CN107698412A - Explosive eutectic preparation based on pneumatic nebulization antisolvent crystallisation - Google Patents
Explosive eutectic preparation based on pneumatic nebulization antisolvent crystallisation Download PDFInfo
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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
- C06B21/0033—Shaping the mixture
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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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Abstract
The invention discloses a kind of explosive eutectic preparation based on pneumatic nebulization antisolvent crystallisation, be will be envisaged for preparing eutectiferous two kinds of explosives be dissolved in it is a kind of have to two kinds of explosives solution altogether is formed close in the solvent of solubility, and a kind of solvent all insoluble to two kinds of explosives is selected as anti-solvent, common solution is acted on compressed gas, it is injected in after nozzle at high speeds sprays atomization in anti-solvent phase, make common solution and the abundant mixed at high speed of anti-solvent, crystallization separates out explosive eutectic ultra-fine grain.Preparation method of the present invention can realize the industrial volume production of cocrystallized explosive.
Description
Technical field
The invention belongs to energy-containing compound eutectic technical field, is related to a kind of eutectiferous preparation method of explosive, particularly
The eutectiferous method of explosive is prepared using pneumatic nebulization-antisolvent crystallisation.
Background technology
Energy-containing compound eutectic technology is combined from molecular level by different energy-containing compound molecules, to change intramolecular
Portion forms and crystal structure, is effectively improved oxygen balance and sensitivity, improves quick-fried heat, acting ability and the security of energy-containing compound,
Also other performances such as the dissolubility of energy-containing compound, fusing point, heat-resisting can be improved, meet modern weapons change system to high-energy insensitive
The requirement of ammunition, modern weapons power is improved, while ensure personnel and equipment safety.
Eutectic technology just starts to be applied in energetic material field in recent years.The preparation method of cocrystallized explosive has a variety of, bag
Include crystallisation by cooling method, solvent evaporated method, solvent/non-solvent method, sublimed method, fusion method, polishing etc..
Solvent evaporation method is to be dissolved in eutectic each component in solvent according to stoichiometric proportion, with the slow volatilization of solvent
Eutectic is obtained, changes little material mainly for solubility with temperature, can effectively control the pattern and size of crystallization, but
It is time-consuming longer.
(the Improved stability and smart-material functionality realized such as Bolton
in an energetic cocrystal [J]. Angewandte Chemie International Edition, 2011,
50(38):TNT and CL-20 cocrystallized explosive 8960-8963.) have been made using the method for the ethanol that volatilizees.
Yang Zongwei etc. (preparation, structure and performance [J] energetic materials of CL-20/TNT cocrystallized explosives, 2012,20
(6):CL-20/TNT cocrystallized explosives 674-679.) are prepared for solvent evaporation method, appropriate CL-20 and TNT are dissolved in acetic acid
Ethyl ester forms the clear crystals liquid of yellowish, slow solvent flashing, colourless prism-shaped CL-20/TNT eutectics is obtained after 5 days and are fried
Medicine, plane of crystal is smooth complete, uniform in size, 270 μm or so of average grain diameter.
Wang Yu equalitys (preparation of CL-20/DNB cocrystallized explosives and sign [J] energetic materials, 2013,21 (4):
CL-20/DNB eutectics 554-555.) have been synthesized using solvent evaporation method, CL-20 ethanol solutions are respectively configured and DNB ethanol is molten
Liquid, water white transparency crystal solution is mixed to form, is placed in constant incubator slowly crystallization about 10 days, you can obtain mol ratio as 1:1
Colourless prism-shaped CL-20/DNB cocrystallized explosives.
(preparation of 7 kinds of BTF eutectics and sign [J] energetic materials, 2012,20 (4) such as Guo Changyan: 503-504.)
5 kinds of eutectic systems such as BTF and TNT, TNB, TNA, MATNB and TNAZ have been synthesized with solvent evaporation method, and have obtained effective list
Brilliant data (Five Energetic Co-crystals of BTF by Intermolecular Hydrogen Bond and
π-Stacking Interactions [J]. Crystal Growth & Design, 2013, 13: 679-687.).Examination
Test and show, the eutectic sensitivity that BTF is formed with TNT, TNB declines to a great extent compared with BTF, obtains sensitivity and is less than RDX but explosion property
With RDX similar in New Explosives.
Solvent evaporation method can effectively obtain the eutectic of explosive, and weak point is time-consuming relatively long, and can not be selected
The big solvent of solubility, so be not easy to realize industry expansion prepared by eutectic.
Solvent/non-solvent method is the solubility principle according to material, and material is first dissolved in a certain solvent, and solution is carried out
A series of necessary operations such as stirring, then add non-solvent and analyse material in the form of crystallizing or be coated on other materials surface etc.
A kind of method gone out.
(the Preparation and characterization of a novel co-crystal such as Shen Jinpeng
explosive [J]. Crystal Growth & Design, 2011(11):1759-1765.) it is based on crystal life in solution
Theory is grown, has prepared HMX/TATB cocrystallized explosives using solvent/non-solvent method at room temperature, it is at a certain temperature, to incite somebody to action
HMX and TATB obtains mixed solution by certain mass than being dissolved in certain solvent, then by non-solvent within a certain period of time
Uniform stirring in mixed solution is slowly added into, makes two kinds of explosive molecules cocrystallization.
(preparation of HMX/AP eutectics and sign [J] energetic materials, 2013,21 (4) such as Chen Jie:It is 409-413.) sharp
Be prepared for HMX/AP eutectics with solvent/non-solvent method, weigh certain mass than HMX and AP be dissolved in DMSO solution, at 26 DEG C
Constant temperature adds a certain amount of mixing non-solvent, and the solution after being added dropwise to complete, which is placed in thermostatic control oscillator vibration, to be vibrated, and suction filtration obtains
Explosive eutectic.This method not only changes the particle diameter of crystal, and changes the pattern of crystal, but the particle diameter of crystal compares
Greatly, generally 20~60 μm.
Spray drying technology can make common solution be atomized into small droplet, increase its specific surface area.When droplet and hot gas
When body contacts, the volatilization of its solvent, moment high degree of supersaturation can be realized, shorten the growth course of crystal, advantageously formed ultra-fine common
Brilliant particle.
(the Formation of Cocrystals from Stoichiometric Solutions of such as Alhalaweh
Incongruently Saturating Systems by Spray Drying[J]. Crystal Growth & Design,
2010, 10(8): 3302-3305.；Theophylline Cocrystals Prepared by Spray Drying:
Physicochemical Properties and Aerosolization Performance[J]. AAPS
PharmSciTech, 2013, 14(1):Multi-medicament eutectic 265-276.) is prepared for using spray drying technology.
Li Hequn etc. (spray drying of ultra-fine CL-20/TNT cocrystallized explosives is prepared with characterizing [J] energetic materials,
2015, (11):1103-1106.) using acetone as solvent, ultra-fine CL-20/TNT cocrystallized explosives are made using spray drying process.
This method is substantially quick solvent evaporation method, on the basis of solvent evaporation method, makes common solution atomization into fine droplet,
By being contacted with high temperature hot gas body, solvent is set quickly to volatilize to obtain explosive eutectic.This method shortens the time of preparation process,
The ultra-fine cocrystallized explosive of 1~10 μm of particle diameter can be prepared.But its preparation process needs to use high temperature hot gas body to wave solvent
Hair, not only process conditions are complicated whard to control, and security can not ensure, constrain its popularization and application.
Energetic material is very sensitive to stimulations such as heat, electricity, friction, shock wave and shocks, for security consideration, general feelings
Under condition, the eutectic of energetic material is prepared using solution system, without being prepared using non-solution system.Therefore, it is above-mentioned
Cocrystallized explosive preparation method is substantially all also in laboratory stage, and eutectic speed is slow, and yield is small, also larger from practical application
Gap.
Meanwhile the thinning method of traditional cocrystallized explosive, there is also the problems such as complex process, broad particle distribution, effect is not
Enough ideals.
The content of the invention
The purpose of the present invention is that complex process present in explosive eutectic body technique, used time be longer, production for preparing at present
Measure the problem of relatively low, particle diameter is larger, there is provided a kind of explosive eutectic preparation based on pneumatic nebulization-antisolvent crystallisation, with
Being capable of the quick ultra-fine explosive eutectic of volume production prepared sizes.
For achieving the above object, the invention provides one kind to prepare the eutectiferous method of explosive as steps described below.
1）Eutectiferous two kinds of explosives will be envisaged for preparing it will be dissolved in a kind of solvent and form solution altogether, the solvent is to this
Two kinds of explosives have close solubility.
Same explosive, the different solubility in different solvents.Different explosives, the solubility in same solvent
Also it is variant.Therefore, different explosives tends not to reach saturation state simultaneously in same solvent, is also not required to reach simultaneously
Saturation state.The present invention uses according to solubility and explosive eutectic mechanism of two kinds of explosives in different solvents, selection is selected
To two kinds of more similar solvents of explosive solubility, according to the eutectiferous proportion of composing of explosive, two kinds of explosives are dissolved in solvent
In, make and be easily formed eutectiferous explosive solution altogether.Preferably, the concentration of the invention for controlling the explosive to be total to solution is
0.1~0.8mmol/mL.
It is highly preferred that the preparation temperature of the present invention control solution altogether will altogether at 25~35 DEG C, and in process for preparation
Solution vibrates 20~30min, to ensure being completely dissolved for explosive.
2）A kind of solvent all insoluble to above two explosive is selected as anti-solvent.
3）The solution altogether is acted on compressed gas, is injected in anti-solvent phase, makes after nozzle at high speeds sprays atomization
Solution and the abundant mixed at high speed of anti-solvent, crystallization separate out explosive eutectic ultra-fine grain altogether.
When the common solution of explosive driven by high speed compression gas passes through narrow and small nozzle, by high velocity air impact compress Cheng Wei
Small drop, into after anti-solvent phase, by near nozzle because high-speed gas act on the anti-solvent strong turbulence mixed at high speed to be formed,
Reach hypersaturated state using dissolubility difference of the solute in solvent and anti-solvent, solute is nucleated rapidly precipitation, is formed ultra-fine
Eutectic particle.
Wherein it is preferred to which it is 0.4~0.6MPa that the present invention, which controls the injection pressure of compressed gas, solution passes through nozzle altogether
Medicine speed of entering be 20~40mL.min-1。
4）Eutectic particle is isolated from anti-solvent phase, filters, dry, the ultra-fine explosive for obtaining 1~25 μm of particle diameter is total to
Crystal.
The present invention is by the way of pneumatic nebulization-antisolvent crystallisation, by the common solution of two kinds of explosives with the shape of pneumatic nebulization
Formula is sprayed obtains explosive eutectic into explosive anti-solvent phase, in this preparation process, it is necessary to consider solvent and anti-solvent species,
The problems such as rate of charge and crystallization temperature of two kinds of explosives, so that the preferable explosive eutectic of quality is prepared.
Similar for solubility and equimolar two kinds of components, its eutectiferous formation phasor is fairly simple, regular, altogether
The formation of crystal is relative to be easier to.And the phasor that solubility is differed when larger component forms eutectic is more complicated, it is not easy to see
Analysis is examined, eutectic is not easy to be formed.Therefore, in the preparation of cocrystallized explosive, should select as far as possible to each component solubility phase
To close solvent, to expand eutectic area as far as possible, the condition for being advantageous to eutectic generation is created.Recrystallisation solvent selected by the present invention
It is to consider determination by solubility qualitative test, and with reference to solvent cost and toxicity size.
The temperature of anti-solvent phase is the explosive temperature that solution is crystallized altogether., may when anti-solvent phase temperature is higher
Product granularity can be caused to become big, the explosive eutectic of ultra-fine grain diameter can not be obtained due to agglomeration.And the temperature of anti-solvent phase
Than it is relatively low when, the higher solvent of some freezing points just can not be taken into consideration, causes the selection of solvent and anti-solvent to be limited, and grasp
It is bigger to make difficulty.Preferably, the temperature control of the invention by anti-solvent phase is at 15~25 DEG C.
The key for selecting rate of charge is consistent with the proportion of composing of explosive eutectic, makes cloudy solution when contacting non-solvent,
Two kinds of Explosives are easier to be combined into eutectic precipitation.When Explosives mix in proportion in a solvent, tend not to reach simultaneously
To saturation state, saturation is also not required to.Saturation degree is relatively low, it is clear that do not allow to be also easy to produce crystallization and yield also can very little, and degree of supersaturation
Higher, temperature varies slightly just having one-component precipitation, causes the reduction of eutectic purity.Meanwhile solution concentration is excessive also easy
Crystal is separated out at jet pipe, blocks jet pipe.Pneumatic nebulization crystallisation is mainly the moment satiety contacted using solution with anti-solvent
With the rapid motive force for raising, forming crystallization process of degree.The present invention is consistent with eutectic proportion of composing in the ratio of two kinds of explosives
Under the premise of, the concentration control that explosive is total to solution in 0.1~0.8mmol/mL, can ensure between different Explosives molecules compared with
Strong interaction force accounts for principal element, and the adhesion of out-phase molecule is more than same molecules, make two kinds of out-phase molecules be easier with
The form of eutectic is incorporated in lattice, and is no longer combined with monomeric form, is effectively realized the maximization of eutectic, is reduced
The crystallization of one-component, it is easier to obtain the cocrystallized explosive of rock-steady structure.
Solution supersaturation is the necessary requirement that nucleus is formed, and during nucleus growth, must still it solution concentration is maintained slightly
Oversaturated state, a kind of concentration difference is established to be maintained between solution and crystal face, make the solute that preparation crystallizes out to crystal
Shift on surface.So solution supersaturation is the motive force of crystallization process.
During eutectiferous using pneumatic nebulization-antisolvent crystallisation legal system arming medicine, the common solution of two kinds of explosives exists
Under compressed gas effect, with certain injection pressure with enter medicine speed and pass through narrow and small nozzle, by high velocity air impact compress, mist
Fine droplet is melted into, after increasing specific surface area, is driven and is injected in anti-solvent phase by high speed compression gas.High speed compression gas meeting
The anti-solvent near nozzle is set to form strong turbulence so that into common solution and the abundant mixed at high speed of anti-solvent of anti-solvent phase, mistake
Saturation degree raises rapidly, and moment reaches hypersaturated state.Now, the competitiveness of main part out-phase molecule is more than shape between monomer
Into the ability of polymerization, and stronger interaction between out-phase molecule be present, as hydrogen bond action,p-πInteraction,π-πAccumulation
Effect and halogen bond effect etc. so that be no longer combined, but be incorporated in the form of eutectic same with monomeric form between molecule
In one lattice, so, two kinds of explosives are easier to combine to form the cocrystallized explosive of rock-steady structure.
And then although the degree of supersaturation of solution is bigger altogether, substantial amounts of nucleus can be separated out at the very start, due in nozzle
The solute particulate being just nucleated can be dispersed in anti-solvent phase by the strong turbulence being formed about in time, cause the continued growth of crystal grain by
The condition that cannot be fully grown to suppression, eutectic, will appear from homogeneous nucleation.And violent pneumatic nebulization makes small crystalline substance
Sharp impacts occur for grain, are not easy to condense, and so as to which rapid crystallization separates out, shorten the growth course of crystal.Now, the generation of nucleus
Speed is more than the growth rate of crystal, it is impossible to obtains large particle crystal, is advantageous to obtain the explosive eutectic of Ultra-fine
Grain.
Pneumatic nebulization-antisolvent crystallisation method of the present invention is the explosive insensitiveness that a kind of eutectic technology is combined with refinement technology
Compound technology of preparing.The technology reaches a certain degree of drop sense by forming explosive eutectic, while reduces eutectiferous granularity,
So as to further making the sensitivity of explosive reduce, make obtained properties of product more excellent, prepare speed soon and process safety.
Cocrystallized explosive pneumatic nebulization-antisolvent crystallisation method of the present invention is different from traditional cocrystallized explosive preparation side
Method, mainly using pneumatic high-voltage, the characteristics of crystallization and rapid crystallization is atomized, by the common solution moment spray fine of two kinds of explosives
And in anti-solvent moment reach spray pattern, quickly prepare explosive eutectic.Therefore, the inventive method can realize eutectic
The industrial volume production of explosive.
Brief description of the drawings
Fig. 1 is the pictorial diagram of CL-20/TNT explosives eutectic prepared by embodiment 1 and its raw material.
Fig. 2 is the microscope figure of CL-20/TNT eutectics.
Fig. 3 is the thermal performance test figure of CL-20/TNT eutectics and its raw material.
Fig. 4 is the pictorial diagram of CL-20/HMX explosives eutectic prepared by embodiment 2 and its raw material.
Fig. 5 is the microscope figure of CL-20/HMX eutectics.
Fig. 6 is the thermal performance test figure of CL-20/HMX eutectics and its raw material.
Embodiment
Following embodiments are only the preferred technical solution of the present invention, are not used to carry out any restrictions to the present invention.For
For those skilled in the art, the present invention can have various modifications and variations.Within the spirit and principles of the invention, made
Any modification, equivalent substitution and improvements etc., should be included in the scope of the protection.
Embodiment 1.
All larger to the solubility of two kinds of components of CL-20 and TNT and similar acetone is selected as solvent.Water is as conventional
Anti-solvent, wide material sources, and CL-20 and TNT is almost insoluble in water, therefore it is anti-solvent to select water.
CL-20 and two kinds of explosives of TNT are added in solvent acetone according to 1: 1 mol ratio, control solution temperature is at 30 DEG C
Left and right, 20~30min of sonic oscillation filter to being completely dissolved, obtain the CL-20 and TNT that total concentration is about 0.10mmol/mL
The common solution of explosive.
Under compressed gas effect, accelerate by nozzle, explosive is total to solution with 0.4MPa injection pressure, 30mL.min-1Jet velocity be atomized into small drop, be injected in 20 DEG C of aqueous phase, make explosive be total to solution and water carry out it is fully mixed at a high speed
Close, moment degree of supersaturation raises rapidly, and rapid crystallization separates out tiny CL-20/TNT eutectic particles.
Crystallization is the PROCESS FOR TREATMENT such as separated to, filtered, being dried, obtains the CL-20/TNT explosives that particle diameter is 10~20 μm
Eutectic.
Fig. 1 gives raw material CL-20, TNT and the preparation eutectiferous product pattern of CL-20/TNT explosives.Can from Fig. 1
To find out, raw material CL-20 is white powder material, and TNT is light yellow powder material, and the eutectic sample being prepared is then
For yellow crystal, there is obvious difference on exterior appearance with raw material, judgement forms a kind of novel substance.
Fig. 2 then provides lower 40 times eutectiferous crystal morphologies of CL-20/TNT explosives observed of microscope.Can by Fig. 2
To find out, eutectic is sheet of transparent crystal, has well-regulated structure, uniform size and smooth surface, and particle diameter is only
15~17 μm.After particle diameter diminishes, mechanical impacting sensitivity reduces.
The eutectiferous differential scanning calorimetric (DSC) of CL-20/TNT explosives that Fig. 3 is raw material CL-20, TNT and preparation is surveyed
Test result.From figure 3, it can be seen that the maximum endothermic peak temperature of test sample is 136.8 DEG C, compared to raw material TNT fusing point
78.4 DEG C improve 58 DEG C or so.And as temperature raises, there is two exothermic decomposition processes, its summit temperature difference in sample
For 224.1 DEG C and 254.1 DEG C, it is coincide with the hot property of CL-20/TNT eutectics, judgement sample is CL-20/TNT explosive eutectics.
Compared with raw material CL-20 and TNT exothermic maximum peak value, the exothermic peak of eutectic is changed, and changes two kinds of raw material groups
The thermal decomposition characteristic divided.
Embodiment 2.
CL-20 and two kinds of explosives of HMX are added in solvent acetone according to 2: 1 mol ratio, control solution temperature is at 30 DEG C
Left and right, 20~30min of sonic oscillation filter to being completely dissolved, obtain the CL-20 and HMX that total concentration is about 0.11mmol/mL
The common solution of explosive.
Under compressed gas effect, accelerate by nozzle, explosive is total to solution with 0.5MPa injection pressure, 40mL.min-1Jet velocity be atomized into small drop, be injected in 20 DEG C of aqueous phase, make explosive be total to solution and water carry out it is fully mixed at a high speed
Close, moment degree of supersaturation raises rapidly, and rapid crystallization separates out tiny CL-20/HMX eutectic particles.
Crystallization is the PROCESS FOR TREATMENT such as separated to, filtered, being dried, obtains the CL-20/HMX explosives that particle diameter is 1~10 μm and is total to
Crystal.
Fig. 4 gives raw material CL-20, HMX and the preparation eutectiferous product pattern of CL-20/HMX explosives.Can from Fig. 4
To find out, raw material CL-20 and HMX are white powder material, and the eutectic sample being prepared is white flaky crystals, with original
Material has obvious difference on exterior appearance, and judgement forms a kind of novel substance.
Fig. 5 then provides lower 40 times eutectiferous crystal morphologies of CL-20/HMX explosives observed of microscope.Can by Fig. 5
To find out, eutectic is block transparent crystal, has well-regulated structure, uniform size and smooth surface, and particle diameter is only about
For 6 μm.After particle diameter diminishes, mechanical impacting sensitivity reduces.
The eutectiferous differential scanning calorimetric (DSC) of CL-20/HMX explosives that Fig. 6 is raw material CL-20, HMX and preparation is surveyed
Test result.From fig. 6, it can be seen that endothermic peak do not occur in CL-20/HMX eutectics, 281.4 DEG C of the fusing point compared to raw material HMX is
Change.As temperature raises, there is the process of exothermic decomposition in eutectic, 241.3 DEG C of its summit temperature, with CL-20/HMX eutectics
Hot property coincide, judgement sample is CL-20/HMX explosive eutectics.With raw material CL-20 and HMX exothermic maximum peak value phase
Than the exothermic peak of eutectic is changed, and changes the thermal decomposition characteristic of two kinds of raw material components.
Embodiment 3.
All larger to the solubility of two kinds of components of HMX and NTO and similar acetone is selected as solvent.HMX and NTO is not
Chloroform is dissolved in, therefore it is anti-solvent to select chloroform.
HMX and two kinds of explosives of NTO are added in solvent acetone according to 1: 1 mol ratio, control solution temperature is on 30 DEG C of left sides
The right side, 20~30min of sonic oscillation are filtered to being completely dissolved, and obtain HMX that total concentration is about 0.12mmol/mL and NTO explosive
Solution altogether.
Under compressed gas effect, accelerate by nozzle, explosive is total to solution with 0.6MPa injection pressure, 40mL.min-1Jet velocity be atomized into small drop, be injected in 25 DEG C of chloroform phase, explosive is total to solution and anti-solvent and carry out
Abundant mixed at high speed, moment degree of supersaturation raise rapidly, and rapid crystallization separates out tiny HMX/NTO eutectic particles.
Crystallization is the PROCESS FOR TREATMENT such as separated to, filtered, being dried, obtains tiny HMX/NTO explosive eutectics.
Claims (7)
1. the explosive eutectic preparation based on pneumatic nebulization-antisolvent crystallisation, is to prepare explosive eutectic as steps described below
Body：
1）Eutectiferous two kinds of explosives will be envisaged for preparing it will be dissolved in a kind of solvent and form solution altogether, the solvent is to this two kinds
Explosive has close solubility；
2）A kind of solvent all insoluble to above two explosive is selected as anti-solvent；
3）The solution altogether is acted on compressed gas, is injected in anti-solvent phase, makes molten altogether after nozzle at high speeds sprays atomization
Liquid and the abundant mixed at high speed of anti-solvent, crystallization separate out explosive eutectic ultra-fine grain；
4）Eutectic particle is isolated from anti-solvent phase, filters, dry, obtain the ultra-fine explosive eutectic of 1~25 μm of particle diameter.
2. preparation method according to claim 1, it is characterized in that the concentration of the solution altogether is 0.1~0.8mmol/mL.
3. preparation method according to claim 1, it is characterized in that the injection pressure of the compressed gas be 0.4~
0.6MPa。
4. preparation method according to claim 1, it is characterized in that by the solution altogether with 20~40mL.min-1Enter medicine speed
Degree passes through nozzle.
5. preparation method according to claim 1, it is characterized in that preparing solution altogether under 25~35 DEG C of environment.
6. preparation method according to claim 1, it is characterized in that the temperature of the anti-solvent phase is 15~25 DEG C.
7. preparation method according to claim 1 or 5, it is characterized in that in the process for preparation of common solution, will be described molten altogether
Liquid vibrates 20~30min.
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| CN115466155A (en) * | 2022-08-30 | 2022-12-13 | 浙江工业大学 | LLM-105/AP energetic composite material and preparation method thereof |
| CN115677436A (en) * | 2021-07-28 | 2023-02-03 | 北京理工大学 | Hexanitrohexaazaisowurtzitane and nitroimidazole eutectic energetic material and preparation method thereof |
| CN115677459A (en) * | 2022-10-27 | 2023-02-03 | 山东博宏新化工科技有限公司 | Crystallization production process of methyl octabromoether |
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| CN115959956A (en) * | 2022-12-15 | 2023-04-14 | 南京理工大学 | TKX-50/AP eutectic crystal and preparation method thereof |
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