CN107353172B - A kind of dispersing method of nanometer catalyst in composite propellant - Google Patents
A kind of dispersing method of nanometer catalyst in composite propellant Download PDFInfo
- Publication number
- CN107353172B CN107353172B CN201710767890.2A CN201710767890A CN107353172B CN 107353172 B CN107353172 B CN 107353172B CN 201710767890 A CN201710767890 A CN 201710767890A CN 107353172 B CN107353172 B CN 107353172B
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- CN
- China
- Prior art keywords
- nanometer catalyst
- nanometer
- composite propellant
- catalyst
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- 239000003054 catalyst Substances 0.000 title claims abstract description 30
- 239000003380 propellant Substances 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 26
- 239000002131 composite material Substances 0.000 title claims abstract description 19
- 239000006185 dispersion Substances 0.000 claims abstract description 15
- 239000004094 surface-active agent Substances 0.000 claims abstract description 8
- 239000003814 drug Substances 0.000 claims abstract description 5
- 239000002002 slurry Substances 0.000 claims abstract description 5
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 21
- 239000000725 suspension Substances 0.000 claims description 10
- VJHINFRRDQUWOJ-UHFFFAOYSA-N dioctyl sebacate Chemical compound CCCCC(CC)COC(=O)CCCCCCCCC(=O)OCC(CC)CCCC VJHINFRRDQUWOJ-UHFFFAOYSA-N 0.000 claims description 9
- 150000001875 compounds Chemical class 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- 229920002121 Hydroxyl-terminated polybutadiene Polymers 0.000 claims description 6
- 229920001213 Polysorbate 20 Polymers 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 235000010486 polyoxyethylene sorbitan monolaurate Nutrition 0.000 claims description 3
- 239000000256 polyoxyethylene sorbitan monolaurate Substances 0.000 claims description 3
- XYIBRDXRRQCHLP-UHFFFAOYSA-N ethyl acetoacetate Chemical compound CCOC(=O)CC(C)=O XYIBRDXRRQCHLP-UHFFFAOYSA-N 0.000 claims 1
- 238000002156 mixing Methods 0.000 abstract description 5
- 239000002904 solvent Substances 0.000 abstract description 3
- GDDNTTHUKVNJRA-UHFFFAOYSA-N 3-bromo-3,3-difluoroprop-1-ene Chemical compound FC(F)(Br)C=C GDDNTTHUKVNJRA-UHFFFAOYSA-N 0.000 description 18
- JGDFBJMWFLXCLJ-UHFFFAOYSA-N copper chromite Chemical compound [Cu]=O.[Cu]=O.O=[Cr]O[Cr]=O JGDFBJMWFLXCLJ-UHFFFAOYSA-N 0.000 description 9
- 239000000203 mixture Substances 0.000 description 9
- 239000000523 sample Substances 0.000 description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 235000019441 ethanol Nutrition 0.000 description 3
- -1 AP compound Chemical class 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000011246 composite particle Substances 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000011943 nanocatalyst Substances 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- ZEARRFOSVATHLW-UHFFFAOYSA-L O[Cr](O)=O Chemical compound O[Cr](O)=O ZEARRFOSVATHLW-UHFFFAOYSA-L 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 239000013068 control sample Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000007872 degassing Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000000320 mechanical mixture Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 description 1
- 229920000053 polysorbate 80 Polymers 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- 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
- C06B21/00—Apparatus or methods for working-up explosives, e.g. forming, cutting, drying
-
- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B29/00—Compositions containing an inorganic oxygen-halogen salt, e.g. chlorate, perchlorate
- C06B29/22—Compositions containing an inorganic oxygen-halogen salt, e.g. chlorate, perchlorate the salt being ammonium perchlorate
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
Abstract
It is to solve the problems, such as that prior art difficulty is dispersed, step is more, complex process the invention discloses a kind of dispersing method of nanometer catalyst in composite propellant.Steps are as follows for the dispersing method: being to carry out ultrasonic disperse to nanometer catalyst using surfactant and decentralized medium first, then it is added to have premixed and be mixed in the other component medicine slurries of uniform composite propellant, the solvent in rough vacuum removing decentralized medium is heated, nanometer catalyst is completed and disperses in composite propellant.Operation of the present invention is simple, using conventional ultrasonic disperse and kneader mixing dispersion, realizes uniform, the stable dispersion of nanometer catalyst and composite propellant.
Description
Technical field
The present invention relates to a kind of dispersing methods of nano material, and the high burn rate suitable for the catalyst containing nanometer is compound to be pushed away
Into the preparation of agent.
Background technique
Nanometer catalyst particle size is small, specific surface area, and surface atom rate is high, has very high chemical activity and catalysis effect
Rate substitutes micron order catalyst, can improve the burn rate of propellant, but nanometer catalyst has from agglomeration, if not
Can effectively it disperse, then its practical catalytic efficiency substantially reduces.Disperse in composite propellant to improve nanocatalyst, " contains energy
It is catalyzed the preparation research of composite nano materials " your ice, wait explosive wastewater journal, 2000,23 (3): 9~12. disclose use
Solvent-nonsolvent method prepares ammonium perchlorate (AP) cladding nanoscale copper chromite (c.c) and forms compound particle method, by nanometer
It is added in ethyl alcohol after grade copper chromite and ammonium perchlorate (content 98% that the content of c.c is 2%, AP) mixing, in ultrasonic wavelength-division
Under the conditions of dissipating, it is configured to alcohol suspension；Then this hanging drop is added in the beaker that one fills ethyl acetate, makes to analyse
Ammonium perchlorate crystal grain out coats copper chromite nanoparticle；It is finally dried in vacuo, obtains composite particles.Composite particles dispersion
The method of nanocatalyst has that complex process, risk are high, because in HTPB composite propellant, AP content 70%
More than, even if 20% AP will increase the technical process of composite propellant, increase is prepared into for dispersing nanometer copper chromite
This, makes process complications, and compound particle activity is high, also high using risk.
Summary of the invention
In order to overcome the shortcomings of background technique, a kind of nanometer that the present invention provides scatter operation simple process, facilitates operation
Dispersing method of the combustion catalyst in composite propellant.
Dispersing method of the nanometer catalyst provided by the invention in composite propellant, comprising the following steps:
A.a. surfactant and decentralized medium are added into dispersion cup, is configured to dispersion solution, nanometer is added
Catalyst, obtains suspension, and ultrasonic disperse 30min obtains the suspension of nanometer catalyst；The concentration for dispersing solution is 1g
Surfactant/1L decentralized medium, every dispersion 1g nanometer catalyst are added 5mL~15mL and disperse solution；
B. in having premixed uniform composite propellant component HTPB, AP, Al medicine slurry, nanometer catalyst is added
Suspension mixes 60min, and 50 DEG C of constant temperature, vacuum degree 50KPa vacuumizes 20min, and then vacuum degree 10KPa vacuumizes 40min and removes
Ethyl acetate is removed, nanometer catalyst is completed and disperses in composite propellant.
Wherein surfactant is Tween-80 or Tween-20, and decentralized medium is ethyl acetate and Plexol 201
(DOS), the quality of DOS is consistent with compound propulsion agent prescription, and the mass ratio of ethyl acetate and DOS are 1:1；
Advantages of the present invention: (1) operation of the present invention step is few, and the scatter operation period is short, and in background technique, it is added dropwise and is precipitated
AP and vacuum, which are driven, molten increases the lead time；(2) present invention is realized using conventional ultrasonic disperse and kneader mixing dispersion
Uniform, the stable dispersion of nanometer catalyst and composite propellant, and background technique is in addition to ultrasonic disperse, also using being added dropwise
AP is precipitated and vacuum drive is molten, not only increases manufacturing cycle, but also the AP compound particle of the copper chromite containing nanometer, catalytic activity is high,
Use risk height；(3) present invention is molten using the combined drive of rough vacuum, increases solvent residence time in system, right
HTPB system has plasticization, and the viscosity of mixture is low, and dispersing uniformity improves, and background technique is to dropwise addition alcohol suspension
Speed do not limit clearly, too fast rate of addition will lead to the reunion of nanometer copper chromite, influence nanometer copper chromite
The uniformity of dispersion.
Specific embodiment
Nanometer catalyst used in the present invention is nanometer copper chromite, granularity (d50) it is 50nm, Institutes Of Technology Of Nanjing's powder
The production of body center.
Below with reference to embodiment, invention is further described in detail.In HTPB compound propulsion agent prescription, chromous acid
The additional amount of copper is usually 0.5%, and the DOS additional amount as dispersion liquid selects typical compound propulsion between 2%-3.5%
Agent prescription and its composition such as following table, propellant gross mass are 1000g.
1 exemplary complex propellant formulation of table and composition content
| Content | HTPB | Curing agent | AP | Al powder | Nanometer c.c | DOS |
| % | 10.5 | 0.5 | 71 | 15 | 0.5 | 2.5 |
| g | 105 | 5 | 710 | 150 | 5 | 25 |
Embodiment 1
In a 200mL beaker, 0.05g Tween-80,25g Plexol 201 and 25g ethyl acetate is added, uses
Glass bar stirring, obtains solution, and the nanometer catalyst nano copper chromite (d of 5g is then added into beaker50For 50nm),
Stirring makes after sufficiently infiltrating, and ultrasonic 30min obtains the suspension of nanometer catalyst；It is uniform having premixed
In 965gHTPB, AP, Al medicine slurry, above-mentioned suspension is added, with kneader mixing 60min, under 50 DEG C of heating, vacuum degree 50KPa
20min slowly is vacuumized, then vacuum degree 10KPa degasification 40min, remove ethyl acetate, completes nanometer catalyst multiple
It closes and disperses in propellant, be eventually adding 5g curing agent toluene diisocyanate (TDI), complete the mixing of composite propellant medicine slurry.
Performance test
Test equipment is TA company DSCQ200 thermal analyzer
Test condition: heating rate is 5 DEG C/min, test scope: room temperature~500 DEG C, the nanometer of the dispersion of test
The exothermic peak temperature (Tp) of catalyst and AP mixture the results are shown in Table 2, and nanometer C.C and AP mixture compare according to 2% and 98% respectively
Example, dispersion liquid is mixed with AP ultrasonic disperse, drives away solvent therein, carries out DSC test.
Influence of the 2 nanometer catalyst of table to AP exothermic peak temperature
| Sample name | Tp, DEG C | △Tp |
| C.C and AP mechanical mixture | 338.7 | - |
| Nanometer C.C/AP mixture | 289.1 | 49.6 |
| Control methods sample | 291.4 | 47.3 |
Using target collimation method, test the burn rate of control sample propellant, and with do not dispersed, nanometer C.C is directly added
The sample (sample 1) for entering propellant formulation compares, and the results are shown in Table 3.
Embodiment 2
This example implementation method and example 1 are essentially identical, except that surfactant be Tween-20, remaining component and its
Content is same as Example 1.
Test method the results are shown in Table 3 with embodiment 1.
Influence of the nanometer C.C that table 3 disperses to propellant burning rate
The above results show that, using the present invention, nanometer C.C/AP mixture thermal decomposition temperature is significantly reduced, better than comparison
Method；The propellant sample being mixed to get using this method, the C.C containing nanometer that burn rate is not dispersed also significantly greater than are compound
Propellant sample (sample 1).
Claims (1)
1. a kind of dispersing method of nanometer catalyst in composite propellant, it is characterised in that the following steps are included:
A. surfactant and decentralized medium are added into dispersion cup, is configured to dispersion solution, nanometer catalyst is added,
Suspension is obtained, ultrasonic disperse 30min obtains the suspension of nanometer catalyst；The concentration for dispersing solution is 1g surface-active
Agent/1L decentralized medium, every dispersion 1g nanometer catalyst are added 5mL~15mL and disperse solution；The surfactant is to spit
Temperature -80 or Tween-20, decentralized medium are the ethyl acetate and Plexol 201 that mass ratio is 1:1, Plexol 201
Quality it is consistent with compound propulsion agent prescription；
B. in having premixed uniform composite propellant component HTPB, AP, Al medicine slurry, the suspension of nanometer catalyst is added
Liquid mixes 60min, and 50 DEG C of constant temperature, vacuum degree 50KPa vacuumizes 20min, and then vacuum degree 10KPa vacuumizes 40min and removes second
Acetoacetic ester is completed nanometer catalyst and is dispersed in composite propellant.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710767890.2A CN107353172B (en) | 2017-08-31 | 2017-08-31 | A kind of dispersing method of nanometer catalyst in composite propellant |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710767890.2A CN107353172B (en) | 2017-08-31 | 2017-08-31 | A kind of dispersing method of nanometer catalyst in composite propellant |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107353172A CN107353172A (en) | 2017-11-17 |
| CN107353172B true CN107353172B (en) | 2019-02-12 |
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| CN201710767890.2A Expired - Fee Related CN107353172B (en) | 2017-08-31 | 2017-08-31 | A kind of dispersing method of nanometer catalyst in composite propellant |
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| CN111925263B (en) * | 2020-06-10 | 2022-01-04 | 湖北航天化学技术研究所 | High-combustion-speed azide micro-smoke propellant and preparation process thereof |
| CN115532294B (en) * | 2022-09-26 | 2023-11-17 | 西北工业大学 | Fe with nitrogen vacancy 2 N nanowire combustion catalyst and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1513596A (en) * | 2003-07-07 | 2004-07-21 | 深圳大学 | Nano-copper-lead composite oxide powder and its preparation method |
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| US20080190525A1 (en) * | 2007-02-12 | 2008-08-14 | Kerry Lee Wagaman | Inorganic nitrate-hydrogen peroxide adducts and methods for their preparation |
| CN101549289B (en) * | 2009-05-12 | 2012-08-22 | 武汉大学 | Nucleocapsid energizing agent for propelling agent and method for preparing same |
| CN101921160B (en) * | 2010-09-14 | 2012-11-07 | 西安近代化学研究所 | Preparation method of super-thermite Al/PbO nano-composite energetic material |
| CN106187655B (en) * | 2016-07-19 | 2019-06-11 | 合肥科斯孚安全科技有限公司 | A kind of high burn rate solid propellant of low burn temperature and preparation method thereof |
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| CN1513596A (en) * | 2003-07-07 | 2004-07-21 | 深圳大学 | Nano-copper-lead composite oxide powder and its preparation method |
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Granted publication date: 20190212 |