A biological anionic salt preparation and its preparation method
By adjusting the water activity and pulse pressure of the lignocellulose carrier, anionic salt particles are driven to deeply embed into the tracheid lumen. Combined with acoustic impedance feedback adjustment, the problems of embedding and stabilization of anionic salt preparations during mechanized stirring are solved, achieving high drug loading and physical steady state, and reducing feed intake and production costs.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- CHANGCHUN BORUI FEED
- Filing Date
- 2026-03-25
- Publication Date
- 2026-05-26
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Figure CN121926291B_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of animal feed processing technology, and particularly relates to a biological anionic salt preparation and its preparation method. Background Technology
[0002] Currently, in the process of regulating metabolic diseases in dairy cows during the peripartum period, the use of anionic salt preparations to adjust the anion-cation difference is a widely accepted feeding method in the industry. The mainstream technology mostly uses oils or polymers as taste-masking media, covering salt particles through surface physical encapsulation, thereby solving the problem of feed inhibition caused by the bitterness of the components. Such solutions can play a certain role in masking taste under specific working conditions. However, in the mechanized mixing and automated feeding process of total mixed rations, the encapsulation layer is subject to high-intensity shearing and collision, which can easily lead to physical peeling, causing the active components to dissolve instantly and causing the risk of refusal to eat. In order to maintain the structural strength of the encapsulation layer, it is usually necessary to increase the proportion of the taste-masking medium added, reduce the active component loading in the preparation, increase the animal's feed load and production costs.
[0003] Biomass carriers possess natural tracheal lumen micropores, ideal spaces for containing salt particles. However, due to the elastic modulus characteristics of plant fibers, the entrances to these micropores are often in a contracted state under normal conditions. When hard particles are pressed in, an arching effect occurs, leading to low embedding efficiency. A linear approach of increasing processing pressure can cause irreversible collapse damage to the fiber skeleton, while chemical opening methods can destroy the carrier's bioactivity and leave residues. Existing technologies face irreconcilable technical constraints regarding drug loading, physical homeostasis, and bioactivity protection. Besides the limitations of the hardware carrier's morphology, control methods also have limitations. For example, Chinese invention patent CN1203897C discloses a continuously releasing pharmaceutically active peptide salt and its production. It utilizes the interaction between anions and cations between peptide compounds and carrier macromolecules to form a water-insoluble salt to achieve sustained release. However, this chemical salt bridge-based binding method lacks mechanical anti-peeling strength when facing the high-intensity physical stress of feed mechanical stirring. The process, which relies on static concentration matching, lacks real-time dynamic feedback on the microscopic response state of the material, making it difficult to ensure that the active components achieve deep embedding and stable retention in the micropores of the heterogeneous natural biomass carrier.
[0004] Therefore, the technical problem to be solved by this invention is how to achieve deep and dense physical integration between anionic salt particles and carrier micropores without damaging the integrity of the biomass carrier skeleton, and to establish a lasting physicochemical taste masking mechanism. Summary of the Invention
[0005] This invention provides a method for preparing a biological anionic salt preparation, comprising the following steps:
[0006] Step S1: Mix the wood fiber carrier and anionic salt particles in a mixing device and adjust the moisture content of the mixture; wherein, the wood fiber carrier has tracheid lumens and bound water is distributed on the inner wall of the tracheid lumens;
[0007] Step S2: Heat the mixture to maintain its temperature between 60°C and 90°C, so that the cellulose skeleton of the wood fiber carrier enters the plasticized state and the bound water is kept in a state of liquid accumulation pressure.
[0008] Step S3: Apply pulse pressure to the plasticized mixture through a pressure generating mechanism, control the pressurization rate of the pulse pressure to be between 10 MPa / s and 30 MPa / s, induce the bound water in the tracheid lumen to generate volume expansion stress, and use the volume expansion stress to drive the tracheid lumen inlet to generate radial strain.
[0009] Step S4: Under the pressure peak of the pulse pressure, the anionic salt particles are forced into the tracheid lumen.
[0010] Step S5 involves cooling the mixture while removing the pulse pressure, utilizing the solubility difference between the anionic salt particles and the lignocellulose carrier to precipitate crystals on the inner wall of the tracheid lumen, and accumulating the crystals at the tracheid lumen entrance to form a sealing layer.
[0011] Preferably, in step S3, the peak pressure of the pulse pressure is 20 MPa to 50 MPa; in step S4, the penetration depth of the anion salt particles into the tracheid lumen is 3 to 5 times the average pore size of the tracheid lumen.
[0012] Preferably, in step S1, the lignocellulose carrier is selected from at least one of corn cob, rice husk, wheat straw, and wood chips.
[0013] Preferably, in step S1, the anionic salt particles are selected from at least one of ammonium chloride, calcium chloride, magnesium chloride, ammonium sulfate, calcium sulfate, and magnesium sulfate.
[0014] Preferably, in step S3, the pressure generating mechanism dynamically adjusts the duty cycle of the pulse pressure according to the real-time acoustic impedance feedback signal of the mixed material. The duty cycle D of the pulse pressure satisfies the following relationship: D=k×(Z / Z0), where k is a proportionality constant, Z is the real-time acoustic impedance value of the mixed material obtained by the sensor, with the unit being Pa·s / m, and Z0 is the reference acoustic impedance value of the mixed material when it is in the initial stacking state, with the unit being Pa·s / m.
[0015] Preferably, in step S1, the ratio of the average particle size of the anionic salt particles to the average diameter of the tracheid inlet is 0.8 to 1.2.
[0016] Preferably, in step S5, the sealing layer includes a crystalline film formed by anionic salt particles during the cooling process, the crystalline film being bonded to the cellulose hydroxyl groups on the inner wall of the tracheid lumen via hydrogen bonds.
[0017] Preferably, in step S3, the driving current signal of the power unit in the pressure generating mechanism is acquired, the harmonic component characteristics of the driving current signal are extracted to identify the rheological state of the mixture, and the frequency of the pulse pressure is adjusted according to the rheological state. The pulse width of the rising edge of the pulse pressure is less than the elastic relaxation time of the fiber skeleton in the tracheid lumen, so that the tracheid lumen inlet produces instantaneous elastic expansion.
[0018] Preferably, in the biological anionic salt formulation, the mass percentage of anionic salt particles is 40% to 60%.
[0019] A biological anionic salt preparation, which is prepared by the method described above.
[0020] Compared with existing technologies, the preparation method of the biological anionic salt preparation of the present invention has the following advantages:
[0021] 1. In biological anionic salt formulations, by regulating the water activity of the biomass carrier, the fiber skeleton enters a transient plasticization stage. Combined with pulse pressure with a specific rising slope, the anionic salt particles are driven to overcome the bridging resistance at the tracheid lumen entrance and slide into the deeper layers. This structural transformation from external coating to endogenous physical embedding allows the anionic salt to achieve physical taste masking without relying on chemical coatings. While maintaining a high drug loading, it avoids the instantaneous dissolution of bitter components in the animal's oral cavity, eliminating the risk of refusal to eat due to palatability bias.
[0022] 2. By utilizing the transient dynamic response of bound water within the carrier excited by pulsed pressure, micron-level volume expansion stress is generated in the fiber wall, achieving dynamic expansion of the tracheid lumen inlet. This guides salt particles to penetrate along the fiber axis to a depth exceeding three times the average pore size of the tracheid lumen. Based on this, in conjunction with the synergistic effect of salt components with opposite heat of solution properties, a glassy crystalline film is induced during pressure removal and cooling, forming a sealing layer on the inner wall of the fiber. This mechanism physically blocks the water migration path, enhances the formulation's resistance to moisture absorption in high humidity environments, and ensures physical stability during storage.
[0023] 3. By collecting the harmonic component characteristics of the driving current of the power unit, the acoustic impedance feedback of the material bed to the pressure wave is analyzed in real time, and the duty cycle of the pulse pressure is dynamically adjusted accordingly. This closed-loop adjustment mechanism based on material state feedback enables adaptive matching between the processing energy output and the batch heterogeneity of the biomass carrier. While ensuring that materials from different sources can achieve deep embedding, it prevents the fiber skeleton from brittlely breaking due to local stress concentration, thus ensuring the structural stability of the product during subsequent processing and stirring. Attached Figure Description
[0024] Figure 1 This is a flow chart of the pulse pressure deep embedding preparation process of the biological anionic salt formulation of the present invention;
[0025] Figure 2 This is a logic control architecture diagram of the intelligent fabrication process system with acoustic impedance feedback closed-loop adjustment according to the present invention. Detailed Implementation
[0026] The technical solutions of the embodiments of this application will be clearly described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of this application, not all embodiments. All other embodiments obtained by those skilled in the art based on the embodiments of this application are within the scope of protection of this application.
[0027] It should be noted that all directional and positional terms used in this invention, such as: up, down, left, right, front, back, vertical, horizontal, inner, outer, top, bottom, transverse, longitudinal, center, etc., are only used to explain the relative positional relationship and connection between components in a specific state (as shown in the accompanying drawings). They are only for the convenience of describing this invention and do not require that this invention be constructed and operated in a specific orientation. Therefore, they should not be construed as limiting this invention. In addition, the descriptions of "first," "second," etc., in this invention are for descriptive purposes only and should not be construed as indicating or implying their relative importance or implicitly specifying the number of technical features indicated.
[0028] In the description of this invention, unless otherwise explicitly specified and limited, the terms installation, connection, and linking should be interpreted broadly. For example, they can refer to fixed connections, detachable connections, or integral connections; they can refer to mechanical connections; they can refer to direct connections or indirect connections through an intermediate medium; they can refer to the internal connection of two components. For those skilled in the art, the specific meaning of the above terms in this invention can be understood according to the specific circumstances.
[0029] In the description of this specification, references to the terms "an embodiment," "some embodiments," "illustrative embodiments," "examples," "specific examples," or "some examples," etc., indicate that a specific feature, structure, material, or characteristic described in connection with that embodiment or example is included in at least one embodiment or example of the present invention. In this specification, the illustrative expressions of the above terms do not necessarily refer to the same embodiment or example, and the specific features, structures, materials, or characteristics described may be combined in any suitable manner in one or more embodiments or examples.
[0030] This invention provides a biological anionic salt formulation and its preparation method. The feed processing technology is divided into a material conditioning stage, a preliminary coating stage, a deep embedding stage, and a structure locking stage. In the material conditioning stage, water activity regulation is used to achieve transient plasticization of the lignocellulose carrier. In the preliminary coating stage, differential shear force is used to achieve physical coverage of the anionic salt particles and the fiber layer. In the deep embedding stage, pulsed pressure is applied to drive the anionic salt particles into the tracheid lumen. In the structure locking stage, a sealing layer is generated through cooling and moisture removal procedures, thus constructing a sustained-release formulation with high drug loading and high physical stability. Composite System; For lignocellulose carriers with high lignification, whose tracheid inlets are in a contracted state under natural conditions, conventional high-pressure extrusion methods can cause irreversible collapse damage to the fiber skeleton. To address this challenge, this invention employs a material conditioning process, mixing at least one lignocellulose carrier selected from corn cobs, rice husks, wheat straw, or sawdust with at least one anionic salt particle selected from ammonium chloride, calcium chloride, magnesium chloride, ammonium sulfate, calcium sulfate, or magnesium sulfate in a mixing device. The moisture content is adjusted by adding atomized water to the mixture, thus increasing the material's water activity α. w The mixture is heated within the range of 0.65 to 0.85, maintaining the material temperature between 60°C and 90°C. The synergistic effect of temperature and moisture induces the cellulose skeleton of the lignocellulose carrier into a transient plasticized state, while maintaining the bound water distributed on the tracheid lumen wall in a state of liquid accumulation pressure. To ensure that the bound water distributed on the tracheid lumen wall of the lignocellulose carrier maintains a state of liquid accumulation pressure between 60°C and 90°C, the preparation process establishes a static equilibrium pressure within the range of 0.15 MPa to 0.35 MPa during heating via a pressure generating mechanism to counteract the saturated vapor pressure of moisture. This static equilibrium pressure prevents moisture from vaporizing before pulse pressurization by inhibiting the kinetic energy escape of liquid phase molecules inside the tracheid lumen. This allows the liquid medium inside the carrier to generate sufficient volume expansion stress to overcome the elastic resistance at the tracheid lumen inlet under the transient rising edge of the subsequent pulse pressure, thereby ensuring the generation of radial strain at the pore inlet.
[0031] During material flow in the plasticized state, hard salt particles are prone to bridging and blockage at the inlet when entering the microscale tracheid lumen. This invention employs a pulse excitation procedure, applying pulse pressure to the plasticized mixture through a pressure generating mechanism. The pulse pressure is controlled within the range of 10 MPa / s to 30 MPa / s, utilizing a specific upward slope to excite the dynamic response of bound water within the tracheid lumen, generating micron-level volumetric expansion stress. This stress is transmitted from the inside of the pores outward and counteracts the contraction tension of the fiber wall, driving periodic radial strain and elastic expansion at the tracheid lumen inlet. Under the pressure peak of the pulse pressure, anionic salt particles with an average particle size to tracheid lumen inlet average diameter ratio of 0.8 to 1.2 are forced into the tracheid lumen, causing them to micro-slip along the fiber axis. This achieves physical intercalation of anionic salt particles within the tracheid lumen to a depth of 3 to 5 times the average pore diameter. Due to batch-to-batch variations in lignification and porosity in natural biomass materials... Fluctuations and fixed processing parameters make it difficult to guarantee consistent embedding rates. To address this challenge, this invention employs an adaptive compensation procedure based on acoustic impedance feedback. During the application of pulse pressure, the power unit in the pressure generating mechanism acquires its driving current signal. By executing a fast Fourier transform algorithm, the harmonic component characteristics in the driving current signal are extracted to identify the rheological state of the material bed. The system calculates the real-time acoustic impedance value Z of the material and dynamically adjusts the duty cycle D of the pulse pressure according to the formula D=k×(Z / Z0), where D is the duty cycle of the pulse pressure; k is a proportionality constant; Z is the real-time acoustic impedance value of the mixture in Pa·s / m; and Z0 is the reference acoustic impedance value of the mixture in its initial stacking state in Pa·s / m. When the damping attenuation coefficient in the acoustic impedance signal exceeds a preset threshold, the system determines that the carrier pores are in a closed impedance state. At this time, the duty cycle D of the pulse pressure is automatically extended to overcome the elastic resistance at the tracheid inlet.
[0032] In step S3, the real-time drive current signal of the pressure generating mechanism's power unit is acquired by a sensor with a sampling frequency of no less than 1000Hz, and fast Fourier transform processing is performed to extract the sum of squares of the amplitudes of the 3rd and 5th harmonic components. The system opens a ring buffer with a length of 512 sampling points in the random access memory and stores the drive current signal data of the power unit in real time at a sampling frequency of 1000Hz. A fast Fourier transform calculation task is triggered every 256 sampling points, i.e., the overlap rate of the sampling window is 50%. Before the calculation, the original current sampling data in the buffer is weighted by a Hanning window to suppress spectral leakage. The amplitudes at frequency points near 150Hz and 250Hz are extracted, and their sum of squares is used as the real-time energy characteristic value for identifying the rheological state of the material. The weighted average of the sum of squares of the amplitudes is used as the real-time energy characteristic value for characterizing the material flow resistance. The real-time acoustic impedance value Z of the mixture is determined according to the pre-stored energy-impedance comparison data. When the density of the material bed fluctuates, the lignin heterogeneity is compensated by adjusting the pulse pressure duty cycle D. To reduce osmotic resistance, the embedding depth of anionic salt particles in different batches of carriers is maintained at 3 to 5 times the average pore size of the tracheid lumen. Z is the real-time acoustic impedance value of the mixture obtained by the sensor, in Pa·s / m. The proportionality constant k and the reference acoustic impedance value Z0 are determined by the formula D=k×(Z / Z0) as follows: A wood fiber carrier with a moisture content of 15% is selected, and a static preload of 1MPa is applied at a plasticizing temperature of 75℃. The initial driving current signal is collected, and the reference acoustic impedance value Z0 is determined by spectral analysis. The peak pulse pressure is also considered. Within the range of 20MPa to 50MPa, five sets of pulse pressure duty cycles D with gradient differences were set, and the average embedding depth of anion salt particles in the tracheid lumen was recorded under different duty cycles. The embedding depth and impedance ratio Z / Z0 were linearly fitted using the least squares method to determine the proportional constant k that makes the embedding depth reach the preset target. When the real-time acoustic impedance value Z deviates from the reference value Z0 by more than 5%, the duty cycle D is automatically corrected. k is the proportional constant, and Z0 is the reference acoustic impedance value of the mixture in the initial stacking state, with the unit being Pa·s / m.
[0033] To address the spatial segregation problem caused by differences in friction coefficients during the mixing of formulations in total mixed rations, this invention employs surface texturing in the initial coating stage. During the differential shearing process in the non-uniform diameter power unit, the actuator superimposes periodically varying lateral oscillating stress on top of the principal axial shear force, causing the frequency f of the oscillating stress to... swing With pulse pressure frequency f pulse Satisfy the ratio f swing / f pulseA mapping relationship of 0.3 to 0.5 is used to generate micron-scale spiral folds on the surface of the plasticized carrier using an asymmetric stress field, forming a non-smooth frictional surface. This texture increases the physical interlocking force between the formulation particles and the roughage, ensuring that they maintain a synchronized motion trajectory with the bulk materials during mixing and eliminating spatial segregation. In the initial coating stage, a resonant field is generated by controlling the axial shear force and lateral oscillation stress of the actuator, with the lateral oscillation stress frequency f... swing Set as pulse pressure frequency f pulse The dynamic friction coefficient μ of the formulation particles is increased to the target value by 0.3 to 0.5 times. This is achieved by utilizing an asymmetric stress field to generate a spiral fold texture with a depth of 15 μm to 25 μm on the surface of the plasticized carrier. This increases the surface friction area of the formulation particles, enhances the physical meshing force with roughage, and increases the dynamic friction coefficient μ of the formulation particles to the target value during the stirring cycle. Under mechanical collision conditions, this maintains the synchronous movement trajectory of the formulation and bulk materials, eliminating spatial segregation. swing The frequency of the oscillation stress is expressed in Hz, f. pulse is the pulse pressure frequency, in Hz, and μ is the coefficient of kinetic friction.
[0034] To limit the mass percentage of anionic salt particles in the formulation to 40% to 60%, the system executes a loading calculation procedure based on carrier volume constraints, by measuring the total pore volume V of the tracheid lumen of the lignocellulose carrier. total The addition limit M is determined by the true density ρ of the anionic salt particles. limit Control the actual added mass of anionic salt particles to not exceed the addition limit value M. limit This method achieves 90% accuracy, avoiding the arching effect caused by space congestion at the tracheid inlet of anionic salt particles. It ensures that anionic salt particles can smoothly slide along the fiber axis and embed into the tracheid lumen to a predetermined depth under the drive of the pulse pressure peak. After deep embedding, to suppress the deliquescence caused by the migration of anionic salts to the surface under high osmotic pressure, this invention implements a crystallization anchoring procedure. While removing the pulse pressure, the mixture is cooled. Utilizing the solubility difference generated during rapid water loss and cooling, the salts inside the tracheid lumen and at the inlet undergo transient dissolution and recrystallization, forming a glassy crystalline film tightly adhering to the fiber wall. This crystalline film binds to the cellulose hydroxyl groups on the tracheid lumen inner wall through hydrogen bonds, accumulating at the tracheid inlet to form a physical sealing layer. This sealing layer blocks the water migration path, transforming the water permeation path into a labyrinthine flow, reshaping the anionic salt release kinetics, and achieving stable dissolution of the active component in the rumen environment.
[0035] Example 1: In peripartum dairy cow feeding conditions with an ambient humidity of 85% and accompanying mechanical mixing stress, corn cob particles, with a particle size ranging from 1.0 mm to 2.0 mm, were used as a lignocellulose carrier and mixed with anionic salt particles composed of ammonium chloride in a stirring device. The moisture content of the mixture was adjusted by adding atomized water to increase the water activity α of the material. w To reach a strength of 0.78, the mixture is placed in a pressure vessel and heated to 75°C. The synergistic effect of temperature and moisture causes the cellulose skeleton of the corn cob particles to be in a plasticized state. At this time, the bound water distributed on the inner wall of the tracheid lumen is in a state of liquid accumulation pressure, providing a physical prerequisite for the subsequent dynamic expansion of the channels. For different batches of lignocellulose carriers, the elastic relaxation time of the fiber skeleton in the tracheid lumen is obtained through no-load testing of the production line. The specific method is as follows: at a plasticization temperature of 75°C, a single step pressure command with an amplitude of 5 MPa and a pulse width of 100 ms is applied to the carrier material. The pressure decay curve on the surface of the material is monitored in real time using a sensor. The time required for the pressure value to drop from the peak value to 10% of the reference value is defined as the elastic relaxation time. In this embodiment, based on the material hardness feedback, this time is measured to be in the range of 12 ms to 18 ms.
[0036] Deep embedding is performed under the above conditions. A pulse pressure with a pressurization rate of 20 MPa / s is applied to the mixture through a pressure generating mechanism. During the rising edge of the pulse pressure, the bound water in the tracheid cavity is excited by the transient pressure, generating micron-level volume expansion stress. This stress is transmitted from the inside of the channel outward and counteracts the contraction tension of the fiber wall, causing radial strain at the tracheid cavity inlet. At this time, anionic salt particles with an average particle size of 150 μm are forced into the tracheid cavity with a depth of 600 μm under the pressure peak. During this period, the system monitors the acoustic impedance value Z in real time and adjusts the duty cycle D of the pulse pressure according to the formula D=k×(Z / Z0), where D is the duty cycle of the pulse pressure; k is a proportionality constant; and Z is the real-time acoustic impedance value of the mixture, which is 1.2×10 in this embodiment. 6 Pa·s / m; Z0 is the reference acoustic impedance value when the mixture is in the initial stacking state; when the real-time acoustic impedance value Z is detected to deviate, the system adjusts the duty cycle D of the pulse pressure to 45% and uses this closed-loop feedback mechanism to compensate for the penetration resistance caused by the lignification heterogeneity of the carrier, so that the anionic salt particles can achieve physical integration in the deep layer of the fiber skeleton.
[0037] After deep embedding, structural locking is performed, and the flash valve is quickly opened to reduce the system pressure to atmospheric pressure within 5 seconds. The sudden drop in moisture induces supersaturated crystallization of salt at the tracheid inlet, forming a glassy crystalline film with a thickness of 5μm to 10μm on the inner wall of the tracheid lumen. This crystalline film binds to cellulose hydroxyl groups through hydrogen bonds and forms a physical sealing layer at the pore opening. During the mechanical stirring process of the resulting formulation with a total mixed diet (TMR) with a moisture content of 55% for 30 minutes, the dissolution rate of its anionic salts is less than 2% / min. The active components are retained in the tracheid lumen, reducing the exposure of anionic salts in the oral environment. This keeps the actual feed intake of dairy cows at a stable level compared to the control group, achieving physical stability of the formulation under high humidity processing conditions.
[0038] Example 2: A physical testing platform simulating the intensity gradient of feed processing was constructed to verify the structural stability and component retention capacity of bio-based anionic salt formulations under different mechanical stress levels. This physical testing platform included a horizontal twin-shaft impeller mixer with an effective volume of 50L, whose stirring speed could be adjusted from 15rpm to 75rpm. The experimental data acquisition system integrated a high-precision conductivity sensor and a particle strength analyzer. The conductivity sensor's sampling frequency was set to 10Hz, with a measurement resolution better than 0.01mS / cm, used to characterize the dissolution rate of the anionic salt in the simulated liquid phase in real time. In the parameter decision logic, the stirring speed setting depended on the balance between mechanical friction intensity and processing efficiency. 30rpm, 45rpm, and 60rpm were selected as low, medium, and high physical stress levels, respectively. The pressure application rate of the pulse pressure was set, along with the generation rate of volumetric expansion stress and the fiber wall stress limit. When the pressure application rate was 20MPa / s, the kinetic response speed of the bound water inside the material was sufficient to generate the radial strain required to open the tracheid inlet.
[0039] To simulate the high humidity environment of a pasture and introduce engineering disturbances, an ultrasonic humidification device was used to maintain a relative humidity of 85% in the mixing chamber, and ±3% humidity noise was introduced. Four groups were set up for the experiment. The sample group of this invention adopted the complete preparation process, namely material conditioning, preliminary coating, deep embedding, and structural locking. Control group A lacked the pulse pressure step and used an atmospheric pressure mixing method. Control group B had a set water activity a. w The value was 0.92, exceeding the upper limit of 0.85. The control group C was set with a pressurization rate of 5 MPa / s, which was lower than the lower limit of 10 MPa / s. The anion salt dissolution rate and particle surface wear depth of each sample group were tested after a stirring cycle of 30 min. The specific data are shown in Table 1.
[0040] Table 1: Performance Comparison Data under Different Stress Gradients
[0041]
[0042] Analysis of the data in Table 1 shows that the dissolution rate of the sample group of this invention increases gradually with increasing mechanical stress. When the rotation speed increases from 30 rpm to 60 rpm, the dissolution rate increases from 12.4% to 24.3%, indicating that the active component is located inside the tracheid lumen rather than on the carrier surface, reducing the loss caused by external mechanical friction. The dissolution rate of control group A reaches 92.5% under moderate stress, confirming that the lack of pulse pressure rising edge excitation prevents the tracheid lumen inlet from expanding, making it difficult for anionic salt particles to achieve physical intercalation. Regarding the performance inflection point at the parameter boundary, control group B, due to water activity exceeding the 0.85 range, excessive plasticization causes the fiber skeleton to undergo radial compression closure under pressure, resulting in an embedding depth of only 215.3 μm. The dissolution rate is 55.6% higher than that of the sample group of this invention. Control group C, due to the pressurization rate being below the lower limit of 10 MPa / s, cannot induce sufficient volume expansion stress in the bound water, and the embedding efficiency shows a non-linear decrease. In the sample group of this invention, the real-time acoustic impedance value Z monitored by the system is 1.18 × 10⁻⁶. 6 The pulse pressure duty cycle D was adjusted to 45% according to the formula D=k×(Z / Z0), where: D is the pulse pressure duty cycle; k is a proportionality constant; Z is the real-time acoustic impedance value of the mixture, in Pa·s / m; and Z0 is the reference acoustic impedance value of the material in its initial stacking state, in Pa·s / m. This feedback mechanism compensates for the heterogeneity resistance of the biomass carrier, enabling the anionic salt particles to achieve a stable distribution in the deep tracheid lumen. The experimental results confirm that the formulation based on the tracheid lumen embedding mechanism has extremely high physical stability. The measured thickness of the glassy crystalline film formed during the structural locking stage is 7.6 μm. This sealing layer is locked to the inner wall of the fiber through hydrogen bonds, blocking the water penetration path. The formulation maintains a drug loading stability of 40% to 60% during the mixing of the total mixed ration. The anionic salt is retained deep in the fiber skeleton, reducing the instantaneous release during animal chewing and maintaining the actual feed intake of dairy cows.
[0043] Example 3: This example combines Figures 1 to 2 A description of a biological anionic salt preparation and its preparation method, such as... Figure 1As shown, step S1 involves mixing a lignocellulosic carrier with tracheid lumens and bound water on its inner wall with anionic salt particles in a stirring device, and adjusting the moisture content of the mixture. Step S2 involves heating the mixture and maintaining the temperature between 60°C and 90°C, causing the cellulose skeleton of the lignocellulosic carrier to enter a plasticized state, and maintaining the bound water in a liquid accumulation pressure state. Based on this physical state, step S3 involves applying a pulse pressure with a pressurization rate of 10 MPa / s to 30 MPa / s, inducing volume expansion stress in the bound water, and driving radial strain at the tracheidulosic lumen inlet. Step S4 is then performed, where the anionic salt particles are forced into the tracheidulosic lumen under the pressure peak of the pulse pressure. Finally, step S5 involves removing the pulse pressure and simultaneously cooling the mixture, utilizing the difference in solubility to precipitate crystals on the inner wall of the tracheidulosic lumen and accumulate at the tracheidulosic lumen inlet to form a sealing layer.
[0044] like Figure 2 As shown, the architecture is centered on an intelligent process control hub, which internally runs acoustic impedance characteristic analysis, rheological state identification, and closed-loop decision-making algorithms. This hub is connected to the raw material conditioning station and controls the atomization, heating actuators, and temperature and humidity sensors by sending temperature and humidity setting signals. In the pulse embedding master station stage, the high-frequency pulse generator, impedance monitoring probe, and lateral swing mechanism work together to transmit signals to the intelligent process control hub through a real-time impedance feedback channel and receive duty cycle commands issued by the hub. At the same time, the intelligent process control hub communicates with the structure locking station and controls the operation of the flash evaporation pressure relief valve group and the rapid cooling module by sending pressure relief timing commands.
[0045] Example 4: To address the acoustic impedance fluctuations in corn cob particles caused by differences in lignification levels, a proportionality constant is applied. The calibration procedure establishes the adjustment reference for the duty cycle D of the pulse pressure; the initial state is defined, corn cob particles with a moisture content of 15% are selected, and the driving current signal of the initial stacking state is collected using the pressure generating mechanism at a plasticizing temperature of 75℃, and the reference acoustic impedance value Z0 is determined to be 0.98×10. 6 Pa·s / m; Set the duty cycle D of the gradient-increasing pulse pressure, record the average embedding depth of anion salt particles in the tracheid lumen under different duty cycles, and perform linear fitting of the embedding depth and impedance ratio using the least squares method to determine the proportional constant k as 0.52; In the underlying algorithm logic of the controller, this proportional constant k corresponds to a discrete mapping table of 10 sets stored in memory, whose input variable is the ratio of the real-time acoustic impedance value to the reference acoustic impedance value, and the lookup step accuracy is 0.05; When the ratio is in the range of 1.15 to 1.20, the corresponding proportional constant k is increased by 0.03 on the basis of the reference value of 0.52; If the real-time ratio fluctuates by more than 20%, the safety limiting logic is automatically triggered to fix the output pulse pressure duty cycle D at 60%.
[0046] An acoustic impedance feedback mechanism is employed to perform adaptive compensation in the production process. The real-time acoustic impedance value Z is subjected to moving average filtering, with a moving average time window length set to 500ms. The system utilizes a deviation threshold T to determine the deviation. z Monitor the material status. When the real-time acoustic impedance value Z and the reference acoustic impedance value Z0 satisfy the relationship |(Z-Z0) / Z0|>T z Time-triggered adjustment, in this embodiment, T is set z The value was 0.05; in one operating condition, the real-time acoustic impedance value Z was monitored to rise to 1.15 × 10⁻⁵. 6 Pa·s / m, since the deviation is 17.3% at this point and exceeds the threshold T z The system adjusts the duty cycle D of the pulse pressure from 40% to 61% according to the formula D=k×(Z / Z0), where: D is the duty cycle of the pulse pressure; k is a proportionality constant, which is 0.52 in this embodiment; Z is the real-time acoustic impedance value of the mixture, in Pa·s / m; and Z0 is the reference acoustic impedance value of the material in its initial stacking state, in Pa·s / m. After deep embedding, the opening degree of the flash valve is adjusted to control the cooling rate R. The system pressure is reduced to atmospheric pressure within 5s by depressurization flash evaporation. Utilizing the inverse proportional relationship between the cooling rate R and the thickness h of the glassy crystalline film, the cooling rate R is controlled to be in the range of 5℃ / s to 8℃ / s, generating a sealing layer with a thickness of 8.2μm at the tracheid inlet. This process ensures that different batches of lignocellulose carriers achieve a consistent anion salt retention rate, and that the instantaneous release of anion salts in the formulation decreases by no less than 65% in the simulated ruminant chewing and squeezing test.
[0047] Example 5: In situations involving batch switching of wood fiber carriers and fluctuations in the physical characteristics of raw materials, the system performs standardized pre-calibration to establish a monitoring reference benchmark; defining the initial state, the wood fiber carrier to be processed is placed under the pressure head of the pressure generating mechanism, and a small signal pulse excitation with an amplitude of 1MPa is applied at a plasticizing temperature of 75℃; the power unit collects the response current signal and calculates it according to formula Z. base =V / (I⋅S), the calculated value is stored in the controller's memory as the reference variable Z0 for the adaptive compensation logic; where Z... base The intrinsic acoustic impedance is the reference value, in Pa·s / m; V is the excitation voltage signal; I is the response current signal; and S is the indenter contact area. This calibration procedure establishes the initial impedance characteristics of raw materials from different sources.
[0048] In the debugging process of adapting surface texture parameters for specific ruminant feed component formulations, the system determines the oscillation frequency ratio by monitoring the lateral feedback stress of the actuator during kneading; within the ratio range of 0.3 to 0.5, a step test is performed, recording the dynamic friction coefficient μ and spatial segregation index σ of the resulting formulation particles during the mixing process of the total mixed ration; the system selects a value that minimizes the segregation index σ and satisfies the target dynamic friction coefficient μ. target The required frequency mapping point is taken as the operating point; at this operating point, the frequency f of the oscillation stress... swing With pulse pressure frequency f pulse The resulting resonant field generates a spiral fold texture on the plasticized carrier surface with preset spatial meshing geometry, keeping the deviation of the movement trajectory between the formulation particles and the diet matrix within a preset process threshold.
[0049] Example 6: In a production deployment where wheat straw pellets are used as the lignocellulose carrier and their physical hardness characteristics fluctuate from batch to batch, the system executes an amplitude sweep frequency program to determine the lateral oscillation stress amplitude of the actuator during kneading; wheat straw pellets in a plasticized state are selected as calibration samples, and the actuator is controlled to perform a step sweep frequency within a frequency ratio range of 0.3 to 0.5. The depth H of the spiral wrinkles on the carrier surface is recorded in real time using a displacement sensor. tex ; where H tex The spiral fold depth is expressed in μm. The system analyzes the surface texture characteristics under different oscillating stresses to select the spiral fold depth H. tex The stress value that is stable in the range of 15μm to 25μm and has no crack damage to the carrier skeleton is used as the working amplitude, and the quantitative correlation between the processing stress field and the physical interlocking force between particles is established.
[0050] When the system is in offline optimization mode for calibrating the crystal anchoring thickness of anionic salt components with different solubility characteristics, the system performs a gradient experiment of cooling rate R by adjusting the opening speed of the flash valve. During this period, the system uses an infrared thermal imaging sensor to collect temperature drop data of the material surface and determines the corresponding glassy crystalline film thickness h by combining the results of electronic characterization. Here, R is the cooling rate in °C / s, and h is the glassy crystalline film thickness in μm. The system fits the cooling rate R and cooling time t based on measured data under different ambient humidity conditions. cool The characteristic relationship; where t cool The cooling time is expressed in seconds. This procedure ensures that the thickness deviation of the sealing layer generated at the tracheid inlet is controlled within 0.5 μm within the transient window after pressure removal, so that the anion salt protection rate of the formulation is maintained above 98% under the simulated total mixed diet stirring environment.
[0051] The embodiments of this application have been described above with reference to the accompanying drawings. Unless otherwise specified, the embodiments and features in the embodiments of this application can be combined with each other. This application is not limited to the specific embodiments described above. The specific embodiments described above are merely illustrative and not restrictive. Those skilled in the art can make many other forms under the guidance of this application without departing from the spirit of this application and the scope of protection of this invention, and all of these forms are within the protection scope of this application.
Claims
1. A method for preparing a biological anionic salt preparation, characterized in that, Includes the following steps: Step S1: Mix the wood fiber carrier and anionic salt particles in a mixing device and adjust the moisture content of the mixture; wherein, the wood fiber carrier has tracheid lumens and bound water is distributed on the inner wall of the tracheid lumens; Step S2: Heat the mixture to maintain its temperature between 60°C and 90°C, so that the cellulose skeleton of the wood fiber carrier enters the plasticized state and the bound water is kept in a state of liquid accumulation pressure. Step S3: Apply pulse pressure to the plasticized mixture through a pressure generating mechanism, control the pressurization rate of the pulse pressure to be between 10 MPa / s and 30 MPa / s, induce the bound water in the tracheid lumen to generate volume expansion stress, and use the volume expansion stress to drive the tracheid lumen inlet to generate radial strain. Step S4: Under the pressure peak of the pulse pressure, the anionic salt particles are forced into the tracheid lumen. Step S5 involves cooling the mixture while removing the pulse pressure, utilizing the solubility difference between the anionic salt particles and the lignocellulose carrier to precipitate crystals on the inner wall of the tracheid lumen, and accumulating the crystals at the tracheid lumen entrance to form a sealing layer.
2. The method for preparing a biological anionic salt preparation according to claim 1, characterized in that, In step S3, the peak pressure of the pulse pressure is 20 MPa to 50 MPa; in step S4, the penetration depth of the anion salt particles into the tracheid lumen is 3 to 5 times the average pore size of the tracheid lumen.
3. The method for preparing a biological anionic salt preparation according to claim 1, characterized in that, In step S1, the lignocellulose carrier is selected from at least one of corn cob, rice husk, wheat straw, and wood chips.
4. The method for preparing a biological anionic salt preparation according to claim 1, characterized in that, In step S1, the anionic salt particles are selected from at least one of ammonium chloride, calcium chloride, magnesium chloride, ammonium sulfate, calcium sulfate, and magnesium sulfate.
5. The method for preparing a biological anionic salt preparation according to claim 1, characterized in that, In step S3, the pressure generating mechanism dynamically adjusts the duty cycle of the pulse pressure based on the real-time acoustic impedance feedback signal of the mixed material. The duty cycle D of the pulse pressure satisfies the following relationship: D=k×(Z / Z0), where k is a proportionality constant, Z is the real-time acoustic impedance value of the mixed material obtained by the sensor, with the unit being Pa·s / m, and Z0 is the reference acoustic impedance value of the mixed material when it is in the initial stacking state, with the unit being Pa·s / m.
6. The method for preparing a biological anionic salt preparation according to claim 1, characterized in that, In step S1, the ratio of the average particle size of the anionic salt particles to the average diameter of the tracheid inlet is 0.8 to 1.
2.
7. The method for preparing a biological anionic salt preparation according to claim 1, characterized in that, In step S5, the sealing layer includes a crystalline film formed by anionic salt particles during the cooling process, the crystalline film being bonded to the cellulose hydroxyl groups on the inner wall of the tracheid lumen via hydrogen bonds.
8. The method for preparing a biological anionic salt preparation according to claim 1, characterized in that, In step S3, the driving current signal of the power unit in the pressure generating mechanism is acquired, the harmonic component characteristics of the driving current signal are extracted to identify the rheological state of the mixture, and the frequency of the pulse pressure is adjusted according to the rheological state. The pulse width of the rising edge of the pulse pressure is less than the elastic relaxation time of the fiber skeleton in the tracheid lumen, so that the tracheid lumen inlet produces instantaneous elastic expansion.
9. The method for preparing a biological anionic salt preparation according to claim 1, characterized in that, In biological anionic salt preparations, the mass percentage of anionic salt particles is 40% to 60%.
10. A biological anionic salt preparation, characterized in that, The biological anionic salt preparation is prepared by the method described in claim 1.