DE4212752A1 - Silicone resins prodn. - by passing solns. of siloxane(s) obtd. by known methods through thin-film evaporator at specified parameters - Google Patents
Silicone resins prodn. - by passing solns. of siloxane(s) obtd. by known methods through thin-film evaporator at specified parametersInfo
- Publication number
- DE4212752A1 DE4212752A1 DE19924212752 DE4212752A DE4212752A1 DE 4212752 A1 DE4212752 A1 DE 4212752A1 DE 19924212752 DE19924212752 DE 19924212752 DE 4212752 A DE4212752 A DE 4212752A DE 4212752 A1 DE4212752 A1 DE 4212752A1
- Authority
- DE
- Germany
- Prior art keywords
- solns
- siloxane
- solutions
- film evaporator
- pref
- 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.)
- Ceased
Links
- 229920002050 silicone resin Polymers 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims abstract description 22
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical compound [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 239000010409 thin film Substances 0.000 title claims abstract description 16
- 239000002904 solvent Substances 0.000 claims abstract description 12
- -1 siloxanes Chemical class 0.000 claims abstract description 8
- 230000007062 hydrolysis Effects 0.000 claims abstract description 7
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 7
- 150000001367 organochlorosilanes Chemical class 0.000 claims abstract description 5
- 239000003054 catalyst Substances 0.000 claims abstract description 4
- 239000003112 inhibitor Substances 0.000 claims abstract description 4
- 150000001282 organosilanes Chemical class 0.000 claims abstract description 4
- 239000003849 aromatic solvent Substances 0.000 claims abstract 2
- 239000003960 organic solvent Substances 0.000 claims abstract 2
- 238000009833 condensation Methods 0.000 claims description 9
- 230000005494 condensation Effects 0.000 claims description 9
- 239000000047 product Substances 0.000 claims description 8
- 239000007859 condensation product Substances 0.000 claims 1
- 238000002360 preparation method Methods 0.000 claims 1
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 abstract description 19
- 229920005989 resin Polymers 0.000 abstract description 18
- 239000011347 resin Substances 0.000 abstract description 18
- 239000002184 metal Substances 0.000 abstract description 3
- 229910052751 metal Inorganic materials 0.000 abstract description 3
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 abstract description 2
- 150000003839 salts Chemical class 0.000 abstract description 2
- 238000003860 storage Methods 0.000 abstract description 2
- 239000008096 xylene Substances 0.000 abstract description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 abstract 2
- 239000002519 antifouling agent Substances 0.000 abstract 1
- 238000010030 laminating Methods 0.000 abstract 1
- 239000003208 petroleum Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 30
- 238000002844 melting Methods 0.000 description 10
- 230000008018 melting Effects 0.000 description 10
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 5
- 239000007787 solid Substances 0.000 description 5
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000007863 gel particle Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 150000007513 acids Chemical class 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241000282326 Felis catus Species 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- UZHDGDDPOPDJGM-UHFFFAOYSA-N Stigmatellin A Natural products COC1=CC(OC)=C2C(=O)C(C)=C(CCC(C)C(OC)C(C)C(C=CC=CC(C)=CC)OC)OC2=C1O UZHDGDDPOPDJGM-UHFFFAOYSA-N 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- YGZSVWMBUCGDCV-UHFFFAOYSA-N chloro(methyl)silane Chemical compound C[SiH2]Cl YGZSVWMBUCGDCV-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 150000001991 dicarboxylic acids Chemical class 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000003502 gasoline Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 210000003734 kidney Anatomy 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- 239000004945 silicone rubber Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/46—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with organic materials
- C04B41/49—Compounds having one or more carbon-to-metal or carbon-to-silicon linkages ; Organo-clay compounds; Organo-silicates, i.e. ortho- or polysilicic acid esters ; Organo-phosphorus compounds; Organo-inorganic complexes
- C04B41/4905—Compounds having one or more carbon-to-metal or carbon-to-silicon linkages ; Organo-clay compounds; Organo-silicates, i.e. ortho- or polysilicic acid esters ; Organo-phosphorus compounds; Organo-inorganic complexes containing silicon
- C04B41/495—Compounds having one or more carbon-to-metal or carbon-to-silicon linkages ; Organo-clay compounds; Organo-silicates, i.e. ortho- or polysilicic acid esters ; Organo-phosphorus compounds; Organo-inorganic complexes containing silicon applied to the substrate as oligomers or polymers
- C04B41/4961—Polyorganosiloxanes, i.e. polymers with a Si-O-Si-O-chain; "silicones"
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/60—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only artificial stone
- C04B41/61—Coating or impregnation
- C04B41/62—Coating or impregnation with organic materials
- C04B41/64—Compounds having one or more carbon-to-metal of carbon-to-silicon linkages
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/06—Preparatory processes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/32—Post-polymerisation treatment
- C08G77/34—Purification
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Silicon Polymers (AREA)
Abstract
Description
Die Erfindung betrifft ein Verfahren zur Herstellung von Silicon harzen, insbesondere von Methylsiliconharzen, aus Lösungen von Si loxanen, die nach bekannten Verfahren hergestellt wurden. Die er haltenen Siliconharze finden u. a. als Elektroisolier- und Lami nierharze sowie als Bautenschutzanstrichstoffe Anwendung.The invention relates to a method for producing silicone resins, in particular methyl silicone resins, from solutions of Si loxanes, which were prepared by known processes. Which he find silicone resins u. a. as electrical insulation and lami kidney resins as well as building protection paints application.
Zur Herstellung von Siliconharzen werden Hydrolyseprodukte von Or ganosilanen und/oder Organochlorsilanen bevorzugt bei höheren Kon zentrationen thermisch oder katalytisch kondensiert. Als Katalysa toren können Säuren, Basen oder Metallverbindungen eingesetzt wer den.Hydrolysis products from Or ganosilanes and / or organochlorosilanes preferred at higher cones concentrations condensed thermally or catalytically. As a cat gates, acids, bases or metal compounds can be used the.
Bevorzugt wird die metallkatalysierte Kondensation in Gegenwart von Lösungsmitteln durchgeführt. Damit ist es möglich, sich bildendes Kondensationswasser sofort azeotrop zu entfernen und die Reaktion durch Verdünnen mit Lösungsmittel abzubrechen.The metal-catalyzed condensation is preferred in the presence of Solvents. So it is possible to educate yourself Condensate immediately remove azeotropically and the reaction cancel by dilution with solvent.
Mit diesem Verfahren gelingt es nicht, niederviskose Siliconharze mit z. B. Viskositäten unter 20 mPas (bei 25 °C als 55%iger tolue nischer Lösung) herzustellen. Ein weiterer Nachteil des Verfahrens besteht im niedrigen Schmelzpunkt lösungsmittelfreier Harze bzw. im Sintern der Siliconharzpulver bei Raumtemperatur. Diese Nachteile sind weder durch weitere Kondensation noch durch Modifizierung von Kondensation oder Destillation, wie z. B. Strippen mit Wasserdampf, zu beheben.This process does not succeed in low-viscosity silicone resins with z. B. viscosities below 20 mPas (at 25 ° C as 55% tolue African solution). Another disadvantage of the process exists in the low melting point of solvent-free resins or in Sinter the silicone resin powder at room temperature. These disadvantages are neither by further condensation nor by modification of Condensation or distillation, such as. B. stripping with water vapor, to fix.
Aufgabe der Erfindung war es, ein Verfahren zur Herstellung von Siliconharzen aufzufinden, das es ermöglicht, neben den üblicher weise hergestellten Siliconharztypen, bevorzugt niederviskose Sili conharzlösungen sowie lösungsmittelfreie Harze mit einem gezielt einstellbaren Schmelzpunkt und vollständiger Rücklöslichkeit herzu stellen. Dabei ist von nach bekannten Verfahren hergestellten Si loxanlösungen verschiedener Kondensationsgrade auszugehen. The object of the invention was to provide a method for producing Find silicone resins that allows, in addition to the usual wise manufactured silicone resin types, preferably low-viscosity sili con resin solutions as well as solvent-free resins with a targeted adjustable melting point and complete solubility put. Here, Si produced by known processes loxane solutions of various degrees of condensation.
Erfindungsgemäß werden Siloxanlösungen, die nach bekannten Verfah ren hergestellt wurden, durch einen Dünnschichtverdampfer bei 1 bis 100 hPa und 100 bis 300 °C, vorzugsweise bei 5 bis 50 hPa und 150 bis 250 °C, geführt.According to the invention, siloxane solutions which are prepared by known methods ren were produced by a thin film evaporator at 1 to 100 hPa and 100 to 300 ° C, preferably at 5 to 50 hPa and 150 up to 250 ° C.
Der Dünnschichtverdampfer wird üblicherweise zur thermischen Tren nung von flüssigen Stoffgemischen genutzt. In der Siliconchemie wird er beispielsweise zur Trennung des Gemisches von cyclischen und linearen Verbindungen bei der Herstellung von Siliconkautschuk polymeren eingesetzt.The thin film evaporator is usually used for thermal separation liquid mixtures. In silicone chemistry it is used, for example, to separate the mixture from cyclic ones and linear compounds in the manufacture of silicone rubber polymers used.
Es war überraschend, daß der Dünnschichtverdampfer erfindungsgemäß hervorragend bei der Herstellung von Siliconharzen, die eine ver netzte Stuktur aufweisen, einsetzbar ist.It was surprising that the thin film evaporator according to the invention excellent in the production of silicone resins, which ver have a net structure, can be used.
Für das erfindungsgemäße Verfahren sind alle handelsüblichen Dünn schichtverdampfer geeignet. So können Dünnschichtverdampfer aus Glas oder Metall eingesetzt werden, die mit beweglichen oder fest stehenden Wischblättern und mit einem innen- oder außenliegenden Kondensator ausgestattet sind.All commercially available thins are for the process according to the invention layer evaporator suitable. So thin film evaporators can Glass or metal can be used with movable or fixed standing wiper blades and with an inside or outside Capacitor.
Es ist vorteilhaft, die Siloxanlösungen einmalig durch den Dünn schichtverdampfer zu führen. Es sind jedoch auch mehrere Durchläufe möglich. Vor dem Eintritt in den Dünnschichtverdampfer ist es gün stig, die Siloxanlösung auf Siedetemperatur zu bringen bzw., spe ziell beim Einsatz von oligomeren Siloxanlösungen, die Lösungen auf 50 bis 95 Gew.-% Siloxan zu konzentrieren. Während des Durchlaufes durch den Dünnschichtverdampfer ist der Einsatz von Inertgasen zur Förderung der gasförmigen Produkte aus der Verdampferzone möglich. Der Produktaustrag aus dem Dünnschichtverdampfer erfolgt diskonti nuierlich in Form von Siliconharzschmelzen oder Festharzen bzw. bei kontinuierlicher Herstellung in Form von zwangsgeförderten Silicon harzschmelzen.It is advantageous to pass the siloxane solutions once through the thin layer evaporator. However, there are also several runs possible. Before entering the thin film evaporator it is green stig to bring the siloxane solution to boiling temperature or, spe the solutions when using oligomeric siloxane solutions Concentrate 50 to 95 wt .-% siloxane. During the run the use of inert gases for the thin film evaporator Conveying gaseous products from the evaporator zone is possible. The product discharge from the thin film evaporator is discounted nuously in the form of silicone resin melts or solid resins or at continuous production in the form of forcibly conveyed silicone resin melting.
Als Siloxanlösungen können Lösungen oligomerer Siloxane, die durch Hydrolyse von Organosilanen und/oder Organochlorsilanen entstehen oder die nach der Konzentrierung der Hydrolyseprodukte auf vorzugs weise 50 bis 95 Gew.-% Siloxan erhaltenen Lösungen eingesetzt wer den. Weiterhin ist es möglich die nach Kondensation oder Teilkon densation, die thermisch oder in Gegenwart bekannter Katalysatoren, wie z. B. in Gegenwart von Metallsalzen organischer oder anorgani scher Säuren, durchgeführt werden kann, anfallenden Siloxanlösungen durch den Dünnschichtverdampfer zu führen. Inhibitoren, wie z. B. Carbon- und/oder Dicarbonsäuren, können ebenfalls in der Siloxanlö sung enthalten sein. Als Lösungsmittel sind die für die Silicon harzherstellung bekannten organischen, vorzugsweise aromatischen Lösungsmittel enthalten, die während der Kondensation mit dem ent stehenden Kondensationswasser azeotrope Gemische bilden, wie z. B. Toluol, Xylol oder Benzine.Solutions of oligomeric siloxanes which are caused by Hydrolysis of organosilanes and / or organochlorosilanes arise or preferred after concentrating the hydrolysis products 50 to 95% by weight of solutions obtained from siloxane are used the. It is also possible that after condensation or partial con densation, the thermal or in the presence of known catalysts, such as B. in the presence of metal salts organic or inorganic shear acids, can be carried out, resulting siloxane solutions through the thin film evaporator. Inhibitors such as B. Carbon and / or dicarboxylic acids can also be found in the siloxane solution solution. The solvents are those for silicone resin production known organic, preferably aromatic Contain solvents, which during the condensation with the ent standing water of condensation form azeotropic mixtures, such as. B. Toluene, xylene or gasoline.
Das den Dünnschichtverdampfer verlassende, lösungsmittelfreie Sili conharz kann gezielt thermisch oder katalytisch, gegebenenfalls in Gegenwart von Lösungsmitteln, kondensiert bzw. nachkondensiert wer den. Es ist jedoch auch möglich, das erhaltene, lösungmittelfreie Siliconharz vollständig zu lösen, wodurch es gelingt, speziell niedrigviskose Siliconharzlösungen herzustellen, was den Einsatz niedrigkondensierter Produkte voraussetzt.The solvent-free sili leaving the thin film evaporator conharz can be targeted thermally or catalytically, optionally in Presence of solvents, condensed or post-condensed the. However, it is also possible to use the solvent-free solution obtained Solvent silicone resin completely, which makes it possible, especially produce low-viscosity silicone resin solutions what use low-condensed products.
Das als Endprodukt erhaltene Siliconharz, welches als Festharz oder in gelöster Form vorliegen kann, weist eine sehr gute Lagerstabi lität und thermische Stabilität auf. Das Festharz ist mit einer gezielten Schmelztemperatur herstellbar und bei Raumtemperatur sin terfrei; daraus hergestellte Lösungen sind gelteilchenfrei. Weiter hin gelingt es mit dem erfindungsgemäßen Verfahren extrem nieder viskose Siliconharzlösungen herzustellen.The silicone resin obtained as the final product, which as a solid resin or can be in dissolved form, has a very good storage stability lity and thermal stability. The solid resin is with a targeted melting temperature can be produced and at room temperature terfrei; Solutions made from it are free of gel particles. Next it succeeds extremely low with the inventive method to produce viscous silicone resin solutions.
Als Ausgangsprodukt wurde eine kondensierte, toluolische Methylsi liconharzlösung einer Siloxankonzentration von 50 Gew.-% einge setzt.A condensed, toluene methylsi was used as the starting product licon resin solution of a siloxane concentration of 50 wt .-% puts.
-
a) Zur vollständigen Abtreibung des Lösungsmittels wurde ein Dünn
schichtverdampfer aus Glas, der mit Mantelheizung, Kondensator
(Temperatur: 10 °C) und Kühlfalle (Temperatur: -80 °C) ausge
stattet war, unter Einhaltung der folgenden Parameter, verwen
det.
Heizfläche: 540 cm2
Rotordrehzahl: 450 min-1
Heizmanteltemperatur: 200 °C
Durchsatz: 1048 ml/h
Druck: 40 hPa.Erhalten wurde ein lösungsmittelfreies Methylsiliconharz mit einem Schmelzbeginn von 47,8 °C.a) To completely abort the solvent, a thin-film evaporator made of glass, which was equipped with jacket heating, condenser (temperature: 10 ° C) and cold trap (temperature: -80 ° C), was used in compliance with the following parameters. Heating area: 540 cm 2
Rotor speed: 450 min -1
Heating jacket temperature: 200 ° C
Flow: 1048 ml / h
Pressure: 40 hPa. A solvent-free methyl silicone resin was obtained with a melting point of 47.8 ° C. - b) Das Lösungmittel wurde durch Strippen mit Wasserdampf entfernt. Das erhaltene Festharz wies einen Schmelzbeginn unterhalb von 20 °C auf.b) The solvent was removed by stripping with steam. The solid resin obtained had an onset of melting below 20 ° C.
Eine toluolische Methylsiliconharzlösung, hergestellt durch Hydro lyse eines Umsetzungsproduktes von Methylchlorsilan und Methanol, wurde auf herkömmliche Weise durch Abdestillieren auf einen Silo xangehalt von 50 Gew.-% konzentriert.A toluene methyl silicone resin solution made by Hydro lysis of a reaction product of methylchlorosilane and methanol, was distilled onto a silo in a conventional manner xan content of 50 wt .-% concentrated.
- a) Dieser Harzlösung wurde im o. a. Dünnschichtverdampfer das rest liche Lösungsmittel entzogen und anschließend das lösungsmittel freie Methylsiliconharz in Toluol gelöst. Die erhaltene 55%ige Lösung wies eine Viskosität von 10 mPas (bei 25 °C) auf. a) This resin solution was in the above. Thin film evaporator the rest withdrawn solvent and then the solvent free methyl silicone resin dissolved in toluene. The 55% obtained Solution had a viscosity of 10 mPas (at 25 ° C).
- b) Ein anderer Teil der Harzlösung wurde durch Abtreiben des Lö sungsmittels mit Hilfe von Wasserdampf aufkonzentriert. Die erhaltene 55%ige toluolische Methylharzlösung wies eine Viskosität von 35 mpas (bei 25 °C) auf.b) Another part of the resin solution was removed by driving off the Lö concentrated with the help of steam. The 55% toluene methyl resin solution obtained had one Viscosity of 35 mpas (at 25 ° C).
Eingesetzt wurde die auf 50 Gew.-% Siloxan konzentrierte Methyl harzlösung aus Beispiel 2.The methyl concentrated to 50% by weight of siloxane was used resin solution from Example 2.
- a) Die Methylharzlösung wurde durch den Dünnschichtverdampfer ge führt. Das aus dem Dünnschichtverdampfer austretende, lösungs mittelfreie Methylsiliconharz wies einen Schmelzbeginn von 34 °C auf. Es wurde in Gegenwart von 10 ppm Eisen(III)chlorid als Ka talysator lösungsmittelfrei bis zu einem Schmelzbeginn von 47,7 °C kondensiert. Die damit hergestellte Harzlösung war klar und gelteilchenfrei.a) The methyl resin solution was ge through the thin film evaporator leads. The solution emerging from the thin film evaporator Medium-free methyl silicone resin had a melting point of 34 ° C on. It was in the presence of 10 ppm iron (III) chloride as Ka Talysator solvent-free up to the start of melting 47.7 ° C condensed. The resin solution made with it was clear and gel particle free.
- b) Das in der konzentrierten Methylsiliconharzlösung enthaltene Toluol wurde durch Strippen mit Wasserdampf entfernt. Das erhal tene Festharz wies einen Schmelzbeginn von 17 °C auf. Es wurde in Gegenwart von 10 ppm Eisen(III)chlorid kondensiert, bis ein Schmelzbeginn von 47 °C erreicht war. Die daraufhin hergestellte Lösung war nicht gelteilchenfrei und somit nicht verwendungsfä hig.b) The contained in the concentrated methyl silicone resin solution Toluene was removed by steam stripping. Get that Solid resin had a melting point of 17 ° C. It was condensed in the presence of 10 ppm iron (III) chloride until a Start of melting of 47 ° C was reached. The subsequently made Solution was not free of gel particles and was therefore not suitable for use hig.
Claims (9)
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
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DE19924212752 DE4212752A1 (en) | 1992-04-16 | 1992-04-16 | Silicone resins prodn. - by passing solns. of siloxane(s) obtd. by known methods through thin-film evaporator at specified parameters |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
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DE19924212752 DE4212752A1 (en) | 1992-04-16 | 1992-04-16 | Silicone resins prodn. - by passing solns. of siloxane(s) obtd. by known methods through thin-film evaporator at specified parameters |
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DE4212752A1 true DE4212752A1 (en) | 1993-10-21 |
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DE19924212752 Ceased DE4212752A1 (en) | 1992-04-16 | 1992-04-16 | Silicone resins prodn. - by passing solns. of siloxane(s) obtd. by known methods through thin-film evaporator at specified parameters |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE19507594A1 (en) * | 1995-03-04 | 1996-09-12 | Huels Silicone Gmbh | Prodn. of silicone resin for mica insulating materials, emulsions etc. |
WO2006126824A1 (en) * | 2005-05-23 | 2006-11-30 | Lg Chem, Ltd. | Method for concentrating organic silicate polymerite solution |
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DE2042952A1 (en) * | 1970-08-29 | 1972-05-31 | Owens Illinois Inc | Solid organopolysiloxanes prodn - by heat treatment of prepolymer film |
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EP0203565A2 (en) * | 1985-05-30 | 1986-12-03 | Wacker-Chemie GmbH | Continuous process for changing the molecular weight of organosilicon compounds |
SU1689381A1 (en) * | 1989-08-25 | 1991-11-07 | Государственный научно-исследовательский институт химии и технологии элементоорганических соединений | Method for obtaining oligomethylsiloxanes of branched structure |
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DE859163C (en) * | 1948-11-24 | 1952-12-11 | Dow Corning | Process for the continuous production of organosiloxanes from organochlorosilanes |
DE831694C (en) * | 1950-09-22 | 1952-02-18 | Hellmuth Holz Dr | Process for hydrolyzing organosilicon compounds |
US2883272A (en) * | 1955-09-13 | 1959-04-21 | Gen Electric | Apparatus for the continuous polymerization of organopolysiloxanes |
DE2042952A1 (en) * | 1970-08-29 | 1972-05-31 | Owens Illinois Inc | Solid organopolysiloxanes prodn - by heat treatment of prepolymer film |
SU998471A1 (en) * | 1973-05-28 | 1983-02-23 | Феб Хемиверк Нюнхритц (Инопредприятие) | Process for producing organosilicon resin |
DE2717496A1 (en) * | 1976-04-21 | 1977-11-03 | Gen Electric | PROCESS FOR CONTINUOUSLY PRODUCING LINEAR DIORGANOPOLYSILOXANE LIQUID |
EP0203565A2 (en) * | 1985-05-30 | 1986-12-03 | Wacker-Chemie GmbH | Continuous process for changing the molecular weight of organosilicon compounds |
SU1689381A1 (en) * | 1989-08-25 | 1991-11-07 | Государственный научно-исследовательский институт химии и технологии элементоорганических соединений | Method for obtaining oligomethylsiloxanes of branched structure |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE19507594A1 (en) * | 1995-03-04 | 1996-09-12 | Huels Silicone Gmbh | Prodn. of silicone resin for mica insulating materials, emulsions etc. |
DE19507594B4 (en) * | 1995-03-04 | 2005-01-13 | Wacker-Chemie Gmbh | Process for the preparation of silicone resins |
WO2006126824A1 (en) * | 2005-05-23 | 2006-11-30 | Lg Chem, Ltd. | Method for concentrating organic silicate polymerite solution |
US8013060B2 (en) | 2005-05-23 | 2011-09-06 | Lg Chem, Ltd. | Method for concentrating organic silicate polymer solution |
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Owner name: HUELS SILICONE GMBH, 01612 NUENCHRITZ, DE |
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