Synthetic method of B-trichloroborazine

A technology of trichloroborazine and a synthesis method, which is applied in the field of synthesis of trichloroborazane, can solve the problems of difficult boron trichloride feeding amount, difficult experimental operation, low product synthesis yield and the like, and achieves the The effect of improving the utilization rate of boron source, easy mass production, and improving synthesis yield
CN101607715BInactive Publication Date: 2010-09-22NAT UNIV OF DEFENSE TECH
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
NAT UNIV OF DEFENSE TECH
Publication Date
2010-09-22
Estimated Expiration
Not applicable · inactive patent

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Abstract

The invention discloses a synthetic method of B-trichloroborazine, which comprises the following steps of: fully and evenly mixing dimethyl sulphide boron trichloride complex and inorganic ammonium salt compound according to a mole ratio of an element B to an element N in the material of 1:1 to 3:1 and then dispersing the mixture in an organic solvent; adding the dispersed turbid liquor into a reactor with a stirring and low-temperature condensing back flow device, carrying out synthetic reaction for 10 to 20 hours under the conditions of temperature of 110 to 150 DEG C and violent stirring after vacuumization and filling dried nitrogen; carrying out condensing back flow when the temperature of the outlet end is controlled to -20 to -10 DEG C; and cooling the temperature to room temperature, filtering, recovering the organic solvent by reducing pressure and distilling, and obtaining the colourless needle crystal product. The synthetic method releases boron trichloride slowly by complex dissociation reaction of the dimethyl sulphide boron trichloride at the reaction temperature, and improves synthetic yield and boron utilization ratio, the material throwing amount is easy to accurately calculated, the technique equipment is simple and large-scale production is easy to realize.
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Description

technical field

[0001] The invention relates to a synthesis method of trichloroborazine. Background technique

[0002] Boron nitride fiber has excellent characteristics such as high temperature resistance, chemical corrosion resistance, excellent dielectric properties, good electrical insulation, and good thermal conductivity, and has broad application prospects in cutting-edge technical fields such as aviation, aerospace, electric power, and electronics. And trichloroborazine (B-trichloroborazine, referred to as TCB) and its derivatives are ideal intermediates for the preparation of high-performance boron nitride ceramic fibers by the precursor conversion method. The existing synthetic method of trichloroborazine has Brown etc., is to place the dry ammonium chloride powder in the long glass tube of heating, simultaneously the boron trichloride air flow is slowly passed through the tube, thereby preparing a small amount of trichloroborazine Azane, the yield is only 35% (J. ...

Claims

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