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 pitchInfo
- 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
Links
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 title claims description 40
- 229920000223 polyglycerol Polymers 0.000 title claims description 9
- 238000000034 method Methods 0.000 title claims description 5
- 150000005846 sugar alcohols Polymers 0.000 title claims description 5
- 235000011187 glycerol Nutrition 0.000 claims description 15
- 239000002253 acid Substances 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 150000007513 acids Chemical class 0.000 claims description 3
- 239000003960 organic solvent Substances 0.000 claims description 3
- 150000003839 salts Chemical class 0.000 claims description 3
- 230000002745 absorbent Effects 0.000 claims description 2
- 239000002250 absorbent Substances 0.000 claims description 2
- 238000000605 extraction Methods 0.000 claims description 2
- 238000006386 neutralization reaction Methods 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims 1
- 239000000126 substance Substances 0.000 claims 1
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 150000001298 alcohols Chemical class 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- 150000008043 acidic salts Chemical class 0.000 description 1
- 238000004061 bleaching Methods 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- UBUHAZKODAUXCP-UHFFFAOYSA-N iron(2+);oxygen(2-);hydrate Chemical class O.[O-2].[Fe+2] UBUHAZKODAUXCP-UHFFFAOYSA-N 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 238000009896 oxidative bleaching Methods 0.000 description 1
- 239000012286 potassium permanganate Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D19/00—Recovery 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)
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)
| 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 |
-
1937
- 1937-12-31 DE DE1937H0154187 patent/DE696822C/en not_active Expired
Cited By (2)
| 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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