CN108393088B - Preparation method of gamma-ferric oxide/rGO composite material with flower-like microsphere structure - Google Patents
Preparation method of gamma-ferric oxide/rGO composite material with flower-like microsphere structure Download PDFInfo
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/343—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of ultrasonic wave energy
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B23/00—Compositions characterised by non-explosive or non-thermic constituents
- C06B23/007—Ballistic modifiers, burning rate catalysts, burning rate depressing agents, e.g. for gas generating
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- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06D—MEANS FOR GENERATING SMOKE OR MIST; GAS-ATTACK COMPOSITIONS; GENERATION OF GAS FOR BLASTING OR PROPULSION (CHEMICAL PART)
- C06D5/00—Generation of pressure gas, e.g. for blasting cartridges, starting cartridges, rockets
Abstract
A preparation method of a gamma-ferric oxide/rGO composite material with a flower-like microsphere structure comprises the steps of adding soluble ferric salt into an ethylene glycol solution of graphene oxide, uniformly stirring, then dropwise adding a sodium hydroxide aqueous solution, stirring for 30min, reacting for 12-18 h at 150-180 ℃, washing, and drying for 12h at 200 ℃ to obtain the gamma-ferric oxide/rGO composite material with the flower-like microsphere structure. The iron oxide surface in the product of the invention has a large amount of void structures, and the special structure thereof obviously increases the specific surface area and the reaction active sites, and is more beneficial to the transfer of electrons and the conduction of protons in the process of catalytic pyrolysis of energy-containing components. Fe of the invention2O3the/rGO composite material can be used as a combustion catalyst and has excellent catalytic effect on energetic materials HNIW.
Description
Technical Field
The invention belongs to the technical field of nano composite material preparation, and relates to a preparation method of a gamma-ferric oxide/rGO composite material with a flower-shaped microsphere structure.
Background
At present, with the continuous development of solid propulsion technology, high-energy, insensitive, high-burning rate and low-pressure strength indexes become decisive indexes for evaluating the comprehensive application performance of the propellant. In order to meet the requirements of the advanced technology, it is necessary to develop a novel combustion catalyst. Research shows that the single metal oxide as a combustion catalyst has obviously poorer catalytic effect than a composite combustion catalyst.
Graphene, as a novel carbon nanomaterial with a high specific surface area, has excellent conductivity and mechanical properties. The catalyst can be used as a catalyst to be applied to the field of propellants, and can also be used as a substrate substance to be compounded with other components. The single metal oxide has small particle size and high specific surface energy, and the particles are easy to agglomerate, so that the active sites on the surface are reduced. The graphene is compounded with the metal oxide, so that metal oxide particles can be uniformly loaded on the surface of the graphene, and the purposes of inhibiting the agglomeration of the particles and increasing active sites are achieved. Therefore, when the composite material is applied to the field of solid propellant, the complementary synergistic effect of the composite material and the solid propellant can be fully exerted, and the catalytic effect is improved.
Disclosure of Invention
The invention aims to provide a simple, convenient, easy-to-operate and controllable preparation method of a gamma-ferric oxide/rGO composite material with a flower-like microsphere structure.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a gamma-ferric oxide/rGO composite material with a flower-like microsphere structure comprises the steps of adding soluble ferric salt into an ethylene glycol solution of graphene oxide, uniformly stirring, then dropwise adding a sodium hydroxide aqueous solution, stirring for 30min, reacting for 12-18 h at 150-180 ℃, washing, and drying to obtain the gamma-ferric oxide/rGO composite material with the flower-like microsphere structure.
A further improvement of the present invention is that the ethylene glycol solution of graphene oxide is prepared by the following method: 5-40 mg: and adding 10mL of graphene oxide into ethylene glycol, and performing ultrasonic treatment to obtain the graphene oxide.
The invention has the further improvement that the power of the ultrasonic wave is 600W, and the time is 2-3 h.
The invention has the further improvement that the mass ratio of the graphene oxide to the soluble iron salt is 5-40 mg: 0.248 g.
In a further improvement of the invention, the soluble ferric salt is ferric nitrate nonahydrate.
The invention has the further improvement that the ratio of the graphene oxide to the sodium hydroxide is 5-40 mg: 1g of the total weight of the composition.
A further development of the invention is that the concentration of the aqueous sodium hydroxide solution is 5 mol/L.
The invention is further improved in that the drying temperature is 200 ℃ and the drying time is 12 h.
Compared with the prior art, the invention has the following beneficial effects: the raw materials adopted in the preparation process are low in price and easy to obtain; the preparation process is simple and has strong controllability; and does not adopt any surfactant, the production cost is cheap; the product prepared by the invention has good dispersibility and uniform particle size distribution. The surface of the iron oxide in the product has a large number of void structures, the specific surface area of the particles is obviously increased by the special structure of the iron oxide, more reactive active sites are provided, and the iron oxide is more beneficial to the transfer of electrons and the conduction of protons in the process of catalytic pyrolysis of energy-containing components. Fe of the invention2O3the/rGO composite material can be used as a combustion catalyst and has excellent catalytic effect on energetic material Hexanitrohexaazaisowurtzitane (HNIW).
Drawings
FIG. 1 is Fe prepared in example 1 and example 32O3And Fe2O3XRD pattern of/rGO.
FIG. 2 Fe prepared in example 32O3High resolution XPS plot of Fe2p for/rGO.
FIG. 3 is Fe prepared in example 12O3SEM image of (d).
FIG. 4 is Fe prepared in example 22O3SEM image of/rGO.
FIG. 5 is Fe prepared in example 32O3SEM image of/rGO.
FIG. 6 is Fe prepared in example 42O3SEM image of/rGO.
FIG. 7 is Fe prepared in example 32O3TEM image of/rGO.
FIG. 8 is Fe prepared in example 2 and example 32O3DSC comparison graph of thermal decomposition of/rGO catalytic energetic material HNIW.
FIG. 9 shows examples 1 and 93 Fe produced2O3And Fe2O3DSC comparison graph of catalytic thermal decomposition of/rGO to energetic material HNIW.
Detailed Description
The present invention will be described in detail below with reference to specific examples.
Example 1
(1) Weighing 0.248g ferric nitrate nonahydrate, dissolving in 10mL ethylene glycol, and magnetically stirring for 30 min;
(2) adding sodium hydroxide into water to obtain a 5mol/L sodium hydroxide aqueous solution, slowly dropwise adding the 5mol/L sodium hydroxide aqueous solution into the solution obtained in the step (1), and continuously stirring for 30 min;
(3) after stirring, transferring the reaction solution into a 25mL hydrothermal kettle, and reacting for 12-18 h at 150-180 ℃;
(4) and after the reaction is finished, naturally cooling to room temperature, centrifugally washing, and drying by air blowing at 200 ℃ for 12 hours to obtain the product 1.
(5) The volume ratio of the solvent required by the reaction is as follows: ethylene glycol: water 2: 1.
Example 2
(1) Weighing 5mg of graphene oxide in 10mL of ethylene glycol, and ultrasonically dispersing for 2-3 h at 600W until brown yellow transparent turbid liquid is formed;
(2) weighing 0.248g of ferric nitrate nonahydrate in the suspension obtained in the step (1), and magnetically stirring for 30 min;
(3) adding sodium hydroxide into water to obtain a 5mol/L sodium hydroxide aqueous solution, slowly dropwise adding the 5mol/L sodium hydroxide aqueous solution (the volume of the water is 5mL) into the solution obtained in the step (2), and continuously stirring for 30min after dropwise adding is finished to obtain a reaction solution;
(4) transferring the reaction solution into a 25mL hydrothermal kettle, and reacting for 12h at 150 ℃;
(5) after the reaction is finished, naturally cooling to room temperature, centrifugally washing, and drying by air blowing at 200 ℃ for 12h to obtain the gamma-ferric oxide/rGO composite material with the flower-like microsphere structure, namely a product 2 (marked as Fe)2O3/rGO-0.5)。
Example 3
(1) Weighing 20mg of graphene oxide in 10mL of ethylene glycol, and ultrasonically dispersing for 2-3 h at 600W until brown yellow transparent turbid liquid is formed;
(2) weighing 0.248g of ferric nitrate nonahydrate in the suspension obtained in the step (1), and magnetically stirring for 30 min;
(3) adding sodium hydroxide into water to obtain a 5mol/L sodium hydroxide aqueous solution, slowly dropwise adding the 5mol/L sodium hydroxide aqueous solution (the volume of the water is 5mL) into the solution obtained in the step (2), and continuously stirring for 30min after dropwise adding is finished to obtain a reaction solution;
(4) after stirring, transferring the reaction solution into a 25mL hydrothermal kettle, and reacting for 12h at 150 ℃;
(5) after the reaction is finished, naturally cooling to room temperature, centrifugally washing, and drying by air blast at 200 ℃ for 12h to obtain the gamma-ferric oxide/rGO composite material with the flower-like microsphere structure, namely a product 3 (marked as Fe)2O3/rGO-2)。
Example 4
(1) Weighing 40mg of graphene oxide in 10mL of ethylene glycol, and ultrasonically dispersing for 2-3 h at 600W until brown yellow transparent turbid liquid is formed;
(2) weighing 0.248g of ferric nitrate nonahydrate in the suspension obtained in the step (1), and magnetically stirring for 30 min;
(3) adding sodium hydroxide into water to obtain a 5mol/L sodium hydroxide aqueous solution, slowly dropwise adding the 5mol/L sodium hydroxide aqueous solution (the volume of the water is 5mL) into the solution obtained in the step (2), and continuously stirring for 30min after dropwise adding is finished to obtain a reaction solution;
(4) after stirring, transferring the reaction solution into a 25mL hydrothermal kettle, and reacting for 12h at 150 ℃;
(5) after the reaction is finished, naturally cooling to room temperature, centrifugally washing, and drying at 200 ℃ for 12 hours to obtain the gamma-ferric oxide/rGO composite material with the flower-like microsphere structure, namely a product 4 (marked as Fe)2O3/rGO-4)。
As can be seen from FIG. 1, all the characteristic diffraction peaks of the XRD profile of the product prepared in example 1 were associated with γ -Fe2O3Match (PDF # 39-1364). Characterization in XRD Profile of the product prepared from example 3The peaks also all matched the standard card and no impurity peaks appeared, indicating Fe produced2O3the/rGO is a pure phase material.
As can be seen from FIG. 2, it is Fe prepared in example 32O3XPS high resolution Fe2p spectra corresponding to/rGO. From satellite peaks clearly present in the XPS chart, it can be concluded that iron in the prepared iron oxide is +3 valent.
As can be seen from FIG. 3, Fe prepared in example 12O3The surfaces of the particles are provided with a large number of gaps, and the flower-shaped microspheres with the particle size of about 1um are self-assembled by a large number of sheet structures in the hydrothermal reaction process and slightly agglomerate.
As is clear from FIG. 4, Fe obtained in example 22O3in/rGO-0.5, Fe2O3The particles are not uniformly dispersed, the particle morphology is not uniform, part of the particles still keep a microspherical shape of about 1um, and part of the particles show a flower-shaped structure with obviously reduced particle size and obviously changed morphology.
As can be seen from FIG. 5, Fe prepared in example 32O3in/rGO-2, Fe2O3The particles are uniformly dispersed, uniform in appearance, and all have flower-shaped structures with the size of about 200nm, and are uniformly loaded on the graphene sheet layer. Addition of graphene to Fe2O3The microstructure of (a) is significantly changed. The graphene suppresses agglomeration of particles and allows the particle size of the particles to be greatly reduced.
As can be seen from FIG. 6, Fe prepared in example 42O3/rGO-4，Fe2O3The particles are uniformly dispersed and uniform in particle morphology, and the particles are attached between graphene sheet layers and slightly agglomerated.
As is clear from FIG. 7, Fe obtained in example 32O3TEM image of/rGO-2, Fe2O3The particles are all shown as flower-like structures and are uniformly dispersed on the surface of the graphene lamellar structure, and Fe2O3SEM images of/rGO-2 are consistent.
Fe synthesized by the methods of example 1, example 2 and example 32O3And Fe2O3(ii)/rGO is mixed with HNIW at a ratio of 1: 4, mixing and grinding uniformly. And (3) researching the thermal decomposition catalytic effect of the prepared sample on HNIW by adopting differential scanning calorimetry. And (3) testing conditions are as follows: the sample dosage is as follows: 0.10-0.18 mg; the heating rate is 10 ℃/min; temperature range: 40-300 ℃; atmosphere: and (3) a nitrogen atmosphere.
From fig. 8, it can be seen that Fe with two different graphene concentrations was prepared2O3the/rGO complex shows different catalytic effects on HNIW. Wherein, Fe2O3The thermal decomposition temperature of/rGO-2 to HNIW has the maximum change range, and the decomposition temperature is reduced by 6.58 ℃, so that Fe2O3The catalytic thermal decomposition effect of/rGO-2 on HNIW is better than that of Fe2O3/rGO-0.5. According to SEM image analysis, the change of the graphene concentration has obvious influence on the particle size, the graphene concentration is increased, the iron oxide particle size is reduced, the specific surface area is increased, contact sites with HNIW are increased, and the catalytic effect is enhanced.
As can be seen from FIG. 9, Fe2O3Pure component Fe in/rGO-2 ratio2O3The effect on the thermal decomposition temperature of HNIW is more obvious. Due to the addition of the graphene, on one hand, the agglomeration of iron oxide particles is inhibited, the diameter of the iron oxide particles is obviously reduced, and the specific surface area is increased; on the other hand, graphene has excellent heat conductivity and mechanical strength, and complementary synergistic effect of the graphene and the graphene is utilized, so that the thermal decomposition temperature and the thermal decomposition apparent activation energy of HNIW are reduced, the burning rate is further improved, and the catalytic pyrolysis effect on the thermal decomposition of the energetic material is more excellent.
Example 5
According to the weight proportion of 30 mg: adding 10mL of graphene oxide into ethylene glycol, and performing ultrasonic treatment for 3 hours at 600W to obtain an ethylene glycol solution of the graphene oxide; 1g of sodium hydroxide was added to 5mL of water to prepare an aqueous sodium hydroxide solution.
Adding 0.248g of ferric nitrate nonahydrate into an ethylene glycol solution of graphene oxide, uniformly stirring, then dropwise adding a sodium hydroxide aqueous solution, stirring for 30min after dropwise adding, then reacting for 18h at 150 ℃, naturally cooling to room temperature after the reaction is finished, centrifugally washing, and drying for 12h at 200 ℃ to obtain the gamma-ferric oxide/rGO composite material with a flower-like microsphere structure.
Example 6
According to the weight ratio of 40 mg: 10mL, adding 40mg of graphene oxide into ethylene glycol, and performing ultrasonic treatment for 3 hours at 600W to obtain an ethylene glycol solution of the graphene oxide; 1g of sodium hydroxide was added to 5mL of water to prepare an aqueous sodium hydroxide solution.
Adding 0.248g of ferric nitrate nonahydrate into an ethylene glycol solution of graphene oxide, uniformly stirring, then dropwise adding a sodium hydroxide aqueous solution, stirring for 30min after dropwise adding, then reacting at 180 ℃ for 12h, naturally cooling to room temperature after the reaction is finished, centrifugally washing, and drying at 200 ℃ for 12h to obtain the gamma-ferric oxide/rGO composite material with a flower-like microsphere structure.
Example 7
According to the weight ratio of 20 mg: 10mL, adding 20mg of graphene oxide into ethylene glycol, and performing ultrasonic treatment for 3 hours at 600W to obtain an ethylene glycol solution of the graphene oxide; 1g of sodium hydroxide was added to 5mL of water to prepare an aqueous sodium hydroxide solution.
Adding 0.248g of ferric nitrate nonahydrate into an ethylene glycol solution of graphene oxide, uniformly stirring, then dropwise adding a sodium hydroxide aqueous solution, stirring for 30min after dropwise adding, then reacting for 16h at 160 ℃, naturally cooling to room temperature after the reaction is finished, centrifugally washing, and drying for 12h at 200 ℃ to obtain the gamma-ferric oxide/rGO composite material with a flower-like microsphere structure.
Example 8
According to the weight proportion of 10 mg: 10mL, adding 10mg of graphene oxide into ethylene glycol, and performing ultrasonic treatment for 3 hours at 600W to obtain an ethylene glycol solution of the graphene oxide; 1g of sodium hydroxide was added to 5mL of water to prepare an aqueous sodium hydroxide solution.
Adding 0.248g of ferric nitrate nonahydrate into an ethylene glycol solution of graphene oxide, uniformly stirring, then dropwise adding a sodium hydroxide aqueous solution, stirring for 30min after dropwise adding, then reacting at 170 ℃ for 13h, naturally cooling to room temperature after the reaction is finished, centrifugally washing, and drying at 200 ℃ for 12h to obtain the gamma-ferric oxide/rGO composite material with a flower-like microsphere structure.
The composite material can be used as a combustion catalyst of a solid propellant, so that the combustion rate is improved, and the pressure index is reduced.
Claims (5)
1. The application of the gamma-ferric oxide/rGO composite material with the flower-like microsphere structure in the combustion catalyst serving as a solid catalyst is characterized in that a soluble ferric salt is added into an ethylene glycol solution of graphene oxide, the mixture is uniformly stirred, then a sodium hydroxide aqueous solution is dripped, after the dripping is finished, the mixture is stirred for 30min, the mixture reacts for 12 to 18 hours at the temperature of 150 to 180 ℃, and the mixture is washed and dried to obtain the gamma-ferric oxide/rGO composite material with the flower-like microsphere structure; wherein the mass ratio of the graphene oxide to the soluble iron salt is 5-40 mg: 0.248g, the ratio of graphene oxide to sodium hydroxide is 5-40 mg: 1g of a compound; the soluble ferric salt is ferric nitrate nonahydrate.
2. The use of a gamma-ferric oxide/rGO composite material of flower-like microsphere structure as claimed in claim 1 in a combustion catalyst as a solid catalyst, characterized in that the ethylene glycol solution of graphene oxide is prepared by the following method: 5-40 mg: and adding 10mL of graphene oxide into ethylene glycol, and performing ultrasonic treatment to obtain the graphene oxide.
3. The application of the gamma-ferric oxide/rGO composite material with the flower-like microsphere structure in the combustion catalyst as the solid catalyst according to claim 2 is characterized in that the power of ultrasound is 600W, and the time is 2-3 h.
4. The use of a gamma-ferric oxide/rGO composite material with a flower-like microsphere structure as claimed in claim 1 in a combustion catalyst as a solid catalyst, wherein the concentration of the aqueous sodium hydroxide solution is 5 mol/L.
5. The use of a gamma-ferric oxide/rGO composite material with a flower-like microsphere structure as claimed in claim 1 in a combustion catalyst as a solid catalyst, wherein the drying temperature is 200 ℃ and the drying time is 12 h.
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| CN102847536A (en) * | 2012-09-17 | 2013-01-02 | 河海大学 | Composite photocatalytic material, and preparation method and application thereof |
| CN107043133A (en) * | 2017-03-27 | 2017-08-15 | 淮阴师范学院 | Flower-shaped γ Fe2O3The preparation method of microballoon |
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| CN102847536A (en) * | 2012-09-17 | 2013-01-02 | 河海大学 | Composite photocatalytic material, and preparation method and application thereof |
| CN107043133A (en) * | 2017-03-27 | 2017-08-15 | 淮阴师范学院 | Flower-shaped γ Fe2O3The preparation method of microballoon |
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