US1037019A - Process of manufacturing alkali-metal cyanids. - Google Patents

Process of manufacturing alkali-metal cyanids. Download PDF

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US1037019A
US1037019A US59087310A US1910590873A US1037019A US 1037019 A US1037019 A US 1037019A US 59087310 A US59087310 A US 59087310A US 1910590873 A US1910590873 A US 1910590873A US 1037019 A US1037019 A US 1037019A
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vessel
furnace
carbon
tube
cyanid
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US59087310A
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James Alfred Kendall
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JOSEPH WILSCH SWAN
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JOSEPH WILSCH SWAN
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01CAMMONIA; CYANOGEN; COMPOUNDS THEREOF
    • C01C3/00Cyanogen; Compounds thereof
    • C01C3/002Synthesis of metal cyanides or metal cyanamides from elementary nitrogen and carbides
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/80Compositional purity

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  • This invention relates to the nianutaetui'e ol' illlii i metal cyanitls by reaction hetneen (.illitili. nitrogen. and alkali. a a high temperature. and the said invention has tor its :llljttt lo pi'nvide means Wherehy the re- (plll'ttl cyanid can he conveniently.etiicientlv. and continuously produced in a condition ol great purity.
  • the nitrogen and the required alkali. metal containing mat ter, such as carbonate, 0! hydrate, of polar siuni or of sodium are "fed in a carefu regulated manner into the lower part of" a reaction chaniher, or vessel, containing carbon. and the vapor of alkali metal c xnnid, tlne to the reaction, passes into a ,ontl nsing ehainlici' or WSSth n'hich is provided at its lower part with means by which the. liqiulied alkali metal cyanid coi'itlensed passes out.
  • the aforesa d apparatus is made oi 11l(l-I( oi' cobalt, 0]. other suitable metal. or alloy. hut pretei'ahly nickel plate. either %as.. 1: rolled, and containing one half of one per cent. of manganese. or plate cast from melted nickel to which a small quantity of carbon has been added. The plate should he autogeiu usly welded in forming the appaiatus.
  • the apparatus is heated in a furnao? hooded with the flame. got by the combustion of hydroearlum gas, 01' oil fuel. the fiaine heing driven into the furnace by jets of fill so as to completely till it and allow a small surplus of flame to issue at openings provided for the purpose.
  • Figures 1 and 9 Show the apparatus in ele' vations'at right l each other, The furnace is shown Fig. 1. out is omitted from F shows a modified detail as her at?" is a side elevation of a i action vessel and condenser.
  • a. tube l so dered into the lOWtl' part oi the reaction chauihei. or vessel. extends upward outside the ieactimi and condensing chambers and is connected at top with the supply oi nitro gen entering h the ipe r7. lnto the said tuhe ll ope! nether lulie E which also extends up ⁇ '
  • This tuhe E is for the admis ion oi the fused allcali uietal containing n'iatei'ial "which can he supplied to. and he used in.
  • a tunnel pietcrahly cylin (hi all at the to'pot the tuhe. for example when using a carbonate: or the Fused alkali metal containing material can he allowed to (hip into the funnel e. for example when using; a hydrate. or it can he supplied in the Fm-in ot compressed pellets.
  • the 'lhe apparatus is placed in a furnace l so that the reaction chainhei. 01 vessel. A. and the lonei" pai't oi the condensingchanihe. or vessel. l"). and the tuhes l) and and the lou'ev pact of the tin ucl c which receives the alltali metal contain material. are in the furnace. the upper paitof the condensing (llflllll)( ⁇ . or vessel 3 intending to outside the furnace.
  • said tunnel c can be provided with means .tor passing coal-gas, or the like, into it to prevent access of air.
  • the pipe 'at- H is for thispurpose.
  • the tube 1), by which nitrogen is supplied, is preferably made with an enlargenu it u at the part where it emerges from the furnace, so as to prevent any alkali. which may penetrate into the said tube, causing (:iJFiITUCilOH to the flow of nitrogen.
  • the tunnel c for the alkali metal containing material, and the pipe D forthe nitrogen, can be supported by a clamp I fastened to the upper part of the condensing chamber, or vessel, B, as illustrated.
  • the outlet tube (1, and its cup-like termination C should becso supported as to relieve strain tion. his may be done by means of a hook. J on a chain 17' passing over a pulley j and provided witha counterweighb 7' the book being applied to the boss of the cup 0 or to the end part of the cup-like termination 0 of the outlet tube.
  • the entire apparatus within the furnace is made of metal which will withstand the action of the materials, and the high ten perature employed, preferably nickel with a small percentage of manganese, or carbon,-
  • the furnace may be made of refractory earthenware and the top may be made of removable bricks K. It is preferred to mount ,the reaction chamber, or vessel, A on a disk I of nickel, or the like, sup 'iorted from the floor of the furnace by bricks Z and to put alittle refractory earth on the said disk to prevent the reaction vessel adheiriru to it at the high temperature enn'iloyed. .lhe flame which passes out by the channel around the'cyanid outlet tube C will keep the cy'anid in the said tube in a sutliciently liquid condition to cause it to flow out.
  • the said channel. f can he made as a slot from the top of the furnace and the and compensate for expansion and contracmovable brick (or removable bricks) when the apparatus is in place in the furnace.
  • reaction vessel A when in use, is completely filled with carbon which should extend up into the condensing chamber, or
  • the temperature required for the reaction I find is 1300 centigrade.
  • the condensingvcssel B instead of being superposed on the reaction vessel A, may, if desired, be situated at the required elevation at the side thereof, as illustrated for example in Fig. 4.
  • the vessel A is made of such length that its upper part project above the furnace, the to of which is indicated by the dotted line
  • the vessels A and B are in communication with each other for T allowing the gaseous and vaporous products to pass from the vessel A to the condensing vessel 13, which can be conveniently effected by two tubes W and X screwed together.
  • the top of the vessel A is provided with a stopper Y which is removed when it is necessary to introduce fresh carbon.
  • the clamp for sup orting the nitrogen tube and thopotash unnel can be carried by the upper part of the vessel A.
  • the weight of the condensing vessel B can be counterpoised in order to prevent undue strain on the tubes W' and X. This can be done by inserting two metal pegs (Z) into the upper part of the vessel B and connecting to these pegs the chain attached to a counterpoise like that shown in the first arrangement.
  • the parts which correspond with those shown in the other figures are marked with the reference letters.
  • alkali metal cyanids which consists in feeding n1- trogcn and alkali metal containing matter to the lower portion of a quantity of carbon in a reaction chamber, highl heating the latter, leading the cyanid vapors u Yard through the carbon to a heated condenser containing carbon and leading off therefrom in liquid form, the cyanid condensed therein, substantially as described.
  • the method of manufacturing alkali metalcyanids which consists in feeding nitrogen and alkali metal containing matter to the lower portion of a quantity of carbon inv a reaction ahamber, highly ter, leading the cyanid *apors upward through the carbon to a heated condenser an-d ;lea ling oll' therefrom in liquid form through a. heated outlet the cyanid condensed' therein, substantially as described.
  • alkali In tal cyanide which consists in feeding nitrogen and at all metal containing matter to the lower portion. of a quantity of carbon in heating the lata reaction chamber, highly heating the latter, leading the cyanid vapors upward through the carbon to a heated condenser ing matter to the bottom thereof, highly heating the reaction chamber, leading the cyanid vapors upward through the carbon to a heated condenser and leading off from the latter, in liquid form, the cyanid condensed therein, substantially as described.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Toxicology (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Description

J. A. KENDALL.
PROCESS OF MANUFACTURING ALKALI METAL GYANIDS.
APPLICATION FILED NOV. 5,1910.
1,037,01 9 V A Patented. Aug-27, 1912.
2 SHEETS-SHEET l 'INVEN 7'0]? WIT/V55 s y Y A fim fill-FR e1: KENM L v y ya i," v i v J. A; KENDALL.
PROGE SS OF MANUFAGTURING ALKALI METAL GYANIDS. APPLICATION r LnDNov. 5, 1910.
1,037,019. nted Aug. 27,1912.
2 SHBETS-SHEET 2.
Jam E5 1% FRED KE L hunt. in the count of London. ling3- [application filed November Z 162/ whom it may It-(mccrn lie it known that JALxLs fun-nun mm, a suhjwt ot' the Fine of Great lh-itin and lieland. of 45% Fairniile avenue. Sir
lHH'L invented a new and useful Pi'oci .llaiuilactui'ing .tlltali-Ii'letal Cyani which the following a specification.
This invention relates to the nianutaetui'e ol' illlii i metal cyanitls by reaction hetneen (.illitili. nitrogen. and alkali. a a high temperature. and the said invention has tor its :llljttt lo pi'nvide means Wherehy the re- (plll'ttl cyanid can he conveniently.etiicientlv. and continuously produced in a condition ol great purity.
According to this invention the nitrogen and the required alkali. metal containing mat ter, such as carbonate, 0! hydrate, of polar siuni or of sodium are "fed in a carefu regulated manner into the lower part of" a reaction chaniher, or vessel, containing carbon. and the vapor of alkali metal c xnnid, tlne to the reaction, passes into a ,ontl nsing ehainlici' or WSSth n'hich is provided at its lower part with means by which the. liqiulied alkali metal cyanid coi'itlensed passes out. The aforesa d apparatus is made oi 11l(l-I( oi' cobalt, 0]. other suitable metal. or alloy. hut pretei'ahly nickel plate. either %as.. 1: rolled, and containing one half of one per cent. of manganese. or plate cast from melted nickel to which a small quantity of carbon has been added. The plate should he autogeiu usly welded in forming the appaiatus. The apparatus is heated in a furnao? hooded with the flame. got by the combustion of hydroearlum gas, 01' oil fuel. the fiaine heing driven into the furnace by jets of fill so as to completely till it and allow a small surplus of flame to issue at openings provided for the purpose.
The apparatus. the. furnace hy which it is l'icated. are. pi'ei eiuhly construct d as hereinafter desciihed with reference to the accompany q auing. hutv I do notv limit myself to ie pieeise details which l shall desc ibe.
Figures 1 and 9 Show the apparatus in ele' vations'at right l each other, The furnace is shown Fig. 1. out is omitted from F shows a modified detail as her at?" is a side elevation of a i action vessel and condenser.
Specification of Letters Extent.
, 1930. Serial No. 596.875.
formation). the said in shiineih or provided with a. /I so to term .1 huh-- I surromuling the uppe 'eaciion ehauihei'. o:- vessel.
so of coni it i (it) the i and. from this channel or trough, Z) lent an outlet tube (7 for the liquefied C Y'iUliil. .d tuhe being provined with a flange c ieai its end {to prevent any creepinghacl:
0!, e5anul) and mixing a cup-like iei'nnnu tn screwed onto its end. onto which cuplike termination the c vanul trickles. and
ti-uni which it will tall into a receiver.
For the supply of nitrogen. a. tube l so dered into the lOWtl' part oi the reaction chauihei. or vessel. extends upward outside the ieactimi and condensing chambers and is connected at top with the supply oi nitro gen entering h the ipe r7. lnto the said tuhe ll ope! nether lulie E which also extends up\\' This tuhe E is for the admis ion oi the fused allcali uietal containing n'iatei'ial "which can he supplied to. and he used in. a tunnel (pietcrahly cylin (hi all at the to'pot the tuhe. for example when using a carbonate: or the Fused alkali metal containing material can he allowed to (hip into the funnel e. for example when using; a hydrate. or it can he supplied in the Fm-in ot compressed pellets.
'lhe apparatus is placed in a furnace l so that the reaction chainhei. 01 vessel. A. and the lonei" pai't oi the condensingchanihe. or vessel. l"). and the tuhes l) and and the lou'ev pact of the tin ucl c which receives the alltali metal contain material. are in the furnace. the upper paitof the condensing (llflllll)(}. or vessel 3 intending to outside the furnace. so .'f111i(l reaction will escape by its contracted upper opening L and so that fresh supplies thut gases produced in the space between the condensing chamber, or upper part of this slot/be filled in by a rovessel, and the opening 7' 1n the roof of the l'urnacc through which it passes to allow of the passage oi the surplus flame around the said outlet tube (f, and around the condensing chamber, or vessel, l3. Besides these openings for the escape of flame, I provide an outlet which can be opened and closed by a movable brick. especially in the case of a .turnace o'l la rgc size. The furnace is provided with openings f in lts wall, opposite which openings are burners G and means for 'lorein air, with the flames of the burners. into the interior of the furnace.
l or preventing the escape oi nitrogen gas through the funnel e .by which the alkali metal containing material is supplied, the opening leading from the said funnel into the tube i below it can be closed by a plug ("-1 or the said tube can be made of siphon form. as illustrated at E in Fig. 3. The
said tunnel c can be provided with means .tor passing coal-gas, or the like, into it to prevent access of air. The pipe 'at- H is for thispurpose. The tube 1), by which nitrogen is supplied, is preferably made with an enlargenu it u at the part where it emerges from the furnace, so as to prevent any alkali. which may penetrate into the said tube, causing (:iJFiITUCilOH to the flow of nitrogen.
The tunnel c for the alkali metal containing material, and the pipe D forthe nitrogen, can be supported by a clamp I fastened to the upper part of the condensing chamber, or vessel, B, as illustrated. The outlet tube (1, and its cup-like termination C should becso supported as to relieve strain tion. his may be done by means of a hook. J on a chain 17' passing over a pulley j and provided witha counterweighb 7' the book being applied to the boss of the cup 0 or to the end part of the cup-like termination 0 of the outlet tube.
The entire apparatus within the furnace is made of metal which will withstand the action of the materials, and the high ten perature employed, preferably nickel with a small percentage of manganese, or carbon,-
as aforesaid, the parts being autogenously welded together. The furnace may be made of refractory earthenware and the top may be made of removable bricks K. It is preferred to mount ,the reaction chamber, or vessel, A on a disk I of nickel, or the like, sup 'iorted from the floor of the furnace by bricks Z and to put alittle refractory earth on the said disk to prevent the reaction vessel adheiriru to it at the high temperature enn'iloyed. .lhe flame which passes out by the channel around the'cyanid outlet tube C will keep the cy'anid in the said tube in a sutliciently liquid condition to cause it to flow out. The said channel. f can he made as a slot from the top of the furnace and the and compensate for expansion and contracmovable brick (or removable bricks) when the apparatus is in place in the furnace.
Should the carbon, or the alkali metal containing material, contain any appreciable quantity of ash, or non volatile matter, means should be provided for removing such ash, or non-volatile matter, without it being necessary to remove the apparatus from the furnace for the purpose. This may be done by leading av tube a from the bottom of the reaction chamber, or vessel, A, this tube a passing out through a hole f in the floor of the furnace, and the furnace being supported on columns, or the like, which will allow of access to the said tube a and a separate burner can be used at this hole so that the said tube a can be strongly heated when required. *oW'hen ash, or non-volatile matter, is to be renuived, the temperature ot the furnace is reduced considerably below the working heat and a quantity of fused alkali metal containing matter is passed down the tube E which feeds in the said matter, and, if-necessary, some alkaline borate can be added to it. The fused alkali containing matter will carry the ash, ornon-volatile matter, out through the tube which isheated to the necessary temperature. The said tube may be closed by a plug of nickel, or other suitable material, during IIOIll'llll work. or the said tube may have a siphon bend in it.
The reaction vessel A, when in use, is completely filled with carbon which should extend up into the condensing chamber, or
vessel, B, so as to partially fill it also.
The temperature required for the reaction I find is 1300 centigrade. A
The condensingvcssel B, instead of being superposed on the reaction vessel A, may, if desired, be situated at the required elevation at the side thereof, as illustrated for example in Fig. 4. The vessel A is made of such length that its upper part project above the furnace, the to of which is indicated by the dotted line The vessels A and B are in communication with each other for T allowing the gaseous and vaporous products to pass from the vessel A to the condensing vessel 13, which can be conveniently effected by two tubes W and X screwed together.
The top of the vessel A is provided with a stopper Y which is removed when it is necessary to introduce fresh carbon. The clamp for sup orting the nitrogen tube and thopotash unnel can be carried by the upper part of the vessel A. The weight of the condensing vessel B can be counterpoised in order to prevent undue strain on the tubes W' and X. This can be done by inserting two metal pegs (Z) into the upper part of the vessel B and connecting to these pegs the chain attached to a counterpoise like that shown in the first arrangement. The parts which correspond with those shown in the other figures are marked with the reference letters.
,}I' claim asmy invention:
1. The method of nmnutacturing alkali metal cyanids which consists in feeding nitrogen and alkali metal containing matter to the lower portion of a quantity of carbon -in a reaction chamber, highly heating the latter, leading the cyanid vapors upward through the carbon to a heated condenser and leading off therefrom in liquid form the cyanid condensed therein, substantially as described.
The method of manufacturing alkali metal cyanids which consists in feeding n1- trogcn and alkali metal containing matter to the lower portion of a quantity of carbon in a reaction chamber, highl heating the latter, leading the cyanid vapors u Yard through the carbon to a heated condenser containing carbon and leading off therefrom in liquid form, the cyanid condensed therein, substantially as described.
The method of manufacturing alkali metalcyanids which consists in feeding nitrogen and alkali metal containing matter to the lower portion of a quantity of carbon inv a reaction ahamber, highly ter, leading the cyanid *apors upward through the carbon to a heated condenser an-d ;lea ling oll' therefrom in liquid form through a. heated outlet the cyanid condensed' therein, substantially as described.
4. The method of manufacturing alkali In tal cyanide which consists in feeding nitrogen and at all metal containing matter to the lower portion. of a quantity of carbon in heating the lata reaction chamber, highly heating the latter, leading the cyanid vapors upward through the carbon to a heated condenser ing matter to the bottom thereof, highly heating the reaction chamber, leading the cyanid vapors upward through the carbon to a heated condenser and leading off from the latter, in liquid form, the cyanid condensed therein, substantially as described.
(3. The method of manufacturing alkali metal cyanid which consists in filling a reaction chamber and at least partially filling a superposed condensing chamber with carbon, feeding, to the lower portion of the reaction chambcr a controlled quantity of ni trogen and alkali metal containing matter, heating the reaction chamber, leading the cyanid vapors upward. through the carbon to the condenser, and leading off therefrom, in liquid form, the cyanid condensed therein, substantially as described.
In testimon whereof I have signed my name to. this specification in the presence of two subscribing witnesses.
JAl-dES ALF tED KENDALL.
Witnesses EDWARD Gnonon Davin-s, Gunner FLETCHER Tyson.
US59087310A 1910-11-05 1910-11-05 Process of manufacturing alkali-metal cyanids. Expired - Lifetime US1037019A (en)

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