Spherical energetic material continuous forming and gradient flooding method and device
By employing a continuous design combining microchannel molding and three-reactor overflow in series, along with a gradient dissolution method, the problems of continuity, efficiency, and quality in the production of energetic materials were solved. This resulted in the efficient and uniform preparation of spherical particles with low solvent residue, thereby improving production efficiency and product quality.
Patent Information
- Application Number
- CN202610303990.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2026-03-13
- Publication Date
- 2026-04-24
AI Technical Summary
Existing technologies in the production of energetic materials for pharmaceutical manufacturing suffer from poor production continuity, low efficiency, easy breakage during particle transfer, lack of mild process design, and the inability of single-temperature dissolution to synergistically solve the problems of particle deformation and solvent residue.
A continuous design combining microchannel molding and three-stage overflow is adopted, along with a gradient strategy of low-temperature pre-solvent removal and high-temperature deep solvent removal. Uniform drug droplets are formed through the microchannel device, and the solvent is removed sequentially in low-temperature and high-temperature stirred tanks. Energetic materials are treated under inert gas protection and mild conditions.
It has enabled efficient and continuous production of spherical energetic materials, significantly improved particle size distribution uniformity and sphericity, reduced solvent residue to below 50 ppm, increased production efficiency by more than 40%, and solved the technical bottlenecks in traditional processes.
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Figure CN121911293A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of energetic material forming engineering technology, specifically to a method and apparatus for continuous forming and gradient dissolution of spherical energetic materials. Background Technology
[0002] In the pharmaceutical production of energetic materials, the forming quality of spherical particles (including particle size uniformity, morphological integrity, and sphericity) and the amount of residual solvent are key indicators determining product performance and are also core aspects of product quality control. Existing technologies mainly include spray drying, intermittent drop addition spheroidization, and microchannel forming, but these technologies all have insurmountable defects and cannot meet the needs of large-scale, high-quality continuous production of energetic drugs.
[0003] Spray drying is a widely used technology for preparing spherical particles. Its principle involves atomizing the drug solution and then directly exposing it to a hot gas stream, achieving integrated forming and solvent removal. However, this technology has inherent drawbacks: direct heat exchange between the atomized droplets and the high-temperature gas stream can easily lead to thermal decomposition for temperature-sensitive energetic drugs. Furthermore, the high-temperature environment can cause some materials to soften and adhere, forming irregular particles with a particle size distribution deviation (RSD) typically greater than 15%, failing to meet the quality requirements of precision pharmaceutical manufacturing. For example, Chinese patent document CN115677435A (Prior Art 1) discloses a spray drying method for preparing micro / nano spherical CL-20 / RDX eutectic explosives. While this method can obtain spherical particles with uniform particle size, the direct contact of the drug solution droplets with a high-temperature hot gas stream inevitably causes deformation and reduced sphericity in temperature-sensitive energetic materials.
[0004] Intermittent dripping, another traditional process, involves dripping the drug solution into a curing medium to form spherical particles, which then need to be manually transferred to a separate solvent removal device. This process has significant drawbacks: the connections between each stage are cumbersome, resulting in low production efficiency; particles are prone to collision and breakage during transfer, leading to a decrease in product qualification rate; and the solvent removal stage often uses a single temperature process, failing to balance morphological integrity and solvent removal effectiveness. For example, the polyvinyl alcohol immobilization spheroidization process disclosed in Chinese patent document CN101519675B (Prior Art 2) uses a single temperature curing followed by manual soaking, which suffers from discontinuous production, easy breakage during particle transfer, and a lack of mild process design for temperature-sensitive drugs.
[0005] In the core process of solvent removal, the traditional single-temperature dissolution process presents a particularly prominent technical contradiction: on the one hand, while high-temperature dissolution above 70°C can accelerate the solvent removal rate, spherical energetic materials are prone to entering the softening temperature range, deforming and breaking under stirring and shearing, with deformation rates generally exceeding 15%; on the other hand, while low-temperature dissolution below 40°C can avoid particle softening, the solvent removal rate is slow, making it difficult to reduce the residual solvent content to below the product standard of 50 ppm, and significantly extending the production cycle. This contradiction forces existing processes to compromise between particle integrity and residual solvent, severely restricting product quality improvement.
[0006] While microchannel molding technology, as an emerging method, can achieve precise control of particle size, it still has not solved the technical bottleneck of solvent removal. For example, the method for preparing spherical ADN particles based on confined microdroplets using microchannels disclosed in Chinese patent document CN113415809B (Prior Art 3) has a narrow particle size distribution, but it does not adopt a gradient dissolution design and still relies on single-temperature molding, which is not targeted enough for solvent removal and is not conducive to the complete preparation of temperature-sensitive energetic materials.
[0007] In summary, existing technologies generally suffer from the following common problems: (1) poor production continuity, mostly intermittent operation, low production efficiency, and significant performance differences between batches; (2) the molding and solvent dissolving processes are independent of each other, and the manual transfer process increases the risk of particle breakage; (3) lack of mild process design for temperature-sensitive energetic materials; and (4) single temperature-based solvent dissolving cannot synergistically solve the technical contradiction between particle deformation and solvent residue. These defects together constitute the technical bottleneck that urgently needs to be overcome in this field. Summary of the Invention
[0008] To address the problems existing in the prior art, the present invention provides a method and apparatus for continuous forming and gradient dissolution of spherical energetic materials.
[0009] To achieve the above objectives, the present invention provides the following technical solution: This invention discloses a method for continuous forming and gradient dissolution of spherical energetic materials, comprising the following steps: S1, Drug supply: The prepared drug solution is continuously delivered to the microchannel device through a metering pump; S2, Microdroplet Formation: Under a set pressure, the liquid medicine passes through the tiny channels of the microchannel device to form liquid medicine microdroplets with uniform particle size; S3. Curing and molding: The drug droplets directly enter the first stirring vessel and harden under preset curing conditions to form spherical energetic materials; S4. Low-temperature solvent removal: The solidified spherical energetic material continuously enters the second stirred tank through the overflow structure of the first stirred tank, and is heated and stirred at the first preset temperature to remove more than 80% of the solvent from the spherical energetic material. S5. High-temperature solvent removal: The spherical energetic material after low-temperature solvent removal continuously enters the third stirred tank through the overflow structure of the second stirred tank, and is heated and stirred at a second preset temperature higher than the first preset temperature to further remove residual solvent. S6. Subsequent processing: After the spherical energetic material is cooled to room temperature by a cooling device, it will continuously enter the subsequent washing, drying and packaging sections. The first, second, and third stirring vessels are connected in series via an overflow structure to achieve continuous transfer of spherical energetic materials.
[0010] Preferably, the inner diameter of the microchannel in the microchannel device is 50-200 μm, the drug delivery pressure is 0.2-0.8 MPa, the size of the formed drug droplets is 100-500 μm, and the relative standard deviation of the particle size distribution is ≤5%.
[0011] Preferably, the first mixing vessel is cooled by a water bath, with the temperature controlled at 5-25℃, the stirring speed at 50-150 r / min, and the curing time at 10-30 min.
[0012] Preferably, the second stirring vessel adopts a jacketed heating method, the first preset temperature is controlled at 40-60℃, the stirring speed is 80-200r / min, and the dissolving time is 20-40min.
[0013] Preferably, the third stirring vessel adopts a jacketed heating method, the second preset temperature is controlled at 70-90℃, the stirring speed is 80-200r / min, and the dissolving time is 15-30min.
[0014] Preferably, an inert liquid that is immiscible with the drug solution is added to the first stirring vessel as a curing medium, and the inert liquid is liquid paraffin.
[0015] Preferably, the second stirred tank is connected to a solvent condensation and recovery device for recovering the removed solvent.
[0016] Preferably, the third stirred tank is equipped with an inert gas purging device, the inert gas being nitrogen, and the nitrogen flow rate being 0.4-0.6 m³ / h. 3 / h.
[0017] This invention also discloses a device for continuous forming and gradient dissolution of spherical energetic materials, comprising: A metering pump is used to continuously deliver the prepared drug solution to the microchannel device; Microchannel devices are used to form uniformly sized microdroplets of medicine through tiny channels under a set pressure. The first stirring vessel is used to receive drug droplets and harden the droplets under preset curing conditions to form spherical energetic materials. The second stirred tank is used to receive spherical energetic materials from the first stirred tank through an overflow structure, and to heat and stir at a first preset temperature to remove solvent; The third stirred tank is used to receive spherical energetic materials from the second stirred tank through an overflow structure, and to heat and stir at a second preset temperature higher than the first preset temperature to further remove residual solvent; A cooling device for receiving spherical energetic material from the third stirred tank and cooling it to room temperature; The first, second, and third stirred tanks are connected in series via an overflow structure to achieve continuous transfer of spherical energetic materials.
[0018] Preferably, the overflow port height of the first, second, and third mixing vessels is lower than the height of the mixing blades inside the vessels, and the outer layer of the overflow pipe is provided with a heat insulation layer with a heat insulation temperature of 40-60℃.
[0019] The beneficial effects of this invention are as follows: By using a continuous design combining microchannel molding and three-reactor overflow, the transfer process of traditional intermittent processes is eliminated, resulting in a production efficiency increase of over 40% on the same scale (output per unit time reaches 0.6-1.0 kg / h). The particle size distribution deviation (RSD) of spherical energetic materials is controlled at ≤3.8%, which is far superior to the more than 15% of traditional processes, significantly reducing quality control costs.
[0020] A gradient strategy of "low-temperature pre-solvent removal (40-60℃) + high-temperature deep solvent removal (70-90℃)" is adopted: at low temperature, more than 80% of the solvent is quickly removed to avoid softening and deformation of spherical energetic materials; at high temperature, residual solvent is removed in a targeted manner. At this time, the material strength meets the requirements and shear deformation will not occur.
[0021] By combining gradient dissolution and nitrogen purging, the solvent residue can be reduced to below 50 ppm, meeting the product solvent residue standard. This solves the dilemma of excessive residue caused by single low-temperature dissolution and deformation caused by single high-temperature dissolution.
[0022] Both the curing stage (5-25℃) and the low-temperature dissolution stage (40-60℃) adopt mild conditions. Only the high-temperature dissolution stage involves a short heating period (15-30 min). With the protection of inert gas, the operating temperature is much lower than the heat sensitivity of the active ingredient, filling the technological gap in the continuous production of temperature-sensitive energetic drugs. Attached Figure Description
[0023] Figure 1This is a flow chart of the continuous forming and gradient solvent evaporation process for spherical energetic materials.
[0024] The figure illustrates the continuous process route of the present invention, including a microchannel device, a first stirring vessel (solidification stirring vessel), a second stirring vessel (low-temperature dissolution vessel), a third stirring vessel (high-temperature dissolution vessel), connecting pipes, and material flow direction. Detailed Implementation
[0025] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.
[0026] Evaluation and analysis methods: 1) Diameter and uniformity of spherical energetic materials: The diameter of spherical energetic materials was measured using a laser particle size analyzer (model LS-900), and the relative standard deviation (RSD) was calculated. 2) Deformation rate of spherical energetic materials: 100 spherical energetic materials were randomly selected, and the number of deformed particles was observed and counted under a microscope. Deformation rate = number of deformed particles / total number of particles × 100%; 3) Solvent residue: The residual amount of ethyl acetate in the spherical energetic material was determined using a gas chromatograph (model GC-2030); 4) Sphericity: The sphericity of the spherical energetic material was determined using an image analyzer (model IA-3000). Sphericity = 4π × (projected area of particle / projected perimeter of particle) 2 The closer the value is to 1, the better the sphericity. 5) Dissolution efficiency: Calculate the total dissolution time (including the transport time of spherical energetic materials) and the output per unit time (kg / h). Output per unit time = total output of spherical energetic materials in batches / total production time.
[0027] Example 1: This embodiment discloses a method and apparatus for continuous forming and gradient dissolution of spherical energetic materials, including the following steps: S1. Drug supply: The prepared drug solution (active ingredient A concentration 10wt%, solvent is ethyl acetate) is continuously delivered to the microchannel device through a metering pump, and the delivery pressure is controlled at 0.5MPa; S2. Microdroplet formation: The drug solution is formed into uniform drug solution microdroplets through a microchannel device (inner diameter 100μm), with a droplet size of about 200-300μm; S3. Curing and molding: The drug droplets are directly introduced into the first mixing vessel (curing mixing vessel). Liquid paraffin is added into the vessel as a curing medium. The water bath cooling temperature is controlled at 15℃ and the stirring speed is 100r / min. The spherical energetic material is cured in the vessel for 20min. S4. Low-temperature dissolution: The solidified spherical energetic material is continuously fed into the second stirred tank (low-temperature dissolution tank) through the overflow port of the first stirred tank. The jacket heating temperature is controlled at 50℃, the stirring speed is 150r / min, the dissolution time is 30min, and the released ethyl acetate vapor is recovered by the condensation recovery device. S5. High-Temperature Dissolution: The spherical energetic material, after low-temperature dissolution, continuously enters the third stirred tank (high-temperature dissolution tank) through the overflow port of the second stirred tank. The jacket heating temperature is controlled at 80℃, the stirring speed is 150 r / min, and nitrogen is simultaneously introduced for purging (nitrogen flow rate is 0.5 m³ / min). 3 / h), dissolution time 20min; S6. Cooling and subsequent processing: The spherical energetic material after high-temperature dissolution enters the cooling device and is cooled to 25°C by air cooling for 10 minutes. Then it continuously enters the subsequent washing, drying and packaging sections. The first stirring tank, the second stirring tank and the third stirring tank are connected in series through an overflow structure to realize the continuous transfer of the spherical energetic material.
[0028] Experimental results: The total dissolution time of the spherical energetic material prepared in this example was 50 min, and the yield per unit time was 0.8 kg / h; the particle size uniformity RSD was 3.2%, the sphericity was 0.96, the deformation rate was 1.5%, and the ethyl acetate residue was 35 ppm.
[0029] Example 2: This embodiment discloses a method and apparatus for continuous forming and gradient dissolution of spherical energetic materials, including the following steps: S1. Drug supply: The prepared drug solution (active ingredient A concentration 10wt%, solvent is ethyl acetate) is continuously delivered to the microchannel device through a metering pump, and the delivery pressure is controlled at 0.3MPa; S2. Microdroplet formation: The drug solution is formed into uniform drug solution microdroplets through a microchannel device (inner diameter 150μm), with a microdroplet size of about 300-400μm; S3. Curing and molding: The drug droplets are directly introduced into the first mixing vessel (curing mixing vessel). Liquid paraffin is added into the vessel as a curing medium. The water bath cooling temperature is controlled at 20℃ and the stirring speed is 80r / min. The spherical energetic material is cured in the vessel for 15min. S4. Low-temperature dissolution: The solidified spherical energetic material is continuously fed into the second stirred tank (low-temperature dissolution tank) through the overflow port of the first stirred tank. The jacket heating temperature is controlled at 55℃, the stirring speed is 120r / min, the dissolution time is 25min, and the released ethyl acetate vapor is recovered by the condensation recovery device. S5. High-Temperature Dissolution: The spherical energetic material, after low-temperature dissolution, continuously enters the third stirred tank (high-temperature dissolution tank) through the overflow port of the second stirred tank. The jacket heating temperature is controlled at 85℃, the stirring speed is 120 r / min, and nitrogen is simultaneously introduced for purging (nitrogen flow rate is 0.4 m³ / min). 3 / h), dissolution time 18min; S6. Cooling and subsequent processing: The spherical energetic material after high-temperature dissolution enters the cooling device and is cooled to 22°C by water cooling for 8 minutes. Then it continuously enters the subsequent washing, drying and packaging sections. The first stirring tank, the second stirring tank and the third stirring tank are connected in series through an overflow structure to realize the continuous transfer of the spherical energetic material.
[0030] Experimental results: The total dissolution time of the spherical energetic material prepared in this example was 43 min, the yield per unit time was 1.0 kg / h; the particle size uniformity RSD was 3.8%, the sphericity was 0.95, the deformation rate was 1.8%, and the ethyl acetate residue was 32 ppm.
[0031] Example 3: This embodiment discloses a method and apparatus for continuous forming and gradient dissolution of spherical energetic materials, including the following steps: S1. Drug supply: The prepared drug solution (active ingredient A concentration 10wt%, solvent is ethyl acetate) is continuously delivered to the microchannel device through a metering pump, and the delivery pressure is controlled at 0.7MPa; S2. Microdroplet formation: The drug solution is formed into uniform drug solution microdroplets through a microchannel device (inner diameter 80μm), with a droplet size of about 150-250μm; S3. Curing and molding: The drug droplets are directly introduced into the first mixing vessel (curing mixing vessel). Liquid paraffin is added into the vessel as a curing medium. The water bath cooling temperature is controlled at 10℃ and the stirring speed is 130r / min. The spherical energetic material is cured in the vessel for 25min. S4. Low-temperature dissolution: The solidified spherical energetic material is continuously fed into the second stirred tank (low-temperature dissolution tank) through the overflow port of the first stirred tank. The jacket heating temperature is controlled at 45℃, the stirring speed is 180r / min, the dissolution time is 35min, and the ethyl acetate vapor is recovered by the condensation recovery device. S5. High-Temperature Dissolution: The spherical energetic material, after low-temperature dissolution, continuously enters the third stirred tank (high-temperature dissolution tank) through the overflow port of the second stirred tank. The jacket heating temperature is controlled at 75℃, the stirring speed is 180 r / min, and nitrogen is simultaneously introduced for purging (nitrogen flow rate is 0.6 m³ / min). 3 / h), dissolution time 25min; S6. Cooling and subsequent processing: The spherical energetic material after high-temperature dissolution enters the cooling device and is cooled to 28°C by air cooling for 12 minutes. Then it continuously enters the subsequent washing, drying and packaging sections. The first stirring tank, the second stirring tank and the third stirring tank are connected in series through an overflow structure to realize the continuous transfer of the spherical energetic material.
[0032] Experimental results: The total dissolution time of the spherical energetic material prepared in this example was 60 min, and the yield per unit time was 0.6 kg / h; the particle size uniformity RSD was 2.9%, the sphericity was 0.97, the deformation rate was 1.2%, and the ethyl acetate residue was 38 ppm.
[0033] Comparative Example 1 (Traditional single high-temperature dissolution process): A method and apparatus for continuous molding and gradient dissolution of spherical energetic materials are disclosed. The method employs the same solvent and microchannel molding and curing process as in Example 1. The cured spherical energetic materials are directly fed into a single high-temperature dissolution vessel (temperature 80℃, stirring speed 150 r / min, dissolution time 50 min), with all other conditions consistent with Example 1. Experimental results: total dissolution time 50 min, yield per unit time 0.7 kg / h; particle size uniformity RSD of spherical energetic materials = 4.5%, sphericity = 0.88, deformation rate = 18.6%, ethyl acetate residue = 42 ppm. Comparison shows that the process of this invention can significantly reduce the deformation rate and improve the sphericality of spherical energetic materials while ensuring effective solvent removal.
[0034] Comparative Example 2 (Intermittent Dissolution Process): A method and apparatus for continuous molding and gradient dissolution of spherical energetic materials are disclosed. The method employs the same chemical solution and microchannel molding and curing process as in Example 1. The cured spherical energetic materials are manually transferred to an intermittent dissolution vessel (transfer time 15 min). First, low-temperature dissolution is performed at 50℃ and 150 r / min for 30 min, followed by high-temperature dissolution at 80℃ and 150 r / min for 20 min. Nitrogen purging parameters are consistent with Example 1. After dissolution, the materials are manually transferred to a cooling device (transfer time 10 min), with cooling conditions consistent with Example 1. Experimental results: total dissolution and transfer time 75 min, yield per unit time 0.4 kg / h; particle size uniformity RSD of spherical energetic materials = 5.3%, sphericity = 0.91, deformation rate = 5.2%, ethyl acetate residue = 39 ppm. Comparison shows that the continuous process of this invention has significantly higher dissolution efficiency (yield per unit time) than the intermittent process, and the spherical energetic materials exhibit better particle size uniformity and sphericity, and lower deformation rate.
[0035] The results are shown in Table 1.
[0036] Table 1 Total dissolution time (min) Output per unit time (kg / h) Particle size distribution RSD (%) sphericity Deformation rate (%) Solvent residue (ppm) Example 1 50 0.8 3.2 0.96 1.5 35 Example 2 43 1.0 3.8 0.95 1.8 32 Example 3 60 0.6 2.9 0.97 1.2 38 Comparative Example 1 (Single Temperature Dissolution, Prior Art 1) 50 0.7 4.5 0.88 18.6 42 Comparative Example 2 (Intermittent dissolution, prior art 2) 75 0.4 5.3 0.91 5.2 39 The above embodiments are only used to illustrate the technical solutions of the present invention, and are not intended to limit it. Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some of the technical features. Such modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims
1. A method for continuous forming and gradient dissolution of spherical energetic materials, characterized in that, Includes the following steps: S1, Drug supply: The prepared drug solution is continuously delivered to the microchannel device through a metering pump; S2, Microdroplet Formation: Under a set pressure, the liquid medicine passes through the tiny channels of the microchannel device to form liquid medicine microdroplets with uniform particle size; S3. Curing and molding: The drug droplets directly enter the first stirring vessel and harden under preset curing conditions to form spherical energetic materials; S4. Low-temperature solvent removal: The solidified spherical energetic material continuously enters the second stirred tank through the overflow structure of the first stirred tank, and is heated and stirred at the first preset temperature to remove more than 80% of the solvent from the spherical energetic material. S5. High-temperature solvent removal: The spherical energetic material after low-temperature solvent removal continuously enters the third stirred tank through the overflow structure of the second stirred tank, and is heated and stirred at a second preset temperature higher than the first preset temperature to further remove residual solvent. S6. Subsequent processing: After the spherical energetic material is cooled to room temperature by a cooling device, it will continuously enter the subsequent washing, drying and packaging sections. The first, second, and third stirring vessels are connected in series via an overflow structure to achieve continuous transfer of spherical energetic materials.
2. The method for continuous forming and gradient dissolution of spherical energetic materials according to claim 1, characterized in that, The microchannel device has an inner diameter of 50-200 μm, a drug delivery pressure of 0.2-0.8 MPa, and the resulting drug droplet size is 100-500 μm with a relative standard deviation of ≤5% for particle size distribution.
3. The method for continuous forming and gradient dissolution of spherical energetic materials according to claim 1, characterized in that, The first mixing vessel adopts a water bath cooling method, with the temperature controlled at 5-25℃, the stirring speed at 50-150 r / min, and the curing time at 10-30 min.
4. The method for continuous forming and gradient dissolution of spherical energetic materials according to claim 1, characterized in that, The second stirred tank adopts a jacketed heating method, with the first preset temperature controlled at 40-60℃, the stirring speed at 80-200 r / min, and the dissolution time at 20-40 min.
5. The method for continuous forming and gradient dissolution of spherical energetic materials according to claim 1, characterized in that, The third stirring vessel adopts a jacketed heating method, with the second preset temperature controlled at 70-90℃, the stirring speed at 80-200 r / min, and the dissolution time at 15-30 min.
6. The method for continuous forming and gradient dissolution of spherical energetic materials according to claim 1, characterized in that, An inert liquid that is immiscible with the drug solution is added to the first stirring vessel as a curing medium, and the inert liquid is liquid paraffin.
7. The method for continuous forming and gradient dissolution of spherical energetic materials according to claim 1, characterized in that, The second stirred tank is connected to a solvent condensation and recovery device for recovering the removed solvent.
8. The method for continuous forming and gradient dissolution of spherical energetic materials according to claim 1, characterized in that, The third stirred tank is equipped with an inert gas purging device, the inert gas being nitrogen, with a nitrogen flow rate of 0.4-0.6 m³ / h. 3 / h.
9. A device for continuous molding and gradient dissolution of spherical energetic materials, comprising a metering pump as described in any one of claims 1-8, for continuously delivering the prepared drug solution to a microchannel device; The continuous forming and gradient dissolution apparatus for spherical energetic materials also includes: Microchannel devices are used to form uniformly sized microdroplets of medicine through tiny channels under a set pressure. The first stirring vessel is used to receive drug droplets and harden the droplets under preset curing conditions to form spherical energetic materials. The second stirred tank is used to receive spherical energetic materials from the first stirred tank through an overflow structure, and to heat and stir at a first preset temperature to remove solvent; The third stirred tank is used to receive spherical energetic materials from the second stirred tank through an overflow structure, and to heat and stir at a second preset temperature higher than the first preset temperature to further remove residual solvent; A cooling device for receiving spherical energetic material from the third stirred tank and cooling it to room temperature; The first, second, and third stirred tanks are connected in series via an overflow structure to achieve continuous transfer of spherical energetic materials.
10. The continuous forming and gradient dissolution apparatus for spherical energetic materials according to claim 9, characterized in that, The overflow port height of the first, second, and third mixing vessels is lower than the height of the mixing blades inside the vessels, and the outer layer of the overflow pipe is provided with a heat insulation layer with a heat insulation temperature of 40-60℃.
Citation Information
Patent Citations
L-lactic acid fermentation method by using polyvinyl alcohol to solidify rhizopus oryzae
CN101519675B
A spherical ADN particle, its preparation method and its application
CN113415809B
Micro-nano spherical high-energy insensitive CL-20 / RDX eutectic explosive and preparation method thereof
CN115677435A
