Preparation method of dendritic micron ammonium perchlorate

Abstract

The invention discloses a preparation method of dendritic micron ammonium perchlorate, which comprises the following steps: firstly, dissolving ammonium perchlorate in a pyridine solvent at a certain temperature to form an ammonium perchlorate saturated solution; then, adding the saturated ammonium perchlorate solution into a high-carbon alcohol anti-solvent at a certain temperature at a certain feeding rate for recrystallization; and after a period of time, separating, washing and drying the product to obtain the dendritic micron ammonium perchlorate. The invention provides the preparation method of the dendritic micron ammonium perchlorate, the method is simple in process and simple and convenient to operate, and the obtained product is regular in morphology, high in yield, good in repeatability and suitable for large-scale production of the dendritic micron ammonium perchlorate.

Description

Technical Field

[0001] The present invention relates to a preparation method, and more particularly to a preparation method of dendritic micron ammonium perchlorate. Background Art

[0002] Ammonium perchlorate is a strong oxidizer and is widely used in fields such as propellants, pyrotechnics, and thermites. The morphology of ammonium perchlorate has a great influence on its sensitivity, charge density, and thermal decomposition performance. Therefore, the morphology control of ammonium perchlorate has always been a concern.

[0003] At present, researchers have used various crystallization methods to prepare ammonium perchlorate with various morphologies such as hexahedron (Adv. Powder Tech. 21 (2010)443–447), cube (CN117285010A), hollow structure (CN117285011A), needle beam (CN117285009A), porous (CN118637561A), butterfly (CN117285008A), and circular sheet (CN117285012A); however, in the prior art, there is still a lack of a preparation method for dendritic ammonium perchlorate with regular morphology. Summary of the Invention

[0004] The purpose of the present invention is to provide a preparation method of dendritic micron ammonium perchlorate. The method has simple process, easy operation, regular morphology of the obtained product, high yield, good repeatability, and is suitable for large-scale production of dendritic micron ammonium perchlorate.

[0005] The technical solution of the present invention is: a preparation method of dendritic micron ammonium perchlorate, characterized in that: using pyridine as a solvent and a higher alcohol as an antisolvent, and obtaining dendritic micron ammonium perchlorate by an antisolvent crystallization method; the specific steps are as follows: (1) At a certain temperature, dissolve ammonium perchlorate in a pyridine solvent to form a saturated ammonium perchlorate solution; (2) Add the saturated ammonium perchlorate solution to a higher alcohol antisolvent at a certain temperature at a certain feeding rate for recrystallization; (3) After a period of time, separate, wash, and dry the product to obtain dendritic micron ammonium perchlorate.

[0006] In step (1), the certain temperature is 20 - 30 °C.

[0007] In step (2), the certain feeding rate is 5 - 10 mL / min.

[0008] In step (2), the higher alcohol antisolvent at a certain temperature is 15 - 25 °C.

[0009] In step (2), the higher alcohol antisolvent is one of nonanol and decanol.

[0010] In step (2), the volume ratio of the ammonium perchlorate saturated solution to the higher alcohol is controlled to be 0.005 - 0.2.

[0011] In step (3), the one-stage reaction time is 5 - 15 min.

[0012] The beneficial effects of the present invention are as follows: 1. The dendritic micron ammonium perchlorate prepared by the present invention expands the morphological categories of ammonium perchlorate.

[0013] 2. The dendritic micron ammonium perchlorate prepared by the present invention has regular morphology, good dispersibility and uniform particle size.

[0014] 3. The preparation raw materials of the present invention are simple, only involving two reagents, pyridine and higher alcohol, and the production cost is low.

[0015] 4. The preparation process and production equipment of the present invention are simple and suitable for industrial production.

[0016] 5. The product of the present invention has good stability, good repeatability and high yield.

[0017] 6. The raw material ammonium perchlorate of the present invention is industrial ammonium perchlorate, with no limitation on particle size, morphology or crystal form. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] Figure 1 is the scanning electron microscope picture of the dendritic micron ammonium perchlorate obtained in Example 1; Figure 2 is the scanning electron microscope picture of the dendritic micron ammonium perchlorate obtained in Example 2; Figure 3 is the scanning electron microscope picture of the dendritic micron ammonium perchlorate obtained in Example 3; Figure 4 is the scanning electron microscope picture of the ammonium perchlorate obtained in Comparative Example 1; Figure 5 is the scanning electron microscope picture of the ammonium perchlorate obtained in Comparative Example 2; Figure 6 is the scanning electron microscope picture of the ammonium perchlorate obtained in Comparative Example 3. DETAILED DESCRIPTION OF THE INVENTION

[0019] The technical solution of the present invention will be further described below in combination with examples and comparative examples, but it should not be construed as a limitation to the technical solution. Any adaptive improvement based on this belongs to the protection scope of the present invention.

[0020] Example 1: Prepare dendritic micron ammonium perchlorate according to the following steps (1) At a temperature of 20°C, dissolve ammonium perchlorate in a pyridine solvent to form an ammonium perchlorate saturated solution; (2) Add the saturated ammonium perchlorate solution to the higher-carbon alcohol antisolvent at a temperature of 15 °C at a certain feeding rate of 10 mL / min for recrystallization; wherein, the volume ratio of the saturated ammonium perchlorate solution to the higher-carbon alcohol is controlled at 0.005, and the higher-carbon alcohol antisolvent is nonanol; (3) After 5 min, separate, wash, and dry the product to obtain dendritic micron ammonium perchlorate.

[0021] Comparative Example 1: The steps and parameters are the same as those in Example 1, except that N-methylpyrrolidone is used instead of pyridine solvent.

[0022] Example 2: Prepare dendritic micron ammonium perchlorate according to the following steps (1) Dissolve ammonium perchlorate in pyridine solvent at a temperature of 25 °C to form a saturated ammonium perchlorate solution; (2) Add the saturated ammonium perchlorate solution to the higher-carbon alcohol antisolvent at a temperature of 20 °C at a certain feeding rate of 7.5 mL / min for recrystallization; wherein, the volume ratio of the saturated ammonium perchlorate solution to the higher-carbon alcohol is controlled at 0.1025, and the higher-carbon alcohol antisolvent is decanol; (3) After 10 min, separate, wash, and dry the product to obtain dendritic micron ammonium perchlorate.

[0023] Comparative Example 2: The steps and parameters are the same as those in Example 2, except that formamide is used instead of pyridine solvent.

[0024] Example 3: Prepare dendritic micron ammonium perchlorate according to the following steps (1) Dissolve ammonium perchlorate in pyridine solvent at a temperature of 30 °C to form a saturated ammonium perchlorate solution; (2) Add the saturated ammonium perchlorate solution to the higher-carbon alcohol antisolvent at a temperature of 25 °C at a certain feeding rate of 5 mL / min for recrystallization; wherein, the volume ratio of the saturated ammonium perchlorate solution to the higher-carbon alcohol is controlled at 0.2, and the higher-carbon alcohol antisolvent is nonanol; (3) After 15 min, separate, wash, and dry the product to obtain dendritic micron ammonium perchlorate.

[0025] Comparative Example 3: The steps and parameters are the same as those in Example 3, except that N,N-dimethylformamide is used instead of pyridine solvent.

[0026] Figure 1 and Figure 2 and Figure 3 are the scanning electron microscope pictures of the dendritic micron ammonium perchlorate obtained in Examples 1, 2, and 3 respectively; it can be seen from the figure that when pyridine solvent is used for ammonium perchlorate, dendritic micron ammonium perchlorate can be obtained in nonanol or decanol antisolvent.

[0027] Figures 3 - 5Scanning electron microscope images of ammonium perchlorate products obtained in Comparative Examples 1-3, respectively; it can be seen from the figure that when N-methylpyrrolidone, formamide, and N,N-dimethylformamide are used instead of pyridine solvent, dendritic micron ammonium perchlorate cannot be obtained in nonanol or decanol antisolvents. It can be seen that the combination of pyridine solvent and nonanol or decanol antisolvent of higher alcohols in the present invention is crucial for the formation of dendritic micron ammonium perchlorate.

Claims

1. A preparation method of dendritic micron ammonium perchlorate, characterized in that: Using pyridine as the solvent and higher alcohols as the antisolvent, dendritic microammonium perchlorate is obtained by the antisolvent crystallization method. The specific steps are as follows: (1) At a certain temperature, ammonium perchlorate is dissolved in a pyridine solvent to form a saturated ammonium perchlorate solution; (2) The saturated ammonium perchlorate solution is added to a higher alcohol antisolvent at a certain temperature at a certain feeding rate for recrystallization; (3) After a period of time, the product is separated, washed, and dried to obtain dendritic microammonium perchlorate.

2. The preparation method of dendritic micro ammonium perchlorate according to claim 1, characterized in that: In step (1), the certain temperature is 20-30 °C.

3. The preparation method of dendritic micron ammonium perchlorate according to claim 1, characterized in that: In step (2), the certain feeding rate is 5-10 mL / min.

4. The preparation method of dendritic micron ammonium perchlorate according to claim 1, characterized in that: In step (2), the higher alcohol antisolvent at a certain temperature is 15-25 °C.

5. The preparation method of dendritic micron ammonium perchlorate according to claim 1, characterized in that: In step (2), the higher alcohol antisolvent is one of nonanol and decanol.

6. The preparation method of dendritic micro ammonium perchlorate according to claim 1, characterized in that: In step (2), the volume ratio of the saturated ammonium perchlorate solution to the higher alcohol is controlled at 0.005-0.

2.

7. The preparation method of dendritic micron ammonium perchlorate according to claim 1, characterized in that: In step (3), the period of reaction time is 5-15 min.

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