DE1745939C3 - Verfahren zum Modifizieren von Carboxylgruppen enthaltenden Äthylenpolymeren - Google Patents

Verfahren zum Modifizieren von Carboxylgruppen enthaltenden Äthylenpolymeren

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DE1745939C3
DE1745939C3 DE1745939A DEP0036184A DE1745939C3 DE 1745939 C3 DE1745939 C3 DE 1745939C3 DE 1745939 A DE1745939 A DE 1745939A DE P0036184 A DEP0036184 A DE P0036184A DE 1745939 C3 DE1745939 C3 DE 1745939C3
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acid
mixed
mixing
copolymer
zone
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DE1745939A1 (de
DE1745939B2 (de
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Richard Watkin Wilmington Del. Rees (V.St.A.)
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EIDP Inc
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EI Du Pont de Nemours and Co
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/04—Oxygen-containing compounds
    • C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
    • C08K5/098—Metal salts of carboxylic acids
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
    • B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
    • B32B17/10—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin
    • B32B17/10005—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing
    • B32B17/1055—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the resin layer, i.e. interlayer
    • B32B17/10743—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the resin layer, i.e. interlayer containing acrylate (co)polymers or salts thereof
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F255/00—Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F8/00—Chemical modification by after-treatment
    • C08F8/30—Introducing nitrogen atoms or nitrogen-containing groups
    • C08F8/32—Introducing nitrogen atoms or nitrogen-containing groups by reaction with amines
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F8/00—Chemical modification by after-treatment
    • C08F8/44—Preparation of metal salts or ammonium salts
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/04—Oxygen-containing compounds
    • C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/16—Nitrogen-containing compounds
    • C08K5/17—Amines; Quaternary ammonium compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F2800/00—Copolymer characterised by the proportions of the comonomers expressed
    • C08F2800/20—Copolymer characterised by the proportions of the comonomers expressed as weight or mass percentages
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L23/04—Homopolymers or copolymers of ethene
    • C08L23/08—Copolymers of ethene
    • C08L23/0846—Copolymers of ethene with unsaturated hydrocarbons containing other atoms than carbon or hydrogen atoms
    • C08L23/0869—Acids or derivatives thereof
    • C08L23/0876—Neutralised polymers, i.e. ionomers
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S260/00—Chemistry of carbon compounds
    • Y10S260/31—Ionic cross-link
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    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S273/00—Amusement devices: games
    • Y10S273/22—Ionomer
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    • Y10S36/00—Boots, shoes, and leggings
    • Y10S36/02—Plastic
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/13—Hollow or container type article [e.g., tube, vase, etc.]
    • Y10T428/1352—Polymer or resin containing [i.e., natural or synthetic]
    • Y10T428/139—Open-ended, self-supporting conduit, cylinder, or tube-type article
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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Processes Of Treating Macromolecular Substances (AREA)

Description

und in welcher die flüchtigen Materialien, z. B. Wasser und Säure (die sich bildet, wenn man das Mischpolymerisat mit einem Salz umsetzt), verdampft und entfernt werden. In der.vierten Zone wird das Polymerisat aus dem Entgasungsextruder entfernt. In dem Extruder können natürlich mehr als eine Zone des jeweiligen Typs vorliegen; auch können die Zonen unterschiedliche Abmessungen haben.
Der Vorteil des erfindungsgemäßen Verfahrens ge- ■ genüber dem Verfahren unter Verwendung eines Kautschukmahlwerkes liegt in der größeren Gleichmäßigkeit der Endprodukte und der viel kürzeren Reaktionszeit.
Be i s ρ iele 1 bis 8 iS
In die Zuführungsöffnung eines 5-cm-Entgasungsextruders gibt man in getrennten Strömen Teilchen eines Mischpolymerisats aus Äthylen und Methacrylsäure und eine Metallverbindung, die im wesentlichen in dem geschmolzenen Polymerisat unlöslich ist. Die Zuführungsgeschwindigkeit *des Mischpolymerisates variiert von 6,8 bis 10,0 kg Std. Die Schnecke erstreckt sich über einen Plastifizierabschnitt, der 8mal so lang ist wie der Durchmesser, einem Mischabschniit, wie er in der USA.-Patentschrift 3 006 029 beschrieben ist und der J3,5mal so lang ist wie der Durchmesser, einem Drossclring, der es erlaubt, in dem Mischabschnitt einen Druck aufrechtzuerhalten, einem Entgasungsabschnitt, der 5mal so lang ist wie der Durchmesser urfd einem Pumpabschnitt, der 4mal so lang ist wie der Durchmesser. Dort, wo der Mischabschnitt beginnt, spritzt man in das geschmolzene Harz eine Säurelösung ein. Die Schmelztemperatur beträgt an dieser Stelle 156 C und der Druck 28,1 kg cm2. Das Gemisch läßt man im Mischabschnitt reagieren; anschließend leitet man das 210 C heiße, geschmolzene Gemisch über den Drosselring in die Entgasungszone. Die Schmelze entdampft man im Vakuum (686 mm Hg). Anschließend extrudiert man das getrocknete geschmolzene, durch Ionen vernetzte Mischpolymerisat; den erhaltenen Strang kühlt man in Wasser und granuliert ihn.
Die einzelnen Arbeitsweisen, die eingesetzten Reagentien und einige der beeinflußten Polymerisateigenschaften sind in Tabelle 1 angegeben.
Tabelle
Saures Mischpolymerisat Steifig Metallverbindung Zu-
führungs- 		Säurelös iing I γη wäßrige Zu-
führungs- 		Pw-
duktions- 		Produkt Steifig
Bei
spiel 		Meth
acryl 		Schmelz keit. geschwin- Lösung geschwin- gcschwin- Schmclz- keit.
säure, index, Typ digkeit Volum digkcit digkcit index.
Gewichts kg/cm2 kg/Std. Propion prozent cm* Min. kg/Std. kg;cmä
prozent g/10 Min. 861,3 0.363 säure ' 50 5,29 7,48 g/10Min. 3139,7
1 15 71 ZnO Essig ; 1,52
861,3 0,476 säure 100 6,0 8,39 3689,8
2 15 71 ZnO Meth 0,28
861,3 0,676 acryl 60 9,17 7,94 3779,4
3 15 71 ZnO säure 0,19
Milch
861,3 0,535 säure*) 60 5,85 7,17 4241,9
4 15 71 ZnO Essig 0,29
1705,0 0,508 säure 50 5,22 9,98 3728.8
5 15,3 6,3 ZnO Isopro-
panol
Heptan-		 0,13
säure 25
1705,0 0,485 Essig 61.9 9,0 9,98 3168,1
6 15,3 6,3 ZnO säure 0,16
Essig 22,7
säure
— 0,404 Essig 50 4,83 8,66 64 —
.7 10**) 90 ZnO säure 2,46
— 0,163 50 5,5 6,12 —
8 9***) 178 ZnO 25
·) Die Milchsäure löst ZnO unter den Reaktionsbedingungen nicht vollständig. Ein weiteres Mischen ergibt eine vollständige Lösung. ♦·) Terpolymerisat aus 67U/O Äthylen, 247,, Vinylacetat und 10°/u Methacrylsäure. ·**) Terpolymerisat aus T0°/„ Äthylen, 20"/,, Vinylacetat und 90°/0 Methacrylsäure.
B e i s ρ i e 1 e 9 bis 16
In die ZufUhrungsöffnung eines 8,9-cm-Entgasungsextruders gibt man in getrennten Strömen Teilchen eines Mischpolymerisates aus Äthylen und Methacrylsäure und eine trockne pulverartige Mischung (bezeichnet als Vorgemisch), die aus einer oder mehreren Metallverbindungen, feinzerteiltem Mischpolymerisat und gleichen Teilen Dilaurylthiodipropionat und Dodecylpentaerythritol-Diphosphat als Stabilisator besteht. Der erste Plastifizierabschnitt im Extruder ist 7mal so lang wie der Durchmesser und wird auf einer Temperatur von etwa 158"C gehalten. Dort, wo der Mischabschnitt beginnt, spritzt man eine Säurelösung
in die geschmolzene Masse mit Hilfe einer Düse. Der Mischabschnitt (entsprechend USA.-Patentschrift 3 006 029) ist 13mal so lang wie der Durchmesser und wird auf 270 bis 280 C gehalten. Dort findet die Reak-
tion der Polymerisatschmelze unter Neutralisation der Säuregruppen statt.
Hinter dem Mischabschnitt wird die Masse, die aus ionisch vernetztem Mischpolymerisat und aus Nebenprodukten besteht, die sich infolge der Umsetzung gebildet haben, durch ein Druck-Lenkungsventil und ein Rohr in den Entgasungsabi.chnitt geleitet, der einen Durchmesser von 5 cm hat. Die Temperatur der Masse vor dem Ventil beträgt 2800C und der Druck 52,7 kg/ cm2. Im Entgasungsabschnitt sind zwei Eatgasungszoned, wobei jede etwa 4mal so lang wie dei Durchmesser ist. In der ersten Entgasungszone hält man ein
Vakuum von 686 und in der zweiten eins von 711 mm Hg aufrecht. Die Temperatur der Schmelze hält man zwischen 270 und 2803C. In der Entgasungszone werden die flüchtigen Bestandteile aus dem geschmolzenen, durch Ionen vernetzten Mischpolymerisat entfernt. Das anschließend in Form von Strängen extrudierte Polymerisat kühlt man in Wasser und granuliert es.
Die einzelnen Arbeitsbedingungen, die eingesetzten ίο Reagentien und einige der beeinflußten Polymerisateigenschaften ersieht man aus der nachstehend angeführten Tabelle II.
Methacrylsäure-Mischpolymerisal S·) Steifigkeit, Tabe noil Vorgemisch ZnO Teile Stabilisator Z**)
Säure,
Gewichts 		kg/cm1 Metallverbindung Mg(OH1) teile
Beispiel prozent 45 843,7 Misch
polymerisat, 		Typ Mg(C2H3O2), · 4,54 0,80
9,5 45 843,7 Teile 4H2O 4,20 0,14 1,41
9 9.5 Mg(OH2)
10 8,74 Mg(C2H3O2V 4,54
45 843,7 4H2O 4,20 0,14 1,11
9,5 ZnO
11 8,74 Mg(OH)2 9,08
45 843,7 Mg(C2H3O2), · 5,0 0,15 1,39
9,5 5,9 1293,6 4H2O 0,20 1,43
12 11,7 9,08 LiOH · H2O
13 7.5 ZnO 4,41
4,3 984,3 Mg(OH)2 4,23 0,07 0,75
9,5 Mg(C2H3O2)2 · 4,54
14 6,3 1705,0 8,64 4H2O 0,14 0,95
15,3 LiOH · H2O
15 8,74 ZnO 4,41
6,3 1705,0 0,07 0,79
15,3
16 8,64
(Fortsetzung)
wäßrige Lösung von Säure Ζ·**> Geschwindig
keit 		Produkt Steifigkeit,
Beispiel Essigsäure Volumprozent 13,8 kg/Std. kg/cm*
Essigsäure 40 13,0 24,9 !> > 2573,2
9 Essigsäure 40 13,5 21,3 0,7 2698,7
10 Essigsäure 40 13,5 21,3 0,52 2668,5
11 Milchsäure 37 24,5 1,52 2419,5
12 Essigsäure 3,8 13,0 1,72
Essigsäure 40 13,8 25,9 2601,0
13 Essigsäure 40 13,8 27,2 0,37 2327,0
14 Essigsäure 40 13,8 26,8 1,2 3719,3
15 40 26,3 1,25 4366,0
16 0,84
S *) Schmelzindex, g/10 Min. Z **) Zufuhrungsgeschwindigkeit, kg/Std. Z***) Zuluhrungsgcschwindigkeit, cm'/Min.

Claims (3)

  1. enthaltenden Äthylenpolymeren durch homogenes
    Patentansprüche: Vermischen der Polymerisate mit solchen ionischen,
    ein- bis dreiwertigen, wasserlöslichen Metallverbin-
    i. Verfahren zum Modifizieren von Carboxyl- düngen, deren Nichtmetallrest mit dem Wasserstoffgruppen enthaltenden Äthylenpolymeren durch 5 atom aus der Carbonsäure bei Reaktionsbedingungen homogenesVermischen der Polymerisate mit solchen entfernt werden kann, unter gleichzeitiger Neutralisaionischen, ein- bis dreiwertigen, wasserlöslichen tion von wenigstens 10°/? der Carboxylgruppen, das Metallverbindungen, deren Nichtmetallrest mit dadurch gekennzeichnet ist, daß man als Carboxyldem Wasserstoffatom aus der Carbonsäure bei gruppen enthaltendes Athylenpolymerisat ein Misch-Reaktionsbedingungen entfernt werden kann, un- io polymerisat mit einem Schmelzindex von 0,1 bis ter gleichzeitiger Neutralisation von wenigstens 100 g/10 Minuten einsetzt, das wenigstens 50 MoI-10% der Carboxylgruppen, bei dem man als Carb- prozent Äthyleneinheiten und 0,2 bis 25 Mclprozent oxylgruppen enthaltendes Athylenpolymerisat ein Einheiten von ^,^-ungesättigten Monocarbonsäuren, Mischpolymerisat mit einem Schmelzindex von gegebenenfalls Einheiten eines mischpolymerisier-0,1 bis 100 g/10 Minuten einsetzt, das wenigstens 15 baren, einfach ungesättigten dritten Comonomeren 50 MolprozentÄthyleneinheitenund0,2 bis 25MoI- enthält und in bekannter Weise durch direkte Mischprozent Einheiten von .^-ungesättigten Mono- polymerisation der Monomeren hergestellt worden ist. carbonsäuren, gegebenenfalls Einheiten eines misch- Nach dem Hauptpatent wird die Vernetzungsreakpolymerisierbaren, einfach ungesättigten dritten tion bei Bedingungen durchgeführt. 'veJche eine homo-Comonomeren enthält, und in bekannter Weise ao gene Verteilung des Vernetzungsmittels in der Mischdurch direkte Mischpolymerisation der Mono- polymerisat-Grundlage erlauben. Beispielsweise kann meren hergestellt worden ist, nach Patent 1 520 506, das Carboxylgruppen enthaltende Mischpolymerisat dadurch gekennzeichnet, daß man mit der Metallverbindung schmelzvermischt werden, das Vermischen des Mischpolymerisates mit der Aufgabe der Erfindung ist es, für das Verfahren Metallverbindung in einem Entgasungsextruder 25 des Hauptpatentes eine besonders vorteilhafte Verfahvornimmt. rensweise zum Schmelzvermischen des Carboxyl-
  2. 2. Verfahren nach Anspruch 1, dadurch gekenn- gruppen enthaltenden Mischpolymerisates mit der zeichnet, daß man bei einer Temperatur zwischen Metallverbindung zur Verfugung zu stellen.
    100 und 290 C und unter einem Druck von 7 bis Es wurde nämlich gefunden, daß das Vermischen
    700 kg/cm2 arbeitet. 30 besonders vorteilhaft vorgenommen werden kann,
  3. 3. Verfahren nach Anspruch 1 oder 2. dadurch wenn man das Mischpolymerisat mit der Mctallvergekennzeichnet, daß man die Metallverbindung bindung kontinuierlich in einem Entgasungsextruder in situ erzeugt, indem man eine im wesentlichen mischt.
    wasserunlösliche Metallverbindung in das ge- Das Vermischen wird vorzugsweise bei einer Tem-
    schmolzene Mischpolymerisat einmischt, dann 35 peratur zwicchen 100 und 290 C und einem Druck dieser geschmolzenen Masse eine Säurelösung ein- zwischen 7 bis 700 kg cm2 vorgenommen,
    verlernt und anschließend die Schmelze unter ver- Das Kationen bildende Material gibt man zum
    minderlem Druck von flüchtigen Bestandteilen Mischpolymerisat als wäßrige Lösung oder in einer befreit. im wesentlichen trockenen Form hinzu.
    40 Nach einer anderen Ausführungsform kann man
    die für das erfindungsgemäße Verfahren geeignete
    Metallverbindung auch in situ erzeugen, indem man eine im wesentlichen wasserunlösliche Metallverbin-
    Mischpolymerisate aus Äthylen oder anderen \-OIe- dung in das geschmolzene Mischpolymerisat cinfinen mit \,/?-ungesättigten Carbonsäuren sind be- 45 mischt, dann dieser geschmolzenen Masse eine Säurekannt. Aus der französischen Patentschrift 1 255 077 iösung einverleibt und anschließend die Schmelze ist es weiterhin bekannt, solche Mischpolymerisate unter vermindertem Druck von flüchtigen Bestandteilen mit Oxiden oder Hydroxiden von mehrwertigen Me- befreit. Zu solchen, im wesentlichen wasserunlöslichen tallen oder mit Säuresalzen von Metallen zu ver- Metallverbindungen, gehören beispielsweise Metallmischen, wodurch man eine Vernetzung der Poly- 50 oxyde, -hydroxyde und -carbonate. Zu geeigneten merisate erzielt. Verwendet man jedoch, wie dies in Säuren gehören beispielsweise Essigsäure, Milchsäure, der genannten französischen Patentschrift beschrieben Propionsäure und Mischungen dieser Säuren,
    wird, solche Mischpolymerisate aus Äthylen und Unter den angegebenen Temperatur- und Druck-
    \,/?-ungesättigten Carbonsäuren, welche durch Auf- bedingungen erhält man durch die Mischwirkung des pfropfen der \,/?-äthylenisch ungesättigten Carbon- 55 Extruders ein anscheinend einphasiges Gemisch und säure auf ein Polyolefin erhalten worden sind, so sind demzufolge einen gleichmäßigen Neutralisationsgrad, die erzielten Ergebnisse noch nicht voll befriedigend. Das Verfahren im Entgasungsextruder kann man in
    Insbesondere sind die mit den vorgenannten Metall- vier Stufen entsprechend vier Zonen einteilen. In der " verbindungen vernetzten Pfropfpolymerisate aus einem ersten Zone wird das Mischpolymerisat bei hohem Polyolefin und einer darauf aufgepfropften «,/?-äthy- 60 Druck gründlich gemischt und auf eine Temperatur lenisch ungesättigten Carbonsäure nicht durchsichtig, oberhalb seines Schmelzpunktes gebracht; das Katioso daß man aus diesen an sich in ihren rheologischen nen bildende Material kann in die erste Zone gegeben und weiteren physikalischen Eigenschaften verbesser- werden. In der zweiten Zone findet die Neutralisation ten Massen keine dickwandigen, durchsichtigen Kör- der Carbonsäuregruppen statt. Falls das Kationen per, wie Flaschen, dicke Folien u. dgl,, herstellen 65 bildende Material in der ersten Zone noch nicht zukann, gegeben worden ist, fügt man es in der zweiten Zone Gegenstand des Hauptpatentes 1 520 506 ist ein zu. Das Mischpolymerisat leitet man dann in fine Verfahren zum Modifizieren von Carboxylgruppen dritte Zone, in weicherein verminderter Druck herrscht,
DE1745939A 1961-08-31 1965-03-01 Verfahren zum Modifizieren von Carboxylgruppen enthaltenden Äthylenpolymeren Expired DE1745939C3 (de)

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US13514761A 1961-08-31 1961-08-31
US16883962A 1962-01-25 1962-01-25
US27147763 US3264272A (en) 1961-08-31 1963-04-08 Ionic hydrocarbon polymers
US34829364 US3404134A (en) 1961-08-31 1964-02-28 Process of crosslinking polymers

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DE1745939A1 DE1745939A1 (de) 1971-01-14
DE1745939B2 DE1745939B2 (de) 1973-07-19
DE1745939C3 true DE1745939C3 (de) 1974-02-21

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DE1962P0030096 Pending DE1520506B2 (de) 1961-08-31 1962-08-27 Verfahren zum modifizieren von carboxylgruppen enthaltenden aethylenpolymeren
DE1963P0031004 Pending DE1520518B2 (de) 1961-08-31 1963-01-24 Verfahren zur herstellung von modifizierten copolymerisaten aus ungesaettigten kohlenwasserstoffen und ungesaettigten carbonsaeuren
DE1520601A Granted DE1520601B2 (de) 1961-08-31 1964-04-08 Verfahren zum Modifizieren von Carboxylgruppen enthaltenden Äthylenpolymeren
DE1595112A Expired DE1595112C3 (de) 1961-08-31 1965-03-01 Verfahren zur Herstellung von modifizierten Copolymerisaten aus ungesättigten Kohlenwasserstoffen und ungesättigten Carbonsäuren
DE1965P0036183 Granted DE1745938B2 (de) 1961-08-31 1965-03-01 Verfahren zum modifizieren von carboxylgruppen enthaltenden aethylenpolymeren
DE1745939A Expired DE1745939C3 (de) 1961-08-31 1965-03-01 Verfahren zum Modifizieren von Carboxylgruppen enthaltenden Äthylenpolymeren

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DE1962P0030096 Pending DE1520506B2 (de) 1961-08-31 1962-08-27 Verfahren zum modifizieren von carboxylgruppen enthaltenden aethylenpolymeren
DE1963P0031004 Pending DE1520518B2 (de) 1961-08-31 1963-01-24 Verfahren zur herstellung von modifizierten copolymerisaten aus ungesaettigten kohlenwasserstoffen und ungesaettigten carbonsaeuren
DE1520601A Granted DE1520601B2 (de) 1961-08-31 1964-04-08 Verfahren zum Modifizieren von Carboxylgruppen enthaltenden Äthylenpolymeren
DE1595112A Expired DE1595112C3 (de) 1961-08-31 1965-03-01 Verfahren zur Herstellung von modifizierten Copolymerisaten aus ungesättigten Kohlenwasserstoffen und ungesättigten Carbonsäuren
DE1965P0036183 Granted DE1745938B2 (de) 1961-08-31 1965-03-01 Verfahren zum modifizieren von carboxylgruppen enthaltenden aethylenpolymeren

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NL288151A (de) 1900-01-01
DE1745938C3 (de) 1974-02-21
GB1034268A (en) 1966-06-29
DE1520506B2 (de) 1971-06-09
DE1520518B2 (de) 1971-07-22
DE1745939A1 (de) 1971-01-14
DE1745938A1 (de) 1971-01-14
DE1520601A1 (de) 1970-05-14
DE1745939B2 (de) 1973-07-19
SE311229B (de) 1969-06-02
NL128027C (de) 1900-01-01
DE1520601B2 (de) 1973-01-04
BE627537A (de) 1900-01-01
FR1430478A (fr) 1966-03-04
US3404134A (en) 1968-10-01
GB1063436A (en) 1967-03-30
DK125713B (da) 1973-03-26
CH445861A (de) 1967-10-31
NL129542C (de) 1900-01-01
US3264272A (en) 1966-08-02
DE1595112A1 (de) 1970-04-09
DE1520506A1 (de) 1970-02-19
SE303882B (de) 1968-09-09
NL282755A (de) 1900-01-01
GB1011981A (en) 1965-12-01
DE1595112B2 (de) 1973-07-05
DE1520518A1 (de) 1969-07-03
DE1595112C3 (de) 1974-03-14
GB1029035A (en) 1966-05-11
DE1745938B2 (de) 1973-07-19
CH435741A (de) 1967-05-15
BE621846A (de) 1900-01-01

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E77 Valid patent as to the heymanns-index 1977