PL124273B1 - Method of electrochemical regeneration of chromates and dichromates - Google Patents

Method of electrochemical regeneration of chromates and dichromates Download PDF

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Publication number
PL124273B1
PL124273B1 PL21836479A PL21836479A PL124273B1 PL 124273 B1 PL124273 B1 PL 124273B1 PL 21836479 A PL21836479 A PL 21836479A PL 21836479 A PL21836479 A PL 21836479A PL 124273 B1 PL124273 B1 PL 124273B1
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Poland
Prior art keywords
chromates
dichromates
current
electrochemical regeneration
electrolysers
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PL21836479A
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Polish (pl)
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PL218364A1 (en
Inventor
Adam Korczynski
Maciej Gonet
Jozef Swiderski
Andrzej Doniec
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Politechnika Slaska Im Wincent
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Priority to PL21836479A priority Critical patent/PL124273B1/en
Publication of PL218364A1 publication Critical patent/PL218364A1/xx
Publication of PL124273B1 publication Critical patent/PL124273B1/en

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  • Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
  • Chemical Treatment Of Metals (AREA)

Description

Przedmiotem wynalazku jest sposób elektroche¬ micznej regeneracji chromianów i dwuchromianów na zasadzie reakcji utleniania zwiazków soli chro¬ mowych do chromianów i dwuchromianów w sro¬ dowisku wodnego roztworu kwasu siarkowego.Znane sa wodne roztwory chromianów i dwu¬ chromianów w srodowisku kwasu siarkowego sto¬ sowane jako utleniacz w procesach organicznych.Zuzyte w wyniku utleniania roztwory zawieraja sole chrome, kwas siarkowy oraz zwiazkami orga¬ nicznymi.Znane sa z opisów patentowych: USA nr 4006067, ZSRR nr 574482, a takze z J. Apol. Chem. Biotech- nol. 26407.1976 r., Chim. Twierdowo Toplina 6.110. 1975 r., Chemie-Ing-Techn. 5.386.1963 r. elektro¬ chemiczne metody regeneracji chromianów i dwu¬ chromianów, w celu ich wielokrotnego uzycia. Re¬ generacje prowadzi sie w elektrolizerach (np. pat USA 4006067, 3663412 oraz Chemie-Ing-Techn. 5386. 1963 i Chim. Twierdowo Toplina 6.110.1975 r.).Znane sposoby elektrochemicznej regeneracji chromianów i dwuchromianów polegaja na prze¬ plywie pradu o jednakowej gestosci przez uklad wszystkich elektrolizerów.Sposoby te realizowano w ukladzie elektrolize¬ rów o jednakowym ksztalcie geometrycznym i identycznej powierzchni elektrod laczonych w ta¬ ki sposób, ze kazdy stopien kaskady zawieral iden¬ tyczna ilosc elektrolizerów. Wszystkie elektrolizery kaskady pracujac przy stosunkowo niskiej gesto- 10 15 sci pradu do 10 A/dmf), gdyz dalszy wzrost war¬ tosci tego parametru powoduje silny spadek wy¬ dajnosci pradowej w ostatnich elektrolizerach kas¬ kady.W wyniku tak prowadzonego procesu zdolnosc produkcyjna instalacji jest niewielka.Sposób elektrochemicznej regeneracji chromia¬ nów i dwuchromianów wedlug wynalazku polega na tym, ze regenerowany roztwór poddaje sie dzia¬ laniu pradu o gestosci malejacej korzystnie o ge¬ stosci od 30—7 A/dm*. Do elektrolitu korzystnie wprowadza sie kwas o-fosforowy w takiej ilosci, aby stezenie jonów fosforanowych wynosilo 1— 100 g/dm*.Wedlug wynalazku elektrolizie podaje sie roz¬ twór zawierajacy 10—140 g/dms chromu (III), 50— 500 g/dm* kwasu siarkowego oraz okolo lf/t pozo¬ stalosci po utlenianiu zwiazków organicznych i chro¬ miany lub dwuchromiany.Proces realizuje sie w urzadzeniu do elektroche¬ micznego utleniania skladajacego sie z kaskady co najmniej 3 diafragmowych elektrolizerów pracu¬ jacych przy róznej gestosci pradu dla kazdego stopnia kaskady. Pierwszy elektrolizer pracuje przy anodowej gestosci pradu 20—30 A/dml korzystnie 20—22 A/dm1), ostatni ponizej 10 A/dms (korzystnie 7—10 A/dm1), a pozostale przy wartosciach posred¬ nich. Anody wykonane sa z olowiu lub stopu olo¬ wiu z antymonem lub antymonem i cyna: kato¬ dy ze stali kwasoodpornej lub z materialu uzyte- 1242733 124273 4 go na anody. Temperatura procesu wynosi 50— 95°C (korzystnie 70—90°C).Roztwór do regeneracji wprowadzony jest w spo¬ sób ciagly do. przestrzeni katodowej pierwszego elektrolizera kaskady, przeplywa przez przestrzenie katodowe pozostalych elektrolizerów i nastepnie .zawracany jest do przestrzeni anodowej pierwsze- -ge^ elektrolizera. Na wylocie ostatniego elektroli¬ zera otrzymuje sie roztwór zregenerowany, zawie¬ rajacy (zaleznie od wymagan) do 95—98*/o chromu (VI) wzgledem calkowitej ilosci chromu.W trafcie elektrolizy uzupelnia sie ubytki wody w poszczególnych elektrolizerach tak, aby nateze¬ nie przeplywu strumienia na wyjsciu bylo równe jego wartosci na wejsciu. Do roztworu regenero¬ wanego dodaje sie kwas fosforowy w takiej ilosci, aby jego stezenie wynosilo 1^-100 g/dm8 (korzyst¬ nie 10 g/dm8), co poprawia wydajnosc pradowa.Dla powyzszego rezimu technologicznego uzysku¬ je sie wydajnosc pradowa 70—85°/o, a wiec taka sama jak przy jednakowej, nizszej gestosci pradu we wszystkich elektrolizerach. Tak prowadzony proces technologiczny zachodzi jednak kilkakrot¬ nie szybciej i wymaga mniejszej powierzchni pro¬ dukcyjnej w stosunku do metod dotychczas zna¬ nych.Zastrzezenia patentowe 10 i. Sposób elektrochemicznej regeneracji chromia¬ nów i dwuchromianów na zasadzie reakcji utle¬ niania metoda ciagla, znamienny tym, ze regene¬ rowany roztwór poddaje sie dzialaniu pradu o ge¬ stosci malejacej. i* 2. Sposób wedlug zastrz. i, znamienny tym, ze regenerowany roztwór poddaje sie dzialaniu pradu o gestosci od 30—7 A/dm2. 3. Sposób wedlug zastrz. 1, znamienny tym, ze do elektrolitu wprowadza sie kwas o-fosforowy w 20 takiej ilosci, aby stezenie jonów fosforanowych wy¬ nosilo 1—100 g/dm8.Drukarnia Narodowa, Zaklad Nr 6. 308/84 Cena 100 zl PLThe subject of the invention is a method of electrochemical regeneration of chromates and dichromates by the oxidation of compounds of chromates to chromates and dichromates in an aqueous solution of sulfuric acid. Aqueous solutions of chromates and dichromates in a sulfuric acid environment are known. oxidant in organic processes. The solutions used as a result of oxidation contain chrome salts, sulfuric acid and organic compounds. They are known from the following patents: US 4,006,067, USSR No. 574,482, and also from J. Apol. Chem. Biotechnol. 26407.1976, Chim. Twierdowo Toplina 6.110. 1975, Chemie-Ing-Techn. On 5 June 1963, electrochemical methods for the regeneration of chromates and dichromates in order to reuse them. Regeneration is carried out in electrolysers (e.g. U.S. Pat. No. 4006067, 3663412 and Chemie-Ing-Techn. 5386. 1963 and Chim. Twierdowo Toplina on 6.110.1975). of the same density by the arrangement of all the electrolysers. These methods were carried out in a system of electrolysers of the same geometric shape and identical surface area of electrodes connected in such a way that each stage of the cascade contained the same number of electrolysers. All electrolysers in the cascade operate at a relatively low current density (up to 10 A / dmf), as a further increase in the value of this parameter causes a strong drop in the current efficiency in the last electrolysers of the cascade. As a result of this process, the production capacity of the installation According to the invention, the method of electrochemical regeneration of chromates and dichromates is based on the fact that the regenerated solution is subjected to a current of preferably decreasing density from 30 to 7 amps / dm. Preferably, o-phosphoric acid is introduced into the electrolyte in such an amount that the concentration of phosphate ions is 1 to 100 g / dm *. According to the invention, electrolysis is given a solution containing 10-140 g / dm of chromium (III), 50 to 500 g. / dm * of sulfuric acid and about 1 / t of residue after oxidation of organic compounds and chromates or dichromates. The process is carried out in an electrochemical oxidation device consisting of a cascade of at least 3 diaphragm electrolysers operating at different current densities for each step of the cascade. The first electrolyser operates at an anodic current density of 20-30 A / dm1, preferably 20-22 A / dm1), the last one below 10 A / dms (preferably 7-10 A / dm1) and the others at intermediate values. The anodes are made of lead or an alloy of lead with antimony or antimony and tin: cathodes of acid-resistant steel or of the material used for the anodes. The temperature of the process is 50-95 ° C. (preferably 70-90 ° C.). The regeneration solution is continuously introduced into. the cathode space of the first electrolyser of the cascade flows through the cathode spaces of the remaining cells and then returns to the anode space of the first electrolyser. At the outlet of the last electrolyser, a regenerated solution is obtained, containing (depending on the required) up to 95-98% of chromium (VI) in terms of the total amount of chromium. In the electrolysis, the losses of water in individual electrolyzers are replaced so that no stream flow at the output was equal to its value at the input. Phosphoric acid is added to the regenerated solution in such an amount that its concentration is 1-100 g / dm8 (preferably 10 g / dm8), which improves the current efficiency. For the above technological regime, the current efficiency is obtained 70 —85 ° / o, so the same as with the same, lower current density in all electrolysers. The technological process carried out in this way is, however, several times faster and requires a smaller production area in relation to the methods known hitherto. Patent claims 10 i. The method of electrochemical regeneration of chromates and dichromates by the oxidation reaction by the continuous method, characterized by this that the regenerated solution is subjected to a current of decreasing intensity. and * 2. A method according to claim and, characterized in that the regenerated solution is subjected to a current with a density of 30-7 A / dm2. 3. The method according to p. A method according to claim 1, characterized in that o-phosphoric acid is introduced into the electrolyte in such an amount that the concentration of phosphate ions amounts to 1-100 g / dm8. National Printing House, Plant No. 6 308/84 Price PLN 100 PL

Claims (3)

1. Zastrzezenia patentowe 10 i. Sposób elektrochemicznej regeneracji chromia¬ nów i dwuchromianów na zasadzie reakcji utle¬ niania metoda ciagla, znamienny tym, ze regene¬ rowany roztwór poddaje sie dzialaniu pradu o ge¬ stosci malejacej. i* 1. Claims 10 i. A method of electrochemical regeneration of chromates and dichromates by a continuous oxidation reaction, characterized in that the regenerated solution is subjected to a current of decreasing intensity. and* 2. Sposób wedlug zastrz. i, znamienny tym, ze regenerowany roztwór poddaje sie dzialaniu pradu o gestosci od 30—7 A/dm2. 2. The method according to claim and, characterized in that the regenerated solution is subjected to a current with a density of 30-7 A / dm2. 3. Sposób wedlug zastrz. 1, znamienny tym, ze do elektrolitu wprowadza sie kwas o-fosforowy w 20 takiej ilosci, aby stezenie jonów fosforanowych wy¬ nosilo 1—100 g/dm8. Drukarnia Narodowa, Zaklad Nr 6. 308/84 Cena 100 zl PL3. The method according to p. The method of claim 1, wherein o-phosphoric acid is introduced into the electrolyte in such an amount that the concentration of phosphate ions is 1-100 g / dm8. National Printing House, Plant No. 6. 308/84 Price PLN 100 PL
PL21836479A 1979-09-17 1979-09-17 Method of electrochemical regeneration of chromates and dichromates PL124273B1 (en)

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PL124273B1 true PL124273B1 (en) 1983-01-31

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