CN101642710A - Cu2O-Bi2O3/carbon nano-tube composite powder and preparation method thereof - Google Patents
Cu2O-Bi2O3/carbon nano-tube composite powder and preparation method thereof Download PDFInfo
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- CN101642710A CN101642710A CN200810142777A CN200810142777A CN101642710A CN 101642710 A CN101642710 A CN 101642710A CN 200810142777 A CN200810142777 A CN 200810142777A CN 200810142777 A CN200810142777 A CN 200810142777A CN 101642710 A CN101642710 A CN 101642710A
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- tube composite
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- bi2o3
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Abstract
The invention provides Cu2O-Bi2O3/carbon nano-tube composite powder and a preparation method thereof. The components of the Cu2O-Bi2O3/carbon nano-tube composite powder are Cu2O, Bi2O3 and multi-walled carbon nano-tubes (MWCNT), wherein the mixture ratio by weight of the components is: 40 to 60 percent of Cu2O-Bi2O3 (wherein Cu2O accounts for 20 to 40 percent, and Bi2O3 accounts for 20 to 40 percent), the particle size of the Cu2O-Bi2O3 is 10 to 20 nm, and 40 to 60 percent of MWCNT. The preparation method comprises the steps of purifying the multi-walled carbon nano-tubes, performing oxidationmodification on the surfaces of the multi-walled carbon nano-tubes, adding the multi-walled carbon nano-tubes to stoichiometric bismuth salt and copper salt solutions, ultrasonically dispersing, stirring, standing, performing alkalization deposition, washing, filtering, burning, performing other processes and obtaining the composite powder. The Cu2O-Bi2O3/carbon nano-tube composite powder as a combustion catalyst has excellent catalytic effect on the combustion of double-base or modified double-base propellants, is free from toxicity and pollution, and is an environment-friendly combustion catalyst.
Description
Technical field
That the present invention relates to is a kind of Cu
2O-Bi
2O
3/ carbon nano-tube composite powder and preparation method thereof.Cu
2O-Bi
2O
3/ carbon nano-tube composite powder can be used as the environmentally friendly combustion catalyst of solid propellant.
Technical background
Double base propellant and modified double base propellant are the used class high-energy fuel of rocket and guided missile, actual with the time need to add combustion catalyst and improve its combustibility.Development along with missilery, development low signature, environmentally friendly high-performance propellant 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 propellant.
CNT is owing to have huge specific area and cavity structure, and there is fault of construction again in its surface and edge, makes it have unique catalytic performance and adsorption property, is a kind of special catalyst, is again a kind of good catalyst carrier.As catalyst carrier, can be prepared into environmentally friendly composite catalyst with avirulence or hypotoxicity metallic compound and CNT are compound.CNT plays dual parts catalyst and carrier, catalyst with the nanoparticle form high degree of dispersion on the tube wall of CNT, CNT can stop the mutual reunion between metal oxide nanoparticles as " carbon skeleton ", can give full play to the efficient catalytic effect of nano particle.Because CNT is made up of carbon, can not produce toxic and harmful after the burning, therefore can not pollute environment, the metal oxide of simultaneously load again can with the catalytic performance " complementation " of CNT, promote the catalytic action of metal oxide.
Bismuth is a kind of nontoxic element, and copper is a kind of low toxicity element, and they are that the burning of propellant all has catalytic action preferably to double-basis.With Bi
2O
3And Cu
2O is compound on nanoscale, and their catalytic performance can " complementation ", produces strong " cooperative effect ", can significantly improve its catalytic effect, and can be by changing Bi
2O
3And Cu
2The ratio of O is optimized catalytic performance.Therefore, exploitation Cu
2O-Bi
2O
3The compound burningrate catalyst of/carbon nanometer tube loaded type can be solid propellant environmentally friendly efficient burning catalyst is provided.
Summary of the invention
The objective of the invention is for the problems referred to above, a kind of Cu that is used as the combustion catalyst of double-basis or modified double base propellant is provided
2O-Bi
2O
3/ carbon nano-tube composite powder.
Another object of the present invention provides Cu
2O-Bi
2O
3The preparation method of/carbon nano-tube composite powder.
The invention provides a kind of Cu
2O-Bi
2O
3/ carbon nano-tube composite powder, its key component is: Cu
2O, Bi
2O
3And multi-walled carbon nano-tubes (MWCNT), the content of various components is counted by weight percentage and is Cu
2O-Bi
2O
3: 40~60% (Cu wherein
2O:20~40%; Bi
2O
3: 20~40%), MWCNT:40~60%.
Described Cu
2O-Bi
2O
3In/the carbon nano-tube composite powder: the diameter of used multi-walled carbon nano-tubes is 60~90nm, and length is 500~3000nm, loads on the Cu of carbon nano tube surface
2O-Bi
2O
3The particle diameter of compound particle is 10~20nm.
Cu of the present invention
2O-Bi
2O
3The preparation method of/carbon nano-tube composite powder, 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 12~20 hours; (2) the purified effective nitration mixture of multi-wall carbon nano-tube (ratio of the red fuming nitric acid (RFNA) and the concentrated sulfuric acid is: 1: 3) was 60~90 ℃ of following oxidations 1~2 hour; (3) a certain proportion of soluble bismuth salt and soluble copper salt are dissolved in the distilled water and add an amount of rare nitric acid be mixed with transparent mixed solution; (4) in the mixed solution of bismuth salt and mantoquita, add the multi-walled carbon nano-tubes of stoichiometric purified and oxidation, stir and add ultrasonic dispersion 30 minutes; (5) at room temperature stir 4~6 hours, left standstill then 4~5 hours; (6) under agitation splash into 2.5wt% ammoniacal liquor, left standstill 4~6 hours then pH value to 7.5~8.5 of regulator solution; (7) suction filtration, washing, drying; (8) under nitrogen protection, calcined 2 hours, and can make Cu for 300~450 ℃
2O-Bi
2O
3/ carbon nano-tube composite powder.Described used soluble bismuth salt is: bismuth nitrate; Soluble copper salt is: copper nitrate, Schweinfurt green.
Cu of the present invention
2O-Bi
2O
3/ carbon nano-tube composite powder has good catalytic effect as combustion catalyst to the burning of double-basis or modified double base propellant, and is nontoxic, pollution-free.
Description of drawings
The Cu of Fig. 1 for obtaining behind the case study on implementation 1
2O-Bi
2O
3The X-ray diffractogram of/CNT, a is the X-ray diffraction result of CNT after the preliminary treatment among the figure; B is Cu among the figure
2O-Bi
2O
3The X-ray diffraction result of/carbon nano-tube composite powder contrasts with the PDF card: loaded article is mainly bismuth oxide (PDF card 65-1209) and cuprous oxide (PDF card 65-3288).
The Cu of Fig. 2 for obtaining behind the case study on implementation 1
2O-Bi
2O
3The transmission electron microscope photo of/CNT can be found out from transmission electron microscope photo, loads on the nanometer Cu of carbon nano tube surface
2O-Bi
2O
3Be spheroidal particle, the about 16nm of average grain diameter.
The Cu of Fig. 3 for obtaining behind the case study on implementation 1
2O-Bi
2O
3The EDS energy spectrogram of/carbon nano-tube composite powder, EDS composes four kinds of elements such as existing C, O, Bi, Cu, illustrates that product only contains C, O, four kinds of elements of Bi, Cu.
The specific embodiment
Cu of the present invention
2O-Bi
2O
3The concrete preparation method of/carbon nano-tube composite powder combustion catalyst is provided in detail by following examples.
(1) multi-walled carbon nano-tubes that takes by weighing 0.400g places round-bottomed flask, add nitration mixture (red fuming nitric acid (RFNA): the concentrated sulfuric acid=1: 3), constant temperature refluxed 1 hour under 70 ℃ of temperature, cooling, washing is filtered, and is dry, grind.
(2) the five water bismuth nitrates that take by weighing 0.370g add 30ml 1.0mol/L nitric acid, ultrasonic dissolution in round-bottomed flask.The nitrate trihydrate copper that takes by weighing 0.600g in round-bottomed flask, ultrasonic dissolution.Bismuth salting liquid and copper salt solution are mixed, add the multi-walled carbon nano-tubes of 0.300g through step (1) oxidation processes, ultrasonic being uniformly dispersed, at room temperature constant temperature stirred 5 hours, left standstill then 5 hours.Under agitation splashing into 1mol/L NaOH to pH value is 7.8, leaves standstill then 5 hours.Suction filtration adds ultrasonic wave to product washing 2 times and 1 time with distilled water, ethanol respectively, and 60 ℃ lower dry, and 350 ℃ of calcinations are 2 hours under nitrogen protection, can make CuO-Bi
2O
3/ carbon nano-tube composite powder.The content that gets Bi element in the product with atomic spectroscopic analysis count by weight percentage into: the content of 22.0%, Cu element is: 22.5%; Conversion obtains containing Bi
2O
3For: 24.5%, contain Cu
2O is: 25.3%.
(1) multi-walled carbon nano-tubes that takes by weighing 0.400g places round-bottomed flask, add nitration mixture (red fuming nitric acid (RFNA): the concentrated sulfuric acid=1: 3), constant temperature refluxed 1 hour under 70 ℃ of temperature, cooling, washing is filtered, and is dry, grind.
(2) the five water bismuth nitrates that take by weighing 0.550g add 40ml 1mol/L nitric acid in round-bottomed flask, and ultrasonic dissolution becomes transparent clear solutions.The copper nitrate that takes by weighing 0.900g in round-bottomed flask, ultrasonic dissolution.Bismuth salting liquid and copper salt solution are mixed, add the multi-walled carbon nano-tubes of 0.300g through step (1) oxidation processes, ultrasonic being uniformly dispersed at room temperature stirred 5 hours, left standstill then 6 hours.Under agitation splashing into 1mol/L NaOH to pH value is 8.0, leaves standstill then 5 hours.Suction filtration adds ultrasonic wave to product washing 2 times and 1 time with distilled water, ethanol respectively, and 60 ℃ lower dry, and 350 ℃ of calcinations are 2 hours under nitrogen protection, can make Cu
2O-Bi
2O
3/ carbon nano-tube composite powder.The content that gets Bi element in the product with atomic spectroscopic analysis count by weight percentage into: the content of 25.7%, Cu element is: 26.3%; Conversion obtains containing Bi
2O
3For: 28.7%, contain Cu
2O is: 29.6%.
Claims (4)
1, a kind of Cu
2O-Bi
2O
3/ carbon nano-tube composite powder is characterized by: Cu
2O-Bi
2O
3The key component of/carbon nano-tube composite powder is: Cu
2O, Bi
2O
3And multi-walled carbon nano-tubes (MWCNT), the content of various components is counted by weight percentage and is Cu
2O-Bi
2O
3: 40~60% (Cu wherein
2O:20~40%; Bi
2O
3: 20~40%), MWCNT:40~60%.
2, Cu according to claim 1
2O-Bi
2O
3/ carbon nano-tube composite powder is characterized in that: the diameter of used multi-walled carbon nano-tubes is 60~90nm, and length is 500~3000nm, loads on the Cu of carbon nano tube surface
2O-Bi
2O
3The particle diameter of compound particle is 10~20nm.
3, claim 1 or 2 described Cu
2O-Bi
2O
3The preparation method of/carbon nano-tube composite powder, carry out according to the following steps: the effective hydrochloric acid of (1) multi-wall carbon nano-tube soaks and carried out purifying in 12~20 hours; (2) the purified effective nitration mixture of multi-wall carbon nano-tube (ratio of the red fuming nitric acid (RFNA) and the concentrated sulfuric acid is: 1: 3) was 60~90 ℃ of following oxidations 1~2 hour; (3) a certain proportion of soluble bismuth salt and soluble copper salt are dissolved in the distilled water and add an amount of rare nitric acid be mixed with transparent mixed solution; (4) in the mixed solution of bismuth salt and mantoquita, add the multi-walled carbon nano-tubes of stoichiometric purified and oxidation, stir and add ultrasonic dispersion 30 minutes; (5) at room temperature stir 4~6 hours, left standstill then 4~5 hours; (6) under agitation splash into 2.5wt% ammoniacal liquor, left standstill 4~6 hours then pH value to 7.5~8.5 of regulator solution; (7) suction filtration, washing, drying; (8) under nitrogen protection, calcined 2 hours, and can make Cu for 300~450 ℃
2O-Bi
2O
3/ carbon nano-tube composite powder.
4, according to the described Cu of claim 3
2O-Bi
2O
3The preparation method of/carbon nano-tube composite powder is characterized in that: used soluble bismuth salt is: bismuth nitrate; Soluble copper salt is: copper nitrate, Schweinfurt green.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102698766A (en) * | 2012-05-15 | 2012-10-03 | 中国科学院力学研究所 | Combustion catalyst and preparation method thereof |
CN102895979A (en) * | 2012-10-15 | 2013-01-30 | 深圳大学 | Cu2O-Bi2O3/graphene oxide composite powder and preparation method thereof |
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CN1513596A (en) * | 2003-07-07 | 2004-07-21 | 深圳大学 | Nano-copper-lead composite oxide powder and its preparation method |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102698766A (en) * | 2012-05-15 | 2012-10-03 | 中国科学院力学研究所 | Combustion catalyst and preparation method thereof |
CN102698766B (en) * | 2012-05-15 | 2014-12-31 | 中国科学院力学研究所 | Combustion catalyst and preparation method thereof |
CN102895979A (en) * | 2012-10-15 | 2013-01-30 | 深圳大学 | Cu2O-Bi2O3/graphene oxide composite powder and preparation method thereof |
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