DE977869C - Process for the production of stable polyvinyl nitrate - Google Patents

Process for the production of stable polyvinyl nitrate

Info

Publication number
DE977869C
DE977869C DEL29599A DEL0029599A DE977869C DE 977869 C DE977869 C DE 977869C DE L29599 A DEL29599 A DE L29599A DE L0029599 A DEL0029599 A DE L0029599A DE 977869 C DE977869 C DE 977869C
Authority
DE
Germany
Prior art keywords
production
nitrate
polyvinyl nitrate
acid
product
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
DEL29599A
Other languages
German (de)
Inventor
Karl Dr Meyer
Werner Dipl-Chem Dr Diepold
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.)
Bundesrepublik Deutschland
Original Assignee
Bundesrepublik Deutschland
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 Bundesrepublik Deutschland filed Critical Bundesrepublik Deutschland
Priority to DEL29599A priority Critical patent/DE977869C/en
Application granted granted Critical
Publication of DE977869C publication Critical patent/DE977869C/en
Expired legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L29/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal or ketal radical; Compositions of hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Compositions of derivatives of such polymers
    • C08L29/02—Homopolymers or copolymers of unsaturated alcohols
    • C08L29/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids

Landscapes

  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)

Description

Es ist bereits bekannt, Polyvinylnitrat aus Polyvinylalkohol dadurch herzustellen, daß man den Polyvinylalkohol nach vorheriger Lösung in konzentrierter Schwefelsäure mit Nitriersäure zusammenbringt und unter Temperatursteigerung die Bildung und Abscheidung des Nitrats bewirkt (deutsche Patentschrift 537 303 und K r c ζ i 1, Kurzes Handbuch der Polymerisationstechnik, Bd. I, 1940, S. 613).It is already known to produce polyvinyl nitrate from polyvinyl alcohol by the Polyvinyl alcohol brings together with nitrating acid after prior dissolution in concentrated sulfuric acid and causes the formation and deposition of the nitrate by increasing the temperature (German patent 537 303 and K r c ζ i 1, Kurzes Handbuch der Polymerizationstechnik, Vol. I, 1940, p. 613).

Ferner ist es bekannt, Polyvinylnitrat aus PoIyvinylalkoholpulver herzustellen. Das in einer organischen, gegen die zur Verwendung kommenden Säuren indifferenten Flüssigkeit suspendierte Pulver wird dabei in starke Salpetersäure, Nitriersäure oder ein Gemisch von Salpetersäure und Phosphorsäure eingerührt und zur Vermeidung der sonst bei der Nitrierung eintretenden Oxydation die Temperatur zweckmäßig bei ο bis — 300 C gehalten (Patentschrift 4749 des Amtes für Erfindungs- und Patentwesen in Ost-Berlin; Chem. Zentralblatt, 1955, S. 4714).It is also known to produce polyvinyl nitrate from polyvinyl alcohol powder. The powder, which is suspended in an organic liquid that is indifferent to the acids used, is stirred into strong nitric acid, nitrating acid or a mixture of nitric acid and phosphoric acid and, in order to avoid the oxidation that otherwise occurs during the nitration, the temperature is expediently from 0 to -30 ° C (Patent 4749 of the Office for Invention and Patents in East Berlin; Chem. Zentralblatt, 1955, p. 4714).

Dabei wurde festgestellt, daß der makromolekulare Charakter des Polyvinylnitrates dafür verantwortlich ist, daß bei der Ausfällung des zunächst gelösten Nitrierproduktes in Wasser geringe Säuremengen in dem dann anfallenden festen Nitrierprodukt eingeschlossen werden.It was found that the macromolecular character of the polyvinyl nitrate is responsible for this is that when the nitration product, which is initially dissolved, is precipitated in water, small amounts of acid are then included in the solid nitration product.

Diese Säuremengen begünstigen einen fortschreitenden Zerfall des erhaltenen Produktes und müssen aus ihm entfernt werden, wenn das Produkt technische Brauchbarkeit aufweisen soll.These amounts of acid favor a progressive decomposition of the product obtained and must be removed from it if the product is to have technical usefulness.

Es wurde nun gefunden, daß man zu einem hochwertigen und stabilen Polyvinylnitratprodukt dadurch gelangen kann, daß man bei der NitrierungIt has now been found that this leads to a high quality and stable polyvinyl nitrate product that one can get in the nitration

bis zu etwa 20 %> eines nitrierbaren, in Salpetersäure löslichen Polymeren, wie z. B. Polystyrol od. dgl. zusetzt und das erhaltene Produkt durch mehrfaches Kochen mit Wasser stabilisiert.
5 Ohne einen Zusatz an Polystyrol oder einer ähnlichen Verbindung während des Nitrierungsprozesses läßt sich das erhaltene Polyvinylnitrat nicht stabilisieren, weil das Produkt bei etwa 700 C erweicht und sich zu einem in der Wärme gummiartigen Klumpen zusammenballt. Dies wird selbst bei höchsten Polymerisatioiisgraden beobachtet.up to about 20%> of a nitrable, nitric acid-soluble polymer, such as. B. polystyrene or the like. Adds and the product obtained is stabilized by boiling several times with water.
5 Without the addition of polystyrene or a similar compound during the nitration process, the polyvinyl nitrate obtained cannot be stabilized because the product softens at about 70 ° C. and agglomerates into a rubber-like lump when heated. This is observed even at the highest degrees of polymerisation.

Um die Zusammenballung zu vermeiden, muß die Temperatur unter 6o° C gehalten werden. Bei dieser Temperatur konnte bisher jedoch noch kein hinreichend stabiles Produkt erhalten werden, da die Diffusion der eingeschlossenen Säure zu langsam vor sich geht.To avoid agglomeration, the temperature must be kept below 60 ° C. at this temperature, however, has not yet been able to obtain a sufficiently stable product, since the diffusion of the trapped acid is too slow.

Beispielexample

ao Polyvinylalkohol wird beim Nitrierprozeß mit bis zu 20% Polystyrol versetzt, nach der Nitrierung in Wasser ausgefällt, abfiltriert und gewaschen, von der Abfallsäure filtriert und in mehrfachen Operationen mit Wasser gekocht.ao polyvinyl alcohol is used in the nitration process up to 20% polystyrene added, precipitated after nitration in water, filtered off and washed, from the waste acid is filtered and boiled with water in multiple operations.

Es ergibt sich ein stabiles Endprodukt, welches einen weit über der Norm liegenden Wert beim ABEL-Test ergibt.The result is a stable end product, which has a value that is far above the norm ABEL test results.

Claims (1)

PATENTANSPRUCH:PATENT CLAIM: Verfahren zur Herstellung von stabilem Polyvinylnitrat durch Nitrieren von Polyvinylalkohol, dadurch gekennzeichnet, daß man bei der Nitrierung bis zu etwa 20 % eines nitrierbaren, in Salpetersäure löslichen Polymeren, wie z. B. Polystyrol od. dgl., zusetzt und das erhaltene Produkt durch mehrfaches Kochen mit Wasser stabilisiert.Process for the production of stable polyvinyl nitrate by nitriding polyvinyl alcohol, characterized in that up to about 20% of a nitrable, polymers soluble in nitric acid, such as. B. polystyrene od. Like., Adds and the obtained Product stabilized by boiling with water several times. In Betracht gezogene Druckschriften:
Deutsche Patentschrift Nr. 537303;
Patentschrift Nr. 4749 des Amtes für Erfindungs- und Patentwesen in Ost-Berlin (gleich: Chemisches Zentralblatt, 1955, S. 4714).Considered publications:
German Patent No. 537303;
Patent No. 4749 of the Office for Invention and Patents in East Berlin (same as: Chemisches Zentralblatt, 1955, p. 4714). 109 649/1 11.71109 649/1 11.71
DEL29599A 1958-02-04 1958-02-04 Process for the production of stable polyvinyl nitrate Expired DE977869C (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
DEL29599A DE977869C (en) 1958-02-04 1958-02-04 Process for the production of stable polyvinyl nitrate

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DEL29599A DE977869C (en) 1958-02-04 1958-02-04 Process for the production of stable polyvinyl nitrate

Publications (1)

Publication Number Publication Date
DE977869C true DE977869C (en) 1971-12-02

Family

ID=7264920

Family Applications (1)

Application Number Title Priority Date Filing Date
DEL29599A Expired DE977869C (en) 1958-02-04 1958-02-04 Process for the production of stable polyvinyl nitrate

Country Status (1)

Country Link
DE (1) DE977869C (en)

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE4749C (en) * A. reitze in Hannover Operating mechanism for smaller machines
DE537303C (en) * 1929-11-15 1931-11-02 Consortium Elektrochem Ind Representation of polyvinyl nitrate

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE4749C (en) * A. reitze in Hannover Operating mechanism for smaller machines
DE537303C (en) * 1929-11-15 1931-11-02 Consortium Elektrochem Ind Representation of polyvinyl nitrate

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