US943132A - Process of producing nitrids. - Google Patents

Description

C. E. ACKBR. PROCESS 0F PRODUGING NITEIDS. APPLICATION FILED MAR. Ia, 1909.

Patented Dec. 14, 1909.

CHARLES E. ACKER, OF NEW YORK, N. Y., ASSIGNOR TO THE CORPORATION OF NEW YORK.

PROCESS 0F PRODUCING NITRIDS.

Specification of Letters Patent.

Patented Dec. 14, 1909.

\ Application Afiled March 18, 1909. Serial No. 484,187.

To all whom it may concern:

Be it known that I, CHARLES E. AcKnR, a citizen of the United States, residing at New York, in the county of New York and State of New York, have invented certain new and useful Improvements in Processes of Producing Nitrids,of which the following is a specification.

This process relates to the electrolytic production of nitrids, especially those of the alkali and alkaline-earth` metals.

The preferred process comprises the steps of electrolyzing a molten compound of the metal which is to be combined with nitrogen, alloying the separated metal with a-cathode metal, reacting on the alloyed metal with a nitrogenous gas, and returning the residual metal to the cathode. Incidental steps are the injection of the nitrogenous gas in a direction to cause or assist the circulationy of the alloy and residual metal; and the cooling of the alloy before treatment with the gas, especially by maintaining opposed adjacent streams of the alloy and residual metal.. Apparatus which may be used in carrying out the process is shown in the accompany` ing drawings, in Which- Y Figures l, 2, 3 are vertical'l'ongitudinal sections of three different constructions, each comprising an electrolytic cell and a separate connected chamber for treating the alloy.

Each apparatus illustrated has the l .eral construction of that heretofore devised by me for the production of caustic alkali. the electrolytic cell comprising a cast iron vessel l lined at the sides with magnesia brick 2, inclosed in brickwork 3 and covered by a refractory slab 4, throughwhich pass the depending carbon anodes 5. In the bottom of the vessel is a shallow layer 6 of a molten heavy inert metal such as lead, constituting the cathode, upon Which is the molten electrolyte 7. Theivessel 1 -is connected by delivery and return pipes or ducts 8, 9 to a separate chamber 10, into which the nitrogenous gas may be introduced by a valved pipe 11. The chamber 10 may be inclosed in the brickwork 3, as shown in Figs. 1, 3, or may be outside it as shown in Fig. 2, depending desired to maintain therein.

The delivery pipe 8 of the apparatus shown in Fig. 1 is provided with a series of genon the temperature which it is annular heat-radiating flanges 12, to cool the alloy therein. v The delivery pipe 82 of the apparatus shown in Fig. 2 has a lower portion which receives a. supplemental gas inlet pipe 13 and thence inclinesupward to the chamber 10, the gas injected through the pipe 13 and the light compounds produced by the gas -rising and moving along the pipe, facilitating the reaction therein. In the apparatus of Fig. 3, a portion of the delivery pipe 83 is enlarged and receives the return pipe 93, so that heat may be transferred from the outflowing alloy to the returning residual metal. and metal may be effected either solely by the current of injected gas, as in the apparatus of Figs. 1, 3, or by a mechanical device, for example the screw shown in Fig. 2, or by both. If desired, the alloy may be cooled by injecting a regulated amount of a cooled and 4compressed gaseous reagent.

The reaction chamber l0 is of the general construction of that employed in mycaustic alkali apparatus, comprising a vertical cen- The circulation of the alloy NITROGEN COMPANY, A

tral pipe 14, which -receives the molten alloy and injected as. The nitrid resulting from the reaction, eing usually lighter than the residual metal, rises and collects as a floating layer, which may be run out through a suitable outlet 15, the metal returning to the electrolytic cell to reconstitute the cathode.

A specific process which may be carried out is the production of calcium nitrid by the injection of nitrogen into an electrolytic calcium-lead alloy.

I claim:

1. The cyclic process-of producing nitrids, whichA consists in repeatedly reacting with nitrogen on an alloy comprising an inert metal and a nitrid-forming metal, separating the resulting nitrid, and alloying more of the nitrid-forming metal with the residual l inert metal.

2. The cyclic process of producing nitrids, which consists in repeatedly reacting with nitrogen on a molten alloy comprising an inert metal and a nitridorming metal, sepa` rating the resulting nitrid, and alloyin more of the nitrid-forming metal with the residual inert metal.

3. 'The cyclic process of producing nitrids, Which consists in repeatedly reacting with nitrogen on a molten alloy comprislng an inert metal and a nitrid-forming metal, separating the resulting ntrid, and alloying more of the nitrid-lt'orming metal With the residual molten inert metal.

4. The cyclic process of producing nitrids, which consists in injecting a nitrogenous gas into a molten alloy comprising an inert metal and a nitrid-forming metal, separating the resulting nitrid, and alloying more ot' the nitrid-forming metal with the residual metal for further treatment. l

5. The electrolytic process of producing nitrids, which consists in electrolyzing a molten compound of'a nitrid-forming metal, alloying the separated metal with an inert .cathode metal, reacting on the molten alloy with nitrogen, separating the resulting nitrid, and ree'mploying the residual' inert metal'in the cathode.

6. The electrolytio process of producing nitrids, which consists in electrolyzing a molten compound of a nitrid-forming metal, alloying tlie separated metal With an inert cathode metal, injecting a nitrogenous `gas into the molten alloy, separating the resulting nitrid, and remploying the inert residual metal in the cathode. y 7. The cyclic process of producing alkaline-earth metal nitrids, which consists in repeatedlyreacting Withnitrogen on an alloy comprising an inert metal Aand an alkalineearth metal, separating the resultant nitrid, and alloying more of the alkaline-earth metal with the residual inert metal.

.8. The cyclic process of producing calcium nitrid, which consists in repeatedly reacting `with nitrogen on an alloy 'comprising an inert metal and calcium, separating the resultantn1tr1d,'and alloying more calcium with the residual inert metal.

In testimony whereof, I aiix my signature m presence of two witnesses.

CHARLES ACKER.- Titnesses i ROBERT HARRISON, SUSIE E. SAMrsoN..

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