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at a high temperature, 170°-195° C., with oxygen in a pure state or a gas containing oxygen such as air.
PROCESS OF MAKING CAMPHOR. Lorenz Ach, of Mannheim, Germany, assignor to C. F. Boehringer & Soehne. Patent No. 802,792, dated October 24, 1905.
This invention relates to a process of producing camphor from isoborneol.
It has been common heretofore to oxidize isoborneol by means of acid solutions to produce camphor. It has also been proposed to oxidize borneol in an alkaline solution-namely, by acting upon it with a weak solution of permanganate in water. These methods, however, do not lead to a ready production of camphor. It is now found that the conversion of isoborneol to camphor can be done very easily and rapidly by the action of chlorin upon the isoborneol. In employing chlorin it may be used either in the gaseous state or in solution-for example, in water, carbontetrachlorid, chloroform. Upon leading chlorin gas over finely-powdered isoborneol a reaction takes place, the mass becoming warmer and hydrochloric acid being evolved. In order to moderate the reaction, the chlorin may be diluted with any suitable indifferent or inert gas—for example, air, carbonic acid—care being taken that the reaction proceeds in a moderate manner by exterior cooling, preferably to a temperature of about 30° C., and by a thorough mixing or stirring of the mass. The isoborneol instead of being used in a pulverized condition may also be employed in solution in any suitable medium-as, for example, benzene or chloroform. When working in aqueous solution, one can employ either the calculated amount of saturated chlorin water or a smaller quantity of water wherein the requisite weight of chlorin gas is gradually passed.
PROCESS OF MAKING CAMPHOR. Lorenz Ach, of Mannheim, Germany, assignor to C. F. Boehringer & Soehne. Patent No. 802,793, dated October 24, 1905.
On passing so-called “ gaseous nitrous acid”
over isoborneol the former rapidly absorbed, heat is liberated and the isoborneol gradually deliquesces. A mobile liquid is formed, which gradually becomes clouded by separation of water. On saturating the well-cooled liquid with the gas until a bluish-green coloration is attained and letting the liquid stand for a time a rise of temperature takes place and nitrous fumes are evolved. The product thus obtained consists of two liquid layers, of which the upper is a clear slightly-colored oil, the lower one consisting of a comparatively small quantity of aqueous fluid. The oil possesses the property of solidifying to a mass of crystalline comphor on mixing with water. The same reaction takes place when nitrous gases are passed over borneol. On this property of the two borneols is founded the process for the preparation of camphor from these materials. Its advantage consists in the fact that by it a good yield of camphor is attained, the same being pure and free from by-products. The amount of nitrous acid consumed during the process is comparatively small, inasmuch as the gases which escape from the liquid react with the atmospheric oxygen, regenerating nitrous acids, which may be reintroduced into the process. Instead of solid borneols a suitable solution of the same can be used employing as solvents—chloroform, ligroine, or ether.
PROCESS OF MAKING AMMONIA BY SYNTHESIS.
Herman Charles Woltereck, of Westminster, London, England, assignor to the Eschweiler-Woltereck Process Syndicate, Limited, of London, England. Patent No. 803,651, dated November 7, 1905.
This invention relates to the production of ammonia by synthesis, and has for its object to render the product cheaper and to increase the available supply.
The process consists in passing a mixture of air and a gascontaining hydrogen—such as coal-gas or water-gas—in about equal quantities and saturated with steam over iron oxid heated to a dull-red heat or other metallic oxid adapted to act as a carrier of oxygen. The oxid is advantageously disposed in such a manner as to offer the most intimate contact and largest surface to the mixture of gases employed. When coal-gas is employed, a quantity of organic amins is produced which may be destroyed to liberate the ammonia by passing the gases through boiling caustic solutions or over heated lime before absorbing the ammonia in acid in the ordinary manner.
PROCESS OF MAKING AMMONIA BY SYNTHESIS.
Herman Charles Woltereck, of London, England, assignor to the Chemicals Proprietary Company, Limited, of London. Patent No. 803,652, dated November 7, 1905.
This is an elaboration of the process described in U. S. Patent No. 803,651. It is now found that if air and steam only heated to a temperature between 300° and 400° C., and preferably to 350° C., are passed over iron (or other suitable element) offering a large surface and intimate contact ammonia is formed in considerable quantities, while the iron, &c., is oxidized. It is preferable that the iron or other contact material should also be heated to the temperature required to prevent loss of action by cooling. The formation of ammonia decreases with the progress of the oxidation of the contact material; but it is possible to hold the oxidation in check by the admixture of a small quantity of a reducing-gas, such as carbon monoxid or hydrogen or of gases containing either or both of same, to the air and steam used, and to thus insure the continuity of the process. The gases may be mixed prior to their entering the reaction tube or chamber containing the iron, (or other suitable metal,) or they may be separately introduced and allowed to mix in the reaction tube or chamber itself. The air and reducing-gas may be first passed and the steam afterward over the iron or other suitable metal. Any oxygen-carrier metal is a suitable metal, and although iron has yielded the best results almost as good results are obtained with bismuth and chromium.
PROCESS OF MAKING AMMONIA BY SYNTHESIS.
Herman Charles Woltereck, of London, England, assignor to the Chemicals Proprietary Company, Limited, of London. Patent No. 803,653, dated November 7, 1905.
This process is based on that described in U. S. Patent No. 803,651.
It is now found that if air and steam only, heated to a temperature between 300° and 400° C., and preferably to 350° C., are passed over iron, (or other suitable element,) offering a large surface and intimate contact ammonia is formed in considerable quantities, while the iron, &c., is oxidized. It is preferable that that the iron or other contact material should also be heated to temperature required to prevent loss of action by cooling. After the operation has proceeded for some time the action decreases and the iron or other metallic oxid formed has to be reduced again by the introduction of a suitable reducing agent, such as carbon monoxid, hydrogen, or gases containing either or both of the same. This reducing operation has to be repeated from time to time. The gases may be mixed prior to their entering the reaction tube or chamber containing the iron (or other suitable metal) or they may be separately introduced and allowed to mix in the reaction tube or chamber itself. The air may be first passed and the steam afterward over the iron or other suitable metal. Any oxygen-carrier metal is a suitable metal, and although iron has yielded the best results, almost as good can be obtained with bismuth and chromium.
PROCESS OF MAKING HYDROSULPHITE PREPA
RATIONS. Rudolf Müller, of Höchst-on-the-Rhine, Germany, assignor to Farbwerke vorm. Meister, Lucius & Brüning. Patent No. 804,157, dated November 7, 1905.
The inventor has found that alkali hydrosulphite may be combined with acetone, but that stable preparations may be obtained only if the hydrosulphites are brought together with ketones, such as dimethyl and ethylmethylketone, in presence of alkali and preferably simultaneously with ammonia. The solutions thus obtained may be concentrated in a vacuum at a low temperature, whereby products are obtained which are stable for a considerable time. They may be usefully employed for discharging purposes, such as the discharge of naphthylamin-bordeaux.
PROCESS OF MAKING AND SEPARATING HYDRO
CHLORIC AND SULPHURIC ACIDS.
Paul Askenasy and Martin Mugdan, of Nuremberg, Germany. Patent No. 804,515, dated November 29, 1905.
It is known that the reaction of chlorin and sulphurous acid in water results in the formation of hydrochloric and sulphuric acids.
The production and separation of hydrochloric acid and sulphuric acid by utilizing this reaction are carried out in the following manner: In a suitable chamber or tower which is preferably filled with stones and in which pure or diluted sulphurous acid (pyritic gases) and chlorine are introduced at the bottom, only so much water is introduced from above as corresponds with the quantity of gaseous hydrochloric acid and concentrated (sixtyfive to eighty per cent.) sulphuric acid produced. The reaction continues until the remainder of the gases is consumed, when the reaction substances are allowed to act upon each other for a sufficient length of time, which can be attained by varying the proportions of the reaction-chamber according to requirement. At the commencement of the process a violent reaction takes place at the point where the gases come into contact with the current of liquid, which produces a mixture of aqueous hydrochloric acid and sulphuric acid. This mixture sinks in the reaction-chamber and comes into contact with fresh quantities of the gas mixture, thus forming fresh quantities of acid until finally a saturated solution of hydrochloric and sulphuric acid is formed. As soon as this point has been attained the sulphuric acid then formed by the