DE42011C - - Google Patents

Description

IMPERIAL

PATENT OFFICE.

Those from the publications (Ber.XVII, 343, 603, 876, 1350, R. 525, and XVIII, R 627) has become known series of azo dye derivatives of paraphenylenediamine so far technically unevaluated. According to recent observations, however, some have so far Members of this series (not shown) have the property of cotton in an excellent degree to dye intensively, air-, light- and soap-fast without the use of mordants.

These are the following disazo compounds or combinations of tetrazophenyl with:

a) 2 molecules of alphanaphthol - alphamonosulfonic acid (corresponding to Piria's naphthoic acid), dyes cotton reddish blue; the color is resistant to diluted acetic acid and becomes pure blue with caustic soda;

b) ι Molecül Alphanaphthol-alphamonosulfonic acid (as above under a) and 1 molecule of betanaphthol-alphadisulfonic acid (R-Salz) stains Cotton blue, is not changed by acetic acid or caustic soda.

Griefs' amidodiazobenzene is used to represent the dyes mentioned (Ber. XVII, 603) or, more appropriately, from the acetylated diazo compound, Nietzki's diazoacetanilide (Ber. XVII, 343), the diazo compound of monacetyl-paraphenylenediamine and initially eliminates this Diazo compounds per 1 Molecül Alphanaphthol-alphamonosulfonic acid act. If the acetylated diazo compound is used, correspondingly acetylated amidoazo compounds are obtained, from which the acetyl group is then eliminated by boiling with caustic alkalis or dilute sulfuric acid. The amidoazo compound thus obtained, which is hereinafter referred to as p-amidobenzolazo-alphanaphthol-alphamonosulfonic acid is to be designated, is then diazotized and with 1 molecule of alphanaphthol - alphamonosulfonic acid, Betanaphthylamine monosulfonic acid or betanaphthol-alphadisulfonic acid combined.

For the representation of the dye combination mentioned under b) one can, however, also first the betanaphtol-alphadisulfonic acid in the already known amidoazo dye, the ρ - amidobenzene - azo - betanaphtol - alphadisulfonic acid (Ber. XVII, 343, 603) transfer this The dye is then diazotized and finally on ι Molecül Alphanaphtol-alphamonosulfosäure let absorb.

The following examples explain the special display method:

I. Preparation of p-amidobenzene-azoalphanaphthol-alphamonosulfonic acid the end

the diazoacetanilide.
ι 5 kg of acetylparaphenylenediamine (p - amidoacetanilide) are dissolved in a mixture of 45 kg of hydrochloric acid (32 pct.), 200 kg of water and 200 kg of ice. 7 kg of sodium nitrite, dissolved in three times the amount of water, are added to this solution, the mixture is stirred for 1 hour and then the solution of the resulting diazoacetanilide is added to a solution of 25 kg of alphanaphthol-alphamonosulfonic acid and 30 kg of soda ash in 2,000 kg of water .

Claims (4)

The alphanaphthol-alphamonosulfonic acid is expediently used in the form of its solution how to obtain such by reacting the diazonaphtionic acid, and determines their Content by titration with diazobenzene in a known manner. After standing for 24 hours, the resulting dye is precipitated by means of table salt, the mixture then boiled and left to cool. The crystalline azo body is then filtered, pressed and processed further while still moist. To separate the acetyl group, each 40 kg of the dry compound contained in the Prefsteig is boiled with 60 kg of sodium hydroxide solution (40 ⁰ B.) and 500 kg of water for several hours, replacing the evaporated water, until a sample is pure after diazotization and supersaturation with soda turns blue. II. Representation of the blue disazo compound from ρ - amidobenzene - azo alphanaphtol-alphamonosulfonic acid and Alphanaphtol - alphamonosulfonic acid (Combination a). The ρ - amidobenzene-azo-alphanaphtol alphamdnosulfosäure is diazotirt after cooling their obtained as above alkaline solution and dilution from 120 kg of hydrochloric acid (20 ⁰ B.) and precipitated with 7 kg of sodium nitrite; for complete formation of the diazo compound, the mixture is stirred at 0 ° for 24 hours. The diazo compound is then added to a solution of 25 kg of alphanaphthol-alphamonosulfonic acid and 60 kg of calcined soda in 1,000 kg of water. After 24 hours, the dye is precipitated with common salt from the violet solution formed and worked up as usual. III. Representation of the ρ - amidobenzolazo-alphanaphtol-alphamonosulfo acid from the amidodiazobenzene.
18 parts by weight of hydrochloric acid paraphenylenediamine are dissolved in 600 parts by weight of water; 50 parts by weight of crystallized sodium acetate, 100 parts by weight of glacial acetic acid and 100 parts by weight of ice are added to the solution. It is diazotized with a solution of 7 parts by weight of sodium nitrite (dissolved in three times the amount of water). The mixture temporarily turns green. From time to time a sample is checked for parapbenylenediamine by adding bichromate, which can be recognized by a green color. After about ₂ hours, paraphenylenediamine can no longer be detected in this way. The yellowish solution of the diazo body is then brought to a solution of parts by weight of alphanaphthol-alpha-monosulfonic acid and 120 parts by weight of calcined soda in 2,500 parts by weight of water. After 24 hours, the amidoazo dye is precipitated with table salt and as usual worked up. Pateντ claims: ι. Procedure for the representation of the ρ - amidobenzene - azo - alphanaphthol - alphamonosulfonic acid, consisting in the fact that one diazoacetanilide (the diazo compound of monacetylparaphenylenediamine) combined with alphanaphthol-alphamonosulfonic acid and then added the acetyl group is split off by treatment with alkalis or acids. 2. Process for the preparation of the amidoazo compound mentioned under 1. by combination of p-amidodiazobenzene (Griefs, Ber. XVII, p. 607) with alphanaphthol-alphamonosulfonic acid. ' 3. Process for the preparation of blue azo dyes, consisting in the fact that the ρ - amidobenzene - azoalphanapbtol-alphamonosulfonic acid mentioned under 1 diazotized and with alphanaphthol-alphamonosulfonic acid respectively. with betanaphtol-slphadisulfonic acid combined. 4. Process for the preparation of the blue azo dye obtainable by process 3., consisting in that the amidoazo dye can be obtained from p-amidodiazobenzene and betanaphthol-alphadisulfonic acid (Ber. XVIL, p. 608) diazotized and with alphanaphthol-alpha-monosulfonic acid combined.