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Method and device for preparing borazine

A technology of borazine and sodium borohydride, applied in the field of mechanochemical methods for synthesizing borazine and devices thereof, can solve the problems of complex, dangerous, highly toxic and the like, and achieves low synthesis cost, simple equipment and environmental pollution. low pollution effect

Inactive Publication Date: 2013-07-24
NAT UNIV OF DEFENSE TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But the raw material diborane B2H6 used in this method is highly toxic, can spontaneously combust, and is very dangerous, and the equipment used in this method is complicated, which is not conducive to industrial scale production
The Mine Safety Appliances Company of the United States developed a method for preparing borazine with borane-ammonia complex (US Patent 4,150,097), but the raw material borane-ammonia complex required by this method is extremely expensive, which leads to the limitation of borazine extremely expensive
[0005] At present, borazine and its polymers have not been widely promoted or applied. The main reason is that there is no efficient and low-cost synthetic method

Method used

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  • Method and device for preparing borazine
  • Method and device for preparing borazine
  • Method and device for preparing borazine

Examples

Experimental program
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Effect test

Embodiment 1

[0020] The preparation method of the borazine of the present embodiment: first weigh 500g of ammonium chloride, place in the vibrating ball milling reactor, then add 250g of sodium borohydride, then vacuumize the vibrating ball milling reactor (vacuum degree is 100Pa), then Start the vibrating motor, and raise the reaction temperature to 280°C at the same time, and the borazine produced by the reaction is continuously collected in a collection bottle in cold hydrazine (the temperature of cold hydrazine is -70°C), the reaction time is 10 hours, and finally Distilled under reduced pressure at low temperature (-5°C, 300Pa) to obtain 60g of borazine with a purity of 95%.

[0021] refer to image 3 , implement the device of above-mentioned method, comprise vibrating ball milling reactor 1, collecting bottle 2, cold hydrazine 3, vacuum pump 4, described vibrating ball milling reactor 1 is positioned on the supporting frame, and the bottom plate of described supporting frame is provi...

Embodiment 2

[0024] The preparation method of the borazine of the present embodiment: take by weighing 1000g ammonium chloride earlier, place in the vibrating ball milling reactor, then add 560g sodium borohydride and catalyst copper powder 20g, then vacuumize the vibrating ball milling reactor (vacuum degree 100Pa), then start the vibrating motor, and raise the reaction temperature to 300°C at the same time, the borazine generated by the reaction is continuously collected in the collection bottle in cold hydrazine (the temperature of cold hydrazine is -68°C), and the reaction time is After 8 hours, finally low-temperature and vacuum distillation (-5°C, 300Pa), 65 g of borazine with a purity of 93% was obtained.

[0025] The device for implementing the method is the same as in Example 1.

Embodiment 3

[0027] The preparation method of the borazine of the present embodiment: take by weighing 500g ammonium chloride earlier, place in the vibrating ball milling reactor, then add 200g sodium borohydride and catalyst nickel powder 50g, then vacuumize the vibrating ball milling reactor (vacuum degree 100Pa), then start the vibrating motor, and raise the reaction temperature to 320°C at the same time, the borazine generated by the reaction is continuously collected in the collection bottle in cold hydrazine (the temperature of cold hydrazine is -72°C), and the reaction time is After 5 hours, 50 g of borazine with a purity of 94% was obtained by low-temperature and reduced-pressure distillation (-5°C, 300 Pa).

[0028] The device for implementing the method is the same as in Example 1.

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Abstract

The invention relates to a method and a device for preparing borazine. The method preparing borazin comprises the following steps of: adding sodium borohydride and ammonium chloride in a mass ratio of 37 / 60-37 / 80 into a vibratory milling reactor; vacuumizing the vibratory milling reactor; mechanically performing vibratory milling; rising the reaction temperature to 180 and 350 DEG C; continuouslycollecting coarse borazine generated by reaction in a collection bottle arranged in cold hydrazine; and finally performing reduced pressure distillation at low temperature to obtain borazine. The invention also comprises the device for executing the method preparing borazin borazine. By using the method and device, the preparation cost is lower, and the pollution to environment is small.

Description

technical field [0001] The invention relates to a method for preparing borazine and a device thereof, in particular to a mechanochemical method for synthesizing borazine and a device thereof. Background technique [0002] The structure of borazine is very similar to that of benzene, so it is also called inorganic benzene. [0003] Since borazine does not contain impurity elements such as carbon, it can be converted into high-purity BN by dehydrogenation at high temperature; boronazine can be polymerized at about 70°C to obtain polymerized borazine with different viscosities, which has easy-to-adjust process performance. Because BN is not easy to sinter, nor can it be dissolved or melted, borazine has almost become a necessary raw material for the preparation of high-purity BN fibers, coatings and composite materials. It is used in the manufacture of high-temperature oxidation-resistant aircraft brake discs (C f / BN composite material), high-purity BN fiber, high-purity BN c...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B35/14
Inventor 曹峰张长瑞王思青李斌
Owner NAT UNIV OF DEFENSE TECH