DE121835C - - Google Patents
Info
- Publication number
- DE121835C DE121835C DE1900121835D DE121835DA DE121835C DE 121835 C DE121835 C DE 121835C DE 1900121835 D DE1900121835 D DE 1900121835D DE 121835D A DE121835D A DE 121835DA DE 121835 C DE121835 C DE 121835C
- Authority
- DE
- Germany
- Prior art keywords
- tin
- hydrochloric acid
- cathode
- parts
- weight
- Prior art date
- Legal status (The legal status 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 status listed.)
- Expired - Lifetime
Links
- VEXZGXHMUGYJMC-UHFFFAOYSA-N HCl Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 16
- ATJFFYVFTNAWJD-UHFFFAOYSA-N tin hydride Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 13
- 238000005868 electrolysis reaction Methods 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- 150000001412 amines Chemical class 0.000 claims description 3
- 125000000751 azo group Chemical group [*]N=N[*] 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- CBCKQZAAMUWICA-UHFFFAOYSA-N P-Phenylenediamine Chemical compound NC1=CC=C(N)C=C1 CBCKQZAAMUWICA-UHFFFAOYSA-N 0.000 claims description 2
- 230000000875 corresponding Effects 0.000 claims description 2
- 239000003792 electrolyte Substances 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- AXZWODMDQAVCJE-UHFFFAOYSA-L Tin(II) chloride Chemical compound [Cl-].[Cl-].[Sn+2] AXZWODMDQAVCJE-UHFFFAOYSA-L 0.000 claims 1
- 239000003929 acidic solution Substances 0.000 claims 1
- 125000003368 amide group Chemical group 0.000 claims 1
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims 1
- 229910052739 hydrogen Inorganic materials 0.000 claims 1
- 239000001257 hydrogen Substances 0.000 claims 1
- 239000000243 solution Substances 0.000 claims 1
- HPGGPRDJHPYFRM-UHFFFAOYSA-J Tin(IV) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 description 5
- 230000005611 electricity Effects 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000005755 formation reaction Methods 0.000 description 2
- 125000000449 nitro group Chemical group [O-][N+](*)=O 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- -1 hydrochloric acid amines Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
Description
KAISERLICHES A IMPERIAL A
PATENTAMT.PATENT OFFICE.
PATENTSCHRIFTPATENT LETTERING
- M 121835 KLASSE Uq. - M 121835 CLASS Uq.
Zusatz zum Patente 116942 vom 24. Mai 1899.Addendum to patent 116942 of May 24, 1899.
Patentirt im Deutschen Reiche vom 27. März lgoo ab. Längste Dauer: 23. Mai 1914.Patented in the German Empire from March 27th from lgoo. Longest duration: May 23, 1914.
Nach dem Verfahren des Patentes 116942 gelingt es, Nitrokörper mittelst einer Zinnkathode oder bei Anwesenheit von Zinn im Elektrolyten mittelst einer indifferenten Kathode zu den entsprechenden Aminen zu reduziren, wenn man in den Kathodenraum einer elektrolytischen Zersetzungszelle, in welcher sich die zu reduzirenden Nitrokörper in Salzsäure gelöst oder suspendirt befinden, den elektrischen Strom einleitet.According to the method of patent 116942 it is possible to produce nitro bodies by means of a tin cathode or in the presence of tin in the electrolyte by means of an inert cathode to be reduced to the corresponding amines when one enters an electrolytic chamber in the cathode compartment Decomposition cell in which the nitro bodies to be reduced are dissolved in hydrochloric acid or suspended, introducing the electric current.
Dieses Verfahren läfst sich auch zur Reduktion von Azokörpern verwenden, doch ist es in diesem Falle zweckmäfsig, die Zinn- oder indifferente Kathode vorher mit einer Schicht Zinnschwamm zu überziehen, die Temperatur im Kathodenraum bis 60 ° zu halten und mit niedereren Stromdichten, als in der Patentschrift 116942 angegeben, zu arbeiten.This method can also be used to reduce azo bodies, but it is in In this case it is advisable to coat the tin or indifferent cathode beforehand To cover tin sponge, to keep the temperature in the cathode compartment up to 60 ° and with lower current densities than specified in patent 116942 to work.
Die Formirung der Kathode kann man umgehen, wenn man bei Beginn der Elektrolyse eine verhältnifsmäfsig geringe Menge elektrolytisch gefälltes, pulverförmiges Zinn zusetzt.The formation of the cathode can be avoided by starting the electrolysis a relatively small amount of electrolytically precipitated, powdery tin is added.
Gegenüber der üblichen Reduktion mit Zinn und Salzsäure und darauf folgenden Reduktion durch Elektrolyse bietet das vorliegende Verfahren wesentliche Vortheile. Bei der Elektrolyse von Zinnchlorid-haltigen Reduktionslaugen •— und solche werden bei der üblichen Reduktionsmethode mit Zinn und Salzsäure stets erhalten — gehen erstens 20 pCt. der Stromarbeit verloren. Dazu kommt, dafs die Zinnchloriddoppelsalze der Amine in der Regel recht schwer löslich sind, sie fallen daher aus dem Reduktionsgemisch aus, so dafs dasselbe, um es der Elektrolyse zugänglich zu machen, erst wieder durch gröfere Wassermengen verdünnt werden mufs. Mit dieser Verdünnung ist aber natürlich neben der Unbequemlichkeit der Apparatur wieder ein Spannungsmehrverbrauch verknüpft.Compared to the usual reduction with tin and hydrochloric acid and the subsequent reduction by electrolysis the present process offers essential advantages. In electrolysis of reduction liquors containing tin chloride • - and these are used with the usual reduction method Always preserved with tin and hydrochloric acid - first, 20 pCt. the electricity work lost. In addition, the tin chloride double salts of the amines are, as a rule, very difficult to dissolve, and they therefore precipitate the reduction mixture, so that the same, in order to make it accessible to electrolysis, must only be diluted again with larger amounts of water. With this dilution but of course, in addition to the inconvenience of the apparatus, there is again an increased consumption of voltage connected.
Diese-Schwierigkeiten werden nun durch die vorliegende combinirte Methode mit einem Schlage beseitigt. Trotz der Anwesenheit einei nur kleinen Menge Zinn und des Säureüberschusses verläuft nämlich bei dem vorliegenden Verfahren die Reaktion immer nur bis zur Bildung von Zinnchlorür, woraus der elektrische Strom sofort unter vollkommener Ausnutzung der Stromenergie wieder metallisches Zinn abscheidet. Es kommt in keinem Stadium des Processes zur Ausscheidung von Zinnsalzen oder zur Bildung des schlecht elektrolysirbaren Zinnchlorides. Zum Schlüsse der Operation finden sich im Reaktionsraume die zinnfreien salzsauren Amine in tadelloser Reinheit vor.These difficulties are now combined with one by the present method Beat eliminated. Despite the presence of only a small amount of tin and the excess of acid This is because in the present process the reaction only takes place up to the formation of tin chloride, from which the electrical Electricity immediately separates metallic tin again with full utilization of the electricity energy. At no stage of the process does tin salts precipitate or form that which is poorly electrolyzable Tin chloride. At the end of the operation, the tin-free ones are found in the reaction space hydrochloric acid amines in impeccable purity.
i. Reduktion des Paraamidoazobenzols zu Paraphenylendiamin.i. Reduction of paraamidoazobenzene to paraphenylenediamine.
In einer elektrolytischen Zersetzungszelle wird durch Einsetzen eines Diaphragmas ein Anoden- und Kathodenraum hergestellt. In den ersteren giefst man 10 pCt. Schwefelsäure und verwendet eine aus einem anodisch indifferenten Material hergestellte Anode. In den Kathodenraum füllt man eine Lösung bezw. Suspension von 100 Raumtheilen Wasser, 250 Raum-In an electrolytic decomposition cell, an anode is created by inserting a diaphragm. and cathode compartment made. In the former one pour 10 pCt. Sulfuric acid and used an anode made of an anodically indifferent material. In the cathode room if you fill a solution bezw. Suspension of 100 parts of water, 250 parts of
Claims (2)
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
AT8176D AT8176B (en) | 1899-05-23 | 1901-07-24 | Process for the reduction of azo bodies. |
Publications (1)
Publication Number | Publication Date |
---|---|
DE121835C true DE121835C (en) |
Family
ID=390808
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
DE1900121835D Expired - Lifetime DE121835C (en) | 1899-05-23 | 1900-03-26 |
Country Status (1)
Country | Link |
---|---|
DE (1) | DE121835C (en) |
-
1900
- 1900-03-26 DE DE1900121835D patent/DE121835C/de not_active Expired - Lifetime
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