NO892598L - PROCEDURE FOR THE PREPARATION OF TIN (II) SULPHATE. - Google Patents
PROCEDURE FOR THE PREPARATION OF TIN (II) SULPHATE.Info
- Publication number
- NO892598L NO892598L NO89892598A NO892598A NO892598L NO 892598 L NO892598 L NO 892598L NO 89892598 A NO89892598 A NO 89892598A NO 892598 A NO892598 A NO 892598A NO 892598 L NO892598 L NO 892598L
- Authority
- NO
- Norway
- Prior art keywords
- tin
- copper
- sulphate
- solution
- precipitate
- Prior art date
Links
- 238000000034 method Methods 0.000 title claims description 15
- OBBXFSIWZVFYJR-UHFFFAOYSA-L tin(2+);sulfate Chemical compound [Sn+2].[O-]S([O-])(=O)=O OBBXFSIWZVFYJR-UHFFFAOYSA-L 0.000 title claims description 7
- 238000002360 preparation method Methods 0.000 title description 4
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 31
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 22
- 229910052802 copper Inorganic materials 0.000 claims description 21
- 239000010949 copper Substances 0.000 claims description 21
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 16
- 238000006243 chemical reaction Methods 0.000 claims description 16
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 15
- FAKFSJNVVCGEEI-UHFFFAOYSA-J tin(4+);disulfate Chemical compound [Sn+4].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O FAKFSJNVVCGEEI-UHFFFAOYSA-J 0.000 claims description 12
- 239000002244 precipitate Substances 0.000 claims description 10
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 8
- 230000003647 oxidation Effects 0.000 claims description 7
- 238000007254 oxidation reaction Methods 0.000 claims description 7
- 239000007789 gas Substances 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 239000000428 dust Substances 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 3
- 230000001681 protective effect Effects 0.000 claims description 3
- 229910000375 tin(II) sulfate Inorganic materials 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims 1
- 229910021653 sulphate ion Inorganic materials 0.000 claims 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 229910000365 copper sulfate Inorganic materials 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 239000012065 filter cake Substances 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 230000007306 turnover Effects 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 1
- SCZFCWIBJIAITP-UHFFFAOYSA-H S(=O)(=O)([O-])[O-].[Cu+2].[Sn+4].S(=O)(=O)([O-])[O-].S(=O)(=O)([O-])[O-] Chemical compound S(=O)(=O)([O-])[O-].[Cu+2].[Sn+4].S(=O)(=O)([O-])[O-].S(=O)(=O)([O-])[O-] SCZFCWIBJIAITP-UHFFFAOYSA-H 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 229910001431 copper ion Inorganic materials 0.000 description 1
- BQJTUDIVKSVBDU-UHFFFAOYSA-L copper;sulfuric acid;sulfate Chemical compound [Cu+2].OS(O)(=O)=O.[O-]S([O-])(=O)=O BQJTUDIVKSVBDU-UHFFFAOYSA-L 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G19/00—Compounds of tin
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Electrolytic Production Of Metals (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Glass Compositions (AREA)
- Catalysts (AREA)
- Ceramic Products (AREA)
Description
Foreliggende oppfinnelse vedrører fremgangsmåte for fremstilling av tinn(II)-sulfat, der tinn blir tilsatt en svovelsur kobbersulfatoppløsning. The present invention relates to a method for the production of tin (II) sulphate, where tin is added to a sulfuric acid copper sulphate solution.
En slik fremgangsmåte er kjent (J.D. Donaldson og W. Moser i J. Chem. Soc. London 1960, 4000): Etter tilsetning av metallisk tinn, blir oppløsningen kokt og dermed utfelles kobberet. Ved slutten av reaksjonen blir oppløsningen fargeløs. Ved det blir bunnfallet farget grått, fordi tinn blir utfelt på overflaten av kobberet. På dette tidspunkt blir oppløsningen raskt filtrert og konsentrert. Det på kobberbunnfallet igjen utfelte tinnet reduserer omsetnings-hastigheten mellom kobber og tinn. Such a procedure is known (J.D. Donaldson and W. Moser in J. Chem. Soc. London 1960, 4000): After adding metallic tin, the solution is boiled and thus the copper is precipitated. At the end of the reaction, the solution becomes colorless. In doing so, the precipitate is colored gray, because tin is precipitated on the surface of the copper. At this point, the solution is quickly filtered and concentrated. The tin that has re-precipitated on the copper precipitate reduces the turnover rate between copper and tin.
Til grunn for oppfinnelsen ligger den oppgave å tilveiebringe en fremgangsmåte av den Innledningsvis nevnte art hvor tapene av tinn er vesentlig redusert. The invention is based on the task of providing a method of the type mentioned in the introduction in which the losses of tin are substantially reduced.
Denne oppgave blir derigjennom løst ved at tinnstøv blir anvendt. Oppfinnelsen legger følgende overveielse til grunn: Tinntapet kan tilbakeføres til kokingen av kobbersulfat-tinn-oppløsningen. En fra en høyere omsetningsrate mellom kobber og tinn resulterende reduksjon av tinntapet kan derved oppnås når reaksjonen forløper ved en lavere temperatur. For å oppnå en praktisk brukbar reaksjonshastighet for omsetningen mellom kobbersulfat og tinn, er derfor i foreliggende oppfinnelse tinnets overflate økt, ved at meget finfordelt tinnstøv blir anvendt. Derigjennom finner reaksjonen sted med i praksis brukbar reaksjonshastighet allerede ved rom-temperatur. Ved at oppløsningen nå ikke lenger mer trenger å kokes, adskiller det allerede omsatte tinnet seg ikke Igjen fra kobbersulfatet. Det er fastslått ifølge foreliggende oppfinnelses fremgangsmåte at nesten 1:1-omsetning mellom kobber og tinn er oppnåelig. This task is thereby solved by using tin dust. The invention is based on the following consideration: The loss of tin can be attributed to the boiling of the copper sulphate-tin solution. A reduction of the tin loss resulting from a higher conversion rate between copper and tin can thereby be achieved when the reaction proceeds at a lower temperature. In order to achieve a practically usable reaction rate for the reaction between copper sulphate and tin, the tin's surface is therefore increased in the present invention by using very finely divided tin dust. As a result, the reaction takes place with a practically usable reaction rate already at room temperature. As the solution no longer needs to be boiled, the already reacted tin does not separate again from the copper sulphate. It has been determined according to the method of the present invention that almost 1:1 conversion between copper and tin is achievable.
For å forbruke minst mulig kobber ved en gjentatt fremstilling av tinnsulfatoppløsning eller av tinnsulfat i en annen form, foreslås det at den for fremstilling av ytterligere tinnsulfat påkrevde kobbersulfatoppløsning fremstilles ved oksidasjon av bunnfallet fraskilt fra den tidligere tinnsulfatoppløsningen, omsetning av bunnfallet med svovelsyre og adskillelse av det derved oppnådde kobbersulfatet fra resten av bunnfallet. Hovedandelen av kobberet blir så gjenanvendt. En tilsvarende mengde kobber blir dermed innspart. Også avfallsproblemene blir derigjennom mindre. In order to consume as little copper as possible during a repeated preparation of tin sulphate solution or of tin sulphate in a different form, it is proposed that the copper sulphate solution required for the manufacture of further tin sulphate is produced by oxidation of the precipitate separated from the previous tin sulphate solution, reaction of the precipitate with sulfuric acid and separation of the copper sulphate thus obtained from the rest of the precipitate. The main part of the copper is then recycled. A corresponding amount of copper is thus saved. As a result, the waste problems are also reduced.
For å unngå, ved gjenanvendelse av kobberet, at en del av tinnet som skal tilsettes oksideres av resten av oksidasjons-midlet som er tilsatt for å bevirke den forutgående oksidasjon av kobberet, og på denne måten går tapt for reaksjonen mellom kobbersulfat og tinn, forelås det at det fra det tidligere utfelte tinnsulfat adskilte bunnfallet oksideres med hydrogenperoksid, hvis ikke-omsatte andel deretter spaltes ved oppvarming. In order to avoid, when reusing the copper, that part of the tin to be added is oxidized by the rest of the oxidizing agent that has been added to cause the prior oxidation of the copper, and in this way is lost to the reaction between copper sulfate and tin, it is proposed the fact that the precipitate separated from the previously precipitated tin sulphate is oxidized with hydrogen peroxide, the unreacted portion of which is then decomposed by heating.
For å undertrykke oksidasjon av tinn med luftens oksygen eller med oksygen oppløst i vann, foreslås det at fremgangsmåten gjennomføres under oksygenfri beskyttelsesgass. In order to suppress oxidation of tin with the oxygen of the air or with oxygen dissolved in water, it is suggested that the process be carried out under an oxygen-free shielding gas.
For å beholde en klor- og kobberionefrI tinnsulfatoppløsning, foreslås det I fremgangsmåten at høyrent elektrolyttkobber blir anvendt i fremstilling av kobbersulfatoppløsningen. For renheten av tinnsulfatoppløsningen er det på samme måte også fordelaktig når mest mulig rent tinnpulver blir anvendt. In order to keep a tin sulphate solution free of chlorine and copper ions, it is proposed in the method that high-purity electrolytic copper is used in the preparation of the copper sulphate solution. For the purity of the tin sulphate solution, it is likewise advantageous when the purest possible tin powder is used.
For å oppnå en kobbersulfatfri tinnsulfatoppløsning, er det nødvendig med en fullstendig omsetning av kobber. Derfor foreslås det at et ubetydelig overskudd av tinn tilsettes. In order to obtain a copper sulfate-free tin sulfate solution, a complete conversion of copper is necessary. It is therefore suggested that a negligible excess of tin be added.
I det følgende beskrives et utføringseksempel på oppfinnelsen ved hjelp av det på figuren angitte flytskjemaet. In the following, an embodiment of the invention is described using the flow chart shown in the figure.
Målet er fremstilling av en ca. 10,7 vekt-# tinn(II)-sulfatoppløsning. Samtlige reaksjonsforløp blir gjennomført under nitrogenbeskyttelsesgass. For fremstilling av kobber-sulf atoppløsningen anbringes, etter hverandre fullstendig deionisert vann, svovelsyre og kobberpulver under omrøring, I den nitrogenspylte reaksjonsbeholderen. Deretter følger tilsats av hydrogenperoksid. Doseringen gjennomføres på den måten at kartemperaturen ikke overstiger 70-75<0>C som er spaltningstemperaturen til hydrogenperoksid. Etter fullstendig oksidasjon av kobber, blir kobbersulfatoppløsningen opphetet til en temperatur over 85°C, slik at ennå foreliggende hydrogenperoksid spaltes termisk. Denne kobbersul-fatoppløsning blir tilslutt kjølt til ca. 20° C under nitrogengass. The aim is to produce an approx. 10.7 wt # of tin(II) sulfate solution. All reaction processes are carried out under nitrogen protective gas. To prepare the copper sulfate solution, completely deionized water, sulfuric acid and copper powder are placed one after the other with stirring, in the nitrogen-flushed reaction vessel. This is followed by the addition of hydrogen peroxide. Dosing is carried out in such a way that the vessel temperature does not exceed 70-75<0>C, which is the decomposition temperature of hydrogen peroxide. After complete oxidation of copper, the copper sulphate solution is heated to a temperature above 85°C, so that the hydrogen peroxide still present is thermally decomposed. This copper sulphate solution is finally cooled to approx. 20° C under nitrogen gas.
Til fremstilling av tinnsulfatoppløsningen blir tinnpulveret kontinuerlig innenfor 30-40 minutter tilsatt den til 20° C avkjølte kobbersulfatoppløsningen, under bibeholdelse av kartemperaturen på 20°C. Denne tilsats må igjen gjennomføres under beskyttelsesgass (nitrogengass). To prepare the tin sulphate solution, the tin powder is added continuously within 30-40 minutes to the copper sulphate solution cooled to 20°C, while maintaining the vessel temperature of 20°C. This addition must again be carried out under protective gas (nitrogen gas).
Omsetning av tinn følger spontant. Etter avsluttet reaksjon filtreres reaksjonsblandingen, som består av tinnsulfat, kobber og ikke-omsatt tinn, som også inneholder 4-verdig tinn. Deretter føres filtratet først i et kretsløp, slik at et flytende sjikt av kobberutfelling kan dannes. Det filtreres inntil filtratet er blitt klart og fargeløst. Til slutt tørkes filterkaken med nitrogen ved 3 bar og føres bort. Denne filterkaken anvendes i en fornyet fremstilling av tinn(II)-sulfatoppløsning sammen med rent kobber. Turnover of tin follows spontaneously. After completion of the reaction, the reaction mixture, which consists of tin sulphate, copper and unreacted tin, which also contains 4-valent tin, is filtered. The filtrate is then first passed through a circuit, so that a liquid layer of copper precipitation can be formed. It is filtered until the filtrate has become clear and colourless. Finally, the filter cake is dried with nitrogen at 3 bar and taken away. This filter cake is used in a renewed production of tin(II) sulphate solution together with pure copper.
Utførelse av fremgangsmåten under nitrogenbeskyttelsesgass og anvendelse av hydrogenperoksid til oksidering av kobberet, hvorved etter ,oksideringen hydrogenperoksid ved oppvarming blir spaltet, muliggjør en omsetning mellom tinn og kobbersulfat i praktisk talt oksygenfrie omgivelser. Derigjennom unngås en tinnoksidasjon ved tilsatsen av fint tinnstøv, og praktisk talt alt det tilsatte tinnmetall blir omsatt med kobbersulfat. Sammen med tilbakeføringen av kobberslam er på dette vis en spesiell høy økonomisk fordel oppnåelig, ifølge denne fremstilling av tinn(II)-sulfatoppløsning. Carrying out the process under nitrogen shielding gas and using hydrogen peroxide to oxidize the copper, whereby after the oxidation the hydrogen peroxide is split by heating, enables a reaction between tin and copper sulfate in a practically oxygen-free environment. As a result, tin oxidation is avoided by the addition of fine tin dust, and practically all the added tin metal is reacted with copper sulphate. Along with the return of copper sludge, a particularly high economic advantage is thus obtainable, according to this preparation of tin(II) sulfate solution.
Utførelseseksemplet er sammenfattende gjengitt i tegningen. The design example is summarized in the drawing.
Claims (6)
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE3821133A DE3821133A1 (en) | 1988-06-23 | 1988-06-23 | METHOD FOR PRODUCING TIN (II) SULFATE |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| NO892598D0 NO892598D0 (en) | 1989-06-22 |
| NO892598L true NO892598L (en) | 1989-12-27 |
Family
ID=6357040
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| NO89892598A NO892598L (en) | 1988-06-23 | 1989-06-22 | PROCEDURE FOR THE PREPARATION OF TIN (II) SULPHATE. |
Country Status (15)
| Country | Link |
|---|---|
| EP (1) | EP0351550A1 (en) |
| JP (1) | JPH0244025A (en) |
| KR (1) | KR900000295A (en) |
| CN (1) | CN1040014A (en) |
| AU (1) | AU3677289A (en) |
| BR (1) | BR8903047A (en) |
| DD (1) | DD283985A5 (en) |
| DE (1) | DE3821133A1 (en) |
| DK (1) | DK307389A (en) |
| FI (1) | FI893065A (en) |
| HU (1) | HUT50728A (en) |
| NO (1) | NO892598L (en) |
| NZ (1) | NZ229673A (en) |
| PT (1) | PT90931A (en) |
| ZA (1) | ZA894756B (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3933139A1 (en) * | 1989-10-04 | 1991-04-18 | Henkel Kgaa | METHOD FOR PRODUCING TIN (II) SULFATE SOLUTION |
| DE19833603C2 (en) * | 1998-07-25 | 2000-06-15 | Economic Versicherungs Vermitt | Use of tin (II) sulfate |
| CN104591266B (en) * | 2014-12-31 | 2016-08-24 | 柳州百韧特先进材料有限公司 | The method extending stannous sulfate shelf life of products |
| CN114890456A (en) * | 2022-04-20 | 2022-08-12 | 柳州华锡有色设计研究院有限责任公司 | Method for deeply reducing stannic tin in stannous sulfate solution |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2726926A (en) * | 1951-12-01 | 1955-12-13 | Rhone Poulenc Sa | Process for the production of lithium borohydride |
| DE1592429A1 (en) * | 1965-09-09 | 1970-12-17 | Heitger Monica | Process for the production of tin dioxide |
| FR2584704B1 (en) * | 1985-07-12 | 1987-10-30 | Rhone Poulenc Chimie | PROCESS FOR THE PREPARATION OF STANE SALT SOLUTIONS |
-
1988
- 1988-06-23 DE DE3821133A patent/DE3821133A1/en not_active Withdrawn
-
1989
- 1989-06-15 EP EP89110838A patent/EP0351550A1/en not_active Withdrawn
- 1989-06-20 CN CN89104100A patent/CN1040014A/en active Pending
- 1989-06-21 PT PT90931A patent/PT90931A/en not_active Application Discontinuation
- 1989-06-21 DD DD89329823A patent/DD283985A5/en not_active IP Right Cessation
- 1989-06-21 DK DK307389A patent/DK307389A/en not_active Application Discontinuation
- 1989-06-22 AU AU36772/89A patent/AU3677289A/en not_active Abandoned
- 1989-06-22 NO NO89892598A patent/NO892598L/en unknown
- 1989-06-22 NZ NZ229673A patent/NZ229673A/en unknown
- 1989-06-22 ZA ZA894756A patent/ZA894756B/en unknown
- 1989-06-22 HU HU893193A patent/HUT50728A/en unknown
- 1989-06-22 BR BR898903047A patent/BR8903047A/en unknown
- 1989-06-22 KR KR1019890008658A patent/KR900000295A/en not_active Application Discontinuation
- 1989-06-22 FI FI893065A patent/FI893065A/en not_active Application Discontinuation
- 1989-06-23 JP JP1162499A patent/JPH0244025A/en active Pending
Also Published As
| Publication number | Publication date |
|---|---|
| DK307389A (en) | 1989-12-24 |
| FI893065A0 (en) | 1989-06-22 |
| NZ229673A (en) | 1990-08-28 |
| DE3821133A1 (en) | 1989-12-28 |
| FI893065A (en) | 1989-12-24 |
| DK307389D0 (en) | 1989-06-21 |
| PT90931A (en) | 1989-12-29 |
| NO892598D0 (en) | 1989-06-22 |
| ZA894756B (en) | 1990-02-28 |
| AU3677289A (en) | 1990-01-04 |
| DD283985A5 (en) | 1990-10-31 |
| EP0351550A1 (en) | 1990-01-24 |
| BR8903047A (en) | 1990-02-06 |
| CN1040014A (en) | 1990-02-28 |
| KR900000295A (en) | 1990-01-30 |
| JPH0244025A (en) | 1990-02-14 |
| HUT50728A (en) | 1990-03-28 |
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