DE426033C - Process for the production of diazotization preparations - Google Patents

Process for the production of diazotization preparations

Info

Publication number
DE426033C
DE426033C DEC35937D DEC0035937D DE426033C DE 426033 C DE426033 C DE 426033C DE C35937 D DEC35937 D DE C35937D DE C0035937 D DEC0035937 D DE C0035937D DE 426033 C DE426033 C DE 426033C
Authority
DE
Germany
Prior art keywords
preparations
sulfuric acid
diazotization
mixture
production
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
Application number
DEC35937D
Other languages
German (de)
Inventor
Dr Karl Schnilzspahn
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.)
JG Farbenindustrie AG
Original Assignee
JG Farbenindustrie 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 JG Farbenindustrie AG filed Critical JG Farbenindustrie AG
Priority to DEC35937D priority Critical patent/DE426033C/en
Application granted granted Critical
Publication of DE426033C publication Critical patent/DE426033C/en
Expired 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
    • C09BORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
    • C09B67/00Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
    • C09B67/0071Process features in the making of dyestuff preparations; Dehydrating agents; Dispersing agents; Dustfree compositions

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Air Bags (AREA)

Description

Verfahren zur Herstellung von Diazotierungspräparaten. Es wurde gefunden, daß aus p-Nitroanilin und aus anderen aromatischen Nitroaminoverhindungen, welche keine Sulfo- oder Carboxylgruppe enthalten. Präparate dargestellt werden können, die durch bloßes Einrühren in kaltes Wasser gebrauchsfertige Diazolösungen liefern. Das Verfahren besteht darin, daß die Nitroaminoverbindungen mit der zur Diazotierung genügenden Menge starker Schwefelsäure vermischt und wenn nötig erwärmt werden, so daß aus Nitrobase und Schwefelsäure Sulfatbildung erfolt und ein Teil der Schwefelsäure in freier' Form vorhanden bleibt. In der Regel genügen 3 Äquivalente Schwefelsäure auf i Mol. Nitroaminoverbindung. Anstatt der freien Nitrobase kann natürlich auch deren Sulfat oder saures Sulfat angewandt werden, ferner kann ein Teil der Schwefelsäure auch als Alkalibisulfat verwendet werden. Die so erhaltenen, in der Regel schon fast trocknen Mischungen von freier Schwefelsäure und Sulfat der Nitrobase werden alsdann durch Zumischung geeigneter trockner und Feuchtigkeit aufsaugender Verdünnungsmittel in trocken erscheinende Pulver übergeführt. Alsdann kann, obschon freie Schwefelsäure bzw. Bisulfat vorhanden ist, die zur späteren Dianotierung nötige ':Menge trocknes Nitrit ohne Entwicklung nitroser Gase und ohne daß in merklicher Menge Diazosalz gebildet wird, in das Gemisch eingerührt werden.Process for the production of diazotization preparations. It was found, that from p-nitroaniline and from other aromatic nitroamino compounds, which contain no sulfo or carboxyl group. Preparations can be displayed, which deliver ready-to-use diazo solutions by simply stirring them into cold water. The method consists in that the nitroamino compounds with the for diazotization sufficient amount of strong sulfuric acid mixed and, if necessary, heated, so that sulphate is formed from the nitro base and sulfuric acid and part of the sulfuric acid remains in free 'form. As a rule, 3 equivalents of sulfuric acid are sufficient on one mole of nitroamino compound. Instead of the free Nitrobase you can of course also use their sulfate or acid sulfate can be used, and part of the sulfuric acid can also be used as alkali bisulfate. Those obtained in this way, as a rule, already almost dry mixtures of free sulfuric acid and sulphate of the nitro base will be then by adding suitable dry and moisture-absorbing diluents converted into dry appearing powder. Then, although free sulfuric acid can be used or bisulfate is present, the amount necessary for later dianotation: quantity dry Nitrite without the development of nitrous gases and without any noticeable amount of diazo salt is formed, are stirred into the mixture.

Die beten Präparate werden erhalten,' wenn als indifferente Verdünnungsmittel einerseits teilentwässertes Aluminiumsulfat oder teilentwässerter Alaun, anderseits Arylsulfonate oder Mischungen von Arylsulfonaten mit teilentwässertem Alaun oder Aluminiumsulfat angewandt werden. Durch Verwendung solcher geeigneter Verdünnungsmittel werden Präparate erhalten, die nicht stark hygroskopisch sind und auch ein längeres Lagern bei 6o bis 65° C gut aushalten. Beispiel i. 69 Teile p-Nitroanilin werden in 79 Teile 94prozentige Schwefelsäure eingerührt. Nachderg die Sulfatbildung erfolgt ist, werden i5o Teile teilentwässertes Aluminiumsulfat von etwa 133 Prozent Reingehalt, bezogen auf Mo1.-Gew. 667, eingeknetet. Nach kurzer Zeit wird die Mischung staubtrocken. Alsdann werden 36 Teile trocknes Natriumnitrit zugesetzt und die Mischung gleichmäßig vermahlen. Wird i Teil dieses Präparates in 4 bis_ 5 Teile kaltes Wasser eingetragen, so erfolgt fast vollständige Dianotierung des p-Nitroanilins.The best preparations are obtained if, on the one hand, partially dehydrated aluminum sulfate or partially dehydrated alum, on the other hand aryl sulfonates or mixtures of aryl sulfonates with partially dehydrated alum or aluminum sulfate, are used as inert diluents. By using such suitable diluents, preparations are obtained which are not highly hygroscopic and which can also withstand prolonged storage at 60 to 65 ° C. Example i. 69 parts of p-nitroaniline are stirred into 79 parts of 94 percent sulfuric acid. After the sulfate formation has taken place, 150 parts of partially dehydrated aluminum sulfate with a purity of about 133 percent, based on Mo1.-wt. 667, kneaded in. After a short time, the mixture will be bone dry. Then 36 parts of dry sodium nitrite are added and the mixture is ground evenly. Is entered i part of this preparation in 4 to 5 parts _ cold water, so is almost complete Dianotierung of p-nitroaniline.

Beispiel e.Example e.

69 Teile p-Nitroanilin werden in 79 Teile 94prozentige Schwefelsäure eingerührt. Nachdem die Sulfatbildung erfolgt ist, werden 5o Teile teilentwässertes Aluminiumsulfat eingeknetet. Der alsbald trocken gewordenen Mischung werden sodann ioo Teile trocknes Gemisch von naphthalintri- und -tetrasulfosauretn Natrium, wie es durch Sulfierung von r Mol. 'Naphthalin mit 4. Mol. Schwefelsäureanhydrid erhältlich ist, zugemischt. Dieser Mischung werden alsdann 36 Teile Natriumnitrit zugegeben und das Ganze gleichmäßig vermahlen.69 parts of p-nitroaniline are converted into 79 parts of 94 percent sulfuric acid stirred in. After the sulphate has formed, 50 parts become partially dehydrated Kneaded in aluminum sulfate. The mixture, which has soon become dry, then becomes 100 parts dry mixture of naphthalenetri- and -tetrasulfosauretn sodium, such as it by sulphonation of r moles of naphthalene with 4. moles of sulfuric anhydride is available, admixed. 36 parts of sodium nitrite are then added to this mixture added and grind the whole thing evenly.

An Stelle von p-Nitroanilin können auch andere aromatische Nitroaminoverbindungen zur Verwendung kommen.Instead of p-nitroaniline, other aromatic nitroamino compounds can also be used come to use.

Claims (1)

PATENT-ANSPRUCH_ Verfahren zur Herstellung von Diazotierungspräparaten aus aromatischen diazotierbaren Nitroaminoverbindungen, welche keine Sulfo- oder Carboxylgruppe enthalten, darin bestehend, daß einer Mischung von z Mol. Nitrobase mit mehr als 2 Äquivalenten Schwefelsäure, wobei ein Teil der Schwefelsäure durch Bisulfat ersetzt sein kann und wobei an Stelle der Nitrobase auch deren neutrales oder saures Sulfat angewandt werden kann, zunächst geeignete Verdünnungsmittel zugefügt werden, und daß dieser Mischung alsdann trocknes Nitrit zugefügt wird.PATENT CLAIM_ Process for the production of diazotization preparations from aromatic diazotizable nitroamino compounds which do not contain sulfo or Carboxyl group, consisting in that a mixture of z moles. Nitrobase with more than 2 equivalents of sulfuric acid, with some of the sulfuric acid passing through Bisulfate can be replaced and where the nitro base is also neutral or acid sulphate can be used, first suitable diluents are added and that dry nitrite is then added to this mixture.
DEC35937D 1924-12-28 1924-12-28 Process for the production of diazotization preparations Expired DE426033C (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
DEC35937D DE426033C (en) 1924-12-28 1924-12-28 Process for the production of diazotization preparations

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DEC35937D DE426033C (en) 1924-12-28 1924-12-28 Process for the production of diazotization preparations

Publications (1)

Publication Number Publication Date
DE426033C true DE426033C (en) 1926-03-05

Family

ID=7022068

Family Applications (1)

Application Number Title Priority Date Filing Date
DEC35937D Expired DE426033C (en) 1924-12-28 1924-12-28 Process for the production of diazotization preparations

Country Status (1)

Country Link
DE (1) DE426033C (en)

Similar Documents

Publication Publication Date Title
DE426033C (en) Process for the production of diazotization preparations
DE2741925A1 (en) PROCESS FOR CONTINUOUS INDIRECT DIAZOTATION OF AROMATIC AMINES
DE716217C (en) Process for the production of phosphoric acid from rock phosphates
DE708305C (en) Dry mix of chemicals
DE593053C (en) Method of tanning
DE442075C (en) Durable diazotization preparations
DE727685C (en) Process for the production of concentrated diazolo solutions from solid diazonium chloride-chlorozinc double salts
EP0137243B1 (en) Process for the manufacture of acid nitro dyes
DE561715C (en) Process for the production of sulfuric acid compounds from oils and fats
DE692070C (en) Dispersants and protective agents
DE451784C (en) Process for the manufacture of products which absorb ultraviolet light
AT156159B (en) Process for the preparation of organic disulfides.
DE453985C (en) Durable diazotization preparations
DE624765C (en) Process for the production of azo dyes on the fiber
DE605577C (en) Process for the preparation of solid diazonium salts
DE964092C (en) Process for the production of long-lasting solutions of rhodanic acid and / or of acidic solutions of rhodanides which are suitable for disinfection purposes
DE587509C (en) Coloring preparations
DE677842C (en) Process for the production of potassium nitrate via the double salt KSO HNO
DE496833C (en) Process for improving the shelf life of diazo compounds in the presence of iron
AT345052B (en) BATHROOM ACCESSORY FOR CHROME ELECTRIC PLATING BATHS
DE586355C (en) Process for the preparation of diazo compounds in solid form
DE609476C (en) Process for the preparation of solid diazonium salts
DE3114768A1 (en) "IRON II TANNING AGENT AND METHOD FOR TANNING ANIMAL SKIN AND SKIN"
AT111541B (en) Process for the production of films, skins, tapes, capsules, hollow bodies and similar non-thread-like structures from viscose and similar aqueous cellulose solutions.
DE454460C (en) Process for the preparation of diarylmethane derivatives containing free amino groups