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Process for preparing shelf-stable curable polysilazanes, and polysilazanes prepared thereby

A technology of polysilazane and dihalosilane, which is applied in the field of preparing curable polysilazane-containing compositions, can solve problems such as high cost and large odor, and achieve convenient purification, easy storage, and high industrial compatibility Effect

Inactive Publication Date: 2012-09-12
3M INNOVATIVE PROPERTIES CO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0013] Although the use of pyridine has numerous disadvantages (such as greater odor, higher cost, hydrophilicity, and boiling point), methods for the preparation of perhydropolysilazanes and copolysilazanes generally involve relatively large excesses of Use of pyridine (e.g. at least about 12 times the stoichiometric amount of silicon-halogen bonds in the starting silane)

Method used

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  • Process for preparing shelf-stable curable polysilazanes, and polysilazanes prepared thereby
  • Process for preparing shelf-stable curable polysilazanes, and polysilazanes prepared thereby
  • Process for preparing shelf-stable curable polysilazanes, and polysilazanes prepared thereby

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preparation example Construction

[0057] Preparation of dihalosilane-base adducts

[0058] Dihalosilane-base adducts can be prepared by combining at least one of the aforementioned dihalosilanes with at least one of the aforementioned bases. Dihalosilanes can react with bases to form adducts, and the rate of formation and their stability may depend on the acidity of the dihalosilanes and the basicity of the base. The dihalosilane and base can be selected so as to produce an adduct that is stable enough to serve as a reaction intermediate capable of reacting with ammonia or primary amines. In particular, one mole of dichlorosilane is known to react with two moles of pyridine to form a 1:2 (halide:base) adduct or with one mole of tetramethylethylenediamine to form a 1:1 adduct (as e.g. H.J.Campbell-Ferguson and E.A.V.Ebsworth described in J.Chem.Soc. (A), 1966,1508, its relevant adduct description content is incorporated herein by reference; According to Campbell-Ferguson and Ebsworth described, with Substit...

example

[0092] Objects and advantages of this invention are further illustrated by the following examples, but the particular materials and amounts thereof recited in these examples, as well as other conditions and details, should not be construed to unduly limit this invention. These examples are for illustrative purposes only and are not intended to limit the scope of the appended claims.

[0093] All parts, percentages, ratios, etc. in the examples, as well as in the remainder of the specification, are by weight unless otherwise indicated. Solvents and other reagents used were obtained from Aldrich Chemical Company, Milwaukee, WI unless otherwise indicated.

[0094] Material

[0095] Hexane was obtained from Aldrich Chemical Company, Milwaukee, WI.

[0096] Anhydrous pyridine was obtained from Aldrich Chemical Company, Milwaukee, WI.

[0097] Dichlorosilane (25% by weight in xylene) was obtained from Gelest, Inc., Morrisville, PA.

[0098] Methyldichlorosilane was obtained fr...

example 1 and comparative example A

[0106] preparation

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Abstract

A process for preparing curable oligomeric and / or polymeric polysilazanes comprises (a) forming at least one dihalosilane-base adduct by reacting at least one dihalosilane with at least one base; (b) optionally, combining at least one dihalosilane-base adduct and at least one organodihalosilane; and (c) carrying out ammonolysis of at least one dihalosilane-base adduct or of the resulting combination of at least one dihalosilane-base adduct and at least one organodihalosilane; with the proviso that the base (1) is used for the dihalosilane-base adduct formation in a limited amount that is less than or equal to twice the stoichiometric amount of silicon-halogen bonds in the dihalosilane or (2) is used for the dihalosilane-base adduct formation in excess of this limited amount and, prior to the ammonolysis, the total amount of the resulting reacted and unreacted base is reduced to no more than this limited amount.

Description

[0001] priority statement [0002] This patent application claims priority to US Provisional Patent Application No. 61 / 289,101, filed December 22, 2009, the contents of which are hereby incorporated by reference. technical field [0003] The present invention relates to a process for the preparation of curable polysilazane-containing compositions and, in another aspect, to the compositions thus prepared. Background technique [0004] Ceramic materials are well known and widely used in different applications due to some of their outstanding properties, such as relatively high modulus, hardness, high temperature stability and / or chemical resistance. However, ceramic materials can also be relatively heavy, brittle and / or difficult to process. Organic polymers, on the other hand, may be relatively tough, flexible, lightweight and / or easy to make and process, but their relatively low modulus and relatively low decomposition temperature prevent their use in some applications. P...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/62
CPCC08G77/62
Inventor 杨宇乔治·G·I·莫尔
Owner 3M INNOVATIVE PROPERTIES CO
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