USRE14656E - Nathan sttlzberger - Google Patents

Description

- sT rEs PATE E NATHAN SULZBEBGEB, OF NEW YORK, N. Y.

METAL ,comrormn AND PROCESS or raonucmc TEE-sun.

Specification o1 Beissued Letters Patent. R issu May 27, 1919 no Drawin Original 110. 1,104,141; dated December 14, 1915, Serial No. 876,494,11ed December 10, 1914.

Application for reissue med December 12, 1917. Serial 110. 206,889.

To all whom it may concern:

Be it known that I, NATHAN SULZBERGER, a c1t1zen of the United States, residin in New York, county of New York, and tate of- New York, have invented certain new and useful Improvements in Metal Comounds and Processes of Producing the ame; and I do hereby declare the following to a full, clear, and exact description of the 1nvention,- such as will enable others skilled in the art to which it appertains to make and use the same.

It is well known that metallic nickel tamed by reducing nickel oxid or similar high temperatures in hydrogen, can be used for effecting catalytic reactions, articularly reactions of reduction. Metallic nickel produced in this way, at temperatures which compounds of nitrogen containing hydromake the product catalytically active, is a strongly pyrophoric product, that is to say, it becomes incandescent spontaneously when exposed to the air at ordinary temperatures immediately after reduction. In order to overcome such pyrophoric properties, special precautions are necessary in handlin the reduced nickel or in treating it to neu tralize or overcome its pyrophoric proper-1 V ties.

The'present invention relates to catalysts which are produced in a wet way, as distinguished from catalysts produced by reduction with hydrogen at high tempera-- 'tures, and which, as produced, are none yrophone; as well as to the non-pyrop one catalysts themselves.

1Hydrazin in partlcular, as well as other gen (as for instance hydroxylamin) and possessing reducing properties, vcan not certain cases be used as reducing, agents. 1 have found, that, in many of these instances, however, the reducing properties of hydrazin, etc., can be increased or'made to exert themselves,'if certain metal compounds, even in very small amounts, metals I have found those belonging to the platinum group especially valuable, which group, as is well known, includes the metals osmium, iridium, latinum, ruthenium, rhodium and palla ium. 'Other metals and the suspended are added. As such their salts may also be employed, as, for instance: sulfate of copper, chlorid of gold, etc. In the following I give, as an example of my novel process, the reduction of nickelborate by means of hydrazin-hydrate, it being, however, distinctly understood, that I wish in no wise to limit myself to the given quantities or to the workin method specifically stated and here emp oyed.

Nickel-borate, representing a greenish powder insoluble in water, does not, even when heated in water containing hydrazinhydrate undergo any visible change. Thus reduclble nickel compounds at relatively even when its. suspension is boiled there seems to be no evolution of gas, due to the decomposition of the hydrazin; This. fact by itself shows that the reducing qualities offthe hydrazin are not exerted. If, however, to the suspension of the nickel-borate in water a very. small amount (oftentimes even only a trace) of, for example, a solu-' tion containing palladium-iammonium-protochlorid 'is added, and then the liquid containing hydrazin (or a salt of hydrazin, as, for instance, sulfate of hydrazin and an alkali), the evolution of hydrogen-gas soon becomes visible. This evolution of gas becomes very violent, particularly on heating, while the nickel-borate changes its color, darkening and finally precipitates practically all its nickel-content in consequence of the reducing action of the hydrazin, which action has been incited by the ad: dition of the palladium-metal.-

In one instance to a sus ension of two 7 grams of nickel-borate in a ut ten cc. of

.added four grams of hydrazinsulfate,

which had been made alkaline by the addition of caustic soda. On heating a very v1olent evolution of gas was observed, while borate of nickel darkenedin ten to fifteen minutes the color. After nickel metal had deposited itself as a black, voluminous, spong mass, while theliquid above the same, ha become water-like clear. This nickel possesses very marked magnetic properties and is particularly valuable also I in'hydroge'nating fats inloils as, for incontainin for instance,

1 hydrogen-compounds in .T the metal-compounds which .65

ten are only suspended in the same. nitrate of which are practically the said compounds with basic stance, cottonseed oila A sample of cottonseed oil, which was hardened with the above nickel-metal, proved to 'be particularly white in color, and the nickel (the catalyzer) had settled out of the oil at the end of the hydrogenization in the bottom of the test tube so well, that the hot oil stood over 3 the catalyzer as a clear liquid. During the process,'however, the oil was black, due to the very'minute and fine suspension of the nickel in the same. The presence of the small amounts of that most eflicient catalyzer lpa1ladium.makes this nickel especially valua le for such a catalytic process. Similarly, also, other salts of nickel, cobalt, etc., may be reduced by the action of a liquid hydrazin with the addition of an inciting metal (or a mixture of such metals) among which may be such salts, as,

nickel nitrate, which are soluble in water, as well as such, as for instance, nickel-silicate (nickel-carbonate, cobalt-carbonate, etc.,) which, being'insoluble in wa- Even nickel, which, soluble in water, cannot be reduced by a solution containing hydrazin, even when heated with the, same, can readily be reduced, if the hydrazin is used in connection with a metal, which incites its action, as, for instance, latinum-chlorid. V

The a ove described working methods can variously be modified without leaving the scope of this invention. Thus the b'orate of ulckel can also'be reduced if the hydrazinhydrate, using as an inciter platinumchlorld. The incitingmetal-salt may also be added to the borate simultaneously-with the hydrazincontaining liquid. ,I prefer in manycases to add the hydrazin to the liquid contamlngthe compound, which is to be reduced, and the inciting metal.

The process may, also, be of special technical value in the metallurgical separation of nickel, etc., from other products. As

basic compounts of nitrogen and hydrogen prlncipally to be considered are hydrazin (hydrazln-hydrate, salts of hydrazin with an alkah) and hydroxylamin (salts plus alkali) and derivatives, the value as reduclng agentsof which is increased or started by theaddition ofmetals. Having thus described my invention what cla1m is: I 1. Process for reducing metal-compounds,

unreducible with nitrogen-hydrogen-compounds possessing reduclng-actlon alone, consisting in treating such metal-compounds with such nitrogenpresence of a catalytically acting metal. i a

2. The process of reducing reducible comprises treating nitrogenalthough easily I scribed.

I as described.

hydrogen compounds possessing reducing action, in the presence of another catalytically acting metal.

3. The process of reducing reducible metal-compounds which comprises treating the said components .with basic nitrogenhydrogen compounds possessing reducing action, in thepresence-of a catalytically. act'- ing metal belonging to the platinum group.

4. The process of reducing reducible metal-compounds which comprises treating the said compounds with hydrazin, in the the said compounds with hydrazin in the presence of palladium.

he process of reducing nickel-compounds which comprises. treating the same with hydrazin in the presence of a catalytically acting metal.

8. The process of reducing nickel-compounds which comprises treating the said compounds With hydrazin, 1n the presence of palladium. i

9. As a new product, a product of reduction 7 in a wet way of a reducible compound of a catalytic metal, together with a'metal of the platinum group, sa1d,product being a black" non-pyrophoric magnetic powder immediately after reduction; substantially as de- 7 10. As a new product, a product ofreduction with hydrazin in a wet way, and in the presence of a metal of the platinum group, of a reduciblecompound of another metal,

' said product being a black non-pyrophoric magnetic powder immediately after reduction and containing the metals in anintimate state of combination; substantially as described.

11. As a new product,.catalyt-ically active nickel produced in a wet way by the reduction of reducible nickel compound, said product being a black non-pyrophoric magnetic powderimmediately after reduction, and being in admixture with an inciting agent; substantially as described.

12. As a new product, catalyticallyactive nickel obtainable in a wet way by the reduction of a reducible nickel compound with hydrazin in the presence of a metal of the platinum group, said product being a black non-pyrophoric magnetic powder immediately after reduction and containing nickel and a metal of, the platinum grou in an in timate state of combination; substantially product being a 13. As a new product, catalytically active nickel obtainable in a wet way by the re-. duction of a reducible nickel compound with ence of a metal of the platinum 'oup, said product being a black, non-pyrop oric magnetic powder immediately after reduction; substantially as described.

15. As a new .product a catalytically active metal produced in a wet way by reduction With hydrazin in the presence of a metal of the platinum roup, said product containing the catalyticzfily active metal and the metal of theplatinum group in a most intimate state of association; substantially as described.

NATHAN 'SULZBERGER.