Novel efficient cyclic mixing preparation process of high-precision delay powder

By using a high-efficiency circulating mixer and automatic ball-material separation technology, the problems of uneven mixing and safety risks in the preparation of delay agents have been solved, realizing efficient and automated preparation of delay agents and improving the combustion stability and delay accuracy of delay agents.

CN120965432APending Publication Date: 2025-11-18XIAN NORTH QINGHUA ELECTRIC APP CO LTD
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Patent Information

Application Number
CN202511148491.9
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-08-17
Publication Date
2025-11-18

AI Technical Summary

Technical Problem

Existing delayed drug preparation processes suffer from problems such as low mixing efficiency, inconsistent drug quality, easy introduction of impurities during ball milling, and difficulty in separating ball materials, which affect the accuracy and safety of the delay time and prevent automated production.

Method used

An automatic continuous circulating mixing system is adopted, combined with automatic ball material separation technology. A high-efficiency circulating mixer made of zirconia ceramic material is used for automatic feeding, mixing, discharging and cleaning. High-efficiency mixing is achieved through agitator and material circulation. The ball milling media circulates in the filter screen to ensure mixing uniformity and safety.

Benefits of technology

It improves mixing efficiency and the accuracy of delay time for delay agents, achieves human-machine isolation and automated production, ensures stable agent quality, shortens the mixing cycle, and enhances the stability of the combustion process and the accuracy of the delay time for delay agents.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention relates to a novel efficient cyclic mixing preparation process of a high-precision delay powder, and solves the problems of low mixing efficiency and poor powder quality of the existing process. An adopted device comprises an automatic feeding system, an automatic mixing system, a feed liquid circulating system, a cooling system, an automatic discharging system and an automatic cleaning system. The process comprises the following steps: S101, automatic feeding; s102, high-efficiency circulating mixing is carried out; s103, automatic discharging is carried out; and S104, automatic cleaning is carried out. Compared with the prior art, the preparation process is convenient to operate and short in mixing period, so that the mixing efficiency is greatly improved; when the efficient circulating mixer is adopted for mixing, impurities are few, chemical components are uniformly mixed, and the chemical preparation quality can be improved, so that the delay precision of the chemical is greatly improved, and the targets of stable combustion process, accurate delay time and the like are achieved; continuous circulating mixing production can be achieved, man-machine isolation operation and automatic ball material separation can be achieved, and the safety of the preparation process is guaranteed.
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Description

TECHNICAL FIELD

[0001] The present application relates to a new type of high-efficiency circulating mixing preparation process of high-precision delay composition, belonging to the technical field of pyrotechnic composition. BACKGROUND

[0002] Delay composition is a pyrotechnic composition with constant burning rate and stable combustion, which provides precise delay time for the transmission sequence or the transmission sequence. It is widely used in time fuzes, self-destruction devices, release mechanisms, second-level delay detonators, igniters and other pyrotechnic devices to realize functions such as delay initiation, millisecond blasting or delay ignition of the next level of pyrotechnic products. Delay composition is a time control agent necessary for electromagnetic interference resistance in the point transmission sequence of weapon system, and its delay time precision and point transmission reliability directly affect the reliability of weapon system action.

[0003] The traditional preparation process of delay composition is to use oxidizing agent, combustible agent, slow-burning agent and binder as raw materials, to stir them basically uniformly in a container by hand, then to stir them into a paste after adding the binder, and then to squeeze the paste into particles by forced screening, and to obtain delay composition particles after drying and screening. This process has the disadvantages of low mixing efficiency, inconsistent quality of the composition, etc., which directly affects the flowability of the charging process and the delay precision of the delay body. With the development of automatic equipment, the preparation of domestic delay composition mainly adopts physical mixing methods such as shear emulsification or ball milling, and realizes engineering production through shear emulsification machines or ball mills. However, the shear emulsification machine has mixing dead angles and stagnation layers in the container wall, bottom circumferential corners and other places, which have a great influence on the uniformity of the delay composition mixing. The rotary speed of the drum-type ball mill is low, the mixing efficiency is low, and the mixing period of the composition is long. The planetary ball mill adopts belt transmission, and is affected by factors such as belt tightness, temperature and aging, etc. There are problems such as speed difference between each ball milling unit and poor speed control precision. In particular, the ball milling tank and the ball are made of stainless steel and are not wear-resistant, and impurities are easily mixed in the ball milling process, which leads to poor controllability of the quality of the composition and affects the delay time precision. In addition, the existing delay composition adopts single-tank ball milling, V-type ball milling, planetary ball milling and other ball milling technologies, and there is a problem of manual separation of balls and materials. When separating balls and materials, a filter screen is placed above the collection tool to facilitate the filtration of the milling balls, and then the milling balls are repeatedly washed with solvent. In this whole operation process, the manual operation directly involves the handling of the composition, which has high safety risk and cannot realize automatic production. Therefore, a new type of high-efficiency circulating mixing preparation process is urgently needed to replace the existing ball milling process to improve the mixing efficiency and the quality of the composition, and to realize automatic separation of balls and materials to meet the needs of automatic production process. SUMMARY

[0004] The application aims to provide a novel high-efficiency circulating mixing preparation process for high-precision delay composition, better improve the mixing efficiency and uniformity of the composition, improve the delay precision of the delay composition under high-overload, extreme temperature and other environments, and further meet the requirements of weapon systems on delay time and delay precision.

[0005] The application is realized by the following technical solutions.

[0006] A novel high-efficiency circulating mixing preparation process for high-precision delay composition, which comprises an automatic feeding system, an automatic mixing system, a liquid circulating system, a cooling system, an automatic discharging system and an automatic cleaning system, and comprises the following steps:

[0007] S101: automatic feeding

[0008] After starting the automatic feeding system, the binder, organic solvent, oxidant and combustible agent in the feeding device are automatically fed into the high-efficiency circulating mixer storage container tank of the automatic mixing system, and the automatic feeding is closed after feeding;

[0009] S102: high-efficiency circulating mixing

[0010] The oxidant, combustible agent and binder added into the ball mill cavity of the high-efficiency circulating mixer of the automatic mixing system are automatically mixed, in the mixing process, the ball mill medium is driven by the high-speed operation of the stirrer in the ball mill cavity to strongly mix the liquid, the cooling system is opened during the mixing process, the ball mill cavity is cooled by circulating cooling water, and the temperature of the liquid is controlled at a safe temperature; the pump body of the liquid circulating system realizes the automatic circulation of the liquid in the high-efficiency circulating mixer, the liquid is ball milled in the ball mill cavity, at the same time, the liquid is discharged through the centrifugal filter screen and reenters the high-efficiency circulating mixer for repeated ball milling and mixing by the external circulation technology;

[0011] S103: automatic discharging

[0012] After the circulating mixing is completed, the liquid circulating system and the cooling system are closed, the automatic discharging system is opened, the liquid is automatically discharged from the discharge port to the collection container, and after the liquid in the high-efficiency circulating mixer is completely discharged, the automatic discharging system is closed;

[0013] S104: automatic cleaning

[0014] Water or cleaning solvent is automatically added into the high-efficiency circulating mixer in a certain amount to realize the automatic cleaning of the high-efficiency circulating mixer, and the cleaning waste liquid is automatically discharged and collected in the waste liquid barrel after the cleaning is completed.

[0015] Preferably, the mass ratio of the oxidizing agent is 60%-80%, the mass ratio of the combustible agent is 20%-40%, and the mass ratio of the adhesive is 1%-8%.

[0016] Preferably, the ball milling cavity and the ball milling medium are made of zirconia ceramic material.

[0017] Preferably, the high-efficiency circulating mixer comprises a main motor, a ball milling shaft, a stirrer, a storage container tank, a cylinder, a ball milling cavity, a ball milling medium, a cooling water inlet, a cooling water outlet, a filter screen, and a discharge port. The working process is as follows: after the material is added into the storage container tank, it enters the front part of the ball milling cavity. The main motor drives the ball milling shaft to move at a high speed. The stirrer on the ball milling shaft causes the material to collide, rub, shear, and mix with the moving ball milling medium to produce a complex physical ball milling process, which sharply refines the material. The material is pumped out from the rear part of the ball milling cavity by the pump body of the material liquid circulating system and is sent into the storage container tank for repeated circulation. At the same time, the ball milling medium cannot pass through the filter screen and is left inside the ball milling cavity, forming an internal circulation of material suction, ball milling, dispersion, and pump-out.

[0018] Preferably, during the mixing process, the mixing speed and the mixing time are remotely set and controlled through the touch display screen. During the cooling process, the temperature of the material liquid is displayed and monitored in real time on the touch display screen. During the cleaning process, the cleaning time is remotely set and controlled through the touch display screen.

[0019] Preferably, when the high-efficiency circulating mixer automatically feeds, the mixing speed is 100-500 r / min. When the high-efficiency circulating mixer mixes, the mixing speed is 500-3000 r / min.

[0020] Preferably, the oxidizing agent is one or more of lead trioxide, lead dioxide, iron sesquioxide, potassium perchlorate, barium peroxide, or barium chromate. The combustible agent is any one of tungsten powder, silicon powder, or boron powder. The adhesive is any one of fluororubber, rosin, methyl cellulose, shellac paint, or nitrocellulose paint. The organic solvent is one or more of anhydrous ethanol, acetone, or n-hexane. The cleaning solvent when the high-efficiency circulating mixer automatically cleans is one or more of water, anhydrous ethanol, acetone, or n-hexane.

[0021] Preferably, the particle size of the oxidizing agent is 20-75 μm, the particle size of the combustible agent is 10-40 μm, and the concentration of the adhesive is 2%-8%. The particle size of the ball milling medium of the high-efficiency circulating mixer is 1-5 mm.

[0022] Preferably, the ratio of the material liquid in the high-efficiency circulating mixer is 1:1-3:1, and the ratio of the ball to the material inside the ball milling cavity of the high-efficiency circulating mixer is 1:1-1:5.

[0023] Preferably, the high-efficiency circulating mixer has a circulating mixing time of 10-60 minutes, a material liquid temperature of 20-40°C during mixing, and a material liquid temperature of 20-40°C inside the ball mill cavity; the high-efficiency circulating mixer has an automatic cleaning time of 5-30 minutes.

[0024] Compared with the prior art, the beneficial effects of this invention are: (1) The preparation process is convenient to operate and has a short mixing cycle, thereby greatly improving the mixing efficiency. (2) When the preparation process uses a high-efficiency circulating mixer for mixing, there are fewer impurities and the reagent components are mixed evenly, which can improve the quality of reagent preparation, thereby greatly improving its delay accuracy and achieving the goals of stable combustion process and accurate delay time. (3) This preparation process can realize continuous circulating mixing production, realize human-machine isolation operation and automatic ball separation, so as to ensure the safety of the preparation process. Attached Figure Description

[0025] Figure 1 This is a flow chart of a novel and efficient cyclic mixing process for preparing a high-precision delayed-release drug;

[0026] Figure 2 This is a schematic diagram of the working process of a high-efficiency circulating mixer;

[0027] Figure 3 This is a schematic diagram of the ball mill cavity structure of a high-efficiency circulating mixer. Detailed Implementation

[0028] like Figures 1-3 As shown, this invention is a novel and efficient cyclic mixing process for preparing high-precision delayed-release drugs, the process is as follows: Figure 1 As shown, during the specific preparation process, the raw materials are weighed manually according to the feeding ratio and then placed sequentially into the feeding device of the high-efficiency circulating mixer. Subsequent production can achieve automatic feeding, automatic mixing, material circulation, and automatic discharge. After the discharge is completed, the equipment can be automatically cleaned.

[0029] The working process diagram of the high-efficiency circulating mixer is as follows: Figure 2 As shown, the specific systems include the following:

[0030] (1) Automatic feeding system: After the automatic feeding is started, the adhesive, organic solvent, oxidant and combustible agent in the feeding device are automatically added to the storage container of the high-efficiency circulating mixer.

[0031] (2) Automatic Mixing System: The oxidant, combustible agent, and binder added to the ball mill chamber of the high-efficiency circulating mixer are automatically mixed. During the mixing process, the high-speed rotation of the agitator inside the ball mill chamber drives the ball milling media to powerfully mix the liquid materials, improving the uniformity of the mixture. Process parameters such as mixing speed and mixing time can be remotely set and controlled via a touch screen.

[0032] (3) Liquid circulation system: The liquid is automatically circulated inside the high-efficiency circulating mixer through the pump body. While the liquid is ball-milled in the ball milling chamber, it is discharged through the centrifugal filter and re-enters the high-efficiency circulating mixer for repeated ball milling and mixing using external circulation technology, so as to achieve the purpose of fine ball milling.

[0033] (4) Cooling System: The cooling system is activated during the mixing process of the high-efficiency circulating mixer. Circulating cooling water is used to cool the ball mill cavity, controlling the temperature of the liquid material at a safe temperature to ensure the safety of the circulating mixing process. The temperature of the liquid material can be displayed and monitored in real time on the touch screen.

[0034] (5) Automatic discharge system: After the cyclic mixing process is completed, the ball material inside the ball mill cavity can be automatically separated and the liquid material can be automatically discharged.

[0035] (6) Automatic cleaning system: Automatically adds water or cleaning solvent to the high-efficiency circulating mixer in a metered manner to achieve automatic cleaning of the high-efficiency circulating mixer. After cleaning, the cleaning waste liquid can be automatically discharged and collected into the waste liquid tank. Parameters such as cleaning time can be remotely set and controlled through the touch screen.

[0036] The ball milling cavity and the ball milling media are both made of zirconia ceramic, which is harder than stainless steel. After long-term operation, the inner wall of the ball milling cavity and the surface of the ball milling media remain smooth and there is no material shedding, which solves the problem of impurities being easily mixed in during the ball milling process, and also has corrosion resistance.

[0037] Preferably, the oxidant can be one or more of lead tetroxide, lead dioxide, ferric oxide, potassium perchlorate, barium peroxide, or barium chromate.

[0038] Preferably, the particle size of the oxidant is in the range of 20-75 μm.

[0039] Preferably, the combustible agent is any one of metallic or non-metallic elements such as tungsten powder, silicon powder, or boron powder.

[0040] Preferably, the particle size of the combustible agent is between 10 and 40 μm.

[0041] Preferably, the mass ratio of the oxidant is 60%-80%.

[0042] Preferably, the mass ratio of the combustible agent is 20%-40%.

[0043] Preferably, the adhesive can be any one of fluororubber, rosin, methylcellulose, shellac, or nitrocellulose lacquer.

[0044] Preferably, the mass ratio (added) of the adhesive is between 1% and 8%, and the concentration of the adhesive is between 2% and 8%.

[0045] Preferably, the organic solvent can be one or more of anhydrous ethanol, acetone, or n-hexane.

[0046] Preferably, the feeding amount of the high-efficiency circulating mixer during automatic feeding is 0.5-3 kg.

[0047] Preferably, the mixing speed of the high-efficiency circulating mixer during automatic feeding is 100-500 r / min.

[0048] Preferably, the material-to-liquid ratio in the high-efficiency circulating mixer is 1:1 to 3:1.

[0049] Preferably, the high-efficiency circulating mixer has a mixing speed of 500-3000 r / min during the circulating mixing process.

[0050] Preferably, the high-efficiency circulating mixer has a circulating mixing time of 10-60 minutes.

[0051] Preferably, the temperature of the liquid material during mixing in the high-efficiency circulating mixer is 20-40℃.

[0052] Preferably, the temperature of the liquid material inside the ball mill cavity of the high-efficiency circulating mixer is 20-40℃.

[0053] Preferably, the grinding media inside the ball milling cavity of the high-efficiency circulating mixer is zirconia balls.

[0054] Preferably, the ball-to-material ratio inside the ball mill cavity of the high-efficiency circulating mixer is 1:1 to 1:5.

[0055] Preferably, the ball milling chamber volume of the high-efficiency circulating mixer is 0.5-2L.

[0056] Preferably, the particle size of the ball milling media in the high-efficiency circulating mixer is 1-5 mm.

[0057] Preferably, the cleaning solvent used in the automatic cleaning of the high-efficiency circulating mixer can be one or more of water, anhydrous ethanol, acetone or n-hexane.

[0058] Preferably, the automatic cleaning time of the high-efficiency circulating mixer is 5-30 minutes.

[0059] Preferably, the amount of cleaning solvent added during the automatic cleaning of the high-efficiency circulating mixer is 1-5L.

[0060] The schematic diagram of the ball mill cavity of the high-efficiency circulating mixer is shown below. Figure 3 As shown, its working principle is as follows:

[0061] The main motor drives the ball mill shaft at high speed. The agitator on the shaft moves the grinding media, generating shear force to grind and mix the material. The molten material is automatically discharged using the equipment's own kinetic energy. After being added to the storage container, the material enters the front of the ball mill chamber. Inside the chamber, driven by the high-speed agitator, the material undergoes a complex physical grinding process involving intense impact, friction, shearing, and mixing with the moving grinding media, resulting in rapid refinement. The refined material is then pumped from the rear of the chamber into the storage container for repeated circulation. Simultaneously, grinding media that cannot pass through the filter are retained inside the grinding chamber. This creates a highly efficient internal circulation: material intake → grinding → dispersion → pump discharge, resulting in highly efficient ball milling and mixing for the purpose of fine grinding.

[0062] The present invention will be further illustrated below with reference to specific embodiments, but the embodiments do not limit the present invention in any way. The essential features and significant effects of the present invention can be seen from the following embodiments. The described embodiments are some embodiments of the present invention, but not all embodiments. Therefore, they do not limit the present invention in any way. Any non-essential improvements and adjustments made by those skilled in the art based on the content of the present invention are within the protection scope of the present invention.

[0063] Example 1:

[0064] The agent mixed using the aforementioned high-efficiency circulating mixer is designated as Delay Agent No. 1. Its components include oxidizers A and B, combustible agent C, and binder D. Oxidizer A accounts for 56%, oxidizer B accounts for 22%, combustible agent C accounts for 22%, and binder is added at 1%.

[0065] (1) Raw material pretreatment and weighing

[0066] Oxidizing agents A and B, as well as combustible agent C, were all dried in an 80℃ water bath vacuum oven for 4 hours. Using a balance or electronic scale, 560g of pretreated oxidizing agent A, 220g of oxidizing agent B, and 220g of combustible agent C were weighed according to the proportions, and the weighed raw materials were placed on weighing paper. Using a graduated cylinder and beaker, 10g of adhesive D with a concentration of 4% was prepared.

[0067] (2) Automatic feeding

[0068] 0.5 kg of zirconia balls with a particle size of 1 mm were cleaned with anhydrous ethanol and placed inside the ball mill chamber. The mixing speed was set to 200 r / min on the touch screen. 10 g of the prepared binder D and 500 mL of anhydrous ethanol were added to the feeding device of the high-efficiency circulating mixer. The automatic feeding and liquid circulation systems were turned on in sequence. The binder D and anhydrous ethanol in the feeding device entered the storage container. The automatic feeding was paused. 560 g of oxidant A, 220 g of oxidant B, and 220 g of combustible agent C were added to the feeding device of the high-efficiency circulating mixer. The automatic feeding was restarted. The oxidant A, oxidant B, and combustible agent C in the feeding device entered the storage container. After adding them, the automatic feeding was turned off.

[0069] (3) High-efficiency circulating mixing

[0070] Turn on the cooling system and adjust the mixing speed to 2000 r / min and the mixing time to 30 min on the touch screen. At this time, the liquid material is automatically circulated and mixed inside the high-efficiency circulating mixer through the pump body. The agitator inside the ball mill chamber rotates at high speed, driving the ball milling media to powerfully mix the liquid material.

[0071] (4) Automatic material discharge

[0072] Before automatic feeding, place a container below the discharge port to collect the product. After the high-efficiency circulating mixing is completed, turn off the liquid circulation system and cooling system in sequence on the touch screen, and turn on automatic discharge. The liquid will automatically be discharged from the discharge port into the collection container. After the liquid inside the high-efficiency circulating mixer has been completely discharged, turn off automatic discharge.

[0073] (5) Automatic cleaning

[0074] After discharge, the high-efficiency circulating mixer is automatically cleaned. Specifically, 1.5L of anhydrous ethanol is added to the feeding device of the high-efficiency circulating mixer, and the automatic feeding is turned on. The anhydrous ethanol is automatically added to the storage container. After addition, the automatic feeding is turned off. The mixing speed is set to 200 rpm, and the liquid circulation system is turned on. The anhydrous ethanol will circulate and clean inside the high-efficiency circulating mixer for 10 minutes. After the cleaning time is up, the liquid circulation system is turned off, and the automatic discharge is turned on to automatically discharge the cleaning waste liquid and collect it in the waste liquid tank. After cleaning with anhydrous ethanol, the above steps are repeated to clean the high-efficiency circulating mixer again with 1.5L of clean water. The cleaning waste liquid is automatically discharged and collected in the waste liquid tank. After all the cleaning solvent inside the high-efficiency circulating mixer has been discharged, the automatic discharge is turned off.

[0075] To investigate the effect of mixing time on the delay performance of the prepared delayed drug during efficient circulating mixing, the mixing speed of the efficient circulating mixer was set to 2000 r / min, and other process parameters such as ball-to-material ratio and liquid-to-material ratio and process flow were kept constant. Only the mixing time during efficient circulating mixing was changed to prepare other examples, as shown in Table 1.

[0076] Table 1 Examples under different mixing times

[0077]

[0078] To investigate the effect of mixing speed on the delay performance of the prepared delayed drug during efficient circulating mixing, the mixing time of the efficient circulating mixer was set to 30 min. Other process parameters such as ball-to-material ratio and liquid-to-material ratio, as well as the process flow, were kept constant. Only the mixing time during efficient circulating mixing was changed. Other embodiments were prepared using the efficient circulating mixer, as shown in Table 2.

[0079] Table 2 Examples at different mixing speeds

[0080]

[0081] To investigate the effects of mixing speed and mixing time on the delay performance of the delaying agent, a burning rate test was conducted on the above-mentioned embodiments. The specific steps are as follows: After weighing the delaying agent, it was pressed into the plexiglass tube in the order of igniter-delaying agent-igniter, and the height of the propellant column was recorded. The pressing pressure was 3000±200N, the pressure holding time was 5s, the test voltage was 30V, and the nichrome alloy wire was heated to ignite the agent. A high-speed camera was used to collect and record the burning time in an open environment, and the burning rate of the agent was calculated.

[0082] Burn-up rate tests were conducted on the above embodiments. Three rounds of each embodiment were randomly sampled and tested. The test results are shown in Table 3.

[0083] Table 3. Combustion rate test results of the examples under different mixing speeds and mixing times.

[0084]

[0085] Comparing the burning rate experimental results of Examples 1, 2, and 3, it can be found that when other process parameters are kept constant and the mixing speed is set to 2000 r / min, the standard deviation of the burning rate of the No. 1 delay agent decreases with the increase of mixing time. When the mixing time is 10 min, the average burning rate of the No. 1 delay agent is 13.67 s / cm, and the standard deviation of the burning rate is 0.804; when the mixing time is 60 min, the average burning rate of the No. 1 delay agent is 12.34 s / cm, and the standard deviation of the burning rate is 0.254. The results show that the mixing time has a significant impact on the delay performance of the delay agent; as the mixing time increases, the burning rate of the No. 1 delay agent becomes more stable and the delay accuracy is higher.

[0086] Similarly, comparing the burning rate experimental results of Examples 1, 4, and 5, it can be found that when other process parameters are kept constant and the mixing time is set to 30 min, the standard deviation of the burning rate of the No. 1 delay agent decreases as the mixing speed increases. When the mixing speed is 500 r / min, the average burning rate of the No. 1 delay agent is 14.35 s / cm, and the standard deviation of the burning rate is 0.999; when the mixing speed is 2000 r / min, the average burning rate of the No. 1 delay agent is 12.34 s / cm, and the standard deviation of the burning rate is 0.254. The results show that the mixing speed has a significant impact on the delay performance of the delay agent; when the mixing speed increases, the burning rate of the No. 1 delay agent becomes more stable and the delay accuracy is higher.

[0087] Analysis suggests that when the mixing time is short or the mixing speed is low, the liquid material does not circulate sufficiently within the high-efficiency circulating mixer, resulting in insufficient and uneven mixing. This leads to low contact between components and uneven dispersion. Furthermore, the ball milling media within the ball mill chamber does not adequately mill the liquid material, causing variations in particle size and morphology, which in turn leads to deviations in the delay time of the delayed-release drug and poor delay accuracy. Increasing the mixing speed and time of the high-efficiency circulating mixer ensures thorough circulation and mixing of the liquid material, resulting in a delayed-release drug with excellent delay performance and precise delay time.

[0088] The combustion rate test results show that when the mixing speed of the high-efficiency circulating mixer is 2000 r / min and the mixing time is over 30 min, the combustion rate of the No. 1 delay agent prepared using the high-efficiency circulating mixer ranges from 11.71 s / mm to 12.82 s / mm. For a delay agent with a time limit of seconds, the combustion rate is relatively stable. Images captured by a high-speed camera show that the propellant column burns layer by layer downwards after ignition, indicating that the No. 1 delay agent prepared using this process is mixed relatively evenly, the combustion process of the propellant column is stable, and the delay time is accurate, thus improving the delay performance and quality of the delay agent. Furthermore, compared to traditional ball milling, the mixing time for preparing delay agents using the high-efficiency circulating mixer is significantly shortened, from 2 hours to less than 60 minutes, resulting in a substantial improvement in mixing efficiency. Simultaneously, the high-efficiency circulating mixer enables continuous circulating production, human-machine isolation, automatic separation of ball materials, and simple and convenient operation, raising the delay agent preparation process to a new level.

Claims

1. A novel and efficient cyclic mixing process for preparing high-precision delayed-release drugs, characterized by: The equipment used includes: an automatic feeding system, an automatic mixing system, a liquid circulation system, a cooling system, an automatic discharging system, and an automatic cleaning system. The process includes the following steps: S101: Automatic feeding After starting the automatic feeding system, the adhesive, organic solvent, oxidant and combustible agent in the feeding device are automatically added to the storage container of the high-efficiency circulating mixer of the automatic mixing system. After adding, the automatic feeding is turned off. S102: High-efficiency circulating mixing The oxidant, combustible agent, and binder added to the ball mill chamber of the high-efficiency circulating mixer in the automatic mixing system are automatically mixed. During the mixing process, the agitator inside the ball mill chamber rotates at high speed, driving the ball milling media to powerfully mix the liquid. The cooling system is activated during the mixing process, and the ball mill chamber is cooled by circulating cooling water to control the temperature of the liquid at a safe temperature. The pump of the liquid circulation system realizes the automatic circulation of the liquid inside the high-efficiency circulating mixer. While the liquid is ball milling in the ball mill chamber, it is discharged through a centrifugal filter and re-enters the high-efficiency circulating mixer for repeated ball milling using external circulation technology. S103: Automatic material discharge After the circulation mixing is completed, the liquid circulation system and cooling system are turned off, and the automatic discharge system is turned on. The liquid is automatically discharged from the discharge port into the collection container. After the liquid inside the high-efficiency circulation mixer is completely discharged, the automatic discharge system is turned off. S104: Automatic Cleaning The machine automatically adds water or cleaning solvent in a measured amount to the high-efficiency circulating mixer to achieve automatic cleaning of the high-efficiency circulating mixer. After cleaning, the cleaning waste liquid is automatically discharged and collected into the waste liquid tank.

2. The novel and efficient cyclic mixing preparation process for high-precision delayed-release drugs according to claim 1, characterized in that: The oxidant has a mass ratio of 60%-80%, the combustible agent has a mass ratio of 20%-40%, and the adhesive has a mass ratio between 1%-8%.

3. The novel and efficient cyclic mixing preparation process for high-precision delayed-release drugs according to claim 1, characterized in that: The ball milling cavity and the ball milling media are both made of zirconia ceramic.

4. The novel and efficient cyclic mixing preparation process for high-precision delayed-release drugs according to claim 1, characterized in that: The high-efficiency circulating mixer includes a main motor, a ball mill shaft, an agitator, a storage container, a cylinder, a ball mill cavity, ball milling media, a cooling water inlet, a cooling water outlet, a filter screen, and a discharge port. The working process is as follows: After the material is added to the storage container, it enters the front of the ball mill cavity. The main motor drives the ball mill shaft to move at high speed. The agitator on the ball mill shaft causes the material and the moving ball milling media to undergo a complex physical ball milling process, such as violent impact, friction, shearing, and mixing, which rapidly refines the material. The material is then pumped from the rear of the ball mill cavity through the pump of the material circulation system and sent to the storage container for repeated circulation. At the same time, the ball milling media cannot pass through the filter screen and is retained inside the ball mill cavity, forming a high-efficiency internal circulation of material intake → ball milling → dispersion → pump discharge.

5. The novel and efficient cyclic mixing preparation process for high-precision delayed-release drugs according to claim 1, characterized in that: During the mixing process, the mixing speed and mixing time are remotely set and controlled via a touch screen; during the cooling process, the liquid temperature is displayed and monitored in real time on the touch screen; during the cleaning process, the cleaning time is remotely set and controlled via a touch screen.

6. The novel and efficient cyclic mixing preparation process for a high-precision delayed-release drug according to claim 1, characterized in that: The high-efficiency circulating mixer has a mixing speed of 100-500 r / min during automatic feeding and a mixing speed of 500-3000 r / min during mixing.

7. The novel and efficient cyclic mixing preparation process for a high-precision delayed-release drug according to claim 1, characterized in that: The oxidant is one or more of lead tetroxide, lead dioxide, ferric oxide, potassium perchlorate, barium peroxide, or barium chromate; the combustible agent is any one of tungsten powder, silicon powder, or boron powder; the adhesive is any one of fluororubber, rosin, methylcellulose, shellac, or nitrocellulose varnish; the organic solvent is one or more of anhydrous ethanol, acetone, or n-hexane; and the cleaning solvent used in the automatic cleaning of the high-efficiency circulating mixer is one or more of water, anhydrous ethanol, acetone, or n-hexane.

8. The novel and efficient cyclic mixing preparation process for a high-precision delayed-release drug according to claim 1, characterized in that: The particle size range of the oxidant is 20-75 μm, the particle size range of the combustible agent is 10-40 μm, and the concentration range of the binder is 2%-8%; the particle size of the ball milling media of the high-efficiency circulating mixer is 1-5 mm.

9. The novel and efficient cyclic mixing preparation process for a high-precision delayed-release drug according to claim 1, characterized in that: The material-to-liquid ratio in the high-efficiency circulating mixer is 1:1-3:1, and the ball-to-material ratio inside the ball mill cavity of the high-efficiency circulating mixer is 1:1-1:

5.

10. The novel and efficient cyclic mixing preparation process for a high-precision delayed-release drug according to claim 1, characterized in that: The high-efficiency circulating mixer has a circulating mixing time of 10-60 minutes, a material liquid temperature of 20-40°C during mixing, and a material liquid temperature of 20-40°C inside the ball mill cavity; the high-efficiency circulating mixer has an automatic cleaning time of 5-30 minutes.