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Novel silizane and/or polysilazane compounds and methods of making

A technology for polysilazane and silazane is applied in the field of preparation of aminolysis products, and can solve the problems of difficult pyrolysis to form ceramic materials, low yield of polysilazane, etc.

Inactive Publication Date: 2003-01-08
AZ ELECTRONICS MATERIALS LUXEMBOURG R L
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, most of the prepared organocyclosilazanes are limited by the starting compounds to only have 3-4 Si-N bonding units, and the yield of polysilazane is low
Also, the silazanes produced are volatile and difficult to pyrolyze to form ceramic materials

Method used

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  • Novel silizane and/or polysilazane compounds and methods of making
  • Novel silizane and/or polysilazane compounds and methods of making
  • Novel silizane and/or polysilazane compounds and methods of making

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0139] Ammonolysis of methyl dichlorosilane using the inventive method

[0140] The 6 liter pressure reactor was filled with 2.5 liters of commercial grade anhydrous liquid ammonia. Ammonia was transferred directly from the bulk tank without additional purification. The pressure reactor is equipped with thermometer and pressure gauge. For mixing, a circulating reflux pump draws liquid from the bottom of the reactor and injects it below the surface of the liquid ammonia in the upper part of the reactor.

[0141] Methyldichlorosilane (237.2 g, 2.06 mol) was kept in a glass pressure tube, blanketed with nitrogen, and maintained at 100 psig above the expected reactor pressure.

[0142] The ammonia was vented from the reactor to cool the system to -6°F. Methyldichlorosilane was added to the reactor in batches until the heat released by the reaction raised the pressure in the reactor to a predetermined height (about 70 psi). The methyldichlorosilane feed was then stopped and the r...

Embodiment 3

[0152] Preparation and polymerization of tetramethyldisilazane using the method of the present invention

[0153] The 6 liter pressure reactor was filled with 4 liters of commercial grade refrigerated (-30°) anhydrous liquid ammonia. About 1 kg (7.5 moles) of dimethylchlorosilane was added to the addition tank, which was pressurized with nitrogen to about 160 psi. Dimethylchlorosilane is added to anhydrous liquid ammonia using the pressure difference between the two tanks. After about half of the halosilane had been charged with anhydrous liquid ammonia, the reactor was vented to reduce the pressure and further freeze the system. The remainder of the halosilane was added over about 30 minutes to complete the addition. The reaction vessel was stirred for about 10 minutes, then the stirring was stopped. The reaction mixture spontaneously separated into two distinct layers. Samples are taken from the upper layer and any dissolved ammonia is distilled off. A clean sample was ...

Embodiment 4

[0158] Further Polymerization of a Known Silazane - Methylhydromethylvinylpolysilazane

[0159] A sample of methylhydrogenatedmethylvinylpolysilazane with available Si-H bonds, as shown in the following structure, where R is methylvinyl, was prepared by the prior art method outlined in Example 2.

[0160] Add the prepared sample to anhydrous liquid ammonia and a catalytic amount of NH 4 Cl mixture to further polymerize the sample. figure 2 is the control FTIR spectrum of methylhydrogenmethylvinylpolysilazane before polymerization treatment and after 25 hours of treatment. observe figure 2 When the middle time is 0 ≈ 1500cm -1 (dotted line), it is clear that methylhydrogenmethylvinylpolysilazane is initially at ≈1500cm -1 With limited amine (NH 2 ) functionality. After 25 hours in liquid ammonia solution containing ionized acid catalyst (solid line), ≈1500cm -1 The amine functionality at the position increases significantly, such as ≈2120cm -1 Si-H bond reduction show...

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Abstract

This invention is directed to novel ammonolysis products including novel silazanes and polysilazanes characterized by repeating units of silicon-nitrogen in a polymeric compound having a reduced amount of Si-H bonds relative to the amount of Si-H bonds in the starting compound. Preparation of these novel ammonolysis products comprises introducing a starting compound containing at least one Si-H bond, such as a halosilane into a stoichiometric excess of anhydrous liquid ammonia wherein an ammonium halide is generated acting as an acid catalyst to provide an ionic and / or acidic environment for preparing the novel ammonolysis compounds. The prepared novel ammonolysis products are retained in a separated liquid-phase layer and distinct from the anhydrous liquid ammonia containing the ionized ammonium halide. Also provided are methods to purify ammonolysis products and to modify ammonolysis products by controllably increasing viscosity from a liquid to a solid and viscosities there between.

Description

technical field [0001] The present invention relates to the preparation of ammonolysis products, more particularly to the synthesis of novel silazane and / or polysilazane compounds, including monomers, oligomers and polymers containing Si-N structures in their molecules. Background of the invention [0002] Silazanes, which have a Si-N-Si bond configuration, are becoming increasingly important due to their pyrolysis to produce ceramic materials such as silicon carbide and silicon nitride. [0003] Silazanes are usually synthesized by the ammonolysis method, in which ammonia or primary amines are reacted with halosilanes. Ammonolysis of organohalosilanes is a complex process consisting of several concurrent reactions shown below. These formulas do not imply specific structures, they are just general formulas used to illustrate reactions such as the following: [0004] replace: [0005] As well as homofunctional and heterofunctional condensations. with [0006] The pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07B61/00C07F7/10C07F7/21C08G77/62
CPCC07F7/21C08G77/62
Inventor 艾伯特·E·埃布尔特蕾西·A·克鲁格罗伯特·W·莫克加里·J·纳西亚克
Owner AZ ELECTRONICS MATERIALS LUXEMBOURG R L
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