US1207416A - Process for manufacturing nitrogen compounds. - Google Patents

Description

I E. KOCHENDOERFER.

PROCESS FOR MANUFACTURING NITROGEN COMPOUNDS.

APPLICATION FILED MAR. 26. I913.

-Pateni7ed like. 5, 19M.

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PROCESS FOR MANUFACTURING NITROGEN GOMPOUNDS.

Specification of Letters Patent.

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Patented, Dec" 51 It Application filed March 26, 1913. Serial No 756,864;

lit has particular relation to the well known cyanization of certain gases, resulting from the carhonization of distillers' wash and the like, by means of overheating. Said gases have a conside'ahle content of nitrogen, which renders them very valuable for the manufacture of nitrogen compounds, such as cyanogen compounds and ammonia.

There are quite a number of processes for such manufacture, but these processes are not sufliciently satisfactory because the yield of nitrogen compounds is considerably be low that to he expected on theoretical cal culations. In my U. S. Letters Patent, No. 1,165,358, patented Dec. 21, 1915, entitled Processes for manufacturing nitrogen compounds, I have pointed out in a rather detailed way such gases as result from the carbonization of distillers Wash and these gases are hereinafter simply called gas es.

In the present state of the art of cyanizing gases generated by the carhonization of dis-- tillers wash and other like gases by super heating the same, little attention has been paid either to the material or to the surfaces ofthe channels through which the gases are passed to he superheated. l have discov cred, however, that in the art of cyanizing such gases, due attention must be given to the material of which the channels are made and that the economy of the cyanizing process is considerably reduced if the surface of the channels is rough and porous. l have furthermore discovered that this injurious effect caused by'the rough. and porous surfaces of the superheater-channels.may he counteracted by increasing the speed of the gases through the channels in such a way that each of the molecules of gas is in con-- tact with the rough and porous surfaces for only a very short time. Finally I have also discovered that the injurious ellects caused lay the catalytic action of the surfaces of. the

superheaterichannels are more easily avoid ed if. the supcrheator-channels are made from a material gh ing'an acid reaction iii-- stead of from a material of basic character, although even with material of basic charactor almost theoretical yields of nitrogen compounds may be obtained. it high temperatures and great speed of the gases through the channels are resorted to.

By reason of my invention l have now succeeded in overcoi-ning the well-known diliiculties of the other processes oi cyanizing gases provided the operations are car ried out in the Way described below.

in practising my invention the inside of the channels of a superheater of any of the well-known constructions is lined with any suitable lire proof material, as for in stance the well known Dims-stones which consist chiefly of quarta In selecting this lining material I do not attribute particular importance to the physical condition of said Dinas-stones inasmuch as it is immaterial whether the smoothness of their sul. "aces as well as the density of the material. is more or less perfect. o

In order to counteract the decomposition caused by the rough surfaces as well as by the porosity of the stones, it is essential to first establish the measruements of the crosssection of the channels in View of the composition of the distillers wash to he carbonized, and then to find out that particular speed of the gases which is most 'h'worahle for the elimination of the decomposing effect of the catalytic action of the surfaces. The speed of the gases cannot be pcrmanently maintained at the same rate hut is always subject to the composition or the distillers wash which is known to vary greatly:

I have found it advantageous to pass the gases, which are to he cyanined and which. contain the nitrogen, mostly in the form of pyridin compounds, through the superheater channels at a speed not exceeding 7 meters per second; care must be taken during this operation that the gases at this speed actually attain the high temperature requiredcontaining the nitrogen ireferably in the form of amino compounds may he treated at the same temperature while passing the superheater chaimels at a much higher speed, the speed in this case being 10 meters and even more per second.

The operations described above otter the further advantage of permitting a direct till lllll passage of the gases from the carbonizer into the superheater-channels the gases not sustaining a change in their composition during such passage.

Up to the present it has been considered necessary to separate the nitrogenous tar hour the gases on their travel from the carbonizer to the superheater and to sepa rately cyanize the so-obtained tar; another modification of the cyanizing process has consisted in the perfect separation of the gases into those liable to undergo cyanization and those not undergoing cyanization.

It is conceded that the two modifications mentioned above really result in a higher yield of nitrogen compounds, but such yields were still considerably below the theoretical one and are not in proportion to the expense entailed by carrying out the cumbersome op erations referred to.

The gases undergoing cyanization constitute only a rather small part of the gases leaving the carbonizer and though they are accompanied by a great excess of water vapor and other gases, not undergoing cy anization and only retarding the reaction, yet 1 am able by my invention to convert the Lt'hrmer kind of gases into cyanogen compounds and ammonia with an almost theoretical yield, the more valuable cyanogen compounds however, prevailing in the ob tained products to a considerable extent, thus increasing the economical importance of my invention.

The economical results of my process are rather considerable inasmuch as I am able to avoid several cumbersome operations by the practice of my new process; the improved results-obtained thereby enable me also especially to take advantage of the heat contained in the gases when leaving the carbonizer and finally to obtain a most satisfactory yield of cyanogen compounds.

The technical operation of my new process depends a great deal on the carbonization, which is governed by the composition of the raw material to be gasilied. If the carbonizcation occurs at a hightemperature any condensation of compounds may be prevented by carefully insulating the connection pipes between the carbonizer and the superheater, this precaution being assisted favorably by installing connection pipes of proper dimensions.

In case a raw material is to be gasified which will give the greatest yield of cyanisable gases only when carbonized at a relatively low tenq )eralure, lhe gases and vapors will accordingly be of low temperature when leaving the carbonizer; it is obvious that the operation of the carbonizer is very important for the regulation of the whole process, for by slackening the lire under the car- 1,. 1* cu. .r i a I. oo izer i can in st Ur ah ieducc the tempera w a r. s v oi. the gases, ii: ecessaiy, and by tnus controlling the fire as pointed out above I can furthermore also regulate the speed of the gases as required by the relation between the same and the heating surface of the channels. On the other side the higher I heat the carbonizer the greater will be the pressure of the gases and consequently also their traveling speed, while of course a reduction. in the supply of heat will ultimately also reduce their speed accordingly. If it is advisable that the gases leaving the carbonizer have a low temperature, the connection pipe between the carbonixer and superheater must be provided with some suitable means which will permit of immediately heating said pipe sulliciently so as to prevent any segregation of liquids within the pipe. This feature of preventing any liquefaction of gases by submitting the same to heat, may be successfully carried out by using waste heat'lrom the many sources existing in cyanid factories.

F or the further elucidation of my invention a construction of the apparatus preferred for carrying out the process is illustrated, by way of example, in the accompanying drawing, which is a vertical sectional view partly diagranunatic of said apparatus. The distillers wash, for example. is carbonized in the fire clay retorts A and the distillation gases escape through connection pipes B into the main pipe C whence they travel into a super-heater channel I) surrounded. by a. suitable mantle it made of lire clay bricks or other suitable material. As the superheater channel I) is heated to a high temperature, flues'lj of suliicient width are interposed between the mantle E and channel D and an inlet G and exit H is pro vided for the heating gases. The distillation gases are cyanized while passing through the hot superheater channel and leave through exit I to be further treated to assume marketable form.

The process as described is particularly valuable in manufacturing nitrogen com pounds. such as cyanogen compounds and ammonia, and under the term. nitrogen compounds as used in the claims. I mean to include cyanogen and. ammonia. as well as other compounds coming within that broad designation.

What I claim and desire to secure by Letters Patent is:

1. In the process of manufacturing nitrogen compounds from the gases generated by the carlmnization o l" dist-illcrs wash and the like nitrogenous substances, carboni'lziug said substance. superhiating the resulting gases and reducing "the time of contact oi said gases with the superl'ieating surface by increasing the speed of said gases over said surface.

in the process of manufacturing nitrocompounds from. thegases generated by carbonization of distillers Wash and like nitrogenous substances, carbonizsaid substance, super-heating the resultgases, reducing the timeof Contact of the the ing ing said gases with-the supcrheiiiting surface by increasing the speed of said gases over said surface and varying said increased speed ing the ratio between the superheating area and the speed of the gases passing over the same.

the carbonization of distillers wash and the like nitrogenous substances, carbonizing the substance, super-heating the resulting gases, controlling the time of'contact of said gases with the superheating surface by 'arying the ratio between the superheating area and the speed of the gases passing over the same and varying said speed according to the composition of'said gases.

In testimony whereof I have signed. this specification in. the presence of two subscribing Witnesses.

ERNST KOCHENDOERFER. \Vitnesses Y HoRs'r ZIEGLER, ALBRECHT TI-IOMA.

Copies of this patent may be obtained for five cents each, by addressingthe Commissioner of Patents. Washington, D 0.

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