CN105537605A - Preparation method of Al/Fe2O3 thermite - Google Patents
Preparation method of Al/Fe2O3 thermite Download PDFInfo
- Publication number
- CN105537605A CN105537605A CN201610019023.6A CN201610019023A CN105537605A CN 105537605 A CN105537605 A CN 105537605A CN 201610019023 A CN201610019023 A CN 201610019023A CN 105537605 A CN105537605 A CN 105537605A
- Authority
- CN
- China
- Prior art keywords
- thermite
- powder
- preparation
- heating
- submicron order
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000003832 thermite Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 title abstract 5
- 239000000843 powder Substances 0.000 claims abstract description 30
- 238000010438 heat treatment Methods 0.000 claims abstract description 23
- 239000007787 solid Substances 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims description 24
- 229910052782 aluminium Inorganic materials 0.000 claims description 19
- 238000006243 chemical reaction Methods 0.000 claims description 16
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 15
- 238000005406 washing Methods 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 9
- 206010013786 Dry skin Diseases 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 239000012065 filter cake Substances 0.000 claims description 7
- 239000006185 dispersion Substances 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- 239000002243 precursor Substances 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 4
- 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
- 238000002156 mixing Methods 0.000 abstract description 2
- 230000008569 process Effects 0.000 abstract description 2
- 239000002270 dispersing agent Substances 0.000 abstract 2
- 238000001816 cooling Methods 0.000 abstract 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 15
- 238000003980 solgel method Methods 0.000 description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000004411 aluminium Substances 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
- 238000012546 transfer Methods 0.000 description 3
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- 239000003638 chemical reducing agent Substances 0.000 description 2
- 238000000227 grinding Methods 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
- 238000001291 vacuum drying Methods 0.000 description 2
- 230000008901 benefit Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007812 deficiency Effects 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
- 239000002360 explosive Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 238000005272 metallurgy Methods 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
- 238000000926 separation method 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 preparation method of an Al/Fe2O3 thermite. The method comprises the following steps: evenly mixing the former body of Fe2O3 and a sub-micron Al powder into a dispersing agent, and then removing the dispersing agent, so as to obtain a dried solid; and putting the dried solid obtained into a crucible, heating at a temperature of 300 DEG C to 330 DEG C for 5 to 10 hours, and then cooling, so as to obtain the Al/Fe2O3 thermite. The preparation method of the Al/Fe2O3 thermite, provided by the invention is short in period, and simple and convenient to operate, the obtained thermite is high in heat value, and the defects of long preparation method and complex operation process in the prior art can be overcome.
Description
Technical field
The present invention relates to a kind of Al/Fe
2o
3the preparation method of thermite, is specifically related to a kind of preparation method of submicron order aluminium powder thermite.
Background technology
Along with the development of material preparation technology, the research of nano aluminum thermit powder becomes focus.Nano aluminum thermit powder is that nanometer aluminium powder and nano-metal-oxide carry out compound at Nano grade.Nano aluminum thermit powder has the close high feature of energy, has a wide range of applications in metallurgy, battery, pottery, military field.The preparation method of nano aluminum thermit powder mainly contains solid reaction process, response inhabitation polishing, sol-gel process, spray heating decomposition, self-assembly method, wherein sol-gel process is the outstanding method of preparation nano aluminum thermit powder, and the method makes the thermit reaction thermal discharge between reactant with higher contact area and Geng Gao.(the Al/Fe such as Wang Yi
2o
3the preparation of nano combined thermite and response characteristic research " priming system " the 4th phase in 2008 11 pages ~ 14 pages thereof) adopt sol-gel process to prepare Al/Fe
2o
3nano aluminum thermit powder, nanometer aluminium powder is joined Fe (NO by the method
3)
39H
2disperse in O ethanolic solution, after temperature constant, add 1,2-expoxy propane, and monitor reaction temperature and pH value change, make generation gel reaction, by the aging placement of gel mixed system that obtains after 6 days, vacuum drying 5 days, then Al/Fe is obtained after grinding, washing, centrifugal, drying
2o
3nano aluminum thermit powder, its calorific value is 1648Jg
-1.(heat treatment is to Al/Fe for Gao Kun etc.
2o
3impact " explosive wastewater journal " the 6th phase in 2012 19 pages ~ 22 pages of nano aluminum thermit powder performance) with sol-gel process, and obtain Al/Fe through heat treatment
2o
3nano aluminum thermit powder, its most high heating value is 1209Jg
-1.It is long to there is synthesis cycle in sol-gel process, the defect that operating process is numerous and diverse.
Summary of the invention
The technical problem to be solved in the present invention is the deficiency for existing in background technology, provides that a kind of manufacturing cycle is short, easy and simple to handle, the Al/Fe of high heating value
2o
3thermite preparation method.
Tradition thermite material in, oxidant and reducing agent are physical mixed, oxidant and reducing agent particle separation, and the interface interaction between different component hinders the diffusion of its reaction heat, cause the energyreleaserate of conventional aluminum thermit powder and energy conversion efficiency lower.Nano aluminum thermit powder is large due to contact area between reactant, decreases mass transfer and heat conducting distance, has higher energy density, can produce high heat in thermit reaction process.In current techniques, the good method of preparation nano aluminum thermit powder is sol-gel process, but the method manufacturing cycle is long, trivial operations.
The present invention is by Fe
2o
3presoma and submicron order Al powder mixed processing after, by heating, in-situ preparation Fe
2o
3crystal, combines closely with Al, is conducive to mass transfer, heat transfer, to improve energy conversion efficiency.The inventive method manufacturing cycle is short, easy and simple to handle.
Al/Fe of the present invention
2o
3the preparation method of thermite, comprises the following steps: by Fe
2o
3precursor, submicron order Al powder and dispersion solvent join in reaction vessel, wherein the mol ratio of Al and Fe is 1:0.50 ~ 1.32, and the mass volume ratio of submicron order Al powder and dispersion solvent is 1g:63ml ~ 170ml, 20 DEG C ~ 33 DEG C ultrasonic disperse, filter, use absolute ethanol washing filter cake, drain, 20 ~ 25 DEG C of dryings, obtain drying solid, the drying solid obtained is put into crucible, 300 DEG C ~ 330 DEG C heating 5h ~ 10h, be cooled to 20 ~ 25 DEG C, obtain Al/Fe
2o
3thermite; The Fe used
2o
3precursor for through heating after can be transformed into Fe
2o
3material, particularly FeO (OH), Fe
3o
4; Al is the submicron order Al powder of particle diameter 200nm ~ 300nm; Dispersion solvent is alkane, aromatic hydrocarbon.
The preferred Al/Fe of the present invention
2o
3thermite is preparation method comprise the following steps: get FeO (OH), submicron order Al powder that particle diameter is 200nm ~ 300nm and toluene, join in reaction vessel, wherein the mol ratio of Al and Fe is 1:1.12, the mass volume ratio of submicron order Al powder and toluene is 1g:167ml, 23 ~ 33 DEG C of ultrasonic 15min, filters, with absolute ethanol washing filter cake two times, drain, 20 ~ 25 DEG C of dryings, obtain drying solid; The drying solid obtained is put into crucible, and 300 DEG C ~ 330 DEG C heating 8h, are cooled to 20 ~ 25 DEG C, obtain Al/Fe
2o
3thermite.
Advantage of the present invention: documents method uses sol-gel process to prepare Al/Fe
2o
3thermite, gel mixed system is aging needs placement 6 days, vacuum drying 5 days; There is gel reaction under detected temperatures and pH value, then through overaging, drying, grinding, washing, centrifugal, drying steps, obtain Al/Fe
2o
3thermite, Al/Fe
2o
3the most high heating value of thermite is 1648Jg
-1.The longest operating procedure of the present invention is heating 5h ~ 10h; Experimentation is mixing, filter, washing, dry, heating simple operations, the Al/Fe obtained
2o
3the most high heating value of thermite is 1934.67Jg
-1.Compared with background technology, the inventive method manufacturing cycle is short, easy and simple to handle, and thermite calorific value is high.
Accompanying drawing explanation
Fig. 1 embodiment 3 thermite SEM schemes
Fig. 2 embodiment 3 thermite XRD schemes
Fig. 3 embodiment 3 thermite DSC schemes
Detailed description of the invention
Below in conjunction with embodiment, the present invention is further described, but the present invention is not by the restriction of the following example.
Analytical instrument: field emission scanning electron microscope (U.S. FEIQuanta600FEG type); X-ray powder diffraction instrument (Dutch PANalytical company EMPYREAN type); TG-DSC combined instrument (Mettler Toledo Inc. of Switzerland TGA/DSC2STAR
esystem type)
Embodiment 1
Get the Fe that particle diameter is 20nm
3o
43.5g, particle diameter is the submicron order Al powder 1g of 200nm ~ 300nm, and normal octane 65ml, joins in reaction vessel, 21 DEG C ~ 26 DEG C ultrasonic 15min, filters, and with absolute ethanol washing filter cake two times, drain, 20 ~ 25 DEG C of dryings, obtain drying solid.
The drying solid obtained is put into crucible, and 300 DEG C ~ 320 DEG C heating 5h, are cooled to 20 ~ 25 DEG C, obtain Al/Fe
2o
3thermite.Under high-purity argon gas atmosphere, heating rate 10 DEG C of min
-1, temperature range 30 DEG C ~ 1000 DEG C, it is 1296.51Jg that DSC tests thermite calorific value
-1.
Embodiment 2
Get FeO (OH) 1.1g, particle diameter is the submicron order Al powder 0.5g of 200nm ~ 300nm, and n-hexane 60ml, joins in reaction vessel, 20 ~ 29 DEG C of ultrasonic 15min, filter, with absolute ethanol washing filter cake two times, drain, 20 ~ 25 DEG C of dryings, obtain drying solid.
The drying solid obtained is put into crucible, and 320 DEG C ~ 330 DEG C heating 5.5h, are cooled to 20 ~ 25 DEG C, obtain Al/Fe
2o
3thermite.Under high-purity argon gas atmosphere, heating rate 10 DEG C of min
-1, temperature range 30 DEG C ~ 1000 DEG C, it is 1503.50Jg that DSC tests thermite calorific value
-1.
Embodiment 3
Get FeO (OH) 1.1g, particle diameter is the submicron order Al powder 0.3g of 200nm ~ 300nm, and toluene 50ml, joins in reaction vessel, 23 ~ 33 DEG C of ultrasonic 15min, filter, with absolute ethanol washing filter cake two times, drain, 20 ~ 25 DEG C of dryings, obtain drying solid.
The drying solid obtained is put into crucible, and 300 DEG C ~ 330 DEG C heating 8h, are cooled to 20 ~ 25 DEG C, obtain Al/Fe
2o
3thermite.Under high-purity argon gas atmosphere, heating rate 10 DEG C of min
-1, temperature range 30 DEG C ~ 1000 DEG C, it is 1934.67Jg that DSC tests thermite calorific value
-1.
Claims (3)
1. an Al/Fe
2o
3the preparation method of thermite, the method comprises the following steps: by Fe
2o
3precursor, submicron order Al powder and dispersion solvent join in reaction vessel, wherein the mol ratio of Al and Fe is 1:0.50 ~ 1.32, and the mass volume ratio of submicron order Al powder and dispersion solvent is 1g:63ml ~ 170ml, 20 DEG C ~ 33 DEG C ultrasonic disperse, filter, use absolute ethanol washing filter cake, drain, 20 ~ 25 DEG C of dryings, obtain drying solid, the drying solid obtained is put into crucible, 300 DEG C ~ 330 DEG C heating 5h ~ 10h, be cooled to 20 ~ 25 DEG C, obtain Al/Fe
2o
3thermite; The Fe used
2o
3precursor for through heating after can be transformed into Fe
2o
3material; Al is the submicron order Al powder of particle diameter 200nm ~ 300nm; Dispersion solvent is alkane, aromatic hydrocarbon.
2. Al/Fe according to claim 1
2o
3the preparation method of thermite, the Fe used
2o
3precursor be FeO (OH), Fe
3o
4.
3. Al/Fe according to claim 1
2o
3the preparation method of thermite, comprise the following steps: get FeO (OH), submicron order Al powder that particle diameter is 200nm ~ 300nm and toluene, join in reaction vessel, wherein the mol ratio of Al and Fe is 1:1.12, and the mass volume ratio of submicron order Al powder and toluene is 1g:167ml, 23 ~ 33 DEG C of ultrasonic 15min, filter, with absolute ethanol washing filter cake two times, drain, 20 ~ 25 DEG C of dryings, obtain drying solid; The drying solid obtained is put into crucible, and 300 DEG C ~ 330 DEG C heating 8h, are cooled to 20 ~ 25 DEG C, obtain Al/Fe
2o
3thermite.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610019023.6A CN105537605B (en) | 2016-01-12 | 2016-01-12 | A kind of Al/Fe2O3The preparation method of thermite |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610019023.6A CN105537605B (en) | 2016-01-12 | 2016-01-12 | A kind of Al/Fe2O3The preparation method of thermite |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105537605A true CN105537605A (en) | 2016-05-04 |
| CN105537605B CN105537605B (en) | 2018-01-23 |
Family
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610019023.6A Expired - Fee Related CN105537605B (en) | 2016-01-12 | 2016-01-12 | A kind of Al/Fe2O3The preparation method of thermite |
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| Country | Link |
|---|---|
| CN (1) | CN105537605B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107245746A (en) * | 2017-04-28 | 2017-10-13 | 重庆大学 | Al/CuO thermites and preparation method thereof |
| CN112341300A (en) * | 2020-11-11 | 2021-02-09 | 西安近代化学研究所 | Micron-sized core-shell thermite and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102500383A (en) * | 2011-11-23 | 2012-06-20 | 西安近代化学研究所 | Double oxide composite type super thermite and preparation method thereof |
| CN104551005A (en) * | 2015-01-07 | 2015-04-29 | 北京化工大学 | Nanometer core shell 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 |
-
2016
- 2016-01-12 CN CN201610019023.6A patent/CN105537605B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102500383A (en) * | 2011-11-23 | 2012-06-20 | 西安近代化学研究所 | Double oxide composite type super thermite and preparation method thereof |
| CN104551005A (en) * | 2015-01-07 | 2015-04-29 | 北京化工大学 | Nanometer core shell 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 |
Non-Patent Citations (4)
| Title |
|---|
| 安亭 等: "超级铝热剂的制备、表征及其燃烧催化作用", 《无机化学学报》 * |
| 李兆娜: "纳米铝热剂的制备及其表征", 《中国优秀硕士学位论文全文数据库（工程科技Ⅰ辑）》 * |
| 王毅 等: "Fe2O3/Al纳米复合铝热剂的制备及其反应特性研究", 《火工品》 * |
| 高坤 等: "制备方法对Al/Fe2O3纳米铝热剂性能的影响", 《火***学报》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107245746A (en) * | 2017-04-28 | 2017-10-13 | 重庆大学 | Al/CuO thermites and preparation method thereof |
| CN112341300A (en) * | 2020-11-11 | 2021-02-09 | 西安近代化学研究所 | Micron-sized core-shell thermite and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105537605B (en) | 2018-01-23 |
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