DE1745939B2 - Verfahren zum modifizieren von carboxylgruppen enthaltenden aethylenpolymeren - Google Patents
Verfahren zum modifizieren von carboxylgruppen enthaltenden aethylenpolymerenInfo
- Publication number
- DE1745939B2 DE1745939B2 DE1965P0036184 DEP0036184A DE1745939B2 DE 1745939 B2 DE1745939 B2 DE 1745939B2 DE 1965P0036184 DE1965P0036184 DE 1965P0036184 DE P0036184 A DEP0036184 A DE P0036184A DE 1745939 B2 DE1745939 B2 DE 1745939B2
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- Prior art keywords
- acid
- copolymer
- metal
- mixing
- zone
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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
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- 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
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- 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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- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- 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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- 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
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S36/00—Boots, shoes, and leggings
- Y10S36/02—Plastic
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- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S428/00—Stock material or miscellaneous articles
- Y10S428/91—Product with molecular orientation
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- 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
- 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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- 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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- 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]
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- 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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- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/31504—Composite [nonstructural laminate]
- Y10T428/31678—Of metal
- Y10T428/31692—Next to addition polymer from unsaturated monomers
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- 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
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/31504—Composite [nonstructural laminate]
- Y10T428/31855—Of addition polymer from unsaturated monomers
- Y10T428/31938—Polymer of monoethylenically unsaturated hydrocarbon
Description
Bndin vrelcher die flüchtigen Materialien, z. B. Wasser
und Sätie (die sieh 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 gegenübej:
dem Verfahren unter Verwendung eines Kautschukmahlwerkes liegt in der größeren Gleichmäßigkeit
der Endprodukte und der viel kürzeren Reaktionszeit
Beispiele 1 bis 8
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 Mischabschnitt, wie er in der USA.-Patentschrift 3006029 beschrieben
ist und der 13,5mal so lang ist wie der Durchmesser, einem Drosselring, der es erlaubt, in dem Mischabschnitt einen Druck aufrechtzuerhalten, (einem Entga&ungsabschnitt,
der 5mal so lang ist wie der Durchmesser und 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/cm*. 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
ao Wasser und granuliert ihn.
Die einzelnen Arbeitsweisen, die eingesetzten Reagentien und einige der beeinflußten Polymerisateigenschaften
sind in Tabelle I angegeben.
·' | 6 | Saures | Mischpolymerisat | Steifig | Metall verbindung | Zu- führungs- |
Säurelösung | Typ | wäßrige | Zu- führungs- |
Pro- duktions- |
Produkt | Steifig | |
Bei spiel |
Meth acryl |
Schmelz | keit, | geschwin- | lösung | geschwin- | geschwin- | Schmelz | keit, | |||||
säure, | index, | Typ | digkeit | Volum | digkeit | digkeit | index, | |||||||
Gewichts | kg/cm* | kg/Std. | Propion | prozent | cm'/Min. | kg/Std. | kg/cm* | |||||||
1 | 7 ' | prozent | g/10 Min. | 361,3 | 0,363 | säure | 50 | 5,29 | 7,48 | g/10Min. | 3139,7 | |||
15 | 71 | ZnO | Essig | 11,52 | ||||||||||
2 | 8 < | 861,3 | 0,476 | säure | 100 | 6,0 | 8,39 | 3689,8 | ||||||
15 | 71 | ZnO | Meth | 0,28 | ||||||||||
3 | 861,3 | 0,676 | acryl | 60 | 9,17 | 7,94 | 3779,4 | |||||||
15 | 71 | ZnO | säure | 0,19 | ||||||||||
Milch | ||||||||||||||
4 | 861,3 | 0,535 | säure*) | 60 | 5,85 | 7,17 | 4241,9 | |||||||
15 | 71 | ZnO | Essig | 0,29 | ||||||||||
5 | 1705,0 | 0,508 | säure | 50 | 5,22 | 9,98 | 3728,8 | |||||||
15,3 | 6,3 | ZnO | Isopro- | 0,13 | ||||||||||
panol | 25 | |||||||||||||
Heptan- | ||||||||||||||
1705,0 | 0,485 | säure | 61,9 | 9,0 | 9,98 | 3168,1 | ||||||||
15,3 | 6,3 | ZnO | Essig | 0,16 | ||||||||||
säure | 22,7 | |||||||||||||
Essig- : | ||||||||||||||
— | 0,404 | säure | 50 | 4,83 | 8,66 | 64 | — | |||||||
10**) | 90 | ZnO | Essig | 2,46 | ||||||||||
— | 0,163 | säure | 50 | 5,5 | 6,12 | — | ||||||||
9***) | 178 | ZnO | 25 | |||||||||||
*) Die Milchsäure löst ZnO unter den Reaktionsbedingungen nicht vollständig. Ein weiteres Mischen ergibt eine vollständige Lösung.
**) Terpolymerisat aus 67% Äthylen, 24% Vinylacetat und 10% Methacrylsäure.
***) Terpolymerisat aus 70% Äthylen, 20 V0 Vinylacetat und 90% Methacrylsäure. ■;
Beispiele 9 bis 16
In die Zuführungsöffnung 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-Diphosphait
ails 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 2800C gehalten. Dort findet die Reak-
tion der Polymerisatschmelze unter Neutralisation der
Säuregruppen statt
'■■ Hinter dem Mischabsehnitt wild die Masse, die aus
ionisch vernetztem Mischpolymerisat und aus Neben· produkten besteht, die sich infolge der Umsetzung ge- S
bildet haben, durch ein Druck-Lenkungsventil und ein Rohr in den Entgasungsabschnitt geleitet« der einen
Durchmesser von 5 ein hat. Die Temperatur der Masse
vor äem Ventil beträgt 2800G und der Druck 52,7 kg/
cm1. Im Entgasungsabschnitt sind zwei Entgasung?-
zoaen, wobei jede etwa 4mal so lang wie der Durchmesser
ist In der ersten Entgasungszone hält man ein
Vakuum von 686 und in 4er zweiten eins von 711 mm
Hg aufrecht Die Temperatur der SchmaJae hält man
zwischen 270 und 280° G In der Entgasjingszone werden
die flüchtigen Bestandteile aus dem geschmolzenen, durch Ionen vernetzten Mischpolymerisat entfernt.
Das anschließend in Form von Strategen extrudierte
Polymerisat kühlt man in Wasser und granuliert
es.
Die einzelnen Arbeitebedingungenj 4ie eingesetzten
Reagentien und einige der beeinflußten Polymerisateigenschaften
ersieht man aus der nachstehend angeführten Tabelle Π.
Methacrylsäure-MischpoI/merisat | S·) | Steifigkeit, |
Misch
polymerisat, |
Vorgernisch | ZnO | Teile | Stabilisator | Z*·) | |
Beispiel |
Säure,
Gewichts |
kg/cm1 | teile | Metall verbindung | Mg(OH8) | teile | |||
prozent | 45 | 843,7 | Typ | Mg(C2H3O2), ■ | 4,54 | 0,80 | |||
9 | 9,5 | 45 | 843,7 | 8,74 | 4H2O | 4,20 | 0,14 | 1,41 | |
10 | 9,5 | Mg(OH2) | |||||||
Mg(C8H8O2), · | 4,54 | ||||||||
45 | 843,7 | 8,74 | 4H„O | 4,20 | 0,14 | 1,11 | |||
11 | 9,5 | ZnO | |||||||
Mg(OH)2 | 9,08 | ||||||||
45 | 843,7 | 9,08 | Mg(C4H3O1), ■ | 5,0 | 0,15 | 1,39 | |||
12 | 9,5 | 5t9 | 1293,6 | 7,5 | 4H2O | 0,20 | 1,43 | ||
13 | 11,7 | LiOH · H8O | |||||||
ZnO | 4,41 | ||||||||
4,3 | 984,3 | 8,64 | Mg(OH)2 | 4,23 | 0,07 | 0,75 | |||
14 | 9,5 | Mg(CaH,O2)2 · | 4,54 | ||||||
6,3 | 1705,0 | 8,74 | 4H8O | 0,14 | 0,95 | ||||
15 | 15,3 | LiOH · H8O | |||||||
ZnO | 4,41 | ||||||||
6,3 | 1705,0 | 8,64 | 0,07 | 0,79 | |||||
16 | 15,3 | ||||||||
(Fortsetzung)
wäßrige Lösung Von | Säure | Z**·) |
Geschwindig
keit |
Produkt | Steifigkeit, | |
Beispiel | Essigsäure | Volumprozent | 13,8 | kg/Std. | kg/cms | |
Essigsäure | 40 | 13,0 | 24,9 | * I | 2573,2 | |
9 | rissigsäure | 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 | |||||
Claims (3)
1. Verfahren zum Modifizieren von Carboxyl- düngen, deren Nichtmetallrest mit dem Wasserstoffgruppen
enthaltenden Äthylenpolymeren durch 5 atom aus der Carbonsäure bei Reaktionsbedingungen
homogenesVermischenderPolymerisatemitsolchen 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 Äthylenpolymerisat 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 Carb1- i '.Prozent Ätbyleneinhjeiteii und 0,2 bis 25 Molprozent
oxylgruppen enthaltendes Äthylenpolymerisat ein Einheiten von ajS-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 MolprozentÄthyleneinheitenund 0,2 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 Vernetzungsreakpolymeriaierbaren,
einfach ungesättigten dritten tion bei Bedingungen durchgeführt, welche eine-homo-Comonomeren
enthält, und in bekannter Weise 20 gene Verteilung des Vernetzungsmittels in der Mischdurch
direkte Mischpolymerisation der Mono- polymerisat-Grundlage erlauben. Beispielsweise kann
meren hergestellt worden ist, nach Patent 1520 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 Schmelzvennischen des Carboxyl-
2. Verfahren nach Anspruch 1, dadurch gekenn- gruppen enthaltenden Mischpolymerisates mit der
zeichnet, daß man bei einer Temperatur zwischen Metallverbindung zur Verfügung 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. Verfahren nach Anspruch 1 oder 2, dadurch wenn man das Mischpolymerisat mit der Metallvergekennzeichnet,
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 zwischen 100 und 290° C und einem Druck
dieser geschmolzenen Masse eine Säurelösung ein- zwischen 7 bis 700 kg/cm* vorgenommen,
verleibt und anschließend die Schmelze unter ver- Das Kationen bildende Material gibt man zum
minderten! 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 α-Öle- dung in das geschmolzene Mischpolymerisat ein-
;finen mit α,/9-ungesättigten Carbonsäuren sind be- 45 mischt, dann dieser geschmolzenen Masse eine Säurekannt.
Aus der französischen Patentschrift 1 255 077 lösung 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- S'ö 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- <%,/J-ungesättigten Carbonsäuren, welche durch Auf- r bedingungen erhält man durch die Mischwirkung des pfropfen der α,/3-äthylenisch ungesättigten Carbon*·''^'Extruders ein anscheinend einphasiges Gemiseh und säure auf ein Polyolefin erhalten worden sind, s,o 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 α,/9-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 Theologischen 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 I 520 506 ist ein zu. Das Mischpolymerisat leitet man dann in eine Verfahren zum Modifizieren von Carboxylgruppen dritte Zone, in welcher ein verminderter Druck herrscht,
wird, solche Mischpolymerisate aus Äthylen und Unter den angegebenen Temperatur- und Druck- <%,/J-ungesättigten Carbonsäuren, welche durch Auf- r bedingungen erhält man durch die Mischwirkung des pfropfen der α,/3-äthylenisch ungesättigten Carbon*·''^'Extruders ein anscheinend einphasiges Gemiseh und säure auf ein Polyolefin erhalten worden sind, s,o 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 α,/9-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 Theologischen 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 I 520 506 ist ein zu. Das Mischpolymerisat leitet man dann in eine Verfahren zum Modifizieren von Carboxylgruppen dritte Zone, in welcher ein verminderter Druck herrscht,
Applications Claiming Priority (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
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 |
Publications (3)
Publication Number | Publication Date |
---|---|
DE1745939A1 DE1745939A1 (de) | 1971-01-14 |
DE1745939B2 true DE1745939B2 (de) | 1973-07-19 |
DE1745939C3 DE1745939C3 (de) | 1974-02-21 |
Family
ID=27495141
Family Applications (6)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
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 |
DE1745939A Expired DE1745939C3 (de) | 1961-08-31 | 1965-03-01 | Verfahren zum Modifizieren von Carboxylgruppen enthaltenden Äthylenpolymeren |
DE1965P0036183 Granted DE1745938B2 (de) | 1961-08-31 | 1965-03-01 | Verfahren zum modifizieren von carboxylgruppen enthaltenden aethylenpolymeren |
Family Applications Before (4)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
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 |
Family Applications After (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
DE1965P0036183 Granted DE1745938B2 (de) | 1961-08-31 | 1965-03-01 | Verfahren zum modifizieren von carboxylgruppen enthaltenden aethylenpolymeren |
Country Status (9)
Country | Link |
---|---|
US (2) | US3264272A (de) |
BE (2) | BE627537A (de) |
CH (2) | CH445861A (de) |
DE (6) | DE1520506B2 (de) |
DK (1) | DK125713B (de) |
FR (1) | FR1430478A (de) |
GB (4) | GB1011981A (de) |
NL (4) | NL129542C (de) |
SE (2) | SE311229B (de) |
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US2646425A (en) * | 1953-07-21 | Ereparation of ethylene polymers | ||
US2607762A (en) * | 1948-12-07 | 1952-08-19 | Monsanto Chemicals | Dry process manufacture of watersoluble derivatives of styrenemaleic anhydride type heteropolymers |
US2757153A (en) * | 1949-12-14 | 1956-07-31 | Monsanto Chemicals | Process for water-soluble styrenemaleic anhydride derivatives |
US2599123A (en) * | 1950-08-18 | 1952-06-03 | Du Pont | Copolymers of ethylene with an alkyl acrylate and an alkyl monoester of a butene-1,4-dioic acid |
US2798053A (en) * | 1952-09-03 | 1957-07-02 | Goodrich Co B F | Carboxylic polymers |
US2757106A (en) * | 1953-05-28 | 1956-07-31 | Rohm & Haas | Coated paper products and method of making |
DE1016228B (de) * | 1955-09-06 | 1957-09-26 | Monsanto Chemicals | Verfahren zum Schlichten von Polyamidfaeden oder -garnen |
US2999056A (en) * | 1956-10-04 | 1961-09-05 | Du Pont | Irradiation bonding of acidic compounds to shaped polymeric structures |
US3132120A (en) * | 1961-02-03 | 1964-05-05 | Du Pont | Method for the preparation of ethylene copolymers |
NL128027C (de) * | 1961-08-31 | 1900-01-01 |
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- 1965-03-01 DE DE1745939A patent/DE1745939C3/de not_active Expired
- 1965-03-01 DE DE1965P0036183 patent/DE1745938B2/de active Granted
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BE627537A (de) | 1900-01-01 |
SE303882B (de) | 1968-09-09 |
FR1430478A (fr) | 1966-03-04 |
DK125713B (da) | 1973-03-26 |
DE1745939A1 (de) | 1971-01-14 |
DE1595112C3 (de) | 1974-03-14 |
DE1745939C3 (de) | 1974-02-21 |
NL288151A (de) | 1900-01-01 |
CH445861A (de) | 1967-10-31 |
SE311229B (de) | 1969-06-02 |
NL128027C (de) | 1900-01-01 |
DE1520518B2 (de) | 1971-07-22 |
NL129542C (de) | 1900-01-01 |
US3264272A (en) | 1966-08-02 |
GB1063436A (en) | 1967-03-30 |
DE1595112B2 (de) | 1973-07-05 |
DE1520506B2 (de) | 1971-06-09 |
GB1011981A (en) | 1965-12-01 |
BE621846A (de) | 1900-01-01 |
GB1029035A (en) | 1966-05-11 |
GB1034268A (en) | 1966-06-29 |
DE1520506A1 (de) | 1970-02-19 |
DE1520518A1 (de) | 1969-07-03 |
CH435741A (de) | 1967-05-15 |
DE1745938B2 (de) | 1973-07-19 |
DE1595112A1 (de) | 1970-04-09 |
US3404134A (en) | 1968-10-01 |
DE1520601A1 (de) | 1970-05-14 |
DE1745938A1 (de) | 1971-01-14 |
DE1520601B2 (de) | 1973-01-04 |
NL282755A (de) | 1900-01-01 |
DE1745938C3 (de) | 1974-02-21 |
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