying heat to the upper surface of the oil in the still, progressively lowering the point of application of heat, and finally heating the still externally by means of a furnace. C. 0 . H a r v e y .

Continuous distillation and condensation of hydrocarbons. A. C l a r k e , Assr. to U n i t e d H y d r o ­ c a r b o n s Co. (U.S.P. 1,674,852, 26.6.28. Appl., 9.8.21).—

A mixture of gases and vapours, recovered by absorption, is removed from the absorbent medium by distillation and subsequently separated into a gaseous and a liquid fraction by compression and cooling. The vapours and gases are reheated and again passed to the compressing and cooling zones after combining with a further quantity of the vapours to be fractionated.

C . 0. H a r v e y .

Mineral eil still. A. E. P e w , j u n . , Assr. to S u n O i l Co. (U.S.P. 1,674,918, 26.6.28. Appl., 27.2.26).—

A horizontal cylindrical still is reinforced internally by circumferential beams connected by transverse members with a central longitudinal reinforcement.

C. 0 . Ha r v e y.

Refining low -boiling distillates of earth and m ineral o ils. S . S t r a n s k y and F. H a n s g i r g ( B .P .

267,959, 17.3.27. Austria, 18.3.26).—Hydrocarbon frac­

tions of low b.p. are freed from highly unsaturated compounds, which may cause resinification and bad odour, by treatm ent with about 5% of anhydrous aluminium chloride a t room temperature, the mixture being cooled if necessary to maintain the temperature below 35°. Very little loss due to polymerisation of non-objectionable hydrocarbons occurs. After separa­

tion of the aluminium chloride the product is fractionally

distilled. C. 0. H a r v e y .

Refining of liquid hydrocarbons. II. Wa d e.

From S i l i c a G e l C o r p . ( B .P . 292,231, 14.3.27).—

Gasoline, kerosene, benzol, etc. are refined by means of silica gel a t 121—149° to meet various specifications as follows: Removal of elementary sulphur is accom­

plished by the simple gel trea tm e n t; other sulphur compounds are removed by means of gel impregnated with up to about 1% of metallic oxides, such as those of copper and/or iron ; and for removal of gum-forming constituents the gel is impregnated with about 5%

by wt. of sulphuric acid. C. 0 . H a r v e y .

Fractionation of hydrocarbons. W . K. L e w i s and A. A. W e l l s , Assrs. to S t a n d a r d O i l D e v e l o p m e n t Co.

(U.S.P. 1,672,849, 5.6.28. Appl., 5.3.24).—Kerosene hydrocarbons are separated from a gas-oil distiliate by fractional distillation a t about 30 mm. pressure, the vapours being passed through progressively cooler zones

(7)

B ritis h C h em ical A b s tr a c ts —B .

Cl. I I I . — Or g a n i c In t e r m e d i a t e s. 633

w h e re t h e y m e e t a c o u n t e r c u r r e n t o f t h e c o n d e n s a t e p r o d u c e d in t h e c o o le s t z o n e s . C. Ho l l i n s.

Cracking of [petroleum ] oil. W. R. H o w a r d ,

Assr. to U n i v e r s a l O i l P r o d u c t s Co. ( U .S .P . 1,674,827, 26.6.28. Appl., 17.9.20. Renewed 24.4.28).—The oil to be treated is forced into the still by means of a steam pump situated inside the still. The exhaust steam from the pump discharges into the stili. C. 0. H a r v e y .

D istillation of oils w ith catalysts. G . L. P r i t c h a r d

and II. H e n d e r s o n , Assrs. to G u l f R e f i n i n g Co. (U.S.P.

1,672,339, 5.6.28. Appl., 28.11.21).—In the treatm ent of petroleum oils with aluminium chloride to obtai*

lower-boiling oils, the catalyst is more easily recovered in the earlier stages and long before its activity is ex­

hausted. Accordingly the treatment is stopped after 0-1—5 gals, of distillate have been obtained per lb. of aluminium chloride, and the latter (liquefied by the oil) is run off. A highly active aluminium chloride-oil mix­

ture can be recovered by distillation a t 200—300°.

C. H o l l i n s .

Apparatus for treating [cracking] hydrocarbon oils. F. E. We l l m a n (U.S.P. 1,672,668, 5.6.28. Appl., 20.3.23).—The oil is heated in a number of L-shaped tubes in a vertical, baffled furnace, the short limbs projecting laterally through the furnace walls, and the upper part of the long limbs being connected with several vapour drums outside the furnace. From the drums cracked vapour is drawn off to condensers, whilst liquid oil is recirculated to the short limbs of the L-tubes, from which residual oil is removed from time to time, and into which fresh oil is fed.

C. H o l l i n s .

T reatm ent of hydrocarbons. L. d e F l o r e z , Assr.

to T e x a s Co. (U.S.P. 1,674,390, 19.6.28. Appl., 4.8.22).

—Oil is vaporised and the vapours are passed through a cracking zone, the velocity of flow being progressively increased. The vapours remaining after reduction of the velocity of flow by expansion are condensed.

C. O . H a r v e y .

Clarification of benzine. J. J. Wacic(B.P. 292,433, 13.1.28).—In the regeneration of benzine used for dry- cleaning processes, the removal of fatty m atter is effected by centrifuging followed by saponification with a solution, into which it is sprayed, of sodium carbonate containing sodium chloride to assist demulsification and an alkaline hypochlorite. The alkaline solution is covered with a layer of viscous material such as glue, which acts as a filter and prevents any boiling of the benzine on the surface. C. 0. H a r v e y .

Regeneration or purification of lubricating o ils.

S w a n , H u n t e r , & W ig h a m R i c h a r d s o n , L t d . , and

H . J. Y o u n g (B.P. 292,300, 12.4.27).-—Oils drawn from the lubricating systems of internal-combustion engines, while yielding no indications of the presence of corrosive substances when examined by the usual chemical tests, were found to contain sulphuric acid and metallic sul­

phates detectable by digestion with caustic soda or potash. These substances are removed (or replaced by harmless substances) by contact with solids in suit­

able form consisting of metallic zinc, aluminium, or magnesium, and their alloys with one another or with calcium and/or sodium. C. O. H a r v e y .

Production of oxidation products from gaseous hydrocarbons. J . II. J a m e s , Assr. to C. P. B y r n e s

(U.S.P. 1,675,029, 26.6.28. Appl., 21.11.16. Renewed 28.3.25).—Products of incomplete combustion are obtained by passing hydrocarbon-oxygen mixtures (in which the proportion of the former is above the explosive limit) through a catalytic layer containing a compound of an electronegative metal of high m.p. and low atomic

volume. C. 0. H a r v e y .

Purification of m ontan w ax. J . Y. J o h n s o n . From I. G. F a r b e n i n d . A.-G. (B.P. 292,298, 8.4.27).—Crude or pretreated montan wax is separated from resin and fatty acids etc., and a product consisting of practically pure wax esters is obtained by extraction with hot glacial acetic acid. C. 0. H a r v e y .

B itum inous em ulsions. As p h a l t Co l d Mi x, Lt d.,

F. L e v y , and L . G . G a b r i e l (B.P. 292,251, 17.3.27).—

The procedure of B.P. 202,021 (B., 1923, 1013 a ) is modified by the substitution of a solution of an alkali silicate or borate for th a t of the hydroxide or carbonate.

A . B . Ma n n i n g.

[Apparatus for] burning of pulverised solid fuel or of atom ised liquid fuel. F. L. D u f f i e l d

(B.P. 293,330, 31.1.27).

Motor fuel. D . C o s t a g u t a (U.S.P. 1,677,273, 17.7.28. Appl., 1.6.25. Argentina, 10.3.25).—See F.P.

599,271 ; B., 1926, 430.

Working up acid resins obtained from the refining of m ineral oil derivatives into neutral bitum ens. C. S a u t e r m e i s t e r and F. W i l h e l m ( U .S .P . 1,677,731, 17.7.28. Appl., 19.12.25. Rumania.

30.6.25).—See F.P. 606,817 ; B., 1927, 182.

Separation of gaseous m ixtu res (B.P. 292,204).

Gas producers (B.P. 292,052).—See I. Road m aterials (B.P. 292,871).—See IX. Fuel for sm eltin g (B.P.

293,109).—See X.

III.— ORGANIC INTERMEDIATES.

Synthesis of organic com pounds and am m onia from w ater-gas w ithout catalysts. M. B p .u tz k u s

(Compt. rend., 1928, 1 8 7 , 124—125).—By compressing water-gas with air up to 50 atm. as much as 9% of the carbon monoxide can be converted into organic com­

pounds. Aldehydes and organic acids are obtained.

The yield of ammonia is very small. C. W. G ib b y .

Technical analysis of carbazole. E. S c h w e n k

and L. W a n k a (Z. anal. Chem., 1928, 7 4 , 168—187).—

A quantity of the substance containing 0-4—0-5 g. of carbazole is heated under reflux with 450 cic. of glacial acetic acid, and 50 c.c. of a mixture of 15 pts. of chromium trioxide, 10 pts. of water, and 10 pts. of glacial acetic acid are dropped in as rapidly as the reaction will allow.

The mixture is boiled for 1 hr. and distilled until 400 c.c.

of acetic acid have been collected (30—45 min.). The residual liquid in the flask is diluted with 1 litre of water, treated with 15 g. of granulated zinc and 300 c.c. of 30%

sodium hydroxide solution, and distilled with a vertical condenser until 300 c.c. of liquid have been collected in the receiver which has previously been charged with 50 c.c. of 0-liV-hydrochloric acid and 250 c.c. of water.

(8)

B r i t i s h C h e m ic a l A b s t r a c t s — B .

634 Cl. IV.—Dï e s t u t f s.

The excess of acid is then titrated as usual with methyl- red as indicator. The volume of acid neutralised by the ammonia multiplied by 0-01671 gives the weight of carbazole in the original substance. A. R. Po w e l l.

Determ ination of alcohol and ether. Ch e n e l.—

See X X II.

Pa t e n t s.

Manufacture of carbon disulphide. J . Y. Jo h n s o n.

From I. G. Fa r b e n i n d. A.-G. (B.P. 293,172, 26.5.27).—

Carbon disulphide and hydrogen or gases containing it are produced by treating hydrocarbons (especially gaseous ones such as methane) with gaseous compounds which supply sulphur under the working conditions (especially excess of hydrogen sulphide), a t high temperatures or in the electric arc, in the presence or absence of catalysts.

B. Fu l l m a n.

Production of m eth yl and other alcohols and preparation of catalysts therefor. Sy n t h e t i c Am m o n ia & Nit r a t e s, Lt d., and R. G. Fr a n k l i n (B.P.

293,056, 23.12.26).—Methyl alcohol etc. is made from carbon monoxide and hydrogen under pressure using a catalyst obtained by heating a mixture of basic zinc carbonate and basic chromium carbonate (70—80 atoms of Zn to 30—20 atoms of Cr). The basic carbonates are precipitated from a mixed solution of zinc and chromium salts which may be obtained by reduction of sodium dichromate with zinc in presence of an acid, or in a dichromate cell the negative pole of which is zinc.

W . G. Ca r e y.

Manufacture of form aldehyde. J . Y. Jo h n s o n.

From I. G. Fa r b e n i n d. A.-G. (B.P. 293,203, 13.7.27).—

The heat of the reaction products of the catalytic produc­

tion of formaldehyde from methyl alcohol and air is used to preheat the constituents of the reaction mixture separately ; they are mixed below the reaction tem ­

perature. B. Fu l l m a n.

Manufacture of unsaturated aldehydes. O. Y- Imray. From I. G. Farbenind. A.-G. (B.P. 284,458, 19.1.27).—An aldehyde containing no methylene group in the oc-position is condensed w ith an aldehyde of the ty p e R -C H 2-C H 0 in presence of alkali and an alcohol, any w ater present being in am ount insufficient to cause separation into la y e rs ; aldol form ation is thus pre­

vented. Benzaldehyde and propaldehyde w ith alcoholic potassium hydroxide a t 10° give an 86% yield of a-m ethylcinnam aldehyde. New unsaturated aldehydes described are /x-ethylcinnamaldehyde, b.p. 132— 134°/14 mm., oL-isoprapylcinnamaldehyde, b.p. 133— 135°/13 mm.,

■i-mctJwxy-'j.-cthylcimiamaldehyde, b.p. 169—172°/13 mm.,

■i-methoxy-ix.-n-amylcinnamaldehjde, b.p. 195— 200°/13 mm., / \ a-'f-ethyl-a.-n-amyloctenaldehyde, b.p. 150—155°/10 nun., &av-'{-elhyl-a.-ii-amyloctadienaldchyde, b.p. 150—

155°/10 mm., ¡\ay-8-phe?iyl -a.- cthylpenladienaldchyde [a-cinnam ylidenebutaldehydej, b.p. 172— 180°/12 mm., the corresponding a -methyl (m.p. 58°, b.p. 170—180°/15 mm.) and a-n-amyl (b:p. 203— 210°/15 mm.) compounds,

£yi't-'&-plienyl-o.'(-diinethylpentadimaide}iyde, m.p. 43°, b.p.

175— 180°/14 mm., an d ¿S.a'r-?i-phcnyl-y-methyl-y.-ethyl- pentadienaldchyde, b.p. 185— 190°/13 mm. The products liave a strong, pleasant odour. C. H o llin s .

Purification of carbazole. C. J. T h a t c h e r (U.S.P.

1,672,630, 5.6.28. Appl., 15.12.21).— Phenanthrene and

anthracene are removed from impure carbazole by treatm ent with warm carbon tetrachloride sufficient to dissolve the hydrocarbons but only a portion of the carbazole. To remove 10% of hydrocarbon, 800—1000 pts. of carbon tetrachloride at 50° are used for every 100 pts. of impure carbazole. C. Ho l l i n s.

Manufacture of paraform aldehyde. K . Sa t o rand

W . Pf a n n m u l l e r, Assrs. to I. G. Fa r b e n i n d. A.-G.

(U.S.P. 1,677,730, 17.7.28. Appl., 26.6.26. Ger., 2.7.25).—See B . P . 260,908 ; B ., 1927, 59.

1 - M ethyl-2 : 5 : 6-trichloro-3-am inobenzene-4- sulphonic acid. H . Wa g n e r and B. Vo s s e n, Assrs. to

Gr a s s e l l i Dy e s t u f f Co r p. (U.S.P. 1,677,536, 17.7.28.

Appl., 13.8.27. Ger., 11.9.26).—See B.P. 277,372;

B., 1928, 440.

Acetone and butyl alcohol (U.S.P. 1,672,487).—

See XVIII.

IV.— DYESTUFFS.

Constitution of Hansa Yellow 3G, 5G, and 10G (M.L.B.), and Perm anent Yellow R and 4R (A.G.F.A.). A. II. Bu r e and F . M. Ro w e ( J . Soc. Dyers and Col., 1928, 44, 205—207).—Hansa Yellow 3G, m.p.

250°, is 4-chloro-2-nitroaniline —)>- acetoacetanilide (cf.

B.P. 9633 of 1910); the 5G mark is o-nitroaniline — acetoacetanilide, and has m.p. 206°; the 10G mark is 4-chloro-2-nitroaniline acetoacetic o-chloroanilide (B.P. 23,791, 1911), and has m.p. 258°. Acetoacetaryl- amide couplings give much less diazo compound when treated with fuming nitric acid than do other azo couplings.

Permanent Yellow R, m.p. 263°, is o-chloroaniline —)>- l-j>-mtrophenyl-3-methyl-5-pyrazolone (U.S.P. 988,870), the coupling component, m.p. 222°, being made from p-nitrophenylhydrazine. The 4R mark, m.p. 188°, is o-chloroaniline —^ l-phenyl-3-methyl-5-pyrazolone.

C. Ho l l i n s.

Azoic colours. Ra t h. Effect of sulphur dioxide on azo d yes. Ki n g.—See VI. P igm en ts and lakes.

Gr e e n.—See X III.

Pa t e n t s.

Manufacture of thiom orpholines of the anthra- quinone series. I. G. F a r b e n i n d . A.-G. (B.P. 263,179 and Addn. B.P. 263,843, [ a ] 17.12.26, [ b ] 29.12.26.

Ger., [ a ] 17.12.25, [b ] 29.12.25. [ a , b ] Addn. to B.P.

263,178 ; B., 1928, 398).—( a ) The o-amino-(3-hydroxy- alkylthiolanthraquinones of B.P. 263,178 are converted by acid condensing agents (oleum, sulphuric acid, zinc chloride) into thiomorpholine derivatives which are dyes for acetate silk. Examples are : the condensation products from l-amino-2-[3-hydroxyethylthiolanthra- quinone (red), l-amino-2-Py-diliydroxypropylthiol- anthraquinone (red sulphonated dye), 3-chloro-l : 4- diamino-2-p-hydroxycthylthiolanthraquinone (blue), 1 : 5-diamino-2 : 6-di-p-hydroxyethylthiolanthraquinone (bordeaux-red). (b) Similar morpholine derivatives are obtained by condensing l-amino-2-thiolanthraquinone with ethylene dihalides and cyclising the product by heating, e.g., at 100° or in trichlorobenzene with addition of copper. Examples are : ethylene dibromide, chloro- bromide, or dichloride, or Py-dichloropropyl alcohol with

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