CS277373B6 - A method for preparing alkaline earth metal tetracyanonicates - Google Patents

A method for preparing alkaline earth metal tetracyanonicates Download PDF

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CS277373B6
CS277373B6 CS91638A CS63891A CS277373B6 CS 277373 B6 CS277373 B6 CS 277373B6 CS 91638 A CS91638 A CS 91638A CS 63891 A CS63891 A CS 63891A CS 277373 B6 CS277373 B6 CS 277373B6
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Czechoslovakia
Prior art keywords
alkaline earth
earth metal
hydroxide
cyanide
tetracyanonicates
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CS91638A
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Czech (cs)
Slovak (sk)
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CS63891A3 (en
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Jozef Doc Rndr Csc Chomic
Juraj Rndr Csc Cernak
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Prirodovedecka Fakulta Upjs
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Priority to CS91638A priority Critical patent/CS277373B6/en
Publication of CS63891A3 publication Critical patent/CS63891A3/en
Publication of CS277373B6 publication Critical patent/CS277373B6/en

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Abstract

Tetrakyanonikelnatany kovov alkalických *” -I zemin vzorca I, kde M11 je vápnik, stroncium alebo bárium a n je 4 alebo 5 sa pripravujú tak, že na suspenziu kyanidu nikelnatého a hydroxydu kovu alkalické zeminy ako je hydroxyd barnatý, vápenatý alebo stronenatýv molámom pomere kyanid nikelnatý : hydroxyd 1 : 1 sa pósobí kyanovodíkom pri teplote 18 až 24 °C.Alkaline earth metal tetracyanoniclinates of formula I, where M11 is calcium, strontium or barium and n is 4 or 5, are prepared by treating a suspension of nickel cyanide and an alkaline earth metal hydroxide such as barium, calcium or strontium hydroxide in a molar ratio of nickel cyanide:hydroxide of 1:1 with hydrogen cyanide at a temperature of 18 to 24 °C.

Description

1 CS 277373 B6 Xíblast technikyTechnique techniques

Vynález sa týká spósobu přípravy tetrakyanonikelnatanov ko-vov alkalických zemin všeobecného vzorca IThe present invention relates to a process for the preparation of alkaline earth metal tetracyanonicates of formula (I)

Mi:E[Ni(CN)4] ,nH2O (I) kde M11 je vápník, stroncium alebo bárium. jpoteraj-ší stav techniky v / v ’ 'j " >Mi: E [Ni (CN) 4], nH 2 O (I) where M 11 is calcium, strontium or barium. The state of the art in v '' j '>

Tetrakyanonikelnatany kovov alkalických zemin sa doterazpřipravovali podvojnou záměnou například chlordiu barnatéhoa" tetrakyanonikelnatanu draselného podlá reakcieAlkaline earth metal tetracyanonates have so far been prepared by double exchange of, for example, chlorine barium and potassium tetracyanonicate by reaction.

BaCl2 + K2[NÍ(CN)4] —> Ba[NÍ(CN)4] + 2KC1BaCl2 + K2 [Ni (CN) 4] -> Ba [Ni (CN) 4] + 2KC1

Izolácia připraveného hydrátu tetrakyanonikelnatanu sa vykonáfrakčnou kryštalizáciou. Připravený produkt je však čiastočneznečistěný druhou přítomnou solou, napr. chloridom draselným.Isolation of the prepared tetracyanonicate hydrate is carried out by crystallization crystallization. However, the prepared product is partially unpurified by the second salt present, e.g., potassium chloride.

Podstata* vynálezuSUMMARY OF THE INVENTION

Podstata přípravy tetrakyanonikelnatanov kovov alkalickýchzemin podlá vynálezu spočívá v tom, že na suspenziu kyanidu ni-kelnatého a hydroxidu kovu alkalické zeminy ako je hydroxid bar-natý, vápenatý alebo stroncnatý v molárnom pomere kyanid nikelna-tý: hydroxid 1:1 sa pósobí kyanovodíkom pri teplote 18 až 24 °C.The principle of the preparation of alkaline earth metal tetracyanicinates according to the invention is that they are treated with hydrogen cyanide at a temperature of 1: 1 with a nickel-cyanide: hydroxide hydroxide suspension of 1: 1 cyanide: hydroxide hydroxide, calcium hydroxide or calcium hydroxide. 18-24 ° C.

Podlá vynálezu sa zmiešajú čerstvo připravené suspenzie kya-nidu nikelnatého a hydroxidu kovu alkalické zeminy. Do tejto re-akčnej zmesi sa zavádza za miešania kyanovodík. Vznikne roztoktetrakyanonikelnatanu kovu alkalických zemin. Případné póvodnénezreagované vo vodě nerozpustné zrazeniny sa odfiltrujú a z roz-toku po zahuštění vykryštalizuje hydrát tetrakyanonikelnatanu.Z bezpečnostných dóvodov sa syntéza uskutečňuje v uzatvorenejaparatúre. Nespotřebovaný kyanovodík sa absorbuje v absorbériroztokom síranu železnatého, čím sa súčasne zneškodní.According to the invention, freshly prepared nickel-cesulfide suspensions and alkaline earth metal hydroxide are mixed together. Hydrogen cyanide is introduced into this reaction mixture with stirring. An alkaline earth metal tetracyanonicate solution is formed. Possible non-reacted water-insoluble precipitates are filtered off and the tetracyanic anhydrate hydrate crystallizes out of the solution after concentration. For reasons of safety, the synthesis takes place at a closed camera. Unused hydrogen cyanide is absorbed in the ferrous sulfate absorbent solution, thereby simultaneously being disposed of.

Spósobom podlá vynálezu sa pripravia tetrakyanonikelnatanykovov alkalických zemin vo vysokéj čistotě 95 až 97 %. Příklady uskutočnenia vynálezu Příklad 1According to the present invention, alkaline earth tetracyanone-nickel tetracyanone is prepared in a high purity of 95 to 97%. EXAMPLES Example 1

Pri syntéze tetrakyanonikelnatanu barnatého sa do čerstvopripravenej suspenzie obsahujúcej kyanid nikelnatý a hydroxidbarnátý v molárnom pomere 1:1 (suspenzi^-obsahuje 20 hmotnostnýchdielov jtuhých zložiek v 80 hmotnostných dielov vody) zavedie kya-novodík připravený z kyanidu draselného a kyseliny sírovej. Množ-stvo kyanidu draselného a zriedenej kyseliny sírovej sa použijev ekvivalentnom množstve, čím sa dosiahne to, že kyanovodík sanepřipravuje vo velkom přebytku. Po ukončení reakcie sa odfiltru-je nezreagovaná tuhá zložka, roztok sa zahustí a po vykrystalizo-vaní sa z roztoku izoluje Ba[Ni(CN)4] ako tetrahydrát.Hydrogen cyanide prepared from potassium cyanide and sulfuric acid is introduced into the freshly prepared nickel-cyanide-hydroxyl-colorate suspension in a 1: 1 molar ratio (slurry containing 20 parts by weight of solids in 80 parts by weight of water) in the synthesis of barium tetracyanonate. The amount of potassium cyanide and dilute sulfuric acid is used in an equivalent amount, whereby hydrogen cyanide is prepared in a large excess. After the reaction is complete, the unreacted solid is filtered off, the solution is concentrated, and after crystallization, Ba [Ni (CN) 4] is isolated from the solution as a tetrahydrate.

Claims (3)

Spósob přípravy tetrakyanonikelnatanov kovov alkalických zemin všeobecného-vzorcaProcess for the preparation of alkaline earth metal tetracyanonickels of the general formula Mi:E[Ni(CN)4] .nH2O kde M11 je vápník, stroncium alebo bárium a n = 4 alebo 5, vyznáčujúci sa tým, že na suspenziu kyanidu nikelnatého a hydroxidu kovu alkalické zeminy ako je hydroxid barnatý, vápenatý alebo stroncnatý v molárnom pomere kyanid nikelnatý: hydroxid 1:1 sa pósobí kyanovodíkem pri teplote 18 až 24 °C.M i: E [Ni (CN) 4 ] .nH 2 O where M 11 is calcium, strontium or barium and n = 4 or 5, characterized in that the suspension of nickel cyanide and alkaline earth metal hydroxide such as barium hydroxide, calcium hydroxide or strontium in a molar ratio of nickel cyanide: hydroxide of 1: 1 is treated with hydrogen cyanide at a temperature of 18 to 24 ° C.
CS91638A 1991-03-12 1991-03-12 A method for preparing alkaline earth metal tetracyanonicates CS277373B6 (en)

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CS91638A CS277373B6 (en) 1991-03-12 1991-03-12 A method for preparing alkaline earth metal tetracyanonicates

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CS277373B6 true CS277373B6 (en) 1993-01-13

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