阅读说明：本技术 用于制备核壳结构含能材料的同轴静电喷雾装置及方法 (It is used to prepare the coaxial electrostatic spraying device and method of core-shell structure energetic material ) 是由 叶迎华 王悦听 许建兵 沈云 王成爱 张泽华 李福伟 于 2019-08-07 设计创作，主要内容包括：本发明属于含能材料领域,具体为一种用于制备核壳结构含能材料的同轴静电喷雾装置及方法。包括内层管,外层管,导电基底；内层管位于外层管内部且同轴设置,内层管和外层管的前端均为圆锥状,且内层管前端圆锥的锥角小于外层管前端圆锥的锥角,内层管的圆锥顶端位于外层管圆锥顶端上部；外层管圆锥部连接直流高压电源,外层管下部放置有导电基底；内层管和外层管分别连接驱动机构。该方法基于静电喷雾技术,利用含能粒子在溶液环境中具有良好的分散性和流动性的特点,可以将目标核层药剂引入核心层,而壳层药剂均匀包覆在核层上,实现药剂组分间的充分接触,位于壳层的药剂一定程度上还能起到保护核层药剂的作用。(The invention belongs to energetic material field, specially a kind of coaxial electrostatic spraying device for being used to prepare core-shell structure energetic material and method.Including inner tube, outer tube, conductive substrates；Inner tube is located inside outer tube and is coaxially disposed, and the front end of inner tube and outer tube is coniform, and the cone angle of inner tube front end circular cone is less than the cone angle of outer tube front end circular cone, and the cone tip of inner tube is located at outer tube cone tip top；Outer tube conus portion connects DC high-voltage power supply, and outer tube lower part is placed with conductive substrates；Inner tube and outer tube are separately connected driving mechanism.This method is based on electrostatic Spraying technique; have the characteristics that good dispersibility and mobility in solution environmental using energy-containing particle; target stratum nucleare medicament can be introduced into core layer; and shell medicament is evenly coated on stratum nucleare; coming into full contact between realization dosage component can also play the role of protecting stratum nucleare medicament to a certain extent positioned at the medicament of shell.)

1. a kind of coaxial electrostatic spraying device for being used to prepare core-shell structure energetic material, which is characterized in that including inner tube (4), outer tube (7), conductive substrates (10)；

The inner tube (4) is located at outer tube (7) inside and is coaxially disposed, and the front end of the inner tube (4) and outer tube (7) is equal To be coniform, and the cone angle of inner tube (4) front end circular cone is less than the cone angle of outer tube (7) front end circular cone, the inner tube (4) Cone tip is located at outer tube (7) cone tip top；

Outer tube (7) conus portion connects DC high-voltage power supply (8), and outer tube (7) lower part is placed with conductive substrates (10)；

The inner tube (4) and outer tube (7) are separately connected driving mechanism.

2. the apparatus according to claim 1, which is characterized in that the cone angle of inner tube (4) front end circular cone is 20-45 °, The cone angle of outer tube (7) front end circular cone is 90-120 °, and the cone tip of the inner tube (4) is located at outer tube (7) circular cone Top top 0.5-1mm.

3. the apparatus according to claim 1, which is characterized in that the outer layer hangs (7) lower part apart from conductive substrates (10) 8- 9cm。

4. the apparatus according to claim 1, which is characterized in that the voltage of the DC high-voltage power supply (8) is 18- 18.5kV。

5. the apparatus according to claim 1, which is characterized in that the driving mechanism is syringe and micro syringe pump.

6. device according to claim 5, which is characterized in that the driving mechanism specifically: inner tube (4) connection First syringe (2), the outer tube (7) connect the second syringe (5), first syringe (2) and the second syringe (5) Connect micro syringe pump.

7. the apparatus according to claim 1, which is characterized in that be dispersion phase dispersant liquid (3), institute in the inner tube (4) It states in outer tube (7) as mobile phase solution.

8. a kind of method for preparing core-shell structure energetic material using the described in any item devices of claim 1-7, feature exist In including the following steps:

Step (1): it prepares energetic material solution: energetic material being added in solvent, is placed on magnetic stirrer and stirs 1h It is completely dissolved to energetic material；

Step (2): prepare dispersed phase precursor liquid: it is molten that energetic material obtained by step (1) is added in core-shell structure target kernel reagent In liquid, ultrasound 0.5-2h reunites between breaking particle at 500W, 40kHz, is then placed on magnetic stirring apparatus and stirs 1h, obtains Destination scatter phase precursor liquid；

Step (3): preparation mobile phase precursor liquid: the target outershell reagents of core-shell structure are added to absolute ethanol, magnetic is placed in 0.5-1h is stirred on power blender, obtains mobile phase precursor liquid；

Step (4): coaxial electrostatic spraying device is built；

Step (5): electrostatic spray deposits target agent: opening high voltage power supply, the dispersion liquid and mobile phase solution in syringe exist Micro syringe pump effect is lower to be released, and is realized at coaxial syringe needle and is crossed and coat, and start electrostatic spray, final electrostatic spray product is heavy In product to the conductive substrates (10) in ground state.

9. according to the method described in claim 8, it is characterized in that, the energetic material in the step (1) is nitrocotton, gathers partially One of vinyl fluoride；The solvent is ethyl alcohol and ether or DMF and acetone, and the volume ratio of the ethyl alcohol and ether is 3:1, The volume ratio of the DMF and acetone is 7:3.

10. according to the method described in claim 9, it is characterized in that, the nitrogen content of nitrocotton is greater than in the step (1) 12%, Kynoar purity is 99.9%；The propulsion speed of dispersion liquid and mobile phase solution in the step (5) in syringe Degree is 2.5-3ml/h.

Technical field

The invention belongs to energetic material field, specially a kind of coaxial electrostatic spray for being used to prepare core-shell structure energetic material Mist device and method.

Background technique

Energetic material is high Energy Density Materials, and efficient igniting, detonation, propagation of explosion, driving can be provided for weapon system Equal power.The structure of energetic material is to influence the key factor of energetic material property, makes to realize more between energetic material dosage component It is the good approach for improving energetic material work done property efficiently to contact.Wherein core-shell structure can be realized in particle level contains energy Coming into full contact between material medicament is the modified research hotspot of medicament.

The preparation method for realizing core-shell structure medicament containing energy mainly includes vapor deposition, self assembly and in-situ polymerization etc.. Wherein vapour deposition process and situ aggregation method realization rate are cumbersome, single low yield；Autonomous dress method to a certain extent can be real Existing nucleocapsid clad structure, but structure is not sufficiently good, there is a problem of that core-shell structure fulfilling rate is low.In conclusion existing realization The means and method of Composite Energetic Materials core-shell structure many are lacked there are inefficiency or product core-shell structure are not ideal enough etc. Point.

Summary of the invention

The purpose of the present invention is to provide a kind of coaxial electrostatic spraying device for being used to prepare core-shell structure energetic material and Method.

The technical solution for realizing the aim of the invention is as follows:

A kind of coaxial electrostatic spraying device being used to prepare core-shell structure energetic material, including inner tube, outer tube are conductive Substrate；

The inner tube is located inside outer tube and is coaxially disposed, and the front end of the inner tube and outer tube is circular cone Shape, and the cone angle of inner tube front end circular cone is less than the cone angle of outer tube front end circular cone, the cone tip of the inner tube is located at outer Layer pipe cone tip top；

The outer tube conus portion connects DC high-voltage power supply, and the outer tube lower part is placed with conductive substrates；

The inner tube and outer tube are separately connected driving mechanism.

Further, the cone angle of inner tube front end circular cone is 20-45 °, and the cone angle of outer tube front end circular cone is 90-120 °, the cone tip of the inner tube is located at outer tube cone tip top 0.5-1mm.

Further, the outer layer hangs lower part apart from conductive substrates 8-9cm.

Further, the voltage of the DC high-voltage power supply is 18-18.5kV.

Further, the driving mechanism is syringe and micro syringe pump.

Further, the driving mechanism specifically: the inner tube connects the first syringe, the outer tube connection the Two syringes, first syringe and the second syringe connect micro syringe pump.

Further, it is dispersion phase dispersant liquid in the inner tube, is mobile phase solution in the outer tube.

A kind of method that above-mentioned device prepares core-shell structure energetic material, includes the following steps:

Step (1): it prepares energetic material solution: energetic material being added in solvent, is placed on magnetic stirrer and stirs It mixes 1h and is completely dissolved to energetic material；

Step (2): it prepares dispersed phase precursor liquid: the material containing energy obtained by step (1) is added in core-shell structure target kernel reagent Expecting in solution, ultrasound 0.5-2h reunites between breaking particle at 500W, 40kHz, and it is then placed on magnetic stirring apparatus and stirs 1h, Obtain destination scatter phase precursor liquid；

Step (3): preparation mobile phase precursor liquid: the target outershell reagents of core-shell structure are added to absolute ethanol, and are placed In stirring 0.5-1h on magnetic stirring apparatus, mobile phase precursor liquid is obtained；

Step (4): coaxial electrostatic spraying device is built；

Step (5): electrostatic spray deposits target agent: opening high voltage power supply, the dispersion liquid and flowing in syringe mix Liquid is released under micro syringe pump effect, is realized at coaxial syringe needle and is crossed and coat, and electrostatic spray is started, and final electrostatic spray produces Object deposits in the conductive substrates in ground state.

Further, the energetic material in the step (1) is one of nitrocotton, Kynoar；Described is molten Agent is ethyl alcohol and ether or DMF and acetone, and the volume ratio of the ethyl alcohol and ether is 3:1, and the volume ratio of the DMF and acetone is 7:3。

Further, the nitrogen content of nitrocotton is greater than 12% in the step (1), and Kynoar purity is 99.9%； The fltting speed of dispersion liquid and mobile phase solution in the step (5) in syringe is 2.5-3ml/h.

Compared with prior art, the present invention its remarkable advantage is:

(1) the purpose of the present invention is to provide a kind of coaxial electrostatic spraying device for preparing core-shell structure energetic material and sides Method, this method are based on electrostatic Spraying technique, using energy-containing particle with good dispersibility and mobility in solution environmental Core-shell structure target stratum nucleare medicament can be introduced core layer by feature, and shell medicament is evenly coated on stratum nucleare, realizes medicament Coming into full contact between component can also play the role of protecting stratum nucleare medicament to a certain extent positioned at the medicament of shell.

(2) it is high accurately to control the partial size core coefficient of dispersion, reproducibility for this method.

(3) this method can effectively prepare core-shell structure energetic material, and by control experimental material and experiment parameter, can To change the thickness of shell and stratum nucleare.

Detailed description of the invention

Fig. 1 is electrostatic atomizer schematic diagram of the invention.

Description of symbols:

1- micro syringe pump, the first syringe of 2-, 3- disperse phase dispersant liquid, 4- inner tube, the second syringe of 5-, 6- mobile phase Solution, 7- outer tube, 8- DC high-voltage power supply, 9- electrostatic spray product, 10- conductive substrates.

Specific embodiment

Present invention is further described in detail with reference to the accompanying drawing.

As shown in Figure 1, drawing electrostatic spray dispersion phase dispersant liquid 3 and stream respectively with the first syringe 2, the second syringe 5 Dynamic phase solution 6, is placed in micro syringe pump 1, the first syringe 2 is connected to coaxial inner tube 4, the second syringe 5 is connected to Coaxial outer tube 7, conductive substrates 10 is grounded, to enable solvent to volatilize completely, to the distance between conductive substrates at coaxial syringe needle It is set as 8~9cm.Using DC high-voltage power supply 8 to the high pressure for applying 18~18.5kV at coaxial syringe needle, micro syringe pump is opened, Precursor liquid in first syringe 2, the second syringe 5 is pushed out respectively is sent into inner tube 4 and outer tube 7, inner tube dispersion liquid Converge at coaxial syringe needle with outer tube solution, solution realizes the packet to dispersion liquid in inner tube 4 at syringe needle in outer tube 7 It covers.Charged drop is formed under the action of high voltage power supply simultaneously, charged drop is under the action of electric field force in ground state Conductive substrates movement, in motion process, solvent constantly volatilizees, and after solvent volatilization completely, electrostatic spray product deposition is to conductive In substrate.

It is specific the preparation method is as follows:

Step A prepares energetic material solution: energetic material being added in the solvent of certain volume ratio, is placed in magnetic force and stirs It mixes and stirs 1h on machine and be completely dissolved to energetic material；The energetic material is one of nitrocotton, Kynoar, described Solvent and corresponding volume ratio be respectively ethyl alcohol: ether (3:1) or DMF: acetone (7:3)；

Step B prepares dispersed phase precursor liquid: nitrocotton obtained by step A is added in core-shell structure target kernel medicament particle In (Kynoar) solution, ultrasound 1h reunites between breaking particle at 500W, 40kHz, is then placed on magnetic stirring apparatus 1h is stirred, destination scatter phase precursor liquid is obtained；

Step C prepares mobile phase precursor liquid: core-shell structure target shell medicament being added to absolute ethanol, magnetic is placed in 30min is stirred on power blender obtains mobile phase precursor liquid；

Step D builds coaxial electrostatic spraying device: drawing dispersed phase and continuous phase precursor liquid respectively with syringe, respectively It is placed in micro syringe pump, is then separately connected on coaxial inner layer pipe and outer layer pipe, constant flow high pressure power supply is passed through into gold Belong to conducting wire to be connected with needle portion, aluminum foil substrate ground connection, adjustment syringe needle to substrate to suitable distance；

Step E, electrostatic spray deposit target agent: opening high voltage power supply, the dispersion liquid and solution in syringe are in micro- note It penetrates under pumping action and releases, realized at coaxial syringe needle and cross and coat, start electrostatic spray process, final electrostatic spray product is heavy In product to the conductive substrates in ground state.

The nitrogen content of the nitrocotton and Kynoar, nitrocotton is greater than 12%, and Kynoar purity is 99.9%.

A kind of device and method preparing core-shell structure energetic material, the dispersed phase precursor liquid is by nucleocapsid The suspension of energetic material and organic solvent composition in structural object core.

A kind of device and method preparing core-shell structure energetic material, the mobile phase are by core-shell structure mesh Mark the solution of shell energetic material core organic solvent composition.

A kind of device and method preparing core-shell structure energetic material, the coaxial electrostatic spraying device Outer layer pipe and inner layer pipe have reserved certain space in the junction of conical syringe needle, wherein inner layer pipe needle tip angle It is 20~45 °, outer layer pipe needle tip angle is 90~120 °, and distance is 0.5~1mm between the two top.

A kind of device and method preparing core-shell structure energetic material, target agent precursor liquid is in micro syringe pump In fltting speed be 2.5-3ml/h.

A kind of device and method preparing core-shell structure energetic material, being applied to needle portion pressure is 18- 18.5kV。

A kind of device and method preparing core-shell structure energetic material, syringe needle arrive the distance between aluminum foil substrate For 8-9cm.