Process for purifying and recovering boron nitride nanotube crude product

A technology of boron nitride nanotubes and crude products, which can be used in chemical recovery, nitrogen compounds, nanotechnology, etc., and can solve problems such as inappropriate direct application

Inactive Publication Date: 2009-11-18
WUHAN INSTITUTE OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because the crude product of boron nitride nanotubes contains the above-

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Embodiment 1: Preparation of boron nitride nanotube crude product

[0023] Step 1: Ingredients. Weigh 50.03g CaB 6 , 50.25g Co 2 o 3 , CaB 6 、Co 2 o 3 All are analytical reagents, and the molar ratio B:Co is 1:0.21. The second step: mixing. The weighed CaB 6 and Co 2 o 3 Add a high-speed mixer (18000 rpm) and mix for 5 minutes to make it fully uniform. Step Three: Shaping. Pour the mixture into a steel mold, use a 500-ton press, hold the pressure for 15 minutes, shape it, and take it out. Step 4: React. Put the formed material into the reaction tank without sealing. Put the reaction tank into an argon-protected heating furnace, keep it warm at 750°C for 12 minutes, cool it naturally, open the tank and take out the product, which has a black honeycomb shape in appearance. Step Five: Crush. The reacted material was put into a high-speed mixer (18000 rpm) and fully pulverized for 5 minutes, weighed, the mass was 97.65g, and the mass loss rate was 2.6%, seal...

Embodiment 2

[0025] According to the operation steps of Example 1, with 50.03g calcium hexaboride (CaB 6 ) and 50.25g cobalt oxide (Co 2 o 3 ) as raw material to prepare boron nitride nanotube crude product. Continue the purification process: the first step: the crude product of boron nitride nanotubes is pulverized. The crude product of boron nitride nanotubes was added to a high-speed mixer (18000 rpm) for crushing for 5 minutes. The second step: pickling. Pour the pulverized product into a beaker, add 200ml of distilled water to dissolve, then add 250ml of 36wt.% hydrochloric acid, and heat and stir at 40°C for 12 hours. The third step: filtering, washing and drying. The mixed solution was suction-filtered with a circulating water-type vacuum pump to recover the supernatant, and the filter cake was dried at 80° C. for 8 hours. Step Four: Crush. Put the filter cake into a high-speed mixer (18,000 rpm) and crush it for 5 minutes, weigh the boron nitride nanotubes as 69.87 grams, an...

Embodiment 3

[0027] According to the operation steps of Example 1, with 32.13g barium hexaboride (BaB 6 ) and 25.80g iron oxide (Fe 2 o 3 ) is the crude product of boron nitride nanotubes prepared from raw materials. The first step: crushing the crude product of boron nitride nanotubes. The annealed product was added to a high-speed mixer (18000 rpm) and crushed for 6 minutes. The second step: pickling. Pour the pulverized product into a beaker, add 150ml of distilled water to dissolve, then add 200ml of 18wt.% hydrochloric acid, and heat and stir at 70°C for 8 hours. The third step: filtering, washing and drying. The mixed solution was filtered to recover the supernatant, and the filter cake was dried at 80° C. for 8 hours. Step Four: Crush. The filter cake was put into a high-speed mixer (18000 rpm) and crushed for 5 minutes, and the weight of the boron nitride nanotube was 23.35 grams, and the purity was 89.32%. The fifth step: complexation reaction. 164ml of 14wt% concentrated...

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Abstract

The invention relates to a process for purifying and recovering a boron nitride nanotube crude product, comprising the following steps: crashing the boron nitride nanotube crude product, soaking with acid which is hydrochloric acid or hydrogen nitrate, filtrating to obtain filter cake and filtrate, water washing and drying the filter cake to obtain purified boron nitride nanotube powder; adding ammonia in filtrate and precipitating to obtain byproducts, filtrating to obtain filter cake and filtrate, water washing and drying the obtained filter cake to obtain a recycle byproduct-alkaline-earth metal compound, filtering and water washing the obtained filtrate, evaporating the filtrate and waste washing liquid to remove moisture and volatiles, and performing oxidation reaction to obtain recycle transition metal oxide and rare-earth oxide. The beneficial effects of the invention are that: boron nitride nanotube purity can reach above 90wt.% by purifying, the recovery rate of catalyst and byproducts can reach above 95% and the recovered metal catalyst and byproducts can be recycled for preparing boron nitride nanotube.

Description

technical field [0001] The invention relates to the field of preparation of ceramic materials, in particular to a process for purifying and recovering boron nitride nanotubes. Background technique [0002] Boron nitride nanotubes are composed of B-N atoms with sp 2 Hybridization into bonded tubular structures. Theoretical and experimental research results show that boron nitride nanotubes have comparable mechanical properties to carbon nanotubes, and their theoretical elastic modulus is about 1TPa [1-3] ; But the physical and chemical properties are very different from carbon nanotubes. The band gap width of boron nitride nanotubes is about 5.15eV, which is close to the bulk material of hexagonal boron nitride, and has nothing to do with the chirality, diameter and wall thickness of boron nitride nanotubes [4] ;Anti-oxidation temperature up to 900°C [5] , is a new type of structural material and functional material with broad application prospects. [0003] Although som...

Claims

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Application Information

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IPC IPC(8): C01B21/064B82B3/00
CPCY02P20/584
Inventor 谷云乐王吉林
Owner WUHAN INSTITUTE OF TECHNOLOGY
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