NO138653B - PROCEDURE FOR THE PREPARATION OF HYDRATED NICKEL SULPHATE - Google Patents
PROCEDURE FOR THE PREPARATION OF HYDRATED NICKEL SULPHATE Download PDFInfo
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- NO138653B NO138653B NO4512/73A NO451273A NO138653B NO 138653 B NO138653 B NO 138653B NO 4512/73 A NO4512/73 A NO 4512/73A NO 451273 A NO451273 A NO 451273A NO 138653 B NO138653 B NO 138653B
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- Prior art keywords
- nickel
- mother liquor
- chloride
- nickel sulfate
- solution
- Prior art date
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- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 title claims description 25
- 238000000034 method Methods 0.000 title claims description 16
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 26
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 21
- 239000012452 mother liquor Substances 0.000 claims description 19
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 14
- 239000013078 crystal Substances 0.000 claims description 14
- 238000009835 boiling Methods 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 8
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 5
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims description 5
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 3
- 239000011541 reaction mixture Substances 0.000 claims 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 20
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 13
- 229910052759 nickel Inorganic materials 0.000 description 10
- 229940053662 nickel sulfate Drugs 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 8
- 238000002425 crystallisation Methods 0.000 description 7
- 230000008025 crystallization Effects 0.000 description 7
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 3
- 239000000460 chlorine Substances 0.000 description 3
- 229910052801 chlorine Inorganic materials 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000000725 suspension Substances 0.000 description 3
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 2
- 238000005352 clarification Methods 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-M bisulphate group Chemical group S([O-])(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-M 0.000 description 1
- 239000001175 calcium sulphate Substances 0.000 description 1
- 235000011132 calcium sulphate Nutrition 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 210000000003 hoof Anatomy 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000000622 liquid--liquid extraction Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- RRIWRJBSCGCBID-UHFFFAOYSA-L nickel sulfate hexahydrate Chemical compound O.O.O.O.O.O.[Ni+2].[O-]S([O-])(=O)=O RRIWRJBSCGCBID-UHFFFAOYSA-L 0.000 description 1
- 229940116202 nickel sulfate hexahydrate Drugs 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 238000011197 physicochemical method Methods 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 239000001103 potassium chloride Substances 0.000 description 1
- 235000011164 potassium chloride Nutrition 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M sodium chloride Inorganic materials [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000012265 solid product Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000005670 sulfation reaction Methods 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 229910021653 sulphate ion Inorganic materials 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/10—Sulfates
Description
Foreliggende oppfinnelse vedrører en fremgangsmåte av den art The present invention relates to a method of that kind
som er angitt i krav l's ingress. For å fremstille det hydratiserte nikkelsulfat anvendes som utgangsmateriale en opp-løsning av rent nikkelklorid, eksempelvis erholdt i henhold til norsk patent nr. 130.436 el.ler nr. 131.895. which is stated in claim l's preamble. To produce the hydrated nickel sulphate, a solution of pure nickel chloride is used as starting material, for example obtained according to Norwegian patent no. 130,436 or no. 131,895.
Kjente prosesser for fremstilling av nikkelsulfat omfatter omsetning av nikkel eller et nikkelholdig materiale med svovelsyre. Disse prosesser har mange ulemper, som f.eks. be- Known processes for the production of nickel sulphate include reacting nickel or a nickel-containing material with sulfuric acid. These processes have many disadvantages, such as e.g. be-
hovet for å rense de erholdte oppløsningene ved fysikalske eller fysikalsk-kjemiske metoder. Ved enkelte av disse pro- the hoof to purify the obtained solutions by physical or physico-chemical methods. In some of these pro-
sesser fås dessuten en pastalignende fase som er vanskelig å håndtere. sessions, a paste-like phase is also obtained which is difficult to handle.
Fra US-patent nr. 2.902.341 er det eksempelvis kjent frem- From US patent no. 2,902,341, for example, it is known
stilling av metallsulfater ved omsetning av de tilsvarende klorider med sterk svovelsyre og med en etterfølgende full- position of metal sulphates by reacting the corresponding chlorides with strong sulfuric acid and with a subsequent full-
stendig fjernelse av frigjort hydrogenkloridgass. Imidler- constant removal of released hydrogen chloride gas. However-
tid er en fullstendig fjerning av den dannede hydroklorid- time is a complete removal of the formed hydrochloride
gass teknisk vanskelig og kostbar, spesielt når konsentra- gas is technically difficult and expensive, especially when concen-
sjonen av saltsyren er lav. Det fremgår av patentet at man tidligere har forsøkt å fjerne saltsyren ved hjelp av væske-væskeekstraksjon ved hjelp av høyere alkoholer som ekstrak-sjonsmiddel. tion of the hydrochloric acid is low. It appears from the patent that previous attempts have been made to remove the hydrochloric acid by means of liquid-liquid extraction using higher alcohols as extraction agent.
Fra engelsk patent nr. 1.145.389 er kjent en fremgangsmåte A method is known from English patent no. 1,145,389
for fremstilling av saltsyre og et bisulfat og/eller et sulfat ved å innføre natrium- eller kaliumklorid i et reaksjonskam- for the production of hydrochloric acid and a bisulphate and/or a sulphate by introducing sodium or potassium chloride into a reaction chamber
mer hvor reaksjonsmassen holdes ved en temepratur nær dens kokepunkt, og hvor svovelsyre tilføres reaksjonskaret og more where the reaction mass is kept at a temperature close to its boiling point and where sulfuric acid is added to the reaction vessel and
hydrogenklorid gjenvinnes fra den erholdte dampfase. hydrogen chloride is recovered from the vapor phase obtained.
De nevnte patenter vedrører imidlertid ikke fremstilling av hydratisert nikkelsulfat med lavt kloridinnhold, som eksempelvis er fordelaktig hvis det erholdte nikkelsulfat skal anvendes eksempelvis for fornikling. Ved foreliggende fremgangsmåte er energibehovet lite da en fullstendig avdestillering av svovelsyre ikke er nødvendig. Som det vil fremgå av det etterfølgende eksempel 2 er kloridinnholdet i det erholdte hydratiserte nikkelsuflat 0,5%, men denne kloridmengde kan senkes helt ned til 0,04% etter vasking med vann, dette til tross for at kloridkonsentrasjonen i moderluten var 130 g/l. However, the aforementioned patents do not relate to the production of hydrated nickel sulphate with a low chloride content, which is, for example, advantageous if the obtained nickel sulphate is to be used, for example, for nickel plating. In the present method, the energy requirement is low as complete distillation of sulfuric acid is not necessary. As will be seen from the following example 2, the chloride content in the hydrated nickel sulfate obtained is 0.5%, but this amount of chloride can be lowered all the way down to 0.04% after washing with water, this despite the fact that the chloride concentration in the mother liquor was 130 g/ l.
Det er meget overraskende at det er mulig å oppnå tilnærmet kloridfritt, hydratisert nikkelsulfat fra en relativt konsen-trert kloridinneholdende oppløsning, og ytterligere at dette kan oppnås med et realtivt lavt energiforbruk. It is very surprising that it is possible to obtain virtually chloride-free hydrated nickel sulphate from a relatively concentrated chloride-containing solution, and further that this can be achieved with relatively low energy consumption.
Ifølge foreliggende oppfinnelse er det fremskaffet en fremgangsmåte for fremstilling av hydratisert nikkelsulfat med lavt kloridinnhold, og fremgangsmåten er særpreget ved det som er angitt i krav l's karakteriserende del. According to the present invention, a method for the production of hydrated nickel sulphate with a low chloride content has been provided, and the method is characterized by what is stated in the characterizing part of claim 1.
Fremgangsmåten kan utføres på to alternative måter idet den totale svovel sy remengde holdes ved 1,5-3 eller 0,9 - Isgan-ger den støkiometriske mengde for å omdanne alt nikkelklorid til nikkelsulfat. De to alternative fremgangsmåter fremgår henholdsvis av eksemplene 1 og 2, samt under henvisning til den vedlagte tegning. The process can be carried out in two alternative ways, with the total amount of sulfur added being kept at 1.5-3 or 0.9 - times the stoichiometric amount to convert all the nickel chloride into nickel sulphate. The two alternative methods can be seen respectively from examples 1 and 2, and with reference to the attached drawing.
En ren nikkelkloridoppløsning, svovelsyre og moderlut 2 A pure nickel chloride solution, sulfuric acid and mother liquor 2
fra utfelling mates til sulfateringsreaksjonskar 1. Den totale mengden sovelsyre som innmates er mellom 1,5 og 3 ganger den støkiometriske mengde som kreves for å omdanne alt nikkelklorid, som mates til reaksjonskar 1, til nikkelsulfat. from precipitation is fed to sulfation reaction vessel 1. The total amount of sulfuric acid fed in is between 1.5 and 3 times the stoichiometric amount required to convert all nickel chloride, which is fed to reaction vessel 1, into nickel sulfate.
Da moderluten 2 normalt inneholder ubundet svovelsyre, tilsettes bare en supplerende mengde syre ved 1, og da syre av teknisk kvalitet. Reaksjonen som resulterer i dannelse av saltsyre utføres ved kokepunktet, og kan foretas ved at-mosfæretrykk, men utføres fortrinnsvis under redusert trykk As the mother liquor 2 normally contains unbound sulfuric acid, only a supplementary amount of acid is added at 1, and then acid of technical quality. The reaction that results in the formation of hydrochloric acid is carried out at the boiling point, and can be carried out at atmospheric pressure, but is preferably carried out under reduced pressure
som f.eks. 0,5 atm.. like for example. 0.5 atm..
Saltsyre dannet som gass i karet 1 fjernes f.eks. ved absorp-sjon i en foret eller belagt kolonne under resirkulering av en kondensatfraksjon. Etter fjerning av saltsyren blir den gjen-værende suspensjonen tatt ut og kjølt til romtemperatur ved 3, vist som enkle linjer i flyteskjemaet, og suspensjonen filtreres og vaskes med vann ved 4, og moderlut 2 resirkuleres til sulfateringsreaksjonskaret 1. Hydrochloric acid formed as gas in vessel 1 is removed, e.g. by absorption in a lined or coated column during recycling of a condensate fraction. After removal of the hydrochloric acid, the remaining suspension is taken out and cooled to room temperature at 3, shown as single lines in the flowchart, and the suspension is filtered and washed with water at 4, and mother liquor 2 is recycled to the sulphation reaction vessel 1.
Det faste produktet 5, som fås fra filtreringen ved 4, er delvis hydratisert nikkelsulfat som transporteres til et trinn 6 for gjenoppløsning i moderluten 7 eller i vann eller i moderluten 7 som er utspedd med vann. Etter oppkonsentrering blir oppløsningen klaret i kammeret 8, hvor forskjellige forurens-ninger, såsom kalsiumsulfat, kan skilles fra oppløsningen. Oppløsningen blir deretter krystallisert i 9, og de erholdte krystallene tørkes i 10 slik at man får krystaller av rent hydratisert nikkelsulfat som oppsamles ved 11. Moderluten fra krystallisasjonen i 9 og tørkingen i 10 utgjør moderluten 7, som ifølge ovenstående resirkuleres til trinnet 6 hvor gjen-oppløsning av det delvis hydratiserte nikkelsulfat 5 finner sted. The solid product 5 obtained from the filtration at 4 is partially hydrated nickel sulfate which is transported to a step 6 for redissolution in the mother liquor 7 or in water or in the mother liquor 7 diluted with water. After concentration, the solution is clarified in chamber 8, where various impurities, such as calcium sulphate, can be separated from the solution. The solution is then crystallized in 9, and the crystals obtained are dried in 10 so that crystals of pure hydrated nickel sulfate are obtained which are collected at 11. The mother liquor from the crystallization in 9 and the drying in 10 constitutes the mother liquor 7, which according to the above is recycled to step 6 where again -dissolution of the partially hydrated nickel sulfate 5 takes place.
Ved en modifisert utførelsesform av prosessen er den totale mengden ved 1 innmatede svovelsyre mellom 0,9 og 1,1 ganger (fremfor 1,5 - 3 ganger) den støkiometriske mengde, og det er mulig å eliminere trinnene som omfatter delvis hydra-tisering av nikkelsulfat 5 og gjenoppløsning 6. Her omfatter prosesstrinnene, som er angitt ved hjelp av doble linjer i flyteskjemaet, følgende: sulfatering 1, klaring 8, krystallisasjon 9 og tørking 10. Moderluten 7 resirkuleres fra 9 og 10 til sulfateringstrinnet 1. Krystallene av nikkelsulf.at-heksahydrat 11, som fås på denne måte, kan deretter vaskes med vann, med alkohol eller med en oppløsning av nikkelsulfat for å redusere deres kloridionekonsentrasjon. In a modified embodiment of the process, the total amount at 1 feed of sulfuric acid is between 0.9 and 1.1 times (rather than 1.5 - 3 times) the stoichiometric amount, and it is possible to eliminate the steps comprising partial hydration of nickel sulfate 5 and redissolution 6. Here, the process steps, which are indicated by means of double lines in the flow chart, include the following: sulphation 1, clarification 8, crystallization 9 and drying 10. The mother liquor 7 is recycled from 9 and 10 to the sulphation step 1. The crystals of nickel sulph. at-hexahydrate 11, obtained in this way, can then be washed with water, with alcohol or with a solution of nickel sulfate to reduce their chloride ion concentration.
Av etterfølgende eksempler, som beskrives under henvisning til vedlagte tegning, omfatter eksempel 1 den ovenfor beskrevne første utførelsesform, og er angitt ved hjelp av enkle linjer. Eksempel 2 vedrører den andre utførelsesformen, og er vist ved hjelp av doble linjer. Of the following examples, which are described with reference to the attached drawing, example 1 comprises the first embodiment described above, and is indicated by means of simple lines. Example 2 relates to the second embodiment, and is shown by means of double lines.
Eksempel 1 Example 1
109 1 av en oppløsning av nikkelklorid som inneholder 198 g/l nikkel, og 0,5 g/l sulfat-ioner innmates i et dobbelt-vegget reaksjonskar 1. Til dette kar tilsettes likeledes 85 1 moderlut 2 fra krystallisasjonen av delvis hydratisert sulfat, hvilket sulfat stammer fra en foregående syklus, og som inneholder 39 g/l nikkel samt 800 g/l sulfat-ioner. Til denne blanding tilsettes 35 kg 98 prosentig svovelsyre. Innholdet i reaktor 1 oppvarmes til kokepunkt under ettrykk på 0,5 atm. inntil man, og som et resultat av fordampningen og fjerningen av saltsyregass, får en klorid-ione-mengde i oppløsningen som tilsvarer ca. 3 g/l. Oppløsningen tilfores et kar 3 for kjbling under omrbring, og den erholdte suspensjon filtreres ved 4. Herved fås 58,5 kg partielt hydratiserte krystaller 5 av nikkelsulfat, som ble funnet å inneholde 30,65% nikkel og 0,023% klorid-ioner. Filtratet fra 4 utgjor moderlut 2, hvori klorid-konsentrasjonen 109 1 of a solution of nickel chloride containing 198 g/l nickel, and 0.5 g/l sulfate ions are fed into a double-walled reaction vessel 1. 85 1 of mother liquor 2 from the crystallization of partially hydrated sulfate is also added to this vessel, which sulfate originates from a previous cycle, and which contains 39 g/l nickel as well as 800 g/l sulfate ions. 35 kg of 98 percent sulfuric acid is added to this mixture. The contents of reactor 1 are heated to boiling point under a pressure of 0.5 atm. until, as a result of the evaporation and removal of hydrochloric acid gas, an amount of chloride ions in the solution corresponding to approx. 3 g/l. The solution is supplied to a vessel 3 for boiling under stirring, and the suspension obtained is filtered at 4. This gives 58.5 kg of partially hydrated crystals 5 of nickel sulfate, which were found to contain 30.65% nickel and 0.023% chloride ions. The filtrate from 4 constitutes mother liquor 2, in which the chloride concentration
er 3,76 g/l. is 3.76 g/l.
De nevnte 58,5 kg krystaller 5 blir gjenopplbst ved 6 i 60 1 moderlut 7 fra hydratisert sulfat-krystallisasjon, og som stammer fra en foregående syklus, hvoretter man fortynner med 200 1 vann. Etter klaring ved 8, konsentrasjon til en spesifikk vekt på 1,49, krystallisasjon ved 30°C i 9 og tbrking ved 10, The aforementioned 58.5 kg of crystals 5 are recrystallized at 6 in 60 1 of mother liquor 7 from hydrated sulfate crystallization, and which originate from a previous cycle, after which they are diluted with 200 1 of water. After clarification at 8, concentration to a specific gravity of 1.49, crystallization at 30°C in 9 and distillation at 10,
får man 55 kg nikkelsulfat-heksahydrat-krystaller 11, hvilke inneholder 0,006% klorid-ioner. Mengden av klorid-ioner i krystallisasjons-moderlut 7, og som fås i trinnene 9 og 10, er 1,14 g/l. 55 kg of nickel sulfate hexahydrate crystals 11 are obtained, which contain 0.006% chloride ions. The amount of chloride ions in crystallization mother liquor 7, which is obtained in steps 9 and 10, is 1.14 g/l.
Vektsanalyser av de ved 11 erholdte krystaller er fblgende: Weight analyzes of the crystals obtained at 11 are as follows:
Eksempel 2. Example 2.
1,5 1 av en opplosning av nikkelklorid, som inneholder 177 g/l nikkel, sammen med 450 g 93 prosentig svovelsyre innmates i et dobbelvegget reaksjonskar 1, som er utstyrt med et "nedover- 1.5 1 of a solution of nickel chloride, which contains 177 g/l nickel, together with 450 g of 93 percent sulfuric acid are fed into a double-walled reaction vessel 1, which is equipped with a "down-
rettet" kjblesystem. Blandingen holdes ved kokepunktet inntil det på grunn av fordampning og fjerning av HCl opptrer spor av ulbselig sulfat, hvoretter kjblingen fortsetter ved 8 under forsiktig omrbring. Hydratiserte krystaller adskilles ved 9 directed" boiling system. The mixture is kept at the boiling point until, due to evaporation and removal of HCl, traces of insoluble sulfate appear, after which boiling is continued at 8 with gentle stirring. Hydrated crystals are separated at 9
fra moderluten. Etter tbrking ved 10 erholdes nikkelsulfat- from the mother liquor. After boiling at 10, nickel sulfate is obtained
krystaller ved 11, og disse krystaller inneholder 21,7% nikkel og 0,5% klor, og konsentrasjonen av klor i moderluten 7 oppgår til 130 g/l. Analyse av krystallene 11 er for bvrig den samme som i eksempel 1. Klormengden minsker til 0,040% hvis disse kry- crystals at 11, and these crystals contain 21.7% nickel and 0.5% chlorine, and the concentration of chlorine in the mother liquor 7 amounts to 130 g/l. Analysis of the crystals 11 is otherwise the same as in example 1. The amount of chlorine decreases to 0.040% if these crystals
stallene 9 vaskes med vann for de tbrkes ved 10, og da ved anvendelse av forholdet 0,5 1 vann pr. kg hydratisert sulfat. the stables 9 are washed with water before they are bathed at 10, and then using the ratio 0.5 1 water per kg hydrated sulfate.
Det heksahydratiserte sulfat eller det heptahydratiserte sulfat The hexahydrated sulfate or the heptahydrated sulfate
kan erholdes etter bnske ved å justere krystallisasjonstempera- can be obtained as desired by adjusting the crystallization temperature
turen. I eksempel 1, hvor denne temperatur er 30°C, fås en blanding av disse 2 sulfat-typer, hvilket fremgår av det faktum at andelen av nikkel i produktet er 21,4%, mens det teoretisk skulle være 22,3% i rent heksahydratisert sulfat og 20,9% i rent heptahydratisert sulfat. the trip. In example 1, where this temperature is 30°C, a mixture of these 2 sulfate types is obtained, which is evident from the fact that the proportion of nickel in the product is 21.4%, while theoretically it should be 22.3% in pure hexahydrated sulfate and 20.9% in pure heptahydrated sulfate.
Denne fremgangsmåte gjor det mulig å gjenvinne saltsyren, This procedure makes it possible to recover the hydrochloric acid,
som kan anvendes for fremstilling av ytterligere mengder rent nikkelsulfat. which can be used for the production of further quantities of pure nickel sulphate.
Claims (3)
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
FR7242221A FR2207865B1 (en) | 1972-11-28 | 1972-11-28 |
Publications (2)
Publication Number | Publication Date |
---|---|
NO138653B true NO138653B (en) | 1978-07-10 |
NO138653C NO138653C (en) | 1978-10-18 |
Family
ID=9107827
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
NO4512/73A NO138653C (en) | 1972-11-28 | 1973-11-27 | PROCEDURE FOR THE PREPARATION OF HYDRATED NICKEL SULPHATE |
Country Status (18)
Country | Link |
---|---|
JP (1) | JPS5412919B2 (en) |
AU (1) | AU472359B2 (en) |
BE (1) | BE807618A (en) |
BR (1) | BR7309318D0 (en) |
CA (1) | CA994986A (en) |
DE (1) | DE2358728C3 (en) |
ES (1) | ES420949A1 (en) |
FI (1) | FI59236C (en) |
FR (1) | FR2207865B1 (en) |
GB (1) | GB1440679A (en) |
GT (1) | GT197745590A (en) |
IT (1) | IT1001448B (en) |
LU (1) | LU68856A1 (en) |
NL (1) | NL7316210A (en) |
NO (1) | NO138653C (en) |
SE (1) | SE390725B (en) |
ZA (1) | ZA738988B (en) |
ZM (1) | ZM18173A1 (en) |
Families Citing this family (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS57147865A (en) * | 1981-03-05 | 1982-09-11 | Mazda Motor Corp | Connecting structure for battery |
JP6103017B2 (en) * | 2015-10-29 | 2017-03-29 | 住友金属鉱山株式会社 | Nickel sulfate crystallization equipment and crystallization method |
-
1972
- 1972-11-28 FR FR7242221A patent/FR2207865B1/fr not_active Expired
-
1973
- 1973-11-21 BE BE138009A patent/BE807618A/en unknown
- 1973-11-22 GB GB5436873A patent/GB1440679A/en not_active Expired
- 1973-11-23 FI FI3613/73A patent/FI59236C/en active
- 1973-11-26 ZA ZA738988A patent/ZA738988B/en unknown
- 1973-11-26 LU LU68856A patent/LU68856A1/xx unknown
- 1973-11-26 DE DE2358728A patent/DE2358728C3/en not_active Expired
- 1973-11-27 JP JP13423173A patent/JPS5412919B2/ja not_active Expired
- 1973-11-27 CA CA186,826A patent/CA994986A/en not_active Expired
- 1973-11-27 IT IT12959/73A patent/IT1001448B/en active
- 1973-11-27 AU AU62917/73A patent/AU472359B2/en not_active Expired
- 1973-11-27 BR BR9318/73A patent/BR7309318D0/en unknown
- 1973-11-27 NL NL7316210A patent/NL7316210A/xx unknown
- 1973-11-27 ZM ZM181/73A patent/ZM18173A1/en unknown
- 1973-11-27 NO NO4512/73A patent/NO138653C/en unknown
- 1973-11-27 SE SE7316012A patent/SE390725B/en unknown
- 1973-11-28 ES ES420949A patent/ES420949A1/en not_active Expired
-
1977
- 1977-03-09 GT GT197745590A patent/GT197745590A/en unknown
Also Published As
Publication number | Publication date |
---|---|
JPS5412919B2 (en) | 1979-05-26 |
BR7309318D0 (en) | 1974-08-29 |
FR2207865B1 (en) | 1976-04-23 |
DE2358728B2 (en) | 1978-11-02 |
ZA738988B (en) | 1974-10-30 |
AU6291773A (en) | 1975-05-29 |
FI59236C (en) | 1981-07-10 |
GB1440679A (en) | 1976-06-23 |
ES420949A1 (en) | 1976-04-16 |
SE390725B (en) | 1977-01-17 |
LU68856A1 (en) | 1975-08-20 |
NO138653C (en) | 1978-10-18 |
JPS4995895A (en) | 1974-09-11 |
AU472359B2 (en) | 1976-05-20 |
FR2207865A1 (en) | 1974-06-21 |
IT1001448B (en) | 1976-04-20 |
FI59236B (en) | 1981-03-31 |
NL7316210A (en) | 1974-05-30 |
DE2358728A1 (en) | 1974-05-30 |
ZM18173A1 (en) | 1974-10-21 |
GT197745590A (en) | 1978-08-31 |
CA994986A (en) | 1976-08-17 |
BE807618A (en) | 1974-03-15 |
DE2358728C3 (en) | 1979-06-21 |
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