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DE696822C - Process for obtaining the proportions of polyhydric alcohols, in particular di- and polyglycerols, contained in the glycerol pitch - Google Patents

Process for obtaining the proportions of polyhydric alcohols, in particular di- and polyglycerols, contained in the glycerol pitch

Info

Publication number
DE696822C
DE696822C DE1937H0154187 DEH0154187D DE696822C DE 696822 C DE696822 C DE 696822C DE 1937H0154187 DE1937H0154187 DE 1937H0154187 DE H0154187 D DEH0154187 D DE H0154187D DE 696822 C DE696822 C DE 696822C
Authority
DE
Germany
Prior art keywords
polyglycerols
pitch
polyhydric alcohols
contained
proportions
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
DE1937H0154187
Other languages
German (de)
Inventor
Dr Anton Hintermaier
Dr Wilhelm Kapitel
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.)
Henkel AG and Co KGaA
Original Assignee
Henkel AG and Co KGaA
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 Henkel AG and Co KGaA filed Critical Henkel AG and Co KGaA
Priority to DE1937H0154187 priority Critical patent/DE696822C/en
Application granted granted Critical
Publication of DE696822C publication Critical patent/DE696822C/en
Expired legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D19/00Recovery of glycerol from a saponification liquor

Landscapes

  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Polyethers (AREA)

Description

Verfahren zur Gewinnung der im Glycerinpech enthaltenen Anteile an mehrwertigen Alkoholen, insbesondere an Di- und Polyglycerinen Es ist bekannt, daß man beider Destillation des nach den üblichen technischen Verfahren gewonnenen Rohglycerins als Rückstand eine zähe, klebrige, schwarzbraune Masse erhält, das Glycerinpech. Dieser Rückstand, der nur noch wenig freies Glycerin enthält, besteht im wesentlichen aus bei dem Destillationsvorgang gebildeten Di- und Polyglycerinen und Aschenbestandteilen des Rohglycerins sowie ferner aus Metallseifen, Eisenoxydhydraten und Verteerungsprodukten.Process for the extraction of the proportions contained in the glycerine pitch polyhydric alcohols, especially di- and polyglycerols. It is known that one during distillation of the crude glycerol obtained by the customary technical processes A tough, sticky, black-brown mass is obtained as residue, the glycerol pitch. This residue, which contains only a small amount of free glycerine, essentially consists from di- and polyglycerols and ash components formed during the distillation process of raw glycerine and also from metal soaps, iron oxide hydrates and taring products.

Weiter ist es bekannt, die im Glycerinpech enthaltenen mehrwertigen Alkohole, insbesondere Di- und- Polyglycerine, durch Behandlung des Glycerinpechs mit Wasser, Neutralisation der erhaltenen Lösungen mit Säuren oder sauren Salzen, Ausfällung der verunreinigenden Salze und Eindampfen zu gewinnen. Solche Produkte pflegen jedoch einen so hohen Aschegehalt aufzuweisen, daß sie für eine technische Verwertbarkeit nicht in Betracht kommen.It is also known that the polyvalent ones contained in the glycerol pitch Alcohols, especially di- and polyglycerols, by treating the glycerol pitch with water, neutralization of the solutions obtained with acids or acidic salts, Precipitation of the contaminating salts and evaporation to gain. Such products however, tend to have such a high ash content that they are considered to be technical Usability are out of the question.

Es wurde nun gefunden, daß man nahezu aschefreie mehrwertige Alkohole, insbesondere Di- und Polyglycerine, aus Glycerinpech gewinnen kann, wenn man die in bekannter Weise mit Säuren oder sauren Salzen neutralisierten wäßrigen Glycerinpechlösungen mit gro13ohcrfiächigcn oder aufsaugenden Stoffen, z. B. Sägespänen, Bleicherden oder liieselgur, versetzt, die erhaltenen Massen gegebenenfalls trocknet und mit geeigneten organischen Lösungsmitteln, z. B. Aceton, Essigester oder niedrigsiedenden Alkoholen, extrahiert und die Lösungsmittel verdampft. Hieran kann sich eine Entfärbung der Produkte durch Behandeln mit bekannten Entfärbungsmitteln oder durch oxydatve Bleichüng mit Wasserstoffperoxyd, Chlorkalk oder Kaliumpermanganat anschließen.It has now been found that almost ashless polyhydric alcohols, especially di- and polyglycerols, can be obtained from glycerol pitch if you use the Aqueous glycerol pitch solutions neutralized in a known manner with acids or acid salts with large-surface or absorbent materials, e.g. B. sawdust, bleaching earth or liieselgur, added, the resulting masses optionally dried and with suitable organic solvents, e.g. B. acetone, ethyl acetate or low-boiling Alcohols, extracted and the Solvent evaporates. Can discoloration of the products can be achieved by treating them with known decolorizing agents or by oxidative bleaching with hydrogen peroxide, chlorinated lime or potassium permanganate connect.

Die so erhaltenen Di- und Polyglycerine eignen sich als Appreturmittel in der Textilindustrie zur Herstellung von Kunstharzen und kosmetischen Präparaten sowie zur Weiterverarbeitung auf technisch wertvolle Ester.The di- and polyglycerols obtained in this way are suitable as finishing agents in the textile industry for the production of synthetic resins and cosmetic preparations as well as for further processing on technically valuable esters.

Es ist ztvar bekannt, Glycerin aus Brennereischlempen durch Verdicken derselben mit Cellulose; Trocknen der erhaltenen Massen und Extraktion derselben mit organischen Lösungsmitteln zu gewinnen.It is known ztvar to thicken glycerine from distillery liquor by thickening same with cellulose; Drying the masses obtained and extracting them to be obtained with organic solvents.

Jedoch war es auf Grund des Bekannten nicht vorauszusehen, daß sieh ein analoges Verfahren zur Gewinnung von technisch wertvollen Di- und Polyglycerinen aus dem bis in die neueste Zeit als technisch wertlos betrachteten Glycerinpech eignen würde.However, on the basis of what we knew, it could not be foreseen that see an analogous process for the production of technically valuable di- and polyglycerols from glycerine pitch, which until recently was regarded as technically worthless would suit.

Beispiel 5oo Gewichtsteile Glycerinpech werden in derselben Menge Wasser gelöst, worauf nach dem Aufkochen der Lösung filtriert wi;d. Das Filtrat wird dann mit 40 ccm einer 2oa/oigen Schwefelsäure neutralisiert. Die neutrale Lösung wird mit 212 Gewichtsteilen Sägespänen vermischt und die erhaltene Masse bei I8° bis zur Gewichtskonstanz getrocknet. Darauf wird erschöpfend mit Aceton extrahiert; worauf dieses zuerst bei gewöhnlichem und schließlich unter vermindertem Druck abdestilliert wird. Als Rückstand verbleibt eine aus etwas Glycerin und überwiegend Di- und Polyglycerinen bestehende viscose hellgelbe Flüssigkeit, die o,98 % Sulfatasche enthält.Example 500 parts by weight of glycerol pitch are used in the same amount Dissolved water, whereupon, after the solution has boiled, it is filtered; d. The filtrate is then neutralized with 40 cc of 20% sulfuric acid. The neutral solution is mixed with 212 parts by weight of sawdust and the resulting mass at 18 ° dried to constant weight. It is then exhaustively extracted with acetone; whereupon this is distilled off first under normal and finally under reduced pressure will. The residue that remains is made up of some glycerine and predominantly di- and polyglycerols existing viscous light yellow liquid containing 0.98% sulfated ash.

Claims (1)

PATLNTANSPRUCII: Verfahren zur Gewinnung der in Glycerinpech enthaltenen Anteile an mehrwertigen Alkoholen, insbesondere an Di-und Polyglycerinen, durch Behandlung des Glycerinpechs mit Wasser, Neutralisation der erhaltenen Lösungen mit Säuren oder sauren Salzen und Abtrennung der mehrwertigen Alkohole, dadurch gekennzeichnet; daß man die aus den neutralisierten Lösungen durch Zusatz von großoberflächigen oder aufsaugenden Stoffen und gegebenenfalls Entfernung des Wassers erhaltenen Massen mit geeigneten organischen Lösungsmitteln extrahiert und die Lösungsmittel verdampft.PATLNTANSPRUCII: Process for the extraction of the contained in glycerine pitch Shares of polyhydric alcohols, especially di- and polyglycerols, through Treatment of the glycerine pitch with water, neutralization of the solutions obtained with acids or acid salts and separation of the polyhydric alcohols, thereby marked; that you can get from the neutralized solutions by adding large surface areas or absorbent substances and optionally removal of the water obtained masses extracted with suitable organic solvents and evaporated the solvents.
DE1937H0154187 1937-12-31 1937-12-31 Process for obtaining the proportions of polyhydric alcohols, in particular di- and polyglycerols, contained in the glycerol pitch Expired DE696822C (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
DE1937H0154187 DE696822C (en) 1937-12-31 1937-12-31 Process for obtaining the proportions of polyhydric alcohols, in particular di- and polyglycerols, contained in the glycerol pitch

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DE1937H0154187 DE696822C (en) 1937-12-31 1937-12-31 Process for obtaining the proportions of polyhydric alcohols, in particular di- and polyglycerols, contained in the glycerol pitch

Publications (1)

Publication Number Publication Date
DE696822C true DE696822C (en) 1940-09-30

Family

ID=7181845

Family Applications (1)

Application Number Title Priority Date Filing Date
DE1937H0154187 Expired DE696822C (en) 1937-12-31 1937-12-31 Process for obtaining the proportions of polyhydric alcohols, in particular di- and polyglycerols, contained in the glycerol pitch

Country Status (1)

Country Link
DE (1) DE696822C (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2444296A (en) * 1943-04-24 1948-06-29 Colgate Palmolive Pect Company Recovery of glycerol
DE843876C (en) * 1949-06-14 1952-07-14 Wolf Ltd Victor Process for the production of polyglycerols from distillation residues

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2444296A (en) * 1943-04-24 1948-06-29 Colgate Palmolive Pect Company Recovery of glycerol
DE843876C (en) * 1949-06-14 1952-07-14 Wolf Ltd Victor Process for the production of polyglycerols from distillation residues

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