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SE451999B - Ferric sulphate prodn. - Google Patents

Ferric sulphate prodn.

Info

Publication number
SE451999B
SE451999B SE8304826A SE8304826A SE451999B SE 451999 B SE451999 B SE 451999B SE 8304826 A SE8304826 A SE 8304826A SE 8304826 A SE8304826 A SE 8304826A SE 451999 B SE451999 B SE 451999B
Authority
SE
Sweden
Prior art keywords
sulfuric acid
fe2o3
concentration
filtered
weight
Prior art date
Application number
SE8304826A
Other languages
Swedish (sv)
Other versions
SE8304826L (en
SE8304826D0 (en
Inventor
R Bernhard
I Eriksson
Original Assignee
Stora Kopparbergs Bergslags Ab
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Stora Kopparbergs Bergslags Ab filed Critical Stora Kopparbergs Bergslags Ab
Priority to SE8304826A priority Critical patent/SE451999B/en
Publication of SE8304826D0 publication Critical patent/SE8304826D0/en
Priority to FI843491A priority patent/FI74691C/en
Priority to NO843567A priority patent/NO159374C/en
Publication of SE8304826L publication Critical patent/SE8304826L/en
Publication of SE451999B publication Critical patent/SE451999B/en

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00Compounds of iron
    • C01G49/14Sulfates

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Compounds Of Iron (AREA)
  • Primary Cells (AREA)
  • Electrolytic Production Of Metals (AREA)
  • Secondary Cells (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
  • Catalysts (AREA)

Abstract

The concentration of sulphuric acid is 35-45 wt.% and the ferric oxide is finepowdered. The amount of ferric oxide is esp. around 110% of the stoichiometric quantity. They are reacted at esp. 105-110 deg.C 90-100 % of the sulphuric acid is concurred. Any remaining solid material is separated and the remelting solution contains ferric sulphate. It can be diluted with water to at the most 47 wt% esp. 40-45% wt.% as Fe2(SO4)3.

Description

451 999- 2 Sättet att framställa järn(III)-sulfat i form av en stabil lösning kännetecknas enligt uppfinningen av att svavel- syra med en koncentration av 35 - 45 vikts-% och finkornigr järn(III)-oxid i ett Fe2O3-HZSO4-förhållande svarande mot 100 - 150, företrädesvis 105 - 120 %, speciellt omkring 110 % av stökiometrisk mängd får reagera vid en temperatur av minst 1oo°c, företrädesvis 1oo - 12s°c, speciellt 105 -_11o°c~t111g dess att minst 85 %, företrädesvis 90 - 100 % av svavelsyran förbrukats, varefter återstående fast material avskiljes och '-erhâllen lösning innehållande järn(III)-sulfat, om så erford- ras, späds med vatten till en koncentration av högst 47vüds-%, företräaesvis 40 - 45 vikts-% sam Fe2(so ) - * 4 3 Primärt erhålles enligt uppfinningen en järn(III)-sulfat- lösning med 40 - 52 % Fe2(SO4)3. För att uppnå stabila lös- ningar späds primärt erhållna lösningar med en koncentration _över 47 % Fe2(SO4)3 med vatten till koncentrationen 47 % eller lägre. _ För att uppnå en hög omsättning av svavelsyra 90 - 100 % är det av största vikt att hålla hög temperatur, minst 100°C. WS Med ett måttligt överskott, av järn(III)-oxid, ca 10 %, kan reaktionshastigheten och syraomsättningen ökas högst väsent- ligt. Sålunda kan 90 - 100 % svavelsyraomsättning uppnås inom 10 - 20 timmars reaktionstid. . The method of preparing ferrous sulphate in the form of a stable solution is characterized according to the invention by sulfuric acid having a concentration of 35-45% by weight and fine-grained ferric oxide in a Fe 2 O 3 -H 2 SO 4 ratio corresponding to 100 - 150, preferably 105 - 120%, especially about 110% of the stoichiometric amount is allowed to react at a temperature of at least 100 ° C, preferably 100-125 ° C, especially 105 -110 ° C until at least 85%, preferably 90-100% of the sulfuric acid is consumed, after which the remaining solid is separated and the solution containing ferrous sulphate, if required, is diluted with water to a concentration of not more than 47% by weight, preferably 40%. - 45 wt. In order to achieve stable solutions, primarily obtained solutions are diluted with a concentration above 47% Fe 2 (SO 4) 3 with water to a concentration of 47% or lower. In order to achieve a high turnover of sulfuric acid 90 - 100%, it is of the utmost importance to maintain a high temperature, at least 100 ° C. WS With a moderate excess of ferric oxide, about 10%, the reaction rate and acid turnover can be increased very significantly. Thus, 90 - 100% sulfuric acid conversion can be achieved within 10 - 20 hours reaction time. .

Med liten partikelstorlek påverkas reaktionshastigheten' positivt men återstående oreagerat fast material blir mycket svârfiltrerat. Med hänsyn härtill användes med fördel ett järnoxidmaterial med en partikelstorlek i Qmrådet 0,01 - 0,05 mm) Filtreringen försvåras även genom hög svavelsyrakoncentra- tion och lång reaktionstid. Vid svavelsyrakoncentrationer i närheten av övre gränsen av intervallet 35.- 45 vikts-% bör därför reaktionen avbrytas,_innan all svavelsyra förbrukats.With a small particle size, the reaction rate is positively affected, but the remaining unreacted solid material becomes very difficult to filter. In view of this, an iron oxide material with a particle size in the range 0.01 - 0.05 mm is advantageously used. The filtration is also made more difficult by high sulfuric acid concentration and long reaction time. Therefore, at sulfuric acid concentrations in the vicinity of the upper limit of the 35-45% by weight range, the reaction should be stopped before all sulfuric acid has been consumed.

Uppfinningen kommer i det följande att illustreras yt- terligare med hjälp av ett antal utföringsexempel.The invention will be further illustrated in the following by means of a number of exemplary embodiments.

Exempel_ Allmänt Försöken enligt Exempel 1 - 5 samt I utfördes i ett 50 liters slutet reaktionskärl försett med elektriskt värme-_ _/ 451 999 th) i element, temperaturreglering och omrörare. I reaktionskärlet satsades bestämda mängder av vatten, kisaska och sist kon- I centrerad svavelsyra (96 %Fig). Vid tillsatsen av svavelsyra steg temperaturen hastigt till kokpunkten och justerades sedan in på önskat värde med hjälp av temperaturreglerings- utrustningen.Example_ General The experiments according to Examples 1-5 and I were carried out in a 50 liter closed reaction vessel equipped with electric heating (451,999 th) in elements, temperature control and stirrer. In the reaction vessel, certain amounts of water, kis ash and finally concentrated sulfuric acid (96% Fig) were charged. During the addition of sulfuric acid, the temperature rose rapidly to the boiling point and was then adjusted to the desired value with the aid of the temperature control equipment.

Exempel_1 10 kg kisaska med partikelstorlek < 0,01 mm och 86 % Fe203 innehåll, 25 kg vatten och 16,5 kg konc. svavelsyra satsades, S04 och Fe 0 och en 2 2 3 svavelsyrakoncentration av 38 %. Temperaturen hölls strax under vilket innebär stökiometriska mängder H kokpunkten,ca 107°C. Prover tagna under försöket gav följande du resultat : 7 .Example_1 10 kg of kis ash with particle size <0.01 mm and 86% Fe 2 O 3 content, 25 kg of water and 16.5 kg of conc. sulfuric acid was charged, SO 4 and Fe 2 and a sulfuric acid concentration of 38%. The temperature was kept just below which means stoichiometric amounts of H boiling point, about 107 ° C. Samples taken during the experiment gave the following results: 7.

Reaxtionstia h 3 ' e zo Syraomsättning % _ 68,5 |85,2 97,2 Halt Fe2(SO4)3 2 34,2 39,7 45,9 _ Filtrerharhet svår- svårf ' mycket svârf filtrerat filtrerat 0 filtrerat _ Exempel 2.. g V " 10 kg kisaska med partikelstorlek 0,01 - 0,05 mm och 884% Fe2O3 innehåll, 26 kg vatten, 12 kg konc. svavelsyra sat- sades, vilket innebär stökiometriska mängder HZSO4 och Fe2O3 och en svavelsyrakoncentration av 38 %. Temperaturen hölls vid ca 107°C. Följande resultat erhölls : Reaktionstid h 4 - 8 20 7 Syraomsättningu % 67,0 81,1 ' 88,2 Halt Fe2(SO4)3 % 33,4 37,9 40,4 Filtrerbarhet lätt- lätt- tämligen filtrerat filtrerat lättfiltrerat' Exempel 3 10 kg kisaska med partikelstorlek 0,01 - 0,05 mm och 88 % Fe2O3, 19 kg vatten, 17 kg konc, svavelsyra satsades, vilket, innebär stökiometriska mängder HZSO4 och Fe203 och en svavel- syrakoncenfiration av 45 %. _Temperaturen hölls_vid ca 115oC (dvs strax under kokpunkten). Resultat : 451 999 4 Reaktibnstid h 3 46 18 syraomsättning % 69,6 ,_ ss 4 93,4 Halt Fe2(SQ4)3 % 38,3 _ 745,7 48,4 - Filtrerbarhet tämligen tämligen svår- lätt- lätt- filtrerat filtrerat filtrerat ExemQel'4 överskott av klsaska, svavelsyrakoncentration 38 %, 10 kg kisaska med fiartikelstorlek 0,01 - 0,05 mm och 88 % Fe203, 23 kg vatten, 15 kg konc. svavelsyra satsades, vilket innebär överskott av kisaska och en svavelsyrakoncentration av 38 %.Reaction time h 3 'e zo Acid conversion% _ 68.5 | 85.2 97.2 Content Fe2 (SO4) 3 2 34.2 39.7 45.9 _ Filter hardness difficult- difficult very difficult filtered filtered 0 filtered _ Example 2 .. g V "10 kg kis ash with particle size 0.01 - 0.05 mm and 884% Fe2O3 content, 26 kg water, 12 kg conc. sulfuric acid was added, which means stoichiometric amounts of HZSO4 and Fe2O3 and a sulfuric acid concentration of 38% The temperature was maintained at about 107 DEG C. The following results were obtained: Reaction time h 4 - 8 20 7 Acid turnover% 67.0 81.1 '88.2 Content Fe2 (SO4) 3% 33.4 37.9 40.4 Filterability easy Example 3 10 kg of kis ash with a particle size of 0.01 - 0.05 mm and 88% Fe 2 O 3, 19 kg of water, 17 kg of conc, sulfuric acid was charged, which means stoichiometric amounts of H 2 SO 4 and Fe 2 O 3 and a sulfur - acid concentration of 45% _The temperature was maintained_ at about 115oC (ie just below boiling point) Result: 451 999 4 Reactive time h 3 46 18 acid turnover% 69.6, _ ss 4 93.4 Content Fe2 (SQ4 ) 3% 38.3 _ 745.7 48.4 - Filterability rather rather difficult- easy- easily- filtered filtered filtered ExemQel'4 excess klsaska, sulfuric acid concentration 38%, 10 kg kisaske with fi article size 0.01 - 0.05 mm and 88% Fe 2 O 3, 23 kg water, 15 kg conc. sulfuric acid was invested, which means excess kisaska and a sulfuric acid concentration of 38%.

Temperaturen hölls vid ca 107°C. Försöket gav som resultat : Reaktionstid h 4 ' _ 8 20 Syraomsättning % 77,6 - 0 90,8_ 99,3 Halt Fe2(so4)3_% 36,1 }_ 42,5 47,6 Filtrerbarhet lätt- lätt- 1 lätt- filtrerat filtrerat filtrerat Exempel'5 Som i exempel 4 men med övertryck, temperatur ca 120°C.The temperature was maintained at about 107 ° C. The experiment gave as a result: Reaction time h 4 '_ 8 20 Acid turnover% 77.6 - 0 90.8_ 99.3 Content Fe2 (so4) 3_% 36.1} _ 42.5 47.6 Filterability easy- easy- 1 easy filtered filtered filtered Example '5 As in Example 4 but with overpressure, temperature approx. 120 ° C.

Resultat : Reaktionstid h 2 * 5 " 10 Syraomsättning % 70,80 ' 91,3 98,7 Halt Fe2(SO4)3 % 34,5 m - 43,2 46,9 Filtrerbarhet. _ lätt- lätt- lätt- filtrerat filtrerat filtrerat Exempel I Kjämförelseförsök) Som i exempel 4 men med en temperatur av ca 90oC. Resultat: Reaktionstia 5 5 10 _ - 22 Syraomsättning 1% 52,1 I 67,4 ~ 75,6 Halt re2(so4)3 % 26,2 32,9' 35,0 Piltrerbarhet* l lätt- 'e lätt- lätt- filtrerat' filtrerat }f11treratResult: Reaction time h 2 * 5 "10 Acid turnover% 70.80 '91.3 98.7 Content Fe2 (SO4) 3% 34.5 m - 43.2 46.9 Filterability. _ Easy- easy- easy- filtered filtered filtered Example I Comparative experiment) As in Example 4 but with a temperature of about 90 ° C. Result: Reaction path 5 5 10 _ - 22 Acid turnover 1% 52.1 I 67.4 ~ 75.6 Content re2 (so4) 3% 26.2 32.9 '35.0 Filterability * l easily-' e easily- easily- filtered 'filtered} filtered

Claims (2)

1. 451 999 PATENTK RAV , ' 1, Sätt att framställa järn(III)Fsulfat genom inverkan av svavelsyra på Fe2O3, k ä n n e¶t e c k n a_t _a v att svavelsyra med en koncentration av 35 - 45 vikts-% och fin- kornig Fe203 i ett Fe203 - HZSOÅ-förhållande svarande mot ' 100 - 150 %, företrädesvis 105 - 120 %, speciellt omkring 110 % av stökíometrisk mängd får reagera vid en temperatur av minst 1oo°c, företrädesvis 1oo - 12s°c, speciellt 105 - 11o°c, till dess att minst 85 %, företrädesvis 90 -'100 % av svavel- syran förbrukats, varefter återstående fast material avskiljes och erhâllen lösning innehållande järn(III)-snlfat, om så er- fordras, späds med vatten till en koncentration av högst 47 vikts-%, företrädesvis 40 e 45 vikts-% som Fe2(SO4)3.1. 451 999 PATENTK RAV, '1, Method of producing iron (III) Sulphate by the action of sulfuric acid on Fe2O3, characterized by sulfuric acid with a concentration of 35 - 45% by weight and fine-grained Fe2O3 in a Fe 2 O 3 - H 2 SO 4 ratio corresponding to '100 - 150%, preferably 105 - 120%, especially about 110% of the stoichiometric amount is allowed to react at a temperature of at least 100 ° C, preferably 100-125 ° C, especially 105-110 ° ° C, until at least 85%, preferably 90-100% of the sulfuric acid has been consumed, after which the remaining solid is separated and the resulting solution containing ferrous sulfate, if required, is diluted with water to a concentration of at most 47% by weight, preferably 40 and 45% by weight as Fe2 (SO4) 3. 2. sätt enligt krav 1, k ä n n s't s c k nda t a v ' 0 att som Fe2O3 användes en kïsaskafraktion med partikelstorleken 0,01 - 0,05 mm eller Fe2O3 från betbadsregenerering.2. A method according to claim 1, characterized in that as Fe2O3 a cheese ash fraction with a particle size of 0.01 - 0.05 mm or Fe2O3 from beet bath regeneration is used.
SE8304826A 1983-09-08 1983-09-08 Ferric sulphate prodn. SE451999B (en)

Priority Applications (3)

Application Number Priority Date Filing Date Title
SE8304826A SE451999B (en) 1983-09-08 1983-09-08 Ferric sulphate prodn.
FI843491A FI74691C (en) 1983-09-08 1984-09-06 Methods of preparing iron (III) sulfate
NO843567A NO159374C (en) 1983-09-08 1984-09-07 PROCEDURE FOR THE PREPARATION OF IRON (III) SULPHATE.

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
SE8304826A SE451999B (en) 1983-09-08 1983-09-08 Ferric sulphate prodn.

Publications (3)

Publication Number Publication Date
SE8304826D0 SE8304826D0 (en) 1983-09-08
SE8304826L SE8304826L (en) 1985-03-09
SE451999B true SE451999B (en) 1987-11-09

Family

ID=20352415

Family Applications (1)

Application Number Title Priority Date Filing Date
SE8304826A SE451999B (en) 1983-09-08 1983-09-08 Ferric sulphate prodn.

Country Status (3)

Country Link
FI (1) FI74691C (en)
NO (1) NO159374C (en)
SE (1) SE451999B (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1067095A1 (en) * 1999-07-08 2001-01-10 Taki Chemical Co., Ltd. A method for the manufacture of ferric sulfate solution and a water treatment agent using the same
CN100335420C (en) * 2005-09-27 2007-09-05 暨南大学 Production process of solid composite ferric sulfate polymer

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1067095A1 (en) * 1999-07-08 2001-01-10 Taki Chemical Co., Ltd. A method for the manufacture of ferric sulfate solution and a water treatment agent using the same
US6375919B1 (en) 1999-07-08 2002-04-23 Taki Chemical Co., Ltd. Method for the manufacture of ferric sulfate solution and a water treatment agent using the same
CN100335420C (en) * 2005-09-27 2007-09-05 暨南大学 Production process of solid composite ferric sulfate polymer

Also Published As

Publication number Publication date
NO843567L (en) 1985-03-11
FI843491L (en) 1985-03-09
FI843491A0 (en) 1984-09-06
FI74691B (en) 1987-11-30
NO159374C (en) 1988-12-21
FI74691C (en) 1993-06-05
NO159374B (en) 1988-09-12
SE8304826L (en) 1985-03-09
SE8304826D0 (en) 1983-09-08

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