CN102899122A - Bi2O3/oxidized graphene composite powder and preparation method thereof - Google Patents
Bi2O3/oxidized graphene composite powder and preparation method thereof Download PDFInfo
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- CN102899122A CN102899122A CN2012104046804A CN201210404680A CN102899122A CN 102899122 A CN102899122 A CN 102899122A CN 2012104046804 A CN2012104046804 A CN 2012104046804A CN 201210404680 A CN201210404680 A CN 201210404680A CN 102899122 A CN102899122 A CN 102899122A
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- graphene oxide
- composite granule
- oxide composite
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Abstract
The invention discloses Bi2O3/oxidized graphene composite powder and a preparation method thereof. The Bi2O3/oxidized graphene composite powder comprises the following components by mass percent: 50-80 percent of Bi2O3 and 20-50 percent of oxidized graphene, wherein Bi2O3 is loaded on the surface of oxidized graphene by a nano-particle of which the granularity is 10-50nm to form a load-type composite powder material. The preparation method comprises the following steps of: adding oxidized graphene into water for performing ultrasonic dispersion; adding a dispersing agent; adding bismuth salt solution into water; stirring; alkalizing and depositing; filtering; washing; drying; and firing to prepare the composite powder. The Bi2O3/oxidized graphene composite powder prepared by the method is used as a combustion catalyst, so that the burning of a biradical propellant has good catalysis effect; and therefore, the combustion catalyst is toxic-free and environment-friendly.
Description
Technical field
That the present invention relates to is a kind of Bi
2O
3/ graphene oxide composite granule and preparation method thereof.Bi
2O
3/ graphene oxide composite granule can be used as the environmentally friendly combustioncatalysts that double-basis is propelling agent.
Background technology
Double-base propellent and composite modified double base propellant are the used class high energy fuels of rocket and guided missile, actual with the time need to add combustioncatalysts and improve its combustionproperty.Double-basis is that the burningrate catalyst that uses in the propelling agent mainly is lead compound, the adding of lead compound, and the combustion that can improve double-base propellent is fast, also can reduce Pressure Exponent.Because the catalytic performance of composite catalyst is better than unit catalyzer, can " complementation " because form the catalytic performance of the various components of composite catalyst, thereby produce " synergistic effect ", its catalytic effect is better than the unit catalyzer of single component, therefore often adopts the composite catalyst that forms take lead compound as Primary Catalysts.Add a small amount of carbon black and make the binary compound combustion catalyzer that promotor forms " lead-carbon " system in lead compound, its catalytic effect will be significantly higher than lead compound.In the binary composite catalyst of this " lead-carbon " system, lead compound is Primary Catalysts, and carbon black is indispensable promotor.But lead compound has toxicity to human body, experiment, preparation, use and powder column is processed and the links such as rocket engine exhaust to the staff with environment stays directly and indirectly harm.Therefore, the nontoxic or hypotoxicity of exploitation, free of contamination burningrate catalyst become new problem.
Graphene oxide is a kind of carbonaceous novel material of bi-dimensional cellular shape crystalline network, have huge theoretical specific surface area and electronic conduction ability preferably, have excellent heat conductivity and structural stability, and there is again active oxygen-containing functional group in its surface, make it have unique catalytic performance and adsorption property, being 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 graphene oxide are compound.Graphene oxide plays dual parts catalyzer and carrier, catalyzer with the nanoparticle form high dispersing on the graphene oxide surface, graphene oxide is as carrier, can stop the mutual reunion between metal oxide nanoparticles, the nano-metal-oxide catalyzer just can be given full play to the efficient catalytic effect of nanoparticle like this.The simultaneous oxidation Graphene has certain conductivity and heat conductivility, and the electronics of the metal catalyst of institute's load is had modifying function, can the accelerated reaction process in the transfer of electronics and the transmission of heat, increase catalytic effect.As seen, replace carbon black with graphene oxide, will play more excellent promoting catalysis.
Bismuth is a kind of nontoxic element, and bismuth metal and bismuth compound are that the burning of propelling agent has preferably katalysis to double-basis.Although the right katalysis of bismuth compound is lower than lead compound, and is higher than other metallic compound.Therefore, people are that combustioncatalysts has given very large concern to the development bismuth, and obtain some progress, but still remain to be broken through.Replace lead compound with bismuth compound, replace carbon black with graphene oxide, form novel " bismuth-carbon " system binary catalyst, introduce simultaneously nanotechnology, with Bi
2O
3Load on the graphene oxide surface, Bi
2O
3Compound on nanoscale with graphene oxide, their catalytic performance is " complementation " better, produces strong " synergistic effect ", can significantly improve its catalytic effect, and can be by changing Bi
2O
3Content optimize catalytic performance.Therefore, exploitation Bi
2O
3The compound burningrate catalyst of/graphene oxide-loaded type can be solid propellant environmentally friendly efficient burning catalyzer is provided.
Summary of the invention
The objective of the invention is for the problems referred to above, a kind of Bi that is used as the combustioncatalysts of double-basis or composite modified double base propellant is provided
2O
3/ graphene oxide composite granule.
Another object of the present invention provides Bi
2O
3The preparation method of/graphene oxide composite granule.
The invention provides a kind of Bi
2O
3/ graphene oxide composite granule, its component is: Bi
2O
3And graphene oxide, the content of various components is by mass percentage: Bi
2O
3: 50～80%, graphene oxide: 20～50%; Bi
2O
3Load on and form the loading type composite powder material on the graphene oxide surface.
Described Bi
2O
3In/graphene oxide the composite granule: the thickness of used graphene oxide is 1～6nm, loads on the Bi on graphene oxide surface
2O
3The particle diameter of particle is 10～50nm.
Bi of the present invention
2O
3The preparation method of/graphene oxide composite granule, carry out according to the following steps: (1) is dissolved in soluble bismuth salt and is mixed with clear solution in the distilled water; (2) graphene oxide is soluble in water and ultra-sonic dispersion adds an amount of poly(oxyethylene glycol) 400, and dispersed with stirring is even, then adds the bismuth salts solution, at room temperature stirs 1～2 hour; (3) under agitation drip alkaline solution, at room temperature stirred 1 hour the pH value to 9 of regulator solution～10, then stirred 1 hour at 80～90 ℃ of constant temperature; (4) suction filtration, washing, drying; (5) under nitrogen protection, calcined 2 hours, and can make Bi for 300～400 ℃
2O
3/ graphene oxide composite granule.
Described used alkaline solution is: NaOH, KOH, ammoniacal liquor.
Described used soluble bismuth salt is: Bismuth trinitrate.
Bi of the present invention
2O
3/ graphene oxide composite granule double-basis be in the propelling agent as the purposes of environmentally friendly combustioncatalysts, it is that propellant combustion has good catalytic effect to double-basis, and is nontoxic, pollution-free.
Description of drawings
Fig. 1 is graphene oxide and the Bi that obtains behind the case study on implementation 1
2O
3The X-ray diffraction spectrogram (XRD) of/graphene oxide, a is the XRD spectra of graphene oxide; B is Bi
2O
3The XRD spectra of/graphene oxide composite granule, the characteristic diffraction peak that Fig. 1 b occurs and the contrast of PDF card: loaded article is oblique system bismuthous oxide bismuth trioxide (PDF card 65-1209).
Fig. 2 is the Bi that obtains behind the case study on implementation 1
2O
3The transmission electron microscope photo of/graphene oxide can be found out from transmission electron microscope photo, and graphene oxide is very thin transparent sheet-like thing, and thickness is 1nm approximately.Load on the nanometer Bi on graphene oxide surface
2O
3Be spheroidal particle, median size is 40nm approximately.
Fig. 3 is the Bi that obtains behind the case study on implementation 1
2O
3The EDS energy spectrogram of/graphene oxide composite granule, EDS composes three kinds of elements such as existing C, O, Bi, illustrates that product only contains C, O, Bi, three kinds of elements.
Fig. 4 is the burningrate curve of the double-base propellent that obtains behind the case study on implementation 3, as can be seen from Figure 4, adds 3.0% Bi
2O
3/ graphene oxide makes double-base propellent significant hypervelocity burning occur, under 4MPa pressure, contains the combustion speed of propelling agent of catalyzer from 3.19mms
-1Bring up to 7.63mms
-1, improved 139%; At the catalytic efficiency Z of this catalyzer of 4～17MPa (Z=r
c/ r
0, r
0Be the combustion speed of blank formula, r
cFor containing the propellant burning rate of catalyzer) be 2.39,2.05,1.96,1.88,1.78,1.77,1.75.Simultaneously can also significantly reduce Pressure Exponent, the platform combustion zone occurs in 14～20MPa scope, Pressure Exponent is 0.253.
Embodiment
Bi of the present invention
2O
3The concrete preparation method of/graphene oxide composite granule combustioncatalysts is provided in detail by following examples.
Embodiment 1
(1) the five water Bismuth trinitrates that take by weighing 1.32g add 50ml 1.0mol/L salpeter solution in beaker, make mixing solutions, and are stand-by.
(2) take by weighing 0.2g through graphene oxide, add the 200mL deionized water, ultra-sonic dispersion adds the 5mL poly(oxyethylene glycol) 400, mixes, and then adds the bismuth salts solution, and at room temperature constant temperature stirred 1 hour.
(3) under agitation splashing into 2mol/L sodium hydroxide solution to pH value is 9.1, at room temperature stirs 1 hour, then is transferred in the water-bath to stir 1 hour at 85 ℃ of lower constant temperature; Suction filtration adds ultrasonic wave to product washing 2 times and 1 time with distilled water, ethanol respectively, and 60 ℃ lower dry, and under nitrogen protection, 400 ℃ of calcinations 2 hours can make Bi
2O
3/ graphene oxide composite granule.The content that gets Bi element in the product with atomic spectroscopic analysis count by weight percentage into: 67.5%; Conversion obtains containing Bi
2O
3For: 75.3%.
(1) the five water nitric acid that take by weighing 0.80g add 50ml 1.0mol/L nitric acid in beaker, ultrasonic dissolution makes mixing solutions, and is stand-by.
(2) take by weighing the 0.2g graphene oxide, add the 200mL deionized water, ultra-sonic dispersion adds the 5mL poly(oxyethylene glycol) 400, mixes; Then the mixing solutions that adds bismuth salt and mantoquita, at room temperature constant temperature stirred 1 hour; Under agitation splashing into 1mol/L sodium hydroxide to pH value is 9.3, and then stirring at room is 1 hour; Be transferred in the water-bath, stir 1h at 85 ℃ of lower constant temperature.Cooling, suction filtration adds ultrasonic wave to product washing 2 times and 1 time with distilled water, ethanol respectively, 60 ℃ of lower dryings, under nitrogen protection, 400 ℃ of calcinations 2 hours can make Bi
2O
3/ graphene oxide composite granule.The content that gets Bi element in the product with atomic spectroscopic analysis count by weight percentage into: 57.8%; Conversion obtains containing Bi
2O
3For: 64.4%.
Embodiment 3
Bi
2O
3The basic components of the double-base propellent that the katalysis performance test of/graphene oxide composite granule is used is: nitro-cotton (NC, 12.0%N) 59%, nitroglycerine (NG) 30%, diethyl phthalate (DEP) 8.5%, other auxiliary agent 2.5%.Spice is pressed 500g batching, combustioncatalysts Bi
2O
3/ graphene oxide composite granule is outer dosage, and add-on is 3.0%; Contrast blank propelling agent sample and do not contain combustioncatalysts.Sample by absorption-expelling water-put ripe-roll-be cut into the conventional solvent-free companding shaping technique preparation of medicinal strip.
The mensuration of combustion speed adopts the target collimation method.The test temperature of combustion speed test is 20 ℃, pressure range 2MPa～20MPa.
Claims (6)
1. Bi
2O
3/ graphene oxide composite granule is characterized by: Bi
2O
3The component of/graphene oxide composite granule is: Bi
2O
3And graphene oxide, the content of various components is by mass percentage: Bi
2O
3: 50～80%, graphene oxide: 20～50%; Bi
2O
3Load on and form the loading type composite powder material on the graphene oxide surface.
2. Bi according to claim 1
2O
3/ graphene oxide composite granule is characterized in that: the thickness of used graphene oxide is 1～6nm, loads on the Bi on graphene oxide surface
2O
3The particle diameter of particle is 10～50nm.
3. claim 1 or 2 described Bi
2O
3The preparation method of/graphene oxide composite granule, carry out according to the following steps:
(1) soluble bismuth salt is dissolved in is mixed with clear solution in the distilled water;
(2) graphene oxide is soluble in water and ultra-sonic dispersion adds an amount of poly(oxyethylene glycol) 400, and dispersed with stirring is even, then adds the bismuth salts solution, at room temperature stirs 1～2 hour;
(3) under agitation drip alkaline solution, at room temperature stirred 1 hour the pH value to 9 of regulator solution～10, then stirred 1 hour at 80～90 ℃ of constant temperature;
(4) suction filtration, washing, drying;
(5) under nitrogen protection, calcined 2 hours, and can make Bi for 300～400 ℃
2O
3/ graphene oxide composite granule.
4. described Bi according to claim 3
2O
3The preparation method of/graphene oxide composite granule is characterized in that: used alkaline solution is: NaOH, KOH, ammoniacal liquor.
5. described Bi according to claim 3
2O
3The preparation method of/graphene oxide composite granule is characterized in that: used soluble bismuth salt is: Bismuth trinitrate.
6. described Bi according to claim 1
2O
3/ graphene oxide composite granule is as the purposes of environmentally friendly combustioncatalysts in the propelling agent in double-basis.
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| CN105271405A (en) * | 2015-11-25 | 2016-01-27 | 上海交通大学 | Material based on bismuth oxycarbonate or bismuth oxide nano tube and preparation method thereof |
| CN105779081A (en) * | 2016-03-31 | 2016-07-20 | 成都新柯力化工科技有限公司 | Composite graphene nanoplatelet as well as preparation method and application in lubricating grease |
| CN106311256A (en) * | 2016-07-06 | 2017-01-11 | 重庆大学 | Preparation method of graphene/beta-Bi2O3/SrFe12O19 ternary composite magnetic photocatalyst |
| KR20170140020A (en) * | 2016-06-11 | 2017-12-20 | 포항공과대학교 산학협력단 | A process of producing bismuth graphene oxide and a process of adsorbing iodine using bismuth graphene oxide |
| CN107827465A (en) * | 2017-12-23 | 2018-03-23 | 刘彪 | A kind of preparation method of thyrite |
| US10017706B1 (en) | 2014-04-02 | 2018-07-10 | Precision Combustion, Inc. | Additive for combustion enhancement of liquid hydrocarbon fuels |
| CN108913260A (en) * | 2018-07-06 | 2018-11-30 | 合肥市晶谷农业科技开发有限公司 | A kind of biomass fuel pellet |
| CN110336022A (en) * | 2019-07-25 | 2019-10-15 | 广东工业大学 | A kind of preparation method of bismuth compound sulphur combination electrode material |
| CN112591794A (en) * | 2020-12-22 | 2021-04-02 | 武汉工程大学 | Preparation method of bismuth oxide fluorescent quantum dots |
| CN112924534A (en) * | 2021-02-02 | 2021-06-08 | 广东省农业科学院农业质量标准与监测技术研究所 | Preparation method of nano bismuth/graphene composite material and application of nano bismuth/graphene composite material in MALDI-MS |
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| US10017706B1 (en) | 2014-04-02 | 2018-07-10 | Precision Combustion, Inc. | Additive for combustion enhancement of liquid hydrocarbon fuels |
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| CN106311256A (en) * | 2016-07-06 | 2017-01-11 | 重庆大学 | Preparation method of graphene/beta-Bi2O3/SrFe12O19 ternary composite magnetic photocatalyst |
| CN106311256B (en) * | 2016-07-06 | 2019-06-14 | 重庆大学 | A kind of graphene/β-Bi2O3/SrFe12O19The preparation method of tri compound magnetic photocatalyst |
| CN107827465A (en) * | 2017-12-23 | 2018-03-23 | 刘彪 | A kind of preparation method of thyrite |
| CN108913260A (en) * | 2018-07-06 | 2018-11-30 | 合肥市晶谷农业科技开发有限公司 | A kind of biomass fuel pellet |
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| CN110336022A (en) * | 2019-07-25 | 2019-10-15 | 广东工业大学 | A kind of preparation method of bismuth compound sulphur combination electrode material |
| CN112591794A (en) * | 2020-12-22 | 2021-04-02 | 武汉工程大学 | Preparation method of bismuth oxide fluorescent quantum dots |
| CN112924534A (en) * | 2021-02-02 | 2021-06-08 | 广东省农业科学院农业质量标准与监测技术研究所 | Preparation method of nano bismuth/graphene composite material and application of nano bismuth/graphene composite material in MALDI-MS |
| CN112924534B (en) * | 2021-02-02 | 2022-05-03 | 广东省农业科学院农业质量标准与监测技术研究所 | Preparation method of nano bismuth/graphene composite material and application of nano bismuth/graphene composite material in MALDI-MS |
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Application publication date: 20130130 |