CN101440009A - Bismuthous oxide / carbon nano-tube composite powder and preparation thereof - Google Patents
Bismuthous oxide / carbon nano-tube composite powder and preparation thereof Download PDFInfo
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- CN101440009A CN101440009A CNA2007101245985A CN200710124598A CN101440009A CN 101440009 A CN101440009 A CN 101440009A CN A2007101245985 A CNA2007101245985 A CN A2007101245985A CN 200710124598 A CN200710124598 A CN 200710124598A CN 101440009 A CN101440009 A CN 101440009A
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Abstract
The invention relates to dibismuth trioxide/carbon nano tube compound powder and a preparation method thereof. The dibismuth trioxide/carbon nano tube compound powder comprises Bi2O3 and multi-wall carbon nano tube (MWCNT), wherein the weight percentage of the Bi2O3 is 30 to 60 percent, and the grain size of the Bi2O3 is 10 to 30 nanometers. The preparation method comprises the following steps: purifying the multi-wall carbon nano tube and oxidizing and modifying the surface of the multi-wall carbon nano tube, then adding the multi-wall carbon nano tube into stoichiometric bismuth salt solution, and ultrasonic dispersing, stirring, keeping standing, alkalifying, washing, filtering and scorching the mixture to obtain the compound powder. The prepared dibismuth trioxide/carbon nano tube compound powder has excellent catalytic effect for combustion of biradical or modified biradical propelling agent, has no toxin and pollution, and is an environment-friendly combustion catalyst when used as a combustion catalyst.
Description
Technical field
What the present invention relates to is a kind of Bismuthous oxide/carbon nano-tube composite powder and preparation method thereof.Bismuthous oxide/carbon nano-tube composite powder can be used as the environmentally friendly combustioncatalysts of solid propellant.
Technical background
Double-base propellent and composite modified double base propellant are the used class high energy fuels of rocket and guided missile, need add combustioncatalysts during actual the use and improve its combustionproperty.Development along with missilery, development low signature, environmentally friendly high-performance propelling agent are the important development directions, correspondingly need to develop nontoxic or hypotoxicity, pollution-free, novel burningrate catalyst efficiently, satisfy the needs of development novel solid propelling agent.
Carbon nanotube is owing to have huge specific surface area and cavity structure, and there is textural defect again in its surface and edge, makes it have unique catalytic performance and adsorption property, is a kind of special catalyzer, is again a kind of good support of the catalyst.As support of the catalyst, can be prepared into environmentally friendly composite catalyst with nontoxicity or hypotoxicity metallic compound and carbon nanotube are compound.Carbon nanotube plays dual parts catalyzer and carrier, catalyzer with the nanoparticle form high dispersing on the tube wall of carbon nanotube, carbon nanotube is as " carbon skeleton ", the mutual reunion between metal or metal oxide nanoparticles can be stoped, the efficient catalytic effect of nanoparticle can be given full play to.Because carbon nanotube is made up of carbon, can not produce toxic and harmful after the burning, therefore can not pollute environment, the metal oxide of load simultaneously again can with the catalytic performance " complementation " of carbon nanotube, thereby produce strong " synergistic effect ", its catalytic effect will be better than pure nano-metal-oxide catalyzer.
Bismuth is a kind of nontoxic element, is that the burning of propelling agent has catalytic effect preferably to double-basis.Therefore, the compound burningrate catalyst of exploitation Bismuthous oxide/carbon nano-tube loading type can be solid propellant provides environmentally friendly efficient burning catalyzer.
Summary of the invention
The objective of the invention is at the problems referred to above, a kind of Bismuthous oxide/carbon nano-tube composite powder that is used as the combustioncatalysts of double-basis or composite modified double base propellant is provided.
Another object of the present invention provides the preparation method of Bismuthous oxide/carbon nano-tube composite powder.
The invention provides a kind of Bismuthous oxide/carbon nano-tube composite powder, its main ingredient is: Bi
2O
3And multi-walled carbon nano-tubes (MWCNT), various components contents are counted by weight percentage and are Bi
2O
3: 30～60%, MWCNT:40～70%.。
In the described Bismuthous oxide/carbon nano-tube composite powder: the diameter of used multi-walled carbon nano-tubes is 60～90nm, and length is 500～3000nm; Load on the Bi of carbon nano tube surface
2O
3Particle diameter be 10～30nm.
The preparation method of Bismuthous oxide/carbon nano-tube composite powder of the present invention, several steps in the following order carries out: the effective hydrochloric acid of (1) multi-wall carbon nano-tube soaks and carried out purifying in 15～24 hours; (2) (ratio of the concentrated nitric acid and the vitriol oil is the purified effective nitration mixture of multi-wall carbon nano-tube: 1:3) 70～120 ℃ of following oxidations 1～3 hour; (3) soluble bismuth salt is dissolved in rare nitric acid is mixed with solution; (4) in the bismuth salts solution, add the multi-walled carbon nano-tubes (mass ratio of carbon nanotube and bismuth salt is 1: 1～2.5) of stoichiometric purified and oxidation, ultra-sonic dispersion; (5) under 60～80 ℃ of temperature, stirred 30 minutes, left standstill then 3～5 hours; (6) under agitation splash into 2.5wt% ammoniacal liquor, left standstill 2～5 hours then pH value to 9～10 of regulator solution; (7) suction filtration, washing, drying; (8) under nitrogen protection, 300～400 ℃ of calcinations 2 hours can make Bismuthous oxide/carbon nano-tube composite powder.
Described soluble bismuth salt is: Bismuth trinitrate.
Bismuthous oxide/carbon nano-tube composite powder of the present invention has good catalytic effect as combustioncatalysts to the burning of double-basis or composite modified double base propellant, and is nontoxic, pollution-free.
Description of drawings
Fig. 1 is the X-ray diffractogram of the Bismuthous oxide/carbon nano-tube that obtains behind the case study on implementation 1, and a is the X-ray diffraction result of carbon nanotube after the pre-treatment among the figure; B is the X-ray diffraction result of Bismuthous oxide/carbon nano-tube composite powder among the figure, contrasts with the JCPDS card: loaded article is mainly bismuthous oxide bismuth trioxide (JCPDS card 65-1209), also has little metal bismuth (JCPDS card 44-1246) simultaneously.
Fig. 2 as can be seen, loads on the nanometer Bi of carbon nano tube surface for the transmission electron microscope photo of the Bismuthous oxide/carbon nano-tube that obtains behind the case study on implementation 1 from transmission electron microscope photo
2O
3Be spheroidal particle, the about 20nm of median size.
Fig. 3 can spectrogram for the EDS of the Bismuthous oxide/carbon nano-tube composite powder that obtains behind the case study on implementation 1, occurs four kinds of elements such as C, O, Bi, Cu among the figure, and wherein the Cu element comes the copper mesh that self-test is used, and illustrates that product only contains C, O, three kinds of elements of Bi.
Embodiment
The concrete preparation method of Bismuthous oxide/carbon nano-tube composite powder combustioncatalysts of the present invention is provided in detail by following examples.
Embodiment 1
(1) multi-walled carbon nano-tubes that takes by weighing 0.3g places round-bottomed flask, and (concentrated nitric acid: the vitriol oil=1: 3), constant temperature refluxed 2 hours under 80 ℃ of temperature, and cooling is filtered, and is dry, grind to add nitration mixture.
(2) the five water Bismuth trinitrates that take by weighing 0.55g add 10ml1.0mol/L nitric acid, ultrasonic dissolution in round-bottomed flask.Add the multi-walled carbon nano-tubes of 0.2g through step (1) oxide treatment, ultra-sonic dispersion is even, stirs 30 minutes at 80 ℃ of following constant temperature, leaves standstill then 4 hours.Under agitation splashing into 2.5wt% ammoniacal liquor to pH value is 9.0, leaves standstill then 3 hours.Suction filtration adds ultrasonic wave to product washing 2 times and 1 time with distilled water, ethanol respectively, and 60 ℃ dry down, and under nitrogen protection, 400 ℃ of calcinations 2 hours can make Bismuthous oxide/carbon nano-tube composite powder.
The content that gets Bi element in the product with atomic spectroscopic analysis count by weight percentage into: 42.3%, conversion obtains containing Bi
2O
3For: 47.4%.
(1) multi-walled carbon nano-tubes that takes by weighing 0.30g places round-bottomed flask, and (concentrated nitric acid: the vitriol oil=1: 3), constant temperature refluxed 2 hours under 80 ℃ of temperature, and cooling is filtered, and is dry, grind to add nitration mixture.
(2) the five water Bismuth trinitrates that take by weighing 0.43g add 8ml1.12mol/L nitric acid in round-bottomed flask, and ultrasonic dissolution becomes transparent clear soln.Add the multi-walled carbon nano-tubes of 0.2g, ultrasonic it is uniformly dispersed, stirred 30 minutes down, left standstill then 4 hours at 80 ℃ through step (1) oxide treatment.Under agitation slowly splashing into 2.5wt% ammoniacal liquor to pH value is 9.0, leaves standstill then 3 hours.Suction filtration adds ultrasonic wave with distilled water, ethanol product is washed respectively 2 times and 1 time, and 60 ℃ down dry, and under nitrogen protection, 400 ℃ of calcinations 2 hours can make Bismuthous oxide/carbon nano-tube composite powder.Load Bi
2O
3Amount be 36.7%.
Claims (4)
1, a kind of Bismuthous oxide/carbon nano-tube composite powder is characterized by: the main ingredient of Bismuthous oxide/carbon nano-tube composite powder is: Bi
2O
3And multi-walled carbon nano-tubes (MWCNT), various components contents are counted by weight percentage and are Bi
2O
3: 30～60%, MWCNT:40～70%.
2, Bismuthous oxide/carbon nano-tube composite powder according to claim 1 is characterized in that: the diameter of used multi-walled carbon nano-tubes is 60～90nm, and length is 500～3000nm, loads on the Bi of carbon nano tube surface
2O
3Particle diameter be 10～30nm.
3, the preparation method of claim 1 or 2 described Bismuthous oxide/carbon nano-tube composite powders, carry out according to the following steps: the effective hydrochloric acid of (1) multi-wall carbon nano-tube soaks and carried out purifying in 15～24 hours; (2) the purified effective nitration mixture of multi-wall carbon nano-tube (ratio of the concentrated nitric acid and the vitriol oil is: 1: 3) was 70～120 ℃ of following oxidations 1～3 hour; (3) soluble bismuth salt is dissolved in rare nitric acid is mixed with solution; (4) in the bismuth salts solution, add the multi-walled carbon nano-tubes (mass ratio of carbon nanotube and bismuth salt is 1: 1～2.5) of stoichiometric purified and oxidation, ultra-sonic dispersion; (5) under 60～80 ℃ of temperature, stirred 30 minutes, left standstill then 3～5 hours; (6) under agitation splash into 2.5wt% ammoniacal liquor, left standstill 3～5 hours then pH value to 9～10 of regulator solution; (7) suction filtration, washing, drying; (8) under nitrogen protection, 300～400 ℃ of calcinations 2 hours can make Bismuthous oxide/carbon nano-tube composite powder.
4, according to the preparation method of the described Bismuthous oxide/carbon nano-tube composite powder of claim 3, it is characterized in that: used soluble bismuth salt is: Bismuth trinitrate.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007101245985A CN101440009A (en) | 2007-11-23 | 2007-11-23 | Bismuthous oxide / carbon nano-tube composite powder and preparation thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102899122A (en) * | 2012-10-19 | 2013-01-30 | 深圳大学 | Bi2O3/oxidized graphene composite powder and preparation method thereof |
| CN115925496A (en) * | 2022-12-23 | 2023-04-07 | 陕西师范大学 | Carbon nano tube filled green compound nano composite burning rate catalyst |
-
2007
- 2007-11-23 CN CNA2007101245985A patent/CN101440009A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102899122A (en) * | 2012-10-19 | 2013-01-30 | 深圳大学 | Bi2O3/oxidized graphene composite powder and preparation method thereof |
| CN115925496A (en) * | 2022-12-23 | 2023-04-07 | 陕西师范大学 | Carbon nano tube filled green compound nano composite burning rate catalyst |
| CN115925496B (en) * | 2022-12-23 | 2024-02-13 | 陕西师范大学 | Carbon nano tube filled green compound nano composite burning rate catalyst |
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Open date: 20090527 |