CN114835540B - High-energy-density vanadium oxide-loaded boron fuel and impregnation preparation method - Google Patents

High-energy-density vanadium oxide-loaded boron fuel and impregnation preparation method Download PDF

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CN114835540B
CN114835540B CN202210463120.XA CN202210463120A CN114835540B CN 114835540 B CN114835540 B CN 114835540B CN 202210463120 A CN202210463120 A CN 202210463120A CN 114835540 B CN114835540 B CN 114835540B
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boron
vanadium oxide
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powder
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CN114835540A (en
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冯昊
李丹
秦利军
李建国
龚婷
张王乐
惠龙飞
胡逸云
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Xian Modern Chemistry Research Institute
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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
    • C06D5/06—Generation of pressure gas, e.g. for blasting cartridges, starting cartridges, rockets by reaction of two or more solids
    • C—CHEMISTRY; METALLURGY
    • C06—EXPLOSIVES; MATCHES
    • C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
    • C06B21/00—Apparatus or methods for working-up explosives, e.g. forming, cutting, drying
    • C06B21/0083—Treatment of solid structures, e.g. for coating or impregnating with a modifier
    • C—CHEMISTRY; METALLURGY
    • C06—EXPLOSIVES; MATCHES
    • 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
    • C—CHEMISTRY; METALLURGY
    • C06—EXPLOSIVES; MATCHES
    • C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
    • C06B33/00—Compositions containing particulate metal, alloy, boron, silicon, selenium or tellurium with at least one oxygen supplying material which is either a metal oxide or a salt, organic or inorganic, capable of yielding a metal oxide
    • C—CHEMISTRY; METALLURGY
    • C06—EXPLOSIVES; MATCHES
    • C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
    • C06B45/00—Compositions or products which are defined by structure or arrangement of component of product
    • C06B45/18—Compositions or products which are defined by structure or arrangement of component of product comprising a coated component
    • C06B45/30—Compositions or products which are defined by structure or arrangement of component of product comprising a coated component the component base containing an inorganic explosive or an inorganic thermic component
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E30/00—Energy generation of nuclear origin
    • Y02E30/30—Nuclear fission reactors

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Abstract

The invention provides a high-energy-density boron fuel loaded with vanadium oxide and a preparation method thereof by adopting an impregnation method, wherein the method adopts the impregnation method to load the vanadium oxide on the surface of boron powder to form the boron fuel loaded with the vanadium oxide; the impregnation method is to take solution of pentavalent vanadium salt or tetravalent vanadium salt as impregnation liquid, completely soak boron powder particles, and perform drying and calcination to prepare the boron fuel loaded with vanadium oxide; the content of vanadium oxide in the vanadium oxide-loaded boron fuel is 0.1wt.% to 10wt.%. Compared with the traditional physical blending method, the preparation method disclosed by the invention can realize accurate, controllable, uniform and effective distribution of the composition, structure and content of the VOx catalyst on the surface of the boron powder, can effectively improve the utilization efficiency of the catalyst, and has a good application prospect.

Description

High-energy-density vanadium oxide-loaded boron fuel and impregnation preparation method
Technical Field
The invention belongs to the technical field of high-energy solid propellants, relates to boron fuel, and particularly relates to high-energy-density boron fuel loaded with vanadium oxide and an impregnation preparation method.
Background
Metals such as aluminum, boron, beryllium, magnesium, titanium, zirconium, etc. have been used as fuel additives in a wide variety of applications including high explosive, propellant, air-breathing propulsion, ramjet, and military applications. Among these fuels, boron powder has a theoretical mass energy density (58 kJ/g) and a volume energy density (138 kJ/cm) 3 ) Is much higher than common hydrocarbon fuel (42 kJ/g and 38-40 kJ/cm) 3 ). Boron powder has therefore been considered a very potential, important fuel additive for many years. However, although boron is excellent in energy properties, boron particles form a viscous low melting point B on the surface during oxidation 2 O 3 The oxide layer prevents further oxidation of the boron particles in the boron powder, so that the combustion efficiency of the boron particles is low, the energy performance cannot be fully exerted, and the application of the boron powder in the field of explosives and powders is limited.
Previous experimental and theoretical studies have shown that the combustion process of boron particles in an oxygen atmosphere consists of two successive stages. The first stage is an ignition stage, also called ignition delay stage of combustion, in which the boron oxide shell melts to form a liquid and is evaporated when the boron particles are heated, and the reaction rate is slow because the oxidation layer of the liquid phase prevents the oxidant from contacting with the boron in the inner layer; the second stage is a combustion stage, and because the surface of the boron particles does not have a boron oxide shell, the inner layer boron and the oxidant generate violent oxidation reaction to release a large amount of heat energy. Therefore, improving the ignition and combustion performance of boron particles and improving the combustion efficiency of boron powder becomes the fundamental starting point for solving the application of boron powder at present. Researchers have used a variety of methods to improve the ignition and combustion properties of boron, including coatings of different materials, compounding and mixing with other materials, or controlling the oxidizing environment/material, gases or water vapor during the combustion of boron powders.
Studies have shown that compounding boron particles with certain specific metal oxides can improve the ignition and combustion performance of boron particles. The reported metal oxide coated on the surface of boron powder is Fe 2 O 3 、CuO、Bi 2 O 3 And so on.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a high-energy-density boron fuel loaded with vanadium oxide and an immersion method for preparing the same, and solve the technical problem that the ignition and combustion performances of the boron fuel need to be further improved on the premise that the energy density of boron powder is not influenced in the boron fuel in the prior art.
In order to solve the technical problems, the invention adopts the following technical scheme:
a dipping method for preparing boron fuel of load vanadium oxide is provided, which adopts dipping method to load vanadium oxide on the surface of boron powder to form boron fuel of load vanadium oxide;
the dipping method is characterized in that a solution of pentavalent vanadium salt or tetravalent vanadium salt is used as a dipping solution, boron powder particles are completely soaked, and drying and calcining are carried out to prepare the boron fuel loaded with vanadium oxide;
the content of the vanadium oxide in the vanadium oxide-loaded boron fuel is 0.1-10 wt.%.
The invention also has the following technical characteristics:
preferably, the content of the vanadium oxide in the vanadium oxide-loaded boron fuel is 1wt.% to 10wt.%.
The vanadium oxide is V 2 O 2 、V 2 O 3 、VO 2 、V 2 O 4 And V 2 O 5 One or more of (a).
The dipping solution is NH 4 VO 3 An aqueous solution.
Specifically, the method specifically comprises the following steps:
adding boron powder into a reaction container, and testing the saturated water absorption capacity of the boron powder by using water to obtain the volume of impregnation liquid required by the boron powder;
weighing boron powder, pouring the boron powder into a reaction container, and adding magnetons;
thirdly, using a liquid transfer gun to transfer the prepared soaking liquid with the concentration of 0.001-1 mol/L, and adding deionized water to dilute the soaking liquid to the volume of the soaking liquid required by the boron powder;
step four, dropwise adding the impregnation liquid diluted in the step three into the boron powder in the step two to completely soak the boron powder, and ultrasonically stirring;
and step five, placing the boron fuel in an oven to be dried and calcined at the temperature of 60-80 ℃ to prepare the boron fuel loaded with the vanadium oxide.
The invention also protects the boron fuel loaded with the vanadium oxide, and the vanadium oxide is loaded on the surface of the boron powder to form the boron fuel loaded with the vanadium oxide; the content of vanadium oxide in the boron fuel loaded with vanadium oxide is 0.1-10 wt.%.
Preferably, the content of the vanadium oxide in the vanadium oxide-loaded boron fuel is 1wt.% to 10wt.%.
Further preferably, the content of the vanadium oxide in the vanadium oxide-loaded boron fuel is 3.5wt.% to 7wt.%.
Preferably, the vanadium oxide is V 2 O 2 、V 2 O 3 、VO 2 、V 2 O 4 And V 2 O 5 One or more of (a).
Preferably, the boron fuel carrying the vanadium oxide is prepared by adopting the method for preparing the boron fuel carrying the vanadium oxide by the dipping method.
Compared with the prior art, the invention has the following technical effects:
compared with the traditional physical blending method, the preparation method disclosed by the invention can realize accurate, controllable, uniform and effective distribution of the composition, structure and content of the VOx catalyst on the surface of the boron powder, can effectively improve the utilization efficiency of the catalyst, and has a good application prospect.
(II) the boron fuel loaded with vanadium oxide prepared by the invention has the advantages of good ignition performance and low initial oxidation temperature, and compared with pure boron powder, the boron fuel loaded with catalyst VO prepared by the invention x The laser ignition delay time of the boron fuel can be shortened by more than 12ms, and the oxidation exothermic peak temperature is advanced by 154-171 ℃.
Drawings
FIG. 1 shows a 7wt.% -VO prepared by dipping method x SEM and Mapping (B, O, V element distribution) pictures of/B fuel samples.
FIG. 2 shows a 7wt.% -VO prepared by dipping method x XPS data for fuel samples: (A) B1 s; (B) V2 p; (C) O1 s.
FIG. 3 shows boron particles and supported vanadium oxides prepared by impregnationDSC data plots of boron fuel of (a); wherein Blank B is boron particles; IM-1 is 1wt.% -VO x B; IM-2 is 3.5wt.% -VO x B; IM-3 is 7wt.% -VO x B; IM-4 is 10wt.% -VO x /B。
FIG. 4 is a graph of TG data for boron particles and vanadium oxide loaded boron fuel made by the impregnation process; wherein Blank B is boron particles; IM-1 is 1wt.% -VO x B; IM-2 is 3.5wt.% -VO x B; IM-3 is 7wt.% -VO x B; IM-4 is 10wt.% -VO x /B。
FIG. 5 is a graph of ignition delay times for boron particles and vanadium oxide loaded boron fuels prepared using an impregnation process; wherein Blank B is boron particles; IM-1 is 1wt.% -VO x B; IM-2 is 3.5wt.% -VO x B, performing the reaction; IM-3 is 7wt.% -VO x B; IM-4 is 10wt.% -VO x /B。
The present invention will be explained in further detail with reference to examples.
Detailed Description
It is to be understood that all materials and devices known in the art may be used in the present invention without specific recitation.
The vanadium oxide as a transition metal oxide has excellent catalytic performance, and has the advantages of safety, environmental friendliness, low production cost and the like. Therefore, vanadium oxide as an active catalyst is loaded on the surface of the boron powder, so that the ignition and combustion performances of the boron powder are hopefully improved. Therefore, the boron fuel loaded with the vanadium oxide with excellent combustion performance is obtained by compounding the boron particles with an impregnation method, and the application of the boron-based fuel in the field of explosives and powders is effectively promoted.
In the invention:
the boron powder is amorphous boron powder and/or crystal boron powder, and the particle size distribution of the boron powder is micron-scale to nanometer-scale.
VO x the/B refers to boron fuel loaded with vanadium oxide.
The following embodiments of the present invention are provided, and it should be noted that the present invention is not limited to the following embodiments, and all equivalent changes based on the technical solutions of the present invention are within the protection scope of the present invention.
Example 1:
the embodiment provides a dipping method for preparing boron fuel loaded with vanadium oxide, which comprises the steps of loading vanadium oxide on the surface of boron powder by using a dipping method to form boron fuel loaded with vanadium oxide;
the impregnation method is by NH 4 VO 3 The water solution is used as an impregnation solution, boron powder particles are completely infiltrated, and the boron fuel loaded with vanadium oxide is prepared by drying and calcining;
the vanadium oxide is V 2 O 2 、V 2 O 3 、VO 2 、V 2 O 4 And V 2 O 5 One or more of (a).
The equation for the reaction of the impregnation method is:
Figure BDA0003621070390000051
specifically, the method specifically comprises the following steps:
adding boron powder into a reaction container, and testing the saturated water absorption capacity of the boron powder by using water to obtain the volume of impregnation liquid required by the boron powder;
weighing 1g of boron powder, pouring the boron powder into a reaction container, and adding magnetons;
thirdly, using a liquid transfer gun to transfer the prepared NH with the concentration of 0.1mol/L 4 VO 3 Adding deionized water into the aqueous solution to dilute until the boron powder is required to be soaked in NH 4 VO 3 The volume of the aqueous solution;
step four, diluting NH in the step three 4 VO 3 Dropwise adding the aqueous solution into the boron powder obtained in the second step to completely soak the boron powder, performing ultrasonic treatment for 10min, and continuously performing magnetic stirring for 6h, wherein the temperature of a magnetic stirrer is set to 65 ℃;
and step five, placing the boron fuel in an oven to be dried and calcined at the temperature of 80 ℃ to obtain the vanadium oxide-loaded boron fuel.
The contents of vanadium oxide in the vanadium oxide-supported boron fuel prepared in this example were 1wt.%, 3.5wt.%, 7wt.%, and 10wt.%, respectively.
FIG. 1 shows a 7wt.% VO prepared by the dipping method x SEM and Mapping (B, O, V element distribution) pictures of/B fuel samples. The distribution range of V and O elements completely conforms to that of B element, which shows that the deposited VO x Highly dispersed on the surface of the boron fuel.
FIG. 2 shows a 7wt.% VO prepared by the dipping method x XPS data for the/B fuel samples: (A) B1 s; (B) V2 p; (C) O1 s. The binding energy of B1s spectrogram can determine that the surface of the boron powder has B besides zero-valent boron 2 O 3 The existence of the species, the corresponding binding energy of the peak in the V2 p spectrum can be determined as V 5+ And determining that the species deposited on the surface of the boron powder is V by combining an O1s spectrogram 2 O 5 Comparison with pure boron powder, surface B 2 O 3 Presence of species indicates loaded VO x And B possibly interacts to transfer electrons.
Example 2:
this example presents a TG-DSC test of boron fuel loaded with vanadium oxide, the method of the TG-DSC test being: weighing a proper amount of boron fuel loaded with vanadium oxide, placing the boron fuel in a sample table of a TG-DSC instrument, setting the temperature rise rate of the instrument to be 10 ℃/min, setting the test temperature range to be 50-1000 ℃, and setting the test atmosphere to be air atmosphere, thus obtaining the TG and DSC curves of the boron fuel loaded with vanadium oxide.
Specifically, a proper amount of boron fuel loaded with vanadium oxide is weighed and placed in a sample stage of a TG-DSC instrument, the temperature rise rate of the instrument is set to be 10 ℃/min, the test temperature range is 50-1000 ℃, and the test atmosphere is air atmosphere, so that TG and DSC curves of the boron fuel loaded with vanadium oxide can be obtained.
Table 1 shows TG-DSC data for boron fuel loaded with vanadium oxide according to the invention.
TABLE 1 Combustion Performance of boron fuels loaded with vanadium oxides
Sample(s) T p (℃) ΔT(℃)
Pure B 677 -
IM-1wt.％-VO x /B 523 154
IM-3.5wt.％-VO x /B 519 158
IM-7wt.％-VO x /B 512 165
IM-10wt.％-VO x /B 510 167
FIG. 3 is a graph of DSC data for boron particles and vanadium oxide loaded boron fuel made using an impregnation process; wherein Blank B is boron particles; IM-1 is 1wt.% -VO x B; IM-2 is 3.5wt.% -VO x B, performing the reaction; IM-3 is 7wt.% -VO x B; IM-4 is 10wt.% -VO x and/B. The exothermic peak of the boron particles corresponds to a temperature of 677 ℃ compared to 1wt.% to V of the boron particles 2 O 5 The exothermic peak of/B corresponds to a temperature advance of 523 ℃,3.5wt.% -V 2 O 5 The exothermic peak of/B corresponds to a temperature advance of 519 ℃,7wt.% -V 2 O 5 The exothermic peak of the/B is advanced to 512 ℃,10wt.% -V 2 O 5 The exothermic peak of/B was advanced to 510 ℃. The above results also show that the boron fuel supporting vanadium oxide has excellent combustion performance and that the degree of the advancement of the exothermic peak of the boron fuel supporting vanadium oxide is VO x The content was slightly increased by increasing the content, and a small amount of VO was also shown x The combustion performance of the boron-based material can be obviously improved by compounding with boron particles.
FIG. 4 is a graph of TG data for boron particles and vanadium oxide loaded boron fuel made by the impregnation process; wherein Blank B is boron particles; IM-1 is 1wt.% -VO x B; IM-2 is 3.5wt.% -VO x B; IM-3 is 7wt.% -VO x B; IM-4 is 10wt.% -VO x and/B. The initial weight gain temperature of the vanadium oxide loaded boron fuel was significantly advanced compared to the boron particles, this TG result is consistent with the DSC result in fig. 3.
Example 3:
in this example, the ignition delay time test of boron fuel loaded with vanadium oxide is given, and the method for the ignition delay time test is as follows: weighing a proper amount of boron fuel loaded with vanadium oxide, placing the boron fuel in a sample stage of a laser ignition instrument, and setting the instrument parameters as frequency Hz:1000; duty cycle (1-40%): 3; pulse number: 1000, parts by weight; emitting light by a pulse train; power: 40W; pulse energy: 40mJ; pulse width: 30 mus. Thus, ignition delay time data of the boron fuel loaded with the vanadium oxide can be obtained.
Specifically, a proper amount of boron fuel loaded with vanadium oxide is weighed in a sample stage of a laser ignition instrument, and the instrument parameters are set as the following frequency Hz:1000, parts by weight; duty cycle (1-40%): 3; pulse number: 1000, parts by weight; emitting light by a pulse train; power: 40W; pulse energy: 40mJ; pulse width: 30 mus. As shown in fig. 3, the ignition delay time of the boron fuel supporting vanadium oxide prepared by the present invention is significantly shorter than that of boron particles.
FIG. 5 is a graph of ignition delay times for boron particles and vanadium oxide loaded boron fuels prepared using an impregnation process; wherein Blank B is boron particles; i isM-1 is 1wt.% -VO x B; IM-2 is 3.5wt.% -VO x B, performing the reaction; IM-3 is 7wt.% -VO x B; IM-4 is 10wt.% -VO x and/B. Wherein the ignition delay time of the boron particles is 52ms,1wt.% -VO x The ignition delay time of/B was shortened to 43.0ms,3.5wt.% -VO x The ignition delay time of the/B is shortened to 41.8ms,7wt.% -VO x The ignition delay time of/B was shortened to 39.0ms,10wt.% -VO x The ignition delay time of/B is shortened to 38.7ms. Compared with boron particles, the boron particles are mixed with a small amount of VO x The ignition delay time thereof can be significantly shortened.
Compared with the prior art, the boron fuel loaded with the vanadium oxide prepared by the invention has the advantages of good repeatability, environment friendliness, high composite combustion performance and the like. The preparation process of the composite material is simple and convenient. The experimental method adopts a dipping method, the synthesis conditions are mild, and the experimental medicines are common medicines in a laboratory. The cost for preparing the sample is low. The compound of the invention has the advantages of easy preparation, good repeatability and low price, greatly reduces the preparation cost of the boron powder-based fuel, and has good application prospect.

Claims (5)

1. A dipping method preparation method of boron fuel of load vanadium oxide is characterized in that the method adopts the dipping method to load vanadium oxide on the surface of boron powder to form boron fuel of load vanadium oxide;
the dipping method is NH 4 VO 3 The water solution is used as an impregnation solution, boron powder particles are completely infiltrated, and the boron fuel loaded with vanadium oxide is prepared by drying and calcining;
the content of the vanadium oxide in the boron fuel loaded with the vanadium oxide is 0.1-10 wt.%;
the method specifically comprises the following steps:
adding boron powder into a reaction container, and testing the saturated water absorption capacity of the boron powder by using water to obtain the volume of impregnation liquid required by the boron powder;
weighing boron powder, pouring the boron powder into a reaction container, and adding magnetons;
thirdly, using a liquid-transferring gun to transfer the prepared steeping liquor with the concentration of 0.001-1 mol/L, and adding deionized water to dilute the steeping liquor to the volume of the steeping liquor needed by the boron powder;
step four, dropwise adding the dipping solution diluted in the step three into the boron powder in the step two to completely soak the boron powder, and ultrasonically stirring;
and step five, placing the boron fuel in an oven to be dried and calcined at the temperature of 60-80 ℃ to prepare the boron fuel loaded with the vanadium oxide.
2. The method for preparing the vanadium oxide-supported boron fuel by the impregnation method according to claim 1, wherein the content of the vanadium oxide in the vanadium oxide-supported boron fuel is 1wt.% to 10wt.%.
3. The method of claim 1, wherein the vanadium oxide is V 2 O 2 、V 2 O 3 、VO 2 、V 2 O 4 And V 2 O 5 One or more of (a).
4. A vanadium oxide supported boron fuel, characterized in that the vanadium oxide supported boron fuel is prepared by the method for preparing the vanadium oxide supported boron fuel according to any one of claims 1 to 3 by the immersion method.
5. The vanadium oxide-supported boron fuel according to claim 4, wherein the content of the vanadium oxide in the vanadium oxide-supported boron fuel is 3.5wt.% to 7wt.%.
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