DE655487C - Process for the production of sulfur dyes - Google Patents
Process for the production of sulfur dyesInfo
- Publication number
- DE655487C DE655487C DEI55257D DEI0055257D DE655487C DE 655487 C DE655487 C DE 655487C DE I55257 D DEI55257 D DE I55257D DE I0055257 D DEI0055257 D DE I0055257D DE 655487 C DE655487 C DE 655487C
- Authority
- DE
- Germany
- Prior art keywords
- production
- parts
- sulfur dyes
- dyes
- sulfur
- 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
- 239000000988 sulfur dye Substances 0.000 title claims description 5
- 238000004519 manufacturing process Methods 0.000 title claims description 4
- 238000000034 method Methods 0.000 title claims description 4
- 230000004048 modification Effects 0.000 claims 1
- 238000012986 modification Methods 0.000 claims 1
- 239000000975 dye Substances 0.000 description 7
- 229910052979 sodium sulfide Inorganic materials 0.000 description 3
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 229920000742 Cotton Polymers 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 238000004043 dyeing Methods 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 238000010992 reflux Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 235000002852 Olea africana Nutrition 0.000 description 1
- 244000061775 Olea africana Species 0.000 description 1
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 1
- YGEAPCJSIZWGJL-UHFFFAOYSA-L [Cr+3].S(=O)(=O)([O-])[O-].[Cu+2] Chemical compound [Cr+3].S(=O)(=O)([O-])[O-].[Cu+2] YGEAPCJSIZWGJL-UHFFFAOYSA-L 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229940100198 alkylating agent Drugs 0.000 description 1
- 239000002168 alkylating agent Substances 0.000 description 1
- 239000001049 brown dye Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 238000010411 cooking Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002828 nitro derivatives Chemical class 0.000 description 1
- 229920001021 polysulfide Polymers 0.000 description 1
- 239000005077 polysulfide Substances 0.000 description 1
- 150000008117 polysulfides Polymers 0.000 description 1
- 229940072033 potash Drugs 0.000 description 1
- 235000015320 potassium carbonate Nutrition 0.000 description 1
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B49/00—Sulfur dyes
- C09B49/12—Sulfur dyes from other compounds, e.g. other heterocyclic compounds
- C09B49/124—Sulfur dyes from other compounds, e.g. other heterocyclic compounds from polycarbocyclic compounds
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Coloring (AREA)
Description
Verfahren zur Herstellung von Schwefelfarbstoffen Zusatz zum Patent 653 675 Gegenstand des Patents 653 675 ist ein Verfahren zur Herstellung von Schwefelfarbstoffen, das darin besteht, daß man Dekacyclen, gegebenenfalls ?i Anwesenheit von Metallsalzen, mit schwefelnden Mitteln behandelt und die Rohschmelze in bekannter Weise aufarbeitet. Man erhält dabei rotbraune Farbstoffe von besonderer Klarheit und einem bisher nicht erreichten Rotstich der mit ihnen erzielbaren Färbungen.Process for the production of sulfur dyes. Patent addition 653 675 The subject of patent 653 675 is a process for the production of sulfur dyes, that consists in the fact that one decacycles, if necessary? i presence of metal salts, treated with sulphurizing agents and worked up the raw melt in a known manner. This gives red-brown dyes of particular clarity and one not so far achieved red tint of the dyeings that can be achieved with them.
Wie nun weiter gefunden wurde, gelangt man zu gleichfalls wertvollen Schwefelfarbstoffen von gelbbrauner bis braunoliver Tönung ihrer Färbung, wenn man statt des Dekacyclens seine Nitroverbindungen der Schwefelung unterwirft. Durch Nachbehandlung der Färbungen mit Alkylierungsmitteln wird .ein lebhafterer und mit Kupfersülfatchromkali ein grünerer Farbton erhalten.As has now been found, one arrives at equally valuable ones Sulfur dyes from yellow-brown to brown-olive hue of their coloration, if one instead of decacycle, subjects its nitro compounds to sulphurization. By Post-treatment of the dyeings with alkylating agents becomes .a livelier and with Copper sulphate chromium potash obtained a greener shade.
Beispiel 1 i oo Teile Trinitr odekacyclen, das man durch Einwirkung von Salpetersäure (D= 1.q.2) ,auf Dekacyclen bei o bis 18° herstellen kann, werden mit 3oo Teilen kristallisiertem Natriumsulfid und Zoo Teilen Schwefel unter Rühren etwa 26 Stunden bei 118° am Rückfllußkühler gekocht. Die Temperatur der Schmelze wird nun unter Abdestillieren von Wasser langsam auf 17o° gesteigert und etwa, 18 Stunden auf dieser Höhe gehalten. Die Farbstoffrohschmelze kann als solche zum Ausfärben verwendet werden oder aber sie wird mit Natriumsulfid in Wasser gelöst. worauf der Farbstoff in bekannter Weise abgeschieden wird. In diesem Falle erhält man etwa 155 Teile Farbstoff, der Baumwolle in gelbbraunen Tönen von guter Echtheit anfärbt.Example 1 100 parts Trinitr odekacyclen, which one by action of nitric acid (D = 1.q.2), can be produced on decacycles at 0 to 18 ° with 300 parts of crystallized sodium sulfide and zoo parts of sulfur with stirring boiled for about 26 hours at 118 ° on a reflux condenser. The temperature of the melt is now slowly increased to 170 ° while distilling off water and about, 18 Hours at this height. The raw dye melt can be used as such for coloring can be used or it is dissolved in water with sodium sulfide. what the Dye is deposited in a known manner. In this case you get about 155 parts of dye that dyes cotton in yellow-brown shades of good fastness.
Beispiel 2 1 oo Teile H:exanitrodekacyclen, durch Einwirkung von Salpetersäure der Dichte 1,5 auf Dekacyclenbeietwa 2o°;erhalten, werden unter Rühren in eine aus 35o Teilen kristallisiertem l,Tatriumsulfid und 15o Teilen Schwefel hergestellte Polysulfidlösung eingetragen und 24 Stunden bei einer Kochtemperatur von 115° am Rückflußkühler erhitzt. Das Reaktionsgemisch wird dann langsam zur Trockene eingedampft und :etwa 2o Stunden bei 22o nachgebacken. Man löst die erhaltene Rohschmelze in bekannter Weise in Wasser und fällt den Farbstoff mit Säure. Die Ausbeutc beträgt 105 bis i io Teile Farbstoff. Er färbt Baumwolle in braunen Tönen, die neben sonstigen guten Echtheitseigenschaften besonders eine gute Lichtechtheit aufweisen.Example 2 100 parts of H: exanitrodecacycles, by the action of nitric acid with a density of 1.5 to decacycles at about 2o °; are poured into an off with stirring 35o parts of crystallized oil, sodium sulfide and 150 parts of sulfur Polysulfide solution entered and 24 hours at a cooking temperature of 115 ° am Heated reflux condenser. The reaction mixture is then slowly evaporated to dryness and: baked for about 20 hours at 22o. The raw melt obtained is dissolved in known way in water and precipitates the dye with acid. The yield is 105 to 10 parts dye. He dyes cotton in brown tones, in addition to others have good fastness properties, especially good lightfastness.
Claims (1)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DEI55257D DE655487C (en) | 1936-06-17 | 1936-06-17 | Process for the production of sulfur dyes |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DEI55257D DE655487C (en) | 1936-06-17 | 1936-06-17 | Process for the production of sulfur dyes |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| DE655487C true DE655487C (en) | 1938-01-17 |
Family
ID=7194067
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DEI55257D Expired DE655487C (en) | 1936-06-17 | 1936-06-17 | Process for the production of sulfur dyes |
Country Status (1)
| Country | Link |
|---|---|
| DE (1) | DE655487C (en) |
-
1936
- 1936-06-17 DE DEI55257D patent/DE655487C/en not_active Expired
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