CN114276850B - Fluorine-doped graphene-loaded Pb composite material and preparation method and application thereof - Google Patents
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Abstract
The invention belongs to the technical field of nano composite materials, and particularly relates to a fluorine-doped graphene loaded Pb composite material, and a preparation method and application thereof, wherein graphene oxide and lead fluoride are used as raw materials, an N-methyl pyrrolidone solution is used as a solvent, sodium borohydride is used as a reducing agent, a poloxamer surfactant is used, and on the basis of preparing reduced graphene as a carrier, poloxamer hydrolysis and metal ion complexation are utilized to realize in-situ self-assembly loading of lead on the reduced graphene, and the addition of poloxamer plays a role in slow release and stability to enable the lead to slowly grow, so that large particles and agglomeration phenomena are avoided to a certain extent, the prepared reduced graphene composite material has high dispersity and uniformity of loaded particles, and the particle size of the loaded particles can reach 40nm at the minimum. The invention has low operation difficulty and simple experimental equipment, and is beneficial to realizing batch production.
Description
Technical Field
The invention belongs to the technical field of nano composite materials, and particularly relates to a fluorine-doped graphene loaded Pb composite material and a preparation method and application thereof.
Background
In recent years, nanotechnology is well known, and nano catalysts are increasingly applied to the field of catalysis due to small particles, large specific surface area, many active sites and excellent catalytic effect. The combustion rate of solid fuels depends on the contact area of the oxidant and the fuel and the catalytic effect of the catalyst. The burning rate and energy performance directly determine the burning performance of the solid fuel, and Ammonium Perchlorate (AP) is one of the most common oxidants, and the burning rate and stability of the solid fuel can be improved by enhancing the thermal decomposition of the AP. The nano lead and the oxide thereof can effectively catalyze the AP thermal decomposition. The Pb particles grow slowly in the solution, the deposition growth process of the Pb particles on the surface of the carrier is easy to control, and the formation of the nano-scale load particles is facilitated, so that the nano-scale Pb/PbO can improve the burning rate of fuel under low pressure, reduce the burning rate of the formula under high pressure and reduce the pressure index.
The graphene serving as a novel two-dimensional material has ultrahigh specific surface area, thermal property and electrochemical property. Has been a hot spot of research for more than a decade. Heteroatom doping of graphene is a common method for modifying graphene, and newly introduced heteroatoms can change the structure of graphene itself to form new chemical bonds or active sites, so that the structure and properties of graphene are changed to some extent, which often enables the graphene to generate new characteristics or enhance certain properties, such as: thermal conductivity, electrical conductivity, etc., which are advantageous for their application in specific fields. The fluorine element enables the fluorine-doped graphene to have a plurality of unique properties such as further enhanced electrochemical performance, high strength and stable thermodynamic and chemical properties due to the ultra-high electronegativity. But also leads to difficult C-F bond formation, so that the doping of fluorine element requires more harsh environment and conditions compared with the doping of other elements, but the doping brings more active sites for graphene and better catalytic performance.
The problems of reduced mechanical strength, poor stability, increased combustion pressure index and the like exist in the combustion process of some common solid fuels at present, so people generally adopt combustion-supporting catalysts to improve the problems, the addition of the catalysts is accompanied with the improvement of the cost, however, the common nano combustion catalysts are easy to agglomerate, the reduction of active sites is caused, the catalytic performance is reduced, the catalytic effect is not satisfactory, and the simple mechanical mixing of the catalysts and the solid fuels not only easily destroys the structures of the catalysts and the fuels, but also easily weakens the uniform dispersion among the components of the catalysts.
Due to the fact that carbon-fluorine bonds are difficult to form, the difficulty of fluorine doping is greatly increased, researches show that although fluorine and Pb nanoparticles can synergistically catalyze AP thermal decomposition, the fluorine and the Pb nanoparticles have a certain competitive relationship on a graphene carrier, and an effective method for solving the problem is not available in the prior art.
Disclosure of Invention
The invention aims to overcome the problems in the prior art and provide a fluorine-doped graphene loaded Pb composite material and a preparation method and application thereof.
In order to achieve the technical purpose and achieve the technical effect, the invention is realized by the following technical scheme:
a preparation method of a fluorine-doped graphene loaded Pb composite material comprises the following steps:
1) Dissolving a proper amount of graphene oxide in distilled water, adding hydrazine hydrate after ultrasonic dispersion, then transferring the solution to a stainless steel high-temperature reaction kettle, carrying out high-temperature hydrothermal reaction to obtain a mixture, washing the mixture with distilled water, and drying to obtain reduced graphene;
2) Mixing a proper amount of reduced graphene and polyvinylidene fluoride, dissolving in distilled water, performing ultrasonic dispersion, immediately adding trifluoroethylene, stirring in an ice water bath by using magnetic force to obtain a mixed solution, transferring the mixed solution into a stainless steel reaction kettle, and performing high-temperature hydrothermal reaction to obtain fluorine-doped reduced graphene;
3) Adding a proper amount of fluorine-doped reduced graphene into distilled water and N-methyl pyrrolidone, performing ultrasonic dispersion to obtain a mixed solution, adding lead fluoride and excessive sodium borohydride into the mixed solution, heating and reacting under stirring to obtain a product, washing and filtering the product, transferring the product into a porcelain boat, and calcining the product for 1-2 hours at high temperature by using a tubular furnace to obtain the fluorine-doped graphene loaded Pb composite material.
Further, according to the preparation method of the fluorine-doped graphene-loaded Pb composite material, in the step 1), the proportion of the graphene oxide to the hydrazine hydrate is 1g.
Further, in the preparation method of the fluorine-doped graphene-loaded Pb composite material, in the step 2), the temperature of the high-temperature hydrothermal reaction is 80-100 ℃, and the reaction time is 3-5 hours.
Further, in the preparation method of the fluorine-doped graphene-loaded Pb composite material, in the step 2), the mass ratio of the reduced graphene to the polyvinylidene fluoride is 1-3:1.
further, in the preparation method of the fluorine-doped graphene-loaded Pb composite material, in the step 2), the temperature of the high-temperature hydrothermal reaction is 90-200 ℃, and the reaction time is 12-36h.
Further, in the preparation method of the fluorine-doped graphene-loaded Pb composite material, in the step 3), the mass ratio of the fluorine-doped reduced graphene to the lead fluoride is 1.1-0.5.
Further, according to the preparation method of the fluorine-doped graphene-loaded Pb composite material, in the step 3), the poloxamer is added while the lead fluoride is added, and the mass ratio of the fluorine-doped reduced graphene to the lead fluoride to the poloxamer is 1.1-0.5: 1-5.
Further, according to the preparation method of the fluorine-doped graphene-loaded Pb composite material, in the step 3), the heating reaction temperature is 80-120 ℃, and the reaction time is 1-2h.
Further, in the preparation method of the fluorine-doped graphene-loaded Pb composite material, in the step 3), the high-temperature calcination temperature is 400-600 ℃.
A fluorine-doped graphene loaded Pb composite material is prepared by the preparation method. The fluorine-doped reduced graphene loaded Pb composite material has good dispersibility, can still keep stable and unchanged after high-temperature treatment, and has good application in the aspect of catalytic combustion-supporting solid fuel.
The invention has the beneficial effects that:
1. according to the invention, graphene oxide is used as a base material, and the unique characteristics of two-dimensional structure, high surface area and high thermal stability of the graphene oxide are utilized, hydrazine hydrate is firstly used for reducing oxygen-containing functional groups on the surface of the graphene oxide, active sites are increased, surface and structural defect sites are further increased through fluorine doping modification, and the loaded metal nanoparticles are uniformly and highly dispersed on the graphene oxide by an in-situ self-assembly method, so that the capability of the nanoparticles for promoting electron transfer in the reaction process is enhanced, the heat conduction performance is improved, AP thermal decomposition is more effectively catalyzed, and the combustion performance and stability of the solid fuel are further improved.
2. In the preparation process of the fluorine-doped reduced graphene loaded Pb nano composite material, the limit of high temperature and high pressure is avoided, the safety and the stability of the whole process are high, and the loaded nano particles are loaded by an in-situ self-assembly method, so that the loading effect is good, the operation is simple and convenient, the dependence on equipment is low, the risk coefficient in the whole preparation process is low, and the energy consumption is low. The graphene oxide raw material is prepared in a laboratory and produced in a factory, and the mass production in the factory can be realized at present. In summary, the preparation method is simple, safe, reliable, low in cost and controllable.
3. The method is applied to the field of catalyzing AP and AP-based solid fuels, the prepared material is mixed with Ammonium Perchlorate (AP) according to a certain proportion, compared with a mechanical mixing method, the method disclosed by the invention mixes the sample and uses ethanol as a solvent for mixing, so that the sample and the solvent can be mixed more uniformly without damaging the structure of the material, and after the mixture is mixed by the method, the mixture is dried and subjected to experimental tests, so that the experimental result is more accurate and the effect is more obvious.
4. The catalyst has good catalytic performance after being mixed with AP, and can effectively shorten the thermal decomposition plateau period on the basis of reducing the high-temperature thermal decomposition temperature of the AP. As is well known, the thermal decomposition process of AP has a crucial influence on the combustion performance of solid fuel, and test results show that the fluorine-doped reduced graphene loaded Pb nanocomposite prepared by the invention can improve the combustion speed of the solid fuel under the low-pressure condition and limit the combustion speed under the high-pressure condition after being mixed with the AP, and the pressure index in the combustion process is stabilized.
Of course, it is not necessary for any one product that embodies the invention to achieve all of the above advantages simultaneously.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a scanning electron micrograph of the product obtained in example 1;
FIG. 2 is a scanning electron micrograph of the product obtained in example 2;
FIG. 3 is a scanning electron micrograph of the product obtained in example 3;
FIG. 4 is a scanning electron micrograph of the product obtained in example 4;
FIG. 5 is an XRD pattern of the product obtained in example 1;
FIG. 6 is a thermogram of the intermediate product obtained in example 1, the product after mixing with AP.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
According to the preparation method, graphene oxide and lead fluoride are used as raw materials, an N-methyl pyrrolidone solution is used as a solvent, sodium borohydride is used as a reducing agent, a poloxamer surfactant is used, and on the basis that reduced graphene is prepared as a carrier, poloxamer hydrolysis and metal ion complexation are utilized to realize in-situ self-assembly loading of lead on the reduced graphene, and the poloxamer is added to play a role in slow release and stabilization, so that the lead can slowly grow, large particles and agglomeration are avoided to a certain extent, and the loaded particles of the prepared reduced graphene composite material have high dispersibility and uniformity.
The related specific embodiments of the invention are as follows:
example 1
A fluorine-doped graphene loaded Pb composite material is prepared by the following steps:
1) Firstly, 0.1g of graphene oxide is dissolved in 20mL of distilled water, after 30min of ultrasonic dispersion, 10mL of hydrazine hydrate is added and stirred for 10min to obtain a mixed solution a, the mixed solution a is transferred to a high-temperature reaction kettle with a polytetrafluoroethylene lining, the reaction is carried out for 2h at 90 ℃, the obtained mixture is washed by distilled water and dried to obtain reduced graphene, and the preparation is repeated to obtain sufficient samples.
2) And (2) fully mixing 0.1g of reduced graphene and 0.05g of polyvinylidene fluoride (PVDF), dissolving in 30mL of distilled water, performing ultrasonic dispersion for 30min, immediately adding 20mL of trifluoroacetic acid, and performing magnetic stirring for 30min under the ice-water bath condition to obtain a mixed solution b. And transferring the mixed solution b into a Teflon lining, placing the lining into a stainless steel reaction kettle, and reacting for 32 hours at 120 ℃ to obtain the fluorine-doped reduced graphene.
3) Adding 0.1g of fluorine-doped reduced graphene into 10mL of water and 10mL of N-methylpyrrolidone (NMP), performing ultrasonic dispersion for 10min to obtain a mixed solution c, adding 0.05g of lead fluoride and excessive sodium borohydride into the mixed solution c, heating to 90 ℃ under stirring, reacting for 2h to obtain a product, washing and filtering the product, transferring the product into a porcelain boat, heating the product to 600 ℃ in a tubular furnace at the speed of 10 ℃/min, and calcining for 1h at the temperature to obtain the fluorine-doped reduced graphene loaded Pb composite material.
And (2) putting 0.01g of the fluorine-doped reduced graphene loaded Pb material and 0.2g of ammonium perchlorate into 20mL of ethanol, stirring for 1h, drying to obtain a mixed sample, taking 0.01g of the mixed sample, heating to 500 ℃ at 5 ℃/min under a nitrogen atmosphere, and carrying out TG-DTA analysis test, thereby obtaining the evaluation of the AP pyrolysis performance of the fluorine-doped oxidized graphene loaded Pb composite material.
The fluorine-doped reduced graphene loaded Pb composite material prepared by the embodiment has good catalytic performance and stable loaded particle performance, the loaded particles can keep a good original state for a long time after being calcined at high temperature, and after a small amount of the loaded particles are added into AP and uniformly mixed, the thermal decomposition temperature of the AP can be effectively reduced, the burning rate of solid fuel is improved, the burning pressure is stabilized, and the overall burning performance of the solid fuel is improved.
Example 2
A fluorine-doped graphene loaded Pb composite material is prepared by the following steps:
1) Firstly, 0.1g of graphene oxide is dissolved in 20mL of distilled water, after 30min of ultrasonic dispersion, 10mL of hydrazine hydrate is added and stirred for 10min to obtain a mixed solution a, the mixed solution a is transferred to a high-temperature reaction kettle with a polytetrafluoroethylene lining, the reaction is carried out for 4h at 70 ℃, the obtained mixture is washed by distilled water and dried to obtain reduced graphene, and the preparation is repeated to obtain sufficient samples.
2) And (2) fully mixing 0.1g of reduced graphene and 0.05g of polyvinylidene fluoride (PVDF), dissolving in 35mL of distilled water, performing ultrasonic dispersion for 30min, immediately adding 15mL of trifluoroacetic acid, and performing magnetic stirring for 30min under the ice-water bath condition to obtain a mixed solution b. And transferring the mixed solution b into a Teflon lining, placing the lining into a stainless steel reaction kettle, and reacting for 12 hours at 180 ℃ to obtain the fluorine-doped reduced graphene.
3) Taking 0.1g of fluorine-doped reduced graphene, adding 10mL of water and 10mL of N-methylpyrrolidone (NMP), performing ultrasonic dispersion for 10min to obtain a mixed solution c, adding 0.1g of poloxamer (F127 surfactant), 0.05g of lead fluoride and excessive sodium borohydride into the mixed solution c, heating to 80 ℃ under stirring, reacting for 2h to obtain a product, washing and filtering the product, transferring the product into a porcelain boat, entering a tubular furnace, heating to 400 ℃ at a speed of 10 ℃/min, and calcining at the temperature for 2h to obtain the fluorine-doped reduced graphene loaded Pb composite material.
And (3) putting 0.01g of the fluorine-doped reduced graphene loaded Pb material and 0.2g of ammonium perchlorate into 20mL of ethanol, stirring for 1h, drying to obtain a mixed sample, taking 0.01g of the mixed sample, heating to 500 ℃ at 5 ℃/min under the nitrogen atmosphere, and carrying out TG-DTA analysis test, thereby obtaining the evaluation of the catalytic AP pyrolysis performance of the fluorine-doped reduced graphene loaded Pb composite material.
The fluorine-doped reduced graphene Pb-loaded composite material prepared by the embodiment has good catalytic performance, the loaded particles are uniformly dispersed and stable in performance, the particle size is about 100nm, the loaded particles can keep a good original state for a long time after being calcined at high temperature, and after a small amount of the loaded particles are added into AP and uniformly mixed, the AP thermal decomposition temperature can be effectively reduced, the burning rate of solid fuel is improved, the burning pressure is stabilized, and the overall burning performance of the solid fuel is improved.
Example 3
A fluorine-doped graphene loaded Pb composite material is prepared by the following steps:
1) Firstly, 0.1g of graphene oxide is dissolved in 20mL of distilled water, after 30min of ultrasonic dispersion, 10mL of hydrazine hydrate is added and stirred for 10min to obtain a mixed solution a, the mixed solution a is transferred to a high-temperature reaction kettle with a polytetrafluoroethylene lining, the reaction is carried out for 4h at 90 ℃, the obtained mixture is washed by distilled water and dried to obtain reduced graphene, and the preparation is repeated to obtain sufficient samples.
2) And (2) fully mixing 0.1g of reduced graphene and 0.05g of polyvinylidene fluoride (PVDF), dissolving in 40mL of distilled water, performing ultrasonic dispersion for 30min, immediately adding 10mL of trifluoroacetic acid, and performing magnetic stirring for 30min under the ice-water bath condition to obtain a mixed solution b. And (4) transferring the mixed solution b into a Teflon lining, placing the lining into a stainless steel reaction kettle, and reacting for 20 hours at 160 ℃ to obtain the fluorine-doped reduced graphene.
3) Adding 0.1g of fluorine-doped reduced graphene into 10mL of water and 10mL of N-methylpyrrolidone (NMP), performing ultrasonic dispersion for 10min to obtain a mixed solution c, adding 0.3g of poloxamer (F127 surfactant), 0.05g of lead fluoride and excessive sodium borohydride into the mixed solution c, heating to 100 ℃ under stirring, reacting for 2h to obtain a product, washing and filtering the product, transferring the product into a porcelain boat, heating to 600 ℃ in a tubular furnace at a speed of 10 ℃/min, and calcining for 2h at the temperature to obtain the fluorine-doped reduced graphene loaded Pb composite material.
And (3) putting 0.01g of the fluorine-doped reduced graphene loaded Pb material and 0.2g of ammonium perchlorate into 20mL of ethanol, stirring for 1h, drying to obtain a mixed sample, taking 0.01g of the mixed sample, heating to 500 ℃ at 5 ℃/min under the nitrogen atmosphere, and carrying out TG-DTA analysis test, thereby obtaining the evaluation of the catalytic AP pyrolysis performance of the fluorine-doped reduced graphene loaded Pb composite material.
The fluorine-doped reduced graphene loaded Pb composite material prepared by the embodiment has good catalytic performance, good dispersion of the loaded particles and stable performance, the particle size is about 40-80nm, the loaded particles can keep a good original state for a long time after being calcined at high temperature, and after a small amount of the loaded particles are added into AP and uniformly mixed, the thermal decomposition temperature of the AP can be effectively reduced, the burning rate of solid fuel is improved, the burning pressure is stabilized, and the overall burning performance of the solid fuel is improved.
Example 4
A fluorine-doped graphene loaded Pb composite material comprises the following preparation method:
1) Firstly, 0.1g of graphene oxide is dissolved in 20mL of distilled water, after 30min of ultrasonic dispersion, 10mL of hydrazine hydrate is added and stirred for 10min to obtain a mixed solution a, the mixed solution a is transferred to a high-temperature reaction kettle with a polytetrafluoroethylene lining, the reaction is carried out for 4h at 90 ℃, a mixture is obtained, the mixture is washed by distilled water and dried to obtain reduced graphene, and the preparation is repeated to obtain sufficient samples.
2) And (2) fully mixing 0.1g of reduced graphene and 0.05g of polyvinylidene fluoride (PVDF), dissolving in 40mL of distilled water, performing ultrasonic dispersion for 30min, immediately adding 10mL of trifluoroacetic acid, and performing magnetic stirring for 30min under the ice-water bath condition to obtain a mixed solution b. And transferring the mixed solution b into a Teflon lining, placing the lining into a stainless steel reaction kettle, and reacting for 24 hours at 150 ℃ to obtain the fluorine-doped reduced graphene.
3) Adding 0.1g of fluorine-doped reduced graphene into 10mL of water and 10mL of N-methylpyrrolidone (NMP), performing ultrasonic dispersion for 10min to obtain a mixed solution c, adding 0.5g of poloxamer (F127 surfactant), 0.05g of lead fluoride and excessive sodium borohydride into the mixed solution c, heating to 120 ℃ under stirring, reacting for 2h to obtain a product, washing and filtering the product, transferring the product into a porcelain boat, heating to 600 ℃ in a tubular furnace at the speed of 5 ℃/min, and calcining for 2h at the temperature to obtain the fluorine-doped reduced graphene loaded Pb composite material.
And (2) putting 0.01g of the fluorine-doped reduced graphene loaded Pb material and 0.2g of ammonium perchlorate into 20mL of ethanol, stirring for 1h, drying to obtain a mixed sample, taking 0.01g of the mixed sample, heating to 500 ℃ at 5 ℃/min under a nitrogen atmosphere, and carrying out TG-DTA analysis and test, thereby obtaining the evaluation of AP pyrolysis performance of the fluorine-doped reduced graphene loaded Pb composite material.
The fluorine-doped reduced graphene Pb-loaded composite material prepared by the embodiment has good catalytic performance, the loaded particles are uniformly dispersed and stable in performance, the particle size is about 10nm, the loaded particles can be kept in the original state for a long time after being calcined at high temperature, a small amount of the loaded particles is added into AP and uniformly mixed, the thermal decomposition temperature of the AP can be effectively reduced by about 100 ℃, the combustion speed of solid fuel is improved, the combustion pressure is stabilized, and the overall combustion performance of the solid fuel is improved.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims (5)
1. A preparation method of a fluorine-doped graphene loaded Pb composite material is characterized by comprising the following steps:
1) Dissolving a proper amount of graphene oxide in distilled water, adding hydrazine hydrate after ultrasonic dispersion, then transferring the solution to a stainless steel high-temperature reaction kettle, carrying out high-temperature hydrothermal reaction to obtain a mixture, washing the mixture with distilled water, and drying to obtain reduced graphene; the temperature of the high-temperature hydrothermal reaction is 80-100 ℃, and the reaction time is 3-5h;
2) Mixing a proper amount of reduced graphene and polyvinylidene fluoride, dissolving in distilled water, performing ultrasonic dispersion, immediately adding trifluoroethylene, stirring in an ice water bath by using magnetic force to obtain a mixed solution, transferring the mixed solution into a stainless steel reaction kettle, and performing high-temperature hydrothermal reaction to obtain fluorine-doped reduced graphene; the temperature of the high-temperature hydrothermal reaction is 90-200 ℃, and the reaction time is 12-36h;
3) Adding a proper amount of fluorine-doped reduced graphene into distilled water and N-methyl pyrrolidone, performing ultrasonic dispersion to obtain a mixed solution, adding lead fluoride and excessive sodium borohydride into the mixed solution, wherein the mass ratio of the fluorine-doped reduced graphene to the lead fluoride is 1.1-0.5; heating and reacting under stirring at 80-120 deg.C for 1-2h; and washing and filtering the obtained product, transferring the product into a porcelain boat, and calcining the product for 1 to 2 hours at the high temperature of 400 to 600 ℃ by using a tubular furnace to obtain the fluorine-doped graphene loaded Pb composite material.
2. The method of claim 1, wherein: in the step 1), the proportion of the graphene oxide to the hydrazine hydrate is 1g.
3. The production method according to claim 1, characterized in that: in the step 3), adding poloxamer while adding lead fluoride, wherein the mass ratio of the fluorine-doped reduced graphene to the lead fluoride to the poloxamer is 1.1-0.5: 1-5.
4. A fluorine-doped graphene-loaded Pb composite material prepared by the preparation method of any one of claims 1 to 3.
5. The application of the fluorine-doped graphene loaded Pb composite material in the aspect of catalytic combustion-supporting solid fuel.
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