DE1226310B - Process for the preparation of elastomeric silylmethylene polymers - Google Patents

Process for the preparation of elastomeric silylmethylene polymers

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Publication number
DE1226310B
DE1226310B DEJ27841A DEJ0027841A DE1226310B DE 1226310 B DE1226310 B DE 1226310B DE J27841 A DEJ27841 A DE J27841A DE J0027841 A DEJ0027841 A DE J0027841A DE 1226310 B DE1226310 B DE 1226310B
Authority
DE
Germany
Prior art keywords
silylmethylene
polymers
elastomeric
preparation
polymerization
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
DEJ27841A
Other languages
German (de)
Inventor
Nikolai S Nametkin
Valentin M Vdovin
Valery I Zavyalov
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.)
INST NEFTECHIMICHESKOGO SINTEZ
Original Assignee
INST NEFTECHIMICHESKOGO SINTEZ
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 INST NEFTECHIMICHESKOGO SINTEZ filed Critical INST NEFTECHIMICHESKOGO SINTEZ
Priority to DEJ27841A priority Critical patent/DE1226310B/en
Publication of DE1226310B publication Critical patent/DE1226310B/en
Pending legal-status Critical Current

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Classifications

    • 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

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)

Description

Verfahren zur Herstellung von elastomeren Silylmethylenpolymeren Die Erfindung betrifft ein Verfahren zur Herstellung polymerer Organosiliciumverbindungen vom Typ Dieses Polymere unterscheidet sich von seinem Strukturanalogen (Dimethylpolysiloxan), das in der Technik breite Anwendung findet, außer durch hohe chemische Stabilität auch durch hohe Wärmebeständigkeit.Process for the preparation of elastomeric silylmethylene polymers The invention relates to a process for the preparation of polymeric organosilicon compounds of the type This polymer differs from its structural analogue (dimethylpolysiloxane), which is widely used in technology, not only because of its high chemical stability but also because of its high heat resistance.

Bekannt sind folgende Verfahren zur Herstellung von Polymeren dieses Typs: Bekannt ist auch das Verfahren zur Polymerisation des 1,1,3,3 -Tetramethyl- 1,3-disilicacyclobutans in einer inerten Atmosphäre bei t>2500C unter Druck.The following processes for the production of polymers of this type are known: The process for polymerizing 1,1,3,3-tetramethyl-1,3-disilicacyclobutane in an inert atmosphere at t> 2500C under pressure is also known.

Nach den genannten Verfahren erhält man niedermolekulare, ölige Produkte mit einem Molekulargewicht von <15000.The processes mentioned give low molecular weight, oily products with a molecular weight of <15,000.

Ein Nachteil aller bekannten Verfahren besteht darin, daß man nur Silylmethylenpolymere in flüssigem Zustand mit niedrigen Molekulargewichten erhält. A disadvantage of all known methods is that one only Obtains silylmethylene polymers in the liquid state with low molecular weights.

Beansprucht ist ein Verfahren zur Herstellung von elastomeren Silylmethylenpolymeren der allgemeinen Formel durch Polymerisation von 1,1,3,3-Tetramethyl-1,3-disilicacyclobutan unter Erhitzen, das dadurch gekennzeichnet ist, daß man ein 1,1,3,3-Tetramethyl-1,3-disilicacyclobutan verwendet, das vorher mit einem starken Trocknungsmittel bei 10 bis 10-3 mm Hg getrocknet worden ist und die Polymerisation unterhalb 250"C im Vakuum oder in einer inerten Atmosphäre durchführt.What is claimed is a process for the production of elastomeric silylmethylene polymers of the general formula by polymerization of 1,1,3,3-tetramethyl-1,3-disilicacyclobutane with heating, which is characterized in that one uses a 1,1,3,3-tetramethyl-1,3-disilicacyclobutane previously with a strong desiccant has been dried at 10 to 10-3 mm Hg and the polymerization is carried out below 250 "C in vacuo or in an inert atmosphere.

Die erfindungsgemäße Durchführung der Polymerisation macht es möglich, praktisch in quantitativer Ausbeute ein Elastomeres hoher Wärmebeständigkeit, großer chemischer Stabilität und guter mechanischer Festigkeit zu erhalten. The inventive implementation of the polymerization makes it possible practically in quantitative yield an elastomer of high heat resistance, great chemical stability and good mechanical strength.

Die Reaktion verläuft nach folgendem Schema: Man erhält dabei ein Polymeres (ein Elastomeres) mit einem Molekulargewicht von 2-105 bis 6 106.The reaction proceeds according to the following scheme: A polymer (an elastomer) with a molecular weight of 2-105 to 6,106 is obtained.

Nachfolgend wird das Verfahren an Hand von Ausführungsbeispielen näher erläutert. The method is described below on the basis of exemplary embodiments explained in more detail.

Beispiel 1 25 g 1,1,3,3 -Tetramethyl- 1,3 -disilicacyclobutan, welches von anhaftender Luft bei 10-3 mm Hg über metallischem Kalium befreit worden war, wird in eine Ampulle im Vakuum von 10-3 mm Hg destilliert die Ampulle zugeschmolzen und 6 Stunden lang erhitzt. Example 1 25 g of 1,1,3,3-tetramethyl-1,3-disilicacyclobutane which had been freed of adhering air at 10-3 mm Hg above metallic potassium, is distilled in an ampoule in a vacuum of 10-3 mm Hg, the ampoule is melted shut and heated for 6 hours.

Nach der Polymerisation erhält man 17,5 g Silylmethylenelastomeres (die auf das Ausgangsmonomere bezogene Ausbeute beträgt 700/0), welches ein Molekulargewicht von 4. 10-6 (ermittelt nach Lichtstreuungsmethode) aufweist. After the polymerization, 17.5 g of silylmethylene elastomer are obtained (the yield based on the starting monomer is 700/0), which is a molecular weight of 4. 10-6 (determined by the light scattering method).

Beispiel 2 25 g 1,1,3,3 - Tetramethyl - 1,3 - disilicacyclobutan, welches von der anhaftenden Luft bei 10 mm Hg über metallischem Kalium befreit worden war, wird in eine Ampulle im Vakuum von 10 mm Hg destilliert, die Ampulle zugeschmolzen und 6 Stunden lang erhitzt. Example 2 25 g 1,1,3,3 - tetramethyl - 1,3 - disilicacyclobutane, which has been freed from the adhering air at 10 mm Hg over metallic potassium was, is distilled in an ampoule in a vacuum of 10 mm Hg, the ampoule is sealed and heated for 6 hours.

Nach der Polymerisation erhält man 22g Silylmethylenelastomeres (die auf das Ausgangsmonomere bezogene Ausbeute beträgt 900/0), welches ein Mole- kulargewicht von 4 105 (ermittelt nach Lichtstreuungsmethode) aufweist. After the polymerization, 22 g of silylmethylene elastomer (the based on the starting monomer yield is 900/0), which is a mol gross weight of 4 105 (determined by the light scattering method).

Als Trocknungsmittel kommen Na, LiH, CaH sowie beliebige starke Wasserbindungsmittel in Frage. The drying agents used are Na, LiH, CaH and any strong water-binding agents in question.

Claims (2)

Patentansprüche: 1. Verfahren zur Herstellung von elastomeren Silylmethylenpolymeren der allgemeinen Formel durch Polymerisation von 1,1,3,3-Tetramethyl-1,3-disilicacyclobutan unter Erhitzen, d a d u r c h g e k e n n ze i ch n e t, daß man ein 1,1,3,3-Tetramethyl-1,3-disilicacyclobutan verwendet, das vorher mit einem starken Trocknungsmittel bei 10 bis 10-3 mm Hg getrocknet worden ist, und die Polymerisation unterhalb 250"C im Vakuum oder in einer inerten Atmosphäre durchführt.Claims: 1. Process for the production of elastomeric silylmethylene polymers of the general formula by polymerization of 1,1,3,3-tetramethyl-1,3-disilicacyclobutane with heating, characterized in that one uses a 1,1,3,3-tetramethyl-1,3-disilicacyclobutane that was previously with has been dried with a strong desiccant at 10 to 10-3 mm Hg, and the polymerization is carried out below 250 "C in a vacuum or in an inert atmosphere. 2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß man die Polymerisation bei 150 bis 200"C durchführt. 2. The method according to claim 1, characterized in that the Polymerization at 150 to 200 "C is carried out.
DEJ27841A 1965-04-06 1965-04-06 Process for the preparation of elastomeric silylmethylene polymers Pending DE1226310B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
DEJ27841A DE1226310B (en) 1965-04-06 1965-04-06 Process for the preparation of elastomeric silylmethylene polymers

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DEJ27841A DE1226310B (en) 1965-04-06 1965-04-06 Process for the preparation of elastomeric silylmethylene polymers

Publications (1)

Publication Number Publication Date
DE1226310B true DE1226310B (en) 1966-10-06

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Family Applications (1)

Application Number Title Priority Date Filing Date
DEJ27841A Pending DE1226310B (en) 1965-04-06 1965-04-06 Process for the preparation of elastomeric silylmethylene polymers

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DE (1) DE1226310B (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2708635A1 (en) * 1976-02-28 1977-09-01 Res Inst Iron Steel ORGANOSILIC COMPOUNDS WITH HIGH MOLECULAR WEIGHT, PROCESS FOR THE PRODUCTION OF THE SAME SILICON CARBIDE SHAPED BODIES

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2708635A1 (en) * 1976-02-28 1977-09-01 Res Inst Iron Steel ORGANOSILIC COMPOUNDS WITH HIGH MOLECULAR WEIGHT, PROCESS FOR THE PRODUCTION OF THE SAME SILICON CARBIDE SHAPED BODIES
DE2760031C2 (en) * 1976-02-28 1990-05-17 The Research Institute For Iron, Steel And Other Metals Of The Tohoku University, Sendai, Jp

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