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

Inactive Publication Date: 2010-09-22
NAT UNIV OF DEFENSE TECH
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Problems solved by technology

However, since boron trichloride is gaseous at room temperature, it is very easy to be hydrolyzed in the air, and it is extremely corrosive, which requires high requirements for experimental equipment; and it is not easy to accurately measure the amount of boron trichloride in the experimental process, and the experimental operation is difficult. Large, while directly feeding boron trichloride gas, it is easy to volatilize in the reaction process, causing a large amount of boron trichloride loss, resulting in low product synthesis yield

Method used

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  • Synthetic method of B-trichloroborazine

Examples

Experimental program
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Effect test

Embodiment 1

[0018] (1) 95.7g dimethylsulfur boron trichloride ((CH 3 ) 2 S·BCl 3 ) and 20g ammonium chloride (NH 4 C1) The powder is placed in a 1000ml flask after being fully mixed directly, and 500ml of toluene is added and mixed uniformly;

[0019] (2) Add the above-mentioned dispersed turbid liquid into the reactor with magnetic stirring and low-temperature condensation reflux device, repeatedly vacuumize and fill dry nitrogen at least three times to get rid of the air and moisture in the reaction device, then slowly raise the temperature to 110°C, While vigorously stirring, condense and reflux at the outlet end at a low temperature of -20 to -10°C for 15 hours.

[0020] (3) cooling to room temperature, filtering, and recovering the organic solvent toluene through vacuum distillation to obtain 21.7 g of colorless needle-like crystal product with a yield of 94.8% and a boron source utilization rate of 66.3%.

[0021] The appearance of the product obtained in Example 1 is white need...

Embodiment 2

[0023] (1) 99.5g dimethylsulfur boron trichloride ((CH 3 ) 2 S·BCl 3 ) and 25g ammonium sulfate ((NH 4 ) 2 SO 4 ) powder is placed in a 1000ml flask after being fully mixed directly, and 500ml of chlorobenzene is added and mixed evenly;

[0024] (2) Add the above-mentioned dispersed turbid liquid into the reactor with ultrasonic dispersion stirring and low-temperature condensation reflux device, repeatedly vacuumize and fill with dry nitrogen at least three times to remove the air and moisture in the reaction device, and then slowly heat up to 130°C and violently The synthesis reaction was carried out under the condition of stirring, and at the same time, it was condensed and refluxed at the outlet end at a low temperature of -20~-10°C for 12 hours; after the reaction was completed, chlorobenzene was recovered by filtration and vacuum distillation to obtain 21.3 g of a colorless needle-shaped crystal product, with a yield of 91.7%, boron source utilization rate 62.6%.

Embodiment 3

[0026] (1) 95.0g dimethylsulfur boron trichloride ((CH 3 ) 2 S·BCl 3 ) and 20g ammonium chloride (NH 4 C1) The powder is placed in a 1000ml flask after being fully mixed directly, and 500ml xylene is added and mixed evenly;

[0027] (2) Add the above-mentioned dispersed turbid liquid into the reactor with high-speed mechanical stirring and low-temperature condensation reflux device, repeatedly vacuumize and fill with dry nitrogen at least three times to remove the air and moisture in the reaction device, and then slowly raise the temperature to 140°C, While vigorously stirring, condense and reflux at the outlet end at a low temperature of -20 to -10°C for 12 hours. After the reaction was completed, the xylene was recovered by filtration and vacuum distillation to obtain 21.4 g of a colorless needle crystal product with a yield of 93.3% and a boron source utilization rate of 65.8%.

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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.

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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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F5/05C01B35/14
Inventor 宋永才邓橙王应德李义和雷永鹏谢征芳王军
Owner NAT UNIV OF DEFENSE TECH
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