DE109996C - - Google Patents
Info
- Publication number
- DE109996C DE109996C DENDAT109996D DE109996DA DE109996C DE 109996 C DE109996 C DE 109996C DE NDAT109996 D DENDAT109996 D DE NDAT109996D DE 109996D A DE109996D A DE 109996DA DE 109996 C DE109996 C DE 109996C
- Authority
- DE
- Germany
- Prior art keywords
- cellulose
- disodium
- ammonia
- copper
- copper hydroxide
- 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.)
- Active
Links
- 229920002678 cellulose Polymers 0.000 claims description 31
- 239000001913 cellulose Substances 0.000 claims description 30
- 239000005750 Copper hydroxide Substances 0.000 claims description 9
- 229910001956 copper hydroxide Inorganic materials 0.000 claims description 9
- JJLJMEJHUUYSSY-UHFFFAOYSA-L Copper(II) hydroxide Chemical compound [OH-].[OH-].[Cu+2] JJLJMEJHUUYSSY-UHFFFAOYSA-L 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 claims description 4
- ARUVKPQLZAKDPS-UHFFFAOYSA-L Copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 3
- 229910000365 copper sulfate Inorganic materials 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 claims description 2
- QXNVGIXVLWOKEQ-UHFFFAOYSA-N disodium Chemical compound [Na][Na] QXNVGIXVLWOKEQ-UHFFFAOYSA-N 0.000 claims 4
- 150000001879 copper Chemical class 0.000 claims 1
- 235000010980 cellulose Nutrition 0.000 description 26
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 7
- 239000007788 liquid Substances 0.000 description 5
- 229920000742 Cotton Polymers 0.000 description 3
- DBNPDRYVYQWGFW-UHFFFAOYSA-N N.[Cu]=O Chemical compound N.[Cu]=O DBNPDRYVYQWGFW-UHFFFAOYSA-N 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-N Carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N HCl Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L na2so4 Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229920000297 Rayon Polymers 0.000 description 1
- 230000001476 alcoholic Effects 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- -1 copper hydroxide compound Chemical class 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N oxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- KEAYESYHFKHZAL-UHFFFAOYSA-N sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 235000011121 sodium hydroxide Nutrition 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- PANBYUAFMMOFOV-UHFFFAOYSA-N sodium;sulfuric acid Chemical compound [Na].OS(O)(=O)=O PANBYUAFMMOFOV-UHFFFAOYSA-N 0.000 description 1
- 241000894007 species Species 0.000 description 1
- WRWHFVRDUAQRIQ-UHFFFAOYSA-L sulfanylidenemethanediolate Chemical compound [O-]C([O-])=S WRWHFVRDUAQRIQ-UHFFFAOYSA-L 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B1/00—Preparatory treatment of cellulose for making derivatives thereof, e.g. pre-treatment, pre-soaking, activation
- C08B1/006—Preparation of cuprammonium cellulose solutions
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)
- Chemical Or Physical Treatment Of Fibers (AREA)
Description
KAISERLICHESIMPERIAL
»96. 109 996, 118 836, 118 83?. «er.“96. 109 996, 118 836, 118 83 ?. "he.
PATENTAMT.PATENT OFFICE.
H- hH- h
! G ! G
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Es ist eine allgemeine bekannte Thatsache, dafs Baumwolle und andere natürlich vorkommende Cellulosearten in Kupferoxydammoniak löslich sind.It is a well-known fact that cotton and others naturally occur Cellulosic species are soluble in copper oxide ammonia.
Letzteres wird entweder nach der Vorschrift von Schweizer durch Auflösen bis zur Sättigung von reinem Kupferhydroxyd in 22 procentiger Ammoniakflüssigkeit oder auch nach der Vorschrift von Wright durch Lösen von Kupferschnitzeln in starkem Ammoniak unter Zuhülfenahme des Sauerstoffes der Luft hergestellt.The latter is either resolved according to the Swiss rules by dissolving up to Saturation of pure copper hydroxide in 22 percent ammonia liquid or also according to Wright's prescription by dissolving copper chips in strong ammonia produced with the aid of the oxygen in the air.
Genaue Angaben über den Löslichkeitsgrad der verschiedenen Cellulosen, sowie vergleichende Angaben über die physikalischen Eigenschaften der verschiedenen Lösungen und der daraus wieder abgeschiedenen Cellulose fehlen bis jetzt in der Literatur. Nur Cross & Bevan erwähnen in ihrem Werke „Cellulose", London 1895, Longmans, Green & Co., dafs Lösungen von Cellulosehydrat, wie solches z. B. durch Zersetzen der Lösung des Natriumcellulosethiocarbonates derselben Forscher entsteht, zäher und weniger gelatinös seien.Precise information on the degree of solubility of the various celluloses, as well as comparative information Information on the physical properties of the various solutions and the resulting from them Re-deposited cellulose is missing in the literature up to now. Just mention Cross & Bevan in their work Cellulose, London 1895, Longmans, Green & Co., dafs Solutions of cellulose hydrate, such as such. B. by decomposing the sodium cellulose thiocarbonate solution by the same researcher arises that they are tougher and less gelatinous.
In der That ist es sehr schwer, rasch eine gröfsere Quantität Baumwolle in Kupferoxydammoniak zu lösen.Indeed, it is very difficult to rapidly get a large quantity of cotton in cupric ammonia to solve.
. Es entsteht zumeist zuerst eine gallertige Masse, die bei gewöhnlicher Temperatur nur in dem Mafse dünnflüssiger wird, als die Cellulose selbst durch das Kupferoxydammoniak eine Oxydation erleidet, wie dies schon von Prud'homme festgestellt wurde.. Usually a gelatinous mass is formed first, which only occurs at normal temperature to the extent that it becomes thinner than the cellulose itself due to the copper oxide ammonia suffers oxidation, as has already been stated by Prud'homme.
Es liegt dies einerseits daran, dafs die im Cellulosemolecül vorhandenen alkoholischen Hydroxylgruppen, denen zu gleicher Zeit auch Phenolcharakter zukommt, unter den angegebenen Umständen nicht direct mit der KupferoxydammoniakbaseOn the one hand, this is due to the fact that the alcoholic molecules present in the cellulose molecules Hydroxyl groups, which at the same time also have phenolic character, among those indicated Certainly not directly with the copper oxide ammonia base
(C<0NhI = Cu(OH)2,( C <0NhI = Cu (OH) 2 ,
so zu reagiren vermögen, dafs das Kupferhydroxyd mit den phenolartigen Hydroxylgruppen des Cellulosemolecüls eine salzartige Verbindung eingeht.are able to react in such a way that the copper hydroxide with the phenol-like hydroxyl groups of the cellulose molecule enters into a salt-like compound.
Andererseits hält es schwer, die zur Herstellung von mehrprocentigen Celluloselösungen nöthigen Mengen Kupfer in Lösung zu bekommen. On the other hand, it is difficult for the production of multi-percent cellulose solutions to get the necessary amounts of copper in solution.
Entweder erhält man somit gallertige, unflltrirbare Lösungen, oder dünnflüssige, aber unbrauchbare, da die enthaltene Cellulose daraus nicht mehr unverändert abscheidbar ist.Either you get gelatinous, infiltratable solutions, or thin liquid, but unusable, since the cellulose contained can no longer be separated from it unchanged.
Es hat sich nun bei eingehenden Versuchen gezeigt, dafs technisch verwerthbare Lösungen von Cellulose auf ganz einfache und bequeme Weise sofort erhalten werden können, wenn die Cellulose in Form von Kupferhydroxydcellulose gemäfs nachstehender Erfindung als solche in Ammoniak gelöst wird.Thorough experiments have now shown that technically usable solutions of cellulose can be obtained instantly in a very simple and convenient way, though the cellulose in the form of copper hydroxide cellulose according to the invention below as such is dissolved in ammonia.
Am besten wird zur Herstellung der Kupferhydroxydcellulose so verfahren, dafs die fein zertheilte Cellulose aufgeschlossen wird durch Ueberführung in die auch zur Cross & Bevanschen Viscose-Darstellung benutzte, sehr reactionsfähige Natroncellulose.For the production of copper hydroxide cellulose it is best to proceed in such a way that it is fine Divided cellulose is broken down by transferring it to the Cross & Bevanschen Viscose representation used, very reactive soda cellulose.
Diese wird dann in geeigneten Mischmaschinen zusammengerieben mit der molecularen Menge von Kupfersulfat (CuSOi + 5 H2O). DurchThis is then rubbed together in suitable mixing machines with the molecular amount of copper sulfate (CuSO i + 5 H 2 O). By
doppelte Umsetzung entsteht dabei schwefelsaures Natrium und eine lose Verbindung von Kupferhydroxyd und Cellulose.double conversion results in sulfuric acid sodium and a loose connection of Copper hydroxide and cellulose.
Diese lose Verbindung ist durch Wasser genau wie die Natroncellulose zersetzlich unter Abscheidung von Cellulosehydrat und Kupferhydroxyd. In Ammoniak ist sie sofort löslich zu einer selbst bei höherer Temperatur ihre Viscosität bewahrenden Flüssigkeit.This loose connection is decomposable by water just like the soda cellulose Separation of cellulose hydrate and copper hydroxide. It is immediately soluble in ammonia a liquid that retains its viscosity even at higher temperatures.
162 g trockene Cellulose (1 Molecül) werden fein: zerschnitten und bei gewöhnlicher Temperatur mit -einer Lösung von 80 g reinem Natronhydrat in 500 g Wasser gut durchgemischt. Nach etwa einstündigem Stehen werden sodann 249 g (= 1 Molecül) krystallisirten Kupfersulfats (Cu SOi -f 5 H2 O) in fein gepulvertem Zustande zugefügt und unter Vermeidung erheblicherer Erwärmung innig gemischt. 162 g dry cellulose (1 molecule) are finely : cut up and mixed well at normal temperature with a solution of 80 g pure sodium hydrate in 500 g water. After standing for about one hour, 249 g (= 1 mol) of crystallized copper sulphate (Cu SO i -f 5 H 2 O) in a finely powdered state are then added and thoroughly mixed, avoiding considerable heating.
Das so erhaltene homogene hellblaue Product ist direct in concentrirter wässeriger Ammoniakflüssigkeit löslich, wobei der gröfste Theil des gebildeten Natriumsulfates zurückbleibt. Zweekmäfsig werden dabei die Verhältnisse so gewählt, dafs auf je 1 Molecül Kupferhydroxydcellulose beiläufig 16 bis 20 Molecule Ammoniakgas kommen.The homogeneous light blue product thus obtained is directly in a concentrated aqueous ammonia liquid soluble, the greater part of the sodium sulphate formed remaining. Two-way the proportions are chosen so that for every 1 molecule of copper hydroxide cellulose incidentally 16 to 20 molecules of ammonia gas come in.
Zur Verwendung kann gelangen: Baumwolle, ZellstofFoder auch Cellulosehydrat irgend welcher Art. Auch Hydrocellulose (nach Girard aus Cellulose durch Tränken mit 2 procentiger Salzsäure, Trocknen bei 60 bis 8o° und nachheriges Waschen) liefert nach vorstehendem Verfahren bis zu 12 und mehr Procent Cellulose haltende prächtige Lösungen, von collodiumähnlichem Charakter. Da 'diese Hydrocellulose in Schweizer'scher oder Wright'scher Flüssigkeit sonst nur in ganz unbedeutendem Mafse löslich ist, so ist hierin ein wichtiger Beweis zu erblicken für die Richtigkeit der Annahme einer in Ammoniak als solche löslichen Kupferhydroxydverbindung der Cellulose.The following can be used: cotton, cellulose or cellulose hydrate of any kind Art. Also hydrocellulose (according to Girard from cellulose by soaking with 2 percent hydrochloric acid, Drying at 60 to 80 ° and washing afterwards) yields according to the above process Splendid solutions containing up to 12 and more percent cellulose, similar to collodions Character. Since 'this hydrocellulose is in a Swiss or Wright liquid is otherwise soluble only to a very insignificant extent, this is an important proof to see for the correctness of the assumption of a copper hydroxide compound which is soluble in ammonia as such the cellulose.
Die Lösungen sollen im Zeugdruck und zur Herstellung von Glanzstofffäden Verwendung finden.The solutions are intended to be used in fabric printing and for the production of luster threads Find.
Claims (2)
Publications (1)
Publication Number | Publication Date |
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DE109996C true DE109996C (en) |
Family
ID=379839
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