US1061725A - Process of producing molybdenum nitrid. - Google Patents

Description

I l i 1 To all 'whoin it may concern:

, 1,061,725. No Drawing;

. Be it known that we, CA L Boson and ALwIN. MrrrAsoH, subjects; respectively, of the King-of Prussia and the King of Sax Nitrid, of which-the following is a specifica- The usual process of preparing metallic nitrids from the corresponding oxids and nitrogen has hithertobeen jca rried out in' the presence ofsolid reducing agents. Ve'

W have now found'that'we-canobtai'n nitro gen. compounds of molybdenum with great facility by treating-an oxygen compound of molybdenum with nitrogen in the presence of a reducing gas, the process being carried out at a temperature under eight hundred degrees oentigrada We have also found 'that it is not necessary to react on the oxygen compound of molybdenum simultaneously with nitrogen and with the reducing gas, but that, if desired, the oxygen com pound can first be treated with the reducing gas, so that more or less complete reduction of the molybdenum oxygen compound is brought about, and the productbe after Ward treated with nitrogen. Since the reaction, and particularly the fixation of the nitrogen, proceeds more rapidly under pres sure, we prefer to employ pressure above that of the atmosphere when carrying out our process. As instances of oxygen com-' pounds of molybdenum which can be used according to our invention, we mention the oxids and hydroxids of molybdenum and also mixtures of-oxids of molybdenum with metallic molybdenum,'such for instance as 40 are obtainable by the incomplete reduction of oxids of molybdenum. Other com pounds containing oxygen, for instance, ,molybdates, can be employed. If desired th'e'process of this reaction can be carried 45.-out 1n the presence of a suitable catalytic agent, such for instance as iron, cobalt, or mckel, or theircompounds, without depart- .trom the nature of the invention.

he-molybdenum-nitrogen compounds obtainable according to our invention can be employed in various ways, for instance, on

rRooEss or rRonUoING monxnnnnpmgiqrmrni I Specification of Letters area. j Paten'tedil Application filed September 19,1911, serialnoissame.

' being heated to' a? higher 'tnptg .UMT ,ST TEsI rATEETQQEEIQE? f we. Boson AND ALWIN; Miran-Assn, on nunwra's Harm a-ort-TisE-1 z.rr r1in assrenons' 'ro ram-sons ANILIN AND- sonAf FABRIK, torynunwrssnarn pn- THE-RHINE, GERMANY, A oonrorta'rron. V r i 5' erablyin cacao,- they ean be convertedninto metallic molybdenum," which is thus obtain ablewith facility in afpure-state. Or the nitrids of molybdenum can befgempleyedl for producing valuable nitrogen compounds, 'for instance on' treating J the nia-i with hydrogen, or with "steam, ammomat; is formed,'and in the latter case the 'ozfidprof-Qw duced can be re-converted intopthanitrid,

's o'that' the same quantityotjmelybdenum, compound, canbe: employed repea dl. 1

the manufacture of ammonia. a The following examples'willse trate further the nature Of OHI invention] and how. it can be carried into practical ef- 1 feet, but the inyenti onQ-is not confinedtog,

these examples.

Example 1 Heat molybdic acid (11 M00 at a temperature of from five hundredto six hundred degrees centigradc, in a mix ture containing equal parts of hydrogen and nitrogen, while maintaining I a pressure of sixty atmospheres.

Example 2: Reducesublimed 'molybdenum trioxid by means of hydrogen at from.

five hundredth, six hundred degrees centigrade,"'either at ordinary, or at increased,

.pressure, and then, at five hundred degrees centigrade and at a' pressure of fifty atmospheres, treat, with nitrogen, the product thus obtained. 1 J Example 3: Reducepreci'pitated molybdic acid at 700 C. with hydrogen and then, at the-same temperature, pass over pure nitrogen at atmospheric pressurea Instead of hydrogen, other reducing gases, such for instance ascarbon monoxid and hydrocarbons, or mixtures of reducing gases, such for instance as water gas, can be employed. If desired, hydrogen or other indifferent gas can be mixed with the nitrogen.. Example 4: Pass a current of hydrogen and nitrogen, either simultaneously or one after the. other, over a mixture containing l90 parts of molybdicacid and 10 parts oi other oxids; such for instance as iron oxid' i and cobalt 0153, 6 the-"metals themselves or other suitable compounds thereof. v :Examplefi; Pass fir'st methane and thennitrogen oyerlo molybdic acid at from 500 to 600" C, ate pressure of 50 atmospheres.

' Now whatwe'claim is:- .0 o I 'lJThe process-of .producingmolybdenum nitrid by. heatingia compoundof molybdenum containing oxygen with a reducing gas -,nitrid by heating 'a." compound 'of 1nolybdeand with nitrogen at a temperature, between400 and 800 C 2. The process of producing molybdenum n'um containing oxygen with hydrogen and with nitrogen at. a temperature between 400 and 800 C. y I

- 3. The process of producing molybdenum @nitrid by heating a compound of molybdenum containing oxygen with a reducing gas 'perature between 400 and 800 C;

andwith nitrogen. under pressure, at- Ya tem- 4. The process of producing molybdenum nitridiby heating a compound of'molybde num containing-oxygen-first with a reducing; gas 'and thgg'with nitrogen under'pres 400 and.800 C. r

sure at a temperaturebetween 4500 and 5. The process of producing molybdenum nitrid by heating an oxid of molybdenum fiwith hydrogen and with nitrogennnder pres'sureat a temperature between 400 and 000 C I s 6. The process of producing molybdenum nitri'd by heating molybdenum trioxid with; hydrogen and :with nitrogen under pressure eta temperature between 400 and 800 C;

7. .The process of producing molybdenum nitridlby heating molybdenum trioxid first with hydrogen -and thenwith ;jnitrogeri under pressure at a temperature between i In testimony whereof ehuve hereunto set our hands in the. presence of-two'fsubscribing witnesses.

CARL BOSCHQ -J1.Anne/LLOYD; I

JOSEPH Penn-Em. l

' *ALWIN MITTASCH;