DE947736C - Process for the production of polyvinyl compounds - Google Patents
Process for the production of polyvinyl compoundsInfo
- Publication number
- DE947736C DE947736C DEC10431A DEC0010431A DE947736C DE 947736 C DE947736 C DE 947736C DE C10431 A DEC10431 A DE C10431A DE C0010431 A DEC0010431 A DE C0010431A DE 947736 C DE947736 C DE 947736C
- Authority
- DE
- Germany
- Prior art keywords
- compounds
- polymerization
- vinyl compounds
- monomeric vinyl
- production
- 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
- 150000001875 compounds Chemical class 0.000 title claims description 6
- 229920002554 vinyl polymer Polymers 0.000 title claims description 6
- 238000004519 manufacturing process Methods 0.000 title claims description 3
- 238000000034 method Methods 0.000 title claims description 3
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 12
- 238000006116 polymerization reaction Methods 0.000 claims description 10
- 229920002545 silicone oil Polymers 0.000 claims description 9
- 239000003054 catalyst Substances 0.000 claims description 6
- 239000007900 aqueous suspension Substances 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 3
- 238000013019 agitation Methods 0.000 claims description 2
- 229920000642 polymer Polymers 0.000 description 11
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 8
- 238000003756 stirring Methods 0.000 description 5
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 description 4
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 4
- 229960003328 benzoyl peroxide Drugs 0.000 description 4
- 150000002484 inorganic compounds Chemical class 0.000 description 4
- 229910010272 inorganic material Inorganic materials 0.000 description 4
- 125000004430 oxygen atom Chemical group O* 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 239000004342 Benzoyl peroxide Substances 0.000 description 3
- 235000019400 benzoyl peroxide Nutrition 0.000 description 3
- 239000001506 calcium phosphate Substances 0.000 description 3
- 238000000354 decomposition reaction Methods 0.000 description 3
- 229920001296 polysiloxane Polymers 0.000 description 3
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical class [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000010557 suspension polymerization reaction Methods 0.000 description 2
- 235000019731 tricalcium phosphate Nutrition 0.000 description 2
- 229940078499 tricalcium phosphate Drugs 0.000 description 2
- 229910000391 tricalcium phosphate Inorganic materials 0.000 description 2
- -1 vinyl compound Chemical class 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- OEPOKWHJYJXUGD-UHFFFAOYSA-N 2-(3-phenylmethoxyphenyl)-1,3-thiazole-4-carbaldehyde Chemical compound O=CC1=CSC(C=2C=C(OCC=3C=CC=CC=3)C=CC=2)=N1 OEPOKWHJYJXUGD-UHFFFAOYSA-N 0.000 description 1
- FRIBMENBGGCKPD-UHFFFAOYSA-N 3-(2,3-dimethoxyphenyl)prop-2-enal Chemical compound COC1=CC=CC(C=CC=O)=C1OC FRIBMENBGGCKPD-UHFFFAOYSA-N 0.000 description 1
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 1
- 239000005995 Aluminium silicate Substances 0.000 description 1
- HIBWGGKDGCBPTA-UHFFFAOYSA-N C=CC1=CC=CC=C1.C=CC1=CC=CC=C1 Chemical class C=CC1=CC=CC=C1.C=CC1=CC=CC=C1 HIBWGGKDGCBPTA-UHFFFAOYSA-N 0.000 description 1
- 108010010803 Gelatin Proteins 0.000 description 1
- YIVJZNGAASQVEM-UHFFFAOYSA-N Lauroyl peroxide Chemical compound CCCCCCCCCCCC(=O)OOC(=O)CCCCCCCCCCC YIVJZNGAASQVEM-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 229920002125 Sokalan® Polymers 0.000 description 1
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical compound ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 125000005396 acrylic acid ester group Chemical group 0.000 description 1
- 239000012190 activator Substances 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 235000012211 aluminium silicate Nutrition 0.000 description 1
- 229910052586 apatite Inorganic materials 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- 235000011010 calcium phosphates Nutrition 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- LSXWFXONGKSEMY-UHFFFAOYSA-N di-tert-butyl peroxide Chemical compound CC(C)(C)OOC(C)(C)C LSXWFXONGKSEMY-UHFFFAOYSA-N 0.000 description 1
- 239000012969 di-tertiary-butyl peroxide Substances 0.000 description 1
- WMWXXXSCZVGQAR-UHFFFAOYSA-N dialuminum;oxygen(2-);hydrate Chemical class O.[O-2].[O-2].[O-2].[Al+3].[Al+3] WMWXXXSCZVGQAR-UHFFFAOYSA-N 0.000 description 1
- SRXOCFMDUSFFAK-UHFFFAOYSA-N dimethyl peroxide Chemical group COOC SRXOCFMDUSFFAK-UHFFFAOYSA-N 0.000 description 1
- 238000007720 emulsion polymerization reaction Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 229920000159 gelatin Polymers 0.000 description 1
- 239000008273 gelatin Substances 0.000 description 1
- 235000019322 gelatine Nutrition 0.000 description 1
- 235000011852 gelatine desserts Nutrition 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 1
- 239000001095 magnesium carbonate Substances 0.000 description 1
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 1
- 150000004702 methyl esters Chemical class 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 150000002825 nitriles Chemical class 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 150000001451 organic peroxides Chemical group 0.000 description 1
- 239000012074 organic phase Substances 0.000 description 1
- VSIIXMUUUJUKCM-UHFFFAOYSA-D pentacalcium;fluoride;triphosphate Chemical compound [F-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O VSIIXMUUUJUKCM-UHFFFAOYSA-D 0.000 description 1
- 239000004584 polyacrylic acid Substances 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000000375 suspending agent Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
- 229920001567 vinyl ester resin Polymers 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Classifications
-
- 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
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/12—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polysiloxanes
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
Verfahren zur Herstellung von Polyvinylverbindungen Es ist bekannt, Polyyinylverbindungen durch Polymerisation von Vinylverbindungen, wie Styrol, substituierten Styrolen, Vinylester, Vinylchlorid, Vinylidenchlorid, Acrylsäureester, Acrylnitril usw.,' oder deren Gemischen in wäßrigen Suspensionen von pulverförmigen, in den monomeren Vinylverbindungen unlöslichen anorganischen Verbindungen unter mechanischer Bewegung mit Hilfe von Aktivatoren herzustellen. Als unlösliche anorganische Stoffe werden beispielsweise Bariumsulfat, Kaolin, Phosphate des Calciums, Bariums, Magnesiums und Zinks, ferner Talkum, Magnesiumcarbonat, Aluminiumoxydhydrate, Kieselgur, Apatit und andere Mineralien verwendet. :Ulan erhält auf diese Weise kugelförmige Polymerisate, da bei der Polymerisation die durch die starke mechanische Bewegung (Rühren oder Schütteln) gebildeten Tröpfchen der monomeren Vinylverbindungen durch die pulverförmigen anorganischen Verbindungen vor dem Zusammenfließen bzw. Zusammenklumpen geschützt werden. Man hat auch schon die Suspensionspolymerisation von Vinylverbindungen in Gegenwart von hochmolekularen organischen Verbindungen, die in Wasser kolloidal löslich sind, beispielsweise Gelatine, Polyvinylalkohol, Polyacrylsäüre, Polyvinylpyrrolidon, vorgenommen. Die durch Suspensionspolymerisation erhaltenen Polymerisate zeichnen sich vor den durch Emulsionspolymerisation erhaltenen Polymerisaten dadurch aus, daß sie bei Verwendung geeigneter Suspensionsmittel klar und farblos sind und in elektrischer Hinsicht sich wesentlich günstiger als diese verhalten.Process for the production of polyvinyl compounds It is known Polyynyl compounds substituted by polymerization of vinyl compounds such as styrene Styrenes, vinyl esters, vinyl chloride, vinylidene chloride, acrylic acid esters, acrylonitrile etc., 'or their mixtures in aqueous suspensions of powdery, in the monomeric vinyl compounds insoluble inorganic compounds under mechanical Establish movement with the help of activators. As insoluble inorganic substances are for example barium sulfate, kaolin, calcium phosphates, barium, magnesium and zinc, also talc, magnesium carbonate, aluminum oxide hydrates, kieselguhr, apatite and other minerals used. : Ulan gets spherical polymers in this way, because during the polymerization, the strong mechanical movement (stirring or Shaking) droplets of the monomeric vinyl compounds formed by the powdery inorganic compounds protected from flowing together or clumping together will. The suspension polymerization of vinyl compounds in Presence of high molecular weight organic compounds that are colloidal in water are soluble, for example gelatin, polyvinyl alcohol, polyacrylic acid, polyvinylpyrrolidone, performed. Draw the polymers obtained by suspension polymerization prior to the polymers obtained by emulsion polymerization, that they are clear and colorless when using suitable suspending agents and in from an electrical point of view behave much more favorably than this.
Es wurde gefunden, daß man Polyvinylverbindungen durch Polymerisation von monömeren Vinylverbindungen in wäßrigen Suspensionen von pulverförmigen, in den monomeren Vinylverbindungen unlöslichen anorganischen Stoffen unter mechanischer Bewegung mit Hilfe von in den moncmeren Vinylverbindungen löslichen Katalysatoren besonders vorteilhaft -herstellen kann, wenn man in Gegenwart geringei Mengen von Silikonölen arbeitet. Unter Silikonölen werden solche Organopolysiloxane und Organooxypolysiloxane verstanden, die einen linearen bzw. wenig verzweigten Aufbau besitzen und der allgemeinen Formel MD. ,M entsprechen, wobei M monofunktionelle Kettenglieder, wie z. B. (C H,), Si -, die über i Sauerstoffatom und D difunktionelle Kettenglieder, wie z. B. - Si (C H3)2 -, die über 2 Sauerstoffatome niit der Kette verbunden sind, bedeuten. Trifunktionelle, sogenannte T-Glieder, wie zum Beispiel die über 2 Säuerstoffatome mit derselben Kette und über eine drittes Sauerstoffatom die Verknüpfung mit der Nachbarkette, also eine Vernetzung herstellen, sollen nur in untergeordnetem Maße in Silikonölen, die hauptsächlich Alkyl-, insbesondere Methylsilikone mit Viskositäten von 2o bis 2ooo cSt bei 2o° darstellen, vorhanden sein (vgl. E. G. Rochow, Einführung in die Chemie der Silikone, 1952,'S. 95 ff). Man wendet die Silikonöle in Mengen von o,oooi bis o,1 Gewichtsprozent, bezogen auf die monomere Vinylverbindung, an. Die pulverförmigen, in den monomeren Vinylverbindungenunlöslichen anorganischenVerbindungen, die eine Korngröße zwischen etwa o, i ,u und i ,u besitzen, werden in Mengen von 0,05 bis 1,5 Gewichtsprozent; bezogen auf die monomere Vinylverbindung, angewandt. Durch- Variieren der Menge 'des zugesetzten Silikonöls und der pulverförmigen anorganischen Verbindung hat man es in der Hand, die Korngröße der anfallenden Polymerisate in weiten Grenzen. zu verändern. Als Katalysatoren werden öllösliche Verbindungen verwendet, die unter Radikalzerfall die Polymerisation bewirken, beispielsweise BenzöylsuperoXyd; Cumolhydroperoxyd, Lauroylperoxyd, Di-tertiär-bntylperoxyd und andere organische Peroxyde. Auch stickstoffhaltige Katalysatoren von der Art des Azodiisobutteisäurenitrils kommen in Frage. In vielen Fällen kann es von Vorteil sein, bei_ der Polymerisation mehrere Katalysatoren zu verwenden, insbesondere solche, deren Zerfallstemperatur in verschiedenen Bereichen liegt, so daß mit der Erhöhung der Polymerisatiönstemperatur der zweite bzw. weitere Katalysator zum Anspringen kommt. Die Polymerisationstemperatur ist durch die Zerfallstemperatur der Polymerisationsbeschleuniger bedingt und liegt im Bereich von 5o° bis 13o° C. Das Verhältnis der organischen Phase zur wäßrigen Phase kann in verhältnismäßig weiten Grenzen schwanken, bevorzugt wird das Verhältnis -von etwa 1,5: i bis 1 : 1,5, doch sind aber auch Verhältnisse von 3 : 1 bis 1 : 5 noch tragbar. Das pg des Polymeiisationsansatzes liegt im allgemeinen zwischen 5 und g.It has been found that polyvinyl compounds by polymerizing monomeric vinyl compounds in aqueous suspensions of pulverulent inorganic substances insoluble in the monomeric vinyl compounds with mechanical agitation with the aid of catalysts soluble in the monomeric vinyl compounds can be particularly advantageous if one is in the presence of small amounts of Silicone oils works. Silicone oils are understood as meaning those organopolysiloxanes and organooxypolysiloxanes which have a linear or slightly branched structure and the general formula MD. , M correspond, where M monofunctional chain links, such as. B. (C H,), Si -, which have i oxygen atom and D difunctional chain links, such as. B. - Si (C H3) 2 -, which are connected to the chain via 2 oxygen atoms. Trifunctional, so-called T-links, such as the two oxygen atoms with the same chain and a third oxygen atom create a link with the neighboring chain, i.e. a crosslinking, should only be used to a lesser extent in silicone oils, which are mainly alkyl, especially methyl silicones with viscosities of 2o to 2ooo cSt at 2o °, be present (see EG Rochow, Introduction to the chemistry of silicones, 1952, 'p. 95 ff). The silicone oils are used in amounts of from 0.01 to 0.1 percent by weight, based on the monomeric vinyl compound. The powdery inorganic compounds which are insoluble in the monomeric vinyl compounds and which have a grain size between about o, i, u and i, u, are used in amounts of 0.05 to 1.5 percent by weight; based on the monomeric vinyl compound applied. By varying the amount of silicone oil added and the powdered inorganic compound, it is possible to control the grain size of the resulting polymers within wide limits. to change. The catalysts used are oil-soluble compounds which cause the polymerization with radical decomposition, for example benzoyl superoxide; Cumene hydroperoxide, lauroyl peroxide, di-tertiary methyl peroxide and other organic peroxides. Nitrogen-containing catalysts of the azodiisobutietic acid nitrile type are also suitable. In many cases it can be advantageous to use several catalysts during the polymerization, in particular those whose decomposition temperature is in different ranges, so that the second or further catalyst starts up as the polymerization temperature increases. The polymerization temperature is determined by the decomposition temperature of the polymerization accelerator and is in the range from 50 ° to 130 ° C. The ratio of the organic phase to the aqueous phase can vary within relatively wide limits, the ratio of about 1.5: 1 to 1 being preferred : 1.5, but ratios of 3: 1 to 1: 5 are still acceptable. The pg of the polymerization batch is generally between 5 and g.
Beispiel i_ 8 kg Styrol, dem 16g Benzoylperoxyd zugesetzt sind, werden unter Rühren zu einer Suspension gegeben, die aus einer wäßrigen Aufschlämmung von 64 g Bariumsulfat in z61 Wasser besteht. Man polymerisiert unter kräftigem Rühren bei 85° und beendet die Polymerisation n^#.h io Stunden. Die Körnung der erhaltenen Polymerisate liegt zwischen o,i bis 1,5 mm, ohne ein scharf ausgeprägtes Maximum.Example i_ 8 kg of styrene to which 16 g of benzoyl peroxide are added added with stirring to a suspension consisting of an aqueous slurry of 64 g of barium sulfate in 61 water. Polymerize with vigorous stirring at 85 ° and the polymerization ends after n ^ #. h io hours. The grain of the obtained Polymer is between 0.1 and 1.5 mm, without a sharply pronounced maximum.
Führt man jedoch das vorstehende Beispiel unter Zusatz von 500 mg eines im Handel erhältlichen Silikonöls aus, so liegt das Maximum der Korngröße' zwischen o,5 und o,6 mm und beträgt 75 % des Polymerisats. Der Rest verteilt sich auf größere und kleinere Körner.However, if the above example is carried out with the addition of 500 mg of a commercially available silicone oil, the maximum grain size is between 0.5 and 0.6 mm and amounts to 75% of the polymer. The rest is divided into larger and smaller grains.
Beispiel ä 16 kg mit 32 g Benzoylperoxyd aktiviertes Styrol werden einer wäßrigen Suspension von 16 kg Wasser und 3o g Tricalciumph-osphat zugegeben und bei 85° io Stunden lang unter kräftigem Rühren polymerisiert. Man erhält ein sehr uneinheitliches Polymerisat mit einer. Körnung zwischen 0,25 bis 1;5 mm mit einem schwach ausgeprägten Maximum bei 0,5 mm.Example 16 kg of styrene activated with 32 g of benzoyl peroxide are added to an aqueous suspension of 16 kg of water and 30 g of tricalcium osphat and polymerized at 85 ° for 10 hours with vigorous stirring. A very non-uniform polymer is obtained with a. Grain size between 0.25 to 1.5 mm with a weak maximum at 0.5 mm.
Führt man dagegen das vorstehende Beispiel unter Zusatz von 0,5 g des im Beispiel i verwendeten Silikonöls aus, so erhält man ein sehr einheitliches Polymerisat mit einem Maximum der Körnung zwischen 0,5 bis o,75 mm, das mehr als 85 °/a des erhaltenen Polymerisats beträgt. .If, on the other hand, the above example is carried out with the addition of 0.5 g of the silicone oil used in Example i, a very uniform polymer is obtained with a maximum grain size between 0.5 and 0.75 mm, which is more than 85 ° / a of the polymer obtained is. .
Setzt man im vorstehenden Beispiel an Stelle des Styrols 8 kg Methacrylrnethylester ein und arbeitet man im übrigen wie vorstehend in Absatz 2 angegeben, so erhält man nach dem Waschen mit Salzsäure zur Entfernung des Tricalciumphosphats und anschließendem Filtrieren und Waschen Polymethacrylmethylester mit einer' Kornverteilung von o,8 bis 0,4 mm. Gröbere und kleinere Polymerisatkörner sind nur in untergeordnetem Maße entstanden.If, in the above example, 8 kg of methyl methacrylate are used instead of styrene and if you work otherwise as indicated in paragraph 2 above, you get after washing with hydrochloric acid to remove the tricalcium phosphate and then Filtration and washing of polymethacrylic methyl ester with a 'particle size distribution of 0.8 up to 0.4 mm. Coarser and smaller polymer grains are only to a minor extent developed.
Beispiel 3 In einem 2-1-Kolben mit Rückflußkühler und Rührer werden 300 g Styrol, in dem 9 mg Silikonöl, 0,5 g Benzoylperoxyd und 0,15 g Di-tertiär-butylperoxyd gelöst sind, mit 45o g Wasser, in dem o,6 g. Tricalciumphosphat suspendiert sind, unter kräftigem Rühren polymerisiert. Man hält zunächst 8 Stunden lang bei 85°, steigert dann die Temperatur im Verlauf von 2 Stunden auf g5° und für weitere 6 Stunden auf 115°, wobei der Kolben in ein Ölbad eingehängt wird. Es wird'ein körniges Polymerisat erhalten, das einen sehr engen Komverteilungsbereich mit einem Maximum bei 0,5 mm aufweist. .Example 3 In a 2 l flask with reflux condenser and stirrer, 300 g of styrene, in which 9 mg of silicone oil, 0.5 g of benzoyl peroxide and 0.15 g of di-tertiary butyl peroxide are dissolved, are mixed with 45o g of water in which the o , 6 g. Tricalcium phosphate are suspended, polymerized with vigorous stirring. The temperature is initially held at 85 ° for 8 hours, then the temperature is increased to g5 ° in the course of 2 hours and to 115 ° for a further 6 hours, the flask being hung in an oil bath. A granular polymer is obtained which has a very narrow particle size distribution range with a maximum of 0.5 mm. .
Claims (1)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DEC10431A DE947736C (en) | 1954-12-17 | 1954-12-17 | Process for the production of polyvinyl compounds |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DEC10431A DE947736C (en) | 1954-12-17 | 1954-12-17 | Process for the production of polyvinyl compounds |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| DE947736C true DE947736C (en) | 1956-08-23 |
Family
ID=7014761
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DEC10431A Expired DE947736C (en) | 1954-12-17 | 1954-12-17 | Process for the production of polyvinyl compounds |
Country Status (1)
| Country | Link |
|---|---|
| DE (1) | DE947736C (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2405828A1 (en) * | 1974-02-07 | 1975-08-21 | Consortium Elektrochem Ind | PROCESS FOR PREPARING MODIFIED ORGANOPOLYSILOXANES |
-
1954
- 1954-12-17 DE DEC10431A patent/DE947736C/en not_active Expired
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2405828A1 (en) * | 1974-02-07 | 1975-08-21 | Consortium Elektrochem Ind | PROCESS FOR PREPARING MODIFIED ORGANOPOLYSILOXANES |
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