CN105537605B - A kind of Al/Fe2O3The preparation method of thermite - Google Patents
A kind of Al/Fe2O3The preparation method of thermite Download PDFInfo
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- CN105537605B CN105537605B CN201610019023.6A CN201610019023A CN105537605B CN 105537605 B CN105537605 B CN 105537605B CN 201610019023 A CN201610019023 A CN 201610019023A CN 105537605 B CN105537605 B CN 105537605B
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- thermite
- powder
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- submicron order
- drying solid
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- 239000003832 thermite Substances 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims abstract description 31
- 238000001035 drying Methods 0.000 claims abstract description 26
- 239000000843 powder Substances 0.000 claims abstract description 19
- 239000007787 solid Substances 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 13
- 239000002904 solvent Substances 0.000 claims abstract description 8
- 239000006185 dispersion Substances 0.000 claims abstract description 7
- 239000002243 precursor Substances 0.000 claims abstract description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 15
- 238000006243 chemical reaction Methods 0.000 claims description 15
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 229910052782 aluminium Inorganic materials 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 9
- 239000012065 filter cake Substances 0.000 claims description 7
- 206010013786 Dry skin Diseases 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 4
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 150000001335 aliphatic alkanes Chemical group 0.000 claims description 2
- 150000004945 aromatic hydrocarbons Chemical class 0.000 claims description 2
- 230000007547 defect Effects 0.000 abstract description 2
- 230000008569 process Effects 0.000 abstract description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 5
- 238000003980 solgel method Methods 0.000 description 5
- 239000004411 aluminium Substances 0.000 description 4
- 238000012546 transfer Methods 0.000 description 4
- 230000032683 aging Effects 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- 239000003638 chemical reducing agent Substances 0.000 description 2
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 2
- 239000007800 oxidant agent Substances 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 208000021760 high fever Diseases 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 230000037452 priming Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000001294 propane Substances 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
-
- B22F1/0003—
Abstract
The invention provides a kind of Al/Fe2O3The preparation method of thermite, this method is by Fe2O3Precursor be well mixed with submicron order Al powder in dispersion solvent, remove dispersion solvent, obtain drying solid.Obtained drying solid is put into crucible, cools after 300 DEG C~330 DEG C heating 5h~10h, obtains Al/Fe2O3Thermite.The Al/Fe of the present invention2O3The defects of thermite preparation method, the cycle is short, easy to operate, and obtained thermite calorific value is high, overcomes background technology long preparation period, and operating process is numerous and diverse.
Description
Technical field
The present invention relates to a kind of Al/Fe2O3A kind of preparation method of thermite, and in particular to submicron order aluminium powder thermite
Preparation method.
Background technology
With the development of material preparation technology, the research of nanometer thermite becomes focus.Nanometer thermite is nano aluminum
Powder and nano-metal-oxide carry out compound in Nano grade.Nanometer thermite has the characteristics of energy is close high, in metallurgical, electricity
Pond, ceramics, military field have a wide range of applications.The preparation method of nanometer thermite mainly has solid reaction process, response inhabitation
Polishing, sol-gel process, spray heating decomposition, self-assembly method, wherein sol-gel process are prepare nanometer thermite excellent
Frequency showing method, this method make the thermit reaction thermal discharge with higher contact area and Geng Gao between reactant.(the Al/ such as Wang Yi
Fe2O3The preparation of nano combined thermite and its response characteristic research《Priming system》Page 11~page 14 of 4th phase in 2008) using molten
Glue-gel method is prepared for Al/Fe2O3Nanometer aluminium powder is added to Fe (NO by nanometer thermite, this method3)3·9H2O ethanol solutions
In disperse, after temperature is constant, add 1,2- expoxy propane, and monitor reaction temperature and pH value change, make generation gel reaction, will
After obtained gel mixed system aging is placed 6 days, be dried in vacuo 5 days, then ground, washing, centrifugation, dry after obtain Al/
Fe2O3Nanometer thermite, its calorific value is 1648Jg-1.High female grade (is heat-treated to Al/Fe2O3The influence of nanometer thermite performance
《Explosive wastewater journal》Page 19~page 22 of 6th phase in 2012) with sol-gel process, and thermally treated obtain Al/Fe2O3Nanometer aluminothermy
Agent, its highest calorific value are 1209Jg-1.The defects of there is synthesis cycle length in sol-gel process, operating process is numerous and diverse.
The content of the invention
The technical problem to be solved in the present invention is for deficiency present in background technology, there is provided a kind of manufacturing cycle
Short, easy to operate, high heating value Al/Fe2O3Thermite preparation method.
In traditional thermite material, oxidant and reducing agent are physical mixed, and oxidant separates with reducing agent particle, different
Interface interaction between component hinders the diffusion of its reaction heat, causes the energyreleaserate and energy conversion effect of traditional thermite
Rate is relatively low.Nanometer thermite due between reactant contact area it is big, reduce the distance of mass transfer and heat transfer, have it is higher
Energy density, high fever can be produced during thermit reaction.In current techniques, it is molten to prepare the preferable method of nanometer thermite
Glue-gel method, but this method long preparation period, trivial operations.
The present invention is by Fe2O3Presoma and submicron order Al powder mixed processings after, pass through heating, in-situ preparation Fe2O3It is brilliant
Body, combined closely with Al, be advantageous to mass transfer, heat transfer, to improve energy conversion efficiency.The inventive method short preparation period, operation
It is easy.
The Al/Fe of the present invention2O3The preparation method of thermite, comprises the following steps：By Fe2O3Precursor, submicron order
Al powder and dispersion solvent are added in reaction vessel, and wherein Al and Fe mol ratio are 1:0.50~1.32, submicron order Al powder
Mass volume ratio with dispersion solvent is 1g:63ml~170ml, 20 DEG C~33 DEG C ultrasonic disperses, filtering, washed with absolute ethyl alcohol
Filter cake, drain, 20~25 DEG C of dryings, obtain drying solid, obtained drying solid is put into crucible, 300 DEG C~330 DEG C add
Hot 5h~10h, 20~25 DEG C are cooled to, obtains Al/Fe2O3Thermite；Used Fe2O3Precursor for can after heated
It is transformed into Fe2O3Material, particularly FeO (OH), Fe3O4；Al is particle diameter 200nm~300nm submicron order Al powder；Point
It is alkane, aromatic hydrocarbon to dissipate solvent.
Currently preferred Al/Fe2O3Thermite preparation method comprises the following steps：Take FeO (OH), particle diameter be 200nm~
300nm submicron order Al powder and toluene, is added in reaction vessel, and wherein Al and Fe mol ratio are 1:1.12 sub-micron
The mass volume ratio of level Al powder and toluene is 1g:167ml, 23~33 DEG C of ultrasonic 15min, filtering, filter cake is washed with absolute ethyl alcohol
Two times, drain, 20~25 DEG C of dryings, obtain drying solid；Obtained drying solid is put into crucible, 300 DEG C~330 DEG C add
Hot 8h, 20~25 DEG C are cooled to, obtains Al/Fe2O3Thermite.
Advantages of the present invention：Documents method prepares Al/Fe using sol-gel process2O3Thermite, gel mixture
It is that aging needs to place 6 days, is dried in vacuo 5 days；Occur gel reaction under detection temperature and pH value, then by aging, drying, grind
Mill, washing, centrifugation, drying steps, obtain Al/Fe2O3Thermite, Al/Fe2O3Thermite highest calorific value is 1648Jg-1.This
The most long operating procedure of invention is heating 5h~10h；Experimentation is mixing, filters, washs, drying, heating simple operations, is obtained
Al/Fe2O3Thermite highest calorific value is 1934.67Jg-1.Compared with background technology, the inventive method short preparation period, behaviour
Make easy, thermite calorific value height.
Brief description of the drawings
The thermite SEM of Fig. 1 embodiments 3 schemes
The thermite XRD of Fig. 2 embodiments 3
The thermite DSC of Fig. 3 embodiments 3 schemes
Embodiment
With reference to embodiment, the present invention is further described, but the present invention is not limited by the following example.
Analytical instrument：Field emission scanning electron microscope (U.S.'s FEI Quanta 600FEG types)；X-ray powder diffraction instrument (Holland
PANalytical company EMPYREAN types)；TG-DSC combined instruments (Mettler Toledo Inc. of Switzerland TGA/DSC2STARe System
Type)
Embodiment 1
Take the Fe that particle diameter is 20nm3O43.5g, particle diameter are 200nm~300nm submicron order Al powder 1g, normal octane 65ml,
It is added in reaction vessel, 21 DEG C~26 DEG C ultrasonic 15min, filters, wash filter cake two times with absolute ethyl alcohol, drain, 20~25
DEG C drying, obtains drying solid.
Obtained drying solid is put into crucible, 300 DEG C~320 DEG C heating 5h, 20~25 DEG C is cooled to, obtains Al/
Fe2O3Thermite.Under high-purity argon gas atmosphere, 10 DEG C of min of heating rate-1, 30 DEG C~1000 DEG C of temperature range, DSC test aluminium
Thermit powder calorific value is 1296.51Jg-1。
Embodiment 2
FeO (OH) 1.1g is taken, particle diameter is 200nm~300nm submicron order Al powder 0.5g, n-hexane 60ml, is added to
In reaction vessel, 20~29 DEG C of ultrasonic 15min, filtering, wash filter cake two times with absolute ethyl alcohol, drain, 20~25 DEG C of dryings, obtain
To drying solid.
Obtained drying solid is put into crucible, 320 DEG C~330 DEG C heating 5.5h, 20~25 DEG C is cooled to, obtains
Al/Fe2O3Thermite.Under high-purity argon gas atmosphere, 10 DEG C of min of heating rate-1, 30 DEG C~1000 DEG C of temperature range, DSC tests
Thermite calorific value is 1503.50Jg-1。
Embodiment 3
FeO (OH) 1.1g is taken, particle diameter is 200nm~300nm submicron order Al powder 0.3g, toluene 50ml, is added to anti-
Answer in container, 23~33 DEG C of ultrasonic 15min, filter, wash filter cake two times with absolute ethyl alcohol, drain, 20~25 DEG C of dryings, obtain
Drying solid.
Obtained drying solid is put into crucible, 300 DEG C~330 DEG C heating 8h, 20~25 DEG C is cooled to, obtains Al/
Fe2O3Thermite.Under high-purity argon gas atmosphere, 10 DEG C of min of heating rate-1, 30 DEG C~1000 DEG C of temperature range, DSC test aluminium
Thermit powder calorific value is 1934.67Jg-1。
Claims (3)
- A kind of 1. Al/Fe2O3The preparation method of thermite, this method comprise the following steps：By Fe2O3Precursor, submicron order Al powder and dispersion solvent are added in reaction vessel, and wherein Al and Fe mol ratio are 1:0.50~1.32, submicron order Al powder Mass volume ratio with dispersion solvent is 1g:63ml~170ml, 20 DEG C~33 DEG C ultrasonic disperses, filtering, washed with absolute ethyl alcohol Filter cake, drain, 20~25 DEG C of dryings, obtain drying solid, obtained drying solid is put into crucible, 300 DEG C~330 DEG C add Hot 5h~10h, 20~25 DEG C are cooled to, obtains Al/Fe2O3Thermite；Used Fe2O3Precursor for can after heated It is transformed into Fe2O3Material；Al is particle diameter 200nm~300nm submicron order Al powder；Dispersion solvent is alkane, aromatic hydrocarbon It is one or two kinds of.
- 2. Al/Fe according to claim 12O3The preparation method of thermite, used Fe2O3Precursor be FeO (OH)、Fe3O4One or two.
- 3. Al/Fe according to claim 12O3The preparation method of thermite, comprises the following steps：Take FeO (OH), particle diameter For 200nm~300nm submicron order Al powder and toluene, it is added in reaction vessel, wherein Al and Fe mol ratio are 1: 1.12, the mass volume ratio of submicron order Al powder and toluene is 1g:167ml, 23~33 DEG C of ultrasonic 15min, filtering, use are anhydrous Ethanol washing filter cake two times, drains, 20~25 DEG C of dryings, obtains drying solid；Obtained drying solid is put into crucible, 300 DEG C~330 DEG C heating 8h, are cooled to 20~25 DEG C, obtain Al/Fe2O3Thermite.
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| CN107245746A (en) * | 2017-04-28 | 2017-10-13 | 重庆大学 | Al/CuO thermites and preparation method thereof |
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| CN104551005B (en) * | 2015-01-07 | 2017-01-04 | 北京化工大学 | A kind of nanoscale nucleocapsid structure thermite and preparation method thereof |
| CN105177517A (en) * | 2015-09-23 | 2015-12-23 | 南京理工大学 | Nanometer thermite and preparing method thereof |
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