CN110066210B - Preparation method of core-shell type nano metal silver and explosive compound - Google Patents
Preparation method of core-shell type nano metal silver and explosive compound Download PDFInfo
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- CN110066210B CN110066210B CN201910339480.7A CN201910339480A CN110066210B CN 110066210 B CN110066210 B CN 110066210B CN 201910339480 A CN201910339480 A CN 201910339480A CN 110066210 B CN110066210 B CN 110066210B
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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
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- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B33/00—Compositions containing particulate metal, alloy, boron, silicon, selenium or tellurium with at least one oxygen supplying material which is either a metal oxide or a salt, organic or inorganic, capable of yielding a metal oxide
- C06B33/08—Compositions containing particulate metal, alloy, boron, silicon, selenium or tellurium with at least one oxygen supplying material which is either a metal oxide or a salt, organic or inorganic, capable of yielding a metal oxide with a nitrated organic compound
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- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B33/00—Compositions containing particulate metal, alloy, boron, silicon, selenium or tellurium with at least one oxygen supplying material which is either a metal oxide or a salt, organic or inorganic, capable of yielding a metal oxide
- C06B33/08—Compositions containing particulate metal, alloy, boron, silicon, selenium or tellurium with at least one oxygen supplying material which is either a metal oxide or a salt, organic or inorganic, capable of yielding a metal oxide with a nitrated organic compound
- C06B33/10—Compositions containing particulate metal, alloy, boron, silicon, selenium or tellurium with at least one oxygen supplying material which is either a metal oxide or a salt, organic or inorganic, capable of yielding a metal oxide with a nitrated organic compound the compound being an aromatic
Abstract
The invention discloses a preparation method of a core-shell type nano metal silver and explosive compound, which comprises the following steps: (1) adding explosive powder into a dopamine-Tris aqueous solution, stirring, carrying out suction filtration, washing with deionized water, and carrying out vacuum drying; (2) preparing a silver nitrate solution, adding ammonia water for regulation to prepare a silver ammonia solution, and adding a surfactant into the silver ammonia solution; (3) ultrasonically dispersing the explosive powder obtained in the step (1) in water, and then adding the explosive powder into the mixed suspension obtained in the step (2); (4) adding a formaldehyde solution into the solution obtained in the step (3) while shaking uniformly, putting the mixed suspension into a water bath at a certain temperature, standing for a certain time, then shaking the mixture, carrying out suction filtration, and carrying out vacuum drying to obtain the core-shell type nano metal silver and explosive compound. According to the invention, the poly-dopamine layer is coated on the surface of the explosive powder in advance, so that the silver is promoted to be uniformly deposited on the surface of the dopamine, and the silver particles are ensured to be completely deposited on the surface of the explosive, not to be independently aggregated and not to fall off after coating.
Description
Technical Field
The invention relates to a preparation method of an explosive, in particular to a preparation method of a core-shell type nano metal silver and explosive compound, belonging to the field of energetic composite materials.
Background
High energy energetic materials are a continuing goal in the propellant and explosive arts. The effective means for improving the energy release of the energetic material is realized by adding catalytic materials such as metal, metal oxide and the like into the energetic composite. At present, there are many metals such as Al, Mg, B, W, Zr, Ni, Cu, Fe, Ag, Co, In, Pt and the like, and Pb3O4、CuO、Fe2O3Metal oxides for increasing energy contentEnergy release from materials (progression in Energy and Science 2016,57, 75-136). For example, Ting An et al prepared Cu2O-Bi2O3the/GO nano catalyst has a catalytic effect on RDX-CMDB propellant (Propellants applications. Pyrotech.2018,43, 1087-. In the preparation of the composite of the nano-catalyst and the energetic material, the prior art mainly adopts methods such as solid-phase reaction, electrolysis, hydrothermal reaction, precipitation, hydrolysis, sol-gel method and the like to prepare the nano-catalyst, and then the nano-catalyst and the energetic material are compounded to prepare the energetic composite. However, the nano material is easy to agglomerate, and the surface polarity of the nano metal is different from that of the energetic material, so that the dispersibility in the compounding process is poor, and the catalytic combustion efficiency of the energetic compound is low. If the nano metal and the energetic crystal are assembled into a core-shell structure, the problem of dispersibility in the energetic compound can be well solved, and the catalytic efficiency of the nano metal on the energetic material is effectively improved. At present, the report of the preparation method of the core-shell type nanometer metal and energetic material is not seen.
Disclosure of Invention
The invention aims to provide a preparation method of a core-shell type nano metallic silver and explosive compound, aiming at the problem of uneven dispersion of nano metal and energetic materials in the existing nano metal and energetic compound. The silver ion solution is used for in-situ coating reduction of the energetic crystal to form a perfect core-shell structure.
The purpose of the invention is realized by the following technical scheme:
a preparation method of a core-shell type nano metallic silver and explosive compound comprises the following steps:
(1) adding explosive powder into a dopamine-Tris aqueous solution with the pH value of about 8.5, stirring at the speed of 300-500 rpm for a period of time, carrying out suction filtration, washing for 5 times by using deionized water, and carrying out vacuum drying for 8-12 hours at the temperature of 60 ℃;
(2) preparing a silver nitrate solution with a certain concentration, adding ammonia water for regulation to prepare a silver ammonia solution, and adding 1-2 drops of a surfactant into the silver ammonia solution;
(3) ultrasonically dispersing the explosive powder obtained in the step (1) in water for 0.5-2.0 min, and then adding the explosive powder into the mixed suspension obtained in the step (2);
(4) adding a formaldehyde solution into the solution obtained in the step (3) while shaking uniformly, putting the mixed suspension into a water bath at a certain temperature, standing for 2-10 min, shaking the mixture, performing suction filtration, and performing vacuum drying at 40-50 ℃ for 8-12 hours to obtain the core-shell type nano metallic silver and explosive compound.
The further scheme is as follows:
the explosive powder is a water-insoluble explosive and comprises octogen (HMX), 1-oxygen-diamino-3, 5-dinitropyrazine (LLM-105), 1-diamino-2, 2-dinitroethylene explosive (FOX-7), hexanitrohexaazaisopentane (CL-20) and 1,3, 5-triamino-1, 3, 5-trinitrobenzene (TATB), and the particle size of the explosive powder is 5-100 mu m.
The further scheme is as follows:
in the step (1), the dopamine is prepared from dopamine hydrochloride, the concentration of a dopamine-Tris aqueous solution is 2-5 g/L, the mass ratio of explosive powder to dopamine is 4-10, the stirring speed is 300-500 rpm, and the stirring time is 0.5-1 hour.
The further scheme is as follows:
in the step (2), the silver-ammonia solution is a mixed solution of silver nitrate and ammonia water, the concentration of the silver nitrate is 0.1-0.5 mol/L, the surfactant is one of polyvinylpyrrolidone (PVP), alkylphenol polyoxyethylene ether (OP-10) and polyoxyethylene sorbitan monolaurate (Tween-20), and the mass ratio of the surfactant to the explosive is (1: 500) - (1: 200).
The further scheme is as follows:
the frequency of ultrasonic dispersion in the step (3) is 25 KHz-40 KHz.
The further scheme is as follows:
in the step (4), the molar number of the formaldehyde is 3-8 of the molar number of the silver ions, the concentration of the formaldehyde solution is 20wt%, the water bath temperature is 70-75 ℃, and the mass fraction of the silver in the core-shell type nano metal silver and explosive compound is 2-10%.
The reaction principle of the present invention is illustrated below:
the purpose of the step (1) is to control the polydopamine coating condition, so that a small amount of polydopamine is coated on the surface of the explosive powder tightly and uniformly. The coating amount of the polydopamine is positively correlated with the concentration of the solution and the coating time, and the higher the concentration of the solution is or the longer the coating time is, the higher the coating amount of the polydopamine is; on the other hand, the solution concentration, the coating time and the stirring speed also influence the coating tightness of the polydopamine on the surface of the explosive. For example, if the concentration of the solution is too low, polydopamine is not uniformly coated on the surface of the explosive; the concentration of the solution is too high, and polydopamine is independently agglomerated and is not tightly coated. The stirring time is too long, the polydopamine coating amount is too large, the non-energetic shell layer on the surface of the explosive is too thick, and the catalytic energy release of the metal silver in the energetic compound to the explosive is not facilitated. Therefore, the optimized coating conditions in the step (1) are that the concentration of the dopamine aqueous solution is 2 g/L-5 g/L, the mass ratio of the explosive powder to the dopamine is 200-500, the stirring speed is 300 rpm-500 rpm, and the stirring time is 0.5 h-1 h.
And (3) preparing a silver ammonia solution by the aid of the step (2). The ammonia is added dropwise, a yellow precipitate is formed firstly, then the solution becomes a brown precipitate, and then the ammonia is stopped when the solution becomes clear and transparent.
The formaldehyde is dripped in the step (4) in order to reduce silver ions into metallic silver, a uniform metallic silver shell layer is formed on the surface of the explosive powder, the metallic silver reduced and deposited on the surface is ensured not to fall off, and the dripping amount of the formaldehyde and the reaction temperature need to be controlled well.
The invention adopts the principle of silver mirror reaction to reduce silver ions into metallic silver. According to the invention, the dopamine layer is coated on the surface of the explosive powder in advance, so that the silver is promoted to be uniformly deposited on the dopamine surface, and the silver particles are ensured to be completely deposited on the explosive surface through the control of preparation conditions, are not independently aggregated and do not fall off after coating, so that a compact core-shell type nano metal silver and explosive compound is formed.
Drawings
FIG. 1 is a scanning electron micrograph (100 μm scale) of a core-shell type nano-metallic silver and explosive composite obtained in example 1;
FIG. 2 is a scanning electron micrograph (200nm scale) of the core-shell type nano-metallic silver and explosive composite obtained in example 1;
FIG. 3 is an SEM photograph of a core-shell type nano-metallic silver and explosive composite obtained in example 6;
FIG. 4 is an SEM photograph of the composite obtained in example 7.
Detailed Description
The invention is further described with reference to the following figures and specific embodiments.
Example 1
A preparation method of a core-shell type nano metallic silver and explosive compound comprises the following steps:
(1) adding 10g of HMX explosive powder with the average particle size of 100 mu m into 500mL of dopamine-Tris aqueous solution (2g/L and the pH value of about 8.5), stirring at 500rpm for 0.5 hour, performing suction filtration, washing for 5 times by using deionized water, and performing vacuum drying for 8 hours at the temperature of 60 ℃;
(2) preparing 20mL of silver nitrate solution (the concentration is 0.1mol/L), adding ammonia water for regulation to prepare silver ammonia solution, and adding 0.02g of polyvinylpyrrolidone (PVP) into the silver ammonia solution;
(3) dispersing the HMX explosive powder obtained in the step (1) in 20mL of water by 25KHz ultrasonic for 1min, and then adding the dispersed powder into the mixed suspension obtained in the step (2);
(4) adding 2g of 20% formaldehyde solution into the solution obtained in the step (3) while shaking uniformly, putting the mixed suspension into a water bath at 70 ℃, standing for 10min, shaking the mixture, performing suction filtration, and performing vacuum drying at 50 ℃ for 8 hours to obtain the core-shell type nano metal silver and explosive compound. The mass fraction of silver in the composite is 2%. Fig. 1 and 2 are scanning electron micrographs of the obtained core-shell type nano-metallic silver and explosive composite. It can be seen that the silver particles are uniformly distributed on the surface of the explosive particles, and the particle size of the silver particles is about 30 nm.
Example 2
A preparation method of a core-shell type nano metallic silver and explosive compound comprises the following steps:
(1) adding 10g of HMX explosive powder with the average particle size of 50 mu m into 500mL of dopamine-Tris aqueous solution (5g/L and the pH value of about 8.5), stirring at the speed of 400rpm for 0.5 hour, performing suction filtration, washing for 5 times by using deionized water, and performing vacuum drying for 8 hours at the temperature of 60 ℃;
(2) preparing 20mL of silver nitrate solution (the concentration is 0.25mol/L), adding ammonia water for regulation to prepare silver ammonia solution, and adding 0.03g of polyoxyethylene sorbitan monolaurate (Tween-20) into the silver ammonia solution;
(3) dispersing the HMX explosive powder obtained in the step (1) in 10mL of water by 25KHz ultrasonic for 2min, and then adding the dispersed powder into the mixed suspension obtained in the step (2);
(4) adding 4g of 20% formaldehyde solution into the solution obtained in the step (3) while shaking uniformly, putting the mixed suspension into a water bath at 72 ℃, standing for 8min, shaking the mixture, performing suction filtration, and performing vacuum drying at 50 ℃ for 8 hours to obtain the core-shell type nano metal silver and explosive compound. The mass fraction of silver in the composite was 4%.
Example 3
A preparation method of a core-shell type nano metallic silver and explosive compound comprises the following steps:
(1) adding 10g of CL-20 explosive powder with the average particle size of 70 mu m into 500mL of dopamine-Tris aqueous solution (2g/L, the pH value is about 8.5), stirring at the speed of 400rpm for 1 hour, performing suction filtration, washing for 5 times by using deionized water, and performing vacuum drying at the temperature of 60 ℃ for 8 hours;
(2) preparing 20mL of silver nitrate solution (the concentration is 0.5mol/L), adding ammonia water for regulation to prepare silver ammonia solution, and adding 0.02g of alkylphenol polyoxyethylene ether (OP-10) into the silver ammonia solution;
(3) dispersing CL-20 explosive powder obtained in the step (1) in 20mL of water by 25KHz ultrasonic for 0.5min, and then adding the dispersed powder into the mixed suspension obtained in the step (2);
(4) adding 12g of 20% formaldehyde solution into the solution obtained in the step (3) while shaking uniformly, putting the mixed suspension into a water bath at 75 ℃, standing for 2min, shaking the mixture, performing suction filtration, and performing vacuum drying at 40 ℃ for 8 hours to obtain the core-shell type nano metal silver and explosive compound. The mass fraction of silver in the composite is 5%.
Example 4
A preparation method of a core-shell type nano metallic silver and explosive compound comprises the following steps:
(1) adding 10g of LLM-105 explosive powder with the average particle size of 60 mu m into 500mL of dopamine-Tris aqueous solution (2g/L and the pH value of about 8.5), stirring at 500rpm for 1 hour, performing suction filtration, washing for 5 times by using deionized water, and performing vacuum drying for 8 hours at the temperature of 60 ℃;
(2) preparing 30mL of silver nitrate solution (the concentration is 0.1mol/L), adding ammonia water for regulation to prepare silver ammonia solution, and adding 0.02g of polyvinylpyrrolidone (PVP) into the silver ammonia solution;
(3) dispersing the LLM-105 explosive powder obtained in the step (1) in 20mL of water by 40KHz ultrasonic for 0.5min, and then adding the dispersed powder into the mixed suspension obtained in the step (2);
(4) and (3) adding 3g of 20% formaldehyde solution into the solution obtained in the step (3) while shaking uniformly, putting the mixed suspension into a water bath at 70 ℃, standing for 5min, shaking the mixture, performing suction filtration, and performing vacuum drying at 40 ℃ for 8 hours to obtain the core-shell type nano metal silver and explosive compound. The mass fraction of silver in the composite was 3%.
Example 5
A preparation method of a core-shell type nano metallic silver and explosive compound comprises the following steps:
(1) adding 10g of FOX-7 explosive powder with the average particle size of 30 mu m into 500mL of dopamine-Tris aqueous solution (4g/L and the pH value of about 8.5), stirring at the speed of 400rpm for 1 hour, performing suction filtration, washing for 5 times by using deionized water, and performing vacuum drying at the temperature of 60 ℃ for 8 hours;
(2) preparing 20mL of silver nitrate solution (the concentration is 0.2mol/L), adding ammonia water for regulation to prepare silver ammonia solution, and adding 0.04g of polyvinylpyrrolidone (PVP) into the silver ammonia solution;
(3) dispersing the FOX-7 explosive powder obtained in the step (1) in 20mL of water by 40KHz ultrasonic for 2min, and then adding the dispersed powder into the mixed suspension obtained in the step (2);
(4) adding 2g of 20% formaldehyde solution into the solution obtained in the step (3) while shaking uniformly, putting the mixed suspension into a water bath at 70 ℃, standing for 3min, shaking the mixture, performing suction filtration, and performing vacuum drying at 40 ℃ for 8 hours to obtain the core-shell type nano metal silver and explosive compound. The mass fraction of silver in the composite was 4%.
Example 6
A preparation method of a core-shell type nano metallic silver and explosive compound comprises the following steps:
(1) adding 10g of TATB explosive powder with the average particle size of 5 mu m into 500mL of dopamine-Tris aqueous solution (4g/L and the pH value of about 8.5), stirring at the speed of 400rpm for 1 hour, performing suction filtration, washing for 5 times by using deionized water, and performing vacuum drying at the temperature of 60 ℃ for 8 hours;
(2) preparing 20mL of silver nitrate solution (the concentration is 0.5mol/L), adding ammonia water for regulation to prepare silver ammonia solution, and adding 0.05g of polyvinylpyrrolidone (PVP) into the silver ammonia solution;
(3) ultrasonically dispersing TATB explosive powder obtained in the step (1) in 20mL of water at 40KHz for 2min, and then adding the TATB explosive powder into the mixed suspension obtained in the step (2);
(4) and (3) adding 10g of 20% formaldehyde solution into the solution in the step (3) while shaking uniformly, putting the mixed suspension into a water bath at 75 ℃, standing for 5min, shaking the mixture, performing suction filtration, and performing vacuum drying at 50 ℃ for 8 hours to obtain the core-shell type nano metal silver and explosive compound. The mass fraction of silver in the composite is 10%.
Fig. 3 is an SEM photograph of the obtained core-shell type nano-metallic silver and explosive composite.
Example 7
This example is a comparative example to example 6 to illustrate the effect of formaldehyde addition on the formation of a uniform nano-metallic silver shell on the surface of the explosive powder. If the formaldehyde content is not controlled well, the metal silver layer on the surface can fall off. The method comprises the following specific steps:
(1) adding 10g of TATB explosive powder with the average particle size of 5 mu m into 500mL of dopamine-Tris aqueous solution (4g/L and the pH value of about 8.5), stirring at the speed of 400rpm for 1 hour, performing suction filtration, washing for 5 times by using deionized water, and performing vacuum drying at the temperature of 60 ℃ for 8 hours;
(2) preparing 20mL of silver nitrate solution (the concentration is 0.5mol/L), adding ammonia water for regulation to prepare silver ammonia solution, and adding 0.05g of polyvinylpyrrolidone (PVP) into the silver ammonia solution;
(3) ultrasonically dispersing TATB explosive powder obtained in the step (1) in 20mL of water at 40KHz for 2min, and then adding the TATB explosive powder into the mixed suspension obtained in the step (2);
(4) adding 20g of 20% formaldehyde solution into the solution in the step (3) while shaking uniformly, putting the mixed suspension into a water bath at 75 ℃, standing for 5min, shaking the mixture, performing suction filtration, and performing vacuum drying at 50 ℃ for 8 hours to obtain the compound.
FIG. 4 is an SEM photograph of the resulting composite. The exposed explosive crystal and the empty metal silver shell layer can be seen from the figure, which shows that the metal silver shell layer falls off from the surface of the explosive crystal under the action of a large amount of formaldehyde, and is not beneficial to forming a core-shell type nano metal silver and explosive compound.
Although the present invention has been described herein with reference to the illustrated embodiments thereof, which are intended to be preferred embodiments of the present invention, it is to be understood that the invention is not limited thereto, and that numerous other modifications and embodiments can be devised by those skilled in the art that will fall within the spirit and scope of the principles of this disclosure.
Claims (5)
1. A preparation method of a core-shell type nano metal silver and explosive compound is characterized by comprising the following steps:
(1) adding explosive powder into a dopamine-Tris aqueous solution with the pH value of 8.5, stirring at the speed of 300-500 rpm for a period of time, carrying out suction filtration, washing for 5 times by using deionized water, and carrying out vacuum drying for 8-12 hours at the temperature of 60 ℃; the raw material of dopamine is dopamine hydrochloride, the concentration of dopamine-Tris aqueous solution is 2 g/L-5 g/L, the mass ratio of explosive powder to dopamine is 4-10, the stirring speed is 300 rpm-500 rpm, and the stirring time is 0.5 h-1 h;
(2) preparing a silver nitrate solution with a certain concentration, adding ammonia water for regulation to prepare a silver ammonia solution, and adding a surfactant into the silver ammonia solution;
(3) ultrasonically dispersing the explosive powder obtained in the step (1) in water for 0.5-2.0 min, and then adding the explosive powder into the mixed suspension obtained in the step (2);
(4) adding a formaldehyde solution into the solution obtained in the step (3) while shaking uniformly, putting the mixed suspension into a water bath at a certain temperature, standing for 2-10 min, shaking the mixture, performing suction filtration, and performing vacuum drying at 40-50 ℃ for 8-12 hours to obtain the core-shell type nano metallic silver and explosive compound.
2. The method for preparing the core-shell type nano-metallic silver and explosive composite according to claim 1, wherein the method comprises the following steps:
the explosive powder is a non-water-soluble explosive and comprises octogen, 1-oxygen-diamino-3, 5-dinitropyrazine, 1-diamino-2, 2-dinitroethylene explosive, hexanitrohexaazaisowurtzitane and 1,3, 5-triamino-1, 3, 5-trinitrobenzene, and the particle size of the explosive powder is 5-100 mu m.
3. The method for preparing the core-shell type nano-metallic silver and explosive composite according to claim 1 or 2, wherein the method comprises the following steps:
in the step (2), the silver-ammonia solution is a mixed solution of silver nitrate and ammonia water, the concentration of the silver nitrate is 0.1-0.5 mol/L, the surfactant is one of polyvinylpyrrolidone, alkylphenol polyoxyethylene and polyoxyethylene sorbitan monolaurate, and the mass ratio of the surfactant to the explosive added into the silver-ammonia solution is 1: (200-500).
4. The method for preparing the core-shell type nano-metallic silver and explosive composite according to claim 1 or 2, wherein the method comprises the following steps:
the frequency of ultrasonic dispersion in the step (3) is 25 KHz-40 KHz.
5. The method for preparing the core-shell type nano-metallic silver and explosive composite according to claim 1 or 2, wherein the method comprises the following steps:
in the step (4), the molar number of the formaldehyde is 3-8 of the molar number of the silver ions, the concentration of the formaldehyde solution is 20wt%, the water bath temperature is 70-75 ℃, and the mass fraction of the silver in the core-shell type nano metal silver and explosive compound is 2-10%.
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| CN110981670B (en) * | 2019-11-15 | 2021-12-07 | 上海航天化工应用研究所 | Solid propellant containing core-shell modified oxidant and preparation method thereof |
| CN112299936B (en) * | 2020-11-06 | 2021-09-17 | 西南科技大学 | Preparation method and application of photo-thermal material for explosive laser detonation |
| CN113620759B (en) * | 2021-07-16 | 2022-06-07 | 西北工业大学 | Composite solid propellant based on multi-scale modified nitramine oxidant and preparation method thereof |
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