Iron oxide-based ammonium perchlorate composite and method for preparing the same
By preparing an iron oxide-based ammonium perchlorate composite, the problem of the difficulty in dispersing nano-sized iron oxide was solved, the catalytic efficiency and propellant combustion performance were improved, and a highly efficient combustion catalytic effect was achieved.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- XIAN MODERN CHEM RES INST
- Filing Date
- 2023-11-17
- Publication Date
- 2026-05-15
AI Technical Summary
Nanoscale iron oxide combustion catalysts are difficult to disperse effectively, which limits their catalytic combustion performance in composite propellants.
Iron oxide-based ammonium perchlorate complexes were prepared by mixing graphene iron oxide complexes with ammonium perchlorate solution and using spray granulation technology, which promoted the dispersion of nano-iron oxides and improved catalytic efficiency.
It improves the catalytic efficiency of the combustion catalyst and the mechanical properties of the propellant, while reducing the thermal decomposition peak temperature of ammonium perchlorate, thus enhancing combustion performance and safety.
Smart Images
Figure CN117623834B_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of solid propellant technology, and relates to combustion catalysts for solid propellants, specifically to an iron oxide-based ammonium perchlorate composite and its preparation method. Background Technology
[0002] Solid propellants are the power source for rocket and missile engines, and their combustion performance is closely related to the combat effectiveness and survivability of missile weapons. Therefore, the regulation of solid propellant combustion performance has become one of the key technologies restricting weapon performance, and the use of combustion catalysts is one of the most effective and direct means of regulating the burning rate.
[0003] Nanoscale iron oxide exhibits good catalytic combustion performance in composite propellants; however, its large specific surface area and surface energy make it prone to agglomeration, which significantly reduces its catalytic performance. Current physical mixing processes for composite propellants cannot effectively disperse nanoscale catalysts, resulting in poor interaction between the catalytic components and the oxidant AP. This leads to a large amount of inert catalyst being added, hindering efficient catalytic combustion. Summary of the Invention
[0004] To address the shortcomings of existing technologies, the present invention aims to provide an iron oxide-based ammonium perchlorate composite and its preparation method, thereby solving the technical problem that the nano-sized iron oxide combustion catalyst in the prior art is difficult to disperse effectively, thus limiting its combustion catalytic performance.
[0005] To solve the above-mentioned technical problems, the present invention adopts the following technical solution:
[0006] A method for preparing an iron oxide-based ammonium perchlorate composite includes the following steps: ultrasonically dispersing a graphene iron oxide composite in a solvent to obtain a graphene iron oxide composite dispersion; dissolving ammonium perchlorate in the solvent by stirring to obtain an ammonium perchlorate solution; mixing the graphene iron oxide composite dispersion and the ammonium perchlorate solution evenly by stirring, and then spray granulating under a protective atmosphere using a spray granulator. The peristaltic pump of the spray granulator rotates at a speed of 2–20 rpm, and the temperature of the working chamber of the spray granulator is 140–200℃ (depending on the selection of the solvent); after spray granulation, an iron oxide-based ammonium perchlorate composite is obtained.
[0007] The present invention also has the following technical features:
[0008] Optionally and specifically, iron oxide is used instead of graphene iron oxide composite to prepare iron oxide dispersion; the concentration of the iron oxide dispersion is 1-10 mg / mL; the mass ratio of iron oxide to ammonium perchlorate is (0.01-0.1):1.
[0009] Specifically, the solvent is selected from water, acetone, aqueous acetone solution, ethanol, ethyl acetate, and dimethylformamide.
[0010] Preferably, the volume ratio of water to acetone in the acetone aqueous solution is 1:5.
[0011] Specifically, the protective atmosphere is a nitrogen protective atmosphere or an argon protective atmosphere with an oxygen concentration of less than 1%.
[0012] Specifically, the mass ratio of graphene iron oxide composite to ammonium perchlorate is (0.01-0.1):1.
[0013] Specifically, the concentration of the graphene-iron oxide composite dispersion is 1 mg / mL.
[0014] The present invention also protects an iron oxide-based ammonium perchlorate complex prepared by the preparation method of the iron oxide-based ammonium perchlorate complex as described above.
[0015] The beneficial technical effects of this invention compared to the prior art are as follows:
[0016] (I) This invention promotes the direct interaction between iron oxide and graphene iron oxide and ammonium perchlorate by preparing an iron oxide-based ammonium perchlorate composite, thereby improving the combustion catalytic efficiency. At the same time, the use of graphene material as a support helps to disperse nano-iron oxide, further improving the combustion catalytic performance.
[0017] (II) The present invention introduces graphene material in the preparation of combustion catalyst, which helps to improve the mechanical and safety performance of propellant. Attached Figure Description
[0018] Figure 1 This is a SEM image of the iron oxide-based ammonium perchlorate complex.
[0019] Figure 2 DSC curve; Figure 2 In the diagram: the yellow curve A is the DSC curve of the iron oxide-based ammonium perchlorate complex, and the blue curve B is the DSC curve of ammonium perchlorate.
[0020] The technical solution of the present invention will be further described below with reference to the embodiments. Detailed Implementation
[0021] It should be noted that, unless otherwise specified, all raw materials used in this invention are those known in the art. For example, graphene-iron oxide composites are known composites in the prior art, described in the literature Morphology-dependent catalytic activity of Fe2O3 and its graphene-based nanocomposites on the thermal decomposition of AP (M. Zhang, FQ Zhao, H. Li, YJ Yang, T. An, YF Jiang, N. Li, FirePhysChem. 1 (2021) 46-53.), Catalytic Activity of Ferrates (NiFe2O4, ZnFe2O4 and CoFe2O4) on the Thermal Decomposition of Ammonium Perchlorate (M. Zhang, FQ Zhao, YJ Yang, T. An, WG Qu, H. Li, JK Zhang, N. Li, Propell. Explos. Pyro t. 45 (2020) 463-471.), and Effect of rGO-Fe2O3 nanocomposites fabricated indifferent solvents on the thermal The decomposition properties of ammonium perchlo rate (Ming Zhang, Fengqi Zhao, Yanjing Yang, Jiankan Zhang, Na Li, Hongxu Gao. CrystEngComm. 2018, 20, 7010-7019.) are discussed.
[0022] Following the above technical solutions, specific embodiments of the present invention are given below. It should be noted that the present invention is not limited to the following specific embodiments, and all equivalent modifications made based on the technical solutions of this application fall within the protection scope of the present invention.
[0023] Example 1:
[0024] This embodiment provides a method for preparing an iron oxide-based ammonium perchlorate complex. The method specifically includes the following steps: ultrasonically dispersing hollow microspheres of iron oxide in water (concentration 5 mg / mL) to obtain an iron oxide aqueous dispersion; dissolving ammonium perchlorate in water by stirring to obtain an ammonium perchlorate aqueous solution; mixing the iron oxide aqueous dispersion and the ammonium perchlorate aqueous solution evenly by stirring, and then spray granulating under an argon protective atmosphere (oxygen concentration less than 1%) using a spray granulator. The peristaltic pump of the spray granulator rotates at 8 rpm, and the temperature of the working chamber of the spray granulator is 160°C; after spray granulation, the iron oxide-based ammonium perchlorate complex is obtained.
[0025] Example 2:
[0026] This embodiment provides a method for preparing an iron oxide-based ammonium perchlorate complex. The method specifically includes the following steps: ultrasonically dispersing a graphene iron oxide complex in acetone (concentration 1 mg / mL) to obtain an acetone dispersion of the graphene iron oxide complex; dissolving ammonium perchlorate in acetone with stirring to obtain an ammonium perchlorate acetone solution; mixing the graphene iron oxide complex acetone dispersion and the ammonium perchlorate acetone solution evenly with stirring; then spray granulation under an argon protective atmosphere (oxygen concentration less than 1%) using a spray granulator. The peristaltic pump of the spray granulator rotates at 10 rpm, and the working chamber temperature of the spray granulator is 140°C. After spray granulation, the iron oxide-based ammonium perchlorate complex is obtained.
[0027] Example 3:
[0028] This embodiment provides a method for preparing an iron oxide-based ammonium perchlorate composite, which specifically includes the following steps: 1) Ultrasonically dispersing a graphene iron oxide composite in an acetone aqueous solution (the volume ratio of water to acetone in the acetone aqueous solution is 1:5, and the concentration is 1 mg / mL) to obtain a graphene iron oxide composite water-acetone dispersion; 2) Dissolving ammonium perchlorate in an acetone aqueous solution (the volume ratio of water to acetone in the acetone aqueous solution is 1:5) to obtain an ammonium perchlorate water-acetone solution; 3) Mixing the graphene iron oxide composite water-acetone dispersion and the ammonium perchlorate water-acetone solution evenly, and then spray granulating under a nitrogen protective atmosphere (oxygen concentration less than 1%) using a spray granulator. The peristaltic pump speed of the spray granulator is 5 rpm, and the temperature of the working chamber of the spray granulator is 150°C; 4) After spray granulation, the iron oxide-based ammonium perchlorate composite is obtained.
[0029] Material characterization: SEM images of the iron oxide-based ammonium perchlorate composites prepared in Examples 2 and 3 are shown below. Figure 1 As shown.
[0030] Effect verification:
[0031] Figure 2The DSC curves of the iron oxide-based ammonium perchlorate composites and ammonium perchlorate prepared in Examples 2 and 3 are shown. Figure 2 It can be seen that at a heating rate of 10℃ / min, ammonium perchlorate ( Figure 2 The high-temperature decomposition peak of curve B in the figure is 404.3℃, and the iron oxide-based ammonium perchlorate complex ( Figure 2 The high-temperature decomposition peak temperature of curve A) in the figure decreased to 378.5℃. The above results indicate that after being combined with iron oxide, the thermal decomposition peak temperature of ammonium perchlorate can be significantly reduced, which is conducive to the thermal decomposition of ammonium perchlorate.
Claims
1. A method for preparing an iron oxide-based ammonium perchlorate complex, characterized in that, The method specifically includes the following steps: ultrasonically dispersing graphene iron oxide composite in a solvent to obtain a graphene iron oxide composite dispersion; dissolving ammonium perchlorate in a solvent by stirring to obtain an ammonium perchlorate solution; mixing the graphene iron oxide composite dispersion and the ammonium perchlorate solution evenly by stirring, and then spray granulating under a protective atmosphere using a spray granulator. The peristaltic pump of the spray granulator rotates at a speed of 2–20 rpm, and the temperature of the working chamber of the spray granulator is 140–200 ℃; after spray granulation, an iron oxide-based ammonium perchlorate composite is obtained. The solvent is selected from water, acetone, aqueous acetone solution, ethanol, ethyl acetate, and dimethylformamide; The volume ratio of water to acetone in the acetone aqueous solution is 1:5; The protective atmosphere is a nitrogen protective atmosphere or an argon protective atmosphere with an oxygen concentration of less than 1%. The mass ratio of the graphene-iron oxide composite to ammonium perchlorate is (0.01-0.1):1; The concentration of the graphene-iron oxide composite dispersion is 0.1–2 mg / mL.
2. An iron oxide-based ammonium perchlorate complex prepared by the method described in claim 1.