CN117964438A - Low-cost high-heat-value boron-containing aluminum-based composite fuel and preparation method thereof - Google Patents
Low-cost high-heat-value boron-containing aluminum-based composite fuel and preparation method thereof Download PDFInfo
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- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 title claims abstract description 70
- 239000002131 composite material Substances 0.000 title claims abstract description 58
- 229910052796 boron Inorganic materials 0.000 title claims abstract description 57
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 35
- 239000000446 fuel Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000000843 powder Substances 0.000 claims abstract description 95
- 238000000498 ball milling Methods 0.000 claims abstract description 23
- 239000002245 particle Substances 0.000 claims abstract description 16
- 238000001132 ultrasonic dispersion Methods 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims description 18
- 238000001291 vacuum drying Methods 0.000 claims description 14
- 238000013329 compounding Methods 0.000 claims description 13
- 239000007788 liquid Substances 0.000 claims description 13
- 239000003960 organic solvent Substances 0.000 claims description 13
- 238000003756 stirring Methods 0.000 claims description 13
- 238000001816 cooling Methods 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 11
- 238000000926 separation method Methods 0.000 claims description 11
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 8
- 238000007873 sieving Methods 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 7
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 239000006185 dispersion Substances 0.000 claims description 6
- 238000001704 evaporation Methods 0.000 claims description 6
- 238000010907 mechanical stirring Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 238000004886 process control Methods 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- 230000008020 evaporation Effects 0.000 claims description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- 239000000919 ceramic Substances 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 3
- 239000007791 liquid phase Substances 0.000 claims description 3
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 2
- 238000009835 boiling Methods 0.000 claims description 2
- 238000005119 centrifugation Methods 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 239000011261 inert gas Substances 0.000 claims description 2
- 239000011812 mixed powder Substances 0.000 claims description 2
- 239000003208 petroleum Substances 0.000 claims description 2
- 238000003828 vacuum filtration Methods 0.000 claims description 2
- 239000002994 raw material Substances 0.000 abstract description 11
- 238000005516 engineering process Methods 0.000 abstract description 3
- 238000002485 combustion reaction Methods 0.000 description 15
- 229910052751 metal Inorganic materials 0.000 description 8
- 239000002184 metal Substances 0.000 description 8
- 239000002360 explosive Substances 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 6
- 238000004880 explosion Methods 0.000 description 6
- 230000005855 radiation Effects 0.000 description 5
- 239000011777 magnesium Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 239000003380 propellant Substances 0.000 description 4
- 230000001105 regulatory effect Effects 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000009472 formulation Methods 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 229910052500 inorganic mineral Inorganic materials 0.000 description 3
- 229910052749 magnesium Inorganic materials 0.000 description 3
- 239000011707 mineral Substances 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 239000004449 solid propellant Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 229910052582 BN Inorganic materials 0.000 description 1
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 229910000861 Mg alloy Inorganic materials 0.000 description 1
- 229910003023 Mg-Al Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 description 1
- 238000005422 blasting Methods 0.000 description 1
- 229910021538 borax Inorganic materials 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 229910052810 boron oxide Inorganic materials 0.000 description 1
- 239000012267 brine Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000007728 cost analysis Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000003721 gunpowder Substances 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000002779 inactivation Effects 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000004323 potassium nitrate Substances 0.000 description 1
- 235000010333 potassium nitrate Nutrition 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000001698 pyrogenic effect Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- VSZWPYCFIRKVQL-UHFFFAOYSA-N selanylidenegallium;selenium Chemical compound [Se].[Se]=[Ga].[Se]=[Ga] VSZWPYCFIRKVQL-UHFFFAOYSA-N 0.000 description 1
- 239000004328 sodium tetraborate Substances 0.000 description 1
- 235000010339 sodium tetraborate Nutrition 0.000 description 1
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000000935 solvent evaporation Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
Abstract
The invention discloses a low-cost high-heat-value boron-containing aluminum-based composite fuel and a preparation method thereof. The low-cost high-calorific-value boron-containing aluminum-based composite fuel comprises, by mass, 75% -90% of Al powder with the particle size of 1-50 microns, 0% -10% of B powder with D 50 = 1-3 microns, and 10% -20% of superfine B 4 C powder with D 50 less than or equal to 5 microns. According to the invention, the boron-containing aluminum-based composite fuel with specific component proportions is prepared by adopting an ultrasonic dispersion composite or mechanical ball milling composite technology in a mode of partially or completely replacing amorphous boron powder with superfine B 4 C powder, so that the high heat value is obtained, and meanwhile, the effective control of the raw material cost is realized.
Description
Technical Field
The invention belongs to the field of aluminum-based metal fuels, and relates to a low-cost high-heat-value boron-containing aluminum-based composite fuel and a preparation method thereof.
Background
Compared with the traditional hydrocarbon fuel, the metal fuel represented by the micron aluminum (Al) powder has the advantages of high combustion heat value, rich raw materials and the like, and has been widely used as a high-energy additive in energetic systems such as solid propellant, mixed explosive, gunpowder and the like, so as to realize the effects of improving the energy density of the formula, improving the ignition and combustion behavior, increasing the explosion heat and the damage efficiency and the like. In recent years, boron has been widely studied and focused on its high mass and volumetric heating value (58.3 kJ/g,136.4kJ/cm 3), and is considered to be a metal fuel with great potential for use (boron, although non-metallic, is also generally classified into metal fuels in the industry according to its range of application). In the field of solid propellant, meteor air-to-air missiles developed in European six-country cooperation obtain superior performance far exceeding active missile types due to the successful adoption of a boron-containing fuel-rich propellant solid rocket ramjet engine. The successful development of meteor missiles and the demonstration effects brought by the successful development of meteor missiles raise the development of boron-containing fuel-rich propellants in various countries. In the field of mixed explosives and pyrotechnic compositions, although practical application cases are not yet reported, a great deal of academic researches show that adding a certain amount of boron powder can improve the explosion heat and underwater/aerial explosion energy of the mixed explosives and improve the ignition capability and radiation performance of the pyrotechnic compositions. For example, the influence of boron content on the underwater explosion energy of aluminum-containing explosive is studied by Nanjing university Chen Yuan and the like (Chen Yuan, chen Xiang, jiang Wei and the like), and the influence of boron content on the underwater explosion energy of aluminum-containing explosive is studied by using blasting equipment, 2015, 44:1-4), and the research result shows that when the boron content is 10%, the total underwater explosion energy and the bubble energy are respectively improved by 5% and 7% compared with the corresponding mixed explosive without the boron powder, and 5942kJ/kg and 4999kJ/kg are reached; the influence of boron powder content on the combustion and infrared radiation characteristics of KNO 3/Mg-Al infrared decoy and the like (Du, guan Hua, li Jie and the like) of Nanjing university Du, energy-containing material, 2015, 23:368-371) are researched, and research results show that the influence of boron powder content on the radiation characteristics of potassium nitrate/aluminum magnesium alloy-based infrared decoy, the combustion temperature, the radiation brightness and the radiation intensity are continuously increased along with the increase of the boron powder content from 0% to 4%, and the three reach 1046.19 ℃ and 1681.59W/m 2 -sr and 2.64W/sr respectively when the boron powder content is 4%, and are respectively increased by 43.76%, 68.89% and 140% compared with a formulation without the boron.
Although boron powder as a high-energy metal fuel shows application potential as an aluminum powder substitute in the field of explosives and powders, the technical bottlenecks of difficult ignition, low combustion efficiency, poor process compatibility and the like are overcome, and the small industrial scale and high cost also cause great limitation in engineering popularization and application. In the natural world, no elemental boron exists in the form of borate in minerals or brine, and the boron-containing minerals are subjected to a series of pyrogenic, wet separation and purification or reaction processes to obtain products such as borax (Na 2B4O7·10H2 O), boric acid (H 3BO3), boron oxide (B 2O3), boron carbide (B 4 C), elemental boron (crystal boron and amorphous boron), boron nitride (H-BN/C-BN), borohydride and the like, as shown in figure 3.
Currently, the mass production of the elemental boron powder mainly adopts a magnesia-thermal reduction method (3mg+b 2O3 =2b+3mgo), and the reduction products of the boron oxide and the magnesium powder undergo acid leaching, rinsing, filtering to remove MgO, B 2O3 and other impurities, and finally are dried to obtain amorphous boron powder with the boron content of about 85%, and the amorphous boron powder is further refined and purified to obtain the high-purity elemental boron powder. Because of the multiple steps of treatment process and the large amount of waste liquid generated in the process, the price of the currently marketed amorphous boron powder is high, reaching 1700-2800 yuan/kg, which is far higher than that of the conventional micron aluminum powder (30-55 yuan/kg).
Boron carbide (B 4 C) is one of the major products of the boron industry and is commonly used as a wear resistant material, ballistic armor material and nuclear shielding material due to its extremely high hardness, strength and good neutron shielding properties. The mass combustion heat value of B 4 C is 52.0kJ/g, which is slightly lower than that of elemental boron (58.3 kJ/g), and meanwhile, the volume heat value of B 4 C is equivalent to that of boron (131.0 kJ/cm 3 vs.136.4kJ/cm3) due to the higher density (2.52 g/cm 3). Chinese patent application 201810930112.5 discloses a fuel-rich propellant formulation which mentions a fuel for fuel-rich propellant formulation consisting of one or a combination of boron (B), magnesium (Mg), aluminum (Al), titanium (Ti), zirconium (Zr), boron carbide (B 4 C), boron-based metal complexes (B-Mg, B-Al, B-Ti), which is a boron-based composite fuel in which B and B 4 C (the ratio of both is not illustrated) with particle sizes of 1 to 3 μm are main fuels and industrial grade metal (Mg, al, ti, zr) with particle sizes of 1 to 30 μm and boron-based metal complexes are auxiliary fuels, and the raw material cost is still high.
Disclosure of Invention
The invention aims to provide a low-cost high-heat-value boron-containing aluminum-based composite fuel and a preparation method thereof, wherein the boron-containing aluminum-based composite fuel with specific component proportions is prepared by adopting an ultrasonic dispersion compounding or mechanical ball milling compounding technology in a mode of partially or completely replacing amorphous boron powder with superfine B 4 C powder, so that the high-heat-value (more than 32.0 kJ/g) is obtained, and meanwhile, the effective control of the raw material cost (less than 300 yuan/kg) is realized.
The technical scheme for realizing the purpose of the invention is as follows:
The low-cost high-heat-value boron-containing aluminum-based composite fuel consists of, by mass, 75% -90% of Al powder with a particle size of 1-50 mu m, 0% -10% of B powder with D 50 =1-3 mu m and 10% -20% of superfine B 4 C powder with D 50 less than or equal to 5 mu m.
Preferably, the Al powder is spherical or flaky Al powder.
Preferably, the powder consists of 85 to 90 percent of Al powder with the grain diameter of 1 to 50 mu m, 0 to 5 percent of B powder with the D 50 =1 to 3 mu m and 10 percent of superfine B 4 C powder with the D 50 less than or equal to 5 mu m according to the mass percentage.
The invention provides a preparation method of a low-cost high-heat-value boron-containing aluminum-based composite fuel, which adopts an ultrasonic liquid phase dispersion compounding method and comprises the following steps:
According to the ratio of the powder B to the powder B 4 C of 1: (5-25) adding the mixture into an organic solvent, carrying out ultrasonic dispersion while mechanical stirring is assisted, adding Al powder after uniform mixing, continuing ultrasonic dispersion while mechanical stirring is assisted, carrying out solid-liquid separation after complete uniform mixing, carrying out vacuum drying, cooling, and sieving with a 30-100-mesh sieve to obtain the boron-containing aluminum-based composite fuel.
Preferably, the organic solvent is absolute ethanol, isopropanol, ethyl acetate or petroleum ether.
Preferably, the ultrasonic frequency before adding the aluminum powder is 20-40 kHz, the stirring speed is 150-500 rpm, and the treatment time is 15-60 min; the ultrasonic frequency after adding the aluminum powder is 20-40 kHz, the stirring speed is 200-600 rpm, and the treatment time is 30-90 min.
Preferably, the solid-liquid separation is carried out by vacuum filtration, centrifugation or evaporation of the solvent. When the solvent evaporation method is adopted, the evaporation temperature is set to be 0-10 ℃ above the boiling point of the organic solvent, and mechanical stirring is used for evaporation.
Preferably, the vacuum drying temperature is 80-110 ℃ and the drying time is 1-3 h.
The invention provides another preparation method of low-cost high-calorific-value boron-containing aluminum-based composite fuel, which adopts a mechanical ball milling composite method, and takes an organic solvent as a ball milling process control agent, so that on one hand, the ball milling environment temperature and the activity of powder particles can be reduced through the circulation of solvent volatilization-cooling, and the hard agglomeration phenomena such as cold welding, agglomeration and the like among the particles can be prevented; on the other hand, a sealing environment is formed among the powder bodies to avoid oxidation and inactivation in the ball milling process of the powder particles, and the method comprises the following steps:
Mixing Al powder, B powder and B 4 C powder according to a certain proportion, using ceramic balls with phi=1-6 mm as ball milling medium, using organic solvent as process control agent, adopting planetary ball mill to make ball milling compounding on Al/B/B 4 C mixed powder under the protection of inert gas, after ball milling, vacuum-filtering to remove organic solvent, vacuum-drying, cooling, sieving with 30-100 meshes sieve so as to obtain the boron-containing aluminium-base composite fuel.
Preferably, the ceramic balls are Al 2O3、ZrO2 or TiC.
Preferably, the organic solvent is absolute ethanol, n-hexane or cyclohexane.
Preferably, the ball-material ratio is 3:1-9:1, the solid-liquid ratio is 1:1-1:3, the rotating speed is 100-600 rpm, and the ball milling time is 1-3 h.
Preferably, the vacuum drying temperature is 80-110 ℃ and the drying time is 1-3 h.
Compared with the prior art, the invention has the following advantages:
(1) According to the invention, the superfine B 4 C powder with the median diameter D 50 less than or equal to 5 mu m is used for partially or completely replacing amorphous boron powder, and the proportion of the aluminum powder, the superfine B 4 C powder and the boron powder is regulated and controlled, so that the components are simple, the main raw materials are cheap and easy to obtain, and the boron-containing aluminum-based composite powder with the actual combustion heat value more than 32.0kJ/g and the raw material cost less than 300 yuan/kg is obtained.
(2) The invention adopts ultrasonic liquid phase dispersion or mechanical ball milling technology to realize uniform compounding among Al powder, B 4 C powder and B powder in specific proportion, has stable and reliable preparation process and low equipment investment, and can realize batch mass production.
Drawings
FIG. 1 is a particle size distribution and SEM image of ultrafine B 4 C powder.
FIG. 2 is an SEM image of 85Al/10B 4 C/5B composite powder prepared in example 1.
Fig. 3 is a route and cost analysis graph of a prior art boron-containing mineral for producing a boron-containing product.
Detailed Description
The invention will be described in further detail with reference to the drawings and the specific examples.
The starting materials or reagents employed in the examples below were either obtained commercially or prepared by reference to existing methods.
Example 1
255.0G of spherical micron Al powder (FLQT) and 30.0g of superfine B 4 C powder (D 50 =2.7+/-0.2 mu m) and 15.0g of high-purity amorphous boron powder (95B and D 50 =1.3+/-0.1 mu m) are respectively weighed, the B 4 C powder and the B powder are sequentially added into 1.0L of absolute ethyl alcohol to carry out ultrasonic dispersion at the frequency of 40kHz, and a toothed stirring paddle is synchronously adopted to mechanically stir the solvent at the rotation speed of 200rpm during the ultrasonic dispersion; slowly adding aluminum powder after 30min, and then regulating the rotating speed of a stirring paddle to 300rpm for carrying out dispersion and compounding treatment for 60 min; after the composite treatment is finished, solid-liquid separation is carried out by adopting a vacuum suction filter, the obtained 85Al/10B 4 C/5B composite cake is placed in a vacuum drying oven to be dried for 2.0h at 80 ℃, and after full cooling, the 85Al/10B 4 C/5B boron-containing aluminum-based composite powder is obtained through sieving and dispersing by a 60-mesh screen.
FIG. 1 is a particle size distribution and SEM image of ultrafine B 4 C powder. Fig. 2 is an SEM image of the 85Al/10B 4 C/5B composite powder prepared in example 1, and it can be seen that the Al, B and B 4 C particles in the composite powder achieve a more uniform composite, the three particles do not change in morphology and particle size, and remain in an original state, and only a small amount of scratches caused by collision of hard B and B 4 C exist on the surface of the spherical Al particles. As shown in Table 1, the combustion heat value of the composite powder under the pure oxygen environment of 3.0MPa is (32.91 +/-0.34) kJ/g, which is 8.6% higher than the actual combustion heat value (30.3+/-0.2) kJ/g of FLQT Al powder under the same conditions, and the raw material price of the 85Al/10B 4 C/5B composite powder is 175 yuan/kg according to the market average price of Al powder (50 yuan/kg), B powder (2500 yuan/kg) and B 4 C powder (75 yuan/kg).
Table 1 comparison of the Heat value of Mass Combustion of the composite powders in the different examples
The.
Example 2
255.0G of spherical micron Al powder (FLQT 3), 30.0g of superfine B 4 C powder (D 50 =2.7+/-0.2 mu m) and 15.0g of high-purity amorphous boron powder (95B, D 50 =1.3+/-0.1 mu m) are respectively weighed, 1.5kg of phi 3mm zirconia balls are used as ball milling media, 1.0L of normal hexane is used as a process control agent, ball milling compounding is carried out under the protection of high-purity nitrogen at the rotating speed of 200rpm for 1.5h, then a vacuum suction filter is adopted for solid-liquid separation, the materials containing the grinding balls are placed in a vacuum drying box at the temperature of 100 ℃ for drying for 2.0h, and after cooling, the materials are sieved through a 60-mesh screen, so as to obtain the 85Al/10B 4 C/5B boron-containing aluminum-based composite powder.
As shown in Table 1, the combustion heat value of the composite powder in a pure oxygen environment of 3.0MPa is (33.42 +/-0.17) kJ/g, which is improved by 10.3% compared with FLQT Al powder, and is slightly higher than that of the composite powder with the same components prepared by adopting an ultrasonic composite method, which is probably because the uniform composite among Al, B 4 C and B particles is better realized by mechanical ball milling composite.
Example 3
Respectively weighing 150.0g of spherical micron Al powder (FLQT 4), 30.0g of superfine B 4 C powder (D 50 =2.7+/-0.2 mu m) and 20.0g of high-purity amorphous boron powder (95B, D 50 =1.3+/-0.1 mu m), sequentially adding the B 4 C powder and the B powder into 600mL of absolute ethyl alcohol for ultrasonic dispersion at 40kHz, and mechanically stirring the solvent at 200rpm by adopting a toothed stirring paddle synchronously during the ultrasonic dispersion; slowly adding FLQT to the aluminum powder after 30min, and then regulating the rotating speed of a stirring paddle to 300rpm for carrying out dispersion and compounding treatment for 60 min; after the composite treatment is finished, a vacuum suction filter is adopted for solid-liquid separation, the obtained 75Al/15B 4 C/10B composite cake is placed in a vacuum drying oven for drying at 80 ℃ for 2.0h, and after full cooling, the 75Al/20B 4 C/10B boron-containing aluminum-based composite powder is obtained through sieving and dispersing by a 60-mesh screen.
As shown in Table 1, the combustion heat value of the composite powder in a pure oxygen environment of 3.0MPa is (33.12+/-0.27) kJ/g, which is 9.3 percent higher than FLQT Al powder. The raw material price of the 75Al/20B 4 C/10B composite powder is 299 yuan/kg.
Example 4
180.0G of spherical micron Al powder (FLQT < 4 >) and 20.0g of superfine B 4 C powder (D 50 =2.7+/-0.2 mu m) are respectively weighed, B 4 C powder is added into 600mL of absolute ethyl alcohol to carry out ultrasonic dispersion at the frequency of 40kHz, and during the ultrasonic dispersion, a toothed stirring paddle is synchronously adopted to mechanically stir the solvent at the rotating speed of 200 rpm; slowly adding FLQT to the aluminum powder after 30min, and then regulating the rotating speed of a stirring paddle to 300rpm for carrying out dispersion and compounding treatment for 60 min; after the composite treatment is finished, solid-liquid separation is carried out by adopting a vacuum suction filter, the obtained 90Al/10B 4 C composite cake is placed in a vacuum drying oven to be dried for 2.0h at 80 ℃, and the 90Al/10B 4 C boron-containing aluminum-based composite powder is obtained after full cooling and sieving and dispersing by a 60-mesh screen.
As shown in Table 1, the combustion heat value of the composite powder in a pure oxygen environment of 3.0MPa is (32.10+/-0.10) kJ/g, which is improved by 5.9 percent compared with FLQT Al powder. The raw material price of the 90Al/10B 4 C composite powder is 52.5 yuan/kg.
Example 5
Respectively weighing 240.0g of spherical micron Al powder (FLQT) and 60.0g of superfine B 4 C powder (D 50 =2.7+/-0.2 mu m), taking 1.5kg of phi 3mm zirconia balls as a ball milling medium, taking 1.0L of normal hexane as a process control agent, carrying out ball milling compounding for 1.5 hours at the rotating speed of 200rpm under the protection of high-purity nitrogen, then carrying out solid-liquid separation by adopting a vacuum suction filter, drying the materials containing the grinding balls in a vacuum drying oven at 100 ℃ for 2.0 hours, and sieving the materials through a 60-mesh screen after cooling to obtain the 80Al/20B 4 C boron-containing aluminum-based composite powder.
As shown in Table 1, the combustion heat value of the composite powder in a pure oxygen environment of 3.0MPa is (32.68+/-0.23) kJ/g, which is improved by 7.9 percent compared with FLQT Al powder. The raw material price of the 80Al/20B 4 C composite powder is 55 yuan/kg.
Comparative example 1
210.0G of spherical micron Al powder (FLQT 3), 60.0g of superfine B 4 C powder (D 50 =2.7+/-0.2 mu m) and 30.0g of high-purity amorphous boron powder (95B, D 50 =1.3+/-0.1 mu m) are respectively weighed, 1.5kg of phi 3mm zirconia balls are taken as ball milling media, 1.0L of normal hexane is taken as a process control agent, ball milling compounding is carried out under the protection of high-purity nitrogen at the rotating speed of 200rpm for 1.5h, then a vacuum suction filter is adopted for solid-liquid separation, the materials containing the grinding balls are placed in a vacuum drying box at 100 ℃ for drying for 2.0h, and after cooling, a 60-mesh screen is adopted to obtain 70Al/20B 4 C/10B boron-containing aluminum-based composite powder.
As shown in Table 1, the combustion heat value of the composite powder in a pure oxygen environment of 3.0MPa is (28.63+/-0.62) kJ/g, which is reduced by 5.5% compared with FLQT Al powder. In addition, the raw material price of the 70Al/20B 4 C/10B composite powder is 300 yuan/kg.
Claims (10)
1. The low-cost high-heat-value boron-containing aluminum-based composite fuel is characterized by comprising, by mass, 75% -90% of Al powder with a particle size of 1-50 mu m, 0% -10% of B powder with D 50 = 1-3 mu m, and 10% -20% of superfine B 4 C powder with D 50 less than or equal to 5 mu m.
2. The low-cost high-heating-value boron-containing aluminum-based composite fuel according to claim 1, wherein the Al powder is spherical or flake-shaped Al powder.
3. The low-cost high-calorific-value boron-containing aluminum-based composite fuel according to claim 1, which is characterized by comprising, by mass, 85% -90% of Al powder with a particle size of 1-50 μm, 0% -5% of B powder with D 50 = 1-3 μm and 10% of superfine B 4 C powder with D 50 less than or equal to 5 μm.
4. The method for preparing the low-cost high-heat-value boron-containing aluminum-based composite fuel according to any one of claims 1-3, which is characterized by adopting an ultrasonic liquid phase dispersion compounding method and comprising the following steps of:
According to the ratio of the powder B to the powder B 4 C of 1: (5-25) adding the mixture into an organic solvent, carrying out ultrasonic dispersion while mechanical stirring, adding Al powder after uniform mixing, continuing ultrasonic dispersion while mechanical stirring, carrying out solid-liquid separation after complete uniform mixing, carrying out vacuum drying, cooling, and sieving with a 30-100-mesh sieve to obtain the boron-containing aluminum-based composite fuel.
5. The method according to claim 4, wherein the organic solvent is absolute ethanol, isopropanol, ethyl acetate or petroleum ether; the ultrasonic frequency before adding the aluminum powder is 20-40 kHz, the stirring rotation speed is 150-500 rpm, and the treatment time is 15-60 min; the ultrasonic frequency after adding the aluminum powder is 20-40 kHz, the stirring speed is 200-600 rpm, and the treatment time is 30-90 min.
6. The method according to claim 4, wherein the solid-liquid separation is performed by vacuum filtration, centrifugation or evaporation of the solvent; the vacuum drying temperature is 80-110 ℃, and the drying time is 1-3 h.
7. The method of claim 6, wherein the evaporating temperature is set to 0-10 ℃ above the boiling point of the organic solvent and mechanical stirring is used for the evaporation.
8. The method for preparing the low-cost high-heat-value boron-containing aluminum-based composite fuel according to any one of claims 1-3, which is characterized by adopting a mechanical ball milling composite method and comprising the following steps of:
Mixing Al powder, B powder and B 4 C powder according to a certain proportion, taking ceramic balls with phi=1-6 mm as ball milling medium, taking organic solvent as process control agent, adopting a planetary ball mill to perform ball milling and compounding on the Al/B/B 4 C mixed powder under the protection of inert gas, after ball milling, vacuum filtering to remove the organic solvent, vacuum drying, cooling, and sieving with a 30-100 mesh sieve to obtain the boron-containing aluminum-based composite fuel.
9. The preparation method of claim 8, wherein the ceramic balls are Al 2O3、ZrO2 or TiC, the organic solvent is absolute ethyl alcohol, n-hexane or cyclohexane, the ball-to-material ratio is 3:1-9:1, the solid-to-liquid ratio is 1:1-1:3, the rotating speed is 100-600 rpm, and the ball milling time is 1-3 hours.
10. The preparation method according to claim 8, wherein the vacuum drying temperature is 80-110 ℃ and the drying time is 1-3 hours.
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