[go: up one dir, main page]

DE1047965B - Process for the production of water-insoluble azo dyes - Google Patents

Process for the production of water-insoluble azo dyes

Info

Publication number
DE1047965B
DE1047965B DEF20583A DEF0020583A DE1047965B DE 1047965 B DE1047965 B DE 1047965B DE F20583 A DEF20583 A DE F20583A DE F0020583 A DEF0020583 A DE F0020583A DE 1047965 B DE1047965 B DE 1047965B
Authority
DE
Germany
Prior art keywords
water
azo dyes
production
insoluble azo
amino
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
Application number
DEF20583A
Other languages
German (de)
Inventor
Dr Herbert Kracker
Dr Kurt Gengnagel
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Hoechst AG
Original Assignee
Hoechst AG
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Hoechst AG filed Critical Hoechst AG
Priority to DEF20583A priority Critical patent/DE1047965B/en
Publication of DE1047965B publication Critical patent/DE1047965B/en
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D17/00Pigment pastes, e.g. for mixing in paints
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09BORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
    • C09B29/00Monoazo dyes prepared by diazotising and coupling
    • C09B29/10Monoazo dyes prepared by diazotising and coupling from coupling components containing hydroxy as the only directing group
    • C09B29/18Monoazo dyes prepared by diazotising and coupling from coupling components containing hydroxy as the only directing group ortho-Hydroxy carbonamides
    • C09B29/20Monoazo dyes prepared by diazotising and coupling from coupling components containing hydroxy as the only directing group ortho-Hydroxy carbonamides of the naphthalene series
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06PDYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P1/00General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
    • D06P1/02General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using azo dyes

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Textile Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Coloring (AREA)

Description

Verfahren zur Herstellung von wasserunlöslichen Azofarbstoffen Es wurde gefunden, daß man zu wertvollen wasserunlöslichen Azofarbstoffen gelangt, wenn man die Diazoniumverbindung aus 1-Amino-4-fluorbenzol-2-carbonsäuremethylester mit Arylamiden der 2,3-Oxynaphthoesäure in Substanz, auf der Faser oder auf einer anderen Grundlage kuppelt.Process for the production of water-insoluble azo dyes Es it was found that valuable water-insoluble azo dyes can be obtained, when you get the diazonium compound from 1-amino-4-fluorobenzene-2-carboxylic acid methyl ester with aryl amides of 2,3-oxynaphthoic acid in substance, on the fiber or on a other basis couples.

Mit den neuen Farbstoffen erhält man auf der pflanzlichen Faser, einschließlich solcher aus regenerierter Cellulose, nach den bekannten Färbeverfahren orangefarbige bis scharlachrote Färbungen, die sich bei sehr guten Lichtechtheiten vielfach durch gute Chlor- und Superoxydechtheiten auszeichnen. Auf synthetischen Fasern, wie Acetylcellulose-, Polyamid- oder Polyäthylenterephthalatfasern, erhält man ebenfalls Färbungen von wertvollen Echtheitseigenschaften.With the new dyes one gets on the vegetable fiber, including those made from regenerated cellulose, orange-colored according to the known dyeing processes to scarlet colorings, which show very good lightfastness in many cases have good chlorine and superoxide fastness properties. On synthetic fibers, such as acetyl cellulose, Polyamide or polyethylene terephthalate fibers are also obtained by dyeing valuable authenticity properties.

Die Farbstoffe lassen sich auch in Substanz oder auf einem Substrat herstellen und können zum Färben von hochmolekularen plastischen Massen oder für die Zubereitung von Farblacken verwendet werden. Sie können außerdem zur Herstellung gefärbter Filme in Massen aus Celluloseestern oder -äthern eingebracht oder im Pigmentdruckverfahren auf Textilien aufgebracht werden. Die Diazokomponente kann bei dem erfindungsgemäßen Verfahren gegebenenfalls als stabilisierte Diazoverbindung, beispielsweise als Diazoniumchlorid-Chlorzinkdoppelsalz, Diazoaminoverbindung oder als Antidiazotat nach einem der üblichen Färbe- oder Druckverfahren verwendet werden.The dyes can also be used in bulk or on a substrate manufacture and can be used for coloring high molecular weight plastic masses or for the preparation of colored lakes can be used. You can also use it to manufacture colored films introduced in bulk from cellulose esters or ethers or in the pigment printing process can be applied to textiles. The diazo component can be used in the inventive Process optionally as a stabilized diazo compound, for example as a diazonium chloride-chlorozinc double salt, Diazoamino compound or as an antidiazotate by one of the customary dyeing or printing processes be used.

Die Herstellung des als Diazokomponente verwendeten 1-Amino-4-fluorbenzol-2-carbonsäuremethylesters kann nach bekannten Verfahren erfolgen, beispielsweise durch Veresterung des aus 3-Fluorbenzotrichlorid erhaltenen 3-Fluorbenzoylchlorids mit Methylalkohol, Nitrierung des 3-Fluorbenzoesäuremethylesters und Reduktion zur Aminoverbindung.The preparation of the 1-amino-4-fluorobenzene-2-carboxylic acid methyl ester used as the diazo component can be carried out by known methods, for example by esterification of the from 3-fluorobenzotrichloride obtained 3-fluorobenzoyl chloride with methyl alcohol, nitration of 3-fluorobenzoic acid methyl ester and reduction to the amino compound.

Gegenüber den aus der deutschen Patentschrift 942325 bekannten wasserunlöslichen Azofarbstoffen aus diazotiertem 1-Amino-4-chlorbenzol-2-carbonsäureäthylester und 2,3-Oxynaphthoesäurearylamiden zeichnen sich die neuen Farbstoffe durch eine bessere Licht-, Chlor-, Superoxyd- und Bügelechtheit aus.Compared to the water-insoluble ones known from German patent 942325 Azo dyes from diazotized 1-amino-4-chlorobenzene-2-carboxylic acid ethyl ester and 2,3-Oxynaphthoesäurearylamiden the new dyes are characterized by better Fastness to light, chlorine, superoxide and iron.

Beispiel 1 100 kg Baumwollgarn auf Kreuzspulen, das gut vorgereinigt, gespült und entwässert ist, werden 30 Minuten bei 35 bis 40° C in dem nachstehenden Bad behandelt: 2 kg 1-(2',3'-Oxynaphthoylamino)-2-methoxy-4-chlor-5-methylbenzol weiden mit 31 denaturiertem Alkohol angeteigt und unter Rühren in 11 Natronlauge von 38'B6 und 41 Wasser von 40°C gelöst. Nach Zugabe von 1 1 Formaldehydlösung (33°,`g) wird die so erhaltene Lösung nach etwa lO Minuten in ein Bad eingerührt, das in 10001 Wasser 51 eines Kondensationsproduktes aus höhermolekularen Fettsäuren und Eiweißabbauprodukten sowie 101 Natronlauge von 38° B6 enthält.Example 1 100 kg of cotton yarn on cheeses, which has been thoroughly pre-cleaned, rinsed and drained, are treated for 30 minutes at 35 to 40 ° C in the following bath: 2 kg of 1- (2 ', 3'-oxynaphthoylamino) -2-methoxy- 4-chloro-5-methylbenzene is made into a paste with 31 denatured alcohol and dissolved in 11 sodium hydroxide solution at 38 ° C and 41 ° C water at 40 ° C. while stirring. After adding 1 liter of formaldehyde solution (33 °, `g), the resulting solution is stirred, after about 10 minutes, into a bath which contains, in 10001 of water, 51 of a condensation product of higher molecular weight fatty acids and protein degradation products, as well as 101 sodium hydroxide solution of 38 ° B6.

Dann wird auf einen Flottengehalt von etwa 100 0/0 abgesaugt, mit einer Lösung von 30 kg Natriumchlorid und 21 Natronlauge von 38° B6 in 10001 kaltem Wasser zwischengespült, wieder abgesaugt und 30 Minuten bei 10 bis 15° C mit einer Diazolösung entwickelt, die in 10001 Wasser die Diazoverbindung aus 1,69 kg 1-Amino-4-fluorbenzol-2-carbonsäuremethylester, 10,5 kg Mononatriumphosphat, 112 kg Dinatriumphosphat und 0,51 eines Einwirkungsproduktes von etwa 20 12o1 Äthylenoxyd auf 1 DZol eines Fettalkohols enthält.Then it is sucked off to a liquor content of about 100 0/0, rinsed with a solution of 30 kg sodium chloride and 21 sodium hydroxide solution of 38 ° B6 in 10001 cold water, sucked off again and developed for 30 minutes at 10 to 15 ° C with a diazo solution, which in 10001 of water contains the diazo compound of 1.69 kg of 1-amino-4-fluorobenzene-2-carboxylic acid methyl ester, 10.5 kg of monosodium phosphate, 112 kg of disodium phosphate and 0.51 of an action product of about 20121 ethylene oxide to 1 double of a fatty alcohol.

Anschließend wird mit 3 ccm Salzsäure von 20° Be im Liter Wasser gespült, zunächst 20 Minuten bei 60° C mit 1 g äthylendiamintetraessigsaurem Natrium und 1 g eines Einwirkungsproduktes von etwa 10 Mol Äthylenoxyd auf 1 Mol eines Alkylphenols im Liter Wasser, dann 20 Minuten. bei 100° C mit 1 g äthylendiamintetraessigsaurem Natrium und 1 g eines Kondensationsproduktes aus einer Aminoalkylsulfonsäure und einer höhermolekularen Fettsäure im Liter Wasser nachbehandelt, gespült und getrocknet.Then it is rinsed with 3 ccm hydrochloric acid of 20 ° Be in the liter of water, first 20 minutes at 60 ° C with 1 g of ethylenediaminetetraacetic acid sodium and 1 g of an action product of about 10 moles of ethylene oxide to 1 mole of an alkylphenol in a liter of water, then 20 minutes. at 100 ° C with 1 g of ethylenediaminetetraacetic acid Sodium and 1 g of a condensation product of an aminoalkylsulfonic acid and a higher molecular weight Fatty acid post-treated per liter of water, rinsed and dried.

Man erhält ein volles Scharlach von guten Echtheitseigenschaften. Dieselbe Färbung kann auch auf regenerierten Cellulosefasern, wie beispielsweise Reyon oder Zellwolle, nach den bei diesen Fasern üblichen Verfahren erhalten werden.A full scarlet with good fastness properties is obtained. The same coloration can also be used on regenerated cellulose fibers, such as Rayon or rayon, can be obtained by the methods customary for these fibers.

Beispiel 2 16,9 kg 1-Amino-4-fluorbenzol-2-carbonsäuremethylester werden in der üblichen Weise diazotiert. Die mit Natriumacetat auf Kongoneutralität abgestumpfte Diazolösung wird in eine durch Lösen in denaturiertem Alkohol und verdünnter Natronlauge und Ausfällen mit Essigsäure erhaltene Suspension von 35,7 kg 1-(2',3'-Oxynaphthoylamino)-2,5-dimethoxy-4-chlorbenzol eingerührt. Der nach beendeter Kupplung erhaltene Farbstoff wird abfiltriert, gut ausgewaschen und getrocknet. Er stellt ein orangefarbiges Pulver dar.Example 2 16.9 kg of 1-amino-4-fluorobenzene-2-carboxylic acid methyl ester are diazotized in the usual way. Those with sodium acetate on Congo neutrality Blunted diazo solution is converted into one by dissolving in denatured alcohol and diluting it Sodium hydroxide solution and precipitation with acetic acid obtained suspension of 35.7 kg of 1- (2 ', 3'-oxynaphthoylamino) -2,5-dimethoxy-4-chlorobenzene stirred in. The dye obtained after the coupling has ended is filtered off, good washed out and dried. It is an orange powder.

Die folgende Tabelle enthält noch eine Anzahl von weiteren unter Verwendung derselben Diazokomponente erhältlichen Azofarbstoffen sowie die Farbtöne der Baumwollfärbungen, die ebenfalls gute Echtheitseigenschaften besitzen. - -- Azokomponente Farbton 1-(2',3'-Oxynaphthoylamino) 2-methoxy- benzol............................. Orange 1-(2',3'-Oxynaphthoylamino)-2-methoxy- 5-chlorbenzol....................... desgl. 1-(2',3'-Oxynaphthoylamino)-2-methyl- 4-chlorbenzol....................... desgl. 1-(2',3'-Oxynaphthoylamino)- 2,4-dimethoxy-5-chlorbenzol.......... desgl. 2-(2',3'-Oxynaphthoylarnino)-naphthalin Scharlach 1-(6'-Brom-2',3'-oxynaphthoylamino)- 2-methoxybenzol ................... desgl. The following table also contains a number of other azo dyes obtainable using the same diazo component and the hues of the cotton dyeings, which also have good fastness properties. - - Azo component hue 1- (2 ', 3'-oxynaphthoylamino) 2-methoxy- benzene ............................. orange 1- (2 ', 3'-oxynaphthoylamino) -2-methoxy- 5-chlorobenzene ....................... the same. 1- (2 ', 3'-oxynaphthoylamino) -2-methyl- 4-chlorobenzene ....................... the same. 1- (2 ', 3'-oxynaphthoylamino) - 2,4-dimethoxy-5-chlorobenzene .......... the same. 2- (2 ', 3'-oxynaphthoylarnino) -naphthalene scarlet 1- (6'-bromo-2 ', 3'-oxynaphthoylamino) - 2-methoxybenzene ................... the same.

Claims (1)

PATENTANSPRUCH: Verfahren zur Herstellung von wasserunlöslichen Azofarbstoffen, dadurch gekennzeichnet, daß man die Diazoniumverbindung aus 1-Amino-4-fluorbenzol 2-carbonsäuremethylestermitArylamiden der2,3-Oxynaphthoesäure in Substanz, auf der Faser oder auf einer anderen Grundlage kuppelt. In Betracht gezogene Druckschriften: Deutsche Patentschrift Nr. 942325. Bei der Bekanntmachung der Anmeldung sind vier Färbetafeln nebst Erläuterung ausgelegt worden.PATENT CLAIM: Process for the production of water-insoluble azo dyes, characterized in that the diazonium compound is obtained from 1-amino-4-fluorobenzene 2-carboxylic acid methyl ester with arylamides of 2,3-oxynaphthoic acid in substance, on the Fiber or any other basis coupling. Considered publications: German patent specification No. 942325. When the application is published, there are four Coloring tables and explanations have been laid out.
DEF20583A 1956-06-20 1956-06-20 Process for the production of water-insoluble azo dyes Pending DE1047965B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
DEF20583A DE1047965B (en) 1956-06-20 1956-06-20 Process for the production of water-insoluble azo dyes

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DEF20583A DE1047965B (en) 1956-06-20 1956-06-20 Process for the production of water-insoluble azo dyes

Publications (1)

Publication Number Publication Date
DE1047965B true DE1047965B (en) 1958-12-31

Family

ID=7089733

Family Applications (1)

Application Number Title Priority Date Filing Date
DEF20583A Pending DE1047965B (en) 1956-06-20 1956-06-20 Process for the production of water-insoluble azo dyes

Country Status (1)

Country Link
DE (1) DE1047965B (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3321458A (en) * 1961-12-29 1967-05-23 Hoechst Ag Water-insoluble monoazo-dyestuffs

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE942325C (en) * 1952-06-27 1956-05-03 Hoechst Ag Process for the production of dye-fast dyeings on acetyl cellulose and linear polyamides or polyurethanes

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE942325C (en) * 1952-06-27 1956-05-03 Hoechst Ag Process for the production of dye-fast dyeings on acetyl cellulose and linear polyamides or polyurethanes

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3321458A (en) * 1961-12-29 1967-05-23 Hoechst Ag Water-insoluble monoazo-dyestuffs

Similar Documents

Publication Publication Date Title
DE848790C (en) Process for producing real tints
DE1047965B (en) Process for the production of water-insoluble azo dyes
DE2653284A1 (en) PROCESS FOR EVEN COLORING SYNTHETIC FIBER MATERIALS
DE609475C (en) Process for the production of water-insoluble azo dyes on fibrous materials or surface structures from cellulose esters and ethers
DE965346C (en) Process for the preparation of a water-insoluble monoazo dye
DE395917C (en) Process for the preparation of water-insoluble azo dyes
DE1088632B (en) Process for the preparation of a water-insoluble monoazo dye
DE956575C (en) Process for dyeing and printing polyacrylonitrile fibers
DE883284C (en) Process for the production of azo dyes on structures made of synthetic higher molecular weight polyamide compounds or on fiber mixtures which contain fibers from the polyamide compounds
DE899538C (en) Process for the preparation of water-insoluble monoazo dyes
DE556477C (en) Process for the preparation of azo dyes
DE1125099B (en) Process for the production of water-insoluble azo dyes
DE574964C (en) Process for the preparation of water-insoluble azo dyes
DE1088634B (en) Process for the preparation of a water-insoluble disazo dye
DE727946C (en) Process for the preparation of water-insoluble monoazo dyes
AT163420B (en) Process for producing true colorations
DE1019416B (en) Process for the preparation of water-insoluble monoazo dyes
DE2534870C2 (en) Process for the production of water-insoluble azo dyes on the fiber
DE700762C (en) Process for the production of colored threads, films, ribbons, artificial horsehair or similar structures made of cellulose esters or ethers
DE534890C (en) Process for dyeing rayon from regenerated cellulose
DE2214068C3 (en) Process for dyeing textile materials made from polyurethane fibers, synthetic polyamide fibers or from animal or animalized fibers with the use of organic solvents
DE1086833B (en) Process for the production of water-insoluble azo dyes
DE572473C (en) Process for the production of water-insoluble azo dyes on the fiber
CH352764A (en) Process for the production of water-insoluble azo dyes
CH351355A (en) Process for the production of water-insoluble azo dyes