CN107353172A - A kind of process for dispersing of nanometer catalyst in composite propellant - Google Patents

A kind of process for dispersing of nanometer catalyst in composite propellant Download PDF

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Publication number
CN107353172A
CN107353172A CN201710767890.2A CN201710767890A CN107353172A CN 107353172 A CN107353172 A CN 107353172A CN 201710767890 A CN201710767890 A CN 201710767890A CN 107353172 A CN107353172 A CN 107353172A
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China
Prior art keywords
nanometer
catalyst
nanometer catalyst
composite propellant
dispersing
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CN201710767890.2A
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CN107353172B (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

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Catalysts (AREA)

Abstract

The invention discloses a kind of process for dispersing of nanometer catalyst in composite propellant, is to solve the problems, such as that prior art hardly possible is scattered, step is more, complex process.The process for dispersing step is as follows:It is that ultrasonic disperse is carried out to nanometer catalyst using surfactant and decentralized medium first, then add to have premixed and 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.The present invention is simple to operate, is mixed and disperseed using the ultrasonic disperse and kneader of routine, realizes uniform, the stable dispersion of nanometer catalyst and composite propellant.

Description

A kind of process for dispersing of nanometer catalyst in composite propellant
Technical field
The present invention relates to a kind of process for dispersing of nano material, compound pushed away suitable for the high burn rate of the catalyst containing nanometer Enter the preparation of agent.
Background technology
Nanometer catalyst particle size is small, specific surface area, and surface atom rate is high, and there is very high chemism and catalysis to imitate Rate, micron order catalyst is substituted, the burn rate of propellant can be improved, but nanometer catalyst has from agglomeration, if not Can effectively it disperse, then its actual catalytic efficiency substantially reduces.Disperse to improve nanocatalyst in composite propellant,《Containing energy It is catalyzed the preparation research of composite nano materials》Your ice is opened, waits explosive wastewater journals, 2000,23 (3):9~12. disclose use Solvent-nonsolvent method, prepare ammonium perchlorate (AP) cladding nanoscale copper chromite (c.c) and form compound particle method, by nanometer Added after level copper chromite and ammonium perchlorate (c.c content is 2%, AP content 98%) mixing in ethanol, in ultrasonic wavelength-division Under the conditions of dissipating, alcohol suspension is configured to;Then this hanging drop is added in a beaker for filling ethyl acetate, makes analysis The ammonium perchlorate crystal grain cladding copper chromite nano-particle gone out;Finally it is dried in vacuo, obtains composite particles.The composite particles disperse The method of nanocatalyst, the problem of complex process, dangerous high be present, because in HTPB composite propellants, AP contents 70% More than, even if 20% AP is used to disperse nanometer copper chromite, it will all increase the technical process of composite propellant, increase is prepared into This, makes process complications, and compound particle activity is high, using dangerous also high.
The content of the invention
In order to overcome the shortcomings of background technology, the present invention provides a kind of nanometer of simple, the convenient operation of scatter operation technique Process for dispersing of the combustion catalyst in composite propellant.
Process for dispersing of the nanometer catalyst provided by the invention in composite propellant, comprises the following steps:
A.a. toward addition surfactant and decentralized medium in dispersion cup, dispersion soln is configured to, adds nanometer Catalyst, obtains suspension, and ultrasonic disperse 30min obtains the suspension of nanometer catalyst;The concentration of dispersion soln is 1g Surfactant/1L decentralized media, often disperse 1g nanometers catalyst and add 5mL~15mL dispersion solns;
B. in uniform composite propellant component HTPB, AP, Al medicine slurry has been premixed, nanometer catalyst is added Suspension, 60min is mixed, 50 DEG C of constant temperature, vacuum 50KPa vacuumizes 20min, and then vacuum 10KPa vacuumizes 40min and removed 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), DOS quality is consistent with compound propulsion agent prescription, and ethyl acetate and DOS mass ratio are 1:1;
Advantages of the present invention:(1) operating procedure of the present invention is few, and the scatter operation cycle is short, and in background technology, it is added dropwise and separates out AP and vacuum, which are driven, molten adds the lead time;(2) present invention is scattered using conventional ultrasonic disperse and kneader mixing, realizes Uniform, the stable dispersion of nanometer catalyst and composite propellant, and background technology is except ultrasonic disperse, also using being added dropwise Separating out AP and vacuum drive is molten, not only increase manufacturing cycle, and the AP compound particles of the copper chromite containing nanometer, catalytic activity is high, Using dangerous high;(3) present invention is molten using the combined drive of rough vacuum, increases solvent holdup time in system, right HTPB systems have plasticization, and the viscosity of mixture is low, and dispersing uniformity improves, and background technology is to being added dropwise alcohol suspension Speed do not limit clearly, too fast rate of addition will cause the reunion of nanometer copper chromite, influence nanometer copper chromite Scattered uniformity.
Embodiment
Nanometer catalyst used in the present invention is nanometer copper chromite, granularity (d50) it is 50nm, Institutes Of Technology Of Nanjing's powder Body center produces.
The present invention is described in further detail with reference to embodiment.In HTPB compound propulsion agent prescriptions, chromous acid The addition of copper is usually 0.5%, and the DOS additions as dispersion liquid select typical compound propulsion between 2%-3.5% Agent prescription and its composition such as following table, propellant gross mass are 1000g.
The exemplary complex propellant formulation of table 1 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-80s, 25g Plexol 201s and 25g ethyl acetate are added, is used Glass bar is stirred, and obtains solution, and 5g nanometer catalyst nano copper chromite (d is then added into beaker50For 50nm), After stirring makes fully infiltration, ultrasonic 30min, the suspension of nanometer catalyst is obtained;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 50KPa 20min slowly is vacuumized, then vacuum 10KPa degasification 40min, remove ethyl acetate, complete nanometer catalyst multiple Close in propellant and disperse, be eventually adding 5g curing agent toluenes diisocyanate (TDI), complete the mixing of composite propellant medicine slurry.
Performance test
Tester is TA companies DSCQ200 thermal analyzers
Test condition:Heating rate is 5 DEG C/min, test scope:Room temperature~500 DEG C, the scattered nanometer of test The exothermic peak temperature (Tp) of catalyst and AP mixtures the results are shown in Table 2, nanometer C.C and AP mixtures, compare respectively according to 2% and 98% Example, dispersion liquid is mixed with AP ultrasonic disperses, drives away solvent therein, carries out DSC tests.
Influence of the nanometer catalyst of table 2 to AP exothermic peak temperature
Sample name Tp, DEG C △Tp
C.C and AP mechanical mixtures 338.7 -
Nanometer C.C/AP mixtures 289.1 49.6
Control methods sample 291.4 47.3
Using target collimation method, the burn rate of control sample propellant is tested, and with not disperseed, 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 and example 1 are essentially identical, except that surfactant is Tween-20, remaining component and its Content is same as Example 1.
Method of testing the results are shown in Table 3 with embodiment 1.
Influences of the scattered nanometer C.C of table 3 to propellant burning rate
The above results show, using the present invention, nanometer C.C/AP mixture heat decomposition temperatures are significantly reduced, better than contrast Method;The propellant sample being mixed to get using this method, it is compound that its burn rate does not carry out scattered C.C containing nanometer also significantly greater than Propellant sample (sample 1).

Claims (2)

1. process for dispersing of a kind of nanometer catalyst in composite propellant, it is characterised in that comprise the following steps:
A. toward addition surfactant and decentralized medium in dispersion cup, dispersion soln is configured to, adds nanometer catalyst, Suspension is obtained, ultrasonic disperse 30min obtains the suspension of nanometer catalyst;The concentration of dispersion soln is 1g surface-actives Agent/1L decentralized media, often disperse 1g nanometers catalyst and add 5mL~15mL dispersion solns;
B. in uniform composite propellant component HTPB, AP, Al medicine slurry has been premixed, the suspension of nanometer catalyst is added Liquid, 60min is mixed, 50 DEG C of constant temperature, vacuum 50KPa vacuumizes 20min, and then vacuum 10KPa vacuumizes 40min and removes second Acetoacetic ester, complete nanometer catalyst and disperse in composite propellant.
2. process for dispersing according to claim 1, it is characterised in that the surfactant is Tween-80 or Tween-20, Decentralized medium is mass ratio 1:1 ethyl acetate and Plexol 201, the quality and compound propulsion of Plexol 201 Agent prescription is consistent.
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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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111925263A (en) * 2020-06-10 2020-11-13 湖北航天化学技术研究所 High-combustion-speed azide micro-smoke propellant and preparation process thereof
CN115532294A (en) * 2022-09-26 2022-12-30 西北工业大学 Nitrogen vacancy-containing Fe 2 N nanowire combustion catalyst and preparation method thereof

Citations (5)

* Cited by examiner, † Cited by third party
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
US20080190525A1 (en) * 2007-02-12 2008-08-14 Kerry Lee Wagaman Inorganic nitrate-hydrogen peroxide adducts and methods for their preparation
CN101549289A (en) * 2009-05-12 2009-10-07 武汉大学 Nucleocapsid energizing agent for propelling agent and method for preparing same
CN101921160A (en) * 2010-09-14 2010-12-22 西安近代化学研究所 Preparation method of super-thermite Al/PbO nano-composite energetic material
CN106187655A (en) * 2016-07-19 2016-12-07 合肥科斯孚安全科技有限公司 A kind of low burn temperature height combustion speed solid propellant and preparation method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
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
US20080190525A1 (en) * 2007-02-12 2008-08-14 Kerry Lee Wagaman Inorganic nitrate-hydrogen peroxide adducts and methods for their preparation
CN101549289A (en) * 2009-05-12 2009-10-07 武汉大学 Nucleocapsid energizing agent for propelling agent and method for preparing same
CN101921160A (en) * 2010-09-14 2010-12-22 西安近代化学研究所 Preparation method of super-thermite Al/PbO nano-composite energetic material
CN106187655A (en) * 2016-07-19 2016-12-07 合肥科斯孚安全科技有限公司 A kind of low burn temperature height combustion speed solid propellant and preparation method thereof

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111925263A (en) * 2020-06-10 2020-11-13 湖北航天化学技术研究所 High-combustion-speed azide micro-smoke propellant and preparation process thereof
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
CN115532294A (en) * 2022-09-26 2022-12-30 西北工业大学 Nitrogen vacancy-containing Fe 2 N nanowire combustion catalyst and preparation method 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

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