DE600981C - Process for the preparation of fibrous cellulose acetates - Google Patents

Process for the preparation of fibrous cellulose acetates

Info

Publication number
DE600981C
DE600981C DEB152345D DEB0152345D DE600981C DE 600981 C DE600981 C DE 600981C DE B152345 D DEB152345 D DE B152345D DE B0152345 D DEB0152345 D DE B0152345D DE 600981 C DE600981 C DE 600981C
Authority
DE
Germany
Prior art keywords
acid
preparation
fibrous cellulose
cellulose acetates
superchloric
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
DEB152345D
Other languages
German (de)
Inventor
Dr Richard Mueller
Dr Martin Schenck
Dr Wilhelm Wirbatz
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.)
Roche Diagnostics GmbH
Original Assignee
Boehringer Mannheim GmbH
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 Boehringer Mannheim GmbH filed Critical Boehringer Mannheim GmbH
Priority to DEB152345D priority Critical patent/DE600981C/en
Application granted granted Critical
Publication of DE600981C publication Critical patent/DE600981C/en
Expired legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08BPOLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B3/00Preparation of cellulose esters of organic acids
    • C08B3/20Esterification with maintenance of the fibrous structure of the cellulose

Landscapes

  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Biochemistry (AREA)
  • Materials Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Polysaccharides And Polysaccharide Derivatives (AREA)

Description

Verfahren zur Darstellung faserförmiger Celluloseacetate In dem Patent 6oo 979 wurde ein Verfahren zur Darstellung neuartiger faserförmiger Celluloseacetate beschrieben, . das darin besteht, daß man die Acetylierung von Cellulose, gegebenenfalls nach deren Vorbehandlung in bekannter Weise, in Gegenwart von ein Inlösunggehen der Acetylierungsprodukte verhindernden Stoffen mit Überchlorsäure als Katalysator bei gleichzeitiger Anwesenheit "von schwefliger Säure bei in allen Zonen des Reaktionssystems gleichmäßigen, etwa 4o° nicht übersteigenden Temperaturen vornimmt.Method for the preparation of fibrous cellulose acetates In the patent 6oo 979 a method for the preparation of novel fibrous cellulose acetates was described,. This consists in the acetylation of cellulose, if necessary after its pretreatment in a known manner, in the presence of substances preventing the acetylation products from dissolving with superchloric acid as a catalyst with the simultaneous presence of "sulfuric acid" with uniform, about 40 ° in all zones of the reaction system not exceeding temperatures.

In dem Zusatzpatent 6oo 98o wurde dann gezeigt, daß man zu Produkten im wesentlichen gleicher Eigenschaft gelangt, wenn man unter im übrigen analogen Reaktionsbedingungen die Überchlorsäure durch Salze der Überchlorsäure, vornehmlich solcher mit schwächeren Basen, ersetzt.In the additional patent 6oo 98o it was then shown that products essentially the same property is obtained if one under otherwise analogous Reaction conditions the superchloric acid by salts of the superchloric acid, mainly those with weaker bases, replaced.

Gegenstand vorliegender Erfindung ist die Durchführung des Verfahrens des Hauptpatents in Gegenwart von überchlorsauren Salzen bei gleichzeitiger Anwesenheit von Säuren an Stelle von Überchlorsäure. Säurezusatz begünstigt die katalytische Wirkung der überchlorsauren Salze und ermöglicht es insbesondere, auch Salze der Überchlorsäure mit starken Basen, wie Alkaliperchlorate, für die Acetylierung der Cellulose nach dem im Hauptpatent beschriebenen Verfahren zu verwenden.The subject of the present invention is the implementation of the method of the main patent in the presence of superchloric acid salts with simultaneous presence of acids instead of excess chloric acid. The addition of acid favors the catalytic Effect of the superchloric acid salts and makes it possible in particular to also use salts of the Hyperchloric acid with strong bases, such as alkali perchlorate, for the acetylation of the To use cellulose according to the method described in the main patent.

Beispiel ioo Teile Baumwollinters werden nach in bekannter Weise erfolgender Vorbehandlung mit Essigsäure unter guter Durchmischung mit einem aus 42o Teilen Essigsäureanhydrid (go- bis g2°1oig), 84o Teilen Benzol, 43o Teilen schwefliger Säure, 5 Teilen Natriumperchlorat und 4o Teile Chlorwasserstoffsäure bestehenden Gemisch acetyliert. Die Raktionstemperatur beträgt anfänglich io°, wird dann um 25° gehalten und gegen Ende der Acetylierung auf etwa 35 bis 38° gesteigert. Man erhält ein in Methylenchloridalkohol hochviscos lösliches, faserförmiges Cellulosetriacetat, das in üblicher Weise isoliert und gewaschen wird und dann frei von Chlorwasserstofsäure ist und die gleichen guten Eigenschaften besitzt wie die nach dem Patent 6oo 979 und dem Zusatzpatent 6oo 98o erhaltenen Produkte.EXAMPLE 100 parts of cotton lint are acetylated after pretreatment with acetic acid in a known manner with thorough mixing with a mixture consisting of 42o parts of acetic anhydride (up to g2 ° 10ig), 84o parts of benzene, 43o parts of sulphurous acid, 5 parts of sodium perchlorate and 40 parts of hydrochloric acid . The reaction temperature is initially 10 °, is then maintained around 25 ° and increased to about 35 to 38 ° towards the end of the acetylation. A fibrous cellulose triacetate which is highly viscous in methylene chloride alcohol is obtained, which is isolated and washed in the usual way and is then free from hydrochloric acid and has the same good properties as the products obtained according to the patent 6oo 979 and the additional patent 6oo 98o.

Claims (1)

PATENTANSPRUCH: Verfahren zur Darstellung faserförmiger Celluloseacetate gemäß Patent 6oo 979, dadurch gekennzeichnet, daß unter Innehaltung der übrigen, das Verfahren des Hauptpatents charakterisierenden Bedingungen an Stelle von überchlorsäure deren Salze in Gegenwart von Säuren als Katalysatoren verwandt werden.PATENT CLAIM: Process for the preparation of fibrous cellulose acetates according to patent 6oo 979, characterized in that with the rest of the conditions characterizing the process of the main patent instead of superchloric acid the salts of which are used as catalysts in the presence of acids.
DEB152345D 1931-10-02 1931-10-02 Process for the preparation of fibrous cellulose acetates Expired DE600981C (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
DEB152345D DE600981C (en) 1931-10-02 1931-10-02 Process for the preparation of fibrous cellulose acetates

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DEB152345D DE600981C (en) 1931-10-02 1931-10-02 Process for the preparation of fibrous cellulose acetates

Publications (1)

Publication Number Publication Date
DE600981C true DE600981C (en) 1934-08-06

Family

ID=7002622

Family Applications (1)

Application Number Title Priority Date Filing Date
DEB152345D Expired DE600981C (en) 1931-10-02 1931-10-02 Process for the preparation of fibrous cellulose acetates

Country Status (1)

Country Link
DE (1) DE600981C (en)

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