DE600980C - Process for the preparation of fibrous cellulose acetates - Google Patents

Process for the preparation of fibrous cellulose acetates

Info

Publication number
DE600980C
DE600980C DEB150790D DEB0150790D DE600980C DE 600980 C DE600980 C DE 600980C DE B150790 D DEB150790 D DE B150790D DE B0150790 D DEB0150790 D DE B0150790D DE 600980 C DE600980 C DE 600980C
Authority
DE
Germany
Prior art keywords
preparation
fibrous cellulose
cellulose acetates
acid
parts
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
DEB150790D
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 DEB150790D priority Critical patent/DE600980C/en
Application granted granted Critical
Publication of DE600980C publication Critical patent/DE600980C/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
    • C08B3/00—Preparation of cellulose esters of organic acids
    • C08B3/20—Esterification 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 q.0° nicht übersteigenden Temperaturen vornimmt.Method of Preparing Fibrous Cellulose Acetates In the patent 6oo 979 was a process for the preparation of novel fibrous cellulose acetates described, which consists in the acetylation of cellulose, optionally after their pretreatment in a known manner, in the presence of dissolving substances that prevent acetylation products with overchloric acid as a catalyst with the simultaneous presence of sulphurous acid in all zones of the reaction system uniform temperatures not exceeding q.0 °.

Im Verlauf der weiteren Versuche wurde nun gefunden, daß man zu Produkten im wesentlichen gleicher Eigenschaften gelangt, wenn man unter im übrigen analogen Reaktionsbedingungen die Überchlorsäure durch Salze der Überchlorsäure mit einer schwächeren Base, wie Magnesiumperchlorat, Zinkperchlorat o. dgl., ersetzt.In the course of further experiments it has now been found that products essentially the same properties are obtained if one under otherwise analogous Reaction conditions the superchloric acid by salts of the superchloric acid with a weaker base, such as magnesium perchlorate, zinc perchlorate or the like., replaced.

Beispiel i oo Teile Baumwoll-Linters ; mit i, 6 Wassergehalt werden in iooo Teile Eisessig eingetragen, worauf nach q. Stunden abgeschleudert wird. Die so vorbehandelte Cellulose wird dann mittels eines aus q.2o Teilen 9i°/oigen Essigsäureanhydrids, 6oo Teilen Toluo:l, 30o Teilen schwefliger Säure und 3 Teilen Zinkperchlorat bestehenden Gemischs acetyliert. Während der unter ,kräftiger Durchmischung vor sich gehenden Reaktion steigt die Temperatur auf etwa 25'; bei dieser Temperatur wird die Reaktion auch zu Ende geführt. Nach 8'/2 Stunden wird abgeschleudert und das Acetylierungsprodukt gewaschen und getrocknet. ., Es wird von Aceton und kaltem Eisessig nicht gelöst und besitzt, zu 6 g in ioo ccm eines Gemischs von Methylenchlorid und Alkohol vom Volumenverhältnis 9 : i gelöst, bei 25° eine Viskosität von 375 Sekunden, bestimmt im Ostschen Viskosimeter mit einem Glycerinwert von 153. Aus ihm hergestellte Filme von o,i mm Dicke zeigen im Schopperschen Zerreißapparat eine Reißzahl von etwa igkg und eine Dehnung von etwa i8°ja. Ihre Knickzahl liegt bei Zoo.Example 100 parts cotton linters; with 1.6 water content are added to 1000 parts of glacial acetic acid, whereupon after q. Hours is thrown off. The cellulose pretreated in this way is then acetylated by means of a mixture consisting of q20 parts of 90% acetic anhydride, 600 parts of toluene: 1.30 parts of sulfurous acid and 3 parts of zinc perchlorate. During the reaction, which is taking place with vigorous mixing, the temperature rises to about 25 '; the reaction is also completed at this temperature. After 8 1/2 hours it is spun off and the acetylation product is washed and dried. ., It is not dissolved by acetone and cold glacial acetic acid and, 6 g in 100 ccm of a mixture of methylene chloride and alcohol with a volume ratio of 9: i dissolved, has a viscosity of 375 seconds at 25 °, determined in the Ost's viscometer with a glycerol value of 153. Films produced from it with a thickness of 0.1 mm show a tearing number of about igkg and an elongation of about 18 ° yes in the Schopper tearing apparatus. Your buckling number is at Zoo.

Claims (1)

PATENTANSPRUCH: Verfahren zur Darstellung faserförmiger Celluloseacetate gemäß Patent 6oo979, dadurch gekennzeichnet, daß unter Innehaltung der übrigen das Verfahren des Hauptpatents charakterisierenden Bedingungen an Stelle von Überchlorsäure deren Salze mit einer schwächeren Base als Katalysatoren verwandt werden. PATENT CLAIM: Process for the preparation of fibrous cellulose acetates according to patent 6oo979, characterized in that, while maintaining the other conditions characterizing the process of the main patent, the salts thereof with a weaker base are used as catalysts instead of superchloric acid.
DEB150790D 1931-06-30 1931-06-30 Process for the preparation of fibrous cellulose acetates Expired DE600980C (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
DEB150790D DE600980C (en) 1931-06-30 1931-06-30 Process for the preparation of fibrous cellulose acetates

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DEB150790D DE600980C (en) 1931-06-30 1931-06-30 Process for the preparation of fibrous cellulose acetates

Publications (1)

Publication Number Publication Date
DE600980C true DE600980C (en) 1934-08-06

Family

ID=7002282

Family Applications (1)

Application Number Title Priority Date Filing Date
DEB150790D Expired DE600980C (en) 1931-06-30 1931-06-30 Process for the preparation of fibrous cellulose acetates

Country Status (1)

Country Link
DE (1) DE600980C (en)

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