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UNITED STATES PATENT OFFICE 2,313,680 MANUFACTURE of THOCYANATES Lee B

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UNITED STATES PATENT OFFICE 2,313,680 MANUFACTURE of THOCYANATES Lee B Patented Mar. 9, 1943 2,313,680 UNITED STATES PATENT OFFICE 2,313,680 MANUFACTURE OF THOCYANATES Lee B. Smith, Woodbridge, N.J., assignor to Gen eral Chemical Company, New York, N. Y., a corporation of New York No Drawing. Application January 26, 1942, Serial No. 428,222. 10 Claims. (C. 23-5) This invention is directed to processes for mak cyanates by procedure according to the practice ing alkali metal thiocyanates. While the prin of which it is possible to produce alkali metal ciples of the improvements are applicable to thiocyanate crystals of greater purity than here manufacture of potassium thiocyanate, for con tofore, and further to effect such production of venience the invention is discussed largely in 5 high purity alkali metal thiocyanates without connection with production of sodium thiocy necessity of recrystallization, and without dis anate. card from the system of substantial quantities of In the most commonly used commercial meth mother liquor after separation of Crystallized al od for making sodium thiocyanate, a sodium cy kali metal thiocyanates. A further object of the anide Solution is reacted with sulfur in aqueous 0 invention is provision of methods by which the Suspension to form crude sodium thiocyanate liq foregoing object may be attained and at the same uor containing Substantial quantities of sodium time so-called off-grade alkali metal cyanides, compound impurities mostly as sodium carbonate, containing relatively large amounts of alkali net sodium sulfide and sodium hydroxide. In the prior all carbonate, sulfide, and hydroxide impurities, practice, such sodium thiocyanate solution is con may be used as Sources of alkali metal cyanide. centrated and solid sodium thiocyanate subse Since the sought-for alkali metal, thiocyanate quently recovered in crystal form. On account productS are formed by crystallization out of a of the high impurity content of the crude sodium liquor, this mode of Solid product, formation nec thiocyanate solution, the sodium thiocyanate essarily causes contamination of the crystals with Crystals obtained by crystallization are contam 20 impurities if the mother liquor from which the inated with substantial quantities of sodium car alkali metal thiocyanate is crystallized contains bonate and sodium sulfide. For example, first Substantial quantities of impurities. Hence, the Crop Crystals manufactured by this procedure problem presented is minimization of the im often contain 0.7-1.4% sodium carbonate and as purity content of the alkali metal thiocyanate so high as 0.02% sodium sulfide. If more nearly lution from which alkali metal thiocyanate crys pure sodium thiocyanate crystals are desired, it tals are formed. Such minimization in turn re is necessary to resort to expensive and cumber quires conversion of the alkali metal impurities Some recrystallization operations. Furthermore, in the Crude alkali netal thiocyanate liquor to a in the prior art method the sodium carbonate, form in which most of such impurities may be sulfide and hydroxide impurities build up in the 30 removed from the liquor before alkali metal thio mother liquor, from which sodium thiocyanate cyanate Crystallization is effected. is Crystallized, to such an extent that substantial In accordance with this invention, it has been quantities of mother liquor must be discarded found that by treating a crude alkali metal thio from time to time in order to obtain a sodium thio cyanate solution-containing alkali metal com cyanate product of reasonably suitable purity. pound impurities principally in the form of car It has not been feasible in the past to remove bonate, sulfide and hydroxide-with Sulfuric acid sodium compound impurities from crude sodium in a manner hereinafter described, it is possible thiocyanate liquors, prior to sodium thiocyanate to convert alkali metal compound impurities crystallization, by treating the crude iiquor partly to the form of gases which may be expelled with reagents such as calcium nitrate and lead 40 by heating and partly to alkali metal sulfate nitrate which precipitate carbonate and sulfide which may be removed from the alkali metal of the impurities as calcium carbonate and lead thiocyanate liquor, prior to crystallization of al sulfide because the Sodium nitrate simultaneously kali metal thiocyanate, to such an extent that formed is very soluble and cannot be taken out the alkali metal thiocyanate crystals subsequently of the liquor before crystallizing the sodium thio crystallized out of the liuqor are contaminated cyanate. Hence, the sodium nitrate remains in to only a very Small degree with alkali metal the sodium thiocyanate liquor and contaminates sulfate. Subsequently crystallized sodium thiocyanate to Returning to description of the invention in an extent comparable with the contamination connection with manufacture of sodium thiocy brought about by the presence of sodium carbon 50 anate, anhydrous or the dihydrate, the sulfuric ate, sodium sulfide and sodium hydroxide in liq acid treatment and subsequent steps of the inven uors from which sodium thiocyanate is crystal tion are applicable to treatment of crude sodium lized. thiocyanate solutions made according to any The primary object of this invention is provis known or convenient method. It will be under sion of methods for making alkali metal thio-. 55 stood the crude, sodium thiocyanate solutions m 2 2,318,680 formed by reaction of sodium cyanide and Sulfur acid treated liquor to 6.3, and preferably to 5 contain, even if pure sodium cyanide were used, which find to be the most satisfactory working substantial quantities of Sodium hydroxide and figure. While pH lower than 4.2 may be used sodium sulfide, the sodium hydroxide being in some instances, greater acidity is not required, formed by hydrolysis of sodium cyanide, and the and for pH values below 4.2 there is an apprecia sodium sulfide by side reactions involving reac ble tendency to decompose sodium thiocyanate tion of sulfur and sodium hydroxide. Since in in Some Operations. In this sulfuric acid treat practice the sodium cyanide employed is com ment step, Sodium carbonate is converted to so mercial sodium cyanide which contains substan dium sulfate and CO2, sodium sulfide to sodium tial quantities of Sodium carbonate, Sodium hy O Sulfate and H2S, and sodium hydroxide to sodi droxide and sodium cyanate impurities, the re um sulfate and water. I find that by so pro Sulting crude Sodium thiocyanate liquor Con ceeding, the sodium compound impurities present tains, in addition to the sodium hydroxide and in the crude thiocyanate liquor may be converted sodium sulfide formed during the Sodium cyanide partly to gases which are driven off as such and sulfur reaction, sodium carbonate and sodium partly to soluble sodium sulfate which is an im hydroxide impurities brought in with the Com purity having characteristics Such that most of mercial sodium cyanide and also sodium carbon it may be removed from the sodium thiocyanate ate formed by decomposition of sodium cyanate. liquor prior to crystallization of the sought-for Thus crude Sodium thiocyanate Solutions contain sodium thiocyanate products. Further, I am en as the major impurities sodium carbonate, So 20 abled to accomplish impurity removal from crude dium sulfide and Sodium hydroxide. While the sodium thiocyanate solution without decomposs sodium compound impurity content of the crude ing sodium thiocyanate. sodium thiocyanate liquor may obviously vary In carrying out the acid treatment step, Sul over a rather wide range because of differing Op furic acid of any strength may be employed. erating conditions and varying Sodium compound 25 However, to facilitate addition of sulfuric acid impurities contained in the initial SOdium cya to the crude sodium thiocyanate solution with anide, it may be said that typical, crude sodium . out control of rate of acid addition in order to thiocyanate solutions contain from 0.25 to 2.00% avoid local decomposition of sodium thiocyanate, Na2CO3, from 0.02 to 0.25% Na2S, and from nil it is preferred to use sulfuric acid of strength 30 not exceeding 40%. Following completion of ad to In0.25% manufacture NaOH. of sodium cyanide, it often dition of the sulfuric acid, any residual CO2 and happens that there are produced substantial HaS in the liquor may be expelled by agitation quantities of sodium cyanide in which the sodium or aeration preferably while the liquor is warm carbonate, Sodium hydroxide and sodium cyanate. or hot. The liquor is then preferably treated content is too high to satisfy commercial specif 35 with decolorizing carbon and filtered. cations. The nature of the present improvements The Kext step in the process comprises separa is such that this so-called off-grade sodium cy tion of sodium sulfate from the sodium thiocyan anide may be readily used as the Source of NaCN ate liquor. This is accomplished by evaporating in production of crude sodium thiocyanate Solt the liquor to a concentration not in excess of tion. 40 that at which, on cooling of the evaporated liq While the known sodium cyanide-sulfur reac uor to a temperature close to but above the tran tion is being carried out, temperatures are such sition point of anhydrous Sodium thiocyanate to as to decompose most of any sodium cyanate in the dihydrate, the thus cooled liquor is not sat purity present to sodium carbonate, and annonia, urated with respect to anhydrous sodium thio and CO2 both of which pass off as gases. On cyanate. - Sodium sulfate crystallized during completion of reaction, the mass is filtered to evaporation and cooling is then separated out of separate out excess Sulfur. If the filtrate con the liquor. tains any polysulfide, indicated by yellow color Appreciable decomposition of sodium thiocyan ation, the filtrate is heated, if cool, to tempera ate begins to take place at temperatures of about . ture of 85-105 C., and enough sodium cyanide 50 105 C. Hence, during evaporating and concen is added to reduce polysulfide to the colorless trating operations, temperatures in excess of 105 monosulfide, Na2S.
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