DE731794C - Process for the production of alkali salts of cellulose ether carboxylic acids which, with water, result in solutions of increased viscosity - Google Patents

Process for the production of alkali salts of cellulose ether carboxylic acids which, with water, result in solutions of increased viscosity

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Publication number
DE731794C
DE731794C DES126244D DES0126244D DE731794C DE 731794 C DE731794 C DE 731794C DE S126244 D DES126244 D DE S126244D DE S0126244 D DES0126244 D DE S0126244D DE 731794 C DE731794 C DE 731794C
Authority
DE
Germany
Prior art keywords
water
solutions
carboxylic acids
cellulose ether
result
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
DES126244D
Other languages
German (de)
Inventor
Dr Phil Georg Meyer
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.)
Ferdinand Sichel A G
Original Assignee
Ferdinand Sichel A G
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 Ferdinand Sichel A G filed Critical Ferdinand Sichel A G
Priority to DES126244D priority Critical patent/DE731794C/en
Application granted granted Critical
Publication of DE731794C publication Critical patent/DE731794C/en
Expired legal-status Critical Current

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Classifications

    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08BPOLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B11/00Preparation of cellulose ethers
    • C08B11/02Alkyl or cycloalkyl ethers
    • C08B11/04Alkyl or cycloalkyl ethers with substituted hydrocarbon radicals
    • C08B11/10Alkyl or cycloalkyl ethers with substituted hydrocarbon radicals substituted with acid radicals
    • C08B11/12Alkyl or cycloalkyl ethers with substituted hydrocarbon radicals substituted with acid radicals substituted with carboxylic radicals, e.g. carboxymethylcellulose [CMC]
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J25/00Transit-time tubes, e.g. klystrons, travelling-wave tubes, magnetrons
    • H01J25/50Magnetrons, i.e. tubes with a magnet system producing an H-field crossing the E-field
    • H01J25/52Magnetrons, i.e. tubes with a magnet system producing an H-field crossing the E-field with an electron space having a shape that does not prevent any electron from moving completely around the cathode or guide electrode
    • H01J25/54Magnetrons, i.e. tubes with a magnet system producing an H-field crossing the E-field with an electron space having a shape that does not prevent any electron from moving completely around the cathode or guide electrode having only one cavity or other resonator, e.g. neutrode tubes

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  • 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)
  • Adhesives Or Adhesive Processes (AREA)

Description

Verfahren zur Herstellung von Alkalisalzen der Celluloseäthercarbonsäuren, die mit Wasser Lösungen von erhöhter Viskosität ergeben Die wasserlöslichen Salze der Cclluloseätliercarbonsäuren werden bekanntlich als Klebemittel verwendet. Diese Celluloscätherverbindungen werden dadurch hergestellt, daßman Halogenfettsäuren auf Cellulose, Cellulosedcrivate oder cellulosehaltige Stolte bei Gegenwart von Alkali einwirken läßt. Obwohl die freien Säuren in Wasserunlöslich sind Iäßt sich die Reinigung -des Reaktionsproduktes durch Zug< be von wäßrigen Lösungen,. wie Säuren, sauren Salzen u.:däl., praktisch nicht durchführen. da die so entstehenden kolloidalen Carbonsäuren infolge ihrer schleiteigen Beschaffenheit sich nur äußerst schwierig filtrieren und nicht auswaschen lassen. 11an reinigt daher durch Ausfallen und Extraktion mit Alkohol und ,erhält durch ächfolgende Trocknung das wasserlösliche ,\lkalisalz des C'cllulose@ithcrs als Pulver. Trotzdem gelingt: es nicht, dieses in der Praxis frei von anorganischen Salzen herzustellen. da sowohl Natriumchlorid als auch Natriumhydroxyd; die in dem Reaktionsgemisch in großer Menge vorhanden sind, in Alkohol sich verhältnismäßig schwer lösen.Process for the production of alkali salts of cellulose ether carboxylic acids, which result in solutions of increased viscosity with water The water-soluble salts The Cclluloseätliercarbonsäuren are known to be used as adhesives. These Cellulose ether compounds are prepared by using halogen fatty acids on cellulose, cellulose derivatives or cellulose-containing substances in the presence of Let the alkali take effect. Although the free acids are insoluble in water the purification of the reaction product by pulling aqueous solutions. how Acids, acidic salts, etc., practically do not carry out. because the resulting colloidal carboxylic acids, because of their poor quality, are extremely different Difficult to filter and do not wash out. 11an therefore cleanses by failure and extraction with alcohol and, by subsequent drying, the water-soluble one is obtained , \ lkalisalz des C'cllulose @ ithcrs as a powder. Nevertheless, it succeeds: it does not, this one in practice to be produced free of inorganic salts. as both sodium chloride as well as sodium hydroxide; which are present in the reaction mixture in a large amount are relatively difficult to dissolve in alcohol.

Das _llkalisalz löst sich in kaltem Wasser zu einer viskosen klebrigen Masse. Die Beschaffenheit der wäßrigen Lösung ist abhänbig von der Zahl der an das Cellulosemolekül angelagerten Carboxylgruppen. Je-viskoser die Lösung ist, um so ausgiebiger und wirtschaftlicher ist ihre Verwendung..The _llkalisalz dissolves in cold water to form a viscous sticky Dimensions. The nature of the aqueous solution depends on the number of the Carboxyl groups attached to cellulose molecule. The more viscous the solution, the more so their use is more extensive and economical ..

Es wurde nun überraschenderweise gefunden, daß man Salze der Celluloscäthercarbonsäurcn erhält. die -,väfirige Lösungen von sehr viel höherer Viskosität ergeben, wenn .man das durch 1:inwirken von Monohalogenfcttsätiren <auf All;alicelltilose entstandene; heaktiGnsprodukt in bekannter Weise mit' _\luininiimverliiidunneii, wie :Alaun oder Aluininitimacetat, ausfällt, durch Waschen mit Wasser von den Salzen befreit und sodann durch Zugabe äquivalenter Mengen Alkali (bezogen--.auf Aluminium) in den wasserlöslichen Zustand überführt. It has now surprisingly been found that salts of cellulose ether carboxylic acids are obtained. which give vicious solutions of very much higher viscosity if the alicellilose produced by the action of monohalogen functions on all; Heat product in a known way with '_ \ luininiimverliiidunneii, such as: alum or Aluininitimacetat, precipitates, freed from the salts by washing with water and then converted into the water-soluble state by adding equivalent amounts of alkali (based on aluminum).

Die wasserunlöslichen Aluminiumverbindungen fallen dabei, im Gegensatz zu den mit anderen bekannten Fällungsmitteln, wie Säuren oder sauren Salzen, ausgefällten freien Säuren in einer Form aus, die sich äußerst leicht und bequem filtrieren und vollkommen salzfrei auswaschen läßt. Durch Zusatz der Alkalien in wäßriger Lösung erhält man eine gebrauchsfertige Leimlösung.The water-insoluble aluminum compounds fall, in contrast to those precipitated with other known precipitants, such as acids or acid salts free acids in a form that is extremely easy and convenient to filter and Can be washed out completely salt-free. By adding the alkalis in aqueous solution a ready-to-use glue solution is obtained.

Abgesehen davon also, daß man auf diese Weise das teure Extraktionsverfahren mittels Alkohol, das zudem feuergefährlich ist, umgehen kann, gerinnt man erfindungsgemäß, ohne 'trocknen zu müssen, gebrauchsfertige salzfreie Klebstofflösungeii @dieser-wässerlöslichen Celluloseäther. Selbstverständlich kann man die erfindungsgemäß gewonnenen Produkte in bekannter Weise trocknen und als Pulver in den Verkehr bringen. Dieses Pulver kann dann vom Verbraucher durch einfaches Eintragen in kaltes Wasser verwendungsfähig gemacht werden.Apart from the fact that you do the expensive extraction process in this way can handle alcohol, which is also flammable, one coagulates according to the invention, without having to dry, ready-to-use, salt-free adhesive solution that is water-soluble Cellulose ether. Of course, the products obtained according to the invention can be used Dry in the known manner and market as a powder. This powder can then be used by the consumer simply by adding it to cold water be made.

Die kollöiden Lösungen der nach der Erfindung hergestellten Cellulosederivate eignen sich infolge ihrer erhöhten Viskosität besonders gut als Klebstoffe, zum Kleben von Papier, Tapeten- u. dgl., als Buchbinderkleister, als Appretur- und Schlichtemittel sowie als Farbenbindemittel. ' ' Anwendung sbeisp iel iookg ungebleichter Zellstoff «erden mit i.lo kg Monochloressigsäure bei Gegenwart von Alkali in bekannter Weise veräthert. Die feuchte `'lasse wird mit Wasser verdünnt und mit ioo'oiger Alaunlösung bis zur vollkoinmenen Ausfällung versetzt. Die ausgefällte Aluminiumverbindung wird mehrmals mit Wasser gewaschen und filtriert: Der Nieder. schlag wird sodann miC so viel 3o'1biger Natronlauge verknetet, bis er eben schwach alkalisch reagiert, und durch Verdünnen mit Wasser auf eine Konzentration von etwa 4011o gebracht. Es ergibt sich. ein hochviskoser, stark klebender Kleister.The colloidal solutions of the cellulose derivatives produced according to the invention are particularly suitable as adhesives due to their increased viscosity Gluing paper, wallpaper and the like, as bookbinding paste, as a finishing and sizing agent as well as a paint binder. '' Use for example in unbleached cellulose pulp «Ground with 10 kg of monochloroacetic acid in the presence of alkali in a known manner etherified. The wet lass is diluted with water and with 100% alum solution up to the complete precipitation. The precipitated aluminum compound will washed several times with water and filtered: The lower. impact then becomes miC knead as much sodium hydroxide solution as needed until it has a weakly alkaline reaction, and brought to a concentration of about 4011o by diluting with water. It surrendered. a highly viscous, strongly adhesive paste.

Claims (1)

PATENT ANSPIZUCÜ: Verfahren zur Herstellung von Alkalisalzen der Celluloseäthercarbonsäuren, die mit Wasser Lösungen von erhöhter Viskosität ergeben, dadurch gekennzeichnet, daß man das durch Einwirken' von Monohalogenfettsäuren auf Alkalicellulose entstandene -Reaktionsprodukt mit . Aluminiumverbindtmgen. wie Alaun oder Aluniiniumacetat, ausfällt, durch Waschen mit Wasser .von den Salzen befreit und durch Zugabe äquivalenter Mengen Alkali (bezogen auf Aluminium) in den wasserlöslichen Zustand überführt. PATENT ANSPIZUCÜ: Process for the preparation of alkali salts of cellulose ether carboxylic acids which result in solutions of increased viscosity with water, characterized in that the reaction product formed by the action of monohalo-fatty acids on alkali cellulose is mixed with. Aluminum connections. such as alum or aluminum acetate, precipitates, freed from the salts by washing with water and converted into the water-soluble state by adding equivalent amounts of alkali (based on aluminum).
DES126244D 1937-03-02 1937-03-02 Process for the production of alkali salts of cellulose ether carboxylic acids which, with water, result in solutions of increased viscosity Expired DE731794C (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
DES126244D DE731794C (en) 1937-03-02 1937-03-02 Process for the production of alkali salts of cellulose ether carboxylic acids which, with water, result in solutions of increased viscosity

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DES126244D DE731794C (en) 1937-03-02 1937-03-02 Process for the production of alkali salts of cellulose ether carboxylic acids which, with water, result in solutions of increased viscosity

Publications (1)

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DE731794C true DE731794C (en) 1943-02-16

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE923078C (en) * 1948-10-02 1955-02-03 Kalle & Co Ag Process for the production of a paint containing calcium hydroxide using cellulose ethers as binders

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE923078C (en) * 1948-10-02 1955-02-03 Kalle & Co Ag Process for the production of a paint containing calcium hydroxide using cellulose ethers as binders

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