DED0000459MA - Process for the production of sulphurous vat dyes - Google Patents
Process for the production of sulphurous vat dyesInfo
- Publication number
- DED0000459MA DED0000459MA DED0000459MA DE D0000459M A DED0000459M A DE D0000459MA DE D0000459M A DED0000459M A DE D0000459MA
- Authority
- DE
- Germany
- Prior art keywords
- dyes
- production
- sulfur
- sulphurous
- vat dyes
- 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
- 238000000034 method Methods 0.000 title claims description 4
- 238000004519 manufacturing process Methods 0.000 title claims description 3
- 239000000984 vat dye Substances 0.000 title description 3
- 239000000975 dye Substances 0.000 claims description 11
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 5
- 239000011593 sulfur Substances 0.000 claims description 5
- 229910052717 sulfur Inorganic materials 0.000 claims description 5
- 238000004040 coloring Methods 0.000 claims description 3
- GRWZHXKQBITJKP-UHFFFAOYSA-L dithionite(2-) Chemical compound [O-]S(=O)S([O-])=O GRWZHXKQBITJKP-UHFFFAOYSA-L 0.000 claims description 3
- 238000006396 nitration reaction Methods 0.000 claims description 3
- 125000000449 nitro group Chemical group [O-][N+](*)=O 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims 3
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 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
- 239000000203 mixture Substances 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000000988 sulfur dye Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 150000002828 nitro derivatives Chemical class 0.000 description 1
- 229920001021 polysulfide Polymers 0.000 description 1
- 238000005185 salting out Methods 0.000 description 1
- 210000004243 sweat Anatomy 0.000 description 1
- 235000013311 vegetables Nutrition 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Description
j.n.unn 30. to. η jnunn 30. to. η
' Ref.No.1940'Ref.No. 1940
Dr.f.ZERWECKDr.f.ZERWECK
Frankfurt a/M-Fechenheim, 2a.November 1949Frankfurt a / M-Fechenheim, November 2nd, 1949
Es wurde gefunden, dass man neue schwefelhaltige Küpenfarb» stoffe erhält, wenn man l.S^-Benzanthrachinone nitriert, bis mehr als eine Nitrogruppe in da3 Molekül eintritt und das erhaltene Nitrierunga> produkt mit Schwefel alkalien behandelt.It has been found that new sulphurous vat dyes are obtained if 1, S ^ -Benzanthraquinones are nitrated up to more than a nitro group enters the molecule and the nitration product obtained is treated with an alkaline sulfur.
Die Konstitution der so erhaltenen Farbstoffe igt noch un® bekannt, jioch dürfte es sich vielleicht um schwefelhaltige Abkömmlinge des Indoloanthroas der Formel .·The constitution of the dyes obtained in this way is still unknown, but it may be sulfur-containing derivatives of the indoloanthroas of the formula.
handeln. Sie färben pflanzliche Fasern sowohl aus dem Schwe:Act. They dye vegetable fibers both from the sweat:
bade, wie auch aus kalter· oder heieser Hydrosulfitküpe in grauen big schwarzbraunen Tönen, Infolge ihrer Anwendbarkeit bei den verschiede* nen für Küpenfarbstoffe und Schwefelfarbstoffe üblichen Färbemethoden eignen sie sich besonders für Mischungen mit anderen Ktfpen- oder Sehwefelfarbstoffen.bathe, as well as from cold or hot hydrosulfite vat in gray, big black-brown tones, due to their applicability to the various * NEN dyeing methods customary for vat dyes and sulfur dyes, they are particularly suitable for mixtures with other ktfpen or Sulfur dyes.
26 kg 1.2-Beazanthraohinon werden in SOO kg konz.Schwefelsäure gelöst und unter Rühren und Kühles bei etwa 0 bis t5°|Tjnit 18 kg Mischung, die 88% kon z,Salpetersäure und 12% konz. Schwefelsäure hält, nitriert. Nach mehrstündigem Umrühren bei gewöhnlicher tür wird auf Eis gegossen, abgesaugt und neutral gewaschen; die noch feuchte Nitroverbindu,ng wird portionsweise in eine Lösung vor 260 kg Schwefelnatrium kriet. in 400 1+·* Wasser unter· Rühren eingetragen, wo» bei in eine* heftigen Reaktion eine dunkelbraune lösmng entstehtf die die Laufverbindung des neuen Farbstoffs enthält. Die isolierung des? Farbstoffs geschieht auf den üblichen Wegen? beispielsweise durch26 kg of 1,2-beazanthraohinone are dissolved in 50 kg of concentrated sulfuric acid and stirred and cooled at about 0 to t5 ° with 18 kg of mixture containing 88 % conc, nitric acid and 12% conc. Sulfuric acid holds, nitrated. After several hours of stirring at the usual door, it is poured onto ice, filtered off with suction and washed neutral; the still moist nitro compound is added in portions to a solution in front of 260 kg of sodium sulphide. * Water introduced into 400 1 + · · under stirring, where "with a * violent reaction a dark brown lösmng arises f includes the run-connection of the new dye. The isolation of the? Dye happens in the usual ways ? for example through
Ref.No.1940Ref.No. 1940
Aussalzen und Einblasen von Luft oder d,ur©h allmähliche Zugabe von Säuren. Der Farbstoff stellt in trockener Form ein schwarzes Pulver dar, das sowohl aus der Hydrosulfitküpe als auch aus dem Sohwefelna* triuraba&e Baumwolle echt grau färbt. In konz.Schwefeisäure löst er sich mit sfchwarzer Farbe und kann au« dieser Lösung unverändert wie® der in feiner Form gefällt werden.Salting out and blowing in air or, moreover, gradual addition of acids. When dry, the dye is a black powder which dyes cotton really gray both from the hydrosulfite vat and from the Sohwefelna * triuraba & e cotton. It dissolves in concentrated sulfuric acid is black in color and can be precipitated from this solution unchanged as it is in fine form.
Statt des Sehwefelnatriums können mit gleichem Erfolg auch Alkalipolysulfide angewendet werden.Instead of sodium sulphide, alkali polysulphides can also be used with the same success.
Etwas mehr braunschwarz färbende Farbstoffe werden erhalten, wenn man z,B. in BzS-Chlor-l.S-r-benzanthrachinon (Monatshefte,Bd.41, S.592 Anm.) und 3-ChIOr-I.2-benzanthraehinon (Berichte,Bd.4$,S.Θ70) njehr als eine Nitrogrxipp® einführt Tind dünn mit Sohwefelalkalien be® handelt,Somewhat more brownish-black coloring dyes are obtained if, for example,. in BzS-chlorine-l.S-r-benzanthraquinone (monthly booklet, vol. 41, P.592 note) and 3-ChIOr-I.2-benzanthraehinon (reports, vol. 4 $, p. 70) no more than a Nitrogrxipp® introduces Tind thin with soh sulphurous alkalis be® acts,
Wird Tiie Nitrierung mit drei und mehr Molekülen Salpeter® säure ausgeführt, so erhält man bei der weiteren Kondensation mit Sehwefelalkal^sn ga*^ ähnlich färbende Farbstoffe mit gleich guten Echtheitseigenscha ften.If the nitration is carried out with three or more molecules of nitric acid, then with the further condensation one obtains with Sehulfuralkal ^ sn ga * ^ similar coloring dyes with equally good fastness properties.
Claims (1)
Family
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