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Preparation device of polysilazane and preparation method thereof

A technique for preparing polysilazane and equipment, which is applied in chemical instruments and methods, chemical/physical/physicochemical fixed reactors, chemical/physical/physicochemical processes, etc., and can solve the problem of continuous production equipment that does not have a large scale , the by-product reaction rate is greatly affected, and the by-product hinders the reaction, etc., to achieve the effects of improving production efficiency, controlling the reaction rate, and shortening the reaction time

Pending Publication Date: 2019-04-16
718TH RES INST OF CHINA SHIPBUILDING INDAL CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Polysilazane has high chemical reactivity and high heat resistance temperature, and is an important raw material for the preparation of silicon nitride and silicon carbon ceramic precursors. Large-scale continuous production equipment; raw material high-purity ammonia reacts in excess, direct discharge is not only wasteful, but also pollutes the environment; by-products have a greater impact on the reaction rate, and the problem of by-products hindering the reaction is difficult to solve

Method used

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  • Preparation device of polysilazane and preparation method thereof
  • Preparation device of polysilazane and preparation method thereof
  • Preparation device of polysilazane and preparation method thereof

Examples

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Embodiment 1

[0056] The inner diameter of the double-layer tubular reactor 8 in this embodiment is 100 mm, the outer diameter is 140 mm, and the height is 1200 mm.

[0057] A method for preparing polysilazane (with a purity of 95% and a number average molecular weight of 400) using the device of the present invention, the steps of the method are as follows:

[0058] Step S1: transporting nitrogen gas from the gas supply unit to the double-layer tubular reactor 8, purging the device, keeping the device in a nitrogen environment, and eliminating the influence of air moisture and the like;

[0059] Step S2: The cooling device 25 delivers -35°C ethylene glycol cooling liquid to the interlayer of the double-layer tubular reactor 8;

[0060] Step S3: Mix dimethyldichlorosilane and solvent n-hexane according to the volume ratio of 1:10 and add them to the raw material liquid supply device 1, and under the action of the raw material liquid delivery pump 2, transport 26 to the double In the upper ...

Embodiment 2

[0068] The inner diameter of the double-layer tubular reactor 8 in this embodiment is 100 mm, the outer diameter is 140 mm, and the height is 1200 mm.

[0069] A method for preparing polysilazane (with a purity of 98% and a number average molecular weight of 600) using the device of the present invention, the steps of the method are as follows:

[0070] Step S1: transporting nitrogen gas from the gas supply unit to the double-layer tubular reactor 8, purging the device, keeping the device in a nitrogen environment, and eliminating the influence of air moisture and the like;

[0071] Step S2: The cooling device 25 delivers -35°C cooling liquid (mixed solution of glycerol and water) to the interlayer of the double-layer tubular reactor 8;

[0072] Step S3: Mix dimethyldichlorosilane and tetrahydrofuran as a solvent according to a volume ratio of 1:20 and add them to the raw material liquid supply device 1, and transport them to the upper part of the double-layer tubular reactor ...

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Abstract

The invention belongs to the field of chemical engineering and particularly relates to a preparation device of polysilazane and a preparation method thereof. The preparation device comprises a double-layer tubular reactor, a raw material liquid supply device, a gas supply unit, a cooling device, a product separator, a byproduct collection device, a product fractionation device, a solvent collection device, and a polysilazane collection device. The crude product obtained after reaction is fed into the product separator through a lower end opening of the tubular reactor, and unreacted high-purity ammonia gas and the mixed liquid are delivered back to the reactor for circular reaction while the by-product is separated. Full utilization of the raw materials is achieved, raw material waste is greatly reduced, and the conversion rate is improved; the by-product in the preparing process can be effectively separated in time, the shortcoming is avoided that a large amount of by-products in a kettle-type reactor hinders the contact between ammonia gas and raw material liquid, the reaction time is shortened, and the production efficiency is improved.

Description

technical field [0001] The invention belongs to the field of chemical industry, and in particular relates to a polysilazane preparation device and a preparation method thereof. Background technique [0002] Polysilazane has high chemical reactivity and high heat resistance temperature, and is an important raw material for the preparation of silicon nitride and silicon carbon ceramic precursors. Large-scale continuous production equipment; raw material high-purity ammonia reacts in excess, direct discharge is not only wasteful, but also pollutes the environment; by-products have a greater impact on the reaction rate, and the problem of by-products hindering the reaction is difficult to solve. Contents of the invention [0003] In view of this, the object of the present invention is to provide a preparation device capable of continuous production of polysilazane and a preparation method thereof, which fully improves the utilization rate of raw materials and the yield of prod...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/62B01J19/24
CPCB01J19/2465C08G77/62
Inventor 商轶刘保锋石晶王峰蔡淑红陈培红姜燕杨品苏玲燕
Owner 718TH RES INST OF CHINA SHIPBUILDING INDAL CORP
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