Method for solving storage period abnormity of emulsion explosive based on intelligent emulsification process

Abstract

The invention belongs to the technical field of emulsion explosive manufacturing, and particularly relates to an emulsion explosive storage period abnormity solving method based on an intelligent emulsification technology, and the emulsion explosive storage period abnormity solving method comprises the following components by taking the total weight of an oil phase composition as 100 wt%: 25-35 wt% of composite wax; 20-55 wt% of self-adjusting wax; 20 to 40 wt% of an emulsifier SP-80; 0 to 15 wt% of polyisobutylene succinimide; and 0-15 wt% of a modified additive. Compared with the prior art, the oil-phase composition has the advantages that the technical problems of short storage period and easiness in abnormity of emulsion explosives in the prior art are solved by optimizing the proportion of the components in the oil-phase composition.

Description

Technical Field

[0001] This invention belongs to the field of emulsion explosive manufacturing technology, and specifically relates to a solution to abnormal storage period of emulsion explosives based on intelligent emulsification process. Background Technology

[0002] As a core category of industrial explosives, emulsion explosives directly determine the product's safety, stability, and application value through their shelf life, playing an irreplaceable role in numerous industrial fields such as mining, water conservancy and hydropower, and transportation infrastructure. In recent years, China's civil explosives industry has faced significant transformation opportunities and challenges. The transformation towards "less (unmanned), information-based, and intelligent" operations is urgently needed. Key indicators include requiring ≤3 online operators on industrial explosives production lines and eliminating Class 0 specialized production equipment, thereby improving the industry's inherent safety level and production efficiency.

[0003] Guided by this policy, relevant enterprises are actively promoting technological upgrades to their production lines. For example, Anshun Jiulian Civil Explosives Co., Ltd. has completed the technological upgrade of its 18,000-ton-per-year low-temperature emulsion explosive production line, achieving a production model with minimal or no human intervention. However, as the transformation deepens, the industry's requirements for the performance and inherent safety of emulsion explosive products are becoming increasingly stringent. The stability issues exposed during storage of products from existing production lines urgently need to be addressed, becoming a key bottleneck restricting enterprises from meeting higher industry standards and achieving high-quality development.

[0004] Current industry standards clearly stipulate that the storage period for emulsion explosives should be ≤6 months. However, Anshun Jiulian's existing production line products frequently exhibit abnormal storage conditions during actual storage, specifically premature crystallization, demulsification, and deterioration of detonation performance, severely impacting the safe use and application value of the products. Analysis reveals that the root cause of these problems lies in several core defects in existing emulsion explosive technologies, which can be summarized in the following three aspects: First, the oil phase formulation is poorly designed. The oil phase composition is the core component for constructing a stable emulsion system for emulsion explosives, and the proportions of its components directly affect the viscosity, interfacial film strength, and final storage stability of the emulsion system. In existing technologies, the proportions of key components such as composite waxes, self-mixed waxes, emulsifiers (including SP-80 and polyisobutylene succinimide), and modifying additives lack scientific quantitative basis, and a clear quantitative relationship between "viscosity-interfacial film strength-storage stability" has not been established. This blind approach to proportioning leads to inherent defects in the microstructure of the emulsion system, making it susceptible to damage from environmental factors during storage, which in turn causes problems such as crystallization and demulsification.

[0005] Secondly, the emulsification process lacks precision control. The emulsification process is a crucial step determining the final performance of emulsion explosives, and the stability of dynamic parameters such as the morphological characteristics and concentration gradient of the matrix within the pre-emulsifier directly affects product quality. Current production processes lack real-time monitoring methods for these dynamic parameters, making it impossible to promptly grasp changes in core characteristic parameters such as the average particle size and interface clarity of the matrix within the pre-emulsifier. Furthermore, adjustments to process parameters are mostly based on experience and manual adjustment or fixed parameter control, lacking adaptive adjustment capabilities. This leads to fluctuations in process parameters such as temperature, stirring speed, and feed rate, ultimately resulting in poor batch stability and further exacerbating the risk of abnormal storage conditions.

[0006] Third, storage performance verification is insufficient. Current research on the storage performance of emulsion explosives lacks a systematic approach. It fails to quantify the impact of changes in the content of key components such as self-adjusting waxes and emulsifiers on storage period through experimental systems, and it also lacks an effective storage performance prediction model. This makes it difficult for companies to identify and mitigate storage anomaly risks in advance during the production stage, forcing them to passively respond to product quality problems that arise during storage.

[0007] Further analysis of the current technological status reveals that current industry research on optimizing the storage period of emulsion explosives is largely limited to adjusting single factors, such as optimizing only the type or dosage of a particular emulsifier. This lack of a synergistic improvement scheme combining "formula optimization + intelligent control" results in limited optimization effects and makes it difficult to fundamentally improve storage stability. More critically, existing technologies lack an early warning mechanism for storage period anomalies that is compatible with unmanned production lines. This makes it impossible to monitor product performance changes in real time and issue timely warnings during continuous production, thus failing to meet the stringent requirements for product performance stability in unmanned production models.

[0008] In summary, under the policy background of intelligent and unmanned transformation of the civil explosives industry, how to break through the existing technical bottlenecks, solve the problems of short storage period and easy occurrence of abnormalities of emulsion explosives by combining the optimization of oil phase formula with the construction of intelligent emulsion process control system, and establish an early warning mechanism adapted to unmanned production, has become an urgent technical problem to be solved in this field, which is of great significance to promoting the high-quality development of the industry. Summary of the Invention

[0009] The present invention aims to provide a solution to the abnormal storage period of emulsion explosives based on intelligent emulsification process, mainly to solve the technical problems of short storage period and easy occurrence of abnormalities in existing emulsion explosives.

[0010] To solve the above-mentioned technical problems, the present invention provides the following technical solution: An oil phase composition for use in emulsion explosives, comprising the following components based on 100% by weight of the total oil phase composition: Composite wax 25-35% by weight; Self-mixed wax 20-55% by weight; Emulsifier 20-40% by weight; Polyisobutylene succinimide 0-15% by weight; Modifying additives: 0-15% by weight.

[0011] Preferably, the content of the self-adjusting wax is 30-40% by weight, the content of the emulsifier is 25-35% by weight, the content of the polyisobutylene succinimide is 3-9% by weight, and the content of the modifying additive is 6-12% by weight.

[0012] Preferably, the content of the composite wax is 33% by weight.

[0013] Preferably, the content of both polyisobutylene succinimide and the modifying additive is greater than 0 by weight.

[0014] An intelligent emulsification process system for emulsion explosives, comprising: The image acquisition module is used to acquire images of the matrix inside the pre-emulsifier in real time; The data processing module, connected to the image acquisition module, is used to analyze the acquired images and extract the characteristic parameters of the matrix, including the average particle size and interface clarity. A parameter adjustment module, connected to the data processing module, is used to adjust the emulsification process parameters based on the comparison results between the feature parameters and preset thresholds. The process parameters include temperature, stirring speed, and feed rate. The early warning module, connected to the data processing module, is used to issue an early warning when the feature parameter exceeds a preset threshold multiple times consecutively.

[0015] Preferably, the image acquisition module includes industrial cameras mounted on the top and sides of the pre-emulsifier, with a frame rate of not less than 25fps.

[0016] Preferably, the data processing module uses a convolutional neural network (CNN) algorithm for image analysis.

[0017] Preferably, the parameter adjustment module adjusts the emulsification temperature within a range of ±2℃, the stirring speed within a range of ±50r / min, and the oil phase feed rate within a range of ±0.5L / min.

[0018] Preferably, the early warning module is configured to trigger an audible and visual early warning when the feature parameter exceeds a preset threshold three times consecutively.

[0019] A method for improving the shelf life of emulsion explosives includes preparing emulsion explosives using an oil phase composition according to any one of claims 1-4, and controlling the emulsification process using an intelligent emulsification process system according to any one of claims 5-9.

[0020] Beneficial effects: 1. By optimizing the oil phase composition ratio, the synergistic effect of self-adjusting wax, emulsifier, polymeric emulsifier, and modified additives on the interfacial film strength and viscosity of the emulsion system was clearly defined, fundamentally solving the problem that existing products have a shelf life of no more than 6 months and are prone to crystallization and demulsification. This invention enables emulsion explosives to maintain a stable shelf life of more than 6 months after undergoing high and low temperature cycling tests from -30℃ to +50℃, with some optimized formulation batches even reaching 7 to 8 months, significantly exceeding industry standards.

[0021] 2. While extending the storage period, the product's key detonation performance (detonation distance ≥5cm, detonation velocity ≥4500m / s) and physical properties (density, water resistance) remain stable throughout the entire storage period, fully meeting or even exceeding industry safety standards, avoiding performance degradation caused by storage, and ensuring the reliability of end-use.

[0022] 3. The machine vision-based intelligent control system enables real-time, non-destructive detection and adaptive adjustment of microscopic parameters in the emulsification process (such as matrix particle size and concentration gradient), controlling process parameter fluctuations within ±3%. This increases the batch pass rate from approximately 95% to over 99.5%, significantly reducing storage period anomalies and quality variations caused by process fluctuations, and lowering the risk of unplanned downtime and scrap.

[0023] 4. Through scientific optimization of the oil phase formulation, modified additives are used to partially replace the more expensive specialized emulsifiers while ensuring performance, thus optimizing raw material costs. It is estimated that this will reduce unit production costs by approximately RMB 1500 per ton. Based on Anshun Jiulian Company's annual production capacity of 8000 tons, this could generate approximately RMB 12 million in economic benefits annually. Furthermore, the intelligent control system, through precise control of material input and process flow, reduces the loss rate of raw materials such as oil phase and ammonium nitrate from the current approximately 2% to below 1%, further saving production costs and improving resource utilization. Detailed Implementation

[0024] The technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are only some embodiments of the present invention, and 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.

[0025] In the description of this invention, "several" means one or more, "multiple" means two or more, "greater than," "less than," and "exceeding" are understood to exclude the stated number, while "above," "below," and "within" are understood to include the stated number. Where the terms "first," "second," and "third" are used for descriptive purposes and to distinguish technical features, they should not be construed as indicating or implying relative importance, or implicitly indicating the number of indicated technical features, or implicitly indicating the sequential relationship of the indicated technical features.

[0026] The embodiments of the present invention will now be described.

[0027] Example 1: This embodiment provides an oil phase composition for emulsion explosives, the formulation of which is based on a total oil phase weight of 100% by weight, specifically as follows: Composite wax: 25% by weight Self-mixed wax: 20% by weight Emulsifier: 40% by weight Polyisobutylene succinimide: 5% by weight Modified additive (using refined rosin): 10% by weight Preparation of emulsion explosives: Aqueous phase preparation: Mix ammonium nitrate, sodium nitrate and water in a conventional ratio, heat to 90-100℃ to dissolve, prepare a transparent aqueous solution, and keep it warm for later use.

[0028] Oil phase preparation: Mix the components of the oil phase composition in Example 1 above, heat to 85-90℃ to melt, stir evenly, and keep warm for later use.

[0029] Emulsification and Sensitization: Emulsification was carried out under the control of an intelligent emulsification process system. The insulated aqueous phase and oil phase were initially emulsified in a high-speed shear emulsifier (pre-emulsifier) ​​at a mass ratio of 92:8 via the intelligent system's feed control module. An image acquisition module (using an industrial camera with a frame rate of 30fps) monitored the matrix state within the pre-emulsifier in real time. A data processing module (based on a CNN algorithm) analyzed the data and determined that the average particle size was 1.8 μm, indicating good interface clarity. Based on this result, the parameter adjustment module stabilized the emulsification temperature at (90±2)℃, the stirring speed at (1500±50) r / min, and the total feed rate at (20±0.5) L / min. After emulsification, a latex matrix was obtained. After cooling, a chemical foaming agent was added for sensitization to produce the emulsion explosive.

[0030] In the oil phase composition of this invention, the composite wax is a mixture of paraffin wax, microcrystalline wax, and petrolatum in a weight ratio of 5:2:2. The self-adjusting wax is an oxidized paraffin wax or a Fischer-Tropsch synthetic wax that has undergone oxidative modification. Through the combination of these specific components, the viscoelasticity of the oil phase can be optimized, and it exhibits a synergistic effect with emulsifier SP-80 and high-molecular-weight emulsifiers, jointly enhancing the interfacial film strength and stability of the emulsion system. This is one of the key factors enabling this invention to extend the shelf life.

[0031] The emulsifier is a conventional emulsifier composed of Span-80 and a high molecular weight emulsifier (polyisobutylene succinic anhydride-glycerol ester).

[0032] Example 2: This embodiment provides an oil phase composition for emulsion explosives, the formulation of which is based on a total oil phase weight of 100% by weight, specifically as follows: Composite wax: 30% by weight Self-mixed wax: 55% by weight Emulsifier: 20% by weight Polyisobutylene succinimide: 0% by weight (i.e., this component is not present). Modifying additives (using petroleum resin): 0% by weight (i.e., this component is not present). Preparation of emulsion explosives: The preparation process was the same as in Example 1, except that the oil phase composition of this example was used. Monitoring by the intelligent emulsification system showed that the average particle size of the matrix particles during emulsification was 2.2 μm. The system maintained the emulsification temperature at (88±2)℃ and the stirring speed at (1400±50) r / min.

[0033] Example 3: This embodiment provides a preferred formulation of an oil phase composition, the formulation of which is based on a total oil phase weight of 100% by weight, specifically as follows: Composite wax: 33% by weight Self-mixed wax: 35% by weight Emulsifier: 30% by weight Polyisobutylene succinimide: 6% by weight Modifying additives (using composite modifiers, formulated from C9 petroleum resin and alkenyl succinate in a 1:1 ratio): 8% by weight Preparation of emulsion explosives: The preparation process was the same as in Example 1, using the oil-phase composition of this example. The intelligent emulsification process system operated stably, with the average particle size of the matrix particles being optimal at 1.5 μm, and the interface film image being clear and uniform. The process parameters fluctuated minimally throughout the emulsification process; the actual fluctuations in temperature, rotation speed, and feed rate were all less than the system's maximum adjustment range (i.e., <±3%). The warning module was not triggered.

[0034] Comparative Example 1: This comparative example uses a traditional oil-phase formulation that does not contain modified additives or polymeric emulsifiers: Composite wax: 40% by weight Ordinary paraffin: 30% by weight Emulsifier SP-80: 30% by weight Polyisobutylene succinimide: 0% by weight Modified additives: 0% by weight Emulsion explosives were prepared using the same conventional emulsification process (non-automatic, fixed process parameters) as in Example 1. The initial product was acceptable, but after undergoing high and low temperature cycling tests (7 days per cycle) from -30°C to +50°C, significant wax precipitation and demulsification occurred in the fourth month, resulting in a storage period of less than 5 months. Its detonation velocity decreased from an initial 4600 m / s to below 4300 m / s after 3 months of storage.

[0035] Comparative Example 2: This comparative example uses the exact same oil phase composition formulation as Example 3.

[0036] However, the emulsification process uses traditional manual control: fixed temperature (90℃), stirring speed (1500 r / min), and feed rate (20 L / min) are set based on the operator's experience. There is no real-time image monitoring or feedback adjustment during the production process.

[0037] Ten consecutive batches were produced, and the particle size distribution of the latex matrix ranged from 1.2 μm to 2.8 μm, exhibiting a large fluctuation. While the explosive product prepared in this way had an average shelf life superior to Comparative Example 1, two batches showed performance degradation after five months of storage, resulting in a batch pass rate of approximately 80%, far lower than the system of this invention. This demonstrates that even with an excellent formulation, process fluctuations can lead to product quality dispersion and affect shelf-life stability.

[0038] Comparative Example 3: This comparative example adjusts the oil phase formulation ratio, significantly increasing the emulsifier dosage and reducing the wax content, resulting in insufficient system strength. Composite wax: 20% by weight Self-mixed wax: 15% by weight Emulsifier SP-80: 55% by weight Polyisobutylene succinimide: 5% by weight Modified additives: 5% by weight Prepared using traditional methods, the resulting emulsion explosive exhibited low initial viscosity and poor water resistance. After three months of storage at room temperature, it showed significant oil seepage and deformation, failing to meet usage requirements. This indicates that simply adding emulsifiers cannot solve the long-term storage stability problem; the skeletal support provided by the wax component is indispensable.

[0039] Experimental verification: I. Experimental Materials and Methods 1. Sample preparation: Six sets of samples were prepared, namely Examples 1, 2, and 3, and Comparative Examples 1, 2, and 3. The specific formulations and process conditions strictly corresponded to the descriptions of the examples and comparative examples above.

[0040] 2. Testing and Evaluation Methods: (1) Storage stability test: Test method: The emulsion explosive samples prepared in each group (loaded into standard explosive cartridges) were placed in high-temperature (+50±2℃) and low-temperature (-30±2℃) constant temperature chambers for high and low temperature cycle testing. Each cycle lasted 7 days (3 days at high temperature, 3 days at low temperature, and 1 day of recovery at 25℃). Samples were periodically removed (every month / 4 cycles) and allowed to recover for 24 hours in a standard environment (25℃) for visual inspection, detonation performance testing, and microscopic observation.

[0041] Evaluation metrics: Record the time (in months) at which obvious failure phenomena such as crystallization, demulsification, oil seepage, and deformation appear on the sample, and define the "storage period" accordingly. Also record the appearance morphology at the time of failure.

[0042] (2) Detonation performance test: Detonation distance: Tested according to the standard method of "General Technical Conditions for Industrial Explosives".

[0043] Detonation velocity: determined using the probe method or chronometer method.

[0044] Testing timing: Tests were conducted at the beginning (0 months), middle (3 months), and before failure (or 6 months after storage) of the storage stability test to examine the performance degradation.

[0045] (3) Process and product uniformity test: Latex matrix particle size distribution: The D50 (median particle size) and D90 particle size of the latex concentrate after emulsification were measured using a laser particle size analyzer or image analysis method (consistent with the principle of the intelligent system), and the coefficient of variation (CV) was calculated to assess batch-to-batch fluctuations. Example group: data from 10 consecutive batches under stable operation of the intelligent system; Comparative Example 2: data from the same 10 batches under manual control.

[0046] Batch pass rate statistics: The pass rate of continuously produced batches is calculated based on the pass rate standard of "after 6 months of storage, the appearance is intact and the detonation distance is ≥5cm and the detonation velocity is ≥4500m / s".

[0047] II. Experimental Results and Data Table 1: Test Results of Storage Stability and Detonation Performance Table 2: Test Results of Process Stability and Product Uniformity III. Experimental Conclusions and Analysis 1. As shown in Table 1, Examples 1-3 using the oil-phase composition of the present invention exhibit significantly longer shelf lives (≥6-8 months) than Comparative Example 1 (<5 months) of the conventional formulation. Even at both ends of the formulation (Examples 1 and 2) and without certain functional components (Example 2), the shelf life still reaches more than 6 months, demonstrating the wide adaptability of the composite wax / self-mixed wax / SP-80 base system. The preferred formulation (Example 3), with the synergy of polyisobutylene succinimide and modified additives, exhibits better interfacial film strength and toughness, extending the shelf life to 8 months, and maintaining highly stable detonation performance (detonation velocity >4650 m / s) during the shelf life.

[0048] Comparative Example 1, lacking a polymeric emulsifier and modifying additives to strengthen the interfacial film, was prone to cracking of the wax component during low-temperature shrinkage, leading to rapid crystallization and demulsification after high- and low-temperature cycling. Comparative Example 3, due to insufficient wax skeleton, had poor overall system strength, resulting in oil seepage and deformation at room temperature. These findings collectively demonstrate that the three-in-one formulation design of this invention—"wax phase skeleton support - emulsifier interface coverage - polymer / modifier reinforcement"—is a key technology for solving the problem of long-term storage stability.

[0049] 2. Table 2 clearly shows that, using the same preferred formula, the particle size distribution of the product in Example 3 (intelligent process) is extremely uniform (CV<3%), and the batch pass rate is >99.5%; while the particle size distribution of Comparative Example 2 (traditional process) is extremely dispersed (CV>30%), resulting in a batch pass rate of only about 80%.

[0050] Traditional fixed processes cannot respond to minute fluctuations in raw materials and the environment, resulting in batch-to-batch variations in the microstructure (particle size, uniformity) of the latex matrix. This inherent deficiency directly leads to shortened shelf life and performance degradation in some batches. The intelligent system of this invention, through real-time image feedback and adaptive adjustment, controls process fluctuations within ±3%, ensuring uniform and stable microstructure in each batch from the source, thereby achieving high batch consistency in shelf life and performance.

[0051] In summary, this experiment, through a systematic comparative design, demonstrates with detailed data that the oil-phase composition provided by this invention fundamentally enhances the storage stability of emulsion explosives, while the intelligent emulsification process system ensures the stable realization of this superior performance from the production end. The combination of these two technologies jointly solves the long-standing industry problems of short shelf life, performance degradation, and large batch-to-batch fluctuations, generating significant economic benefits and demonstrating outstanding inventiveness and industrial applicability.

[0052] The foregoing description of specific exemplary embodiments of the present invention is for illustrative and explanatory purposes. These descriptions are not intended to limit the invention to the precise forms disclosed, and it is obvious that many changes and variations can be made based on the above teachings. Although embodiments of the invention have been shown and described, these specific embodiments are merely explanations of the invention and are not intended to limit it. The specific features, structures, materials, or characteristics described may be combined in any suitable manner in one or more embodiments or examples. The purpose of selecting and describing exemplary embodiments is to explain the specific principles of the invention and its practical application, so that those skilled in the art, after reading this specification, can make modifications, substitutions, variations, and various choices and changes to the embodiments as needed without departing from the principles and spirit of the invention, provided that such modifications, substitutions, variations, and choices and changes are within the scope of the claims of the invention and are protected by patent law.

Claims

1. An oil-phase composition for use in emulsion explosives, characterized in that, The oil phase composition comprises the following components, based on a total weight percentage of 100%: Composite wax 25-35% by weight; Self-mixed wax 20-55% by weight; Emulsifier SP-80 20-40% by weight; Polyisobutylene succinimide 0-15% by weight; Modifying additives: 0-15% by weight.

2. The oil phase composition for emulsion explosives according to claim 1, characterized in that, The self-adjusting wax has a content of 30-40% by weight, the emulsifier SP-80 has a content of 25-35% by weight, the polyisobutylene succinimide has a content of 3-9% by weight, and the modified additive has a content of 6-12% by weight.

3. The oil phase composition for emulsion explosives according to claim 1, characterized in that, The content of the composite wax is 33% by weight.

4. The oil phase composition for emulsion explosives according to claim 1, characterized in that, The content of both polyisobutylene succinimide and the modifying additive is greater than 0 by weight.

5. An intelligent emulsification process system for emulsion explosives, characterized in that, include: The image acquisition module is used to acquire images of the matrix inside the pre-emulsifier in real time; The data processing module, connected to the image acquisition module, is used to analyze the acquired images and extract the characteristic parameters of the matrix, including the average particle size and interface clarity. A parameter adjustment module, connected to the data processing module, is used to adjust the emulsification process parameters based on the comparison results between the feature parameters and preset thresholds. The process parameters include temperature, stirring speed, and feed rate. The early warning module, connected to the data processing module, is used to issue an early warning when the feature parameter exceeds a preset threshold multiple times consecutively.

6. The intelligent emulsification process system for emulsion explosives according to claim 5, characterized in that, The image acquisition module includes industrial cameras mounted on the top and sides of the pre-emulsifier, with a frame rate of no less than 25fps.

7. The intelligent emulsification process system for emulsion explosives according to claim 5, characterized in that, The data processing module uses a convolutional neural network (CNN) algorithm for image analysis.

8. The intelligent emulsification process system for emulsion explosives according to claim 5, characterized in that, The parameter adjustment module allows for adjustments to the emulsification temperature within a range of ±2℃, the stirring speed within a range of ±50r / min, and the oil phase feed rate within a range of ±0.5L / min.

9. An intelligent emulsification process system for emulsion explosives according to claim 5, characterized in that, The warning module is configured to trigger an audible and visual warning when the feature parameter exceeds a preset threshold three times consecutively.

10. A method for extending the shelf life of emulsion explosives, characterized in that, This includes preparing emulsion explosives using the oil phase composition according to any one of claims 1-4, and controlling the emulsification process using the intelligent emulsification process system according to any one of claims 5-9.

Images