US957843A - Process of making ammonia. - Google Patents

Description

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titanium nitrid (Ti N on being i Be it lmown that l, Cam. Boson, doctor of philosophy and chemist, subject of the King of Prussia, residing at Ludwigshatem on-the-lithine, Germany, have invented new and useful Improvements in Processes oi? alring monia, of which the following is a specification. i

lln the Uomptea Renders (82, page 974) it is stated by Friedel and Guerin that a boiled with concentrated sudfuric acid, gives rise to ammonia and titanic acid. l have now discovered that titanium nitride can be made to yield ammonia Jby oxidationinthe presence of watenun'derwhich term t in clude water bath in the -litpuid statefand' in the form ot vapor or steam. course the oxidation of the titanium nitride should he carried out-under such conditions that none, or practically. none, "ot the ammonia termed becomes outdiaed to tree nitrogen.-

Provided that this condition be maintained, many did'erents oxidation agents and methods may be employed, for instance the reaction can be carried out in alkalinabr' neutral, or acid, solution, or suspension, or even in a melt. As examples oi. onidizing agents ll mention chromic acid, manganese dioxid, iron oxid, copper oxid, cerium oxid, mercury oxid, and salts corresponding to these oxide. The oxidation may also be caused to take place by treating the titanium nitrid with steam in the presence of an oxygen carrier (for instance, a metallic salt, or oxid, or hydroxid, such as sodium carbonate, caustic soda, and calcium chlorid) which, by itself, under the conditions used as to temperature and quantity, has no oxidizing action, or practically no oxidizing action, on the titanrum nitrid. Steam by itself does notreact till upon the titanium nitrid until such a temerature is reached that the ammonia ormed is decomposed again to a greater, or lesser, extent. Or the oxidation may be carried out by heating the titanium nitrid with a bisultate, prov1ded water be present and the temperature employed be not too high. If desired, the treatment with the oxidizing agent may be made to take place under pressure. Electrolysis, with, or without, the use of so-called oxygen carriers, can

also be employed to efiect the oxidation, and

ma errant, assrenon ro nanisonn rearnn-ott-rnn-nrnn, anniuanr, con- -hpeetucatton ct t ammate. 1 p t t d m y to, pom, Application not arch at, ra e. stratum taattt.

even; air can b e used in. the presence of steam, or water (it necessary under pressure, and using an oxygen carrier), to bring about oxidation.-

When carrying out the moose otqny invention the titanium is o tained in the form of its oxid, or of a salt thereof, and

can then easily be reconverted into titanium nitrid,'rnalring use of atmospheric nitrogen. it, when carrying out the oxidation in the resence of air and steam as hereinbefore escribed, a contact body, such for instance as finely divided latinum, be present, the ammonia produced is wholly, or partially, oxidized to oxide of nitrogen. V

' The following examples will serve to illustrate turther the nature ct myinvention,

Which,-Thofwever, is not confined to these exam les. The parts are by weight.

Clave, at about 180 U, 1 part of finely dis ample 1: Heat together, in an autoyided titanium nitrid, 15 parts of. 30 per cent. caustic soda solution, and 2 parts of copper oxid. U11 opening the valve ofithe autoclave ammonia escapes. The reaction which takes place can be represented by the equation ln this example instead of copper oxid,

an equivalent quantity of iron oxid, or

manganese peroxid, or chromic acid, can be employed. 7

Example 2: Heat together at from 100 C, to 140 0., in an autoclave, 1 part of titanium nitrid, 20 parts of 20 per cent. sulturic acid, and one part of 30 per cent. forrous sulfate solution, and pump in air, while 1 stirring Well, until the oxidation is complete.

The reaction which takes place can be represented by the equation If the ferrous sulfatebe omitted, the reaction proceeds more slowly.

Example 3: Suspend 1 part of titanium nitrid in 20 parts of 50 per cent. sulfuric acid, add one part'of chromium sulfate or ferrous sulfate to the suspension and oxidize it electrolytically, at 100 (1;, in a cell provided with a I diaphragm. Thereaction which takes place can be representedby the equation Example 4: Introduce -1- part of finely divided titanium nitrid (T1 N into 10 parts of molten sodium bisulfate, and raise the temperature gradually to from 350 C. to 400 (3., until aquiet melt is obtained. Then allow themelt to cool somewhat, and add a small quantity of water, and heat again to from about 350 C. to about 400 C.

- Repeat this operation until the melt is white, ,or' until the nitrid has disappeared, I when the nitrogen is all obtained in the form T chlorid passes over.

takes of'ammonia. If desired, instead of adding small portions of water as aforesaid, steam can be assed through the melt at a temperature of about from 350- O. to 400 (1., but in this case the reaction-takes a longer time. The reaction which takes place can be represented by the equation Example 5: Heat amixture of 1 part of titanium nitrid' with 3 parts of calcium chlorid in a current of steam at a temperature of 500 0., whereupon ammonium The reaction which place can be represented by the equation a Example 6: Soak titanium nitrid in platinum chlorid solution until it contains rom 2 to 3 parts per 1,000 of platinum, and then heat it at from 300 C. to 400 C. in a current of mixed air and steam. By the catalytic action of the platinum in the presence of an excess of oxygen more or less of the ammonia is converted into oxids of nitrogen. The reaction which takes place can be represented by the equations Now what I claim is:

1. The process of producing ammonia by heating titanium nitrid with an oxidizing agent in the presence of water while maintaining the temperature so low that the production of free nitrogen is practically avoided.

CARL BOSCH V Witnesses:

J. ALEC, LLOYD, Jos. H. LEUTE.