3,3 '-diamino -4, the thinning method of 4 '-azoxy furazan explosive crystals
Technical field
The present invention relates to energetic material field, especially 3,3 '-diamino -4,4 '-azoxy furazan explosive crystals
Thinning method.
Background technique
Slapper detonator for nuclear weapon is the ignition tool with high-performance, high safety.Slapper detonator is with originating
Medicine should have the characteristics that sensitivity is lower, service performance is good, detonation threshold value is low, detonation energy is high and thermostability is good.3,3'- diamino
Base -4,4'- azoxy furazan (DAOAF) is Typical Representative substance in furazan class explosive.But DAOAF rubs to insensitiveness is hit
It is insensitive with electrostatic spark.In recent years, both at home and abroad to RDX (ring trimethylene/trintriamine, popular name hexogen), HMX, HNS (six
Nitro late-maturing) and the multicharges such as TATB (- three amido benzene of trinitro-) carry out the control of pattern and granularity.But it there is no both at home and abroad so far
The relevant report controlled about DAOAF pattern and granularity.
Summary of the invention
The technical problem to be solved by the present invention is in order to solve existing DAOAF to shock insensitiveness, friction and electrostatic spark
Insensitive deficiency, the present invention provides a kind of 3,3 '-diamino -4, the thinning method of 4 '-azoxy furazan explosive crystals,
By further smashing using injection anti-solvent method fast eliminating solvent, while using stirring and ultrasound, it is easier to realize that DAOAF is brilliant
The efficient refinement of body particle.This method is easy to operate, and equipment easily obtains, and the DAOAF of different-grain diameter can be obtained by different operation
Crystal, so that preferably control obtains the crystal of the different-grain diameter of DAOAF.DAOAF after refinement has preferable particle shape, grain
Diameter range is between 500nm to 1 μm.Crystal purity is greater than 99.6%.Meanwhile DAOAF is special as a kind of comprehensive comparison
Energetic material.DAOAF is in Slapper detonator with originate in medicine, high energy composite explosives and high-energy solid propellant will tool after refinement
There is preferable development prospect.
The technical solution adopted by the present invention to solve the technical problems is:
A kind of 3,3 '-diamino -4, the thinning method of 4 '-azoxy furazan explosive crystals, comprising the following steps:
(1) DAOAF solution will be formed after raw material DAOAF and dimethyl sulfoxide DMSO ultrasonic dissolution, and DAOAF solution is fallen
Enter atomizer;
(2) nitrogen pressurization is opened, DAOAF solution is formed into small droplet by atomizer and when non-solvent contacts, super
DAOAF particle is precipitated in crystallization rapidly under the action of sound stirring;
(3) it will filter, and be dried in vacuo after DAOAF particle stirring ultrasound;
(4) DAOAF after recrystallization is carried out to carry out granularity and shape using laser particle analyzer and scanning electron microscope SEM
Looks characterization.
Specifically, the DAOAF solution concentration is 3%.
Specifically, the atomizer bore is 0.8mm or 1mm or 1.2mm.
Specifically, the nitrogen pressure is 0.4~0.6MPa.
Specifically, the ratio of the DAOAF solution and non-solvent is 1:40.
Specifically, the non-solvent is deionized water.
Specifically, it is 450r/min that speed, which is mixed, in the DAOAF solution and non-solvent.
Specifically, the DAOAF solution and non-solvent mixing time are 45min, and non-solvent temperature is 10 degrees Celsius.
The beneficial effects of the present invention are: the present invention provides a kind of 3,3 '-diamino -4,4 '-azoxy furazan explosives
The thinning method of crystal, by further being smashed using injection anti-solvent method fast eliminating solvent, while using stirring and ultrasound,
It is easier to realize the efficient refinement of DAOAF crystal grain.This method is easy to operate, and equipment easily obtains, and can be obtained by different operation
The DAOAF crystal of different-grain diameter, so that preferably control obtains the crystal of the different-grain diameter of DAOAF.DAOAF after refinement have compared with
Good particle shape, particle size range is in 50nm between 200nm.Crystal purity is greater than 98.5%.Meanwhile DAOAF is as a kind of
The special energetic material of comprehensive comparison.DAOAF is in Slapper detonator with originating medicine, high energy composite explosives and high energy after refinement
There to be preferable development prospect in solid propellant.
Detailed description of the invention
Present invention will be further explained below with reference to the attached drawings and examples.
Fig. 1 is DAOAF feed particles distribution map of the invention;
Fig. 2 is the distribution of particles figure of DAOAF crystal after refinement of the invention;
Fig. 3 is the XRD diagram of DAOAF after refinement of the invention;
Specific embodiment
In conjunction with the accompanying drawings, the present invention is further explained in detail.
Fig. 1 is DAOAF feed particles distribution map of the invention, and Fig. 2 is the particle point of DAOAF crystal after refinement of the invention
Butut, Fig. 3 are the XRD diagram of DAOAF after refinement of the invention.
A kind of 3,3 '-diamino -4, the thinning method of 4 '-azoxy furazan explosive crystals, comprising the following steps:
(1) DAOAF solution will be formed after raw material DAOAF and dimethyl sulfoxide DMSO ultrasonic dissolution, and DAOAF solution is fallen
Enter atomizer;
(2) nitrogen pressurization is opened, DAOAF solution is formed into small droplet by atomizer and when non-solvent contacts, super
DAOAF particle is precipitated in crystallization rapidly under the action of sound stirring;
(3) it will filter, and be dried in vacuo after DAOAF particle stirring ultrasound;
(4) DAOAF after recrystallization is carried out to carry out granularity and shape using laser particle analyzer and scanning electron microscope SEM
Looks characterization.
The DAOAF solution concentration is 3%.The atomizer bore is 0.8mm or 1mm or 1.2mm.The nitrogen pressure
It is by force 0.4~0.6MPa.The ratio of the DAOAF solution and non-solvent is 1:40.The non-solvent is deionized water.It is described
It is 450r/min that speed, which is mixed, in DAOAF solution and non-solvent.The DAOAF solution is with non-solvent mixing time
45min, non-solvent temperature are 10 degrees Celsius.
Detecting instrument:
1. field emission scanning electron microscope;
2. laser particle analyzer;
3. high performance liquid chromatograph.
Embodiment one:
Raw material DAOAF is dissolved in dimethyl sulfoxide DMSO first, it is super according to the ratio of DAOAF (g) 3:DMSO (ml) 11
Sound is until be completely dissolved into DAOAF solution, and DAOAF solution is poured into the atomizer that diameter is 0.8mm.
Then it opens nitrogen to pressurize, pressure value 0.6MPa makes DAOAF solution form small droplet by atomizer
Contacted with non-solvent deionized water, rapidly crystallization be precipitated DAOAF particle, while ultrasound and with the mixing speed of 450r/min stirring
45min.Last filtering vacuum is dry.Laser particle analyzer and SEM is recycled to carry out granularity and pattern table to the DAOAF after recrystallization
Sign.
Embodiment two:
It raw material DAOAF and will be dissolved in dimethyl sulfoxide DMSO first, extremely according to the stirring of DAOAF (g) 3:DMSO (ml) 11
It is completely dissolved into DAOAF solution, and DAOAF solution is poured into the atomizer that diameter is 1mm.
Then open nitrogen pressurize, pressure value 0.6MPa, make DAOAF solution by atomizer formed droplet with
Deionized water contact, ultrasound simultaneously stir 45min with the mixing speed of 450r/min.Finally DAOAF particle and drying is precipitated in crystallization.
The advanced instrument and equipments such as scanning electron microscope, laser particle size analysis are recycled to be analyzed and characterized.
Embodiment two:
It raw material DAOAF and will be dissolved in dimethyl sulfoxide DMSO first, extremely according to the stirring of DAOAF (g) 3:DMSO (ml) 11
It is completely dissolved into DAOAF solution, and DAOAF solution is poured into the atomizer that diameter is 1.2mm.
Then open nitrogen pressurize, pressure value 0.6MPa, make DAOAF solution by atomizer formed droplet with
Deionized water contact, ultrasound simultaneously stir 45min with the mixing speed of 450r/min.Finally DAOAF particle and drying is precipitated in crystallization.
The advanced instrument and equipments such as scanning electron microscope, laser particle size analysis are recycled to be analyzed and characterized.
Example IV:
It raw material DAOAF and will be dissolved in dimethyl sulfoxide DMSO first, extremely according to the stirring of DAOAF (g) 3:DMSO (ml) 11
It is completely dissolved into DAOAF solution, and DAOAF solution is poured into the atomizer that diameter is 0.8mm.
Then open nitrogen pressurize, pressure value 0.4MPa, make DAOAF solution by atomizer formed droplet with
Deionized water contact, ultrasound simultaneously stir 45min with the mixing speed of 450r/min.Finally DAOAF particle and drying is precipitated in crystallization.
The advanced instrument and equipments such as scanning electron microscope, laser particle size analysis are recycled to be analyzed and characterized.
Embodiment five:
It raw material DAOAF and will be dissolved in dimethyl sulfoxide DMSO first, extremely according to the stirring of DAOAF (g) 3:DMSO (ml) 11
It is completely dissolved into DAOAF solution, and DAOAF solution is poured into the atomizer that diameter is 1mm.
Then open nitrogen pressurize, pressure value 0.4MPa, make DAOAF solution by atomizer formed droplet with
Deionized water contact, ultrasound simultaneously stir 45min with the mixing speed of 450r/min.Finally DAOAF particle and drying is precipitated in crystallization.
The advanced instrument and equipments such as scanning electron microscope, laser particle size analysis are recycled to be analyzed and characterized.
Embodiment six:
It raw material DAOAF and will be dissolved in dimethyl sulfoxide DMSO first, extremely according to the stirring of DAOAF (g) 3:DMSO (ml) 11
It is completely dissolved into DAOAF solution, and DAOAF solution is poured into the atomizer that diameter is 1.2mm.
Then open nitrogen pressurize, pressure value 0.6MPa, make DAOAF solution by atomizer formed droplet with
Deionized water contact, ultrasound simultaneously stir 45min with the mixing speed of 450r/min.Finally DAOAF particle and drying is precipitated in crystallization.
The advanced instrument and equipments such as scanning electron microscope, laser particle size analysis are recycled to be analyzed and characterized.
Embodiment seven:
It raw material DAOAF and will be dissolved in dimethyl sulfoxide DMSO first, extremely according to the stirring of DAOAF (g) 3:DMSO (ml) 11
It is completely dissolved into DAOAF solution, and DAOAF solution is poured into the atomizer that diameter is 0.8mm.
Then open nitrogen pressurize, pressure value 0.6MPa, make DAOAF solution by atomizer formed droplet with
Deionized water contact stirs 45min without using the mode of ultrasound with the mixing speed of 450r/min.Finally DAOAF is precipitated in crystallization
Particle and drying.The advanced instrument and equipments such as scanning electron microscope, laser particle size analysis are recycled to be analyzed and characterized.
Embodiment eight:
It is formed after DAOAF and DMSO is carried out ultrasonic dissolution according to the ratio of DAOAF (g) 3:DMSO (ml) 11 first
DAOAF solution, and DAOAF solution is poured into the atomizer that diameter is 0.8mm.
Then open nitrogen pressurize, pressure value 0.6MPa, make DAOAF solution by atomizer formed droplet with
Deionized water contact, only ultrasound does not stir and finally crystallizes precipitation DAOAF particle and drying.Recycle scanning electron microscope, laser particle size
The advanced instrument and equipments such as analysis are analyzed and characterized.
Embodiment nine:
It is formed after DAOAF and DMSO is carried out ultrasonic dissolution according to the ratio of DAOAF (g) 3:DMSO (ml) 11 first
DAOAF solution, and DAOAF solution is poured into the atomizer that diameter is 0.8mm.
Then open nitrogen pressurize, pressure value 0.6MPa, make DAOAF solution by atomizer formed droplet with
Deionized water contact, ultrasound simultaneously finally crystallize precipitation DAOAF particle and drying with the mixing speed of 50r/min stirring 45min..
The advanced instrument and equipments such as scanning electron microscope, laser particle size analysis are recycled to be analyzed and characterized.
Embodiment ten:
It is formed after DAOAF and DMSO is carried out ultrasonic dissolution according to the ratio of DAOAF (g) 3:DMSO (ml) 11 first
DAOAF solution, and DAOAF solution is poured into the atomizer that diameter is 0.8mm.
Then open nitrogen pressurize, pressure value 0.6MPa, make DAOAF solution by atomizer formed droplet with
Deionized water contact, ultrasound simultaneously finally crystallize precipitation DAOAF particle and drying with the mixing speed of 200r/min stirring 45min..
The advanced instrument and equipments such as scanning electron microscope, laser particle size analysis are recycled to be analyzed and characterized.
Embodiment 11:
It is formed after DAOAF and DMSO is carried out ultrasonic dissolution according to the ratio of DAOAF (g) 3:DMSO (ml) 11 first
DAOAF solution, and DAOAF solution is poured into the atomizer that diameter is 0.8mm.
Then open nitrogen pressurize, pressure value 0.6MPa, make DAOAF solution by atomizer formed droplet with
Deionized water contact, ultrasound simultaneously finally crystallize precipitation DAOAF particle and drying with the mixing speed of 450r/min stirring 10min..
The advanced instrument and equipments such as scanning electron microscope, laser particle size analysis are recycled to be analyzed and characterized.
Taking the above-mentioned ideal embodiment according to the present invention as inspiration, through the above description, relevant staff is complete
Various changes and amendments can be carried out without departing from the scope of the technological thought of the present invention' entirely.The technology of this invention
Property range is not limited to the contents of the specification, it is necessary to which the technical scope thereof is determined according to the scope of the claim.
The shape appearance figure and DAOAF raw material phase of DAOAF crystal grain after refinement are made using the method for embodiment 1 by the present invention
Than.Raw material DAOAF crystal grain size distribution is uneven and the equal disunity of form, the crystal morphology of the DAOAF after refinement have occurred
It is apparent to change.By anti-solvent method DAOAF is recrystallized first, while being beaten by crystal under the action of ultrasound and stirring
Broken, formation particle is uniformly dispersed and the preferable crystal grain of form.
In conjunction with shown in attached drawing 1 and attached drawing 2, respectively raw material DAOAF and refinement after DAOAF crystal distribution of particles figure.From
It can be seen that raw material DAOAF granule crystal size is larger in figure, average grain diameter is about for 182.528nm or so.And it uses and implements
The partial size that method in example 1 obtains after refining DAOAF obviously becomes smaller, and average grain diameter is about for 108.213nm or so.
Attached drawing 2 and attached drawing 3 respectively indicate the XRD diagram of DAOAF after raw material DAOAF and refinement.As can be seen from the figure it refines
Front and back crystalline form is consistent.
The chemical purity of refinement front and back DAOAF crystal is analyzed using the method for high performance liquid chromatography, respectively
97.74% and 97.35%.Illustrate that still there is high chemical purity using the DAOAF crystal of this method refinement.It can satisfy use
It is required that.