CN111908990B - Energetic material filled layered framework composite structure and preparation method thereof - Google Patents
Energetic material filled layered framework composite structure and preparation method thereof Download PDFInfo
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- CN111908990B CN111908990B CN202010694565.XA CN202010694565A CN111908990B CN 111908990 B CN111908990 B CN 111908990B CN 202010694565 A CN202010694565 A CN 202010694565A CN 111908990 B CN111908990 B CN 111908990B
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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
- C06B45/04—Compositions or products which are defined by structure or arrangement of component of product comprising solid particles dispersed in solid solution or matrix not used for explosives where the matrix consists essentially of nitrated carbohydrates or a low molecular organic explosive
- C06B45/06—Compositions or products which are defined by structure or arrangement of component of product comprising solid particles dispersed in solid solution or matrix not used for explosives where the matrix consists essentially of nitrated carbohydrates or a low molecular organic explosive the solid solution or matrix containing an organic component
- C06B45/10—Compositions or products which are defined by structure or arrangement of component of product comprising solid particles dispersed in solid solution or matrix not used for explosives where the matrix consists essentially of nitrated carbohydrates or a low molecular organic explosive the solid solution or matrix containing an organic component the organic component containing a resin
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- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B21/00—Apparatus or methods for working-up explosives, e.g. forming, cutting, drying
- C06B21/0033—Shaping the mixture
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- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B45/00—Compositions or products which are defined by structure or arrangement of component of product
- C06B45/04—Compositions or products which are defined by structure or arrangement of component of product comprising solid particles dispersed in solid solution or matrix not used for explosives where the matrix consists essentially of nitrated carbohydrates or a low molecular organic explosive
- C06B45/06—Compositions or products which are defined by structure or arrangement of component of product comprising solid particles dispersed in solid solution or matrix not used for explosives where the matrix consists essentially of nitrated carbohydrates or a low molecular organic explosive the solid solution or matrix containing an organic component
Abstract
The invention discloses an energetic material filled laminated frame composite structure and a preparation method thereof, which comprises the steps of preparing sol by polysaccharide or lignin natural polymer materials, adopting an ice template method to induce solvent in the sol to directionally crystallize to form a laminated structure, removing the solvent by freeze drying to form a laminated frame structure with parallel laminated confinement spaces in the frame, introducing energetic material solution into the confinement spaces of the laminated frame structure, crystallizing to form energetic material crystals, and constructing to obtain the energetic material filled laminated frame composite structure. The invention can obtain the composite energetic material with a sandwich type stacked laminated structure, so that the safety performance of the composite energetic material is obviously improved, and the comprehensive performance of the composite energetic material is effectively improved.
Description
Technical Field
The invention belongs to a design and regulation method of an energetic material composite structure, and particularly relates to an energetic material filled layered framework composite structure and a preparation method thereof.
Background
The microstructure of the energetic material has a significant impact on its macroscopic properties.
On the molecular level, the sensitivity of most energetic material molecules with two-dimensional planar configuration, such as triaminotrinitrobenzene (TATB), 2, 6-diamino-3, 5-dinitropyrazine-1-oxide (LLM-105), Hexanitrostilbene (HNS) and the like, is generally superior to that of energetic materials with other configurations, such as cycloidal or cage explosives such as octogen (HMX), hexogen (RDX), hexanitrohexaazaisowurtzitane (CL-20) and the like.
On a microscopic level, energetic material crystals show great difference in safety performance according to the difference of the morphology and the particle size. For example, irregular twin explosive particles are easy to form hot spots under the action of external force, so that the irregular twin explosive particles are easy to detonate, and the safety is reduced; the safety performance of the micro-nano explosive particles is generally better than that of the large-particle explosives.
Therefore, for the development target of 'high energy and insensitive' of new-period energetic materials, the effective regulation and control of the existing high-energy explosive is an effective way for achieving the target.
The key problem at present is that the feasibility thought for improving the safety of the energetic material is relatively lacked by realizing the regularization and the scaling control of the energetic material by a reasonable and effective technical means, and the related regulation theory and technical support are not enough. How to realize the regularization and the accurate scale control of the energetic material in a system is a key technical problem to be solved and is also a common problem faced by the development of the current energetic material.
Disclosure of Invention
The invention aims to provide an energetic material filled layered frame composite structure and a preparation method thereof, and the composite energetic material with a sandwich type stacked layered structure is obtained by adopting a method of preparing a layered frame structure by a combined ice template method and recrystallizing an energetic material solution, so that the safety performance of the composite energetic material is obviously improved, and the comprehensive performance of the composite energetic material is effectively improved.
The composite structure of the energy-containing material filled laminated framework consists of laminated framework structures and energy-containing material crystals filled between the laminated framework structures, and has a regular sandwich-like periodic structure, wherein the laminated framework structures are prepared by preparing sol from polysaccharide or lignin natural polymer materials, adopting an ice template method to induce the solvent in the sol to directionally crystallize to form a laminated structure, freeze-drying to remove the solvent, and forming the laminated framework structure with parallel laminated confinement spaces in the framework, and the energy-containing material crystals are formed by introducing an energy-containing material solution into the confinement spaces of the laminated framework structures and crystallizing.
Furthermore, the layered framework structure is a regular and periodic parallel layered framework, the distance between the layered framework structures is adjustable, the layer thickness of the layered framework is 500 nm-5 μm, and the distance between the layered frameworks, namely the height of the limited space is 10 μm-100 μm.
In the energetic material filled layered frame composite structure, the mass percentage of the energetic material crystals can reach 85-99%.
Specifically, the polysaccharide or lignin natural polymer material of the present invention includes, but is not limited to, chitosan, glucomannan, lignin, and other natural polymer substances that can form a sol.
More specifically, the present invention preferably uses water as a solvent to prepare the polysaccharide or lignin natural polymer material into an aqueous sol.
Furthermore, the energetic material filled layered framework composite structure can be prepared according to the following preparation method.
1) Preparing sol from polysaccharide or lignin natural polymer materials, inducing the solvent in the natural polymer material sol to directionally crystallize by adopting an ice template method to form a regular gradient laminated structure, promoting the solute natural polymer materials to form a micro-nano multilayer frame structure macroscopic body, and removing the solvent between interfaces of the laminated structure by vacuum freeze drying to form a laminated frame structure with parallel laminated confinement spaces in the frame.
2) And taking the layered frame structure as a template, introducing the energetic material solution into the layered frame structure, and recrystallizing the energetic material solution in a limited space of the layered frame structure template by using external acting force to form energetic material crystals and construct an energetic material filled layered frame composite structure.
Furthermore, the invention can repeat the process of introducing the energetic material solution into the layered framework structure for recrystallization for many times until the loading capacity of the energetic material in the layered framework structure meets the requirement.
The invention takes the internally-assigned parallel lamellar limited space of a lamellar framework structure as the filling space of an energetic material crystal, adopts the adding mode of absorbing an energetic material solution by a template, leads the energetic material solution into the limited space of the lamellar framework structure, promotes the crystallization and nucleation of energetic material molecules under the action of crystallization conditions, is limited by the lamellar framework structure limited space, and leads the energetic material molecules to directionally grow and crystallize in the lamellar limited space region through circulating multiple crystallization processes to form a compact energetic material filling lamellar framework composite structure with high filling content.
Furthermore, in the preparation method of the present invention, the energetic material may be any one of simple substance energetic materials such as HMX, CL-20, LLM-105, ADN, DAAF, TKX-50, etc., or a mixed energetic material formed by mixing these simple substance energetic materials.
In the preparation method of the invention, the external force recrystallization mode can be any one of natural volatilization recrystallization, evaporation recrystallization and cooling recrystallization.
By adopting the preparation method, the energetic material with the sandwich-like stacked layered structure can be prepared, the energetic material with the composite structure is filled in the layered frame structure in a regular and scaled manner, the loading capacity of the energetic material is high, the technical problems of irregular shape, irregular particle size and the like are avoided, the safety performance of the composite energetic material is obviously improved, and the comprehensive performance of the composite energetic material is effectively improved.
According to the invention, through structural design and performance regulation and control of an energetic material filled layered framework composite structure, by utilizing a mesoscale confined framework filling method and adopting a mode of combining layered framework structure template preparation and energetic material solution recrystallization, the crystallization, nucleation and oriented growth recrystallization of energetic material molecules in a micro-nano layered confined space are realized, and further the energetic material filled layered framework composite structure material is obtained.
By adopting the method, the loading capacity of the energetic material of the composite structure can be quantitatively regulated and controlled according to later-stage application requirements, and the energetic material filled layered framework composite structure with different filling densities can be obtained. Furthermore, the invention can also design the layered frame structures with different scales according to the actual requirements so as to effectively reduce the sensitivity of the energetic material, improve the safety performance and realize the improvement of the performance of the energetic material.
The appearance structure characterization result shows that in the energetic material filled layered framework composite structure prepared by the method, crystals of the energetic material directionally grow in the limited space of the layered framework structure and are regularly distributed, and the natural high polymer material is uniformly distributed in the composite energetic material system, so that the common problem that the natural high polymer material cannot be uniformly distributed in the composite energetic material system is effectively solved. Furthermore, the frame structure establishes a continuous heat and mass transfer cross-linked network for the composite energetic material system, which is beneficial to enhancing the heat conduction characteristic of the composite energetic material system. Therefore, compared with the energetic material raw material, the impact sensitivity and the friction sensitivity of the energetic material filled laminated frame composite structure are obviously improved.
Drawings
FIG. 1 is a topographical view of a layered framework structure of chitosan in example 1.
FIG. 2 is a topographical view of the loading of the CL-20 solution introduced into the layered framework structure and crystallized by evaporation in example 1.
FIG. 3 is a topographic map of the energetic material CL-20 filled chitosan layered framework composite structure of example 1.
Detailed Description
The following examples further describe embodiments of the present invention. The following examples are only for illustrating the technical solutions of the present invention more clearly, and do not limit the scope of the present invention. Various changes, modifications, substitutions and alterations to these embodiments will be apparent to those skilled in the art without departing from the principles and spirit of this invention.
Example 1.
Dissolving chitosan powder in deionized water, mechanically stirring and shaking to prepare chitosan hydrosol with the concentration of 2 mg/ml.
Pouring the prepared chitosan hydrosol into a polytetrafluoroethylene heat-insulating lining with a metal bottom end by adopting an ice template method, placing the polytetrafluoroethylene heat-insulating lining on a stainless steel low-temperature platform at the temperature of about minus 40 ℃, freezing and inducing gradient crystallization of the chitosan hydrosol, and promoting directional crystallization of solvent deionized water to form layered ice crystals. And continuously freezing to promote the whole hydrosol to realize directional freezing.
And (3) freeze-drying the frozen hydrosol to obtain the chitosan layered framework structure.
And (3) observing the microstructure of the chitosan layered framework structure by using a scanning electron microscope to obtain the SEM appearance shown in the figure 1. As can be seen, the chitosan layered framework structure has a parallel layered structure, the layer thickness of the layered framework is about 500 nm-1 μm, the interlayer gap has a large internal space, and the height of the internal space is between 20 μm-80 μm.
And taking the obtained chitosan layered framework structure as a template, adding a CL-20 acetone saturated solution into the chitosan layered framework structure by adopting a template adsorption energetic material solution introduction mode, placing the chitosan layered framework structure into a vacuum drying oven, evaporating at a constant temperature of 60 ℃ for 25min, and evaporating off solvent acetone to obtain a CL-20 filled layered framework composite structure.
Fig. 2 shows a morphology chart of loading condition of introducing a CL-20 solution into a layered framework structure and evaporating for crystallization observed under a scanning electron microscope, and it can be seen that an energetic material CL-20 is attached in the chitosan layered framework structure, showing a crystallization attachment precipitation process of the CL-20 filled framework structure.
And (3) continuously adding a CL-20 acetone saturated solution into the obtained CL-20 filled layered framework composite structure by adopting the introduction mode of the template adsorption energetic material solution again, and carrying out evaporative crystallization under the same conditions.
And repeating the solution introduction and evaporation crystallization processes for 5 times to obtain a regularization and densification energetic material CL-20 filled chitosan layered framework composite structure with high energetic material loading capacity.
Figure 3 shows the SEM morphology of the regularized, densified energetic material CL-20 filled chitosan layered framework composite structure. As can be seen from fig. 1 and fig. 2, although the parallel layered chitosan layered framework structure has a larger internal space of the interlayer gap, the internal space is constrained by adjacent layers to form a domain-limited spatial structure, the CL-20 acetone saturated solution is introduced, evaporated and recrystallized to realize the preparation of the CL-20 filled layered composite structure material, and the finally obtained composite structure material has a regular and scaled micro-nano parallel sandwich structure.
According to GJB-772B-2005 'method for testing explosives and powders', an impact sensitivity instrument WL-1 is adopted to test the impact sensitivity and the friction sensitivity of the energetic material CL-20 filled chitosan layered frame composite structure, and the test evaluation results are shown in Table 1.
The test result shows that the impact sensitivity and the friction sensitivity of the obtained energetic material CL-20 filled chitosan layered frame composite structure material are respectively 70.4cm and 48 percent, and are insensitive compared with the impact sensitivity of 25.0cm and the friction sensitivity of 100 percent of the raw material CL-20, which shows that the safety performance of the prepared composite structure material is superior to that of the raw material CL-20.
Example 2.
Dissolving glucomannan powder in deionized water, mechanically stirring and shaking to prepare glucomannan hydrosol with the concentration of 2 mg/ml.
Pouring the prepared glucomannan hydrosol into a polytetrafluoroethylene heat-insulating lining with a metal bottom end by adopting an ice template method, placing the polytetrafluoroethylene heat-insulating lining on a stainless steel low-temperature platform at the temperature of about minus 40 ℃, freezing and inducing the glucomannan hydrosol to perform gradient crystallization, and promoting the solvent deionized water to directionally crystallize to form layered ice crystals. And continuously freezing to promote the whole hydrosol to realize directional freezing.
And (3) freeze-drying the frozen hydrosol to obtain a glucomannan layered framework structure with the layer thickness of about 200-500 nm and the height of the interlayer internal space of 40-100 mu m.
And (3) taking the obtained glucomannan layered framework structure as a template, adopting a mode of introducing the template to adsorb an energetic material solution, adding the HMX acetone saturated solution into the glucomannan layered framework structure, placing the glucomannan layered framework structure into a vacuum drying oven, evaporating at the constant temperature of 70 ℃ for 20min, and evaporating off the solvent acetone to obtain the HMX filled layered framework composite structure.
And (3) continuously adding the HMX acetone saturated solution into the obtained HMX filled layered framework composite structure by adopting the introduction mode of the template adsorption energetic material solution again, and carrying out evaporation crystallization under the same conditions.
And repeating the solution introduction and evaporation crystallization processes for 5 times to obtain a regularized and densified energetic material HMX filled glucomannan layered framework composite structure with high energetic material load.
The composite structure was evaluated for safety performance according to the method of example 1, and the results of the evaluation of the relevant mechanical sensitivity test are shown in table 2.
Test results show that the impact sensitivity and the friction sensitivity of the obtained energetic material HMX filled glucomannan layered framework composite structure material are respectively 92.4cm and 40%, and are insensitive compared with the impact sensitivity of 45.2cm and the friction sensitivity of 100% of the raw material HMX, which shows that the safety performance of the prepared composite structure material is superior to that of the raw material HMX.
Example 3.
Dissolving lignin powder in deionized water, mechanically stirring and shaking to prepare lignin hydrosol with the concentration of 2 mg/ml.
Pouring the prepared lignin hydrosol into a polytetrafluoroethylene heat-insulating lining with a metal bottom end by adopting an ice template method, placing the polytetrafluoroethylene heat-insulating lining on a stainless steel low-temperature platform at the temperature of about-40 ℃, freezing and inducing gradient crystallization of the lignin hydrosol, and promoting directional crystallization of solvent deionized water to form layered ice crystals. And continuously freezing to promote the whole hydrosol to realize directional freezing.
And (3) freeze-drying the frozen hydrosol to obtain a lignin laminated frame structure with the layer thickness of about 1-3 mu m and the height of the interlayer internal space of 50-90 mu m.
And (3) adding the LLM-105 dimethyl sulfoxide solution heated to 100 ℃ into the lignin layered framework structure by taking the obtained lignin layered framework structure as a template and adopting a mode of introducing the template adsorption energetic material solution, cooling to room temperature for recrystallization, crystallizing LLM-105 molecules, depositing and growing to obtain the LLM-105 filled layered framework composite structure.
And continuously adding the LLM-105 dimethyl sulfoxide solution at 100 ℃ into the obtained LLM-105 filled layered framework composite structure by adopting the introduction mode of the template adsorption energetic material solution again, and performing cooling recrystallization under the same condition.
Repeating the solution introduction and recrystallization processes for 5 times to obtain a regularized and densified energetic material LLM-105 filled lignin laminated framework composite structure with high energetic material loading.
The composite structure was evaluated for safety performance according to the method of example 1, and the results of the evaluation of the mechanical sensitivity test are shown in table 3.
The test result shows that the impact sensitivity and the friction sensitivity of the obtained energetic material LLM-105 filled lignin laminated frame composite structure material are respectively more than 112.2cm and 32 percent, and the impact sensitivity and the friction sensitivity are both insensitive compared with 74.2cm and 48 percent of the impact sensitivity and the friction sensitivity of the raw material LLM-105, which indicates that the safety performance of the prepared composite structure material is superior to that of the raw material LLM-105.
Claims (7)
1. An energetic material filled laminated frame composite structure is characterized by comprising laminated frame structures and energetic material crystals filled among the laminated frame structures, and the energetic material crystals have a regular sandwich-like periodic structure, wherein the laminated frame structures are prepared by preparing sol from polysaccharide or lignin natural polymer materials, adopting an ice template method to induce the solvent in the sol to directionally crystallize to form a laminated structure, freeze-drying the laminated structure to remove the solvent, forming a regular and periodic parallel laminated frame with parallel laminated confinement spaces in the frame, wherein the layer thickness of the laminated frame is 500 nm-5 mu m, the spacing between the laminated frames is 10 mu m-100 mu m, and the energetic material crystals are formed by introducing energetic material solution into the confinement spaces of the laminated frame structures and crystallizing;
wherein the polysaccharide or lignin natural polymer material is chitosan, glucomannan or lignin; the energetic material is one or more of HMX, CL-20, LLM-105, ADN, DAAF, TKX-50.
2. The energetic material filled layered frame composite structure as claimed in claim 1, wherein the energetic material filled layered frame composite structure contains energetic material crystals in an amount of 85-99% by mass.
3. The energetic material filled layered framework composite structure as recited in claim 1 wherein the polysaccharide or lignin based natural polymer material is prepared as an aqueous sol.
4. A method of making the energetic material filled layered framework composite structure as defined in claim 1, wherein:
1) preparing sol from polysaccharide or lignin natural polymer materials, inducing the solvent in the natural polymer material sol to directionally crystallize by adopting an ice template method to form a regular gradient laminated structure, promoting solute natural polymer materials to form a micro-nano multilayer frame structure macroscopic body, and removing the solvent between interfaces of the laminated structure by vacuum freeze drying to form a laminated frame structure with parallel laminated confinement spaces in the frame;
2) and taking the layered frame structure as a template, introducing the energetic material solution into the layered frame structure, and recrystallizing the energetic material solution in a limited space of the layered frame structure template by using external acting force to form energetic material crystals and construct an energetic material filled layered frame composite structure.
5. The method according to claim 4, wherein the step of introducing the solution of energetic material into the layered framework structure for recrystallization is repeated a plurality of times.
6. The method according to claim 4, wherein the recrystallization is any one of natural evaporation recrystallization, evaporative recrystallization, and temperature-reduced recrystallization.
7. The method according to claim 4, wherein the energetic material solution is introduced into the layered framework template by way of template adsorption of the energetic material solution.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1281729A (en) * | 1969-09-26 | 1972-07-12 | Ireco Chemicals | Slurries containing highly cross-linked thickeners |
| CN101544525A (en) * | 2009-05-05 | 2009-09-30 | 中国科学技术大学 | Energetic film composite type gunpowder and explosive, and preparation method thereof |
| CN103980075A (en) * | 2014-04-30 | 2014-08-13 | 中国工程物理研究院化工材料研究所 | Preparation method for explosive having micro-nano multistage structure |
| CN110372460A (en) * | 2019-08-02 | 2019-10-25 | 中国工程物理研究院化工材料研究所 | A kind of method of lattice intercalation induction FOX-7 explosive densification |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1281729A (en) * | 1969-09-26 | 1972-07-12 | Ireco Chemicals | Slurries containing highly cross-linked thickeners |
| CN101544525A (en) * | 2009-05-05 | 2009-09-30 | 中国科学技术大学 | Energetic film composite type gunpowder and explosive, and preparation method thereof |
| CN103980075A (en) * | 2014-04-30 | 2014-08-13 | 中国工程物理研究院化工材料研究所 | Preparation method for explosive having micro-nano multistage structure |
| CN110372460A (en) * | 2019-08-02 | 2019-10-25 | 中国工程物理研究院化工材料研究所 | A kind of method of lattice intercalation induction FOX-7 explosive densification |
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