Liquid ethylene based polysilazane resin and preparation thereof

A technology of vinyl polysilazane and methyl vinyl dichlorosilane, which is applied in the field of liquid vinyl polysilazane resin and its preparation, and can solve the problem that the viscosity is difficult to meet the requirements of ceramic precursors

Inactive Publication Date: 2009-01-28
NORTHWESTERN POLYTECHNICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because the viscosity of these two types of products is difficult to meet the requirements of prepari

Method used

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  • Liquid ethylene based polysilazane resin and preparation thereof
  • Liquid ethylene based polysilazane resin and preparation thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Example 1: The formula is 0.5 mol (70.5 grams) of methyl vinyl dichlorosilane, 0.15 mol (17.3 grams) of methyl hydrogen dichlorosilane, 500.0 grams of n-hexane, and platinum complex of divinyl tetramethyl disiloxane Compound (platinum content is 0.04mol / L) 0.18 grams.

[0024] Preparation:

[0025] Add the raw materials methylvinyldichlorosilane, methylhydrogendichlorosilane and n-hexane according to the ratio into a 1000mL four-neck flask equipped with a thermometer and a stirrer, put it in an ice-water bath, and start the stirrer to mix the raw materials evenly. Then feed ammonia gas at a flow rate of 15-20 L / h, keep the temperature of the reaction solution at -5°C, and react for 2.5 hours. After the ammonia gas flow was stopped, the ice bath was removed. After the reaction returned to room temperature, the product was filtered to remove the generated salt. The filtrate was de-hexaned at 85°C and 500mmHg, and the solvent was collected for recycling. When no solvent ...

Embodiment 2

[0029] Embodiment 2: formula is methylvinyl dichlorosilane 0.5mol (70.5 grams), methylhydrogen dichlorosilane 0.2mol (23.0 grams), normal hexane 600.0 grams, chloroplatinic acid isopropanol catalyst (platinum content is 0.04 mol / L) 0.18 g.

[0030] Add the raw materials methylvinyldichlorosilane, methylhydrogendichlorosilane and n-hexane according to the ratio into a 1000mL four-neck flask equipped with a thermometer and a stirrer, put it in an ice-water bath, and start the stirrer to mix the raw materials evenly. Then feed ammonia gas at a flow rate of 15-20 L / h, keep the temperature of the reaction solution at -5°C, and react for 2.5 hours. After the ammonia gas flow was stopped, the ice bath was removed. After the reaction returned to room temperature, the product was filtered to remove the generated salt. The filtrate was de-hexaned at 85°C and 500mmHg, and the solvent was collected for recycling. When no solvent flows out, add platinum-based catalyst chloroplatinic acid ...

Embodiment 3

[0034] Example 3: The formula is 0.5 mol (70.5 grams) of methyl vinyl dichlorosilane, 0.2 mol (23.0 grams) of methyl hydrogen dichlorosilane, 500.0 grams of cyclohexane, platinum divinyl tetramethyl disiloxane 0.25 g of the complex (platinum content is 0.04 mol / L).

[0035] Add the raw materials methylvinyldichlorosilane, methylhydrogendichlorosilane and cyclohexane according to the ratio into a 1000mL four-neck flask equipped with a thermometer and a stirrer, put it in an ice-water bath, and start the stirrer to mix the raw materials evenly. Then feed ammonia gas at a flow rate of 15-20 L / h, keep the temperature of the reaction solution at -5°C, and react for 2.5 hours. After the ammonia gas flow was stopped, the ice bath was removed. After the reaction returned to room temperature, the product was filtered to remove the generated salt. The filtrate was de-hexaned at 85°C and 500mmHg, and the solvent was collected for recycling. When no solvent flows out, add the platinum ca...

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Abstract

The invention relates to a preparation method of liquid vinyl poly-silazane resin. The technique is characterized in that: by controlling the proportion of aminolysis-raw material methyl vinyl dichlorsilane and methyl hydrogen dichlorsilane in the preparation method, a hexahydric or octatomic ring-shaped vinyl silazane mixture which is provided with a Si-H bond and 2 to 3 vinyl double bonds on a ring body is synthesized; and by the additive reaction of platina-series catalyst catalyzed silicon hydride and the vinyl double bonds, the vinyl poly-silazane resin which has a branched structure and proper viscosity is polymerized by the micro-molecule silazane mixture. The vinyl poly-silazane resin prepared by the method of the invention has the advantages that: the yield thereof can achieve 44-50 percent of the usage of chlorosilane, the M thereof can be up to 4500 shown by the analysis of gel permeation chromatography (GPC) and the molecular weight dispersion coefficient thereof is within 1.5-3.4. In addition, the viscosity is within 300-2000mPa question mark s( 25 DEG C, tested by a rotation viscometer).

Description

technical field [0001] The invention relates to a liquid vinyl polysilazane resin and a preparation method thereof, belonging to the synthesis method of liquid vinyl polysilazane. Background technique [0002] Silicon nitride and silicon nitride / silicon carbide composite ceramic materials can be prepared by pyrolysis conversion method using polymer ceramic precursors containing silicon, nitrogen and (or) carbon elements. The preparation of ceramic materials by this method has the advantages of adjustable composition of silazane precursors and general polymer processing methods. It has broad application prospects in aerospace thermal protection, ceramic fiber preparation and other fields. [0003] The currently used organosilazane products containing active groups (such as vinyl, etc.) can be divided into two categories in terms of molecular weight and state. One type is small molecule organosilazane, the molecular weight is generally below 500g / mol, and the viscosity of th...

Claims

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Application Information

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IPC IPC(8): C08G77/62
Inventor 陈立新宋家乐
Owner NORTHWESTERN POLYTECHNICAL UNIV
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