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 PDF

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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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nanometer catalyst
nanometer
composite propellant
catalyst
added
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CN107353172A (en
Inventor
胥会祥
李勇宏
来安户
石小兵
赵西鹏
李军强
赵凤起
高红旭
冉秀伦
范红杰
李洋
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Xian Modern Chemistry Research Institute
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Xian Modern Chemistry Research Institute
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    • CCHEMISTRY; METALLURGY
    • C06EXPLOSIVES; MATCHES
    • C06BEXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
    • C06B23/00Compositions characterised by non-explosive or non-thermic constituents
    • C06B23/007Ballistic modifiers, burning rate catalysts, burning rate depressing agents, e.g. for gas generating
    • CCHEMISTRY; METALLURGY
    • C06EXPLOSIVES; MATCHES
    • C06BEXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
    • C06B21/00Apparatus or methods for working-up explosives, e.g. forming, cutting, drying
    • CCHEMISTRY; METALLURGY
    • C06EXPLOSIVES; MATCHES
    • C06BEXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
    • C06B29/00Compositions containing an inorganic oxygen-halogen salt, e.g. chlorate, perchlorate
    • C06B29/22Compositions containing an inorganic oxygen-halogen salt, e.g. chlorate, perchlorate the salt being ammonium perchlorate

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

A kind of dispersing method of nanometer catalyst in composite propellant
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.
CN201710767890.2A 2017-08-31 2017-08-31 A kind of dispersing method of nanometer catalyst in composite propellant Active CN107353172B (en)

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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)

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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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