CN101440008A - Lead oxide / carbon nano-tube composite powder and preparation thereof - Google Patents
Lead oxide / carbon nano-tube composite powder and preparation thereof Download PDFInfo
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- CN101440008A CN101440008A CNA2007101245970A CN200710124597A CN101440008A CN 101440008 A CN101440008 A CN 101440008A CN A2007101245970 A CNA2007101245970 A CN A2007101245970A CN 200710124597 A CN200710124597 A CN 200710124597A CN 101440008 A CN101440008 A CN 101440008A
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Abstract
The invention relates to lead oxide/carbon nano tube compound powder and a preparation method thereof. The lead oxide/carbon nano tube compound powder comprises PbO and multi-wall carbon nano tube (MWCNT), wherein the weight percentage of the PbO is 30 to 60 percent, and the grain size of the PbO is 15 to 35 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 lead salt solution, and ultrasonic dispersing, stirring, keeping standing, alkalifying, washing, filtering and scorching the mixture to obtain the compound powder. The prepared lead oxide/carbon nano tube compound powder has higher catalytic effect for combustion of biradical or modified biradical propelling agent when used as a combustion catalyst.
Description
Technical field
What the present invention relates to is a kind of lead oxide/carbon nano-tube composite powder and preparation method thereof.Lead oxide/carbon nano-tube composite powder can be used as the 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.Because its combustion speed is on the low side, the pressure index is higher, need add combustioncatalysts during actual the use and improve its combustionproperty.Along with the development of missilery, need the development of new burningrate catalyst, 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 with metal or metal oxide and the compound composite catalyst that is prepared into of carbon nanotube.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.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.
Plumbous oxide be a kind of be the combustioncatalysts that the burning of propelling agent has good catalytic effect to double-basis.Therefore, the compound burningrate catalyst of exploitation lead oxide/carbon nano-tube loading type can be solid propellant provides high efficiency combustion catalyst.
Summary of the invention
The objective of the invention is at the problems referred to above, a kind of lead oxide/carbon nano-tube composite powder as double-basis or composite modified double base propellant combustioncatalysts is provided.
Another object of the present invention provides the preparation method of lead oxide/carbon nano-tube composite powder.
The invention provides a kind of lead oxide/carbon nano-tube composite powder, its main ingredient is: PbO and multi-walled carbon nano-tubes (MWCNT), various components contents are counted by weight percentage and are PbO:30～60%, MWCNT:40～70%.。
In the described lead oxide/carbon nano-tube composite powder: the diameter of used multi-walled carbon nano-tubes is 60～90nm, and length is 500～3000nm; The particle diameter that loads on the PbO of carbon nano tube surface is 10～35nm.
The preparation method of lead oxide/carbon nano-tube composite powder of the present invention, several steps of carrying out in the following order: the effective hydrochloric acid of (1) multi-wall carbon nano-tube soaks and carried out purifying in 15～24 hours; (2) the purified effective concentrated nitric acid of multi-wall carbon nano-tube was 100～140 ℃ of following oxidations 2～3 hours; (3) be dissolved in the solubility lead salt in the distilled water and add an amount of acetic acid or rare nitric acid is mixed with transparent solution; (4) purified and multi-walled carbon nano-tubes oxidation joins in the ethanol-water mixed solvent, adds sodium laurylsulfonate and makes dispersion agent, mixes (mass ratio of carbon nanotube and lead salt is 1: 1～2.5) then with lead salt solution, ultra-sonic dispersion; (5) under 50～60 ℃ of temperature, stirred 2～4 hours,, stirred 3～5 hours with pH value to 9.0～10.0 of ammoniacal liquor regulator solution; (6) suction filtration, washing, drying; (7) under nitrogen protection, 250～400 ℃ of calcinations 2 hours can make lead oxide/carbon nano-tube composite powder.
Described solubility lead salt is: lead nitrate, plumbic acetate.
Lead oxide/carbon nano-tube composite powder of the present invention has very high catalytic effect as combustioncatalysts to the burning of double-basis or composite modified double base propellant.For example, can make that combustion speed significantly improves the pressure index decreased under the low pressure of certain double-base propellent.
Description of drawings
Fig. 1 is the transmission electron microscope photo of the lead oxide/carbon nano-tube that obtains behind the case study on implementation 1, we are as can be seen from figure, load on carbon nano tube surface PbO some be coated on carbon nano tube surface with unformed state, some loads on carbon nano tube surface with rod-shaped particle, and median size is about 25nm.
Fig. 2 can spectrogram for the EDS of the lead oxide/carbon nano-tube composite powder that obtains behind the case study on implementation 1, and EDS composes four kinds of elements such as existing C, O, Pb, Cu, 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 Pb.
Embodiment
The concrete preparation method of lead 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 the concentrated hydrochloric acid that adds 20ml soaked 22 hours, and after filtration, after the washing, add concentrated nitric acid 40ml, constant temperature refluxed 2 hours under 100 ℃ of temperature, and cooling is filtered, and is dry, grind.
(2) the acetate trihydrate lead that takes by weighing 0.65g places round-bottomed flask, adds 40ml distilled water, adds the 5ml Glacial acetic acid, is dissolved into transparent clear soln.
(3) in ethanol-water mixed solvent, add sodium laurylsulfonate and make dispersion agent, add multi-walled carbon nano-tubes through step (1) oxide treatment, ultrasonic it is uniformly dispersed.Mixes with the plumbic acetate solution of step (2) configuration then, ultrasonic it is mixed, 50 ℃ of stirrings 3 hours down.With the pH value to 9.45 of ammoniacal liquor regulator solution, stirred 4 hours then.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, 250 ℃ of calcinations 2 hours can make lead oxide/carbon nano-tube composite powder.
Measure to such an extent that product only contains C, O, three kinds of elements of Pb (seeing accompanying drawing 2) with the EDS spectrum.Get the mixture that product is PbO and multi-walled carbon nano-tubes (MWCNT) with the XRD spectrum analysis, PbO is the rhombic system structure; Get Pb in the product with atomic spectroscopic analysis
2+Content count by weight percentage into: 48.2%, conversion obtains containing PbO and is: 51.8%.Tem observation shows that some is coated on carbon nano tube surface with unformed state the PbO in the product, and some loads on carbon nano tube surface with rod-shaped particle, and median size is about 25nm (seeing accompanying drawing 1).
(1) multi-walled carbon nano-tubes that takes by weighing 0.3g places round-bottomed flask, and the concentrated hydrochloric acid that adds 20ml soaked 24 hours, and after filtration, after the washing, add concentrated nitric acid 40ml, constant temperature refluxed 2 hours under 100 ℃ of temperature, and cooling is filtered, and is dry, grind.
(2) take by weighing the 0.55 acetate trihydrate lead that restrains and place round-bottomed flask, add 40ml distilled water, add the 5ml Glacial acetic acid, be dissolved into transparent clear soln.
(3) in ethanol-water mixed solvent, add sodium laurylsulfonate and make dispersion agent, add multi-walled carbon nano-tubes through step (1) oxide treatment, ultrasonic it is uniformly dispersed.Mixes with the plumbic acetate solution of step (2) configuration then, ultrasonic it is mixed, 50 ℃ of stirrings 3 hours down.With the pH value to 9.45 of ammoniacal liquor regulator solution, stirred 4 hours then.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, 250 ℃ of calcinations 2 hours can make lead oxide/carbon nano-tube composite powder.
The median size of PbO is 23nm in the products therefrom, contains the PbO amount to be: 40.6%.
Claims (4)
1, a kind of lead oxide/carbon nano-tube composite powder, it is characterized by: the main ingredient of lead oxide/carbon nano-tube composite powder is: PbO and multi-walled carbon nano-tubes (MWCNT), various components contents % by weight are calculated as: PbO:30～60%, MWCNT:40～70%.
2, lead 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; The particle diameter that loads on the PbO of carbon nano tube surface is 10～35nm.
3, the preparation method of claim 1 or 2 described lead oxide/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 15～24 hours; (2) the purified effective concentrated nitric acid of multi-wall carbon nano-tube was 100～140 ℃ of following oxidations 2～3 hours; (3) be dissolved in the solubility lead salt in the distilled water and add an amount of acetic acid or rare nitric acid is mixed with transparent solution; (4) purified and multi-walled carbon nano-tubes oxidation joins in the ethanol-water mixed solvent, adds sodium laurylsulfonate and makes dispersion agent, mixes (mass ratio of carbon nanotube and lead salt is 1: 1～2.5) then with lead salt solution, ultra-sonic dispersion; (5) under 50～60 ℃ of temperature, stirred 2～4 hours,, stirred 3～5 hours with pH value to 9.0～10.0 of ammoniacal liquor regulator solution; (6) suction filtration, washing, drying; (7) under nitrogen protection, 250～400 ℃ of calcinations 2 hours can make lead oxide/carbon nano-tube composite powder.
4, according to the preparation method of the described lead oxide/carbon nano-tube composite powder of claim 3, it is characterized in that: used solubility lead salt is: lead nitrate, plumbic acetate.
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| CNA2007101245970A CN101440008A (en) | 2007-11-23 | 2007-11-23 | Lead oxide / carbon nano-tube composite powder and preparation thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102335625A (en) * | 2011-07-15 | 2012-02-01 | 西安近代化学研究所 | Application of metal formates as combustion catalyst in solid propellant |
| CN102895966A (en) * | 2012-10-19 | 2013-01-30 | 深圳大学 | PbO/graphene oxide compound powder and preparation method thereof |
| CN104591936A (en) * | 2015-01-29 | 2015-05-06 | 中国工程物理研究院化工材料研究所 | Energetic composite material based on three-dimensional ordered macroporous carbon skeleton and preparation method of energetic composite material |
| US9413001B2 (en) | 2011-07-20 | 2016-08-09 | Bar Ilan University | Functionalized carbon nanotube composite |
| CN106187650A (en) * | 2016-07-25 | 2016-12-07 | 万载县建坤化工有限公司 | Fireworks and firecrackers opens quick-fried medicament composition |
| CN108393082A (en) * | 2018-03-06 | 2018-08-14 | 淮南市通霸蓄电池有限公司 | A kind of Nanometer sized lead oxide-carbon composite and preparation method thereof |
| CN110137452A (en) * | 2019-04-26 | 2019-08-16 | 浙江工业大学 | A kind of preparation method and application of Nanometer sized lead oxide/carbon composite |
| CN113548932A (en) * | 2021-07-27 | 2021-10-26 | 陕西师范大学 | Nano composite burning rate catalyst of copper metal complex filled with carbon nano tube |
| CN114031959A (en) * | 2021-11-29 | 2022-02-11 | 安徽工业大学 | Regulation and control method of carbon black structure, activated carbon black solid and application of activated carbon black solid to catalyst carrier |
-
2007
- 2007-11-23 CN CNA2007101245970A patent/CN101440008A/en active Pending
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102335625A (en) * | 2011-07-15 | 2012-02-01 | 西安近代化学研究所 | Application of metal formates as combustion catalyst in solid propellant |
| CN102335625B (en) * | 2011-07-15 | 2015-11-18 | 西安近代化学研究所 | Metal formate is as the application of combustion catalyst in solid propellant |
| US9413001B2 (en) | 2011-07-20 | 2016-08-09 | Bar Ilan University | Functionalized carbon nanotube composite |
| CN102895966A (en) * | 2012-10-19 | 2013-01-30 | 深圳大学 | PbO/graphene oxide compound powder and preparation method thereof |
| CN104591936A (en) * | 2015-01-29 | 2015-05-06 | 中国工程物理研究院化工材料研究所 | Energetic composite material based on three-dimensional ordered macroporous carbon skeleton and preparation method of energetic composite material |
| CN106187650A (en) * | 2016-07-25 | 2016-12-07 | 万载县建坤化工有限公司 | Fireworks and firecrackers opens quick-fried medicament composition |
| CN106187650B (en) * | 2016-07-25 | 2018-02-27 | 万载县建坤化工有限公司 | Fireworks and firecrackers opens quick-fried medicament composition |
| CN108393082A (en) * | 2018-03-06 | 2018-08-14 | 淮南市通霸蓄电池有限公司 | A kind of Nanometer sized lead oxide-carbon composite and preparation method thereof |
| CN108393082B (en) * | 2018-03-06 | 2020-12-01 | 淮南市通霸蓄电池有限公司 | Nano lead oxide-carbon composite material and preparation method thereof |
| CN110137452A (en) * | 2019-04-26 | 2019-08-16 | 浙江工业大学 | A kind of preparation method and application of Nanometer sized lead oxide/carbon composite |
| CN113548932A (en) * | 2021-07-27 | 2021-10-26 | 陕西师范大学 | Nano composite burning rate catalyst of copper metal complex filled with carbon nano tube |
| CN114031959A (en) * | 2021-11-29 | 2022-02-11 | 安徽工业大学 | Regulation and control method of carbon black structure, activated carbon black solid and application of activated carbon black solid to catalyst carrier |
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Application publication date: 20090527 |