DE392130C - Process for the nitration of water-moist nitrocellulose - Google Patents

Process for the nitration of water-moist nitrocellulose

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Publication number
DE392130C
DE392130C DEB99318D DEB0099318D DE392130C DE 392130 C DE392130 C DE 392130C DE B99318 D DEB99318 D DE B99318D DE B0099318 D DEB0099318 D DE B0099318D DE 392130 C DE392130 C DE 392130C
Authority
DE
Germany
Prior art keywords
water
nitrocellulose
acid
nitration
moist
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
DEB99318D
Other languages
German (de)
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.)
ERNST BERL DR
Original Assignee
ERNST BERL DR
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 ERNST BERL DR filed Critical ERNST BERL DR
Priority to DEB99318D priority Critical patent/DE392130C/en
Application granted granted Critical
Publication of DE392130C publication Critical patent/DE392130C/en
Expired legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B5/00—Preparation of cellulose esters of inorganic acids, e.g. phosphates
    • C08B5/02—Cellulose nitrate, i.e. nitrocellulose

Description

Verfahren zur Umnitrierung wasserfeuchter Nitrozellulose. Es ist bekannt, daß man Nitrozellulose verschiedenster Qualität umnitrieren kann und je nach der Zusammensetzung der angewendeten Mischsäure den Stickstoffgehalt entweder zu erhöhen oder zu vermindern vermag. Es wurde gefunden, daß die Umnitrierung von wasserfeuchter Nitrozellulose irgendeiner Abstammung (Faserform oder gelatinierter Form) sich besonders einfach vollziehen läßt, wenn man das Wasser vorher durch Schwefelsäure (gegebenenfalls gekühlt), zweckmäßig solche von 6o bis 8o Prozent H.S04 Gehalt, oder mit verdünnten Mischsäuren (Abfallsäuren) verdrängt. Nach Abtrennung der überschüssigen Verdrängungssäure wird das nunmehr säurefeuchte Nitrozellulosematerial in Mischsäure geeigneter Konzentration und Temperatur eingetragen und der Umnitrierungsprozeß bis zur Erreichung der gewünschten Qualität durchgeführt.Process for the nitration of water-moist nitrocellulose. It is known, that you can nitrate nitrocellulose of various quality and depending on the Composition of the mixed acid used to either increase the nitrogen content or able to reduce it. It has been found that the nitriding of water moist Nitrocellulose of any origin (fiber form or gelatinized form) is particularly beneficial can be carried out easily if the water is previously treated with sulfuric acid (if necessary cooled), expediently those with 6o to 8o percent H.S04 content, or with diluted Mixed acids (waste acids) displaced. After separating off the excess displacement acid the now acid-moist nitrocellulose material is mixed acid in a suitable concentration and temperature entered and the nitriding process to achieve the desired Quality done.

Beispiel: Nitrozellulose mit 13,0 Prozent Stickstoff-und 35 Prozent Wassergehalt wird mit dem Mehrfachen ihres Gewichtes an 7o prozentiger Schwefelsäure durchgearbeitet, der Überschuß an Schwefelsäure abgetrennt und das nunmehr schwefelsäurefeuchte Material in Mischsäure von etwa 18 Prozent Wassergehalt und 19 Prozent Salpetersäuregehalt eingetragen. Nach kurzer Zeit ist die Umnitrierung beendet und ein in Ätheralkohol völlig lösliches Produkt' entstanden.Example: Nitrocellulose with 13.0 percent nitrogen and 35 percent water content is worked through with several times its weight in 70 percent sulfuric acid, the excess sulfuric acid is separated off and the now sulfuric acid-moist material is added to mixed acid with about 18 percent water content and 19 percent nitric acid content. After a short time, the nitration is complete and a product that is completely soluble in ether alcohol has been created.

Die angegebene Behandlung mit Schwefelsäure von 6o bis 8o Prozenten ergibt keinerlei wesentliche Veränderung des Nitrozellulosematerials. Sie bedingt eine weitgehende Entwässerung der wasserfeuchten Nitrozellulose, so daß die angewendeten Mischsäuren in ihrer Konzentration: nur unwesentlich geändert werden. Überdies ist die Wärmetönung beim Zusammentreffen der schwefelsäurefeuchten Nitrozellulose mit Mischsäure verhältnismäßig gering, so daß Brände und verstärkter Abbau der Nitrozellulose vermieden werden.The specified treatment with sulfuric acid from 6o to 8o percent does not result in any significant change in the nitrocellulose material. You conditionally extensive drainage of the water-moist nitrocellulose, so that the applied Mixed acids in their concentration: can only be changed insignificantly. Moreover is the warmth when the sulfuric acid-moist nitrocellulose meets Mixed acid relatively low, so that fires and increased breakdown of the nitrocellulose be avoided.

Das Patent 46125 von Chardonnet führt mit Hilfe von verdünnter Salpetersäure so weitgehende Denitrierung der angewandten Zellulosenitrate durch, daß diese in Ätheralkohol und in Azeton völlig unlöslich werden. Bei der angegebenen Arbeitsweise tritt indes eine so tiefgehende Änderung, welche zur Vernichtung aller Löslichkeitseigenschaften führt, nicht auf.The Chardonnet patent 46125 leads using dilute nitric acid so extensive denitration of the applied cellulose nitrates by that these in Ether alcohol and become completely insoluble in acetone. With the specified working method however, such a profound change occurs which destroys all solubility properties leads, not on.

Claims (1)

PATENTANSPRUCH Verfahren zur Umnitrierung wasserfeuchter Nitrozellulosr, dadurch gekennzeichnet, daß diese vor der Behandlung mit Mischsäure, mit gegebenenfalls gekühlter Schwefelsäure oder verdünnter Mischsäure (Abfallmischsäure) behandelt wird. PATENT CLAIM Process for re-nitriding water-moist nitrocellulose, characterized in that it is treated with mixed acid, with optionally cooled sulfuric acid or dilute mixed acid (mixed waste acid) before the treatment.
DEB99318D 1921-04-10 1921-04-10 Process for the nitration of water-moist nitrocellulose Expired DE392130C (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
DEB99318D DE392130C (en) 1921-04-10 1921-04-10 Process for the nitration of water-moist nitrocellulose

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DEB99318D DE392130C (en) 1921-04-10 1921-04-10 Process for the nitration of water-moist nitrocellulose

Publications (1)

Publication Number Publication Date
DE392130C true DE392130C (en) 1924-03-17

Family

ID=6989594

Family Applications (1)

Application Number Title Priority Date Filing Date
DEB99318D Expired DE392130C (en) 1921-04-10 1921-04-10 Process for the nitration of water-moist nitrocellulose

Country Status (1)

Country Link
DE (1) DE392130C (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1994006853A1 (en) * 1992-09-14 1994-03-31 Eilenburger Chemie Werke Aktiengesellschaft Process for isolating cellulose nitrate from non-graphited monobasic propellant powders

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1994006853A1 (en) * 1992-09-14 1994-03-31 Eilenburger Chemie Werke Aktiengesellschaft Process for isolating cellulose nitrate from non-graphited monobasic propellant powders

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