DE36827C - Production of acetone-free methyl alcohol from raw wood spirit - Google Patents
Production of acetone-free methyl alcohol from raw wood spiritInfo
- Publication number
- DE36827C DE36827C DENDAT36827D DE36827DA DE36827C DE 36827 C DE36827 C DE 36827C DE NDAT36827 D DENDAT36827 D DE NDAT36827D DE 36827D A DE36827D A DE 36827DA DE 36827 C DE36827 C DE 36827C
- Authority
- DE
- Germany
- Prior art keywords
- methyl alcohol
- acetone
- production
- raw wood
- free methyl
- 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 - Lifetime
Links
- OKKJLVBELUTLKV-UHFFFAOYSA-N methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 title claims description 49
- 238000004519 manufacturing process Methods 0.000 title claims 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 34
- 239000000460 chlorine Substances 0.000 claims description 6
- 229910052801 chlorine Inorganic materials 0.000 claims description 6
- 238000009835 boiling Methods 0.000 claims description 4
- KZBUYRJDOAKODT-UHFFFAOYSA-N chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 claims description 3
- 125000001309 chloro group Chemical group Cl* 0.000 claims description 2
- 238000006467 substitution reaction Methods 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims 1
- MUBZPKHOEPUJKR-UHFFFAOYSA-N oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 6
- 238000004821 distillation Methods 0.000 description 5
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 4
- 235000015450 Tilia cordata Nutrition 0.000 description 4
- 235000011941 Tilia x europaea Nutrition 0.000 description 4
- ZAMOUSCENKQFHK-UHFFFAOYSA-N chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 4
- 239000004571 lime Substances 0.000 description 4
- BULLHNJGPPOUOX-UHFFFAOYSA-N Chloroacetone Chemical compound CC(=O)CCl BULLHNJGPPOUOX-UHFFFAOYSA-N 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- UXVMQQNJUSDDNG-UHFFFAOYSA-L cacl2 Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 2
- 239000001110 calcium chloride Substances 0.000 description 2
- 229910001628 calcium chloride Inorganic materials 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 235000006408 oxalic acid Nutrition 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- CSVFWMMPUJDVKH-UHFFFAOYSA-N 1,1-dichloropropan-2-one Chemical compound CC(=O)C(Cl)Cl CSVFWMMPUJDVKH-UHFFFAOYSA-N 0.000 description 1
- OKJPEAGHQZHRQV-UHFFFAOYSA-N Iodoform Chemical compound IC(I)I OKJPEAGHQZHRQV-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- LCGLNKUTAGEVQW-UHFFFAOYSA-N dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000004508 fractional distillation Methods 0.000 description 1
- 230000000977 initiatory Effects 0.000 description 1
- 229960003172 iodoform Drugs 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C31/00—Saturated compounds having hydroxy or O-metal groups bound to acyclic carbon atoms
- C07C31/02—Monohydroxylic acyclic alcohols
- C07C31/04—Methanol
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Description
KAISERLICHESIMPERIAL
PATENTAMTPATENT OFFICE
Die bisherige Methode, einen acetonfreien Methylalkohol herzustellen, besteht darin, dafs. man aus dem zum Theil gereinigten, rohen Methylalkohol, der hauptsächlich noch Aceton enthält, durch Mischen mit Chlorcalcium eine krystallmische Verbindung abscheidet, die dann durch Trocknen von Aceton befreit und durch Destillation mit Wasser wieder zersetzt wird, was einen reinen, wässerigen Methylalkohol ergiebt, der durch weitere Behandlung auf Colonnenapparaten bezw. Destillation über Kalk wasserfrei gewonnen wird. In ganz reinem Zustande erhält man auch den Methylalkohol durch Zersetzen des Oxalsäuremethyläthers mit Kalilauge. Endlich kann man durch Destillation des rohen Holzgeistes über Kalk, Reinigung mit Kaliumhypermanganat, Schwefelsäure und Natronlauge, sowie Destillation auf Colonnenapparaten ebenfalls einen fast reinen Methylalkohol herstellen, welcher fast nur noch Aceton als Verunreinigung enthält. Die ersten beiden Methoden sind äufserst kostspielig, da die ganze Menge des Methylalkohols in die Verbindung mit Chlorcalcium bezw. mit Oxalsäure überzuführen und nachher wieder zu zersetzen ist, während bei der letztgenannten Methode, selbst bei sorgfältigster Arbeit, der Acetongehalt nur bis auf 0,4 pCt. herunterzubringen ist, was dem Verkaufsproduct noch immer einen Minderwerth verleiht.The previous method of preparing an acetone-free methyl alcohol consists in that. from the partly purified, crude methyl alcohol, which is mainly acetone contains, by mixing with calcium chloride separates a crystalline compound, which then freed from acetone by drying and decomposed again by distillation with water, which gives a pure, watery methyl alcohol, which on further treatment gives up Column apparatus respectively. Anhydrous distillation over lime is obtained. In whole In a pure state, methyl alcohol is also obtained by decomposing the oxalic acid methyl ether with potassium hydroxide. Finally, by distilling the raw wood spirit over lime, Cleaning with potassium hypermanganate, sulfuric acid and sodium hydroxide solution, as well as distillation Column apparatus also produce an almost pure methyl alcohol, which is almost exclusively Contains acetone as an impurity. The first two methods are extremely costly since the whole amount of methyl alcohol in connection with calcium chloride respectively. with oxalic acid is to be transferred and then decomposed again, while with the latter Method, even with the most careful work, the acetone content only down to 0.4 pCt. bring down is what still gives the product of sale an inferiority.
Die vorliegende Erfindung bezieht sich auf ein Verfahren, durch welches der Acetongehalt des Methylalkohols vollständig entfernt wird, und besteht im wesentlichen darin, dafs in gereinigten und noch acetonhaltigen oder auch ganz rohen Methylalkohol unter Erwärmung Chlorgas eingeleitet wird. Der Holzgeist wird zu diesem Zwecke am besten von den anhaftenden Säuren durch Destillation mit Kalk befreit und auf dem Colonnenapparat der Gehalt an Aceton auf ein geringes Mafs (etwa 1 bis 2 pCt.) herabgebracht. Der so erhaltene acetonhaltige Methylalkohol wird mit trockenem Chiorgas behandelt. Dieses geschieht am besten unter Erwärmen des acetonhaltigen Methylalkohols bis auf die Siedetemperatur in einem passenden Gefäfs mit Rückflusskühler, in welches sodann trockenes Chlorgas eingeleitet wird. Dasselbe zersetzt nicht den Methylalkohol, sondern nur das Aceton und bildet aus diesem das Mono- und Dichloraceton, Verbindungen, die bei einer viel höheren Temperatur als der Methylalkohol, 119 und 120°, sieden. Von Zeit zu Zeit wird eine Probe der Flüssigkeit genommen, von den gebildeten Chloracetonen abdestillirt und das Destillat nach bekannter Methode auf Aceton untersucht. Sobald kein Niederschlag von Jodoform mehr entsteht, wird mit dem Einleiten von Chlor aufgehört. Der Methylalkohol wird sodann durch fractionirte Destillation von den. gebildeten schwer siedenden Chlorsubstitutionsproducten des Acetone getrennt und durch Destillation über Kalk von den letzten Resten von anhängendem Chlor gereinigt.The present invention relates to a method by which the acetone content of the methyl alcohol is completely removed, and consists essentially in the fact that in purified and still acetone or even completely crude methyl alcohol is introduced with heating chlorine gas. The wood spirit will for this purpose it is best to remove the adhering acids by distillation with lime freed and the acetone content on the column apparatus to a low level (approx to 2 pct.). The so obtained acetone-containing methyl alcohol is with dry Chiorgas treated. This is best done by heating the methyl alcohol containing acetone up to the boiling point in a suitable vessel with reflux condenser, in which then dry chlorine gas is introduced. The same does not decompose the methyl alcohol, but only the acetone and from this forms the mono- and dichloroacetone, compounds, which at a much higher temperature than the methyl alcohol, 119 and 120 °, boil. From time to time a sample of the liquid is taken from the formed Chloracetones are distilled off and the distillate is examined for acetone by a known method. As soon as there is no longer any precipitate of iodoform, the introduction of chlorine is stopped. The methyl alcohol will then by fractional distillation of the. low-boiling chlorine substitution products formed of the acetone separated and purified from the last residues of adhering chlorine by distillation over lime.
Auf diese Weise gelingt es, einen völlig acetonfreien Methylalkohol herzustellen; das gewonnene Chloraceton kann durch geeignete Zersetzung wieder in Aceton verwandelt werden. Dieses Verfahren der Chloreinleitung kann auch bei rohem Holzgeist angewendet werden, nur ist dann längeres Einleiten erforderlich;In this way it is possible to produce a completely acetone-free methyl alcohol; the Any chloroacetone obtained can be converted back into acetone by suitable decomposition. This method of introducing chlorine can also be used with raw wood spirit, only then longer initiation is necessary;
es werden dann aber zugleich andere Verunreinigungen durch das Chlor mitzerstört und ist die Reinigung des Holzgeistes eine leichtere. Der Vortheil bei diesem Verfahren besteht darin, dafs nicht die ganze Masse des Methylalkohols (98 bis 99 pCt des rohen Methylalkohols) umzuwandeln, zu isoliren und wieder in Methylalkohol zu verwandeln ist, sondern dafs nur der geringe Acetongehalt, 1 bis 2 pCt., fortzuschaffen bleibt.but then at the same time other impurities are also destroyed by the chlorine the cleaning of the wood spirit is an easier one. The advantage of this method is in that not the whole mass of the methyl alcohol (98 to 99 pCt of the crude methyl alcohol) must be converted, isolated, and converted back into methyl alcohol, but that only the low acetone content, 1 to 2 pct., to move away remains.
Claims (1)
Publications (1)
Publication Number | Publication Date |
---|---|
DE36827C true DE36827C (en) |
Family
ID=312618
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
DENDAT36827D Expired - Lifetime DE36827C (en) | Production of acetone-free methyl alcohol from raw wood spirit |
Country Status (1)
Country | Link |
---|---|
DE (1) | DE36827C (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2821503A (en) * | 1953-02-10 | 1958-01-28 | Cities Service Oil Co | Purification of methanol |
-
0
- DE DENDAT36827D patent/DE36827C/en not_active Expired - Lifetime
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2821503A (en) * | 1953-02-10 | 1958-01-28 | Cities Service Oil Co | Purification of methanol |
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