CN106116995A - The method press-fiting aluminum composition modeling powder is prepared in a kind of aqueous suspension - Google Patents
The method press-fiting aluminum composition modeling powder is prepared in a kind of aqueous suspension Download PDFInfo
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- CN106116995A CN106116995A CN201610478426.7A CN201610478426A CN106116995A CN 106116995 A CN106116995 A CN 106116995A CN 201610478426 A CN201610478426 A CN 201610478426A CN 106116995 A CN106116995 A CN 106116995A
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- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B33/00—Compositions 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
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- 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
- C06B23/009—Wetting agents, hydrophobing agents, dehydrating agents, antistatic additives, viscosity improvers, antiagglomerating agents, grinding agents and other additives for working up
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- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B45/00—Compositions or products which are defined by structure or arrangement of component of product
- C06B45/18—Compositions or products which are defined by structure or arrangement of component of product comprising a coated component
- C06B45/30—Compositions or products which are defined by structure or arrangement of component of product comprising a coated component the component base containing an inorganic explosive or an inorganic thermic component
- C06B45/32—Compositions or products which are defined by structure or arrangement of component of product comprising a coated component the component base containing an inorganic explosive or an inorganic thermic component the coating containing an organic compound
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Abstract
The invention discloses a kind of aqueous suspension and prepare the method press-fiting aluminum composition modeling powder.The method press-fits aluminum composition modeling powder by using aqueous suspension comminution granulation to prepare under the conditions of 60～70 DEG C after anticipating superfine aluminium power and explosive surface again.Present invention is especially suited for preparation containing the sensitive explosive such as CL 20 and HMX and particle diameter be 50nm～5um aluminium powder press-fit aluminum composition modeling powder.The present invention provides aqueous suspension to prepare the method press-fiting aluminum composition modeling powder, and research and application for high energy aluminum composition provide necessary material guarantee and technical support.
Description
Technical field
The present invention relates to energetic material field, be specifically related to a kind of preparation method press-fiting aluminum composition modeling powder.
Background technology
Press-fiting aluminum composition is the one press-fiting type polymer bonding explosive.It by high explosive, aluminium powder and other add
Add agent and be prepared as modeling powder granule with binding agent, then process through compressing.High owing to press-fiting aluminum composition density, energy
Amount relatively other type charge is high, and its acting ability being greatly improved ammunition and damage effect have in a lot of warhead charges
Important application prospect, is therefore paid high attention to by association area research worker in recent years.
But, the preparation press-fiting aluminum composition modeling powder is the major issue that restriction press-fits aluminum composition development.Logical
In the case of Chang, the modeling powder press-fiting type polymer bonding explosive without aluminum can be prepared by water suspension method pelletize.But the method
It is not suitable for preparation and press-fits aluminum composition modeling powder.Because aluminium powder (especially superfine aluminium power) is very easy to be released hydrogen by water oxidation
Gas and substantial amounts of heat, considerably increase the danger of operation.The aluminium powder of reaction generates aluminium hydroxide, and aluminium hydroxide is not only to containing aluminum
Explosive energy output not contribution, and aluminium powder releasing in detonation is reacted can be reduced can efficiency.For this problem, employing is pinched
Close extrusion molding preparation press-fiting aluminum composition modeling powder is a technological approaches.Will the compositions such as explosive, aluminium powder, binding agent direct
Batch mixing in kneader, is kneaded into pasty mass and extrudes granulating through banded extruder again after adding solvent.Avoid during whole
Aluminium powder touches water.Picatinny factory of the U.S. has used kneading extrusion molding to be prepared for HMX base aluminum composition, effectively solves
Determine and press-fited problem (Paul Anderson, the et that in the preparation of aluminum composition modeling powder, aluminium powder reacts with water
al.Development,optimization,and application of combined effects explosives,
NDIA Insensitive Munitions&Energetic Materials Technology Symposium,2009).But
It is to mediate the limitation of extrusion molding own big.Many high explosive sensitivity are high, and friction, shock, electrostatic etc. are stimulated sensitivity, mediate
Extrusion molding operation rubbing, clashes into and be likely to result in explosive charge, containing containing press-fiting of sensitive explosive so being not suitable for preparation
Al explosive modeling powder.
Preparation another solution route press-fiting aluminum composition modeling powder containing sensitive explosive is to use aqueous suspension pelletize
The technological process of method.Use other solvent to replace aqueous medium, referred to as non-aqueous media suspension comminution granulation.Such as, the U.S. gram spit of fland
Buddhist nun factory uses a kind of medium to substitute water, and this medium does not reacts with aluminium powder.Ke Tingni factory utilizes the method to be prepared for
PAX-3 (HMX/CAB/plasticizer/Al), PAX-28 (RDX/DNAN/AP/Al) and PAX-30 (HMX/CAB/
Etc. plasticizer/Al) press-fit aluminum composition modeling powder (Paul Anderson, et al.Development,
optimization,and application of combined effects explosives,NDIA Insensitive
Munitions&Energetic Materials Technology Symposium,2009).But the preparation of this non-aqueous media is made
Type powder has a problem in that cost is high, non-aqueous media recovery is difficult.The Liu Yong of China Engineering Physics Research Institute just waits with ethanol for replacing
The medium of Dai Shui, is prepared for a series of press-fiting aluminum composition modeling powder (Chinese invention patent with RDX, HMX as base
ZL201310181105.7).But, this method yet suffers from deficiency and includes that high cost and granulation process control difficulty.
All promote research worker to develop the method that in water, preparation press-fits aluminum composition modeling powder further based on problem above.
AUS maneuver of tanks vehicle-weapon Research Development Engineering Center advances the research worker cooperation research and development of company with thiorubber.
Novel C L-20 base aluminum composition such as PAX-29 (15%Al, 77%CL-20,3.2%CAB, 4.8%BDNPA/F) and PAX-11
(15%Al, 79%CL-20,2.4%CAB, 3.6%BDNPA/F) modeling powder uses aqueous suspension to prepare.It is in order to prevent pelletize
In journey, aluminium powder reacts with water, selects the bigger aluminium powder of particle diameter, and carries out modeling powder under the conditions of 30 DEG C and prepare.The method exists
Problem is that temperature is too low, and in granulation process, the solvent in binder solution is the most volatile, causes the compositions pole of explosive and aluminium powder
Difficulty is agglomerated into grain, disperses and forms modeling powder granule.
In sum, the not enough serious application restricting high energy aluminum composition of aluminum composition modeling powder preparation method is press-fited.
Therefore the preparation method press-fiting aluminum composition modeling powder that development is new is needed badly.
Summary of the invention
[solving the technical problem that]
Present invention aim to address above-mentioned prior art problem, it is provided that a kind of aqueous suspension preparation press-fits aluminum composition moulding
The method of powder.The method is suitable for the preparation that explosive sensitivity is high, be unsuitable for high energy aluminum composition modeling powder prepared by kneading method, and is
Research and the application of high energy aluminum composition provide necessary material guarantee and technical support.
[technical scheme]
In order to reach above-mentioned technique effect, the present invention takes techniques below scheme:
The method press-fiting aluminum composition modeling powder is prepared in a kind of aqueous suspension, and it comprises the following steps:
A, the surface preparation of aluminium powder
First, it is that the ratio of 1g:5mL adds solvent in the aluminium powder of vacuum drying in aluminium powder and solvent quality volume ratio,
Stir 30 minutes under ultrasound condition after being then heated to 80 DEG C；Then in mixture, add dibutyl tin laurate and first
Phenylene diisocyanate, the addition of described dibutyl tin laurate and toluene di-isocyanate(TDI) is respectively with the mass ratio of aluminium powder
0.5:50 and 2:50, mixing post-heating backflow 2h；Continuously add glycidyl azide polymer and be heated to reflux 2h, described poly-nitrine
Glycidyl ether addition is 1/5th of aluminium powder quality；After being finally cooled to room temperature, sucking filtration has also rinsed filter with solvent
Cake 3～5 times, i.e. obtain the aluminium powder of surface preparation after vacuum drying；
Described solvent can be anhydrous acetonitrile, ethyl acetate or butyl acetate.
B, the surface preparation of explosive
Explosive is joined in the solvent containing coating material, after ultrasonic and mechanical agitation is disperseed 5 minutes, explosive is taken out
Filter, drying.
C, aqueous suspension comminution granulation
The coating material cladding that the aluminium powder of the surface preparation obtained through processing of step A and the process of step B are obtained
Explosive is added to the water, and heated and stirred is uniform；Then drip the binder solution prepared, when binder solution be added drop-wise to three/
When two, to this mixed solution spray into appropriate water-dispersible uniformly after, continue to drip remaining binder solution, drip complete
Appropriate water-dispersible, flushing is sprayed into after 10min；Then sucking filtration, vacuum drying, obtains described aqueous suspension preparation and press-fits containing aluminum fried
Medicine modeling powder.
The present invention further technical scheme, in step, described solvent is butyl acetate.
The present invention further technical scheme, in step, described aluminium powder is ball aluminum powder, and its particle size range is
0.05～50 μm.The aluminium powder of the present invention is superfine aluminium power.
The present invention further technical scheme, described aluminium powder particle size range preferably 0.05～5 μm.
The present invention further technical scheme, in stepb, explosive is high sensitivity explosive, it is CL-20, HMX,
One or more compositionss in RDX, LLM-105, TATB, the particle diameter of described explosive is 1～120 μm.
The present invention further technical scheme, in stepb, the described solvent containing coating material refers to polyurethane
It is dissolved in dichloroethanes and forms the solvent that concentration is 0.25～1.0wt%.
The present invention further technical scheme, described high polymer binder is being total to of vinylidene and CTFE
Polymers or polyurethane polymer binding agent.
The present invention further technical scheme, is in step C, the aluminum of the surface preparation that described step A obtains
The explosive of coating material cladding and the mass ratio of binding agent that powder, step B obtain are 10～30:55～90:5～10.
The present invention further technical scheme, in step C, it is 60～70 DEG C that described being heated to be is heated to temperature.
The present invention further technical scheme, in step C, the drop rate of described binder solution is 3mL/min.
Will be described in detail the present invention below.
First the present invention carries out surface process to aluminium powder, after placing aluminium powder contact water, oxidation reaction, and the present invention occurs
Do not have explosive property influential solvent that aluminium powder surface is processed by using, utilize anhydrous acetonitrile or ethyl acetate, acetic acid fourth
Ester dispersion aluminium powder, considers environment and the protection of personnel and reaction effect, the present invention preferred butyl acetate dispersion aluminum
Powder；Then on the isocyanate groups and aluminium powder of catalysis Toluene diisocyanate one end of dibutyl tin laurate
Hydroxyl reaction, the isocyanate groups of the toluene di-isocyanate(TDI) other end reacts with glycidyl azide polymer again.Due to poly-folded
The hydrophobicity of nitrogen glycidyl ether changes the hydrophobicity on aluminium powder surface and the mechanical property of aluminum composition.Mesh due to this aluminium powder
Be to prepare aluminum composition modeling powder, too much glycidyl azide polymer can make aluminium powder conglomeration be difficult to dispersion, therefore, aluminum
The content of the glycidyl azide polymer on powder surface needs suitable control.And the present invention is in the step of aluminium powder surface modification
Needing to control the usage amount of solvent, its principle is to guarantee that aluminium powder reduces the use of organic solvent in the case of the most scattered as far as possible
Amount, is possible not only to reduce cost, further mass production.Due to the fact that first aluminium powder having been carried out surface changes
Property, therefore carries out aqueous suspension comminution granulation and prepares in the step of modeling powder and can select to be heated to 60～70 DEG C, and this temperature is high energy
Press-fiting an important control parameter prepared by aluminum composition modeling powder, first this temperature does not affect the same of high energy hypersensitivity explosive
Time the volatilization of solvent in binder solution when also helping aqueous suspension pelletize, thus the formation of beneficially explosive molding powder.
Another key technology of the present invention is the pretreatment to explosive surface.The most surface treated explosive is exploding containing aluminum
Medicine modeling powder effectively can not be coated with by binding agent, poor mechanical property.Explosive surface preparation can be improved explosive and binding agent
Interaction, thus improve the mechanical property of aluminum composition.During the surface preparation of explosive, blasting explosive granules surface quilt
Minimal amount of coating material cladding (< 0.05%).Described coating material is polyurethane, because explosive surface is had by polyurethane
Stronger bonding cladding, and the sensitivity of explosive can be reduced, to improving, safety is the most favourable；Dissolve the solution of coating material
Require insoluble explosive crystal, optimal with dichloroethanes.
Ultrasonic described in step A of the present invention and step B refer to power be 400～500W, frequency of vibration be 15～
20kHz, ultrasonic time is carry out under conditions of 10～25min ultrasonic.This ultrasound condition should alternative condition the warmest
With and mix quick condition, to ensure in modeling powder preparation process that raw material can be sufficiently mixed uniform preparation process peace simultaneously
Entirely.In the present invention, the drying described in step B and step C is to dry at being 50～60 DEG C in temperature.
[beneficial effect]
The present invention compared with prior art, has a following beneficial effect:
The preparation method of the present invention is especially suitable for that preparation is high containing the explosive sensitivity such as CL-20, HMX, be unsuitable for kneading method prepares
High energy aluminum composition modeling powder.Utilize water suspension method to prepare high energy aluminum composition modeling powder, prilling temperature is set in 60～
The temperature of solvent volatilization in 70 DEG C of applicable binder solutions so that explosive and aluminium powder are by well-bonded cladding granulating, and guarantee aluminum
Powder will not aoxidize in water.The present invention prepare to press-fit aluminum composition modeling powder granule uniform, bulk density is high, powder column
Mechanical property is good, and in component, the content of activated aluminum is high, and explosive energy is high
Accompanying drawing explanation
Fig. 1 is the photo in kind obtaining press-fiting aluminum composition modeling powder prepared by the present invention.
Detailed description of the invention
Below in conjunction with embodiments of the invention, the invention will be further elaborated.
Embodiment 1:
A, the surface preparation of aluminium powder
First, in 500mL three-neck flask, add 250mL butyl acetate, be added thereto to the ultra-fine aluminum of 50g vacuum drying
Powder (mean diameter 50nm).Stir 30 minutes under conditions of ultrasonic after being heated to 80 DEG C, add 0.5g February to three-neck flask
Dilaurylate, is subsequently adding 2.0g toluene di-isocyanate(TDI) (TDI), refluxes under the conditions of 80 DEG C.Add after 2 hours
10.0g glycidyl azide polymer, and backflow stopped heating after 2 hours under the conditions of 80 DEG C, temperature will be produced after being reduced to room temperature
Thing sucking filtration, collects filter cake after rinsing filter cake 3～5 times with butyl acetate, is put in vacuum drying oven drying.I.e. obtain pre-treating aluminium
Powder, wherein the glycidyl azide polymer content on aluminium powder surface is 2.0%.
Water suspension method preparation press-fits the critical process of aluminum composition modeling powder and is intended to explosive and aluminium powder are pre-added to water
In, then dripping binder solution, the temperature of water to be set to 60～70 DEG C, and the solvent in binder solution could volatilize, from
And binding agent is coated on explosive and aluminium powder.First the pretreated aluminium powder of the present embodiment is tested in the water-bath at 70 DEG C
Stability in water, result shows, only has the aluminium powder of 1.5wt.% to be aoxidized by water when 60 minutes.
B, the surface preparation of explosive
It is in the dichloroethanes that 0.5wt% contains polyurethane that explosive CL-20 joins concentration, ultrasonic and mechanical agitation dispersion
After 5 minutes, sucking filtration, drying, obtain blasting explosive granules surface by the coating material cladding of very small amount (< 0.05%).
C, aqueous suspension comminution granulation
By the aluminium powder of the surface preparation obtained through processing of step A and the coating material cladding obtained through the process of step B
Explosive CL-20 be added to the water, and be heated to 60 DEG C and stir；Polymeric binder (Estane) is dissolved into dichloroethanes
Forming concentration in solvent is the solution for later use of 5.0wt%；Then dripping the binder solution prepared, rate of addition is 3mL/
Min, in the process, when binder solution drips 2/3, explosive crystal grain and modified aluminium powder are coated with by binding agent and start to reunite
Granulating, slowly sprays into distilled water with wash bottle to pelletize still wall so that the material dispersion of reunion, stops after being dispersed into uniform little granule
Only adding distilled water, start to drip remaining binder solution after stirring a period of time, binder solution drips complete 10 minutes
After, spray into appropriate distilled water flushing pelletize still inwall；Then pour in pallet after material sucking filtration, and in vacuum drying oven 60
DEG C dry i.e. obtain after 6h being dried press-fit aluminum composition modeling powder product.The performance of its modeling powder is as shown in table 1.Wherein, described
The explosive of coating material cladding and the mass ratio of binding agent that the aluminium powder of the surface preparation that step A obtains, step B obtain are
10:80:10.
Embodiment 2
A, the surface preparation of aluminium powder
First, in 500mL three-neck flask, add 250mL anhydrous acetonitrile, be added thereto to the ultra-fine aluminum of 50g vacuum drying
Powder (mean diameter 1 μm).Stir 30 minutes under conditions of ultrasonic after being heated to 80 DEG C, add 0.5g bis-Laurel to three-neck flask
Acid dibutyl tin, is subsequently adding 2.0g toluene di-isocyanate(TDI) (TDI), refluxes under the conditions of 80 DEG C.10.0g is added after 2 hours
Glycidyl azide polymer, and backflow stopped heating after 2 hours under the conditions of 80 DEG C, product is taken out after being reduced to room temperature by temperature
Filter, collects filter cake after rinsing filter cake 3～5 times with anhydrous acetonitrile, is put in vacuum drying oven drying.I.e. obtain pretreatment aluminium powder, its
The glycidyl azide polymer content on middle aluminium powder surface is 0.8%.
Water suspension method preparation press-fits the critical process of aluminum composition modeling powder and is intended to explosive and aluminium powder are pre-added to water
In, then dripping binder solution, the temperature of water to be set to 60～70 DEG C, and the solvent in binder solution could volatilize, from
And binding agent is coated on explosive and aluminium powder.Therefore the water-bath at 70 DEG C tests the pretreated aluminium powder of the present embodiment at water
In stability, result shows, has the aluminium powder of 1.5wt.% to be aoxidized by water when 60 minutes.
B, the surface preparation of explosive
It is in 0.5% dichloroethanes containing polyurethane that explosive HMX joins concentration, and ultrasonic and mechanical agitation disperses 5 points
Zhong Hou, sucking filtration, drying；The blasting explosive granules surface obtained is by the coating material cladding of very small amount (< 0.05%).
C, aqueous suspension comminution granulation
The explosive HMX of the coating material cladding that the aluminium powder of surface preparation step A obtained and step B obtain adds
In water, and it is heated to 70 DEG C and stirs；Polymeric binder (vinylidene and CTFE 1:1 copolymer) is dissolved into
Forming concentration in ethyl acetate solvent is the solution for later use of 5.0wt%；Then the binder solution prepared, rate of addition are dripped
For 3mL/min, in the process, when binder solution drips 2/3, explosive crystal grain and modified aluminium powder are coated with by binding agent and open
Beginning reunion granulating, slowly sprays into distilled water with wash bottle to pelletize still wall so that the material dispersion of reunion, is dispersed into the least
Stopping adding distilled water after Li, start to drip remaining binder solution after stirring a period of time, binder solution dropping is complete
After 10 minutes, spray into appropriate distilled water flushing pelletize still inwall.Then pour in pallet after material sucking filtration, and dry in vacuum
In case 60 DEG C dry i.e. obtain after 6h being dried press-fit aluminum composition modeling powder product, product is as it is shown in figure 1, the performance of its modeling powder
As shown in table 1.The explosive of coating material that the aluminium powder of the surface preparation that described step A obtains, step B obtain cladding and viscous
The mass ratio of knot agent is 25:70:5.
Modeling powder granule prepared by the present embodiment is uniform, spherical in shape, bulk density 0.80g/cm3；In the modeling powder of preparation
It is 98.2% that activated aluminum accounts for the proportion of aluminium powder.The grain density of the modeling powder compacting prepared by utilization is 1.980g/cm3, quality
Quick-fried heat reaches 7907J/g (1.94 times of TNT equivalents).The Compressive Mechanical intensity of powder column is 16.0MPa, and compression failure strain is up to
3.3%.
Embodiment 3
A, the surface preparation of aluminium powder
First, in 500mL three-neck flask, add 250mL butyl acetate, be added thereto to the ultra-fine aluminum of 50g vacuum drying
Powder (mean diameter 5 μm), stirs 30 minutes after being heated to 80 DEG C under conditions of ultrasonic, adds 0.5g bis-Laurel to three-neck flask
Acid dibutyl tin, is subsequently adding 2.0g toluene di-isocyanate(TDI) (TDI), refluxes under the conditions of 80 DEG C.10.0g is added after 2 hours
Glycidyl azide polymer, and backflow stopped heating after 2 hours under the conditions of 80 DEG C, product is taken out after being reduced to room temperature by temperature
Filter, collects filter cake after rinsing filter cake 3～5 times with butyl acetate, is put in vacuum drying oven drying, i.e. obtains pretreatment aluminium powder, its
The glycidyl azide polymer content on middle aluminium powder surface is 0.5%.
Water suspension method preparation press-fits the critical process of aluminum composition modeling powder and is intended to explosive and aluminium powder are pre-added to water
In, then dripping binder solution, the temperature of water to be set to 60～70 DEG C, and the solvent in binder solution could volatilize, from
And binding agent is coated on explosive and aluminium powder.First the pretreated aluminium powder of the present embodiment is tested in the water-bath at 70 DEG C
Stability in water, result shows, has the aluminium powder of 0.5wt.% to be aoxidized by water when 60 minutes.
B, the surface preparation of explosive
It is 0.25% dichloroethanes containing polyurethane that explosive HMX and LLM-105 (mass ratio 50:20) joins concentration
In, after ultrasonic and mechanical agitation is disperseed 5 minutes, by explosive sucking filtration, drying, the blasting explosive granules surface obtained by very small amount (<
0.05%) coating material cladding.
C, aqueous suspension comminution granulation
Exploding of the coating material cladding that the aluminium powder of surface preparation processing of step A obtained and the process of step B obtain
Medicine is added to the water, and is heated to 70 DEG C and stirs；By polymeric binder (vinylidene and CTFE 1:3 copolymer)
Being dissolved in ethyl acetate solvent formation concentration is the solution for later use of 5.0wt%；Then drip the binder solution prepared, drip
Acceleration is 3mL/min, and in the process, when binder solution drips 2/3, explosive crystal grain and modified aluminium powder are by binding agent bag
Cover and start granulating of reuniting, slowly spraying into distilled water with wash bottle to pelletize still wall so that the material dispersion of reunion, being dispersed into uniformly
Little granule after stop add distilled water, stirring a period of time after start to drip remaining binder solution, binder solution drips
After adding complete 10 minutes, spray into appropriate distilled water flushing pelletize still inwall.Then pour in pallet after material sucking filtration, and
In vacuum drying oven 60 DEG C dry i.e. obtain after 6h being dried press-fit aluminum composition modeling powder product, the performance of its modeling powder such as table 1 institute
Show.
The modeling powder granule of the present embodiment is uniform, spherical in shape；In the modeling powder of preparation, activated aluminum accounts for the proportion of aluminium powder and is
98.5%.The explosive of the coating material cladding that the aluminium powder of the surface preparation that described step A obtains, step B obtain and bonding
The mass ratio of agent is 13:80:7.
Embodiment 4
A, the surface preparation of aluminium powder
First, in 500mL three-neck flask, add 250mL ethyl acetate, be added thereto to the ultra-fine aluminum of 50g vacuum drying
Powder (mean diameter 5 μm), stirs 30 minutes after being heated to 80 DEG C under conditions of ultrasonic, adds 0.5g bis-Laurel to three-neck flask
Acid dibutyl tin, is subsequently adding 2.0g toluene di-isocyanate(TDI) (TDI), refluxes under the conditions of 80 DEG C.10.0g is added after 2 hours
Glycidyl azide polymer, and backflow stopped heating after 2 hours under the conditions of 80 DEG C, product is taken out after being reduced to room temperature by temperature
Filter, collects filter cake after ethyl acetate rinse filter cake 3～5 times, is put in vacuum drying oven drying, i.e. obtains pretreatment aluminium powder, its
The glycidyl azide polymer content on middle aluminium powder surface is 0.5%.
Water suspension method preparation press-fits the critical process of aluminum composition modeling powder and is intended to explosive and aluminium powder are pre-added to water
In, then dripping binder solution, the temperature of water to be set to 60～70 DEG C, and the solvent in binder solution could volatilize, from
And binding agent is coated on explosive and aluminium powder.First the pretreated aluminium powder of the present embodiment is tested in the water-bath at 70 DEG C
Stability in water, result shows, has the aluminium powder of 0.2wt.% to be aoxidized by water when 60 minutes.
B, the surface preparation of explosive
It is that in 1.0% dichloroethanes containing polyurethane, ultrasonic and mechanical agitation is divided that explosive RDX and TATB joins concentration
After dissipating 5 minutes, sucking filtration, drying；The blasting explosive granules surface obtained is by the coating material cladding of very small amount (< 0.05%).
C, aqueous suspension comminution granulation
The explosive of the coating material cladding that the aluminium powder of surface preparation step A obtained and step B obtain adds water
In, and be heated to 70 DEG C and stir；Polymeric binder (vinylidene and CTFE 1:4 copolymer) is dissolved into second
Forming concentration in acetoacetic ester solvent is the solution for later use of 5.0wt%；Then dripping the binder solution prepared, rate of addition is
3mL/min, in the process, when binder solution drips 2/3, explosive crystal grain and modified aluminium powder are coated with by binding agent and start
Reunion granulating, slowly sprays into distilled water with wash bottle to pelletize still wall so that the material dispersion of reunion, is dispersed into uniform little granule
Rear stopping adds distilled water, starts to drip remaining binder solution, binder solution dropping complete 10 after stirring a period of time
After minute, spray into appropriate distilled water flushing pelletize still inwall.Then pour in pallet after material sucking filtration, and at vacuum drying oven
In 60 DEG C dry i.e. obtain after 6h being dried press-fit aluminum composition modeling powder product, the performance of its modeling powder is as shown in table 1.
The modeling powder granule of the present embodiment is uniform, spherical in shape；In the modeling powder of preparation, activated aluminum accounts for the proportion of aluminium powder and is
99.5%.The explosive of the coating material cladding that the aluminium powder of the surface preparation that described step A obtains, step B obtain and bonding
The mass ratio of agent is 12:80:8.
Comparative example 1
The present embodiment is the comparative example as embodiment 2, illustrates that explosive is directly used in aqueous suspension without surface preparation
Method prepares the mechanical property of modeling powder.
A, aluminium powder surface preparation
First, in 500mL three-neck flask, add 250mL anhydrous acetonitrile, be added thereto to the ultra-fine aluminum of 50g vacuum drying
Powder (mean diameter 1 μm), stirs 30 minutes after being heated to 80 DEG C under conditions of ultrasonic, adds 0.5g bis-Laurel to three-neck flask
Acid dibutyl tin, is subsequently adding 2.0g toluene di-isocyanate(TDI) (TDI), refluxes under the conditions of 80 DEG C.10.0g is added after 2 hours
Glycidyl azide polymer, and backflow stopped heating after 2 hours under the conditions of 80 DEG C, product is taken out after being reduced to room temperature by temperature
Filter, collects filter cake after rinsing filter cake 3～5 times with anhydrous acetonitrile, is put in vacuum drying oven drying.I.e. obtain pretreatment aluminium powder, its
The glycidyl azide polymer content on middle aluminium powder surface is 0.8%.
Water suspension method preparation press-fits the critical process of aluminum composition modeling powder and is intended to explosive and aluminium powder are pre-added to water
In, then dripping binder solution, the temperature of water to be set to 60～70 DEG C, and the solvent in binder solution could volatilize, from
And binding agent is coated on explosive and aluminium powder.First to test this comparative example pretreated for the water-bath at 70 DEG C
Aluminium powder stability in water, result shows, has the aluminium powder of 1.5wt.% to be aoxidized by water when 60 minutes.
B, explosive surface preparation
In the present embodiment, explosive HMX does not does pretreatment in surface.
C, aqueous suspension comminution granulation
The aluminium powder of surface preparation step A obtained is added to the water with explosive HMX, and is heated to 70 DEG C and stirs；
Polymeric binder (vinylidene and CTFE 1:1 copolymer) is dissolved in ethyl acetate solvent formation concentration is
The solution for later use of 5.0wt%；Then dripping the binding agent solvent prepared, rate of addition is 3mL/min, in the process, when
When binder solution drips 2/3, explosive crystal grain and modified aluminium powder are coated with by binding agent and start granulating of reuniting, with wash bottle to pelletize
Still wall slowly sprays into distilled water so that the material dispersion of reunion, stops adding distilled water, stirring after being dispersed into uniform little granule
Start to drip remaining binder solution after a period of time, after binder solution drips complete 10 minutes, spray into appropriate distillation
Water rinses pelletize still inwall.Then pour in pallet after material sucking filtration, and i.e. done after 60 DEG C of baking 6h in vacuum drying oven
Dry press-fits aluminum composition modeling powder product, the aluminium powder of the surface preparation that described explosive, processing of step A obtain and binding agent
Mass ratio is 70:25:5.The performance of its modeling powder is as shown in table 1.
Modeling powder granule prepared by this comparative example is uniform, spherical in shape, bulk density 0.72g/cm3；The moulding of preparation
In powder, activated aluminum accounts for the proportion of aluminium powder is 98.0%.The grain density of the modeling powder compacting prepared by utilization is 1.975g/cm3,
The Compressive Mechanical intensity of powder column is 11.0MPa, and compression failure strain is 1.8%.
Visible, compare with embodiment 2, if HMX surface free pretreatment, the aluminum composition modeling powder bulk density of preparation and
The grain density of compacting is the most on the low side, and the mechanical property of powder column is also greatly reduced.To explosive and aluminium powder in this explanation the inventive method
Surface all carries out pretreatment and can be effectively improved and prepare the mechanical property of powder column after the bulk density of modeling powder and molding.
Comparative example 2
The present embodiment is the comparative example as embodiment 2, illustrates that aluminium powder cannot be used directly for water without surface preparation
Suspension method prepares modeling powder.
In the present embodiment, aluminium powder mean diameter is 1 μm.Surface free glycidyl azide polymer processes.
Water suspension method preparation press-fits the critical process of aluminum composition modeling powder and is intended to explosive and aluminium powder are pre-added to water
In, then dripping binder solution, the temperature of water to be set to 60～70 DEG C, and the solvent in binder solution could volatilize, from
And binding agent is coated on explosive and aluminium powder.First pretreatment aluminium powder stablizing in water is tested in the water-bath at 70 DEG C
Property, result shows, has the aluminium powder of 46.6wt.% to be aoxidized by water when 60 minutes.In the process, substantial amounts of hydrogen is had to release.Cause
This, it is contemplated that safety and the low-activity of untreated aluminium powder, this aluminium powder cannot be used directly for water suspension method and prepares explosive molding powder.
Above-described embodiment 1～4 and the performance press-fiting aluminum composition modeling powder of comparative example 1 preparation as shown in table 1:
Table 1 embodiment 1～4 and the performance press-fiting aluminum composition modeling powder of comparative example 1 preparation
As can be seen here, its granule of aluminum composition modeling powder that press-fits utilizing the present invention to prepare is uniform-spherical.Utilize
In the modeling powder that the preparation method of the present invention prepares, effective activity of aluminium powder is all more than 98%, the energy that explosive detonation produces
High.And it is high to prepare aluminum composition modeling powder bulk density by the method for the present invention, and compacting powder column mechanical property is excellent.The present invention
Research and application for high energy aluminum composition provide necessary material guarantee and technical support.
Although reference be made herein to invention has been described for the explanatory embodiment of the present invention, and above-described embodiment is only this
Bright preferably embodiment, embodiments of the present invention are also not restricted to the described embodiments, it should be appreciated that people in the art
Member can be designed that a lot of other amendments and embodiment, and these amendments and embodiment will fall in principle disclosed by the invention
Within scope and spirit.
Claims (10)
1. the method press-fiting aluminum composition modeling powder is prepared in an aqueous suspension, it is characterised in that it comprises the following steps:
A, the surface preparation of aluminium powder
First, in the aluminium powder of vacuum drying, solvent is added in the ratio that mass volume ratio is 1g:5mL of aluminium powder Yu solvent, so
Post-heating stirs 30 minutes after 80 DEG C under ultrasound condition；Then in mixture, add dibutyl tin laurate and toluene
Diisocyanate, the addition of described dibutyl tin laurate and toluene di-isocyanate(TDI) is respectively with the mass ratio of aluminium powder
0.5:50 and 2:50, mixing post-heating backflow 2h；Continuously add glycidyl azide polymer and be heated to reflux 2h, described poly-nitrine
The addition of glycidyl ether is 1/5th of aluminium powder quality；After being finally cooled to room temperature, sucking filtration with solvent washing filter cake 3
～5 times, i.e. obtain the aluminium powder of surface preparation after vacuum drying；
Described solvent is anhydrous acetonitrile, ethyl acetate or butyl acetate；
B, the surface preparation of explosive
Explosive is joined in the solvent containing coating material, after ultrasonic and mechanical agitation is disperseed 5 minutes, sucking filtration, drying, obtain
The explosive of coating material cladding；
C, aqueous suspension comminution granulation
The explosive of the coating material cladding that the aluminium powder of surface preparation step A obtained and step B obtain is added to the water, and adds
Thermal agitation is uniform；Then the binder solution prepared is dripped, when binder solution is added drop-wise to 2/3rds, molten to this mixing
Liquid spray into appropriate water-dispersible uniformly after, continue to drip remaining binder solution, after dripping complete 10min, spray into appropriate water
Dispersion, flushing；Then sucking filtration, vacuum drying, obtains described aqueous suspension preparation and press-fits aluminum composition modeling powder.
The method press-fiting aluminum composition modeling powder is prepared in aqueous suspension the most according to claim 1, it is characterised in that in step A
In, described aluminium powder is ball aluminum powder, and its particle size range is 0.05～50 μm.
The method press-fiting aluminum composition modeling powder is prepared in aqueous suspension the most according to claim 2, it is characterised in that described
Aluminium powder particle size range is 0.05～5 μm.
The method press-fiting aluminum composition modeling powder is prepared in aqueous suspension the most according to claim 1, it is characterised in that in step B
In, described explosive is high sensitivity explosive, and it is one or more compositionss in CL-20, HMX, RDX, LLM-105, TATB, institute
The particle diameter stating explosive is 1～120 μm.
The method press-fiting aluminum composition modeling powder is prepared in aqueous suspension the most according to claim 1, it is characterised in that in step B
In, the described solvent containing coating material refer to be dissolved in polyurethane dichloroethanes formed concentration be 0.25～1.0wt% molten
Agent.
The method press-fiting aluminum composition modeling powder is prepared in aqueous suspension the most according to claim 1, it is characterised in that in step C
In, described binder solution refers to high polymer binder is dissolved in ethyl acetate, butyl acetate or dichloroethanes formation
Solution, its concentration is 4.0～8.0wt%.
The method press-fiting aluminum composition modeling powder is prepared in aqueous suspension the most according to claim 6, it is characterised in that described
High polymer binder is vinylidene and the copolymer of CTFE or polyurethane polymer binding agent.
The method press-fiting aluminum composition modeling powder is prepared in aqueous suspension the most according to claim 1, it is characterised in that in step C
In, the explosive of coating material that the aluminium powder of the surface preparation that described step A obtains, step B obtain cladding and binding agent
Mass ratio is 10～30:55～90:5～10.
The method press-fiting aluminum composition modeling powder is prepared in aqueous suspension the most according to claim 1, it is characterised in that in step C
In, it is 60～70 DEG C that described being heated to be is heated to temperature.
The method press-fiting aluminum composition modeling powder is prepared in aqueous suspension the most according to claim 1, it is characterised in that in step
In C, the drop rate of described binder solution is 3mL/min.
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| CN109482860A (en) * | 2018-12-13 | 2019-03-19 | 中国工程物理研究院化工材料研究所 | A kind of micronized method of spherical shape of nanometer aluminium powder |
| CN113603987A (en) * | 2021-07-28 | 2021-11-05 | 中国工程物理研究院化工材料研究所 | Modified aluminum/fluorine-containing polymer compound and preparation method thereof |
| CN113603987B (en) * | 2021-07-28 | 2022-07-26 | 中国工程物理研究院化工材料研究所 | Modified aluminum/fluorine-containing polymer compound and preparation method thereof |
| CN116143572A (en) * | 2023-03-06 | 2023-05-23 | 南京理工大学 | Boron-aluminum high-energy mixed explosive and preparation method thereof |
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