DE903033C - Verfahren zum Polymerisieren ungesaettigter Verbindungen in waesserigem Medium - Google Patents

Verfahren zum Polymerisieren ungesaettigter Verbindungen in waesserigem Medium

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Publication number
DE903033C
DE903033C DEN4611A DEN0004611A DE903033C DE 903033 C DE903033 C DE 903033C DE N4611 A DEN4611 A DE N4611A DE N0004611 A DEN0004611 A DE N0004611A DE 903033 C DE903033 C DE 903033C
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DE
Germany
Prior art keywords
aqueous phase
monomer
aqueous
compounds
emulsion
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
DEN4611A
Other languages
English (en)
Inventor
Christiaan Pieter Von Dijk
Johannes Fredericus Franciscus
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.)
Bataafsche Petroleum Maatschappij NV
Original Assignee
Bataafsche Petroleum Maatschappij NV
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
Priority claimed from NL158468A external-priority patent/NL75375C/xx
Application filed by Bataafsche Petroleum Maatschappij NV filed Critical Bataafsche Petroleum Maatschappij NV
Application granted granted Critical
Publication of DE903033C publication Critical patent/DE903033C/de
Expired legal-status Critical Current

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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/24—Stationary reactors without moving elements inside
    • B01J19/2415—Tubular reactors
    • B01J19/2435—Loop-type reactors
    • 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
    • C08F14/00—Homopolymers and 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 a halogen
    • C08F14/02—Monomers containing chlorine
    • C08F14/04—Monomers containing two carbon atoms
    • C08F14/06—Vinyl chloride
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    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F2/00—Processes of polymerisation
    • C08F2/12—Polymerisation in non-solvents
    • C08F2/16—Aqueous medium
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    • C08F2/00—Processes of polymerisation
    • C08F2/12—Polymerisation in non-solvents
    • C08F2/16—Aqueous medium
    • C08F2/22—Emulsion polymerisation
    • C08F2/24—Emulsion polymerisation with the aid of emulsifying agents
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    • C08F36/00—Homopolymers and copolymers of compounds having one or more unsaturated aliphatic radicals, at least one having two or more carbon-to-carbon double bonds
    • C08F36/02—Homopolymers and copolymers of compounds having one or more unsaturated aliphatic radicals, at least one having two or more carbon-to-carbon double bonds the radical having only two carbon-to-carbon double bonds
    • C08F36/04—Homopolymers and copolymers of compounds having one or more unsaturated aliphatic radicals, at least one having two or more carbon-to-carbon double bonds the radical having only two carbon-to-carbon double bonds conjugated
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Description

  • Verfahren zum Polymerisieren ungesättigter Verbindungen in wässerigem Medium Das Patent 891 7.16 bezieht sich auf ein Verfahren zum Polymerisieren ungesättigter V erbindungen in wässerigem Medium, gemäß welchem ein Strom von Tropfen der zu polymerisierenden Verbindung bzw. Verbindungen durch die wässerige Phase geführt und die Bewegung der Mononiertropfen gegenüber der wässerigen Phase hauptsächlich. durch den Unterschied im spezifischen Gewicht der beiden Phasen herbeigeführt wird. Die Tropfen des Monomers, die sich durch die wässerige Phase hindurchbew egt haben, trennen sich von dieser ab. Das in dieser Weise gesammelte Monomer wird im allgemeinen außerhalb der mit der Wasserphase gefüllten Kammer zur Beschickungsstelle zurückgeleitet. Zweckmäßig wird in der wässerigen, Phase keinerlei Rühren durch irgendwelche mechanischen Mittel durchgeführt.
  • Bei dem vorliegenden verbesserten Verfahren liegt die getrennte Phase der zu polymerisierenden Verbindung bzw. Verbindungen nicht nur in dem Strom größerer Tropfen. vor, die sich durch die Wasserphase, hindurchbewegen, sondern, auch in emulgierten Tropfen, welche Durchmesser von. der Größenordnung von o,i bis o,ooz mm und weniger aufweisen. Außerdem wird, die, Menge des Monomers vorzugsweise ganz oder teilweise ergänzt, in. dem man, eine Emulsion von Monomer in Wasser zuführt, in welcher die Durchmesser der Monomertropfen von der Größenordnung von o,i bis o,ooi mm und weniger sind.
  • Der hier verwendete Begriff Monomer umfaßt auch Fälle, in welchen verschiedene Monomere vorliegen oder zugeführt werden und! das Produkt derselben ein Mischpolymerisat darstellt.
  • Bei dem Verfahren nach dem Patent 8g-1 746 dient der Kreislauf des MonomeTs; drei Zwecken.: Ergänzung des verbrauchten Monomer's, Kühlen und Rühren. Um ein Polymer von hohem Molgewicht zu erhalten, ist es erforderlich, die Konzentration dies in der wässerigen Phase gelösten. Mono mers auf einen. hohen Wert zu bringen und infolgedeis.sen auch die Geschwindigkeit der Diffusion des Monomers aus der Monomerphase in die wässerige Phase zu steigern. Wann man nach dem Patent 891 746 arbeitet, muß man zur Erzielung dieser Ergebnisse eine große, Menge Monomer je Volumeinheit der wässerigen Phase und je Zeiteinheit im Umlauf halten; in vielen Fällen ist dies eine größere Menge, als für die Zwecke des Kühleras, oder Rührens erforderlich wäre.
  • Nach der verbesserten und bevorzugt angewendeten Arbeitsweise wird die ersterwähnte Funktion vollständig oder teilweise von zugefügtem Mono mar übernommen, das bereits in Wasser emulgiert ist. Auf diese: Weise kann man das Malgewicht des: gebildeten Polymers, unabhängig machen von der Menge des im Kreislauf befindlichen Monomers. Die Ergänzung des Monomers und das Kühlen können dann völlig unabhängig voneinander geregelt werden. Außerdem sind keine Umlaufpumpen von sehr großer Kapazität erforderlich.
  • Vorzugsweise wird das als Emulsion zugeführte Monomer in feindispergierter Form angewandt. Je, feiner die Dispergierung des emu,lgierten: Monomers. ist, um so weniger neigt es zur Abscheidung. Eine stabile Emulsion hat keine schädli@cha Wirkung auf die Abtrennung des Monomers, welches die wässerige Phase in großen Tropfen durchströmt- Außerdenn fördert eine feine Dispergierung die D,ifffus'io.n. ganz beträchtlich. Es isst also ratsam, Emulsionen zu verwenden, die durch gemeinsames Verrühren des Monomers mit einer solchen Menge einer konzentrierten Emulgatorlösung, daß eine gelatinöse Masse entsteht, die dann mit Wasser verdünnt wird, entstanden sind. Die Durchmesser der Monomertropfen, in den: vorzugsweise verwendeten Monomeremulsionen liegen in der Größenordnung von o.oi bis o,ooi mm.
  • Beispiel Die Polymerisation von Vinylidenchlorid wurde in einem zylindrischen Gefäß durchgeführt, dessen Höhe 6o cm und dessen Durchmesser 5,5 cm betrug. 425 ccm Vinylidenchlorid wurden ih, das Ge@-fäß gebracht und außerdenn iooo ccm einer wäsiserigen Phase, die, 0,5"/& Emulgator (das Produkt, welches erhalten wird durch Behandlung gesättigter aliphatiseher Kohlenwasserstoffe, die io bis 2o Kohlensto@ffatome enthalten, mit Schwefeldioxyd und Chlor und nachfolgende alkalische Versaifung der so gebildeten Sulfochloride), o,5 % Ammoniumpersulfat, o,250/9 Na. S 03 und o,25 % NaH C 03 enthielt. Nachdem der Inhalt des Reaktion:sge,-fäßes auf eine Temperatur von 28° gebracht worden war, wurde Vinylidench:lo,rid durch ein Rohr von 6 mm Durchmesser mit einer Geschwindigkeit von 4. Liter je Stunde am oberen Ende des Reaktionsgefäßes eingeführt. Dieses Monomer sank durch die wässerige Phase in; Tropfen mit i bis 5 mm Durchmesser und schied sich am Boden aus der wässemigen Phase ab. Dasi Monomer wurde vom Boden: dösi Reaktionsgefäßes zum oberen Ende; zurückgeführt.
  • Am unteren Ende der Wassersäule, wurden je Stunde 26o ccm einer o,8o/oigen wässerigen Ammoniumparsulfatlösung und 26o ccm einer Monomeremulsion eingeführt. Die Monomeremulsion wurde in der in obiger Beschreibung anvähnten Weise hergestellt, wobei zuerst eine gelatinöse Masse erhalten wurde. Die Zusammensatzung der Emulsion in; Gewichtsprozent war 4o 0/a Vihylidenchlorid, 0,8'/01 Emulgator, 0,4 % Nag S 03, o,4 % Na H C 03, 58,4 0% Wasser. Am oberen Ende das Reaktions@ gefäßes wurde so viel wässerige Phase abgeleitet, daß das Volumen konstant blieb.
  • Durch Kühlen des im Kreislauf geführten Monomers wurde die Temperatur auf 28 ± i0 gehalten. Nachdem das GleichgeRvicht erreicht Zwar, wurde festgestellt, daß die durchschnittliche Polymerisationsgeschwindigkeit 9o g ja Liter der Dispersion je; Stunde betrug und die abgezogene Suspension 1.8 Gewichtsprozent Polymer enthielt. Es ergab sich, daß die Menge des in großen Tropfern: umgeführten Monomers sich während i6 S''tund'ennicht merkbar geändert hatte.
  • Zum Vergleich wurde ein Versuch durchgeführt, bei welchem keine Emulsion eingeleitet wurde, sondern das! verbrauchte Monomer im Kreislaufkanal ergänzt wurde. Jede Stunde wurden 5oo ccm einer Lösung von gleicher Zusammensetzung wie die ursprüngliche Wasserphase am unteren; Ende in die Wassersäule eingeführt. Es wurde gefunden, daß bei denn hierbei erreichten Gleichgewicht die durchschnittliche Polymerisationsgeschwindigkeit igg je Liter Dispersion je Stunde betrug und die abgezogene Suspension etwa 4 Gewichtsprozent Polymer enthielt.

Claims (3)

  1. PATEN TANSPRIJCIIE: i. Verfahren zum Polymerisieren ungesättigter Verbindungen in wässerigem Medium unter Bildung stabiler Polymerdispersionen, bei welchem ein Strom von Tropfen der zu polymerisierenden Verbindung bzw. Verbindungen! durch die wässerige Phase geführt und die Bewegung der Monomertropfen gegenüber der wässerigen Phase hauptsächlich durch diei Differenz im spezifischen; Gewicht der, beiden. Phasen verursacht wird, nach Patenft 891 746, dadurch gekennzeichnet, dä,ß die getrennte Phase der zu polymerisierendem. Verbindung bzw. Verbindungen nicht nur in Form eines Stromes größerer Tropfen, welche durch die wässerige Phase hindurchströmen, vorliegt, sondern, auch in Foren emulgierter Tropfen von der Größenordnung zwischen o,z und. o,oor mm und, darunter.
  2. 2. Verfahren nach Anspruch r, dadurch gekennzeichnet, daß die Polymerisation in einem mit der wässerigen Phase gefüllten Gefäß durchgeführt wird, in welchem die! Bewegung nicht mit mechanischen Vorrichtungen erzielt wird und in welchem das durch die wässerige Phase hindurchgeführte Monomer, nachdem es von der wässerigen Phase abgetrennt worden ist, zu der Stelle zurückgeführt wird, an welcher es, seinen Weg durch die wässerige Phase begann, dadurch gekennzeichnet, d'aß das, Monomer ganz oder teilweise durch Zugabe einer wässerigen Emulsion des Monomers zu der wässerigen Phase ergänzt wird.
  3. 3. Verfahren nach Anspruch 2, dadurch ge- kennzeichnet, daß die zuzusetzende Emulsion hergestellt wird durch Zusammenrühren des Monomers mit einer solchen Menge einer konzentrieTtenv Emulgatorläsung, daß eine gelatiinöse Masse gebildet wird, und Verdünnen dieser Masse mit Wasser.
DEN4611A 1949-12-27 1951-10-25 Verfahren zum Polymerisieren ungesaettigter Verbindungen in waesserigem Medium Expired DE903033C (de)

Applications Claiming Priority (7)

Application Number Priority Date Filing Date Title
NL150701A NL73983C (nl) 1949-12-27 1949-12-27 Werkwijze voor het polymeriseren van onverzadigde verbindingen, in water geëmulgeerd.
NL150701 1949-12-27
NL156888A NL77633C (nl) 1949-12-27 1950-10-27 Werkwijze voor het polymeriseren van onverzadigde verbindingen in water geëmulgeerd.
NL158181 1950-12-27
NL158468A NL75375C (nl) 1951-01-10 1951-01-10 Werkwijze voor het polymeriseren van alkenisch onverzadigde verbindingen in waterig milieu
NL508461X 1951-01-17
FR1060769T 1951-10-25

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DEN3304A Expired DE891746C (de) 1949-12-27 1950-12-23 Verfahren zur Emulsionspolymerisation ungesaettigter Verbindungen
DEN4611A Expired DE903033C (de) 1949-12-27 1951-10-25 Verfahren zum Polymerisieren ungesaettigter Verbindungen in waesserigem Medium
DEN4612A Expired DE900737C (de) 1949-12-27 1951-10-26 Schmierfette und Verfahren zu ihrer Herstellung

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BE (3) BE500275A (de)
CH (1) CH295070A (de)
DE (3) DE891746C (de)
ES (2) ES195939A1 (de)
FR (3) FR1060769A (de)
GB (2) GB687984A (de)
NL (4) NL73983C (de)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1083054B (de) * 1957-07-26 1960-06-09 Hoechst Ag Verfahren zur Herstellung von fuer Pasten geeigneten Polymerisaten oder Mischpolymerisaten des Vinylchlorids
DE1240286B (de) * 1965-01-02 1967-05-11 Basf Ag Verfahren zur kontinuierlichen Emulsions-polymerisation olefinisch ungesaettigter Verbindungen

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Publication number Priority date Publication date Assignee Title
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DE1240286B (de) * 1965-01-02 1967-05-11 Basf Ag Verfahren zur kontinuierlichen Emulsions-polymerisation olefinisch ungesaettigter Verbindungen
DE1255926B (de) * 1965-01-02 1975-06-12 Badische Anilin- S. Soda-Fabrik Aktiengesellschaft, Ludwigshafen/Rhein Verfahren zur kontinuierlichen Emulsionspolymerisation olefinisch ungesättigter Verbindungen

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FR1044161A (fr) 1953-11-16
GB705325A (en) 1954-03-10
DE900737C (de) 1954-01-04
ES200136A2 (es) 1951-12-01
BE508461A (fr) 1952-01-31
CH295070A (de) 1953-12-15
BE506666A (fr) 1951-11-14
FR1060769A (fr) 1954-04-06
NL76240C (nl) 1954-10-15
GB687984A (en) 1953-02-25
NL77633C (nl) 1955-04-15
DE891746C (de) 1953-10-01
NL77634C (nl) 1955-04-15
US2716641A (en) 1955-08-30
BE500275A (fr) 1951-01-15
FR63135E (fr) 1955-08-24
NL73983C (nl) 1954-01-15
ES195939A1 (es) 1952-06-16

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