CN110423182A - The method that CL-20/TATB base Composite Energetic Materials are prepared using emulsion breaking method - Google Patents
The method that CL-20/TATB base Composite Energetic Materials are prepared using emulsion breaking method Download PDFInfo
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- CN110423182A CN110423182A CN201910709395.5A CN201910709395A CN110423182A CN 110423182 A CN110423182 A CN 110423182A CN 201910709395 A CN201910709395 A CN 201910709395A CN 110423182 A CN110423182 A CN 110423182A
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- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B21/00—Apparatus or methods for working-up explosives, e.g. forming, cutting, drying
- C06B21/0008—Compounding the ingredient
- C06B21/0025—Compounding the ingredient the ingredient being a polymer bonded explosive or thermic component
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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
- C06B25/00—Compositions containing a nitrated organic compound
- C06B25/34—Compositions containing a nitrated organic compound the compound being a nitrated acyclic, alicyclic or heterocyclic amine
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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
- C06B45/20—Compositions or products which are defined by structure or arrangement of component of product comprising a coated component the component base containing an organic explosive or an organic thermic component
- C06B45/22—Compositions or products which are defined by structure or arrangement of component of product comprising a coated component the component base containing an organic explosive or an organic thermic component the coating containing an organic compound
- C06B45/24—Compositions or products which are defined by structure or arrangement of component of product comprising a coated component the component base containing an organic explosive or an organic thermic component the coating containing an organic compound the compound being an organic explosive or an organic thermic component
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Abstract
The invention discloses a kind of preparation method of CL-20/TATB Composite Energetic Materials, include the following steps: that weighing CL-20 is add to deionized water, 1-2 drop Tween-80 solution is added dropwise, ultrasonic agitation obtains solution A；It weighs a nanometer TATB to be add to deionized water, is stirred by ultrasonic, obtains solution B；Binder is dissolved in ethyl acetate, is sufficiently stirred until it is completely dissolved, dropwise addition 1-2 drop Tween-80 obtains solution C；Solution C is at the uniform velocity stirred to 30min under the revolving speed of 500r/min and forms lotion, then solution A is added in lotion, constant temperature is to emulsion breaking after being warming up to 60 DEG C, solution B is at the uniform velocity added dropwise after sufficiently demulsification 1h, 80 DEG C are warming up to after reaction 1h to drive away extra ethyl acetate solution, stop reaction, by the solution for being coated with explosive through precipitating, filter, be dried to obtain CL-20/TATB Composite Energetic Materials.Binder and deterrent, compared to traditional water slurry, more uniformly can be coated on the surface CL-20 using demulsification method by the present invention, to obtain preferably dropping sense effect.
Description
Technical field
The invention belongs to energetic material preparation fields, are related to a kind of preparation method of CL-20/TATB Composite Energetic Materials.
Background technique
Plastic bonded explosive (PBX) is based on high explosive, in addition binder, plasticizer, deterrent, sometimes
Add some auxiliary additives, manufactured one kind composite explosives.With the excellent synthesis such as energy is high, sensitivity is low, mechanical property is good
Performance has a wide range of applications in various tips and conventional weapon.
Requirement of the weaponry to explosive at present is high energy, insensitiveness, low rapid wear, so preparation has the low rapid wear of high-energy insensitive
PBX also be always composite explosives field research hotspot.
TATB is a kind of very stable and insensitiveness heat-resistant explosive, because TATB is excellent for heat-resisting and anti-physical impact
In any known energy comparable explosive therewith.TATB has good heat resistance and safety, and TATB base composite explosives are to height
Temperature is hit, impact all unusual insensitiveness, and the security requirement of Modern New ammunition is able to satisfy.TATB base composite explosives both have height
Explosion energy, and there is good security performance, thus be considered as at present most excellent high-energy insensitive Composite Energetic Materials it
One, it is widely used in Qinzhou harbor warhead and high explosive anti-tank cartridge warhead.
Xu Rong is mixed with the TATB of different-grain diameter with CL-20 in " sense research drops to CL-20 in TATB ", studies TATB pairs
The desensitization mechanism of CL-20.Chen Luying is in " the cladding insensitiveness of CL-20 explosive is studied " with Estane and the compound deterrent of graphene
Drop sense research is carried out to CL-20.Bian Hongli is in " preparation and its characterization of CL-20/NQ composite energy-containing microballoon " using spraying knot
Brilliant technique prepares CL-20/NQ microballoon, and microballoon thermal stability is obviously improved compared with CL-20, and mechanical sensitivity significantly reduces.Pass through addition
Insensitiveness high energy material prepares multicomponent explosive, and realizing reduces CL-20 explosive sensitivity and reduce maximum system energy loss, has become solution
Certainly explosive energy important thinking contradictory with safety.
Although the above-mentioned prior art has certain effect to the drop sense of explosive, the relatively simple limitation of idea and method, this is specially
Benefit can obtain preferably drop sense effect by combining nanosizing and cladding drop two kinds of drop sensing methods of sense.
Summary of the invention
It is reduced to solve the problems, such as that traditional insensitiveness coats the output energy that energetic material occurs in actual use, the present invention
Provide a kind of preparation method of high-energy insensitive energetic material.
To achieve the above object, the present invention adopts the following technical scheme: a kind of system of CL-20/TATB Composite Energetic Materials
Preparation Method includes the following steps:
Step 1, the CL-20 for weighing metering is added in suitable deionized water, and 1-2 drop Tween-80 solution, ultrasound is added dropwise
Stirring, obtains solution A；
Step 2, the nanometer TATB for weighing metering is added in suitable deionized water, and ultrasonic agitation obtains solution B；
Step 3, the binder of metering is dissolved in suitable ethyl acetate, be sufficiently stirred until its be completely dissolved, be added dropwise
1-2 drop Tween-80, obtains solution C；
Step 4, solution C is at the uniform velocity stirred to 30min under the revolving speed of 500r/min and forms lotion, then solution A is added
In lotion, constant temperature is at the uniform velocity added dropwise solution B after the 1h that is sufficiently demulsified, is warming up to 80 after reacting 1h to emulsion breaking after being warming up to 60 DEG C
DEG C to drive away extra ethyl acetate solution, up to no ethyl acetate taste sheds, stops reaction, the solution of explosive will be coated with
Through precipitating, filters, is dried to obtain CL-20/TATB Composite Energetic Materials.
Preferably, the mass ratio of CL-20 and TATB is 91:8 or 93:6 or 95:4
Preferably, binder uses polyacrylic resin AR-14 or fluorubber F2603。
Preferably, in step 3, the quality of binder accounts for solid material i.e. CL-20, TATB and binder three's gross mass
1%.
Compared with prior art, the invention has the following advantages that
(1) covering material used in the present invention is TATB, and explosion velocity is up to 7600m/s, while to heat, light, impact
The environmental stimulis such as wave, friction and mechanical impact extremely insensitiveness, heat resistance is also extremely excellent, and thermal decomposition temperature reaches 450 DEG C.
(2) polyacrylic resin (AR-14), F are used2603As binder, effectively TATB and CL-20 can be bonded in
Together.
It (3), can be more uniformly by binder and deterrent packet using demulsification method compared to traditional water slurry
The surface CL-20 is overlayed on, to obtain preferably dropping sense effect.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph of CL-20.
Fig. 2 is the scanning electron microscope (SEM) photograph of nanometer TATB.
Fig. 3 is the scanning electron microscope (SEM) photograph (CL-20:TATB:AR-14=95:4:1) for implementing example 1.
Fig. 4 is the scanning electron microscope (SEM) photograph (CL-20:TATB:AR-14=93:6:1) for implementing example 2.
Fig. 5 is the scanning electron microscope (SEM) photograph (CL-20:TATB:AR-14=91:8:1) for implementing example 3.
Fig. 6 is the scanning electron microscope (SEM) photograph (CL-20:TATB:F for implementing example 42603=95:4:1).
Fig. 7 is the scanning electron microscope (SEM) photograph (CL-20:TATB:F for implementing example 52603=93:6:1).
Fig. 8 is the scanning electron microscope (SEM) photograph (CL-20:TATB:F for implementing example 62603=91:8:1).
Fig. 9 is the X-ray diffraction analysis of CL-20, nanometer TATB and CL-20/TATB/AR-14.
Figure 10 is CL-20/TATB, CL-20/TATB/F2603, CL-20/TATB/AR-14 X-ray diffraction analysis.
Specific embodiment
Below with reference to embodiment and attached drawing, the invention will be further described.
The present invention is by using emulsion breaking method, and binder solution and water are in emulsifier ethyl acetate under strong stirring
Lotion is formed under effect, main body explosive CL-20 is subsequently added into and is uniformly mixed, be then demulsified using method appropriate, make binder
It is precipitated on explosive surface, is eventually adding TATB as deterrent, the surface CL-20 is coated under the action of binder, sufficiently sent out
The insensitiveness effect for waving TATB obtains the CL-20/TATB Composite Energetic Materials of high-energy insensitive.
Embodiment 1
It is CL-20:TATB:AR-14=95:4:1 according to the formula of composite explosives weight percent, weighs 23.75g's
CL-20 (its pattern is shown in Fig. 1), is added in the deionized water of 50ml, and 10min is stirred by ultrasonic；Then the nanometer TATB of 1g is weighed
(its pattern is shown in Fig. 2), is added in the deionized water of 20ml, and 10min is stirred by ultrasonic；Then the AR-14 for weighing 0.25g, is added
The ethyl acetate of 10ml, is sufficiently stirred, until being completely dissolved；The ethyl acetate solution of above-mentioned AR-14 is finally poured into three mouthfuls
In flask, 1-2 drop Tween-80 is added dropwise, 30min is at the uniform velocity stirred under the revolving speed of 500r/min and forms lotion, then by above-mentioned CL-
20 solution are added in lotion, and above-mentioned TATB solution is at the uniform velocity added dropwise after the 1h that is sufficiently demulsified to emulsion breaking in constant temperature after being warming up to 60 DEG C
Into flask, it is warming up to 80 DEG C after reacting 2h to drive away extra ethyl acetate solution, up to no ethyl acetate taste sheds, stops
Only react.By the solution in flask through precipitating, filter, be dried to obtain CL-20/TATB Composite Energetic Materials.
Implement example 2
It is CL-20:TATB:AR-14=93:6:1 according to the formula of composite explosives weight percent, weighs 23.25g's
CL-20 is added in the deionized water of 50ml, and 10min is stirred by ultrasonic；Then the nanometer TATB for weighing 1.5g, is added to 20ml
Deionized water in, be stirred by ultrasonic 10min；Then the AR-14 for weighing 0.25g, is added the ethyl acetate of 10ml, is sufficiently stirred,
Until being completely dissolved；Finally the ethyl acetate solution of above-mentioned AR-14 is poured into three-necked flask, 1-2 drop Tween-80 is added dropwise,
30min is at the uniform velocity stirred under the revolving speed of 500r/min and forms lotion, and then above-mentioned CL-20 solution is added in lotion, is warming up to
Constant temperature is at the uniform velocity added dropwise above-mentioned TATB solution into flask after the 1h that is sufficiently demulsified, is warming up to after reacting 2h to emulsion breaking after 60 DEG C
80 DEG C, to drive away extra ethyl acetate solution, up to no ethyl acetate taste sheds, stop reaction.By the solution warp in flask
It precipitates, filter, being dried to obtain CL-20/TATB Composite Energetic Materials.
Implement example 3
It is CL-20:TATB:AR-14=91:8:1 according to the formula of composite explosives weight percent, weighs 22.75g's
CL-20 is added in the deionized water of 50ml, and 1-2 drop Tween-80 is added, and 10min is stirred by ultrasonic；Then the nanometer of 2g is weighed
TATB is added in the deionized water of 20ml, and 10min is stirred by ultrasonic；Then the AR-14 for weighing 0.25g, is added the acetic acid of 10ml
Ethyl ester is sufficiently stirred, until being completely dissolved；Finally the ethyl acetate solution of above-mentioned AR-14 is poured into three-necked flask, is added
1-2 drop tween water at the uniform velocity stirs 30min under the revolving speed of 500r/min and forms lotion, cream then is added in above-mentioned CL-20 solution
In liquid, constant temperature is at the uniform velocity added dropwise above-mentioned TATB solution into flask after the 1h that is sufficiently demulsified, reacts to emulsion breaking after being warming up to 60 DEG C
80 DEG C are warming up to after 2h to drive away extra ethyl acetate solution, up to no ethyl acetate taste sheds, stopping is reacted.By flask
In solution through precipitating, filter, be dried to obtain CL-20/TATB Composite Energetic Materials.
Implement example 4
Formula according to composite explosives weight percent is CL-20:TATB:F2603=95:4:1 weighs the CL- of 23.75g
20, it is added in the deionized water of 50ml, 10min is stirred by ultrasonic；Then weigh 1g nanometer TATB, be added to 20ml go from
In sub- water, 10min is stirred by ultrasonic；Then the F of 0.25g is weighed2603, the ethyl acetate of 10ml is added, is sufficiently stirred, until completely
Dissolution；Finally by above-mentioned F2603Ethyl acetate solution pour into three-necked flask, be added dropwise 1-2 drop Tween-80, in 500r/min
Revolving speed under at the uniform velocity stir 30min formed lotion, then by above-mentioned CL-20 solution be added lotion in, constant temperature after being warming up to 60 DEG C
To emulsion breaking, above-mentioned TATB solution is at the uniform velocity added dropwise into flask after the 1h that is sufficiently demulsified, is warming up to 80 DEG C after reacting 2h to drive away
Extra ethyl acetate solution, up to no ethyl acetate taste sheds, stopping is reacted.By the solution in flask through precipitating, filtering,
It is dried to obtain CL-20/TATB Composite Energetic Materials.
Implement example 5
Formula according to composite explosives weight percent is CL-20:TATB:F2603=93:6:1 weighs the CL- of 23.25g
20, it is added in the deionized water of 50ml, 10min is stirred by ultrasonic；Then the nanometer TATB for weighing 1.5g, is added to going for 20ml
In ionized water, 10min is stirred by ultrasonic；Then the F of 0.25g is weighed2603, the ethyl acetate of 10ml is added, is sufficiently stirred, until complete
Fully dissolved；Finally by above-mentioned F2603Ethyl acetate solution pour into three-necked flask, be added dropwise 1-2 drop Tween-80, in 500r/
30min is at the uniform velocity stirred under the revolving speed of min and forms lotion, and then above-mentioned CL-20 solution is added in lotion, it is permanent after being warming up to 60 DEG C
Above-mentioned TATB solution is at the uniform velocity added dropwise into flask after the 1h that is sufficiently demulsified to emulsion breaking in temperature, is warming up to 80 DEG C after reacting 2h to drive
Except extra ethyl acetate solution, up to no ethyl acetate taste sheds, stopping is reacted.By the solution in flask through precipitating, mistake
It filters, be dried to obtain CL-20/TATB Composite Energetic Materials.
Implement example 6
Formula according to composite explosives weight percent is CL-20:TATB:F2603=91:8:1 weighs the CL- of 22.75g
20, it is added in the deionized water of 50ml, 1-2 drop Tween-80 is added, 10min is stirred by ultrasonic；Then the nanometer of 2g is weighed
TATB is added in the deionized water of 20ml, and 10min is stirred by ultrasonic；Then the F of 0.25g is weighed2603, the acetic acid of 10ml is added
Ethyl ester is sufficiently stirred, until being completely dissolved；Finally by above-mentioned F2603Ethyl acetate solution pour into three-necked flask, be added
1-2 drop tween water at the uniform velocity stirs 30min under the revolving speed of 500r/min and forms lotion, cream then is added in above-mentioned CL-20 solution
In liquid, constant temperature is at the uniform velocity added dropwise above-mentioned TATB solution into flask after the 1h that is sufficiently demulsified, reacts to emulsion breaking after being warming up to 60 DEG C
80 DEG C are warming up to after 2h to drive away extra ethyl acetate solution, up to no ethyl acetate taste sheds, stopping is reacted.By flask
In solution through precipitating, filter, be dried to obtain CL-20/TATB Composite Energetic Materials.
Comparative example 1
It is CL-20:TATB:Estane5703=95:4:1 according to the formula of composite explosives weight percent, weighs
The CL-20 of 23.75g, is added in the deionized water of 50ml, and 10min is stirred by ultrasonic；Then the nanometer TATB for weighing 1g, is added
Into the deionized water of 20ml, 10min is stirred by ultrasonic；Then the Estane5703 for weighing 0.25g, is added the acetic acid second of 10ml
Ester is sufficiently stirred, until being completely dissolved；Finally the ethyl acetate solution of above-mentioned Estane5703 is poured into three-necked flask,
1-2 drop Tween-80 is added dropwise, 30min is at the uniform velocity stirred under the revolving speed of 500r/min and forms lotion, then by above-mentioned CL-20 solution
It is added in lotion, above-mentioned TATB solution is at the uniform velocity added dropwise to flask after the 1h that is sufficiently demulsified to emulsion breaking in constant temperature after being warming up to 60 DEG C
In, 80 DEG C are warming up to drive away extra ethyl acetate solution after reacting 2h, and up to no ethyl acetate taste sheds, stopping is anti-
It answers.By the solution in flask through precipitating, filter, be dried to obtain CL-20/TATB Composite Energetic Materials.
Test analysis: in such cases, by analyzing raw material and the sample of preparation, mechanical sensitivity is not achieved pre-
Phase requires, therefore this formula is undesirable.
Comparative example 2
It is CL-20:TATB:Estane5703=93:6:1 according to the formula of composite explosives weight percent, weighs
The CL-20 of 23.25g, is added in the deionized water of 50ml, and 10min is stirred by ultrasonic；Then the nanometer TATB for weighing 1.5g, adds
Enter into the deionized water of 20ml, 10min is stirred by ultrasonic；Then the Estane5703 for weighing 0.25g, is added the acetic acid second of 10ml
Ester is sufficiently stirred, until being completely dissolved；Finally the ethyl acetate solution of above-mentioned Estane5703 is poured into three-necked flask,
1-2 drop Tween-80 is added dropwise, 30min is at the uniform velocity stirred under the revolving speed of 500r/min and forms lotion, then by above-mentioned CL-20 solution
It is added in lotion, above-mentioned TATB solution is at the uniform velocity added dropwise to flask after the 1h that is sufficiently demulsified to emulsion breaking in constant temperature after being warming up to 60 DEG C
In, 80 DEG C are warming up to drive away extra ethyl acetate solution after reacting 2h, and up to no ethyl acetate taste sheds, stopping is anti-
It answers.By the solution in flask through precipitating, filter, be dried to obtain CL-20/TATB Composite Energetic Materials.
Test analysis: in such cases, by analyzing raw material and the sample of preparation, mechanical sensitivity is not achieved pre-
Phase requires, therefore this formula is also undesirable.
Referring to the method 601.2 in GJB772A-97, shock sense is carried out to the CL-20/TATB Composite Energetic Materials of preparation
Degree and friction sensitivity test, test condition are as follows: it is dropped hammer using 5kg, 90 ° of pivot angle, gauge pressure 2.45Mpa, dose (35 ± 1) mg,
Test temperature (20 ± 2) DEG C, relative humidity (60 ± 5) %.It needs to be dried before sample testing, is put into 50-60 DEG C of water-bath
Baking oven 2h, taking-up are put into drier, and cooling down the rear 1-2h at room temperature can be used.Every group 25 hair, totally three groups.Test result such as table 1
It is shown
The impact sensitivity and friction sensitivity of 1 CL-20/TATB Composite Energetic Materials sample of table
As shown in Table 1, using nanometer TATB cladding CL-20 Composite Energetic Materials friction sensitivity and impact sensitivity compared with
CL-20 has and significantly reduces, the Composite Energetic Materials best performance of embodiment 3, and impact sensitivity reduces 48.9%, friction
Sensitivity reduces 90%.
Fig. 3-Fig. 5 is CL-20/TATB/AR-14 Composite Energetic Materials obtained, and Fig. 6-Fig. 8 is CL-20/ obtained
TATB/F2603Composite Energetic Materials.It can be seen from the figure that nanometer TATB particle is completely equably coated on the surface CL-20, card
The feasibility of this experiment is illustrated.
Fig. 9, Figure 10 CL-20, nanometer TATB, CL-20/TATB/AR-14 and CL-20/TATB/F2603X-ray diffraction
Analysis.It can be seen that the angle of diffraction of CL-20 principal character peak is at 12.5 °, 13.7 °, 30.3 °, the principal character peak of TATB
The angle of diffraction is at 25.7 °.And the principal character peak of three kinds of Composite Energetic Materials has the form of CL-20 characteristic peak, and diffraction
Angle is identical, illustrates that CL-20 crystal habit is still ε-CL-20 there is no variation in Composite Energetic Materials preparation process；Its
Middle CL-20/TATB cemented explosive also has the characteristic peak form and the identical angle of diffraction of TATB.
Other are changed to 400r/min and 600r/min with embodiment 1, by stirring rate 500r/min, when speed of agitator is
When 400r/min, since revolving speed is lower, after dripping binder, particle aggregation does not meet expected requirement at bulky grain；When stirring
Mix rate be 600r/min when, since revolving speed is very fast, shearing force is larger, thus TATB cannot be uniformly coated on the surface CL-20,
So the revolving speed of selection 500r/min is tested.
Claims (4)
1. a kind of preparation method of CL-20/TATB Composite Energetic Materials, which comprises the steps of:
Step 1, the CL-20 for weighing metering is add to deionized water, and 1-2 drop Tween-80 solution is added dropwise, and ultrasonic agitation obtains
Solution A；
Step 2, the nanometer TATB for weighing metering is add to deionized water, and ultrasonic agitation obtains solution B；
Step 3, the binder of metering is dissolved in ethyl acetate, be sufficiently stirred until its be completely dissolved, be added dropwise 1-2 drop tween-
80, obtain solution C；
Step 4, solution C is at the uniform velocity stirred to 30min under the revolving speed of 500r/min and forms lotion, lotion then is added in solution A
In, solution B is at the uniform velocity added dropwise after the 1h that is sufficiently demulsified to emulsion breaking in constant temperature after being warming up to 60 DEG C, react be warming up to after 1h 80 DEG C with
Drive away extra ethyl acetate solution, stop reaction, by the solution for being coated with explosive through precipitating, filter, be dried to obtain CL-20/
TATB Composite Energetic Materials.
2. the method as described in claim 1, which is characterized in that the mass ratio of CL-20 and TATB is 91:8 or 93:6 or 95:4.
3. the method as described in claim 1, which is characterized in that binder uses polyacrylic resin AR-14 or fluorubber
F2603。
4. the method as described in claim 1, which is characterized in that in step 3, the quality of binder accounts for solid material gross mass
1%。
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| CN115925492A (en) * | 2022-12-15 | 2023-04-07 | 南京理工大学 | Method for reducing CL-20 |
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