DE817812C - Process for the production of solutions of acrylonitrile polymers - Google Patents
Process for the production of solutions of acrylonitrile polymersInfo
- Publication number
- DE817812C DE817812C DEB1580A DEB0001580A DE817812C DE 817812 C DE817812 C DE 817812C DE B1580 A DEB1580 A DE B1580A DE B0001580 A DEB0001580 A DE B0001580A DE 817812 C DE817812 C DE 817812C
- Authority
- DE
- Germany
- Prior art keywords
- solutions
- production
- polyacrylonitrile
- acrylonitrile
- acrylonitrile polymers
- 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
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/09—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in organic liquids
- C08J3/091—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in organic liquids characterised by the chemical constitution of the organic liquid
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2333/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2333/18—Homopolymers or copolymers of nitriles
- C08J2333/20—Homopolymers or copolymers of acrylonitrile
Landscapes
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacture Of Macromolecular Shaped Articles (AREA)
Description
Verfahren zur Herstellung von Lösungen von Acrylnitrilpolymerisaten Acrvlnitrilpolymerisate, wie Polyacrylnitril und it,lisclil>olvmerisate aus Acrylnitril mit anderen polymerisierbaren Stoffen lösen sich bekanntlich nur in wenigen Solventien. Von organischen Lösungsmitteln eignet sich vor allem das Dimethylformamid, das jedoch ziemlich teuer ist. Ein verhältnismäßig gutes Lösungsmittel ist die konzentrierte Schwefelsäure. Diese hat jedoch den Nachteil, daß beim `'Wiederausfällen des Polyacrylnitrils mit Wasser die in dem ausgefällten Polyacrylnitril enthaltenen Reste Schwefelsäure nur äußerst langsam herausdittundieren, wobei in mehr oder weniger großem Umfang partielle Verseifung der Nitrilgruppen eintreten kann. So hergestellte Folien, Fäden und andere Formkörper haben dann nicht die optimalen Eigenschaften.Process for the preparation of solutions of acrylonitrile polymers Acrylonitrile polymers, such as polyacrylonitrile and it, lisclil> olvmerisate made from acrylonitrile It is known that with other polymerizable substances they only dissolve in a few solvents. Of the organic solvents, dimethylformamide is particularly suitable, but that is quite expensive. A relatively good solvent is the concentrated one Sulfuric acid. However, this has the disadvantage that when the polyacrylonitrile precipitates again with water the residues of sulfuric acid contained in the precipitated polyacrylonitrile diffuse out only extremely slowly, and to a greater or lesser extent partial saponification of the nitrile groups can occur. Foils, threads made in this way and other moldings then do not have the optimal properties.
Es wurde nun gefunden, daß man Lösungen von Polyacrvlnitril und von Mischpolymerisaten aus Acrvlnitril mit anderen polymerisierbaren Stoffen, insbesondere Acrylsäureamid oder Amiden anderer a -,B-ungesättigter Carbonsäuren auch erhalten kann, wenn man die genannten Polymerisate in starken organischen oder anorganischen Sauerstoffsäuren anquillt und dann geringe Mengen konzentrierte Schwefelsäure hinzufügt. Geeignete Sauerstoffsäuren sind z. B. Phosphorsäure, Toluolsulfonsäure, Mono-, Di- und Trichloressigsäure. Bei Verwendung dieser Säuren genügt ein Zusatz von höchstens etwa io% konzentrierter Schwefelsäure, um das gequollene Polymerisat klar zu lösen. Aus den Lösungen lassen sich durch Fällen mit Wasser in üblicher Weise Folien, Fäden und andere Formkörper herstellen, ohne daß in wesentlichem Umfang Verseifung der Nitrilgruppen eintritt. Beispiel i 12,5 Teile eines Polyacrylnitrils mit einem K-Wert von etwa 8o werden in 82,5 Teile Trichloressigsäure eingetragen und eingequollen; nach Zugabe von 5 Teilen konzentrierter Schwefelsäure entsteht eine klare Lösung. Diese Lösung wird in üblicher Weise aus Spinndüsen in Wasser verspoctnen; die gewonnenen Fäden werden gründlich gewaschen und mit verdünnten Lösungen basischer Stoffe vollends neutralisiert, aufgehaspelt und getrocknet. Beispiel e Eine nach Beispiel i hergestellte Lösung wird auf einer geeigneten Unterlage, z. B. .einer Glasplatte, in bekannter Weise zu einem Film ausgegossen. Durch Behandeln des Aufstriches mit Wasser erhält man einen Film von Polyacrylnitril. Beispiel 3 Eine nach Beispiel i hergestellte Lösung wird eine Tauchform, z. B. ein Reagenzglas, getaucht. Der an der Form haftende Film wird anschließend durch Eintauchen in Wasser und mehrfaches Wässern in einen Formkörper verwandelt, der der verwendeten Tauchform entspricht.It has now been found that solutions of polyacrylonitrile and of Copolymers of acrylonitrile with other polymerizable substances, in particular Acrylic acid amide or amides of other a-, B-unsaturated carboxylic acids also obtained can, if the polymers mentioned in strong organic or inorganic Oxygen acids swells and then small amounts of concentrated sulfuric acid are added. Suitable oxygen acids are e.g. B. phosphoric acid, toluenesulfonic acid, mono-, di- and trichloroacetic acid. When using these acids, an addition of at most is sufficient about 10% concentrated sulfuric acid to clear the swollen polymer. Films and threads can be converted from the solutions in the customary manner by precipitation with water and produce other shaped bodies without saponification of the substantial amounts Nitrile groups occurs. Example i 12.5 parts of a polyacrylonitrile with a K value of about 8o are trichloroacetic acid in 82.5 parts registered and swollen; after the addition of 5 parts of concentrated sulfuric acid is formed a clear solution. This solution is in the usual way from spinnerets in water propose; the threads obtained are washed thoroughly and diluted with Solutions of basic substances completely neutralized, reeled and dried. example e A solution prepared according to example i is placed on a suitable surface, z. B. .a glass plate, poured into a film in a known manner. By treating After the spread with water, a film of polyacrylonitrile is obtained. Example 3 A solution prepared according to Example i is a dipping mold, for. B. a test tube, submerged. The film adhering to the mold is then immersed in water and repeated soaking is transformed into a shaped body that of the dipping mold used is equivalent to.
Beispiel 4 Man verwendet als Quellmittel an Stelle von Trichloressigsäure konzentrierte Phosphorsäure, Monochloressigsäure oder p-Toluolsulfonsäure und verfährt im übrigen wie in den vorhergehenden Beispielen. Man erhält ebenfalls klare Lösungen und daraus Filme bzw. Folien und Formkörper aus unverseiftem Polyacrylnitril.Example 4 The swelling agent used is in place of trichloroacetic acid concentrated phosphoric acid, monochloroacetic acid or p-toluenesulfonic acid and processes otherwise as in the previous examples. Clear solutions are also obtained and therefrom films or sheets and moldings made of unsaponified polyacrylonitrile.
Beispiels An Stelle von Polyacrylnitril verwendet man ein Mischpolymerisat aus @o Teilen Acrylnitril und 2o Teilen Acrylsäureamid oder -,\-Zethacrylsäureamid und verfährt im übrigen wie in den vorhergehenden Beispielen. Die erhaltenen Lösungen bzw. Fäden, Filme und anderen Formkörper zeigen praktisch den gleichen Gehalt an Nitrilgruppen wie vor der Lösung.Example Instead of polyacrylonitrile, a copolymer is used from @o parts of acrylonitrile and 2o parts of acrylic acid amide or -, \ - zethacrylic acid amide and proceed as in the previous examples. The solutions obtained or threads, films and other shaped bodies show practically the same content Nitrile groups as before the solution.
Claims (1)
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DEB1580A DE817812C (en) | 1950-01-17 | 1950-01-17 | Process for the production of solutions of acrylonitrile polymers |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DEB1580A DE817812C (en) | 1950-01-17 | 1950-01-17 | Process for the production of solutions of acrylonitrile polymers |
Publications (1)
Publication Number | Publication Date |
---|---|
DE817812C true DE817812C (en) | 1951-10-22 |
Family
ID=6952353
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
DEB1580A Expired DE817812C (en) | 1950-01-17 | 1950-01-17 | Process for the production of solutions of acrylonitrile polymers |
Country Status (1)
Country | Link |
---|---|
DE (1) | DE817812C (en) |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE1005724B (en) * | 1955-03-25 | 1957-04-04 | Hoechst Ag | Solvent for acrylonitrile polymers |
DE1111773B (en) * | 1958-08-11 | 1961-07-27 | Phrix Werke Ag | Process for the production of threads, fibers, bristles or foils by spinning solutions of acrylonitrile polymers in strong sulfuric acid |
DE1171609B (en) * | 1961-08-25 | 1964-06-04 | Phrix Werke Ag | Process and device for the continuous production of polyacrylonitrile solutions in sulfuric acid |
-
1950
- 1950-01-17 DE DEB1580A patent/DE817812C/en not_active Expired
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE1005724B (en) * | 1955-03-25 | 1957-04-04 | Hoechst Ag | Solvent for acrylonitrile polymers |
DE1111773B (en) * | 1958-08-11 | 1961-07-27 | Phrix Werke Ag | Process for the production of threads, fibers, bristles or foils by spinning solutions of acrylonitrile polymers in strong sulfuric acid |
DE1171609B (en) * | 1961-08-25 | 1964-06-04 | Phrix Werke Ag | Process and device for the continuous production of polyacrylonitrile solutions in sulfuric acid |
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