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DE1191968B - Process for the production of linear polymeric silicic acid mixed esters - Google Patents

Process for the production of linear polymeric silicic acid mixed esters

Info

Publication number
DE1191968B
DE1191968B DES57724A DES0057724A DE1191968B DE 1191968 B DE1191968 B DE 1191968B DE S57724 A DES57724 A DE S57724A DE S0057724 A DES0057724 A DE S0057724A DE 1191968 B DE1191968 B DE 1191968B
Authority
DE
Germany
Prior art keywords
silicic acid
aromatic
production
mixed esters
linear polymeric
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.)
Pending
Application number
DES57724A
Other languages
German (de)
Inventor
Dr H C Robert Schwarz Dr
Dipl-Chem Dr Wilhelm Kuchen
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.)
Siemens Corp
Original Assignee
Siemens Corp
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
Application filed by Siemens Corp filed Critical Siemens Corp
Priority to DES57724A priority Critical patent/DE1191968B/en
Publication of DE1191968B publication Critical patent/DE1191968B/en
Pending legal-status Critical Current

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Classifications

    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G77/00Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/60Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule in which all the silicon atoms are connected by linkages other than oxygen atoms
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01BCABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B3/00Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
    • H01B3/18Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
    • H01B3/30Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes
    • H01B3/46Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes silicones

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  • Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Description

Verfahren zur Herstellung von linear-polymeren Kieselsäuremischestern Es ist bekannt. Orthokieselsäureester der Formel Si(OR) (R stets das gleiche Alkyl bzw. Aryl) mit Dioxyverbindungen umzusetzen. Je nach den Reaktionsbedingungen und dem molaren Verhältnis der Reaktionspartner entstehen hierbei, da sämtliche vier OR-Gruppen des Si(OR) hinsichtlich der Umesterung mit Dioxyverbindungen gleichwertig sind, mehr oder weniger stark vernetzte polymere Kieselsäureester. so daß in den Polymerisaten sehr leicht unerwünschte räumliche Vernetzung über Struktureinheiten des Typs eintritt (HO - R' - OH aliphatische bzw. aromatische Dioxyverbindung).Process for the production of linear polymeric silicic acid mixed esters It is known. Orthosilicic acid esters of the formula Si (OR) (R always the same alkyl or aryl) to react with dioxy compounds. Depending on the reaction conditions and the molar ratio of the reactants, since all four OR groups of Si (OR) are equivalent in terms of transesterification with dioxy compounds, more or less strongly crosslinked polymeric silicic acid esters are formed. so that in the polymers very easily undesired spatial crosslinking via structural units of the type occurs (HO - R '- OH aliphatic or aromatic dioxy compound).

Durch die Vernetzung erhält das Polymerisat insbesondere ungünstige lacktechnische Eigenschaften. The crosslinking gives the polymer particularly unfavorable properties paint properties.

Es wird unlöslich in organischen Lösungsmitteln und neigt zum Verspröden.It becomes insoluble in organic solvents and tends to become brittle.

Beansprucht ist ein Verfahren zur Herstellung von linear-polymeren Kieselsäuremischestern durch Umesterung von aromatische Substituenten tragenden Orthokieselsäureestern mit organischen Dioxyverbindungen, das dadurch gekennzeichnet ist, daß man als aromatische Substituenten tragenden Orthokieselsäureester den aliphatisch-aromatischen Mischester o,o'-Diphenyldioxy-diisopropoxysilan und als organische Dioxyverbindung 4,4'-Dioxydiphenylpropan verwendet. What is claimed is a process for the production of linear polymers Silica mixed esters by transesterification of aromatic substituents Orthosilicic acid esters with organic dioxy compounds, which is characterized is that the orthosilicic acid ester bearing aromatic substituents is the aliphatic-aromatic Mixed esters o, o'-diphenyldioxy-diisopropoxysilane and as an organic dioxy compound 4,4'-Dioxydiphenylpropane is used.

Die nach dem beanspruchten Verfahren verwendeten Mischester werden nach folgendem Reaktionsschema nach hier nicht beanspruchtem Verfahren gewonnen: Geeignete Alkohole sind z. B. Sithyl-, Butyl- oder Isopropylalkohol.The mixed esters used according to the claimed process are obtained according to the following reaction scheme using a process not claimed here: Suitable alcohols are e.g. B. sithyl, butyl or isopropyl alcohol.

Die erfindungsgemäß als Ausgangsmaterial benutzten Mischester sind im Gegensatz zu Mischestern des Typs (RO)2Si(OR')2 (R und R' = verschiedene Alkyl- bzw. Arylreste) einmal in quantitativer Ausbeute, zum anderen in ausgezeichneter Reinheit erhältlich. Außerdem aber zeigen sie keinerlei Tendenz zur Dismutation, z. B. nach folgendem Schema Ihre Umesterung mit Dioxyverbindungen verläuft nach dem folgenden Reaktionsschema In den erfindungsgemäß erhaltenen Polyestern sind die Si-Atome durch Brücken verbunden, die aus den Resten der Dioxyverbindungen OR'O bestehen.In contrast to mixed esters of the type (RO) 2Si (OR ') 2 (R and R' = different alkyl or aryl radicals), the mixed esters used according to the invention as starting material are obtainable on the one hand in quantitative yield and on the other hand in excellent purity. In addition, however, they show no tendency to dismutation, e.g. B. according to the following scheme Their transesterification with dioxy compounds proceeds according to the following reaction scheme In the polyesters obtained according to the invention, the Si atoms are connected by bridges which consist of the residues of the dioxy compounds OR'O.

Der Hauptvorteil liegt darin, daß bei der erwähnten Arbeitsweise die verwendeten Mischester hinsichtlich der Umesterung mit HO R' - OH nur bifunktionell sind, da bei diesem Prozeß nur das leichtflüchtige ROH aus dem Gleichgewicht entfernt wird.The main advantage is that the mixed esters used in the procedure mentioned are only bifunctional with regard to the transesterification with HO R '- OH, since in this process only the volatile ROH is removed from the equilibrium.

Hierdurch gelangt man zu linearen, thermisch recht stabilen Hochpolymeren, die - wie bereits erwähnt - den vernetzten Produkten lacktechnisch weit überlegen sind. This leads to linear, thermally quite stable high polymers, which - as already mentioned - are far superior to the networked products in terms of coating technology are.

Ein anderer Vorteil beruht auf der Verwendung halogenfreier Ausgangsmaterialien, was vor allem für die Anwendung der Produkte auf dem Gebiet der Elektrotechnik sehr wichtig ist. Another advantage is based on the use of halogen-free starting materials, which especially for the application of the products in the field of electrical engineering important is.

Darüber hinaus sind die so erhaltenen Hochpolymeren nicht nur thermisch, sondern auch chemisch außerordentlich resistent und hierin den bekannten Reaktionsprodukten von aliphatischen oder aromatischen Halogensilanen mit Polyoxyverbindungen überlegen. In addition, the high polymers obtained in this way are not only thermal, but also extremely chemically resistant and the known reaction products superior to aliphatic or aromatic halosilanes with polyoxy compounds.

Die nach dem erfindungsgemäßen Verfahren erhaltenen linear-polymeren Kieselsäuremischester haben insbesondere lacktechnisch wesentlich günstigere Eigenschaften als die bekannten Umsetzungsprodukte aus aromatischen Kieselsäureestern der allgemeinen Formel Si(OR)4 (R stets gleiche aromatische Reste) mit Dioxyverbindungen. The linear polymers obtained by the process according to the invention Mixed silicic acid esters have, in particular, properties that are significantly more favorable in terms of paint technology than the known reaction products of aromatic silicic acid esters of the general Formula Si (OR) 4 (R always the same aromatic radicals) with dioxy compounds.

Auch die rein aromatischen Kieselsäureester, die durch Verwendung von Ortho- oder Polykieselsäureester des Oxydiphenyls erhalten werden, weisen noch nicht die Vorteile der nach dem erfindungsgemäßen Verfahren erhaltenen Produkte auf. Even the purely aromatic silicic acid esters produced by using obtained from orthosilicic or polysilicic acid esters of oxydiphenyl, show still not the advantages of the products obtained by the process according to the invention on.

Während die bekannten Produkte in aromatischen Lösungsmitteln unlöslich sind und zum Verspröden neigen, weisen die erfindungsgemäß erhaltenen linearpolymeren Produkte in lacktechnischer Hinsicht besonders günstige Eigenschaften auf. While the known products are insoluble in aromatic solvents and tend to become brittle, the linear polymers obtained according to the invention have Products have particularly favorable properties in terms of paint technology.

Beispiel Ein Gemisch von 66,0 g (11ã Mol) o,o'-Diphenyldiisopropoxysilan und 45,8 g (1/5 Mol) 4,4'-Dioxydiphenylpropan wird unter Rühren langsam bis auf 1500C erhitzt und 2 Stunden auf dieser Temperatur gehalten. Während der Reaktion destilliert die berechnete Menge Isopropanol (2/ã Mol) ab, und ein braunes viskoses Di wird erhalten, das bei Raumtemperatur zu einem lichtbraunen, transparenten Harz erstarrt. Dieses ist in Benzol, Toluol und Xylol löslich. Sein Si-Gehalt beträgt etwa 15,50in. Die Molgewichte liegen bei etwa 4000. Example A mixture of 66.0 g (11α mol) of o, o'-diphenyldiisopropoxysilane and 45.8 g (1/5 mol) of 4,4'-dioxydiphenylpropane is slowly added to with stirring Heated to 1500C and held at this temperature for 2 hours. During the reaction distilled the calculated amount of isopropanol (2 / ã mol) from, and a brown viscous Di is obtained, which at room temperature to a light brown, transparent resin stiffens. This is soluble in benzene, toluene and xylene. Its Si content is about 15.50in. The molecular weights are around 4000.

Die so gewonnenen Stoffe sind gut hitzebeständig und zeichnen sich auch sonst durch große Stabilität aus. Sie finden als Kunststoffe in der Elektrotechnik, namentlich für Isolations- und Tränkzwecke oder als Lackgrundkörper Verwendung. The substances obtained in this way are good heat-resistant and stand out also otherwise characterized by great stability. You will find plastics in electrical engineering, specifically for insulation and impregnation purposes or as a paint base.

Claims (1)

Patentanspruch: Verfahren zur Herstellung von linear-polymeren Kieselsäuremischestern durch Umesterung von aromatische Substituenten tragenden Orthokieselsäureestern mit organischen Dioxyverbindungen, dadurch gekennzeichnet, daß man als aromatische Substituenten tragenden Orthokieselsäureester den aliphatisch-aromatischen Mischester o,o'-Diphenyldioxy-diisopropoxysilan und als organische Dioxyverbindung 4,4'-Dioxydiphenylpropan verwendet. Claim: Process for the production of linear polymeric silicic acid mixed esters by transesterification of orthosilicic acid esters bearing aromatic substituents with organic dioxy compounds, characterized in that the aromatic Orthosilicic acid ester bearing substituents is the aliphatic-aromatic mixed ester o, o'-diphenyldioxy-diisopropoxysilane and 4,4'-dioxydiphenylpropane as the organic dioxy compound used. In Betracht gezogene Druckschriften: Deutsche Patentschriften Nr. 1 009 813, 1 010 739, 285 285, 973 716, 945 936; USA.-Patentschrift Nr. 2 630 446. Considered publications: German Patent Specifications No. 1 009 813, 1 010 739, 285 285, 973 716, 945 936; U.S. Patent No. 2,630,446.
DES57724A 1958-04-05 1958-04-05 Process for the production of linear polymeric silicic acid mixed esters Pending DE1191968B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
DES57724A DE1191968B (en) 1958-04-05 1958-04-05 Process for the production of linear polymeric silicic acid mixed esters

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DES57724A DE1191968B (en) 1958-04-05 1958-04-05 Process for the production of linear polymeric silicic acid mixed esters

Publications (1)

Publication Number Publication Date
DE1191968B true DE1191968B (en) 1965-04-29

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Family Applications (1)

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DES57724A Pending DE1191968B (en) 1958-04-05 1958-04-05 Process for the production of linear polymeric silicic acid mixed esters

Country Status (1)

Country Link
DE (1) DE1191968B (en)

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE285285C (en) *
US2630446A (en) * 1948-08-04 1953-03-03 Du Pont Polymeric silicates
DE945936C (en) * 1952-09-24 1956-07-19 Siemens Ag Process for the production of an electrical insulating material
DE1009813B (en) 1952-11-21 1957-06-06 Siemens Ag Process for the preparation of polymeric silicic acid esters of higher molecular weight
DE1010739B (en) 1954-11-03 1957-06-19 Kali Chemie Ag Process for the production of polysilicic acid esters of higher alcohols or phenols
DE973716C (en) * 1950-07-07 1960-05-19 Siemens Ag Process for the production of a curable silicon-containing synthetic resin

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE285285C (en) *
US2630446A (en) * 1948-08-04 1953-03-03 Du Pont Polymeric silicates
DE973716C (en) * 1950-07-07 1960-05-19 Siemens Ag Process for the production of a curable silicon-containing synthetic resin
DE945936C (en) * 1952-09-24 1956-07-19 Siemens Ag Process for the production of an electrical insulating material
DE1009813B (en) 1952-11-21 1957-06-06 Siemens Ag Process for the preparation of polymeric silicic acid esters of higher molecular weight
DE1010739B (en) 1954-11-03 1957-06-19 Kali Chemie Ag Process for the production of polysilicic acid esters of higher alcohols or phenols

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