CN114149295B - Coated molecular perovskite energetic material and preparation method thereof - Google Patents

Coated molecular perovskite energetic material and preparation method thereof Download PDF

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CN114149295B
CN114149295B CN202111472837.2A CN202111472837A CN114149295B CN 114149295 B CN114149295 B CN 114149295B CN 202111472837 A CN202111472837 A CN 202111472837A CN 114149295 B CN114149295 B CN 114149295B
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perovskite
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energetic material
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binder
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CN114149295A (en
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曹雄
邓鹏�
安二海
胡双启
谭迎新
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North University of China
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    • C—CHEMISTRY; METALLURGY
    • C06—EXPLOSIVES; MATCHES
    • C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
    • C06B45/00—Compositions or products which are defined by structure or arrangement of component of product
    • C06B45/18—Compositions or products which are defined by structure or arrangement of component of product comprising a coated component
    • C06B45/30—Compositions or products which are defined by structure or arrangement of component of product comprising a coated component the component base containing an inorganic explosive or an inorganic thermic component
    • C06B45/32—Compositions or products which are defined by structure or arrangement of component of product comprising a coated component the component base containing an inorganic explosive or an inorganic thermic component the coating containing an organic compound
    • 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
    • C06B23/001—Fillers, gelling and thickening agents (e.g. fibres), absorbents for nitroglycerine
    • C—CHEMISTRY; METALLURGY
    • C06—EXPLOSIVES; MATCHES
    • C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
    • C06B29/00—Compositions containing an inorganic oxygen-halogen salt, e.g. chlorate, perchlorate
    • C06B29/02—Compositions containing an inorganic oxygen-halogen salt, e.g. chlorate, perchlorate of an alkali metal
    • C06B29/08—Compositions containing an inorganic oxygen-halogen salt, e.g. chlorate, perchlorate of an alkali metal with an organic non-explosive or an organic non-thermic component
    • C—CHEMISTRY; METALLURGY
    • C06—EXPLOSIVES; MATCHES
    • C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
    • C06B29/00—Compositions containing an inorganic oxygen-halogen salt, e.g. chlorate, perchlorate
    • C06B29/22—Compositions containing an inorganic oxygen-halogen salt, e.g. chlorate, perchlorate the salt being ammonium perchlorate
    • C—CHEMISTRY; METALLURGY
    • C06—EXPLOSIVES; MATCHES
    • C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
    • C06B45/00—Compositions or products which are defined by structure or arrangement of component of product
    • C06B45/18—Compositions or products which are defined by structure or arrangement of component of product comprising a coated component
    • C06B45/20—Compositions or products which are defined by structure or arrangement of component of product comprising a coated component the component base containing an organic explosive or an organic thermic component
    • C06B45/22—Compositions or products which are defined by structure or arrangement of component of product comprising a coated component the component base containing an organic explosive or an organic thermic component the coating containing an organic compound

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  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Compositions Of Oxide Ceramics (AREA)

Abstract

The invention provides a coated molecular perovskite energetic material and a preparation method thereof, belonging to the technical field of energetic material preparation, wherein the coated molecular perovskite energetic material is a microcosmic coating structure with a binder coated molecular perovskite energetic material; the coating material comprises 0.5-15% of binder and 85-99.5% of molecular perovskite energetic material by taking the total mass of the coating molecular perovskite energetic material as 100%. The coated molecular perovskite energetic material has a low high-molecular binder coating amount, the safety performance of the coated molecular perovskite energetic material is greatly improved while the mass ratio of the molecular perovskite energetic material is not remarkably reduced, and the mechanical sensitivity evaluation result shows that the mechanical sensitivity of the coated molecular perovskite energetic material can be improved by 30-300% relative to the raw material particles of the molecular perovskite energetic material; compared with the friction sensitivity explosion probability of the molecular perovskite energetic material raw material particles, the friction sensitivity explosion probability is reduced to 30% -90%, and the method has the advantage of good sense reduction and can promote the sense reduction and application of the molecular perovskite energetic material.

Description

Coated molecular perovskite energetic material and preparation method thereof
Technical Field
The invention belongs to the technical field of energetic material preparation, and particularly relates to a coated molecular perovskite energetic material and a preparation method thereof.
Background
The molecular perovskite energetic material is a novel energetic material which is firstly reported and synthesized in Chen Xiaoming in 2018, and is widely concerned in the field of explosives and powders due to the advantages of high detonation performance, cost economy and the like. Represented typically in molecular perovskite energetic materials (H) 2 dabco)[NH 4 (ClO 4 ) 3 ](DAP-4) is taken as an example, the initial exploration of performance evaluation and optimization and application research of the molecular perovskite energetic material is carried out by a few related units in the domestic explosive and powder industry, and the research shows that the actual measured detonation heat value of DAP-4 is 5.691 kJ/g, the actual measured detonation velocity can reach 8.5 km/s, and the better application potential is shown. But the DAP-4 has poor mechanical sensitivity and safetySeverely restricting the application of the medicine.
Disclosure of Invention
The invention provides a coated molecular perovskite energetic material and a preparation method thereof, which realize surface coating of the molecular perovskite energetic material and effectively solve the problem of high sensitivity of the molecular perovskite energetic material.
In order to achieve the purpose, the invention provides a coated molecular perovskite energetic material which has a microscopic coating structure that a binder coats the molecular perovskite energetic material;
the total mass of the coated molecular perovskite energetic material is 100%, wherein the raw material components and the mass fractions thereof are as follows:
adhesive: 0.5 to 15 percent;
molecular perovskite energetic material: 85 to 99.5 percent.
Specifically, the molecular perovskite energetic material is a perchlorate-based molecular perovskite energetic material.
Specifically, the molecular perovskite energetic material is (H) 2 dabco)[NH 4 (ClO 4 ) 3 ]（DAP-4）、(H 2 dabco)[Na(ClO 4 ) 3 ]（DAP-1）、(H 2 dabco)[K(ClO 4 ) 3 ]（DAP-2）、(H 2 mpz)[NH 4 (ClO 4 ) 3 ]（PAP-M4）、(H 2 pz)[NH 4 (ClO 4 ) 3 ]（PAP-4）、(H 2 hpz)[NH 4 (ClO 4 ) 3 ]（PAP-H4）、(H 2 dabco-O)[NH 4 (ClO 4 ) 3 ]（DAP-O4）、(H 2 mdabco)[NH 4 (ClO 4 ) 3 ]（DAP-M4）、(H 2 dabco)[ NH 3 OH(ClO 4 ) 3 ](DAP-6) and (H) 2 dabco)[ NH 2 NH 3 (ClO 4 ) 3 ](DAP-7).
Specifically, the binder is Estane-5703 and F 2602 、F 2604 、F 2311 One of stearic acid and tri-ethyl propyl rubber.
The invention also provides a preparation method of the coated molecular perovskite energetic material, which comprises the following steps:
step A, dissolving a binder in a solvent, and completely dissolving to obtain a binder-containing solution;
step B, after the molecular perovskite energetic material is crushed and hard agglomerated, adding the molecular perovskite energetic material crystal particles into a binder solution to uniformly disperse the molecular perovskite energetic material in the solution to form a suspension;
step C, heating the suspension of the molecular perovskite energetic material to 50-60 ℃, stirring and volatilizing the solvent, putting the suspension into a vacuum oven to expel residual solvent after the solvent is volatilized, and obtaining a dried sample;
and D, washing, filtering and drying the dried sample to obtain the composite energetic material with the binder coated molecular perovskite energetic material.
In the step A, the solvent is a good solvent for dissolving the adhesive, and the dissolving time is 12-24 h.
And B, grinding the molecular perovskite energetic material by using an agate mortar, crushing the hard agglomeration of the molecular perovskite energetic material, adding the molecular perovskite energetic material crystal particles into a binder solution, and ultrasonically stirring for 10-20min.
And C, heating in a water bath.
In the step D, the washing solvent is insoluble high molecular binder and is liquid of insoluble molecular perovskite energetic material crystals.
Preferably, the solvent is one of 1,2-dichloroethane, ethyl acetate, ethanol and cyclohexane, and the washing solvent is ice water or ethanol.
The present invention has the following advantageous effects.
1. The invention provides a coated molecular perovskite energetic material and a preparation method thereof, wherein the coated molecular perovskite energetic material has a low high-molecular binder coating amount, the safety performance of the coated molecular perovskite energetic material is greatly improved while the mass ratio of the molecular perovskite energetic material is not remarkably reduced, and the mechanical sensitivity of the coated molecular perovskite energetic material can be improved by 30-300% compared with that of raw material particles of the molecular perovskite energetic material as shown by a mechanical sensitivity evaluation result; compared with the friction sensitivity explosion probability of the molecular perovskite energetic material raw material particles, the friction sensitivity explosion probability is reduced to 30% -90%, and the method has the advantage of good sense reduction and can promote the sense reduction and application of the molecular perovskite energetic material.
2. The preparation method of the coated molecular perovskite energetic material can regulate and control the content of the binder according to the requirement of safety performance, thereby realizing the regulation and control of the safety performance.
3. The preparation method of the energy-containing material coated with the molecular perovskite has a simple preparation process and is beneficial to large-scale production.
Drawings
FIG. 1 is an SEM photograph of DAP-4 as a raw material in example 1;
FIG. 2 is an SEM image of an Estane-5703 coated molecular perovskite energetic material DAP-4 in example 1.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the accompanying drawings, and it should be understood that the described embodiments are some, but not all embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The energy-containing material of the coated molecular perovskite is calculated by taking the total mass of the energy-containing material of the coated molecular perovskite as 100 percent, wherein the energy-containing material comprises the following raw material components in percentage by mass:
adhesive Estane-5703: 0.5 percent;
molecular perovskite energetic material DAP-4: 99.5 percent.
The preparation method of the coated molecular perovskite energetic material comprises the following specific steps:
step A, dissolving 0.025g of Estane-5703 in 15ml of 1, 2-dichloroethane, and carrying out ultrasonic treatment until the Estane-5703 is completely dissolved to obtain an Estane-5703 solution;
b, lightly grinding the energetic material DAP-4 of the molecular perovskite by using an agate mortar, crushing the hard agglomeration of the energetic material DAP-4, adding 4.975g of DAP-4 particles into Estane-5703 solution, and dispersing the DAP-4 in the solution uniformly by ultrasonic dispersion;
step C, placing the suspension of the DAP-4 into a water bath kettle at 50-60 ℃ for stirring and volatilizing the solvent, and after the solvent is volatilized, placing the suspension into a vacuum oven to expel residual solvent to obtain a dried sample;
and D, washing the dried sample with ethanol, filtering and drying to obtain the composite energetic material with the Estane-5703 coated molecular perovskite energetic material DAP-4.
Example 2
The energetic material of the coated molecular perovskite is calculated by taking the total mass of the coated molecular perovskite as 100 percent, wherein the raw material components and the mass fractions thereof are as follows:
adhesive Estane-5703: 5 percent;
molecular perovskite energetic material DAP-4: 95 percent.
The preparation method of the coated molecular perovskite energetic material comprises the following specific steps:
step A, dissolving 0.25g of Estane-5703 in 15ml of 1, 2-dichloroethane, and carrying out ultrasonic treatment until the Estane-5703 is completely dissolved to obtain an Estane-5703 solution;
b, lightly grinding the energetic material DAP-4 of the molecular perovskite by using an agate mortar, crushing the hard agglomeration of the energetic material DAP-4, adding 4.75g of DAP-4 particles into Estane-5703 solution, and dispersing the DAP-4 in the solution uniformly by ultrasonic dispersion;
step C, placing the suspension of the DAP-4 into a water bath kettle at 50-60 ℃ for stirring and volatilizing the solvent, and after the solvent is volatilized, placing the suspension into a vacuum oven to expel residual solvent to obtain a dried sample;
and D, washing the dried sample with ethanol, filtering and drying to obtain the composite energetic material with the Estane-5703 coated molecular perovskite energetic material DAP-4.
Example 3
The energy-containing material of the coated molecular perovskite is calculated by taking the total mass of the energy-containing material of the coated molecular perovskite as 100 percent, wherein the energy-containing material comprises the following raw material components in percentage by mass:
adhesive Estane-5703: 15 percent;
molecular perovskite energetic material DAP-4: 85 percent.
The preparation method of the coated molecular perovskite energetic material comprises the following specific steps:
step A, dissolving 0.75g of Estane-5703 in 15ml of 1, 2-dichloroethane, and performing ultrasonic treatment until the Estane-5703 is completely dissolved to obtain an Estane-5703 solution;
b, lightly grinding the energetic material DAP-4 of the molecular perovskite by using an agate mortar, crushing the hard agglomeration of the energetic material DAP-4, adding 4.25g of DAP-4 particles into Estane-5703 solution, and dispersing the DAP-4 in the solution uniformly by ultrasonic dispersion;
step C, placing the suspension of the DAP-4 into a water bath kettle at 50-60 ℃ for stirring and volatilizing the solvent, and after the solvent is volatilized, placing the suspension into a vacuum oven to expel residual solvent to obtain a dried sample;
and D, washing the dried sample with ethanol, filtering and drying to obtain the composite energetic material with the Estane-5703 coated molecular perovskite energetic material DAP-4.
Example 4
The energy-containing material of the coated molecular perovskite is calculated by taking the total mass of the energy-containing material of the coated molecular perovskite as 100 percent, wherein the energy-containing material comprises the following raw material components in percentage by mass:
binder F 2602 ： 15%；
Molecular perovskite energetic material DAP-4: 85 percent.
The preparation method of the coated molecular perovskite energetic material comprises the following specific steps:
step A, 0.75g of F 2602 Dissolving in 15ml ethyl acetate, and performing ultrasonic treatment until complete dissolution to obtain F 2602 A solution;
step B, lightly grinding the molecular perovskite energetic material DAP-4 by using an agate mortar, crushing the hard agglomeration of the molecular perovskite energetic material DAP-4, and then adding 4.25g of DAP-4 particles into F 2602 In solution, by ultrafiltrationAfter sound dispersion, the DAP-4 is uniformly dispersed in the solution;
step C, placing the suspension of the DAP-4 into a water bath kettle at 50-60 ℃ for stirring and volatilizing the solvent, and after the solvent is volatilized, placing the suspension into a vacuum oven to expel residual solvent to obtain a dried sample;
step D, washing the dried sample with ethanol, filtering and drying to obtain the compound F 2602 The composite energetic material is coated with the molecular perovskite energetic material DAP-4.
Example 5
The energy-containing material of the coated molecular perovskite is calculated by taking the total mass of the energy-containing material of the coated molecular perovskite as 100 percent, wherein the energy-containing material comprises the following raw material components in percentage by mass:
binder F 2604 ： 15%；
Molecular perovskite energetic material DAP-4: 85 percent.
The preparation method of the coated molecular perovskite energetic material comprises the following specific steps:
step A, 0.75g of F 2604 Dissolving in 15ml ethyl acetate, and performing ultrasonic treatment until complete dissolution to obtain F 2604 A solution;
step B, lightly grinding the molecular perovskite energetic material DAP-4 by using an agate mortar, crushing the hard agglomeration of the molecular perovskite energetic material DAP-4, and then adding 4.25g of DAP-4 particles into F 2604 In the solution, after ultrasonic dispersion, the DAP-4 is uniformly dispersed in the solution;
step C, placing the DAP-4 suspension into a water bath kettle at 50-60 ℃ for stirring and volatilizing the solvent, and placing the DAP-4 suspension into a vacuum oven to remove residual solvent after the solvent is volatilized, so as to obtain a dry sample;
step D, washing the dried sample with ethanol, filtering and drying to obtain the compound F 2604 The composite energetic material is coated with the molecular perovskite energetic material DAP-4.
Example 6
The energy-containing material of the coated molecular perovskite is calculated by taking the total mass of the energy-containing material of the coated molecular perovskite as 100 percent, wherein the energy-containing material comprises the following raw material components in percentage by mass:
binder F 2311 ： 15%；
Molecular perovskite energetic material DAP-4: 85 percent.
The preparation method of the coated molecular perovskite energetic material comprises the following specific steps:
step A, 0.75g of F 2311 Dissolving in 15ml ethyl acetate, and performing ultrasonic treatment until complete dissolution to obtain F 2311 A solution;
step B, lightly grinding the molecular perovskite energetic material DAP-4 by using an agate mortar, crushing the hard agglomeration of the molecular perovskite energetic material DAP-4, and then adding 4.25g of DAP-4 particles into F 2311 In the solution, after ultrasonic dispersion, the DAP-4 is uniformly dispersed in the solution;
step C, placing the suspension of the DAP-4 into a water bath kettle at 50-60 ℃ for stirring and volatilizing the solvent, and after the solvent is volatilized, placing the suspension into a vacuum oven to expel residual solvent to obtain a dried sample;
step D, washing the dried sample with ethanol, filtering and drying to obtain the compound F of the embodiment 2311 The composite energetic material is coated with the molecular perovskite energetic material DAP-4.
Example 7
The energy-containing material of the coated molecular perovskite is calculated by taking the total mass of the energy-containing material of the coated molecular perovskite as 100 percent, wherein the energy-containing material comprises the following raw material components in percentage by mass:
binder stearic acid: 15 percent;
molecular perovskite energetic material DAP-4: 85 percent.
The preparation method of the coated molecular perovskite energetic material comprises the following specific steps:
step A, dissolving 0.75g of stearic acid in 15ml of ethanol, and performing ultrasonic treatment until the stearic acid is completely dissolved to obtain a stearic acid solution;
b, lightly grinding the molecular perovskite energetic material DAP-4 by using an agate mortar, crushing the hard agglomeration of the molecular perovskite energetic material DAP-4, adding 4.25g of DAP-4 particles into a stearic acid solution, and dispersing the DAP-4 in the solution uniformly by ultrasonic dispersion;
step C, placing the suspension of the DAP-4 into a water bath kettle at 50-60 ℃ for stirring and volatilizing the solvent, and after the solvent is volatilized, placing the suspension into a vacuum oven to expel residual solvent to obtain a dried sample;
and D, washing the dried sample with ice water, filtering and drying to obtain the composite energetic material with the stearic acid coated molecular perovskite energetic material DAP-4.
Example 8
The energy-containing material of the coated molecular perovskite is calculated by taking the total mass of the energy-containing material of the coated molecular perovskite as 100 percent, wherein the energy-containing material comprises the following raw material components in percentage by mass:
binder ethylene propylene diene monomer rubber: 15 percent;
molecular perovskite energetic material DAP-4: 85 percent.
The preparation method of the coated molecular perovskite energetic material comprises the following specific steps:
step A, dissolving 0.75g of ethylene propylene diene monomer in 15ml of normal hexane, and performing ultrasonic treatment until the ethylene propylene diene monomer is completely dissolved to obtain an ethylene propylene diene monomer solution;
b, lightly grinding the molecular perovskite energetic material DAP-4 by using an agate mortar, crushing the hard agglomeration of the molecular perovskite energetic material DAP-4, adding 4.25g of DAP-4 particles into an ethylene propylene diene monomer rubber solution, and dispersing the DAP-4 in the solution uniformly by ultrasonic dispersion;
step C, placing the suspension of the DAP-4 into a water bath kettle at 50-60 ℃ for stirring and volatilizing the solvent, and after the solvent is volatilized, placing the suspension into a vacuum oven to expel residual solvent to obtain a dried sample;
and D, washing the dried sample with ethanol, filtering and drying to obtain the composite energetic material with the ethylene propylene diene monomer rubber coated molecular perovskite energetic material DAP-4.
Example 9
The energy-containing material of the coated molecular perovskite is calculated by taking the total mass of the energy-containing material of the coated molecular perovskite as 100 percent, wherein the energy-containing material comprises the following raw material components in percentage by mass:
adhesive Estane-5703: 15 percent;
molecular perovskite energetic material PAP-4: 85 percent.
The preparation method of the coated molecular perovskite energetic material comprises the following specific steps:
step A, dissolving 0.75g of Estane-5703 in 15ml of 1, 2-dichloroethane, and performing ultrasonic treatment until the Estane-5703 is completely dissolved to obtain an Estane-5703 solution;
b, lightly grinding the energetic material PAP-4 of the molecular perovskite by using an agate mortar, crushing the hard agglomeration of the energetic material PAP-4, adding 4.25g of PAP-4 particles into Estane-5703 solution, and dispersing the PAP-4 in the solution uniformly by ultrasonic dispersion;
step C, placing the PAP-4 suspension into a water bath kettle at 50-60 ℃ for stirring and volatilizing the solvent, and placing the suspension into a vacuum oven to remove residual solvent after the solvent is volatilized, so as to obtain a dried sample;
and D, washing the dried sample with ethanol, filtering and drying to obtain the composite energetic material PAP-4 with the Estane-5703 coated molecular perovskite energetic material.
Example 10
The energy-containing material of the coated molecular perovskite is calculated by taking the total mass of the energy-containing material of the coated molecular perovskite as 100 percent, wherein the energy-containing material comprises the following raw material components in percentage by mass:
binder F 2602 ： 15%；
Molecular perovskite energetic material PAP-H4: 85 percent.
The preparation method of the coated molecular perovskite energetic material comprises the following specific steps:
step A, 0.75g of F 2602 Dissolving in 15ml ethyl acetate, and performing ultrasonic treatment until complete dissolution to obtain F 2602 A solution;
step B, lightly grinding the molecular perovskite energetic material PAP-H4 by using an agate mortar, crushing the hard agglomeration of the molecular perovskite energetic material PAP-H4, and adding 4.25g of PAP-H4 particles into F 2602 In the solution, PAP-H4 is uniformly dispersed in the solution after ultrasonic dispersion;
step C, putting the PAP-H4 suspension into a water bath kettle at 50-60 ℃, stirring and volatilizing the solvent, putting the suspension into a vacuum oven after the solvent is volatilized, and removing the residual solvent to obtain a dried sample;
step D, washing the dried sample with ethanol, filtering and drying to obtain the compound F 2602 A composite energetic material of a coated molecular perovskite energetic material PAP-H4.
Example 11
The energy-containing material of the coated molecular perovskite is calculated by taking the total mass of the energy-containing material of the coated molecular perovskite as 100 percent, wherein the energy-containing material comprises the following raw material components in percentage by mass:
binder F 2604 ： 15%；
Molecular perovskite energetic material PAP-4: 85 percent.
The preparation method of the coated molecular perovskite energetic material comprises the following specific steps:
step A, 0.75g of F 2604 Dissolving in 15ml ethyl acetate, and performing ultrasonic treatment until complete dissolution to obtain F 2604 A solution;
step B, lightly grinding the molecular perovskite energetic material PAP-4 by using an agate mortar, crushing the hard agglomeration of the molecular perovskite energetic material PAP-4, and adding 4.25g of PAP-4 particles into F 2604 In the solution, PAP-4 is uniformly dispersed in the solution after ultrasonic dispersion;
step C, placing the PAP-4 suspension into a water bath kettle at 50-60 ℃ for stirring and volatilizing the solvent, and placing the suspension into a vacuum oven to remove residual solvent after the solvent is volatilized, so as to obtain a dried sample;
step D, washing the dried sample with ethanol, filtering and drying to obtain the compound F 2604 A composite energetic material coated with a molecular perovskite energetic material PAP-4.
Example 12
The energy-containing material of the coated molecular perovskite is calculated by taking the total mass of the energy-containing material of the coated molecular perovskite as 100 percent, wherein the energy-containing material comprises the following raw material components in percentage by mass:
binder F 2311 ： 15%；
Molecular perovskite energetic material PAP-H4: 85 percent.
The preparation method of the coated molecular perovskite energetic material comprises the following specific steps:
step A, 0.75g of F 2311 Dissolving in 15ml ethyl acetate, and performing ultrasonic treatment until complete dissolution to obtain F 2311 A solution;
step B, lightly grinding the molecular perovskite energetic material PAP-H4 by using an agate mortar, crushing the hard agglomeration of the molecular perovskite energetic material PAP-H4, and adding 4.25g of PAP-H4 particles into F 2311 In the solution, PAP-H4 is uniformly dispersed in the solution after ultrasonic dispersion;
step C, putting the PAP-H4 suspension into a water bath kettle at 50-60 ℃, stirring and volatilizing the solvent, putting the suspension into a vacuum oven after the solvent is volatilized, and removing the residual solvent to obtain a dried sample;
step D, washing the dried sample with ethanol, filtering and drying to obtain the compound F of the embodiment 2311 A composite energetic material of a coated molecular perovskite energetic material PAP-H4.
Example 13
The energy-containing material of the coated molecular perovskite is calculated by taking the total mass of the energy-containing material of the coated molecular perovskite as 100 percent, wherein the energy-containing material comprises the following raw material components in percentage by mass:
binder stearic acid: 15 percent;
molecular perovskite energetic material PAP-4: 85 percent.
The preparation method of the coated molecular perovskite energetic material comprises the following specific steps:
step A, dissolving 0.75g of stearic acid in 15ml of ethanol, and performing ultrasonic treatment until the stearic acid is completely dissolved to obtain a stearic acid solution;
b, lightly grinding the molecular perovskite energetic material PAP-4 by using an agate mortar, crushing the hard agglomeration of the molecular perovskite energetic material PAP-4, adding 4.25g of PAP-4 particles into a stearic acid solution, and dispersing the PAP-4 in the solution uniformly by ultrasonic dispersion;
step C, placing the suspension of PAP-4 into a water bath kettle at 50-60 ℃ for stirring and volatilizing the solvent, and placing the suspension into a vacuum oven to remove residual solvent after the solvent is volatilized to obtain a dried sample;
and D, washing the dried sample with ice water, filtering and drying to obtain the composite energetic material with the stearic acid coated molecular perovskite energetic material PAP-4.
Example 14
The energy-containing material of the coated molecular perovskite is calculated by taking the total mass of the energy-containing material of the coated molecular perovskite as 100 percent, wherein the energy-containing material comprises the following raw material components in percentage by mass:
binder ethylene propylene diene monomer rubber: 15 percent;
molecular perovskite energetic material PAP-H4: 85 percent.
The preparation method of the coated molecular perovskite energetic material comprises the following specific steps:
step A, dissolving 0.75g of ethylene propylene diene monomer in 15ml of normal hexane, and performing ultrasonic treatment until the ethylene propylene diene monomer is completely dissolved to obtain an ethylene propylene diene monomer solution;
b, lightly grinding the molecular perovskite energetic material PAP-H4 by using an agate mortar, crushing the hard agglomerates, adding 4.25g of PAP-H4 particles into an ethylene propylene diene monomer rubber solution, and dispersing the PAP-H4 in the solution uniformly by ultrasonic dispersion;
step C, putting the PAP-H4 suspension into a water bath kettle at 50-60 ℃, stirring and volatilizing the solvent, putting the suspension into a vacuum oven after the solvent is volatilized, and removing the residual solvent to obtain a dried sample;
and D, washing the dried sample with ethanol, filtering and drying to obtain the composite energetic material with the EPDM-rubber-coated molecular perovskite energetic material PAP-H4.
Example 15
The end products prepared in examples 1 to 14 were tested as follows:
(1) Scanning Electron Microscopy (SEM) characterization: BCPCA, model number: and S4800.
In order to determine the composition of the final product in the examples, the raw material and the final product in example 1 were subjected to Scanning Electron Microscopy (SEM), respectively, and the results are shown in fig. 1. As can be seen from fig. 1, the final product is a composite energetic material with a coating structure, namely the coated molecular perovskite energetic material DAP-4 described in example 1. The SEM test results of the final products of examples 2-14 are similar to the test results of example 1.
(2) And (5) testing mechanical sensitivity. The final products of examples 1 to 14 were tested for their mass heats of combustion according to the 601 impact sensitivity characteristic falling height method and the friction sensitivity explosion probability method in GJB-770B-1997.
The mechanical sensitivity testing method comprises the following steps:
evaluation of impact mechanical sensitivity was carried out by using an impact sensitivity meter model WL-1 according to 601 impact sensitivity characteristic falling height method (2.0 Kg falling weight; sample mass: 30 mg; sample number: 25) in GJB-770B-1997 and friction sensitivity explosion probability method 602 (2.0 Kg pendulum; swing angle: 90 DEG; pressure: 3.92 MPa; sample mass: 30 mg; sample number: 25) in GJB-770B-1997.
The mechanical sensitivity of the final products of examples 1 to 14 was measured, and the results are shown in Table 1:
TABLE 1 mechanical sensitivity of the final products in examples 1 to 14
Figure DEST_PATH_IMAGE001
The test result shows that the composite energetic material prepared by the method for coating the molecular perovskite energetic material has the advantage of better sense reduction.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.

Claims (6)

1. The preparation method of the coated molecular perovskite energetic material is characterized by comprising the following steps of:
step A, taking the total mass of the coated molecular perovskite energetic material as 100%, the mass fraction of the binder is 0.5% -15%, and the binder is Estane-5703 and F 2602 、F 2604 、F 2311 Dissolving a binder in a solvent to obtain a binder-containing solution, wherein the binder is one of stearic acid and ethylene propylene terpolymer;
and step B, taking the total mass of the coated molecular perovskite energetic material as 100%, wherein the mass fraction of the molecular perovskite energetic material is 85% -99.5%, and the molecular perovskite energetic material is (H) 2 dabco)[NH 4 (ClO 4 ) 3 ]、(H 2 dabco)[Na(ClO 4 ) 3 ]、(H 2 dabco)[K(ClO 4 ) 3 ]、(H 2 mpz)[NH 4 (ClO 4 ) 3 ]、(H 2 pz)[NH 4 (ClO 4 ) 3 ]、(H 2 hpz)[NH 4 (ClO 4 ) 3 ]、(H 2 dabco-O)[NH 4 (ClO 4 ) 3 ]、(H 2 mdabco)[NH 4 (ClO 4 ) 3 ]、(H 2 dabco)[NH 3 OH(ClO 4 ) 3 ]And (H) 2 dabco)[ NH 2 NH 3 (ClO 4 ) 3 ]After the molecular perovskite energetic material is crushed and hard agglomerated, adding the crystal particles of the molecular perovskite energetic material into a binder solution to uniformly disperse the molecular perovskite energetic material in the solution to form a suspension;
step C, heating the suspension of the molecular perovskite energetic material to 50-60 ℃, stirring and volatilizing the solvent, putting the suspension into a vacuum oven to expel residual solvent after the solvent is volatilized, and obtaining a dried sample;
and D, washing, filtering and drying the dried sample to obtain the composite energetic material with the binder coated molecular perovskite energetic material.
2. The method for preparing the coated molecular perovskite energetic material according to claim 1, wherein in the step A, the solvent is a good solvent for dissolving the binder, and the dissolving time is 12-24 h.
3. The preparation method of the coated molecular perovskite energetic material according to claim 2, wherein in the step B, the molecular perovskite energetic material is ground by an agate mortar, the hard agglomeration of the molecular perovskite energetic material is crushed, the crystal particles of the molecular perovskite energetic material are added into a binder solution, and the ultrasonic stirring is carried out for 10-20 min.
4. The method for preparing the coated molecular perovskite energetic material according to claim 3, wherein in step C, water bath heating is adopted.
5. The method for preparing the coated molecular perovskite energetic material according to claim 4, wherein in the step D, the washing solvent is an insoluble polymer binder and is a liquid of insoluble molecular perovskite energetic material crystals.
6. The method for preparing the coated molecular perovskite energetic material as claimed in claim 5, wherein the solvent is one of 1,2-dichloroethane, ethyl acetate, ethanol and cyclohexane, and the washing solvent is ice water or ethanol.
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