DE971893C - Process to increase the corrosion resistance of acid-proof steel - Google Patents
Process to increase the corrosion resistance of acid-proof steelInfo
- Publication number
- DE971893C DE971893C DEA16767A DEA0016767A DE971893C DE 971893 C DE971893 C DE 971893C DE A16767 A DEA16767 A DE A16767A DE A0016767 A DEA0016767 A DE A0016767A DE 971893 C DE971893 C DE 971893C
- Authority
- DE
- Germany
- Prior art keywords
- acid
- per
- steel
- oxidation
- plates
- 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
Links
- 229910000831 Steel Inorganic materials 0.000 title claims description 17
- 239000010959 steel Substances 0.000 title claims description 17
- 238000000034 method Methods 0.000 title claims description 8
- 238000005260 corrosion Methods 0.000 title claims description 7
- 230000007797 corrosion Effects 0.000 title claims description 7
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 11
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 10
- 229910019142 PO4 Inorganic materials 0.000 claims description 9
- 229910017604 nitric acid Inorganic materials 0.000 claims description 9
- 235000021317 phosphate Nutrition 0.000 claims description 9
- 239000002253 acid Substances 0.000 claims description 7
- 238000007254 oxidation reaction Methods 0.000 claims description 7
- GQPLMRYTRLFLPF-UHFFFAOYSA-N nitrous oxide Inorganic materials [O-][N+]#N GQPLMRYTRLFLPF-UHFFFAOYSA-N 0.000 claims description 6
- 230000003647 oxidation Effects 0.000 claims description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 6
- 239000010452 phosphate Substances 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 5
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 4
- 230000004580 weight loss Effects 0.000 claims description 4
- 150000002823 nitrates Chemical class 0.000 claims description 3
- 150000003013 phosphoric acid derivatives Chemical class 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims description 2
- 229910001463 metal phosphate Inorganic materials 0.000 claims description 2
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims 6
- PVNIIMVLHYAWGP-UHFFFAOYSA-N Niacin Chemical compound OC(=O)C1=CC=CN=C1 PVNIIMVLHYAWGP-UHFFFAOYSA-N 0.000 claims 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims 2
- 239000000203 mixture Substances 0.000 claims 2
- 238000010907 mechanical stirring Methods 0.000 claims 1
- 235000001968 nicotinic acid Nutrition 0.000 claims 1
- 229960003512 nicotinic acid Drugs 0.000 claims 1
- 239000011664 nicotinic acid Substances 0.000 claims 1
- 235000011007 phosphoric acid Nutrition 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 description 3
- ZPTVNYMJQHSSEA-UHFFFAOYSA-N 4-nitrotoluene Chemical compound CC1=CC=C([N+]([O-])=O)C=C1 ZPTVNYMJQHSSEA-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- OTLNPYWUJOZPPA-UHFFFAOYSA-N 4-nitrobenzoic acid Chemical compound OC(=O)C1=CC=C([N+]([O-])=O)C=C1 OTLNPYWUJOZPPA-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- VLZLOWPYUQHHCG-UHFFFAOYSA-N nitromethylbenzene Chemical compound [O-][N+](=O)CC1=CC=CC=C1 VLZLOWPYUQHHCG-UHFFFAOYSA-N 0.000 description 1
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/73—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals characterised by the process
Description
AUSGEGEBEN AM 9. APRIL 1959ISSUED APRIL 9, 1959
A 16767 VI/48dA 16767 VI / 48d
ist in Anspruch genommenis used
Die Erfindung betrifft ein Verfahren zur Erhöhung der Korrosionsbeständigkeit von säurefestem Stahl.The invention relates to a method for increasing the corrosion resistance of acid-proof Stole.
In den Zweigen der chemischen Industrie, in denen korrodierend wirkende Reagenzien verwendet werden, verursacht die Auswahl des Herstellungsmaterials für die Reaktionsgefäße und insbesondere die Auswahl der dafür in Frage kommenden säurefesten Stähle häufig große Schwierigkeiten. Vor allem genügen die verschiedenen Sorten von säurefestem Stahl noch nicht allen Anforderungen, die an die Beständigkeit gegen Säuren und insbesondere an Salpeter- und Schwefelsäure gestellt werden. Insbesondere ist die Korrosion in solchen Reaktionsgefäßen aus säurefestem Stahl in Gegenwart der erwähnten Satiren dann beträchtlich, wenn Reaktionen bei hoher Temperatur durchgeführt werden sollen.In the branches of the chemical industry in which corrosive reagents are used causes the selection of the manufacturing material for the reaction vessels and in particular the selection of the suitable acid-proof steels for this purpose often presents great difficulties. before All in all, the different grades of acid-proof steel do not yet meet all the requirements the resistance to acids and especially nitric and sulfuric acid. In particular, corrosion is present in such acid-proof steel reaction vessels of the satires mentioned are considerable when reactions are carried out at high temperature should be.
Die Korrosionsbeständigkeit säurefester Stähle kann nun gemäß dem Verfahren nach der Erfindung beträchtlich erhöht werden. Dieses Verfahren ist dadurch gekennzeichnet, daß der Stahl in Gegenwart von anorganischen Metallphosphaten und/oder organischen Phosphaten mit Salpetersäure und/oder nitrosen Gasen und gegebenenfalls Nitraten bei erhöhter Temperatur und unter Druck behandelt wird.The corrosion resistance of acid-proof steels can now be determined according to the method according to the invention can be increased considerably. This method is characterized in that the steel is in the presence of inorganic metal phosphates and / or organic phosphates with nitric acid and / or treated nitrous gases and optionally nitrates at elevated temperature and under pressure will.
Es ist zwar bereits bekannt, Eisenoberflächen mittels Phosphatlösungen zu behandeln; die gleichzeitige Anwendung von Salpetersäure oder nitrosenIt is already known to treat iron surfaces with phosphate solutions; the simultaneous Use of nitric acid or nitrous
809 764/7809 764/7
Gasen unter erhöhtem Druck und erhöhter Temperatur, gegebenenfalls unter gleichzeitiger Anwendung von Nitraten, ist jedoch bisher noch nicht vorgeschlagen worden. Erst dadurch wird die gemaß dem Verfahren erreichte erhöhte Widerstandsfähigkeit gegen die obenerwähnten korrodierenden Einflüsse bewirkt.Gases under increased pressure and temperature, possibly with simultaneous use of nitrates, but has not yet been proposed. Only then is it measured the method achieved increased resistance to the above-mentioned corrosive Influences causes.
Besonders vorteilhaft ist es dabei, die Behandlung in Gegenwart von organischen, bei der Oxydation nitrose Gase bildenden Verbindungen vorzunehmen. Als derartige Verbindungen kommen z. B. p-Nitrotoluol oder Pyridinbasen in Frage. Letztere können auch in Form ihrer Phosphate angewendet werden, z. B. in Form des Phosphats von /ff-Pikolin.It is particularly advantageous to carry out the treatment in the presence of organic substances during the oxidation compounds forming nitrous gases. As such connections come z. B. p-nitrotoluene or pyridine bases in question. The latter can also be used in the form of their phosphates be e.g. B. in the form of the phosphate of / ff-picoline.
Im folgenden werden einige Beispiele für das erfindungsgemäße Verfahren und einige danach erhaltene Versuchsergebnisse angegeben. Was weiter unten gesagt wird, soll jedoch nicht den Umfang dieser Erfindung einschränken.In the following some examples of the process of the invention and some thereafter are obtained Test results given. What is said below, however, is not intended to limit the scope limit this invention.
Beispiel ιExample ι
Säurefester Stahl, Typ i8 Cr/8 Ni, mit niedrigem C-Gehalt wurde in einem Autoklav, der mit p-Nitrotoluol (104 g), 65«/oiger Salpetersäure (189g), Wasser (221 g) und Trinatriumorthophosphat (60 g) beschickt war, eingetaucht. Der Inhalt des Autoklavs wurde unter Schütteln auf etwa 1900 C erhitzt, wobei die Oxydationsreaktion begann. Die Temperatur wurde etwa 20 Minuten lang auf 185 bis 1950 C gehalten. Dabei stieg der Druck auf maximal 35 kg pro cm2. Nach dem Abkühlen wurde nach 3 Stunden der Autoklav entleert. Durch Einwirkung der Salpetersäure bildete sich aus dem Nitrotoluol unter Entwicklung von nitrosen Gasen p-Nitrobenzoesäure, die gegebenenfalls anschließend weiterverarbeitet werden kann.Acid-proof steel, type 18 Cr / 8 Ni, with a low carbon content was in an autoclave which was filled with p-nitrotoluene (104 g), 65% nitric acid (189 g), water (221 g) and trisodium orthophosphate (60 g) was loaded, immersed. The contents of the autoclave were heated to about 190 ° C. with shaking, the oxidation reaction beginning. The temperature was held at 185 to 195 ° C. for about 20 minutes. The pressure rose to a maximum of 35 kg per cm 2 . After cooling, the autoclave was emptied after 3 hours. The action of nitric acid resulted in the formation of p-nitrobenzoic acid from the nitrotoluene with the development of nitrous gases, which can then be further processed if necessary.
Die Probe aus säurefestem Stahl hatte etwas an Gewicht verloren, aber wenn sie erneut einer ähnliehen Behandlung (ohne Anwesenheit von Phosphat) unterworfen wurde, wurde kein Gewichtsverlust festgestellt. Gleichzeitig eingetauchte, nicht vorbehandelte Vergleichsproben hatten eine Korrosion von i,2 g pro m2 und Stunde erlitten. Wenn Phosphat bei der letzten Oxydation anwesend war, wurde eine geringe Gewichtszunahme der Stahlproben beobachtet. Platten, die einmal in der oben angegebenen Weise in Gegenwart von Phosphat behandelt wurden, können der Einwirkung von verdünnter Salpetersäure bei hoher Temperatur und hohem Druck während einer langen Zeit ausgesetzt werden, ohne Korrosion zu erleiden. Ferner sind in dieser Weise behandelte Stahlplatten widerstandsfähig gegen Schwefelsäure, wie Beispiel 2 zeigt.The acid-proof steel sample had lost some weight, but when subjected again to a similar treatment (without the presence of phosphate) no weight loss was observed. Comparative samples immersed at the same time that had not been pretreated suffered corrosion of 1.2 g per m 2 and hour. If phosphate was present during the final oxidation, a slight increase in the weight of the steel samples was observed. Panels which have been treated once in the presence of phosphate in the above-mentioned manner can be exposed to the action of dilute nitric acid at high temperature and high pressure for a long time without suffering corrosion. Furthermore, steel plates treated in this way are resistant to sulfuric acid, as Example 2 shows.
Nach Beispiel 1 behandelte säurefeste Stahlplatten wurden in io°/oige Schwefelsäure getaucht und 50 Stunden unter Rückfluß gekocht. Nach dieser Zeit wurde ein Gewichtsverlust von nur 0,1 g pro m2 und Stunde festgestellt. Selbst gegen 5o°/oige Schwefelsäure war die Widerstandsfähigkeit gut. Nicht vorbehandelte Platten aus dem gleichen Material wurden den gleichen Säurelösungen ausgesetzt. Diese Platten wurden schnell durch die Säure unter Wasserstoffentwicklung angegriffen. Acid-resistant steel plates treated according to Example 1 were immersed in 10% strength sulfuric acid and refluxed for 50 hours. After this time, a weight loss of only 0.1 g per m 2 and hour was found. The resistance was good even against 50% sulfuric acid. Panels made of the same material that had not been pretreated were exposed to the same acid solutions. These plates were quickly attacked by the acid with evolution of hydrogen.
Claims (2)
Deutsche Patentschriften Nr. 643869, 661253; Auszüge deutscher Patentanmeldungen, Bd. 19, 1948, S. 79s, 797. 799-Considered publications:
German Patent Nos. 643869, 661253; Excerpts from German patent applications, Vol. 19, 1948, pp. 79s, 797.799-
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| SE719909X | 1951-11-02 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| DE971893C true DE971893C (en) | 1959-04-09 |
Family
ID=20315945
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DEA16767A Expired DE971893C (en) | 1951-11-02 | 1952-10-30 | Process to increase the corrosion resistance of acid-proof steel |
Country Status (2)
| Country | Link |
|---|---|
| DE (1) | DE971893C (en) |
| GB (1) | GB719909A (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE643869C (en) * | 1930-09-24 | 1937-04-19 | Mij Tot Exploitatie Van De Par | Process for the treatment of magnesium, zinc or iron surfaces |
| DE661253C (en) * | 1937-03-06 | 1938-06-14 | Bruno Waeser Dr Ing | Process for the production of protective layers on objects made of aluminum or aluminum-containing alloys |
-
1952
- 1952-10-30 DE DEA16767A patent/DE971893C/en not_active Expired
- 1952-10-30 GB GB27314/52A patent/GB719909A/en not_active Expired
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE643869C (en) * | 1930-09-24 | 1937-04-19 | Mij Tot Exploitatie Van De Par | Process for the treatment of magnesium, zinc or iron surfaces |
| DE661253C (en) * | 1937-03-06 | 1938-06-14 | Bruno Waeser Dr Ing | Process for the production of protective layers on objects made of aluminum or aluminum-containing alloys |
Also Published As
| Publication number | Publication date |
|---|---|
| GB719909A (en) | 1954-12-08 |
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