CN106083494B - A kind of method using the plasticizing Estane5703 cladding explosives of CL 20 - Google Patents

A kind of method using the plasticizing Estane5703 cladding explosives of CL 20 Download PDF

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Publication number
CN106083494B
CN106083494B CN201610412668.6A CN201610412668A CN106083494B CN 106083494 B CN106083494 B CN 106083494B CN 201610412668 A CN201610412668 A CN 201610412668A CN 106083494 B CN106083494 B CN 106083494B
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estane5703
microwax
explosive
dop
organic solvent
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CN106083494A (en
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焦清介
魏华
郭学永
李航
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Beijing Institute of Technology BIT
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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
    • C06B21/0083—Treatment of solid structures, e.g. for coating or impregnating with a modifier
    • 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
    • C06B23/005—Desensitisers, phlegmatisers
    • 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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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)

Abstract

The present invention relates to a kind of method using the plasticizing Estane5703 cladding explosives of CL 20, this method uses aqueous suspension technology, first the surfaces of CL 20 are coated on deterrent microwax, prepare CL 20 and microwax compound, Estane5703 is coated on to CL 20 and microwax compound surface again, prepares the explosive compounds of CL 20.This method can form uniform, fine and close film on the explosive surfaces of CL 20, significantly reduce the explosive mechanical sensitivities of CL 20.Explosive compound its coating film of CL 20 prepared by the present invention is controlled in nanometer range, and content only accounts for 2% the 4% of total system, smaller to the energy affect of the explosives of CL 20.Impact sensitivity is reduced to 52% 72% by 100% after the explosives of CL 20 cladding, and friction sensitivity is reduced to 40% 80% by 100%.

Description

A kind of method using plasticizing Estane5703 cladding CL-20 explosives
Technical field
The present invention relates to a kind of method using plasticizing Estane5703 cladding CL-20 explosives, belong to energetic material field.
Background technology
Hexanitrohexaazaisowurtzitane (HNIW, being commonly called as CL-20) be Nielsen in 1987 find synthesis high density, High-energy, high explosion velocity, the ammonium nitrate explosive of detonation pressure, it is the explosive of new generation after HMX.Now, industrialized simple substance is fried In medicine, CL-20 energy level is leading, and several parameters such as its maximum explosion velocity, detonation pressure, density are better than HMX, energy output It is higher by 10% to 15% than HMX.CL-20 is applied to all kinds of explosive wastewater products, may all improve the war skill index of related weaponry. But because its mechanical sensitivity is high, crystalline form is irregular, and the factors such as size distribution is wide are, it is necessary to reduce CL-20 mechanical sensitivity and enter Row drop sense processing.
Wherein received much concern using the method for high polymer material cladding sensitive explosive, choose suitable high polymer material conduct Binding agent, is coated on CL-20 surfaces, forms one layer of dense film, completely cut off influence of the external factor to CL-20 effectively reduce or Avoid dehumidification phenomenon, and due to the fabulous mechanical property of high polymer material, both improve explosive mechanical property and surface characteristic, Explosive mechanical sensitivity is improved again.The polymeric PTC materials method of sensitive explosive turns into realizes its insensitiveness, the important way of high reliability One of footpath.
Domestic and foreign scholars are directed to a large amount of high molecular polymers grinding as binding agent cladding CL-20 explosive drop senses for many years Study carefully, achieve many achievements.Wherein use aqueous suspension technology easy to operate with its, easy control of process conditions, covered effect is good, The features such as production efficiency is high, and the method is tested in aqueous phase, it is safer for the cladding of explosive, it has also become A kind of the most frequently used method for coating in laboratory.Concrete operations are：Covering material is dissolved in into specific solvent, and (this solvent does not dissolve In water) and water in, while propellant solid packing is added to moisture and dissipated, then add the solvent of lysed covering material The methods of entering, suspension is made, then being precipitated by evaporation solvent, filtering separates out covering material in the table with propellant filler Face.Domestic and international research and utilization aqueous suspension method is poly- by deterrent such as paraffin, microwax, graphite etc., high molecular polymer fluorubber Urethane, natural rubber etc. be coated on CL-20 surfaces, relative reduction CL-20 mechanical sensitivity.But combine deterrent and high score The technology that sense drops in sub- good characteristic with deterrent with high polymer material compound coating CL-20 simultaneously is not yet found.The present invention is exactly Using water suspension method, deterrent is coated CL-20 under water environment with high polymer material, both ensure process safety, again may be used Covering is uniformly coated on its surface.Clad has the composite attribute of deterrent and high polymer material, to reducing CL-20 Mechanical sensitivity plays a significant role.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of side using plasticizing Estane5703 cladding CL-20 explosives Method, the present inventor have found that deterrent relies on it to absorb focus heat and the theoretical reduction explosive machine of heat absorption insensitiveness by numerous studies Tool sensitivity, macromolecule polymer material are coated on explosive surface, and the mechanical sensitivity of explosive is reduced with its special mechanical property.Root According to the different desensitization mechanisms of two class materials, after synthesis coats CL-20 explosives using deterrent with high molecular polymer, its mechanical sense Degree significantly decline, the practical application of high explosive is had great significance, the present invention in high-energy insensitive explosive have compared with Good application background.
The technical scheme that the present invention solves above-mentioned technical problem is as follows：One kind is using plasticizing Estane5703 claddings CL-20 The method of explosive, including：
1) deterrent microwax is dissolved in the first organic solvent, obtains the microwax solution that mass concentration is 10%-12%；
High polymer binder Estane5703 and plasticizer DOP are dissolved in the second organic solvent, obtaining mass concentration is The 5%-7% solution containing Estane5703 and DOP, mass concentration herein is Estane5703 and DOP quality sums Concentration；
2) by CL-20 and pure water by weight 1:1.1-1：1.3 are placed in aqueous suspension reactor, stirring, make CL-20 points Dissipate uniformly, obtain explosive mixed liquor, explosive mixed liquor is warming up to 64-66 DEG C, open vacuum and air is pumped out, adjust in reactor Pressure is 0.02Mpa, and 1) gained microwax solution is added dropwise into explosive mixed liquor, passes through the first organic solvent evaporation, microwax Precipitation is coated on CL-20 surfaces, after the first organic solvent evaporation is complete, prepares CL-20 and microwax compound；
3) add water into reactor, keep reacting kettle inner pressure, adjustment speed of agitator is 900r/min, is adjusted in reactor Temperature adds 1) solution of the gained containing Estane5703 and DOP to 59-61 DEG C, after the second organic solvent evaporation is complete, Estane5703 is coated on CL-20 and microwax compound surface, and solid product is centrifuged, washed, is dried, is produced CL-20 explosive compounds.
On the basis of above-mentioned technical proposal, the present invention can also do following improvement.
Further, in 1), the microwax is No. 80 microwaxes, is market selling product.Microwax is a kind of approximate The refined synthetic wax of crystallite property, has a good luster, and fusing point is high, the characteristics of lighter color.Its close structure, it is hard and lubricious.
Further, in 1), for first organic solvent to analyze pure petroleum ether, second organic solvent is that analysis is pure Chloroform.
Further, in 1), mass ratio=4 of the Etsane5703 and DOP:1, the Estane5703 are a kind of high Molecular material, belong to PAUR, produced by Lubrizol Corp. of the U.S., the spike of the Suzhou four plasticizing commercially available business of Co., Ltd Product.DOP scientific names dioctyl phthalate used in the present invention, is a kind of organic esterses, is a kind of conventional plasticiser, Plasticizer of the DOP as Estane5703.
Further, in 2), the mixing speed is 450r/min.
Further, in 2), the speed that the microwax solution is added dropwise into explosive mixed liquor is 3mls-1。
Further, in 2), the quality of microwax accounts for the 2%-3% of CL-20 mass in the microwax solution of addition.
Further, the quality of pure water is added in 2) and adds the quality sum of water and the ratio of CL-20 mass to close in 3) It is for 2:1.
Further, in 3), Estane5703 and DOP total matter in the solution containing Estane5703 and DOP of addition Amount accounts for the 2%-3% of CL-20 mass.
Further, in 3), the speed that the solution containing Estane5703 and DOP is added dropwise into reactor is 3mls-1。
The beneficial effects of the invention are as follows：
The present invention discloses the side that one kind prepares low sense Hexanitrohexaazaisowurtzitane (CL-20) the explosive compound of high energy Method, idiographic flow are as shown in Figure 1.CL-20 explosive compounds profile prepared by the present invention in pelletized form, epigranular, size 300 μm -600 μm, CL-20 explosives surface uniformly coats to form fine and close coating film by deterrent and high polymer binder.According to The type tool approach of GJB772A-1997 methods 601.1 tests the explosive compound impact sensitivity, and experimental condition is：Quality of dropping hammer is 10.000±0.010kg；Dose is 50 ± 1mg；Temperature is 10~35 DEG C；Relative humidity≤80%, measurement blast percentage.Survey The impact sensitivity that test result shows to coat front and rear CL-20 explosives drops to 52%-72% by 100%.
According to GJB772A-97《Explosive test method》602.1 regulation, determine it with WJ-1 type pendulum type friction sensibility instruments Explode percentage.Test condition is：20 ± 1mg of dose, pendulum 1.50 ± 0.01kg of quality, 3.92 ± 0.07MPa of pressure, pivot angle 90±1.Environment temperature is 25 DEG C, relative humidity≤58%.Test result shows, coats front and rear CL-20 explosive friction sensitivities 40%-80% is reduced to by 100%.
Brief description of the drawings
Fig. 1 is a kind of method flow diagram that CL-20 explosives are coated using plasticizing Estane5703 of the present invention；
Fig. 2 is the electron-microscope scanning figure of the CL-20 explosive raw materials used in the embodiment of the present invention 1；
Fig. 3 a are the electron-microscope scanning figure of CL-20 explosive compounds prepared by the embodiment of the present invention 1；
Fig. 3 b are the electron-microscope scanning figure of CL-20 explosive composite surfaces prepared by the embodiment of the present invention 1.
Embodiment
The principles and features of the present invention are described below, and the given examples are served only to explain the present invention, is not intended to limit Determine the scope of the present invention.
Embodiment 1
(1) it is 65 DEG C by constant temperature water bath temperature setting, opens water circulation.The pure water for weighing 120g adds reactor, Stirring motor is opened, mixing speed 450r/min, load weighted 100g CL-20 is added in reactor and stirred, makes CL-20 Crystal is uniformly dispersed, and obtains explosive mixed liquor.
(2) in the pure petroleum ether of analysis that 2g No. 80 microwaxes are dissolved in into 18g, the microwax oil of mass concentration 10% is obtained Ethereal solution, it is stand-by.
1.6g Estane5703 and 0.4g DOP are dissolved in the 38g pure chloroform of analysis, obtain containing for mass concentration 5% There are Estane5703 and DOP chloroform soln, it is stand-by.
(3) explosive mixed liquor is warming up to 64-66 DEG C, opens vavuum pump and separate out air, adjusting pressure in kettle is 0.02Mpa, with 3mls-1Rate of addition be added dropwise microwax petroleum ether solution into reactor, evaporated by solvent, insensitiveness No. 80 microwaxes of agent, which separate out, is coated on CL-20 surfaces.After petroleum ether evaporation completely, CL-20 and microwax compound are prepared. Again into reactor add 60 DEG C of water 80g, make water material mass ratio (water be the dosage of water added by step 1 and 3 and, material refer to CL-20's Dosage) it is 2：1.It is 60 DEG C to adjust reactor temperature, and adjustment speed of agitator is 900r/min, and holding reacting kettle inner pressure is 0.02Mpa, with 3mls-1Rate of addition be added dropwise the chloroform soln containing Estane5703 and DOP into reactor.Treat After chloroform evaporation, Estane5703 separates out the surface for being coated on CL-20 and microwax compound.
(4) after chloroform evaporating completely, reactor temperature is reduced to less than 40 DEG C, by solid product centrifugation point From, washing, dry, produce CL-20 explosive compounds 94.3g.
The electron-microscope scanning figure of CL-20 explosive raw materials is as shown in Fig. 2 the CL-20 explosive compound Electronic Speculum that the present embodiment obtains As shown in Figure 3 a, CL-20 explosive composite surfaces electron-microscope scanning figure is as shown in Figure 3 b for scanning figure.CL-20 explosives surface is by insensitiveness Agent and high polymer binder uniformly coat.CL-20 compound productivities are up to 94.3%.Shown by mechanical sensitivity test, this reality The CL-20 explosive compounds impact sensitivity blast percentage for applying example preparation is reduced to 40% by the 100% of raw material, and friction sensitivity is quick-fried Fried percentage is reduced to 32% by the 100% of raw material.
Embodiment 2
(1) it is 65 DEG C by constant temperature water bath temperature setting, opens water circulation.The pure water for weighing 120g adds reactor, Stirring motor is opened, mixing speed 450r/min, load weighted 100g CL-20 is added in reactor and stirred, makes CL-20 Crystal is uniformly dispersed, and obtains explosive mixed liquor.
(2) in the pure petroleum ether of analysis that 2g No. 80 microwaxes are dissolved in into 18g, the microwax oil of mass concentration 10% is obtained Ethereal solution, it is stand-by.
2g fluororubber 23 11 (F2311) is dissolved in 38g analysis pure ethyl acetate, obtains the F2311 of mass concentration 5% Ethyl acetate solution, it is stand-by.
(3) explosive mixed liquor is warming up to 64-66 DEG C, opens vavuum pump and separate out air, adjusting pressure in kettle is 0.02Mpa, with 3mls-1Rate of addition be added dropwise microwax petroleum ether solution into reactor, evaporated by solvent, insensitiveness No. 80 microwaxes of agent, which separate out, is coated on CL-20 surfaces.After petroleum ether evaporation completely, CL-20 and microwax compound are obtained, then to 70 DEG C of water 80g are added in reactor, it is 2 to make water material mass ratio：1 (water be the dosage of water added by step 1 and 3 and, material refer to CL-20 Dosage).It is 70 DEG C to adjust reactor temperature, and adjustment speed of agitator is 900r/min, and holding reacting kettle inner pressure is 0.02Mpa, with 3mls-1Rate of addition F2311 ethyl acetate solution is added dropwise to reactor.After ethyl acetate evaporation, F2311 separates out the surface for being coated on CL-20 and microwax compound.
(4) after ethyl acetate evaporating completely, reactor temperature is reduced to less than 40 DEG C, by solid product centrifugation point From, washing, dry, produce CL-20 explosive compounds 90.9g.
The CL-20 explosive compounds that the present embodiment obtains are observed by electron-microscope scanning.CL-20 explosives surface by deterrent and High polymer binder uniformly coats.CL-20 explosives compound productivity is to 90.9%.Shown by mechanical sensitivity test, this implementation CL-20 explosive compounds impact sensitivity blast percentage prepared by example is reduced to 72% by the 100% of raw material, friction sensitivity blast Percentage is reduced to 80% by the 100% of raw material.
By two embodiments can be seen that it is of the same race under the conditions of, different high polymer binders cladding CL-20 explosives after make Mechanical sensitivity for the CL-20 explosive compounds gone out differs greatly.The CL- prepared using high polymer binder Estane5703 The impact sensitivity blast percentage of 20 explosive compounds is 52%, and friction sensitivity blast percentage is 40%, and utilizes macromolecule The impact sensitivity blast percentage of CL-20 explosive compounds prepared by binding agent F2311 is 72%, friction sensitivity blast percentage For 80%.So the explosive compound for selecting suitable binding agent low to processing machinery sensitivity with deterrent play it is vital Effect.
The foregoing is only presently preferred embodiments of the present invention, be not intended to limit the invention, it is all the present invention spirit and Within principle, any modification, equivalent substitution and improvements made etc., it should be included in the scope of the protection.

Claims (10)

  1. A kind of 1. method using plasticizing Estane5703 cladding CL-20 explosives, it is characterised in that including：
    1) deterrent microwax is dissolved in the first organic solvent, obtains the microwax solution that mass concentration is 10%-12%；
    High polymer binder Estane5703 and plasticizer DOP are dissolved in the second organic solvent, it is 5%-7% to obtain mass concentration The solution containing Estane5703 and DOP；
    2) by CL-20 and pure water by weight 1:1.1-1：1.3 are placed in aqueous suspension reactor, stirring, make CL-20 scattered equal It is even, explosive mixed liquor is obtained, explosive mixed liquor is warming up to 64-66 DEG C, vacuum is opened and air is pumped out, adjust reacting kettle inner pressure For 0.02Mpa, 1) gained microwax solution is added dropwise into explosive mixed liquor, by the first organic solvent evaporation, microwax separates out CL-20 surfaces are coated on, after the first organic solvent evaporation is complete, prepare CL-20 and microwax compound；
    3) add water into reactor, keep reacting kettle inner pressure, adjustment speed of agitator is 900r/min, adjusts reactor temperature To 59-61 DEG C, 1) solution of the gained containing Estane5703 and DOP is added, after the second organic solvent evaporation is complete, Estane5703 is coated on CL-20 and microwax compound surface, and solid product is centrifuged, washed, is dried, is produced CL-20 explosive compounds.
  2. 2. according to the method for claim 1, it is characterised in that in 1), the microwax is No. 80 microwaxes.
  3. 3. according to the method for claim 1, it is characterised in that in 1), first organic solvent is the pure oil of analysis Ether, second organic solvent are the pure chloroform of analysis.
  4. 4. according to the method for claim 1, it is characterised in that in 1), the mass ratio of the Estane5703 and DOP= 4:1, the Estane5703 is produced by Lubrizol Corp. of the U.S..
  5. 5. according to the method for claim 1, it is characterised in that in 2), the mixing speed is 450r/min.
  6. 6. according to the method for claim 1, it is characterised in that in 2), the microwax solution is into explosive mixed liquor The speed of dropwise addition is 3mls-1。
  7. 7. according to the method for claim 1, it is characterised in that in 2), the matter of microwax in the microwax solution of addition Amount accounts for the 2%-3% of CL-20 mass.
  8. 8. according to the method for claim 1, it is characterised in that add the quality of pure water in 2) and add the matter of water in 3) The proportionate relationship for measuring sum and CL-20 mass is 2:1.
  9. 9. according to the method for claim 1, it is characterised in that in 3), addition contains the molten of Estane5703 and DOP Estane5703 and DOP gross mass accounts for the 2%-3% of CL-20 mass in liquid.
  10. 10. according to the method for claim 1, it is characterised in that in 3), the solution containing Estane5703 and DOP to The speed being added dropwise in reactor is 3mls-1。
CN201610412668.6A 2016-06-14 2016-06-14 A kind of method using the plasticizing Estane5703 cladding explosives of CL 20 Expired - Fee Related CN106083494B (en)

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CN108250004B (en) * 2018-01-11 2020-04-14 北京理工大学 Modulus-adjustable ternary ethyl propyl composite insensitive binder and preparation method thereof
CN113024332B (en) * 2020-03-03 2022-04-19 西南科技大学 Process for the preparation of an explosive composition
CN113402345B (en) * 2021-05-26 2022-04-01 常州市范群干燥设备有限公司 Device for coating surface of explosive particles with desensitizer
CN113698266B (en) * 2021-09-09 2022-04-12 北京理工大学 Acidic inhibition type NTO-based mixed explosive molding powder and preparation method thereof
CN114907173B (en) * 2022-05-05 2023-03-24 中国工程物理研究院化工材料研究所 Explosive with strong sense-reducing coating layer structure and preparation method thereof

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