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Preparation method and application of polysilazane material

A technology of polysilazane and synthesis method, applied in the direction of coating and the like, can solve the problems of inability to meet the application of polysilazane, harsh conditions, low molecular weight of polysilazane polymer, etc., so as to improve the polysilazane material. Molecular weight, mild reaction conditions, effect of promoting cross-linking reaction

Active Publication Date: 2019-04-16
大晶信息化学品(徐州)有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, the conditions of the above method are harsh, and the obtained polysilazane polymer has a low molecular weight, which cannot meet the requirements of the existing polysilazane as a coating material.

Method used

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  • Preparation method and application of polysilazane material

Examples

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Effect test

preparation example 1

[0011] Preparation example 1: Preparation of polysilazane pyridine solution for experiment:

[0012] Add dry pyridine to a glass reactor with a gas conduit, a condenser, and a stirrer, and add dichlorosilane to form a white solid complex (SiH 2 Cl 2 -2C 5 h 5 N), while stirring, introduce ammonia gas through the drying tube to carry out the ammonolysis reaction for 2-3h. After the reaction is completed, the by-product ammonium chloride is removed by vacuum filtration to obtain a polysilazane pyridine solution.

Embodiment 1

[0014] Dilute the polysilazane pyridine solution of Preparation Example 1 with an organic mixed solvent of pyridine and xylene, dilute to the second polysilazane solution with a solid content of polysilazane of 5%, add polysilazane mass 0.3% of the initiator azobisisobutyronitrile, after stirring and dissolving, pass a dry nitrogen flow into the reaction system, heat to 40°C and stir for half an hour, then raise the temperature to 50°C, and react at 50°C for 4 hours Cool to room temperature, obtain high molecular weight polysilazane material by distillation replacement.

Embodiment 2

[0016] Dilute the polysilazane solution of Preparation Example 1 with an organic mixed solvent of pyridine and xylene, dilute to the second polysilazane solution with a solid content of polysilazane of 10%, and add 0.3% of the mass of polysilazane % of the initiator azobisisobutyronitrile, stirred and dissolved, passed a dry nitrogen flow into the reaction system, heated to 50°C, stirred and reacted for 4 hours, cooled to room temperature, and obtained high molecular weight polysilazane material by distillation replacement.

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Abstract

The invention relates to the field of polymer materials, in particular to a preparation method and application of a polysilazane material. The method comprises the following specific steps of obtaining a first polysilazane solution by means of a preset synthesis method; diluting the first polysilazane pyridine solution with an organic solvent to obtain a second polysilazane solution; adding an initiator into the second polysilazane pyridine solution and stirring the mixture for a reaction to obtain the polysilazane material. According to the preparation method, the initiator capable of generating free radicals is added into the polysilazane solution, so that a crosslinking reaction among small-molecule polysilazanes is promoted, the reaction conditions are mild, and the molecular weight ofthe polysilazane material is further increased.

Description

technical field [0001] The invention relates to the field of polymer materials, in particular to a preparation method and application of a polysilazane material. Background technique [0002] Polysilazane material (hereinafter referred to as PHPS) is a series of polymer materials with silicon and nitrogen combination. There are mainly inorganic silazanes with only hydrogen atoms substituted on silicon atoms except nitrogen, organic silazanes with organic groups on silicon atoms and copolymers of inorganic silazanes. [0003] The existing polysilazane preparation mainly includes butyllithium reaction method, dialkyldihalosilane ammonolysis reaction, anionic ring-opening polymerization and cationic ring-opening polymerization, such as N, N'-diphenyltetramethoxy ring The reaction between disilazane and phenylenediamine at 200°C can produce oligomeric nitrogen silane, and for example, under the catalysis of potassium ions, octamethylcyclotetrasilazane undergoes ring-opening pol...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/62C09D183/16
CPCC08G77/62C09D183/16
Inventor 康文兵
Owner 大晶信息化学品(徐州)有限公司
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