Method for producing thermoplastic pre-ceramic polymers

Patent metadata

Field	Value
Publication number	US-9745423-B2
Application number	US-201314424024-A
Country	US
Kind code	B2
Filing date	Sep 4, 2013
Priority date	Aug 30, 2012
Publication date	Aug 29, 2017
Grant date	Aug 29, 2017

Abstract

A method for producing high-molecular weight, solid, meltable, thermoplastic, pre-ceramic polymers by converting liquid low-molecular weight polysilazanes in a solvent, in the presence of a catalyst, and a stopping reagent stopping the reaction as soon as the desired degree of polymerization is achieved. The obtained polysilazanes can be processed by conventional industrial methods, such as, for example, extrusion, injection molding, melt spinning, calendering, film and hollow body blowing, rotational molding, fluidized bed sintering, flame spraying and transfer molding (RTM and DP RTM).

First claim

What is claimed is:

1. A method for producing high molecular weight solid, meltable thermoplastic pre-ceramic polymers, having a molecular weight of at least 2000 g/mol to 2 million g/mol, comprising the step of reacting one or more liquid low molecular weight polysilazanes, having a number-average molecular weight of 150 to 150 000 glmol, in a solvent, in the presence of a catalyst by stopping the reaction with a stopping reagent as soon as the desired degree of polymerization is attained, wherein chlorides, bromides, iodides, fluorides and hydroxides of tetraalkyl-substituted ammonium salts are used as the catalyst.

2. The method as claimed in claim 1 , wherein the one or more polysilazanes are of the general formula (1)
—(SiR′R″—NR′″) n —  (1)

where R′, R″ and R′″ are the same or different and each independently are hydrogen or an optionally substituted alkyl, aryl, vinyl or (trialkoxysilyl)alkyl radical, where n is an integer such that the polysilazane has a number-average molecular weight of 150 to 150 000 g/mol.

3. The method as claimed in claim 2 , wherein R′, R″ and R′″ each independently is a radical selected from the group consisting of hydrogen, methyl, ethyl, propyl, isopropyl, butyl, isobutyl, tert-butyl, phenyl, tolyl, vinyl, 3-(triethoxysilyl)propyl and 3-(trimethoxysilylpropyl).

4. The method as claimed in claim 1 , wherein the one or more polysilazanes are perhydropolysilazanes of formula (2)

where n is an integer such that the polysilazane has a number-average molecular weight of 150 to 150 000 g/mol.

5. The method as claimed in claim 1 , wherein the concentration of the catalyst in the reaction mixture is in the range from 0.01 wt % and 10 wt %.

6. The method as claimed in claim 1 , wherein the solvent comprises organic solvents containing no water and also no reactive groups.

7. The method as claimed in claim 1 , wherein the concentration of the starting materials in the reaction medium is in the range of 20-80 wt %.

8. The method as claimed in claim 1 , wherein the solvent comprises aliphatic or aromatic hydrocarbons.

9. A method for producing high molecular weight solid, meltable thermoplastic pre-ceramic polymers, having a molecular weight of at least 2000 g/mol to 2 million g/mol, comprising the step of reacting one or more liquid low molecular weight polysilazanes, having a number-average molecular weight of 150 to 150 000 g/mol, in a solvent, in the presence of a catalyst by stopping the reaction with a stopping reagent as soon as the desired degree of polymerization is attained, wherein hydrides of alkali and alkaline earth metals are used as the stopping reagent.

Assignees

• Clariant Int Ltd
• Clariant Int Ltd

Inventors

• Richter Frank
• Krichel Matthias
• Decker Daniel
• Motz Guenter
• Schmalz Thomas

Classifications

• C08G77/62 Primary

  Nitrogen atoms · CPC title