A method for making small popping beads

Abstract

The present invention relates to the technical field of producing microencapsulated fine popping beads, and specifically to a method for producing the fine popping beads. The method comprises the following steps: preparing a high-purity core material and gelatin and gum arabic wall materials, and mixing them in a ratio of 2.5:1; forming tiny droplets using microencapsulation technology, and regulating the particle size to 0.5-2.0 mm; adding glutaraldehyde for solidification, reacting at pH 6.5, drying with nitrogen after low-temperature centrifugal cleaning, and vacuum drying until the water content is less than 4.5%, thereby obtaining finished fine popping beads with a qualified particle size. The present invention realizes real-time monitoring and precise control of the droplet particle size through the precise coordination of a high-precision microfluidic device and a laser particle size analyzer, ensuring that more than 96% of the droplet particle size is within the ideal range of 0.5-2.0 mm, thereby significantly improving the uniformity and consistency of the popping bead product. At the same time, strict screening and pretreatment of the core material and wall material, as well as refined operations in key steps such as solidification, cleaning and drying, further ensure the quality and performance of the product.

Description

Technical Field

[0001] The invention relates to the technical field of manufacturing microencapsulated fine bursting beads, in particular to a method for manufacturing the fine bursting beads. Background Art

[0002] In the food and tobacco product industries, small popping beads are an important additive or standalone product, and their production technology has always been a focus of attention. However, existing methods for producing small popping beads have obvious shortcomings in many aspects.

[0003] First, when it comes to particle size control, traditional technologies often rely on empirical judgment or simple mechanical operations, resulting in a wide range of particle size distribution in the popping beads, making it difficult to achieve ideal consistency and uniformity. This not only affects the product's appearance and taste, but also limits its application in the high-end market.

[0004] Secondly, the operations of key steps such as raw material processing and curing reaction also lack sufficient refinement. Traditional methods often ignore the pretreatment and purification of raw materials and the precise control of curing reaction conditions, which may lead to instability of the internal composition of the popping beads and affect the quality and performance of the product.

[0005] Furthermore, traditional technologies also have numerous drawbacks during the cleaning and drying processes. For example, incomplete cleaning can leave impurities on the surface of the beads, while uneven drying can compromise their integrity and stability.

[0006] More importantly, the traditional method of making small popping beads lacks efficient production equipment and a strict quality control system. This makes production efficiency low and product quality difficult to guarantee.

[0007] In summary, existing technologies for producing small popping beads suffer from significant deficiencies in particle size control, raw material processing, curing reactions, cleaning and drying, production equipment, and quality control. These shortcomings limit improvements in the quality and performance of popping beads and hinder their widespread application in the food and tobacco industries. Therefore, a novel method for producing small popping beads is urgently needed to address these issues in existing technologies. Summary of the Invention

[0008] Technical problems solved

[0009] In response to the above-mentioned shortcomings of the prior art, the present invention provides a method for producing fine explosive beads. The present invention realizes real-time monitoring and precise control of droplet particle size through the precise coordination of high-precision microfluidic equipment and laser particle size analyzer, ensuring that more than 96% of the droplet particle size is within the ideal range of 0.5-2.0mm, thereby significantly improving the uniformity and consistency of the explosive bead products. At the same time, the strict screening and pretreatment of core materials and wall materials, as well as the refined operations of key steps such as curing, cleaning and drying, further ensure the quality and performance of the product. This scientific and rigorous production method provides a strong guarantee for the preparation of high-quality fine explosive beads.

[0010] Technical Solution

[0011] To achieve the above objectives, the present invention is implemented through the following technical solutions:

[0012] A method for producing small popping beads, comprising the following steps:

[0013] First, prepare the core and wall materials. The core material is a liquid substance containing specific functional ingredients. Its purity is tested using gas chromatography-mass spectrometry to ensure that the purity reaches 99.5%. The wall material uses edible gelatin and gum arabic, mixed at a mass ratio of 2.5:1.

[0014] Next, using microencapsulation technology, the core material is injected into the wall material solution at a frequency of 150 times per second through a high-precision microfluidizer. The temperature is controlled at 27°C and the stirring speed is 400 revolutions per minute. This allows the core material to form tiny droplets in the wall material solution. A laser particle size analyzer is used to monitor the droplet size distribution in real time. When the particle size is greater than 2.0 mm, the pressure of the microfluidizer is increased by 0.7 MPa / time. When the particle size is less than 0.5 mm, the pressure is reduced by 0.4 MPa / time, ensuring that more than 96% of the droplet size is between 0.5 and 2.0 mm.

[0015] Subsequently, a curing agent, glutaraldehyde, was added to the mixed solution containing the droplets. The curing agent was 0.7% of the wall material weight at a drop rate of 3 drops per minute. The mixture was stirred at 120 revolutions per minute and reacted for 45 minutes at a pH of 6.5, so that the wall material formed a shell on the surface of the core material.

[0016] Finally, a low-temperature centrifugal cleaning device was used to clean the beads at a speed of 1200 revolutions per minute and a temperature of 6°C for 12 minutes, and the beads were washed 5 times with deionized water. The impurity content of the cleaning liquid was less than 8 mg / L after cleaning and was considered qualified. The beads were blown dry with nitrogen after cleaning and then dried in a vacuum drying oven at a vacuum degree of -0.095 MPa and a temperature of 45°C for 4 hours. The beads were monitored using a Karl Fischer moisture meter. Drying was stopped when the moisture content was less than 4.5%, and a finished product of fine beads with a particle size of 0.5-2.0 mm was obtained.

[0017] Furthermore, the preparation process of the core material further includes: pre-treating the core material raw material, wherein the core material is a liquid substance containing volatile components, and is stored and prepared in a sealed environment at a temperature controlled at 5°C. During the preparation process, high-performance liquid chromatography analysis is used to accurately control the proportion of each component, and the error is controlled within ±0.3%. The pre-treated core material is filtered using a microporous filter membrane with a pore size of 0.3μm to remove any tiny particulate impurities.

[0018] The method for making small explosive beads according to claim 1 is characterized in that the preparation process of the wall material further comprises: adding gelatin and gum arabic in a mass ratio of 2.5:1 to deionized water, stirring and dissolving at a temperature of 55°C at a speed of 250 revolutions per minute for 75 minutes to form a uniform solution, using a vacuum degassing device, degassing for 15 minutes at a vacuum degree of -0.09 MPa to remove bubbles in the solution, and after degassing, testing the viscosity of the solution by a viscometer to ensure that its viscosity is 25 mPa s to ensure that the core material droplets can be well wrapped in the subsequent microencapsulation process.

[0019] Furthermore, during the microencapsulation process, air purification equipment is used to control the number of air dust particles in the reaction area to less than 8,000 per cubic meter to prevent the influx of external impurities. At the same time, a high-speed camera is used to capture the droplet formation process at a speed of 500 frames per second, and image analysis software is used to dynamically analyze the droplet morphology and particle size changes. The pressure of the microjet equipment is further precisely controlled to ensure accurate control of the droplet particle size.

[0020] Furthermore, during the curing process, the temperature and pH value changes of the reaction system are monitored in real time by temperature sensors and pH sensors. When the pH value deviates from 6.5±0.2, disodium hydrogen phosphate-citric acid buffer solution is automatically added for adjustment to ensure that the curing reaction proceeds stably and forms a strong and uniform wall material shell.

[0021] Furthermore, during the cleaning process, the low-temperature centrifugal cleaning equipment uses a variable frequency speed regulation motor to ensure stable rotation speed during the cleaning process. After the cleaning is completed, the surface of the beads is observed by a scanning electron microscope to ensure that there are no residual impurities. When nitrogen is used for drying, the nitrogen pressure is controlled at 0.2MPa and the drying time is 10 minutes.

[0022] Furthermore, an infrared temperature sensor is provided in the vacuum drying oven to monitor the temperature at different positions of the popping beads in real time to ensure that the popping beads are heated evenly. After drying is completed, an electronic universal material testing machine is used to test the strength of the popping bead shell, and a nuclear magnetic resonance spectrometer is used to test the core material content to ensure that the finished popping beads meet the requirements of a particle size of 0.5-2.0 mm and various performance indicators are qualified.

[0023] Furthermore, during the entire production process, the production equipment is regularly maintained and calibrated, and the mechanical parts of the micro-jet equipment, stirring device and centrifugal cleaning equipment are inspected and maintained once a week, including but not limited to checking the wear of the transmission parts and the sealing of the sealing parts. The measuring instruments of the equipment, including but not limited to pressure sensors, temperature sensors and viscometers, are calibrated monthly using standard measuring instruments to ensure that the error of the measurement data is within ±0.5%.

[0024] Furthermore, a strict quality control system is established during the production process:

[0025] Inspect each batch of raw materials, including core and wall materials, for purity, content, and physical properties;

[0026] Monitor every key step in the production process, including but not limited to droplet size monitoring during microencapsulation, pH value and temperature monitoring during curing, and record relevant data in detail;

[0027] The finished popping beads are fully tested, including but not limited to particle size distribution, shell integrity and core material content. When all test items meet the predetermined standards, the batch of products is judged to be qualified products. If one item fails to meet the standards, production will be stopped immediately, the source of the problem will be traced, the production process parameters will be adjusted, and small-batch trial production will be carried out again until the product is qualified.

[0028] Beneficial effects

[0029] Compared with the known public technology, the technical solution provided by the present invention has the following advantages:

[0030] Beneficial effects:

[0031] 1. The present invention uses a high-precision microfluidic device in conjunction with a laser particle size analyzer to monitor and precisely control the droplet size distribution in real time, ensuring that more than 96% of the droplet size is within the ideal range of 0.5-2.0 mm. This precise particle size control technology greatly improves the uniformity and consistency of the small popping bead products, resulting in the final product having excellent appearance, taste, and release performance, meeting the high-quality requirements of the high-end market for small popping bead products.

[0032] 2. During the curing process, the present invention ensures the stable progress of the curing reaction by precisely controlling the addition amount of the curing agent and the reaction conditions, combined with real-time monitoring and adjustment of the temperature sensor and the pH sensor, thereby forming a strong and uniform wall material shell. At the same time, during the cleaning process, a low-temperature centrifugal cleaning device is combined with deionized water circulation cleaning to effectively remove impurities in the product. After cleaning, the impurity content is less than 8 mg / L, ensuring the purity of the product. In addition, through steps such as nitrogen drying and vacuum drying, the moisture content in the product is further reduced, thereby improving the stability and safety of the product. DETAILED DESCRIPTION

[0033] To make the objectives, technical solutions, and advantages of the present invention more clear, the technical solutions 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 ordinary technicians in this field without making any creative efforts shall fall within the scope of protection of the present invention.

[0034] The present invention will be further described below with reference to the embodiments.

[0035] Example 1

[0036] (1) Material preparation:

[0037] Core material: A volatile liquid natural fragrance containing specific functional ingredients was selected as the core material. First, its purity was tested using gas chromatography-mass spectrometry (GC-MS). After multiple tests and analyses, the purity of the liquid natural fragrance reached 99.5%. Storage and blending were carried out in a sealed environment, using a temperature control system to precisely control the temperature at 5°C. During the blending process, high-performance liquid chromatography (HPLC) analysis was used to precisely control the proportions of each ingredient, with an error of ±0.3%. For example, the target content of the main active ingredient A was 30%, and the actual content was 29.8% after HPLC analysis. The target value was finally reached by adding an appropriate amount of high-concentration active ingredient A standard. After blending, the solution was filtered using a microporous filter with a pore size of 0.3μm to remove any small particulate impurities. Before filtration, a particle counter was used to detect the number of small particles in the solution, which was approximately 500 / mL. After filtration, the number of small particles was reduced to less than 10 / mL, effectively ensuring the purity of the core material.

[0038] Wall material: Edible gelatin and gum arabic were accurately weighed in a mass ratio of 2.5:1. An appropriate amount of deionized water was added. The mixture was stirred and dissolved at 250 rpm at 55°C for 75 minutes to form a homogeneous solution. The solution was degassed using a vacuum degassing device at a vacuum degree of -0.09 MPa for 15 minutes to remove bubbles. After degassing, the solution viscosity was tested using a viscometer. After multiple measurements, the solution viscosity stabilized at 25 mPa·s.

[0039] (2) Microencapsulation process:

[0040] A high-precision microfluidic device was selected and fully calibrated and debugged before use. The number of airborne dust particles in the reaction area was controlled to below 8,000 per cubic meter. This was achieved through the high-efficiency filter in the air purification equipment. The core material was injected into the wall material solution at a frequency of 150 times per second. The temperature was controlled at 27°C and the stirring speed was 400 revolutions per minute. The droplet size distribution was monitored in real time using a laser particle size analyzer. In the early stages of the microencapsulation process, the droplet size distribution was wide, with some droplets larger than 2.0 mm. At this time, the microfluidic device pressure was increased by 0.7 MPa / time. For some droplets smaller than 0.5 mm, the pressure was reduced by 0.4 MPa / time. After multiple adjustments and monitoring, it was finally ensured that more than 96% of the droplet sizes were within the range of 0.5-2.0 mm. At the same time, the droplet formation process was filmed at a rate of 500 frames per second using a high-speed camera. The droplet morphology and particle size changes were dynamically analyzed using image analysis software to further assist in the precise control of the microfluidic device pressure.

[0041] (3) Curing process:

[0042] To the mixed solution containing the droplets, a curing agent, glutaraldehyde, is added in an amount equivalent to 0.7% of the wall material weight. The curing agent is added at a rate of 3 drops per minute using a high-precision metering pump, while stirring at a speed of 120 revolutions per minute. The reaction is carried out for 45 minutes at a pH of 6.5. During the reaction, the temperature and pH changes of the reaction system are monitored in real time by a temperature sensor and a pH sensor. When the pH value deviates from 6.5±0.2, a sodium hydrogen phosphate-citric acid buffer solution is automatically added for adjustment. For example, if the pH value rises to 6.7 after 20 minutes of reaction, the control system immediately starts the metering pump and adds an appropriate amount of buffer solution to quickly restore the pH value to around 6.5, ensuring that the curing reaction proceeds stably and forming a strong and uniform wall material shell.

[0043] (IV) Cleaning process:

[0044] The solidified bead solution was transferred to a low-temperature centrifugal cleaning device, which used a variable frequency speed regulation motor with a set speed of 1200 revolutions per minute and a temperature of 6°C for 12 minutes. After cleaning, the supernatant was poured out and the solution was washed five times with deionized water. After each washing, an inductively coupled plasma mass spectrometer (ICP-MS) was used to detect the impurity content in the cleaning solution. After the first washing, the impurity content in the cleaning solution was about 15 mg / L. After five cycles of washing, the impurity content was reduced to 5 mg / L, which was lower than the qualified standard of 8 mg / L. After the cleaning was completed, nitrogen was used for drying, the nitrogen pressure was controlled at 0.2 MPa, and the drying time was 10 minutes.

[0045] (V) Drying process:

[0046] The nitrogen-dried popping beads were placed in a vacuum drying oven with a vacuum degree of -0.095MPa and a temperature of 45°C and dried for 4 hours. An infrared temperature sensor was installed in the vacuum drying oven to monitor the temperature at different positions of the popping beads in real time to ensure that the popping beads were heated evenly. During the drying process, a Karl Fischer moisture meter was used to monitor the moisture content of the popping beads. After drying for 2 hours, the moisture content was 6%. After continuing to dry for 4 hours, the moisture content dropped to 4.2%, which was lower than the standard of 4.5%. The drying was stopped to obtain fine popping beads with a particle size of 0.5-2.0mm.

[0047] (6) Finished product testing:

[0048] Particle size distribution test: The finished popping beads were tested using a laser particle size analyzer. The results showed that 96.5% of the popping beads had a particle size within the range of 0.5-2.0 mm, which met the expected requirements.

[0049] Shell integrity inspection: The surface of the blasting beads was observed by scanning electron microscope, and no obvious residual impurities, cracks or other defects were found, indicating that the shell was intact.

[0050] Core material content detection: The core material content is detected by nuclear magnetic resonance spectrometer. After calculation, the deviation between the core material content and the theoretical value is within ±2%, which meets the product quality standards.

[0051] Example 2

[0052] (1) Material preparation:

[0053] Core material: Another liquid extract containing functional ingredients and with low volatility was selected as the core material. After GC-MS testing, its purity was 99.6%. It was stored and formulated in a sealed environment at 4°C. HPLC was used to accurately control the ingredient ratio with an error of ±0.2%. For example, the target content of the key ingredient B was 40%, and the actual content after formulation was 39.8%. After fine-tuning, it met the standard. It was also filtered using a 0.3μm microporous membrane. The number of tiny particles before filtration was about 400 / mL, and after filtration it was reduced to less than 8 / mL.

[0054] Wall material: Gelatin and gum arabic were added to deionized water in a mass ratio of 2.5:1. The mixture was stirred and dissolved at 58°C and 280 rpm for 80 minutes. After the solution was formed, it was degassed at a vacuum of -0.092 MPa for 18 minutes. The final viscosity was measured to be 26 mPa·s.

[0055] (2) Microencapsulation process:

[0056] In a purified environment (the number of dust particles is controlled below 7,000 per cubic meter), the microjet device injects the core material at a frequency of 160 times per second, the temperature is controlled at 28°C, and the stirring speed is 420 revolutions per minute. Through the coordinated control of the laser particle size analyzer, high-speed camera and image analysis software, 97% of the droplet particle size is finally in the range of 0.5-2.0mm.

[0057] (3) Curing process:

[0058] The amount of glutaraldehyde added was 0.8% of the wall material weight, the drop rate was adjusted to 4 drops per minute, the stirring speed was 130 revolutions per minute, and the reaction was carried out for 48 minutes at a pH value of 6.6. With the help of temperature and pH sensors and a buffer solution adjustment system, the reaction was stable and a good shell was formed.

[0059] (IV) Cleaning process:

[0060] The low-temperature centrifugal cleaning equipment was set at 1300 rpm, 7°C, and 15 minutes of cleaning, with six cycles of cleaning. ICP-MS analysis revealed impurity levels of approximately 13 mg / L after the first cleaning, which decreased to 4 mg / L after the final cleaning. Nitrogen drying was performed at a pressure of 0.22 MPa for 12 minutes.

[0061] (V) Drying process:

[0062] The mixture was dried in a vacuum drying oven at a vacuum degree of -0.096 MPa and a temperature of 48°C for 5 hours. An infrared temperature sensor was used to monitor and ensure uniform heating. A Karl Fischer moisture meter showed that the moisture content was 5% after 3 hours of drying and reached 4% after 5 hours, at which point the drying was stopped.

[0063] (6) Finished product testing:

[0064] Particle size distribution test: 97.2% of the popping beads have a particle size between 0.5-2.0mm.

[0065] Shell integrity inspection: There are no obvious defects in the shell under the scanning electron microscope.

[0066] Core material content detection: The deviation between the core material content and the theoretical value is ±1.8%.

[0067] Comparative Example 1 (core material purity is low)

[0068] (1) Material preparation:

[0069] Core material: A liquid natural fragrance similar to that in Example 1 was selected, but the purity was only 98%, and no strict ingredient ratio control and filtration treatment was performed.

[0070] Wall material: The same gelatin and gum arabic solution preparation method as in Example 1.

[0071] (2) Microencapsulation process:

[0072] The microencapsulation equipment and parameters of Example 1 were used for operation. However, due to the low purity and untreated core material, the droplet size distribution was relatively dispersed, with only 85% of the droplet size being within the range of 0.5-2.0 mm.

[0073] (3) Curing process:

[0074] The amount of glutaraldehyde added and the operation were the same as in Example 1, but due to the droplet size problem, the uniformity of the shell after curing was poor.

[0075] (IV) Cleaning process:

[0076] The cleaning process parameters were the same as those in Example 1, but due to the large amount of impurities in the early stage, the impurity content after the final cleaning was still as high as 12 mg / L.

[0077] (V) Drying process:

[0078] The drying parameters were the same as those in Example 1, and the moisture content after drying was 5.5%.

[0079] (6) Finished product testing:

[0080] Particle size distribution test: 85% of the popping beads have a particle size range of 0.5-2.0mm, which does not meet the requirements.

[0081] Shell integrity inspection: The shell has some defects and weak points.

[0082] Core material content detection: The deviation between the core material content and the theoretical value reaches ±5%.

[0083] Comparative Example 2 (abnormal wall material viscosity)

[0084] (1) Material preparation:

[0085] Core material: The core material processing method is the same as that in Example 1.

[0086] Wall material: When preparing the wall material solution, the stirring time was shortened to 60 min, resulting in a solution viscosity of only 20 mPa·s.

[0087] (2) Microencapsulation process:

[0088] During the microencapsulation process, due to the low viscosity of the wall material, it is difficult to effectively wrap the core material, and a large number of droplets have a particle size less than 0.5 mm, and only 70% of the droplets have a particle size within the range of 0.5-2.0 mm.

[0089] (3) Curing process:

[0090] Although the curing operation is carried out, the shell is easy to break after curing due to the poor wrapping effect.

[0091] (IV) Cleaning process:

[0092] The cleaning is difficult and many impurities remain. The final impurity content after cleaning is 10 mg / L.

[0093] (V) Drying process:

[0094] The moisture content after drying is 5%, but the beads are easy to stick together.

[0095] (6) Finished product testing:

[0096] Particle size distribution test: 70% of the popping beads have a particle size range of 0.5-2.0mm, which does not meet the standard.

[0097] Shell integrity test: Shell integrity is poor.

[0098] Core material content detection: The deviation between the core material content and the theoretical value is ±4%.

[0099] Comparative Example 3 (poor curing conditions)

[0100] (1) Material preparation:

[0101] Core material: same as the core material in Example 1.

[0102] Wall material: the same as in Example 1.

[0103] (2) Microencapsulation process:

[0104] The microencapsulation process proceeded normally, and the droplet size was controlled to be more than 96% in the range of 0.5-2.0 mm.

[0105] (3) Curing process:

[0106] The amount of glutaraldehyde added was inaccurate, only 0.5% of the wall material weight, and pH monitoring and adjustment were not performed. The pH value fluctuated greatly during the reaction, resulting in incomplete curing and low shell strength.

[0107] (IV) Cleaning process:

[0108] The impurity content after cleaning was 8 mg / L, but due to shell strength issues, some of the beads were damaged during the cleaning process.

[0109] (V) Drying process:

[0110] After drying, the moisture content is 4.8%, but the shape of the popping beads is irregular.

[0111] (6) Finished product testing:

[0112] Particle size distribution test: 96% of the beads have a particle size range of 0.5-2.0mm, but some beads are deformed.

[0113] Shell integrity inspection: The shell has damage and weak points.

[0114] Core material content detection: The deviation between the core material content and the theoretical value is ±3%.

[0115] The data comparison is shown in the table:

[0116]

[0117] Through the detailed description and data comparison of the above embodiments and comparative examples, it can be clearly seen that the method for producing small explosive beads of the present invention can produce high-quality products under the condition of strict control of various parameters. When the key steps or material parameters deviate from the standards, the product quality will be significantly reduced, which fully reflects the scientific nature and superiority of the method of the present invention. In the actual production process, the process parameters and operating steps in the embodiments should be strictly followed to ensure that the quality and performance of the small explosive beads meet the requirements.

[0118] The above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit the same. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the aforementioned embodiments, or make equivalent replacements for some of the technical features therein. However, these modifications or replacements will not cause the essence of the corresponding technical solutions to deviate from the spirit and scope of the technical solutions of the various embodiments of the present invention.

Claims

1. A method for producing small popping beads, characterized in that: The preparation method comprises the following steps: First, prepare the core and wall materials. The core material is a liquid substance containing specific functional ingredients. Its purity is tested using gas chromatography-mass spectrometry to ensure it reaches 99.5%. The wall material uses edible gelatin and gum arabic, mixed at a mass ratio of 2.5:

1. Next, using microencapsulation technology, the core material is injected into the wall material solution at a frequency of 150 times per second through a high-precision microfluidizer. The temperature is controlled at 27°C and the stirring speed is 400 revolutions per minute. This allows the core material to form tiny droplets in the wall material solution. A laser particle size analyzer is used to monitor the droplet size distribution in real time. When the particle size is greater than 2.0mm, the pressure of the microfluidizer is increased by 0.7MPa / time. When the particle size is less than 0.5mm, the pressure is reduced by 0.4MPa / time, ensuring that more than 96% of the droplets are between 0.5-2.0mm in size. Subsequently, a curing agent, glutaraldehyde, was added to the mixed solution containing the droplets. The curing agent was 0.7% of the wall material weight, and the addition rate was 3 drops per minute. The mixture was stirred at 120 revolutions per minute and reacted for 45 minutes at a pH of 6.5, so that the wall material formed a shell on the surface of the core material. Finally, the solidified popping bead solution was transferred to a low-temperature centrifugal washing device, with the speed set at 1200 revolutions per minute and the temperature at 6°C for 12 minutes. After washing, the supernatant was poured out and the solution was washed 5 times with deionized water. The impurity content of the washing solution after washing was less than 8 mg / L and was considered qualified. After washing, the solution was dried with nitrogen. The nitrogen-dried popping beads were placed in a vacuum drying oven with a vacuum degree of -0.095 MPa and a temperature of 45°C for 4 hours. The water content of the popping beads was monitored using a Karl Fischer moisture meter. When the water content was less than 4.5%, the drying was stopped to obtain fine popping beads with a particle size of 0.5-2.0 mm. The core material preparation process further includes: pre-treating the core material raw material, wherein the core material is a liquid substance containing volatile components, storing and preparing it in a sealed environment at a temperature controlled at 5°C, and during the preparation process, using high performance liquid chromatography analysis to accurately control the proportion of each component with an error controlled within ± 0.3%, and filtering the pre-treated core material using a microporous filter membrane with a pore size of 0.3 μm to remove any small particulate impurities; The preparation process of the wall material further includes: adding gelatin and gum arabic in a mass ratio of 2.5:1 to deionized water, stirring and dissolving at a temperature of 55°C and a speed of 250 revolutions per minute for 75 minutes to form a uniform solution, and using a vacuum degassing device to degas for 15 minutes at a vacuum degree of -0.09MPa to remove bubbles in the solution.

2. The method for making small popping beads according to claim 1, characterized in that: The wall material preparation process also includes testing the solution viscosity using a viscometer after degassing to ensure that the viscosity is within 25 mPa·s.

3. The method for making small popping beads according to claim 1, characterized in that: During the microencapsulation process, air purification equipment is used to control the number of air dust particles in the reaction area to less than 8,000 per cubic meter. At the same time, a high-speed camera is used to capture the droplet formation process at a speed of 500 frames per second. Combined with image analysis software, dynamic analysis of droplet morphology and particle size changes is performed to further accurately control the pressure of the microjet equipment.

4. The method for making small popping beads according to claim 1, characterized in that: During the curing process, the temperature and pH value changes of the reaction system are monitored in real time through temperature sensors and pH sensors. When the pH value deviates from 6.5±0.2, disodium hydrogen phosphate-citric acid buffer solution is automatically added for adjustment to ensure that the curing reaction proceeds stably and forms a strong and uniform wall shell.

5. The method for making small popping beads according to claim 1, characterized in that: During the cleaning process, the low-temperature centrifugal cleaning equipment uses a variable frequency speed regulation motor to ensure stable speed during the cleaning process. After cleaning, the surface of the beads is observed by scanning electron microscope to ensure that there are no residual impurities. When nitrogen is used for drying, the nitrogen pressure is controlled at 0.2MPa and the drying time is 10 minutes.

6. The method for making small popping beads according to claim 1, characterized in that: An infrared temperature sensor is installed in the vacuum drying box to monitor the temperature of different positions of the popping beads in real time to ensure that the popping beads are evenly heated. After drying, an electronic universal material testing machine is used to test the strength of the popping bead shell, and a nuclear magnetic resonance spectrometer is used to test the core material content to ensure that the finished popping beads meet the requirements of a particle size of 0.5-2.0mm and various performance indicators are qualified.

7. The method for producing small popping beads according to any one of claims 1 to 6, characterized in that: During the entire production process, the production equipment is regularly maintained and calibrated, including the micro-jet equipment, stirring device and centrifugal cleaning equipment. The mechanical parts are inspected and maintained once a week, including checking the wear of the transmission parts and the sealing of the sealing parts. The measuring instruments of the equipment, including pressure sensors, temperature sensors and viscometers, are calibrated monthly using standard measuring instruments to ensure that the error of the measurement data is within ±0.5%.

8. The method for producing small popping beads according to any one of claims 1 to 6, characterized in that: Establish a strict quality control system during the production process: Inspect each batch of raw materials, including core and wall materials, for purity, content, and physical properties; Monitor every key step in the production process, including droplet size monitoring during microencapsulation, pH value and temperature monitoring during curing, and record relevant data in detail; The finished explosive beads are fully tested, including particle size distribution, shell integrity and core material content. When all test items meet the predetermined standards, the batch of products is judged to be qualified. If one item fails, production will be stopped immediately, the source of the problem will be traced, the production process parameters will be adjusted, and small-batch trial production will be carried out again until the product is qualified.

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