DE1217957B - Process for the production of solutions of copper-chromium (III) complexes that are homogeneously miscible with water - Google Patents
Process for the production of solutions of copper-chromium (III) complexes that are homogeneously miscible with waterInfo
- Publication number
- DE1217957B DE1217957B DEC14011A DEC0014011A DE1217957B DE 1217957 B DE1217957 B DE 1217957B DE C14011 A DEC14011 A DE C14011A DE C0014011 A DEC0014011 A DE C0014011A DE 1217957 B DE1217957 B DE 1217957B
- Authority
- DE
- Germany
- Prior art keywords
- chromium
- copper
- water
- complexes
- iii
- 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.)
- Pending
Links
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims description 8
- 238000000034 method Methods 0.000 title claims description 6
- 238000004519 manufacturing process Methods 0.000 title claims description 5
- OJSIAYFWYKWVKK-UHFFFAOYSA-N copper chromium(3+) Chemical class [Cr+3].[Cu+2] OJSIAYFWYKWVKK-UHFFFAOYSA-N 0.000 title description 3
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 9
- 229910052804 chromium Inorganic materials 0.000 claims description 8
- 239000011651 chromium Substances 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 239000005725 8-Hydroxyquinoline Substances 0.000 claims description 2
- 150000001879 copper Chemical class 0.000 claims description 2
- 229960003540 oxyquinoline Drugs 0.000 claims description 2
- MCJGNVYPOGVAJF-UHFFFAOYSA-N quinolin-8-ol Chemical compound C1=CN=C2C(O)=CC=CC2=C1 MCJGNVYPOGVAJF-UHFFFAOYSA-N 0.000 claims description 2
- GXDVEXJTVGRLNW-UHFFFAOYSA-N [Cr].[Cu] Chemical compound [Cr].[Cu] GXDVEXJTVGRLNW-UHFFFAOYSA-N 0.000 claims 2
- 229940068911 chloride hexahydrate Drugs 0.000 claims 1
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 9
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 6
- 229910052802 copper Inorganic materials 0.000 description 6
- 239000010949 copper Substances 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 5
- 230000001476 alcoholic effect Effects 0.000 description 5
- KRVSOGSZCMJSLX-UHFFFAOYSA-L chromic acid Substances O[Cr](O)(=O)=O KRVSOGSZCMJSLX-UHFFFAOYSA-L 0.000 description 3
- LJAOOBNHPFKCDR-UHFFFAOYSA-K chromium(3+) trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Cl-].[Cr+3] LJAOOBNHPFKCDR-UHFFFAOYSA-K 0.000 description 3
- AWJWCTOOIBYHON-UHFFFAOYSA-N furo[3,4-b]pyrazine-5,7-dione Chemical compound C1=CN=C2C(=O)OC(=O)C2=N1 AWJWCTOOIBYHON-UHFFFAOYSA-N 0.000 description 3
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 3
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 3
- -1 8-hydroxyquinoline-copper-chromium Chemical compound 0.000 description 2
- 229910001122 Mischmetal Inorganic materials 0.000 description 2
- 240000007817 Olea europaea Species 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000010992 reflux Methods 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- JHWIEAWILPSRMU-UHFFFAOYSA-N 2-methyl-3-pyrimidin-4-ylpropanoic acid Chemical compound OC(=O)C(C)CC1=CC=NC=N1 JHWIEAWILPSRMU-UHFFFAOYSA-N 0.000 description 1
- 229920003043 Cellulose fiber Polymers 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- ZCDOYSPFYFSLEW-UHFFFAOYSA-N chromate(2-) Chemical compound [O-][Cr]([O-])(=O)=O ZCDOYSPFYFSLEW-UHFFFAOYSA-N 0.000 description 1
- SOCTUWSJJQCPFX-UHFFFAOYSA-N dichromate(2-) Chemical compound [O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O SOCTUWSJJQCPFX-UHFFFAOYSA-N 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 230000002538 fungal effect Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 125000002524 organometallic group Chemical group 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F11/00—Compounds containing elements of Groups 6 or 16 of the Periodic Table
- C07F11/005—Compounds containing elements of Groups 6 or 16 of the Periodic Table compounds without a metal-carbon linkage
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
Description
Verfahren zur Herstellung von mit Wasser homogen mischbaren Lösungen von Kupfer-Chrom(III)-Komplexen Die Herstellung wasserlöslicher organometallischer Komplexe vom Werner-Typ, die im Kation Chrom und eine organische Komponente enthalten, ist insbesondere in den USA.-Patentschriften 2273 040, 2356161, 2524803 und 2549220 sowie in der französischen Patentschrift 1 130 229 beschrieben.Process for the production of solutions which are homogeneously miscible with water of copper-chromium (III) complexes The production of water-soluble organometallic Werner-type complexes containing chromium and an organic component in the cation, is particularly in U.S. Patents 2273,040, 2356161, 2524803 and 2549220 as well as in French patent specification 1,130,229.
Es wurde nunmehr gefunden, daß man mit Wasser homogen mischbare Lösungen von Kupfer-Chrom(III) Komplexen erhält, wenn man in einem mit Wasser unbeschränkt mischbaren Alkohol bei erhöhter Temperatur das Kupfersalz des 8-Hydroxychinolins mit Chrom(III)-chlorid-hexahydrat umsetzt. It has now been found that solutions which are homogeneously miscible with water can be obtained of copper-chromium (III) complexes obtained, if one is unlimited in one with water miscible alcohol at elevated temperature, the copper salt of 8-hydroxyquinoline with chromium (III) chloride hexahydrate.
Das hydratisierte Chlorid des dreiwertigen Chroms, das zur Durchführung des erfindungsgemäßen Verfahrens benötigt wird, kann durch Reduktion eines Chromats oder eines Bichromats mit Salzsäure erhalten werden. Diese Reduktion kann auch in Gegenwart des Alkohols bewirkt werden, der als Lösungsmittel für die Herstellung der Mischmetallkomplexe dient. The hydrated chloride of trivalent chromium, which is used to carry out of the method according to the invention is required, can by reducing a chromate or a bichromate can be obtained with hydrochloric acid. This reduction can also be done in Presence of the alcohol can be used as a solvent for the manufacture the mischmetal complex is used.
Die erfindungsgemäß erhältlichen Metallmischkomplexe sollen zur Behandlung von Cellulosefasern dienen, um sie gegen Pilzbefall zu schützen. The mixed metal complexes obtainable according to the invention are intended for treatment of cellulose fibers serve to protect them against fungal attack.
Die nachstehenden Beispiele, in denen die angegebenen Teile, falls nichts anderes angegeben ist, Gewichtsteile sind, erläutern die vorliegende Erfindung, ohne den Erfindungsbereich in irgendeiner Weise einschränken zu wollen. The examples below showing the parts indicated, if unless otherwise specified, are parts by weight, illustrate the present invention, without wishing to restrict the scope of the invention in any way.
Beispiel 1 1320 Teile Kupfer-8-oxychinolat werden in 5600 Teilen Isopropylalkohol suspendiert, worauf man 3936 Teile Chrom(III)-chlorid-hexahydrat hinzusetzt und 2 bis 3 Stunden zum Sieden erhitzt. Man erhält auf diese Weise 10500 bis 10800 Teile einer alkoholischen Lösung eines 8-Hydroxychinolin-Kupfer-Chrom(IIt)-Mischkomplexes von olivgrüner Farbe, der 3,92 Grammatome Chrom pro Mol Kupfer-8-oxychinolat enthält. Diese alkoholische Lösung ist in der 50fachen Menge Wasser löslich. Example 1 1320 parts of copper 8-oxyquinolate are used in 5600 parts Isopropyl alcohol suspended, whereupon 3936 parts of chromium (III) chloride hexahydrate added and heated to boiling for 2 to 3 hours. This gives 10500 up to 10800 parts of an alcoholic solution of an 8-hydroxyquinoline-copper-chromium (IIt) mixed complex olive green in color, containing 3.92 gram atoms of chromium per mole of copper 8-oxyquinolate. This alcoholic solution is soluble in 50 times the amount of water.
Beispiel 2 Eine Suspension von 400 Teilen Chromsäure in 1300 Teilen Isopropylalkohol wird gerührt und zum Sieden gebracht. Man hört dann mit dem Erhitzen auf und führt mittels eines Tauchrohrs 438 Teile Chlorwasserstoffgas ein. Auf diese Weise wird die Chromsäure zu dreiwertigem Chrom reduziert. Sobald der gesamte Chlorwasserstoff in die Reaktion eingeführt ist, erhitzt man 30 Minuten lang am Rückfluß und setzt 304 Teile Kupfer-8-oxychinolat hinzu. Man behandelt noch weitere 2 bis 3 Stunden am Rückfluß und erhält schließlich eine alkoholische Lösung eines Mischkomplexes von olivgrüner Farbe, der 4,6 Grammatome Chrom pro Mol Kupfer-8-oxychinolat enthält. Example 2 A suspension of 400 parts of chromic acid in 1300 parts Isopropyl alcohol is stirred and brought to the boil. You then hear with the heating and introduces 438 parts of hydrogen chloride gas by means of a dip tube. To this Chromic acid is reduced to trivalent chromium. Once all of the hydrogen chloride is introduced into the reaction, reflux for 30 minutes and set 304 parts of copper-8-oxyquinolate are added. Treatment is continued for another 2 to 3 hours at reflux and finally receives an alcoholic solution of one Mixed complex Olive green in color, containing 4.6 gram atoms of chromium per mole of copper 8-oxyquinolate.
Diese Lösung ist in der 50fachen Menge Wasser löslich.This solution is soluble in 50 times the amount of water.
Beispiel 3 Man arbeitet wie im Beispiel 1, benutzt indessen 1500 Teile Kupfer-8-oxychinolat und 2250 Teile Chrom(III)-chlorid-hexahydrat. Man erhält auf diese Weise eine alkoholische Lösung eines wasserlöslichen Mischmetallkomplexes, der 2 Grammatome Chrom pro Mol Kupfer-8-oxychinolat enthält. Example 3 The procedure is as in Example 1, but 1500 is used Parts of copper 8-oxyquinolate and 2250 parts of chromium (III) chloride hexahydrate. You get in this way an alcoholic solution of a water-soluble mischmetal complex, which contains 2 gram atoms of chromium per mole of copper 8-oxyquinolate.
Beispiel 4 Man arbeitet wie im Beispiel 2, benutzt indessen 1192 Teile kristallisiertes Natriumbichromat an Stelle von Chromsäure und 1500 Teile Äthanol an Stelle von Isopropylalkohol. Man leitet in die Suspension einen Strom von 1170 Teilen Chlorwasserstoffgas ein. Example 4 The procedure is as in Example 2, but 1192 is used Parts of crystallized sodium dichromate in place of chromic acid and 1500 parts Ethanol instead of isopropyl alcohol. A stream is passed into the suspension of 1170 parts of hydrogen chloride gas.
Das sich niederschlagende Natriumchlorid wird durch Filtration abgetrennt. Man erhält eine alkoholische Lösung eines grünolivfarbigen, wasserlöslichen Komplexes, der 9,25 Grammatome Chrom pro Mol lÇupfer-8-oxychinolat enthält.The precipitating sodium chloride is separated off by filtration. An alcoholic solution of a green-olive-colored, water-soluble complex is obtained, the Contains 9.25 gram atoms of chromium per mole of copper 8-oxyquinolate.
Claims (1)
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| FR1217957X | 1955-11-25 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| DE1217957B true DE1217957B (en) | 1966-06-02 |
Family
ID=9677205
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DEC14011A Pending DE1217957B (en) | 1955-11-25 | 1956-11-24 | Process for the production of solutions of copper-chromium (III) complexes that are homogeneously miscible with water |
Country Status (1)
| Country | Link |
|---|---|
| DE (1) | DE1217957B (en) |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2683156A (en) * | 1951-06-18 | 1954-07-06 | Du Pont | Process for the production of werner type chromium complexes |
-
1956
- 1956-11-24 DE DEC14011A patent/DE1217957B/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2683156A (en) * | 1951-06-18 | 1954-07-06 | Du Pont | Process for the production of werner type chromium complexes |
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