NO120965B - - Google Patents
Info
- Publication number
- NO120965B NO120965B NO14729063A NO14729063A NO120965B NO 120965 B NO120965 B NO 120965B NO 14729063 A NO14729063 A NO 14729063A NO 14729063 A NO14729063 A NO 14729063A NO 120965 B NO120965 B NO 120965B
- Authority
- NO
- Norway
- Prior art keywords
- solution
- lead
- chromium
- electrolysis
- electrolytic
- Prior art date
Links
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 16
- 229910052804 chromium Inorganic materials 0.000 claims description 16
- 239000011651 chromium Substances 0.000 claims description 16
- 238000005868 electrolysis reaction Methods 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 9
- 238000001556 precipitation Methods 0.000 claims description 6
- 239000000356 contaminant Substances 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 claims 1
- 239000000243 solution Substances 0.000 description 24
- 238000011109 contamination Methods 0.000 description 7
- 238000001914 filtration Methods 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 3
- 125000004122 cyclic group Chemical group 0.000 description 3
- 238000000605 extraction Methods 0.000 description 3
- OIDPCXKPHYRNKH-UHFFFAOYSA-J chrome alum Chemical compound [K]OS(=O)(=O)O[Cr]1OS(=O)(=O)O1 OIDPCXKPHYRNKH-UHFFFAOYSA-J 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 230000002411 adverse Effects 0.000 description 1
- 229940037003 alum Drugs 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- RQPZNWPYLFFXCP-UHFFFAOYSA-L barium dihydroxide Chemical compound [OH-].[OH-].[Ba+2] RQPZNWPYLFFXCP-UHFFFAOYSA-L 0.000 description 1
- 229910001863 barium hydroxide Inorganic materials 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 229940055042 chromic sulfate Drugs 0.000 description 1
- GRWVQDDAKZFPFI-UHFFFAOYSA-H chromium(III) sulfate Chemical compound [Cr+3].[Cr+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O GRWVQDDAKZFPFI-UHFFFAOYSA-H 0.000 description 1
- 229910000356 chromium(III) sulfate Inorganic materials 0.000 description 1
- 235000015217 chromium(III) sulphate Nutrition 0.000 description 1
- 239000011696 chromium(III) sulphate Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000003750 conditioning effect Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 239000012527 feed solution Substances 0.000 description 1
- 238000005098 hot rolling Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000035800 maturation Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000029219 regulation of pH Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 229910021653 sulphate ion Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/06—Making microcapsules or microballoons by phase separation
- B01J13/14—Polymerisation; cross-linking
- B01J13/18—In situ polymerisation with all reactants being present in the same phase
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/06—Making microcapsules or microballoons by phase separation
- B01J13/08—Simple coacervation, i.e. addition of highly hydrophilic material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
- B41M—PRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
- B41M5/00—Duplicating or marking methods; Sheet materials for use therein
- B41M5/124—Duplicating or marking methods; Sheet materials for use therein using pressure to make a masked colour visible, e.g. to make a coloured support visible, to create an opaque or transparent pattern, or to form colour by uniting colour-forming components
- B41M5/165—Duplicating or marking methods; Sheet materials for use therein using pressure to make a masked colour visible, e.g. to make a coloured support visible, to create an opaque or transparent pattern, or to form colour by uniting colour-forming components characterised by the use of microcapsules; Special solvents for incorporating the ingredients
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Color Printing (AREA)
- Heat Sensitive Colour Forming Recording (AREA)
- Electrolytic Production Of Metals (AREA)
Description
Fremgangsmåte til å fjerne blyforurensninger fra en kromholdig sulfatoppløsning. Process for removing lead contaminants from a chromic sulfate solution.
Den foreliggende oppfinnelse angår en fremgangsmåte til å fjerne blyforurensninger fra The present invention relates to a method for removing lead contamination from
oppløsninger som anvendes ved elektrolytisk solutions used in electrolytic
utvinning av krom, spesielt kromholdige sul-fatoppløsninger som anvendes som cellemating extraction of chromium, especially chromium-containing sulphate solutions which are used as cell feed
i kromelektrolyse. in chromium electrolysis.
Anoder av bly og andre blyholdige deler Lead anodes and other lead-containing parts
som røreutstyr, slangeopphetere, blyfittings og such as stirring equipment, hose heaters, lead fittings and
liknende, brukes meget i apparatur for elektro-lyseutvinning av krom. Disse materialer vil similar, is widely used in equipment for the electrolytic extraction of chromium. These materials will
forurense elektrolyten og medføre blyforurensning i det utfelte metalliske krom. Når elektrolytisk utfelt krom, som er forurenset med bly, contaminate the electrolyte and cause lead contamination in the precipitated metallic chromium. When electrolytically precipitated chromium, which is contaminated with lead,
anvendes i legeringer med høyt krominnhold, used in alloys with a high chromium content,
opptrer det uunngåelig sprekker under varm-valsing av legeringen. Tilstedeværelse av blyforurensninger i elektrolytisk krom er faktisk cracks inevitably occur during hot-rolling of the alloy. Presence of lead impurities in electrolytic chromium is actual
så kritisk, at fabrikanter av legeringer med so critical, that manufacturers of alloys with
høyt krominnhold tolererer maksimalt 0,003 % high chromium content tolerates a maximum of 0.003%
bly. Dessuten senker tilstedeværelsen av blyforurensninger strømutbyttet ved elektrolysen i betydelig grad. lead. In addition, the presence of lead contaminants significantly lowers the current yield during electrolysis.
Det er derfor hovedformålet med den foreliggende oppfinnelse å skaffe en fremgangsmåte for virkelig fjernelse av blyforurensninger i oppløsninger som anvendes for kromelektrolyse. It is therefore the main purpose of the present invention to provide a method for the actual removal of lead contamination in solutions used for chromium electrolysis.
Andre formål og fordeler ved oppfinnelsen vil fremgå av den følgende beskrivelse. Other purposes and advantages of the invention will be apparent from the following description.
Tegningen viser et arbeidsskjema for en syklisk fremgangsmåte for elektrolytisk utvinning av krom, ved hvilken blyf jernemetoden i henhold til oppfinnelsen er anvendt. The drawing shows a working diagram for a cyclic method for the electrolytic extraction of chromium, in which the lead removal method according to the invention is used.
Den sykliske prosess for elektrolysefremstil-ling av krom som er beskrevet i U. S. patent The cyclic process for the electrolytic production of chromium described in U.S. Pat
2.650.192 anvender i rekkefølge utluting, filtrering, kondisjonering, krystallisering, annen filtrering, modning, tredje filtrering, og oppløs- 2,650,192 uses, in order, leaching, filtration, conditioning, crystallization, second filtration, maturation, third filtration, and dissolving
ning før den resulterende rensede oppløsning føres inn i den elektrolytiske celle. Disse trinn er antydet ved rektanglene 1, 2, 3, 4, 5, 10, 11 og 12 på arbeidsskjemaet. Dessuten anvendes det andre rensetrinn under tilbakeføringen av oppløsningen. ning before the resulting purified solution is fed into the electrolytic cell. These steps are indicated by rectangles 1, 2, 3, 4, 5, 10, 11 and 12 on the worksheet. In addition, the second cleaning step is used during the return of the solution.
Oppfinnerne har funnet at oppløsningen av kromalunkrystaller som erholdes i en slik syklisk prosess med fordel kan behandles i henhold til oppfinnelsen før innføringen i elektrolysecellen, slik at man praktisk talt oppnår fullstendig fjernelse av alle inneholdte blyforurensninger. The inventors have found that the solution of chromalum crystals obtained in such a cyclic process can be advantageously treated according to the invention before introduction into the electrolysis cell, so that practically complete removal of all contained lead contaminants is achieved.
Som vist på tegningen blir kromalunkrystaller oppløst i vann og oppløsningens pH reguleres til en verdi mellom 1,0 og 2,25, ved hvilken det praktisk talt ikke finner sted noen hydrolyse. Denne pH-regulering kan skaffes ved til-setning av ammoniakk, bariumhydroksyd eller hvilken som helst' annen base som ikke vil innvirke uheldig på den senere utfellingen av krom. Den behandlede oppløsning innføres i en elektrolytisk celle av diafragmatypen, hvor den elektrolyseres under anvendelse av mere enn 9,25 amp.timer pr. liter oppløsning. Dette trinn er antydet ved rektangel 12 a på arbeidsskjemaet. Etter elektrolyseringen blir den blyholdige rest filtrert fra oppløsningen og oppløs-ningen innføres på vanlig måte i katalyttrom-met i den elektrolytiske celle. Dette filtrerings-trinn er antydet ved rektangel 12 b på arbeidsskjemaet. As shown in the drawing, chrome alum crystals are dissolved in water and the pH of the solution is adjusted to a value between 1.0 and 2.25, at which practically no hydrolysis takes place. This pH regulation can be obtained by adding ammonia, barium hydroxide or any other base which will not adversely affect the subsequent precipitation of chromium. The treated solution is introduced into a diaphragm-type electrolytic cell, where it is electrolysed using more than 9.25 amp hours per liter of solution. This step is indicated by rectangle 12 a on the work chart. After the electrolysis, the lead-containing residue is filtered from the solution and the solution is introduced in the usual way into the catalyst compartment of the electrolytic cell. This filtering step is indicated by rectangle 12 b on the work chart.
Hvis det dreier seg om en krom-alun-opp-løsning, som har sammensetningen (NH4)2.Cr2 (S04)3.24H20, vil denne av seg selv ha en pH på ca. 1,0, slik at det ikke kreves noen regulering av pH-verdien for å bringe denne innenfor det ønskede område 1,0—2,25. Med slike oppløs-ninger har det vist seg at strømstyrken og varig-heten av behandlingen, hvis det skal oppnås maksimal utfelling av blyforurensningen, er ca. 16 amp.timer pr. liter oppløsning, i løpet av hvilken tid oppløsningens pH stiger til ca. 2,25. For å sikre mot hydrolyse, kan det være nød-vendig å behandle oppløsningen med H2S04-anolytt fra kromutfellingscellene, eller liknende, for å holde oppløsningens pH under 2,25, mens den nevnte elektrolyse foregår. If it is a chrome-alum solution, which has the composition (NH4)2.Cr2 (SO4)3.24H20, this will itself have a pH of approx. 1.0, so that no regulation of the pH value is required to bring it within the desired range of 1.0-2.25. With such solutions, it has been shown that the amperage and duration of the treatment, if maximum precipitation of the lead contamination is to be achieved, is approx. 16 amp hours per liter of solution, during which time the pH of the solution rises to approx. 2.25. To ensure against hydrolysis, it may be necessary to treat the solution with H 2 SO 4 anolyte from the chromium precipitation cells, or the like, to keep the pH of the solution below 2.25, while the aforementioned electrolysis takes place.
I et utførelseseksempel ble elektrolyserommet i cellen av diafragmatypen fylt med cellemate-oppløsning og behandlet med 10 000 amp. i ialt 9 timer. Katolytten besto av 3028 liter krom-alun-oppløsning. Anolytten besto av 757 liter av samme oppløsning. Den følgende tabell angir konsentrasjonen av blyforurensning i katolytt-og anolytt-oppløsningene på forskjellige tids-punkter under elektrolyseringen. In an exemplary embodiment, the electrolysis compartment of the diaphragm type cell was filled with cell feed solution and treated with 10,000 amps. for a total of 9 hours. The catholyte consisted of 3028 liters of chromium-alum solution. The anolyte consisted of 757 liters of the same solution. The following table indicates the concentration of lead contamination in the catholyte and anolyte solutions at different time points during the electrolysis.
Det fremgår av ovenstående tabell at konsentrasjonen av blyforurensning i katolytten ble nedsatt med over 75 % ved ca. 3 timers behandling og at den maksimale utfelling av bly, nemlig over 90 % av det opprinnelige innhold, ble oppnådd etter 5 timers elektro-lysering. Denne behandling representerte 16,5 amp.timer pr. liter katolytt og det viste seg at ytterligere behandling ikke bevirket noen ytterligere senkning av konsentrasjonen av blyforurensningen av oppløsningen. Etter denne behandling ble det utfelte bly filtrert fra oppløs-ningen gjennom en filterpresse av plate- og rammetypen og oppløsningen ble innført i den elektrolytiske celle og elektrolysert, hvorved det på katoden ble utfelt metallisk krom som inneholdt mindre enn 0,002 vektsprosent bly. It appears from the above table that the concentration of lead contamination in the catholyte was reduced by over 75% at approx. 3 hours of treatment and that the maximum precipitation of lead, namely over 90% of the original content, was achieved after 5 hours of electrolysis. This treatment represented 16.5 amp hours per liter of catholyte and it was found that further treatment did not effect any further lowering of the concentration of the lead contamination of the solution. After this treatment, the precipitated lead was filtered from the solution through a filter press of the plate and frame type and the solution was introduced into the electrolytic cell and electrolyzed, whereby metallic chromium containing less than 0.002 weight percent lead was precipitated on the cathode.
Claims (2)
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US16925862A | 1962-01-29 | 1962-01-29 | |
| US25453963A | 1963-01-16 | 1963-01-16 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| NO120965B true NO120965B (en) | 1970-12-28 |
Family
ID=26864908
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| NO14729063A NO120965B (en) | 1962-01-29 | 1963-01-28 |
Country Status (8)
| Country | Link |
|---|---|
| BE (1) | BE627711A (en) |
| CH (1) | CH411561A (en) |
| DE (1) | DE1267961B (en) |
| DK (1) | DK116703B (en) |
| FI (1) | FI43951B (en) |
| GB (2) | GB1042596A (en) |
| NL (2) | NL138970B (en) |
| NO (1) | NO120965B (en) |
Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1465669A (en) | 1972-12-28 | 1977-02-23 | Agfa Gevaert | Pressure sensitive recording materials and pressure-recording procews |
| US4232083A (en) * | 1975-07-22 | 1980-11-04 | Minnesota Mining And Manufacturing Company | Imaging compositions and methods |
| GB1561272A (en) | 1976-04-27 | 1980-02-20 | Ciba Geigy Ag | Azomethine compounds their manufacture and use |
| CH633533A5 (en) * | 1978-04-24 | 1982-12-15 | Ciba Geigy Ag | CARBAZOLYL METHANE COMPOUNDS, THEIR PRODUCTION AND USE AS COLOR IMAGERS IN PRESSURE-SENSITIVE OR HEAT-SENSITIVE RECORDING MATERIALS. |
| DE2951486C2 (en) * | 1979-12-20 | 1982-06-16 | GAO Gesellschaft für Automation und Organisation mbH, 8000 München | Security paper protected against counterfeiting and counterfeiting and process for its manufacture |
| EP0036117B1 (en) | 1980-03-14 | 1986-02-05 | Spezial-Papiermaschinenfabrik August Alfred Krupp GmbH & Co | Pressure-sensitive recording material |
| DE3623413A1 (en) * | 1986-07-11 | 1988-01-14 | Basf Ag | COMPOSITE LAYER |
| GB8706667D0 (en) * | 1987-03-20 | 1987-04-23 | Wiggins Teape Group Ltd | Self-adhesive label assembly |
| DE68912688T2 (en) * | 1988-07-01 | 1994-05-05 | Wiggins Teape Group Ltd | Pressure sensitive recording paper. |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| NL95044C (en) * | 1953-06-30 | |||
| US2929736A (en) * | 1957-07-25 | 1960-03-22 | Ncr Co | Heat and pressure responsive record material |
-
0
- NL NL288246D patent/NL288246A/xx unknown
- BE BE627711D patent/BE627711A/xx unknown
-
1963
- 1963-01-28 NL NL288246A patent/NL138970B/en not_active IP Right Cessation
- 1963-01-28 DE DEP1267A patent/DE1267961B/en active Pending
- 1963-01-28 NO NO14729063A patent/NO120965B/no unknown
- 1963-01-28 DK DK40063A patent/DK116703B/en unknown
- 1963-01-29 FI FI16363A patent/FI43951B/fi active
- 1963-01-29 CH CH111163A patent/CH411561A/en unknown
- 1963-01-29 GB GB371863A patent/GB1042596A/en not_active Expired
- 1963-01-29 GB GB1907266A patent/GB1042599A/en not_active Expired
Also Published As
| Publication number | Publication date |
|---|---|
| DE1267961B (en) | 1968-05-09 |
| CH411561A (en) | 1966-04-15 |
| GB1042599A (en) | 1966-09-14 |
| FI43951B (en) | 1971-03-31 |
| BE627711A (en) | |
| DK116703B (en) | 1970-02-02 |
| GB1042596A (en) | 1966-09-14 |
| NL138970B (en) | 1973-05-15 |
| NL288246A (en) |
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