CN108530239A - A kind of highly filled NEPE solid propellants slurry, propellant and preparation method - Google Patents

A kind of highly filled NEPE solid propellants slurry, propellant and preparation method Download PDF

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Publication number
CN108530239A
CN108530239A CN201810698896.3A CN201810698896A CN108530239A CN 108530239 A CN108530239 A CN 108530239A CN 201810698896 A CN201810698896 A CN 201810698896A CN 108530239 A CN108530239 A CN 108530239A
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slurry
propellant
nepe
aluminium
preparation
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CN108530239B (en
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王小英
张�林
燕为光
唐泉
张艳
潘新洲
李伟
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Hubei Institute of Aerospace Chemical Technology
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Hubei Institute of Aerospace Chemical Technology
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    • CCHEMISTRY; METALLURGY
    • C06EXPLOSIVES; MATCHES
    • C06BEXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
    • C06B33/00Compositions containing particulate metal, alloy, boron, silicon, selenium or tellurium with at least one oxygen supplying material which is either a metal oxide or a salt, organic or inorganic, capable of yielding a metal oxide
    • C06B33/12Compositions containing particulate metal, alloy, boron, silicon, selenium or tellurium with at least one oxygen supplying material which is either a metal oxide or a salt, organic or inorganic, capable of yielding a metal oxide the material being two or more oxygen-yielding compounds
    • C06B33/14Compositions containing particulate metal, alloy, boron, silicon, selenium or tellurium with at least one oxygen supplying material which is either a metal oxide or a salt, organic or inorganic, capable of yielding a metal oxide the material being two or more oxygen-yielding compounds at least one being an inorganic nitrogen-oxygen salt
    • 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
    • C06B21/0008Compounding the ingredient
    • C06B21/0025Compounding the ingredient the ingredient being a polymer bonded explosive or thermic component
    • CCHEMISTRY; METALLURGY
    • C06EXPLOSIVES; MATCHES
    • C06DMEANS FOR GENERATING SMOKE OR MIST; GAS-ATTACK COMPOSITIONS; GENERATION OF GAS FOR BLASTING OR PROPULSION (CHEMICAL PART)
    • C06D5/00Generation of pressure gas, e.g. for blasting cartridges, starting cartridges, rockets
    • C06D5/06Generation of pressure gas, e.g. for blasting cartridges, starting cartridges, rockets by reaction of two or more solids

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  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Combustion & Propulsion (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Adhesives Or Adhesive Processes (AREA)

Abstract

The present invention provides a kind of highly filled NEPE solid propellants slurry, propellant and preparation methods, belong to solid propellant technical field.The preparation method of the slurry, includes the following steps:Weigh raw material, wherein the raw material includes ammonium perchlorate, nitrolite, aluminium powder, adhesive composition, curing agent and function additive, and the aluminium powder is the mixture of special atomized aluminium or special atomized aluminium and FLTQ1 aluminium powders, the granularity d of spy's atomized aluminium50It is 2.5 μm 13 μm;Part described adhesive system is mixed with the aluminium powder, nitrolite and function additive weighed, obtains mixture, the quality of the part described adhesive system is the 9.5 12% of raw material gross mass;In the mixture that the ammonium perchlorate weighed and nitrolite are added, then curing agent and remaining described adhesive system is added in mixing, mixing obtains propellant slurry.The present invention can obviously improve the processing performance of propellant slurry under the premise of not influencing propellant energy, mechanical property and incorporation time.

Description

A kind of highly filled NEPE solid propellants slurry, propellant and preparation method
Technical field
The present invention relates to a kind of NEPE propellants and preparation method thereof, belong to solid propellant technical field.
Background technology
With the application of tactical missile, the requirement to propellant high-energy, low burning rate, strong mechanical performance is higher and higher. To meet performance, the general NEPE high-energy solid propellants used using PET as adhesive, wherein AL powder contents are less than or wait In 18%, use specification specified in GJB 1738-93 for FLTQ1 aluminium powders.Due to the requirement of high-energy, the solid of propellant contains Amount need to generally be up to 77%-81%, this brings to the processing performance of NEPE propellants compared with hang-up.It is to meet low burning rate simultaneously It is required that propellant oxidizing agent and reducing agent are all made of coarser grained component, propellant formulation grading is unreasonable, and solid packing cannot get Fully wetting, causes Propellant Processing Characteristics to deteriorate.Therefore, low burning rate, highly filled NEPE propellants processing performance at For the technical bottleneck of its popularization and application.Discharge medicine after highly filled NEPE propellants (solid content 80%) the 5L mixing on basis The rheological property of slurry is:τy=214.8Pa, η=388.9Pas.Medicine slurry cannot be satisfied motor charge technological requirement, cause Motor charge fails.
The existing technology for improving propellant slurry processing performance mainly has:Reduce bonding agent content, adjustment solid packing grade Match, using process auxiliaries and extension incorporation time etc..These technological means reduce propulsion such as the method for reducing bonding agent content The mechanical property of agent finished medicines;And it is usually to adjust the grading of oxidant to adjust solid packing grading, this method changes propulsion Agent combustibility and mechanical property;The approach for seeking process auxiliaries is that effective process auxiliaries screening difficulty is big, for not androgynous System need to use different auxiliary agents, while auxiliary agent may cause mechanical properties of propellant to change;Extend incorporation time (up to more than ten small When) then it is unfavorable for large-scale production.
Invention content
The technology of the present invention solves the problems, such as:Overcome the deficiencies of the prior art and provide a kind of highly filled NEPE solids Propellant slurry, propellant and preparation method are right under the premise of not influencing propellant energy, mechanical property and incorporation time Propellant burning rate influences very little, can obviously improve the processing performance of propellant slurry.
For achieving the above object, the present invention provides the following technical solutions:
A kind of preparation method of highly filled NEPE solid propellants slurry, which is characterized in that include the following steps:
Step 1 weighs raw material, wherein the raw material includes ammonium perchlorate, nitrolite, aluminium powder, adhesive composition, consolidates Agent and function additive, the aluminium powder are the mixture of special atomized aluminium or special atomized aluminium and FLTQ1 aluminium powders, spy's atomized aluminium Granularity d50It is 2.5 μm -13 μm;
Step 2 mixes part described adhesive system with the aluminium powder, nitrolite and function additive weighed, obtains To mixture, the quality of the part described adhesive system is the 9.5-12% of raw material gross mass;
In step 3, the mixture that the ammonium perchlorate weighed is added, then mixing is added curing agent and remains Remaining described adhesive system, mixing, obtains propellant slurry.
Specifically, the raw material described in step 1 includes following content of component:
29-45 parts of ammonium perchlorate, 17-30 parts of nitrolite, 17-18 parts of aluminium powder, 19-22 parts of adhesive composition, curing agent 0.5-0.8 parts and 0.6-1.2 parts of function additive.
Specifically, the granularity of the ammonium perchlorate is 120-400 μm.
Specifically, the granularity of the nitrolite is 80-110 μm.
In an alternative embodiment, the granularity of spy's atomized aluminium is 2.5-6 μm.
Further, mass percent of the special atomized aluminium in the NEPE solid propellants is 3%-5%.
In an alternative embodiment, the granularity of spy's atomized aluminium is 6.0-13 μm.
Further, mass percent of the special atomized aluminium in the NEPE solid propellants is 5%-18%.
Specifically, described adhesive system includes adhesive and plasticizer, and the mass ratio of the plasticizer and adhesive is (1.5~2.0):1.
Specifically, described adhesive is terminal hydroxy group Ethylene Oxide-Tetrahydrofuran Copolyether;The plasticizer is that nitrification is sweet Oil, triethylene glycol dinitrate, trimethylolethane trimethacrylate nitrate, diglycol dinitrate or 1,2,4- fourths three One or more kinds of combinations in alcohol trisnitrate.
Specifically, step 2 by part described adhesive system and the aluminium powder, nitrolite and the function additive that weigh in telecentricity It is mixed 20-30 minutes under the conditions of slurry linear velocity is 1~1.2m/s, mixing temperature is 50~65 DEG C.
Specifically, it is 1 in telecentricity slurry linear velocity in the mixture that the ammonium perchlorate weighed is added step 3 ~1.2m/s, mixing temperature are to be mixed at 50~65 DEG C 40-50 minutes, and curing agent and remaining described adhesive body is then added Tie up to telecentricity slurry linear velocity be 1~1.2m/s, mixing temperature is to be mixed 15-25 minutes at 40~50 DEG C.
The propellant slurry prepared by the above method.
A kind of preparation method of solid propellant, includes the following steps:
Step 1 weighs raw material, wherein the raw material includes ammonium perchlorate, nitrolite, aluminium powder, adhesive composition, consolidates Agent and function additive, the aluminium powder are the mixture of special atomized aluminium or special atomized aluminium and FLTQ1 aluminium powders, spy's atomized aluminium Granularity d50It is 2.5 μm -13 μm;
Step 2 mixes part described adhesive system with the aluminium powder, nitrolite and function additive weighed, institute The quality for stating part described adhesive system is the 9.5-12% of raw material gross mass, obtains mixture;
Step 3 will mix in the mixture that the ammonium perchlorate weighed is added, and curing agent and residue is then added Described adhesive system mixing, solidification, obtain propellant.
The present invention has the beneficial effect that compared with prior art:
(1) preparation method of highly filled NEPE solid propellants slurry provided in an embodiment of the present invention, by adjusting The granularity of reducing agent aluminium powder changes the grain size cooperation of solid component in formula, meanwhile, added by controlling the initial of adhesive composition Enter amount, under the premise of not changing propellant formulation composition, not influencing propellant energy and mechanical property, makes solid component and liquid Good processing performance in having after the mixing of body component, it is poor to solve highly filled NEPE propellants slurry technique, pours into a mould difficulty Big problem;Meanwhile this method incorporation time is short (longest 100 minutes), is conducive to large-scale production;
(2) present invention substantially reduces highly filled NEPE propellants discharging slurry by adjusting the grading of reducing agent Viscosity and yield value, discharge slurry τ y≤100Pa, η≤300Pas, well below in the prior art using fundamental technology discharging The rheological property of slurry is:τy=214.8Pa, η=388.9Pas, process improving is apparent, meets engine cast and requires.
Specific implementation mode
The specific implementation mode of the present invention is described in further details below in conjunction with specific embodiment.
An embodiment of the present invention provides a kind of highly filled NEPE solid propellants, raw material includes following mass parts group Point:
AP29-45 parts of ammonium perchlorate, 17-30 parts of nitrolite, 17-18 parts of aluminium powder, 19-22 parts of adhesive composition, solidification 0.6-1.2 parts of 0.5-0.8 parts of agent and function additive, wherein the aluminium powder is special atomized aluminium or special atomized aluminium and FLTQ1 aluminium powders Mixture, it is described spy atomized aluminium granularity d50It is 2.5 μm -13 μm;Preferred 120-400 μm of the granularity of the ammonium perchlorate;Institute State preferred 80-110 μm of the granularity of nitrolite.
In the embodiment of the present invention, nitrolite is generally octogen HMX or heisuojin RDX, the function additive include Catalyst, stabilization agent and bonding agent, in the embodiment of the present invention, the preferred triphenyl bismuth of catalyst, the preferred N- of stabilization agent Methyl paranitroaniline MNA or 2- nitrodiphenylamine 2-NDPA, the preferably neutral bonding agent NPBA of the bonding agent;Selected solidification Agent is one or both of six methine polyisocyanates LM-100 of toluene di-isocyanate(TDI) TDI or modified combinations, preferably TDI, alternative LM-100;The highly filled preferred burn rate of NEPE solid propellants provided by the invention is no more than 8.5mm/s;It is described Adhesive composition includes adhesive and plasticizer, and the mass ratio of the plasticizer and adhesive is preferably (1.5~2.0):1, work as increasing When moulding the mixture that agent is two kinds of substances, the mass ratio preferably 1 of described two substances:1;The preferred terminal hydroxy group epoxy of described adhesive Ethane-tetrahydrofuran copolyether PET;The plasticizer is nitroglycerine NG, triethylene glycol dinitrate TEGDN, three hydroxyls In methyl ethane trisnitrate TEMTN, diglycol dinitrate DEGDN or 1,2,4- butanetriol trinitrate BTTN One or more combination.
According to R&D experience, since special atomized aluminium granularity is less than FLQT1 aluminium powders, because without making the mechanical property of formula drop It is low.
In an alternative embodiment, preferred 2.5-6 μm of the granularity of spy's atomized aluminium, spy's atomized aluminium is in the NEPE The preferred 3%-5% of mass percent in solid propellant;
In an alternative embodiment, preferred 6.0-13 μm of the granularity of spy's atomized aluminium, spy's atomized aluminium is described The preferred 5%-18% of mass percent in NEPE solid propellants.
The embodiment of the present invention additionally provides a kind of preparation method of highly filled NEPE solid propellants slurry, including with Lower step:
Step 1 weighs raw material, wherein the raw material includes ammonium perchlorate, nitrolite, aluminium powder, adhesive composition, consolidates Agent and function additive, the aluminium powder are the mixture of special atomized aluminium or special atomized aluminium and FLTQ1 aluminium powders, spy's atomized aluminium Granularity d50It is 2.5 μm -13 μm;
Specifically, the raw material that the present embodiment uses is provided by above-described embodiment, is specifically described and be can be found in above-mentioned raw materials implementation Example, details are not described herein.
Step 2 mixes part described adhesive system with the aluminium powder, nitrolite and function additive weighed, obtains To mixture, the quality of the part described adhesive system is the 9.5-12% of raw material gross mass;
And specifically, it is preferable to be mixed 20-30 minutes in 1~1.2m/s of telecentricity slurry linear velocity, 50~65 DEG C of mixing temperature. In the step, adhesive composition addition is excessive, can influence the function and effect of function additive especially bonding agent, and easily makes technique Penalty;And adhesive composition addition is too small, easily prevents solid constituent from fully soaking, early period, slurry was too dry, tended to have peace Full hidden danger.
In step 3, the mixture that the ammonium perchlorate weighed is added, then mixing is added curing agent and remains Remaining described adhesive system mixing, obtains propellant slurry.
Specifically, mixed for the first time in step 3 preferably telecentricity slurry linear velocity be 1~1.2m/s, mixing temperature be 50~ It is mixed 40-50 minutes at 65 DEG C;The time of mixing is preferably in telecentricity slurry linear velocity 1~1.2m/s of position, mixing temperature for the second time 40~50 DEG C mix 15-25 minutes.
The preparation method of highly filled NEPE solid propellants slurry provided in an embodiment of the present invention, by adjusting reduction The granularity of agent aluminium powder changes the grain size cooperation of solid component in formula, meanwhile, by controlling being initially added for adhesive composition Amount makes solid component and liquid under the premise of not changing propellant formulation composition, not influencing propellant energy and mechanical property Good processing performance in having after component mixing, it is poor to solve highly filled NEPE propellants slurry technique, and cast difficulty is big The problem of;Meanwhile this method incorporation time is short (100 minutes), is conducive to large-scale production;
The present invention substantially reduces the viscosity of highly filled NEPE propellants discharging slurry by adjusting the grading of reducing agent And yield value, discharge slurry τ y≤100Pa, η≤300Pas, well below in the prior art using fundamental technology discharging slurry Rheological property be:τy=214.8Pa, η=388.9Pas, process improving is apparent, meets engine cast and requires;
The embodiment of the present invention additionally provides a kind of preparation method of solid propellant, including:To solid propellant slurry into Row solidification, obtains propellant.
Specifically, the solid solid propellant slurry is made by above-described embodiment method, is specifically described referring to above-mentioned reality Apply example;Preferred 40-60 DEG C of solidification temperature.
It is several specific embodiments of the present invention below:
Embodiment 1
It includes following step to present embodiments provide a kind of highly filled NEPE propellants slurry and propellant, preparation method Suddenly:
Step 1 weighs raw material by the formula of table 1;
PET, NG and TEGDN for weighing are mixed to get adhesive composition by step 2, by 10.8 mass parts described adhesives System and the aluminium powder, nitrolite and the function additive that weigh telecentricity slurry linear velocity be 1m/s, the condition that mixing temperature is 65 DEG C Lower mixing 25 minutes, obtains mixture,
In step 3, the mixture that the AP weighed is added, in telecentricity slurry linear velocity 1m/s, mixing temperature 60 It is mixed at DEG C 45 minutes, curing agent and remaining described adhesive system is then added, be 1m/s, mix in telecentricity slurry linear velocity It is mixed 20 minutes under temperature 45 C, obtains propellant slurry;
Step 4 carries out solidification 168h at 50 DEG C to obtained propellant slurry, obtains solid propellant.
1 propellant formulation of table
Comparative example 1
This comparative example provides a kind of highly filled NEPE propellants slurry and propellant, preparation method and embodiment 1 is essentially identical, and uniquely the difference is that, aluminium powder is all using FLTQ1 aluminium powders.
Embodiment 2
It includes following step to present embodiments provide a kind of highly filled NEPE propellants slurry and propellant, preparation method Suddenly:
Step 1 weighs raw material by the formula of table 2;
PET, NG and TEGDN for weighing are mixed to get adhesive composition by step 2, by 12 mass parts described adhesive bodies It is to mix 20 points at telecentricity slurry linear velocity 1.2m/s, 65 DEG C of mixing temperature with the aluminium powder, nitrolite and function additive weighed Clock obtains mixture,
In step 3, the mixture that the AP weighed is added, in telecentricity slurry linear velocity 1.2m/s, mixing temperature 65 DEG C mix 50 minutes, and curing agent and remaining described adhesive system is then added, in telecentricity slurry linear velocity 1.2m/s, mixing Temperature 50 C mixes 20 minutes, obtains propellant slurry;
Step 4 carries out solidification 168h at 50 DEG C to obtained propellant slurry, obtains solid propellant.
2 propellant formulation of table
Comparative example 2
This comparative example provides a kind of highly filled NEPE propellants slurry and propellant, preparation method and embodiment 2 is essentially identical, and uniquely the difference is that, aluminium powder is all using FLTQ1 aluminium powders.
Embodiment 3
It includes following step to present embodiments provide a kind of highly filled NEPE propellants slurry and propellant, preparation method Suddenly:
Step 1 weighs raw material by the formula of table 3;
The PET weighed and TEGDN are mixed to get adhesive composition by step 2, by 11.2 mass parts described adhesive systems With the aluminium powder, nitrolite and function additive weighed 20 points are mixed in the case where telecentricity slurry linear velocity is 1m/s, mixing temperature is 50 DEG C Clock obtains mixture;
In step 3, the mixture that the AP weighed is added, in telecentricity slurry linear velocity 1.2m/s, mixing temperature 65 DEG C of degree mixes 40 minutes, and curing agent and remaining described adhesive system is then added, in telecentricity slurry linear velocity 1m/s, mixing Temperature 50 C mixes 20 minutes, obtains propellant slurry;;
Step 4 carries out solidification 168 hours at 50 DEG C to obtained propellant slurry, obtains solid propellant.
3 propellant formulation of table
Comparative example 3
This comparative example provides a kind of highly filled NEPE propellants slurry and propellant, preparation method and embodiment 3 is essentially identical, and uniquely the difference is that, aluminium powder is all using FLTQ1 aluminium powders.
Embodiment 4
It includes following step to present embodiments provide a kind of highly filled NEPE propellants slurry and propellant, preparation method Suddenly:
Step 1 weighs raw material by the formula of table 4;
PET, NG and TEGDN for weighing are mixed to get adhesive composition by step 2, by 11.5 mass parts described adhesives System mixes 20 minutes with the aluminium powder, nitrolite and function additive weighed in telecentricity slurry linear velocity 1m/s, 65 DEG C of mixing temperature, Mixture is obtained,
In step 3, the mixture that the AP weighed is added, in telecentricity slurry linear velocity 1.2m/s, mixing temperature 65 DEG C mix 40 minutes, and curing agent and remaining described adhesive system is then added, in telecentricity slurry linear velocity 1.2m/s, mixing Temperature 50 C mixes 20 minutes, obtains propellant slurry;
Step 4 carries out solidification 168h at 50 DEG C to obtained propellant slurry, obtains solid propellant.
4 propellant formulation of table
Comparative example 4
This comparative example provides a kind of highly filled NEPE propellants slurry and propellant, preparation method and embodiment 4 is essentially identical, and uniquely the difference is that, aluminium powder uses FLTQ1 aluminium powders.
Embodiment 5
It includes following step to present embodiments provide a kind of highly filled NEPE propellants slurry and propellant, preparation method Suddenly:
Step 1 weighs raw material by the formula of table 5;
PET, NG and TEGDN for weighing are mixed to get adhesive composition by step 2, by 11 mass parts described adhesive bodies It is to be mixed 25 minutes in telecentricity slurry linear velocity 1m/s, 55 DEG C of mixing temperature with the aluminium powder, nitrolite and function additive weighed, obtains To mixture;
In step 3, the mixture that the AP weighed is added, in telecentricity slurry linear velocity 1m/s, mixing temperature 55 DEG C mix 45 minutes, and curing agent and remaining described adhesive system is then added, in telecentricity slurry linear velocity 1m/s, mixing temperature 45 DEG C of degree mixes 20 minutes, obtains propellant slurry;
Step 4 carries out solidification 168h at 50 DEG C to obtained propellant slurry, obtains solid propellant.
5 propellant formulation of table
Comparative example 5
This comparative example provides a kind of highly filled NEPE propellants slurry and propellant, preparation method and embodiment 5 is essentially identical, and uniquely the difference is that, aluminium powder is all using FLTQ1 aluminium powders.
Embodiment 6
It includes following step to present embodiments provide a kind of highly filled NEPE propellants slurry and propellant, preparation method Suddenly:
Step 1 weighs raw material by the formula of table 6;
PET, NG and TEGDN for weighing are mixed to get adhesive composition by step 2, by 12 mass parts described adhesive bodies It is to be mixed 30 minutes in telecentricity slurry linear velocity 1.2m/s, 50 DEG C of mixing temperature with the aluminium powder, nitrolite and function additive weighed, Obtain mixture;
In step 3, the mixture that the AP weighed is added, in telecentricity slurry linear velocity 1m/s, mixing temperature 65 DEG C mix 40-50 minutes, and curing agent and remaining described adhesive system is then added, and in telecentricity slurry linear velocity 1m/s, mix It closes 40 DEG C of temperature to mix 20 minutes, obtains propellant slurry;
Step 4 carries out solidification 168h at 50 DEG C to obtained propellant slurry, obtains solid propellant.
6 propellant formulation of table
Comparative example 6
This comparative example provides a kind of highly filled NEPE propellants slurry and propellant, preparation method and embodiment 6 is essentially identical, and uniquely the difference is that, aluminium powder is all using FLTQ1 aluminium powders.
Embodiment 7
It includes following step to present embodiments provide a kind of highly filled NEPE propellants slurry and propellant, preparation method Suddenly:
Step 1 weighs raw material by the formula of table 7;
PET, NG and TEGDN for weighing are mixed to get adhesive composition by step 2, by 11.1 mass parts described adhesives System mixes 30 points with the aluminium powder, nitrolite and function additive weighed in telecentricity slurry linear velocity 1.2m/s, 65 DEG C of mixing temperature Clock obtains mixture,
In step 3, the mixture that the AP weighed is added, in telecentricity slurry linear velocity 1m/s, mixing temperature 65 DEG C mix 40-50 minutes, and curing agent and remaining described adhesive system is then added, and in telecentricity slurry linear velocity 1m/s, mix It closes temperature 50 C to mix 20 minutes, obtains propellant slurry;
Step 4 carries out solidification 168h at 50 DEG C to obtained propellant slurry, obtains solid propellant.
7 propellant formulation of table
Comparative example 7
This comparative example provides a kind of highly filled NEPE propellants slurry and propellant, preparation method and embodiment 7 is essentially identical, and uniquely the difference is that, aluminium powder is all using FLTQ1 aluminium powders.
Embodiment 8
It includes following step to present embodiments provide a kind of highly filled NEPE propellants slurry and propellant, preparation method Suddenly:
Step 1 weighs raw material by the formula of table 8;
The PET weighed and TEGDN are mixed to get adhesive composition by step 2, by 10.5 mass parts described adhesive systems It mixes 20 minutes, obtains in telecentricity slurry linear velocity 1m/s, 50 DEG C of mixing temperature with the aluminium powder, nitrolite and function additive weighed Mixture,
In step 3, the mixture that the AP weighed is added, in telecentricity slurry linear velocity 1.2m/s, mixing temperature 65 DEG C of degree mixes 50 minutes, and curing agent and remaining described adhesive system is then added, and in telecentricity slurry linear velocity 1.2m/s, mixes It closes temperature 50 C to mix 20 minutes, obtains propellant slurry;
Step 4 cures obtained propellant slurry at 50 DEG C, obtains solid propellant.
8 propellant formulation of table
Comparative example 8
This comparative example provides a kind of highly filled NEPE propellants slurry and propellant, preparation method and embodiment 8 is essentially identical, and uniquely the difference is that, aluminium powder is all using FLTQ1 aluminium powders.
Embodiment 9
It includes following step to present embodiments provide a kind of highly filled NEPE propellants slurry and propellant, preparation method Suddenly:
Step 1 weighs raw material by the formula of table 9;
PET, NG and TEGDN for weighing are mixed to get adhesive composition by step 2, by 9.5 mass parts described adhesive bodies It is to be mixed 30 minutes in telecentricity slurry linear velocity 1.2m/s, 50 DEG C of mixing temperature with the aluminium powder, nitrolite and function additive weighed, Mixture is obtained,
In step 3, the mixture that the AP weighed is added, in telecentricity slurry linear velocity 1.2m/s, mixing temperature 50 DEG C of degree mixes 40 minutes, and curing agent and remaining described adhesive system is then added, and in telecentricity slurry linear velocity 1.2m/s, mixes It closes temperature 50 C to mix 20 minutes, obtains propellant slurry;
Step 4 carries out solidification 168h at 50 DEG C to obtained propellant slurry, obtains solid propellant.
9 propellant formulation of table
Comparative example 9
This comparative example provides a kind of highly filled NEPE propellants slurry and propellant, preparation method and embodiment 9 is essentially identical, and uniquely the difference is that, aluminium powder is all using FLTQ1 aluminium powders.
Embodiment 10
It includes following step to present embodiments provide a kind of highly filled NEPE propellants slurry and propellant, preparation method Suddenly:
Step 1 weighs raw material by the formula of table 10;
PET, NG and TEGDN for weighing are mixed to get adhesive composition by step 2, by 9.5 mass parts described adhesive bodies It is to be mixed 30 minutes in telecentricity slurry linear velocity 1.2m/s, 50 DEG C of mixing temperature with the aluminium powder, nitrolite and function additive weighed, Mixture is obtained,
In step 3, the mixture that the AP weighed is added, in telecentricity slurry linear velocity 1.2m/s, mixing temperature 50 DEG C of degree mixes 40 minutes, and curing agent and remaining described adhesive system is then added, and in telecentricity slurry linear velocity 1.2m/s, mixes It closes temperature 50 C to mix 20 minutes, obtains propellant slurry;
Step 4 carries out solidification 168h at 50 DEG C to obtained propellant slurry, obtains solid propellant.
10 propellant formulation of table
Comparative example 10
This comparative example provides a kind of highly filled NEPE propellants slurry and propellant, preparation method and embodiment 10 is essentially identical, and uniquely the difference is that, aluminium powder is all using FLTQ1 aluminium powders.
Embodiment 11
It includes following step to present embodiments provide a kind of highly filled NEPE propellants slurry and propellant, preparation method Suddenly:
Step 1 weighs raw material by the formula of table 11;
PET, NG and TEGDN for weighing are mixed to get adhesive composition by step 2, by 10.5 mass parts described adhesives System mixes 30 points with the aluminium powder, nitrolite and function additive weighed in telecentricity slurry linear velocity 1.2m/s, 58 DEG C of mixing temperature Clock obtains mixture,
In step 3, the mixture that the AP weighed is added, in telecentricity slurry linear velocity 1.2m/s, mixing temperature 58 DEG C of degree mixes 40 minutes, and curing agent and remaining described adhesive system is then added, and in telecentricity slurry linear velocity 1.2m/s, mixes It closes temperature 50 C to mix 20 minutes, obtains propellant slurry;
Step 4 carries out solidification 168h at 50 DEG C to obtained propellant slurry, obtains solid propellant.
11 propellant formulation of table
Comparative example 11
This comparative example provides a kind of highly filled NEPE propellants slurry and propellant, preparation method and embodiment 11 is essentially identical, and uniquely the difference is that, aluminium powder is all using FLTQ1 aluminium powders.
In various embodiments of the present invention and comparative example, function additive by catalyst TPB, anti-aging agent (MNA and 2-NDPA according to Mass ratio is 1:2) mixing, bonding agent NPBA are 1 according to mass ratio:6:10 combinations.
Viscosity performance test is carried out to the propellant slurry that various embodiments of the present invention and comparative example obtain, to obtained solid Propellant carries out combustibility and Mechanics Performance Testing, and test result is referring to table 12.
12 propellant slurry of table and performance of propellant parameter list
It can show that the present invention has obviously Propellant Processing Characteristics by all specific embodiments listed above Improve, especially in embodiment 4, after special atomized aluminium replacement FLQT1 is added, early period, adhesive composition addition was solid constituent 11.5%, the viscosity of formula is reduced to 44.2Pa, viscosity to be reduced to 131.4Pas, technique from 388.9Pas from 214.8Pa Improvement is quite apparent, and after the special atomized aluminium of addition, is influenced to propellant burning rate (being scaled to 6.86MPa, n=0.44) maximum Value is no more than 0.38mm/s, selects the spy of different grain size and content thin respectively according to the above results in adjustment of combustion rate opening range Aluminium powder, to improve the processing performance of formula.
Unspecified part of the present invention belongs to common sense well known to those skilled in the art.

Claims (15)

1. a kind of preparation method of highly filled NEPE solid propellants slurry, which is characterized in that include the following steps:
Step 1 weighs raw material, wherein the raw material includes ammonium perchlorate, nitrolite, aluminium powder, adhesive composition, curing agent And function additive, the aluminium powder are the mixture of special atomized aluminium or special atomized aluminium and FLTQ1 aluminium powders, the grain of spy's atomized aluminium Spend d50It is 2.5 μm -13 μm;
Step 2 mixes part described adhesive system with the aluminium powder, nitrolite and function additive weighed, is mixed Object is closed, the quality of the part described adhesive system is the 9.5-12% of raw material gross mass;
In step 3, the mixture that the ammonium perchlorate weighed is added, then curing agent and remaining is added in mixing Described adhesive system, mixing, obtains propellant slurry.
2. the preparation method of highly filled NEPE solid propellants slurry according to claim 1, which is characterized in that step Raw material described in rapid 1 includes following content of component:
29-45 parts of ammonium perchlorate, 17-30 parts of nitrolite, 17-18 parts of aluminium powder, 19-22 parts of adhesive composition, curing agent 0.5- 0.8 part and 0.6-1.2 parts of function additive.
3. the preparation method of highly filled NEPE solid propellants slurry according to claim 2, which is characterized in that institute The granularity for stating ammonium perchlorate is 120-400 μm.
4. highly filled NEPE solid propellants according to claim 2, which is characterized in that the grain of the nitrolite Degree is 80-110 μm.
5. the preparation method of highly filled NEPE solid propellants slurry according to claim 1, which is characterized in that institute The granularity for stating special atomized aluminium is 2.5-6 μm.
6. special according to the preparation method of the highly filled NEPE solid propellants slurry of claim 1-5 any one of them Sign is:Mass percent of the spy's atomized aluminium in the NEPE solid propellants is 3%-5%.
7. the preparation method of highly filled NEPE solid propellants slurry according to claim 1, it is characterised in that:Institute The granularity for stating special atomized aluminium is 6.0-13 μm.
8. the preparation method of the highly filled NEPE solid propellants slurry according to claim 1-4 or 7, feature exist In:Mass percent of the spy's atomized aluminium in the NEPE solid propellants is 5%-18%.
9. the preparation method of highly filled NEPE solid propellants slurry according to claim 1, it is characterised in that:Institute It includes adhesive and plasticizer to state adhesive composition, and the mass ratio of the plasticizer and adhesive is (1.5~2.0):1.
10. the preparation method of highly filled NEPE solid propellants slurry according to claim 9, it is characterised in that: Described adhesive is terminal hydroxy group Ethylene Oxide-Tetrahydrofuran Copolyether;The plasticizer is nitroglycerine, triethylene-glycol two One in nitrate, trimethylolethane trimethacrylate nitrate, diglycol dinitrate or 1,2,4- butanetriol trinitrate Kind or more than one combinations.
11. the preparation method of highly filled NEPE solid propellants slurry according to claim 1, it is characterised in that: Step 2 by part described adhesive system and the aluminium powder, nitrolite and the function additive that weigh telecentricity slurry linear velocity be 1~ 1.2m/s, mixing temperature mix 20-30 minutes under the conditions of being 50~65 DEG C.
12. the preparation method of highly filled NEPE solid propellants slurry according to claim 11, it is characterised in that: In the mixture that the ammonium perchlorate weighed is added step 3, it is 1~1.2m/s, mixes temperature in telecentricity slurry linear velocity Degree is to be mixed at 50~65 DEG C 40-50 minutes, and curing agent and remaining described adhesive system is then added and starches linear speed in telecentricity Degree is 1~1.2m/s, mixing temperature is to be mixed 15-25 minutes at 40~50 DEG C.
13. the preparation method of highly filled NEPE solid propellants slurry according to claim 1, it is characterised in that: The curing agent is the combination of one or both of toluene di-isocyanate(TDI) or modified six methine polyisocyanates.
14. the propellant slurry prepared by any one of claim 1-13.
15. a kind of preparation method of solid propellant, which is characterized in that include the following steps:
Step 1 weighs raw material, wherein the raw material includes ammonium perchlorate, nitrolite, aluminium powder, adhesive composition, curing agent And function additive, the aluminium powder are the mixture of special atomized aluminium or special atomized aluminium and FLTQ1 aluminium powders, the grain of spy's atomized aluminium Spend d50It is 2.5 μm -13 μm;
Step 2 mixes part described adhesive system with the aluminium powder, nitrolite and function additive weighed, the portion It is the 9.5-12% of raw material gross mass to divide the quality of described adhesive system, obtains mixture;
Step 3 will mix in the mixture that the ammonium perchlorate weighed is added, and curing agent and remaining institute is then added Adhesive composition mixing is stated, solidification obtains propellant.
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CN111908988A (en) * 2020-06-30 2020-11-10 湖北航天化学技术研究所 Combined functional additive, preparation method thereof and application thereof in propellant
CN115677438A (en) * 2022-10-28 2023-02-03 东南大学 NEPE propellant slurry formula for melt extrusion molding 3D printing and preparation method
CN116655444A (en) * 2023-06-05 2023-08-29 湖北航天化学技术研究所 High-solid-content low-viscosity thermoplastic propellant and preparation method thereof
CN116789507A (en) * 2023-06-21 2023-09-22 湖北航天化学技术研究所 High-solid-content solid propellant and preparation method thereof

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CN102471175A (en) * 2009-07-01 2012-05-23 Sme公司 Method for producing solid composite aluminized propellants, and solid composite aluminized propellants
CN105801327A (en) * 2016-02-29 2016-07-27 湖北三江航天江河化工科技有限公司 Composite solid propellant and preparation method thereof

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US3506713A (en) * 1965-12-02 1970-04-14 Us Army Poly 1,4-bis(bis(difluoroamino)methyl)-3,5-dioxa-2-hydroxymethylpentane
CN102471175A (en) * 2009-07-01 2012-05-23 Sme公司 Method for producing solid composite aluminized propellants, and solid composite aluminized propellants
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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111908988A (en) * 2020-06-30 2020-11-10 湖北航天化学技术研究所 Combined functional additive, preparation method thereof and application thereof in propellant
CN111908988B (en) * 2020-06-30 2021-09-07 湖北航天化学技术研究所 Combined functional additive, preparation method thereof and application thereof in propellant
CN115677438A (en) * 2022-10-28 2023-02-03 东南大学 NEPE propellant slurry formula for melt extrusion molding 3D printing and preparation method
CN115677438B (en) * 2022-10-28 2024-05-31 东南大学 NEPE propellant slurry formula for melt extrusion molding 3D printing and preparation method
CN116655444A (en) * 2023-06-05 2023-08-29 湖北航天化学技术研究所 High-solid-content low-viscosity thermoplastic propellant and preparation method thereof
CN116655444B (en) * 2023-06-05 2024-04-19 湖北航天化学技术研究所 High-solid-content low-viscosity thermoplastic propellant and preparation method thereof
CN116789507A (en) * 2023-06-21 2023-09-22 湖北航天化学技术研究所 High-solid-content solid propellant and preparation method thereof

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