Natural material emulsification process in washing and caring product processing

Abstract

This invention relates to the field of natural material emulsification and discloses a natural material emulsification process for processing personal care products. The process includes: injecting a dispersed aqueous phase of tea saponin and soybean lecithin into the oil phase at a gradually decreasing pump flow rate at a temperature ranging from 30°C to 42°C, while simultaneously increasing the stirring speed; applying an ultrasonic pulse after the oil phase injection is complete; lowering the stirring speed to stabilize the interfacial film; and reducing the temperature in two stages. This invention matches the interfacial expansion rate with the molecular adsorption rate to eliminate localized oil phase overload, resulting in a uniform monodisperse state of the droplets. Simultaneously, it avoids the peeling and damage of the interfacial film by continuous strong shear fields, locks the lattice arrangement of hydrophobic hydrocarbon segments in the interfacial film, and forms a three-dimensional steric network, thereby increasing the interfacial yield stress, enhancing long-term thermodynamic stability, and suppressing stratification and phase coalescence during long-term storage.

Description

Technical Field

[0001] This invention belongs to the field of natural material emulsification technology, and particularly relates to a natural material emulsification process in the processing of personal care products. Background Technology

[0002] Currently, using natural materials to replace synthetic surfactants to meet the demand for low skin irritation is a mainstream technological trend. Conventional emulsification preparation processes typically disperse solid tea saponin powder and refined soybean lecithin powder in deionized water, and form a continuous aqueous phase substrate by stirring and breaking it up. Oil phase materials are then injected into the reactor at a constant flow rate, and the oil phase is dispersed by a constant-speed, continuous high-shear mechanical stirring method using a dispersion shaft.

[0003] However, these amphiphilic macromolecules, mainly composed of natural saponins and natural phospholipids, possess strong nonlinear surface activity dissipation characteristics. The rate of proton mass transfer adsorption and film formation at the oil-water interface lags significantly behind the instantaneous expansion rate of the oil phase droplet surface area caused by mechanical shear. When the flow field inside the emulsification reactor maintains a high shear energy input, the high mechanical shear stress generated by the rotation of the dispersion shaft blades directly causes physical peeling and surface tearing of the naturally enriched and migrating macromolecular liquid crystal film. This leads to frequent collisions of the phase boundary droplets in the high-frequency motion of the flow field and transient phase merging due to the damage to the surface protective film. In order to improve the dispersion effect, the conventional improvement path of simply increasing the concentration of natural materials or extending the high-shear mixing time often easily triggers local thermal denaturation of macromolecular protein components. In some cases, excessive shearing of the multiphase emulsion system can even cause abnormal transitions in the overall apparent viscosity of the fluid, thereby aggravating oil-water separation. Such linear control methods cannot solve the inherent physical orientation conflict between the demand for highly dispersed droplet generation and the inability of the natural molecular emulsion film to withstand continuous strong shear damage.

[0004] Therefore, the technical problem to be solved by this invention is how to adapt the viscosity changes of the material system by dynamically adjusting the input flow sequence of the oil phase pumping system, and by combining the stepwise retreat of the multi-level mechanical energy field to provide a conformational reforming window free from shear interference, so that the emulsifier molecules can solidify into a three-dimensional steric grid through isotropic lateral recombination. Summary of the Invention

[0005] This invention aims to solve the problems of continuous oil phase injection overload and sustained high shear stress damaging the molecular interface film assembly of natural emulsifiers.

[0006] In this technical solution, a natural material emulsification process in the processing of personal care products includes the following steps:

[0007] Step S101: Under the temperature conditions of 30℃ to 42℃, the material flow containing the oil phase is injected into the dispersed aqueous phase containing tea saponin and soybean lecithin at a pumping flow rate that decreases hourly. At the same time, the speed of the stirring system is continuously increased at a speed rate of 15 rpm / min to 35 rpm / min to form a dispersion flow field inside the dispersed aqueous phase in which the oil-water phase interface expansion rate matches the adsorption rate of natural material molecules.

[0008] Step S102: Apply an ultrasonic pulse with a duration of 3s to 8s and a power of 1200W to 1800W to the oil-water mixture system in the dispersed flow field to break up the droplets. After the ultrasonic pulse stops, adjust the speed of the stirring system to be reduced by 40% to 60% instantly to generate a dynamic yielding action, and control the tea saponin and soybean lecithin to arrange on the surface of the oil droplets to form a transversely reorganized phase interface film.

[0009] Step S103: Maintain the reduced rotation speed and continuously stir the oil-water mixture system at a low speed, and control the oil-water mixture system to cool down in two stages. In the first stage, control the cooling rate to 0.6℃ / min to 1.2℃ / min to cool down to 30℃ to release the residual shear stress in the oil-water mixture system. In the second stage, control the cooling rate to 0.2℃ / min to 0.5℃ / min to continue cooling down to 22℃ to lock the lattice arrangement of hydrophobic hydrocarbon segments in the phase interface film and form a three-dimensional steric network.

[0010] Preferably, in step S101, the initial value of the pumping flow rate that decreases hourly is 40 mL / min to 60 mL / min, the initial speed of the stirring system is 200 rpm to 300 rpm, and the speed after adjustment is 800 rpm to 1200 rpm.

[0011] Preferably, based on the total weight of the system (100%), tea saponin comprises 1.5% to 3.5%, soybean lecithin comprises 2.0% to 5.0%, oil phase comprises 15% to 35%, the dispersed aqueous phase contains 0.5% to 1.5% hydrolyzed wheat protein, and the remainder is water.

[0012] Preferably, in step S101, dynamic torque data is collected by an online torque sensor. When the rate of change of the dynamic torque data over time exceeds the critical threshold of 0.8 N·m / s, the control unit reduces the cooling rate of the first stage and extends the low-speed stirring time in step S103.

[0013] Preferably, step S102 includes the following sub-steps: step S1021, applying an ultrasonic pulse of 20 kHz to 28 kHz to the oil-water mixture system; step S1022, controlling the rotation speed of the stirring system to be reduced to 200 rpm to 400 rpm within 0.5 s to 1.2 s.

[0014] Preferably, in step S103, step S1031 involves cooling the oil-water mixture system to 30°C at a rate of 0.6°C / min to 1.2°C / min; and step S1032 involves cooling the oil-water mixture system to 22°C at a rate of 0.2°C / min to 0.5°C / min.

[0015] Preferably, in step S101, the total time for injecting the material flow containing the oil phase is controlled to be 30 min to 50 min, and the pumping flow rate is gradually reduced from 50 mL / min to 10 mL / min; at the same time, the rotation speed of the stirring system is gradually increased from 200 rpm to 1000 rpm.

[0016] Preferably, the process also includes step S104, whereby after the temperature of the oil-water mixture system drops to 22°C and is kept at a constant temperature for 10 to 15 minutes, the stirring system is stopped and the material is discharged to obtain the final washing and care lotion product.

[0017] Preferably, in step S105, the phase separation thickness data of the final shampoo and conditioner lotion product after being placed at 40°C for 180 days is recorded; in step S106, the separation rate is determined based on the data; in step S107, when the separation rate is less than 0.01 mm / d, the product is determined to meet the factory standard.

[0018] Compared with existing technologies, the natural material emulsification process for processing personal care products according to this invention has the following advantages:

[0019] 1. In the processing of washing and care products, solid tea saponin powder and refined soybean lecithin powder are fully swollen and assembled into a layered liquid crystal precursor by stirring and shearing in deionized water. This precursor provides a continuous phase substrate required for the injection of the oil phase. During the continuous injection of the oil phase material, the instantaneous flow rate is controlled to decrease logarithmically over time, making it inversely correlated with the change in system viscosity. This decreasing flow rate sequence limits the oil phase input rate and makes it spatially and temporally matched with the migration rate of emulsifier molecules to the newly formed phase interface. This eliminates the local oil phase overload caused by oil injection in the reactor, synchronizes the growth rate of droplet fragmentation area with the enrichment rate of molecular interface, and makes the internal phase droplets present a uniform monodisperse state and converge the particle size within a narrow range.

[0020] 2. When the oil phase is fully injected, the control system causes the stirring speed to jump to a pulsed high-shear speed in a short time. The sudden strong shear energy field provides the energy required to cross the surface energy barrier of the droplet, driving the spatial chain segments of tea saponin and the polar ends of soybean lecithin at the phase interface to spontaneously align isotropically. This forms a monomolecular protective layer through in-situ lateral cross-linking on the droplet surface. At the end of the pulse sequence, the stirring rate is suddenly reduced to a low-speed shear state. The kinetic energy cutoff eliminates the mechanical peeling and surface tearing damage of the formed natural emulsion film caused by the continuous strong stress field. This provides an undisturbed conformational reorganization time window for the natural macromolecules with adsorption lag, allowing the emulsifier molecules to spontaneously complete isotropic lateral reorganization under low interfacial tension. Based on the high intrinsic resistance to deformation of the emulsion product, no oil phase precipitation is maintained under centrifugal stress.

[0021] 3. After the emulsified system under low-speed stirring is introduced into the cooling channel, the temperature control system with discrete cooling jacket guides the material into a two-stage discrete gradient cooling process. In the first stage, the material is slowly cooled at a low cooling slope to release the residual shear stress accumulated in the continuous phase fluid by the high-energy flow field, block the outward diffusion of anisotropic defects and maintain the structural integrity of the phase interface. In the second stage, the cooling rate is further reduced to drive the hydrophobic hydrocarbon segments of the emulsifier to generate lattice-ordered arrangement and solidify the three-dimensional steric network through temperature field gradient cooling shock. This transforms the system from a non-equilibrium metastable state to a long-term thermodynamically stable state, firmly confining the internal phase droplets within the three-dimensional topological framework and blocking phase merging during aging and storage, thereby suppressing apparent stratification and wall adhesion failure during long-term storage. Attached Figure Description

[0022] Figure 1 This is a flowchart of the natural material emulsification process of this invention;

[0023] Figure 2 This is a structural diagram of the natural material emulsification system of the present invention. Detailed Implementation

[0024] 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.

[0025] An emulsification process for natural materials in the processing of personal care products includes the following steps:

[0026] Step S101: Under the temperature conditions of 30℃ to 42℃, the material flow containing the oil phase is injected into the dispersed aqueous phase containing tea saponin and soybean lecithin at a pumping flow rate that decreases hourly. At the same time, the speed of the stirring system is continuously increased at a speed rate of 15 rpm / min to 35 rpm / min to form a dispersion flow field inside the dispersed aqueous phase in which the oil-water phase interface expansion rate matches the adsorption rate of natural material molecules.

[0027] Step S102: Apply an ultrasonic pulse with a duration of 3s to 8s and a power of 1200W to 1800W to the oil-water mixture system in the dispersed flow field to break up the droplets. After the ultrasonic pulse stops, adjust the speed of the stirring system to be reduced by 40% to 60% instantly to generate a dynamic yielding action, and control the tea saponin and soybean lecithin to arrange on the surface of the oil droplets to form a transversely reorganized phase interface film.

[0028] Step S103: Maintain the reduced rotation speed and continuously stir the oil-water mixture system at a low speed, and control the oil-water mixture system to cool down in two stages. In the first stage, control the cooling rate to 0.6℃ / min to 1.2℃ / min to cool down to 30℃ to release the residual shear stress in the oil-water mixture system. In the second stage, control the cooling rate to 0.2℃ / min to 0.5℃ / min to continue cooling down to 22℃ to lock the lattice arrangement of hydrophobic hydrocarbon segments in the phase interface film and form a three-dimensional steric network.

[0029] Preferably, in step S101, the initial value of the pumping flow rate that decreases hourly is 40 mL / min to 60 mL / min, the initial speed of the stirring system is 200 rpm to 300 rpm, and the speed after adjustment is 800 rpm to 1200 rpm.

[0030] Preferably, based on the total weight of the system (100%), tea saponin comprises 1.5% to 3.5%, soybean lecithin comprises 2.0% to 5.0%, oil phase comprises 15% to 35%, the dispersed aqueous phase contains 0.5% to 1.5% hydrolyzed wheat protein, and the remainder is water.

[0031] Preferably, in step S101, dynamic torque data is collected by an online torque sensor. When the rate of change of the dynamic torque data over time exceeds the critical threshold of 0.8 N·m / s, the control unit reduces the cooling rate of the first stage and extends the low-speed stirring time in step S103.

[0032] Preferably, step S102 includes the following sub-steps: step S1021, applying an ultrasonic pulse of 20 kHz to 28 kHz to the oil-water mixture system; step S1022, controlling the rotation speed of the stirring system to be reduced to 200 rpm to 400 rpm within 0.5 s to 1.2 s.

[0033] Preferably, in step S103, step S1031 involves cooling the oil-water mixture system to 30°C at a rate of 0.6°C / min to 1.2°C / min; and step S1032 involves cooling the oil-water mixture system to 22°C at a rate of 0.2°C / min to 0.5°C / min.

[0034] Preferably, in step S101, the total time for injecting the material flow containing the oil phase is controlled to be 30 min to 50 min, and the pumping flow rate is gradually reduced from 50 mL / min to 10 mL / min; at the same time, the rotation speed of the stirring system is gradually increased from 200 rpm to 1000 rpm.

[0035] Preferably, the process also includes step S104, whereby after the temperature of the oil-water mixture system drops to 22°C and is kept at a constant temperature for 10 to 15 minutes, the stirring system is stopped and the material is discharged to obtain the final washing and care lotion product.

[0036] Preferably, in step S105, the phase separation thickness data of the final shampoo and conditioner lotion product after being placed at 40°C for 180 days is recorded; in step S106, the separation rate is determined based on the data; in step S107, when the separation rate is less than 0.01 mm / d, the product is determined to meet the factory standard.

[0037] Example 1: In a continuously operating large-capacity shampoo and conditioner product processing line, when the system constructs a pure natural emulsion system using soybean lecithin and tea saponin components under low shear temperature boundary conditions of 30°C, due to the inherent low interfacial tension repair rate and high phase sensitivity of natural macromolecules, the continuous phase flow field is prone to local phase enrichment and in-situ mechanical peeling and damage of the interfacial film when a high proportion of oil phase material flow is introduced. At this time, the material system faces the risk of chain-like liquid aggregation and ripening of highly dispersed droplets in the absence of immediate high-energy cross-linking and locking, as well as the apparent quality defects of product stratification during long-term storage. To solve the physical orientation conflict between the demand for highly dispersed droplet generation and the inability of the natural molecular emulsion film to withstand continuous strong shear damage, a high-precision metering pump controls the initial pumping flow rate of the oil phase at 40 mL / min, while the stirring system is continuously increased from an initial speed of 200 rpm to 800 rpm at an incremental speed of 15 rpm / min, ensuring that the instantaneous input flow rate of the oil phase is injected into the entire process. With pumping time Follow the logarithmic decay rule ,in, For instantaneous input flow, To initially set the pump flow rate, This is the flow attenuation coefficient. For pumping time, where the flow rate attenuation coefficient is... The setting is 0.035 / s; in the logic implementation of the control unit, the above logarithmic decay rule is specifically expressed in mathematical mapping as a standard rational fractional decay function of the instantaneous input flow rate with pumping time, that is, the instantaneous input flow rate Q is equal to the initial set pumping flow rate. Dividing by the sum of the denominator terms, which consists of the constant 1, the flow attenuation coefficient α, and the pumping time t, the microprocessor in the control unit samples the pumping time t in a discrete time step with a control cycle of 10ms, and calculates the instantaneous input flow digital command corresponding to the current timing sequence in a closed loop. This command is converted into the corresponding standard analog voltage signal or pulse width modulation signal and output to the frequency converter of the high-precision metering pump. By adjusting the reciprocating frequency of the metering pump plunger or the rotation step of the gear pump in real time, the actual input oil phase flow rate curve dynamically approximates the above continuous function trajectory within the physical upper limit, ensuring that the cumulative injection volume increases at a gradually slowing logarithmic convergence trend over time. This is achieved by using a variable acceleration sequence of the injection flow rate and an increasing... The control method of spatial phase interlocking in the fragmented flow field limits the instantaneous input rate of the oil phase and keeps it spatiotemporally synchronized with the migration rate of natural emulsifier molecules to the newly formed phase interface. This allows tea saponin and soybean lecithin molecules to be fully enriched and migrate to the interface in a low-stress environment. Thus, within a single control framework, it solves the industry dilemma of localized material overload exceeding the adsorption limit and abnormal fluid transitions caused by excessive shearing, which are common with conventional constant-rate oil injection. Furthermore, the quantitative determination of the match between the oil-water phase interface expansion rate and the adsorption rate of natural material molecules is achieved through dynamic correlation of the characteristic relaxation time of the oil-water mixed multiphase flow system. Specifically, the interface expansion rate is determined by the micro-droplet fragmentation rate caused by the linear increase in the instantaneous oil phase injection flow rate Q and the stirring system rotation speed. The corresponding surface area expansion characteristic time of the newly formed phase interface; the adsorption rate of natural material molecules depends on the effective diffusion coefficient and phase boundary adsorption barrier of tea saponin and soybean lecithin under the current concentration gradient, corresponding to the mass transfer characteristic time of spontaneous molecular enrichment and migration to the interface. This invention, by setting a logarithmically decaying oil phase pump flow rate and a linearly increasing stirring speed, ensures that the growth rate of the newly formed interface area driven by the mechanical energy field and the spontaneous adsorption flux of the phase interface driven by the concentration gradient are at the same physical order of magnitude at any point in time during the entire oil injection cycle. The implemented physical mapping path is characterized by the multiphase fluid in the reactor always maintaining the rheological characteristics of a smooth transition from Newtonian fluid to weakly shear-thinned fluid, thus preventing frequent droplet collisions and phase merging caused by molecular adsorption hysteresis. The triggered abrupt change in apparent viscosity of the bulk phase is detected during the oil phase injection process. An online torque sensor installed on the top of the stirring shaft continuously collects total dynamic torque data. The control unit processes the data in real time to eliminate the rate of change of mechanical inertial torque caused by the motor's active acceleration and the rate of change of gravity load torque caused by the linear increase in the total mass of the fluid due to feeding. The net rate of change of torque caused by the abnormal fluctuation of the fluid's apparent viscosity is then separated. When the net rate of change of torque exceeds the critical threshold of 0.8 N·m / s, the control unit automatically issues a compensation command to reduce the cooling rate of the subsequent first stage from 1.2℃ / min to 0.6℃ / min and extend the low-speed stirring time in step S103 from 20 min to 45 min, thus creating a conformational gap at the in-situ healed phase interface.

[0038] At the instant the oil phase injection is completed, the control system abandons the linear improvement path of extending the traditional high-shear stirring time or simply increasing the concentration of added materials. Instead, it applies an ultrasonic pulse with a duration of 3 seconds and a power of 1200W to the oil-water mixture system in the dispersed flow field to instantly break up the droplets. After the ultrasonic pulse stops, the speed of the stirring system is instantly reduced by 40% to 200 rpm within 0.5 seconds. During this deceleration phase, the drive shaft of the stirring system is connected to an electromagnetic clutch and an energy-consuming braking resistor group. The control unit disengages the mechanical connection between the shaft and the motor through the electromagnetic clutch to eliminate the rotor's mechanical inertia and activates the energy-consuming braking resistor. The damping system absorbs the residual kinetic energy fed back from the main shaft, controlling the mechanical deceleration response time of the impeller within the process range of 0.5s to 1.2s. This avoids mechanical damage to the transmission mechanism caused by the inertia of the large-capacity vessel fluid. Furthermore, the matching of the impeller's mechanical deceleration response time with the attenuation of the multiphase flow shear field is achieved through the synergistic damping effect of the fixed flow-blocking baffles set on the inner wall of the reactor and the viscosity surge of the multiphase flow system itself. When the impeller speed suddenly drops from the pulsed high speed to the low stirring speed within 0.5s to 1.2s, although the large volume of material in the reactor still maintains a macroscopic overall rotational trend under the action of inertia, the instantaneous removal of the main shaft driving force causes the impeller to decelerate. The direct mechanical thrust of the blade on the fluid dissipates instantaneously; simultaneously, the high-speed fluid continuously collides with the fixed flow-blocking baffles on the inner wall, generating strong macroscopic kinetic energy counter-current and turbulent dissipation. Furthermore, since the oil phase has been completely injected and has undergone high-density initial emulsification, the instantaneous apparent viscosity of the system has undergone a leap in magnitude compared to the initial injection stage, forming a significant microscopic internal viscous resistance. This causes the localized actual shear stress acting on the droplet phase interface film to rapidly decay to below the safe stress threshold within 0.5s to 1.2s, achieving kinetic energy cutoff of the local energy field at the microscopic scale, thus dissipating both macroscopic fluid flow inertia and microscopic flow field stress. Achieving thermodynamic self-consistency, the transient pulse energy field provides the energy required to cross the surface energy barrier of the droplet, driving the spatial chain segments of tea saponin and the polar ends of soybean lecithin at the phase interface to spontaneously align isotropically. The dynamic yielding action performed at the film-forming critical point eliminates the parasitic peeling and local tearing damage of the formed natural emulsion film by the continuous strong shear flow field through the instantaneous cutoff of mechanical kinetic energy. This provides an interference-free conformational reorganization time-space window for the natural macromolecules with adsorption lag, allowing the emulsifier molecules to complete isotropic lateral reorganization under the drive of low interfacial tension. Under the condition of continuous low-speed stirring after the speed reduction, 0.Hydrolyzed wheat protein at a 5% mass concentration exhibits steric hindrance reinforcement. Its abundant highly polar glutamine residues undergo spatial expansion of the macromolecular chain under ultrasonic pulse fields. Specifically, during the ultrasonic pulses lasting only 3 to 8 seconds, the high-power acoustic cavitation energy field and transient microjets do not directly induce the instantaneous formation of hydrogen bonds within the strong shear region. Instead, they selectively cleave the existing intramolecular hydrogen bonds and hydrophobic associations within the hydrolyzed wheat protein macromolecules through localized extreme energy, resulting in tightly folded, naturally occurring spherical structures. The conformation undergoes highly efficient unfolding and spatially non-directional unfolding, thereby fully exposing the highly polar amide side chains rich in glutamine residues to the continuous phase of the multiphase system. Within the mechanical kinetic energy cutoff window after the ultrasonic pulse stops abruptly and the stirring speed drops sharply, the external high-energy destructive field completely disappears. Under the gentle, low-speed shear flow field, the highly unfolded and inactive protein macromolecular segments smoothly spread, and the exposed highly polar groups and the densely enriched hydrophilic glycosyl groups of tea saponin, the polar terminal carboxyl groups and hydroxyl groups of soybean lecithin form a spatiotemporal connection. The collision probability reaches a maximum value, thus spontaneously forming a tightly interpenetrating network structure through multi-site multidirectional hydrogen bonds during the stable conformational remodeling period without strong shear interference. This network spontaneously forms multi-site hydrogen bonds with neighboring tea saponin and soybean lecithin molecules, in situ interweaving to form a high-density interfacial steric hindrance framework mesh and significantly increasing the interfacial yield stress. In the preparation of the dispersed aqueous substrate, the hydrolyzed wheat protein was added at a mass percentage concentration of 0.5% to 1.5%, with a weight-average molecular weight of 3000 Da to 5000 Da and a purity of [missing information]. Not less than 98%; when the concentration of hydrolyzed wheat protein added is less than 0.5%, no three-dimensional steric hindrance grid is generated in the shear zone of the flow field, and the stratification rate of the washing and conditioning emulsion increases in the accelerated aging test at 40℃; when the concentration of hydrolyzed wheat protein added is greater than 1.5%, under the action of the ultrasonic pulse field in step S102, the glutamine residues excessively overlap spatially and undergo thermally induced irreversible aggregation of macromolecular chains, causing an abnormal jump in the apparent viscosity of the fluid, resulting in macroscopic gelation or protein precipitation during the cooling and locking stage, making the median average particle size of the finished product greater than 1.50. m, correspondingly, the gradient temperature control jacket guides the oil-water mixture system to cool down in two stages. In the first stage, the cooling rate is controlled at 0.6℃ / min to slowly cool down to 30℃. Within this temperature range, the residual shear stress accumulated in the continuous phase fluid by the high-energy flow field is steadily released to block the outward expansion of anisotropic defects. In the second stage, the cooling rate is controlled at 0.2℃ / min to continue cooling down to room temperature of 22℃. Through the discrete cooling shock of the temperature field gradient, the hydrophobic hydrocarbon segments of the natural emulsifier are driven to generate lattice-ordered arrangement and lock and solidify the three-dimensional steric network, so that the system is transformed from a non-equilibrium metastable state to a long-term thermodynamically stable state.

[0039] Through the deep synergy of the aforementioned temporal flow field changes and temperature gradients, the oil-water mixture system produces a washing and conditioning emulsion product with a median average particle size converging within a narrow dispersion range of 0.25μm to 0.32μm. After being centrifuged at 3000rpm for 30 minutes at room temperature, no free oil phase precipitates at the phase interface. Furthermore, in a high-temperature accelerated aging storage test at 40℃ for 180 days, its stratification rate is less than 0.01mm / d. The product surface shows no buttery oil phase floating or phase merging failure, and the internal phase droplets are permanently confined within the three-dimensional topological framework. This improves the stability index of the natural material emulsification preparation process without adding synthetic chemical stabilizers.

[0040] Example 2: In the continuous operation of a large-capacity processing production line for personal care products, when the system constructs a pure natural emulsion system using soybean lecithin and tea saponin components under the low shear temperature boundary condition of 30°C, due to the inherent low interfacial tension repair rate and high phase sensitivity of natural macromolecules, the continuous phase flow field is prone to local phase enrichment and in-situ mechanical peeling and damage of the interfacial film when a high proportion of oil phase material flow is introduced. At this time, the material system faces the risk of chain liquid aggregation and ripening of highly dispersed droplets in the absence of immediate high-energy cross-linking and locking, as well as the apparent quality defects of product stratification during long-term storage.

[0041] A high-precision metering pump controls the initial pumping velocity of the oil phase material flow at 40 mL / min, while the stirring system continuously increases its speed from an initial speed of 200 rpm to 800 rpm in increments of 15 rpm / min, ensuring the instantaneous input flow rate of the oil phase throughout the entire process. With pumping time Follow the logarithmic decay rule ,in, For instantaneous input flow, To initially set the pump flow rate, This is the flow attenuation coefficient. For pumping time, where the flow rate attenuation coefficient is... The flow rate was set to 0.035 mPa·s. When the above process was carried out at a processing temperature of 30°C, the intermediate layer emulsification characteristics data extracted by the online high-frequency rheometer in the shear zone of the reactor showed that the dynamic viscosity of the intermediate instantaneous inner phase in the experimental group was 74.3 mPa·s at the 30th second of oil injection. The dynamic viscosity of the intermediate instantaneous inner phase in the partially missing control group at the same time point increased significantly to 112.6 mPa·s due to the lack of spatial hydrogen bond-assisted crosslinking of hydrolyzed wheat protein. The dynamic viscosity of the intermediate instantaneous inner phase in the conventional process control group increased dramatically to 245.8 mPa·s due to the local oil phase accumulation overload caused by constant-rate oil injection. This indicates that the logarithmically decaying input flow rate limits the instantaneous input rate of the oil phase and makes it achieve spatiotemporal synchronization with the migration rate of emulsifier molecules to the new phase interface, blocking the physical evolution path of local oil phase aggregation.

[0042] The oil injection process was completed at 180 seconds. An ultrasonic generator applied a 5-second, 1200W ultrasonic pulse to the oil-water mixture to break up the droplets. The control system triggered a retraction action, reducing the stirring speed by 40% to 300 rpm within 0.5 seconds. Finally, a temperature control mantle guided the material system to cool to room temperature (22℃) in two stages at a cooling rate of 0.6℃ / min. An online laser particle size analyzer collected the particle size distribution characteristics of the dispersed phase at three test temperatures: 30℃, 36℃, and 42℃. The median average particle size of the wash and conditioner emulsion products produced in the experimental group converged within narrow dispersion ranges of 0.254μm, 0.278μm, and 0.312μm, respectively. In contrast, the partially deficient control group, lacking interfacial steric hindrance and mesh locking, showed a different result. The final product emulsion particle size increased to 0.684 μm. In the conventional process control group, the internal structure of the assembled lamellar liquid crystal of the natural emulsion film was damaged by continuous high shear stress, and the internal phase droplets underwent non-uniform aggregation, with the median average particle size diverging to 1.425 μm. The data confirmed that the processing temperature range of 30℃ to 42℃ was limited by the thermodynamic solubility of natural macromolecules and the dissipation of interfacial desorption shear. To ensure the product's storage stability, after being placed in a high-temperature accelerated storage environment of 40℃ for 180 days, the phase boundary stratification rate of the experimental group was only 0.006 mm / d, which was lower than the 0.32 mm / d of the conventional process control group and the 0.43 mm / d of the out-of-range control group. This proves that this method maintains the long-term thermodynamic stability of the washing and care emulsion product in a material environment without the addition of synthetic chemical surfactants and chemical stabilizers.

[0043] Example 3: In the continuous operation of a large-capacity processing production line for washing and care products, when the stirring system and heating jacket temperature in the shearing reactor are constant, the initial dynamic viscosity of the continuous phase substrate changes due to fluctuations in the physical properties of soybean lecithin and tea saponin powder raw materials purchased from different batches. When the system uses a fixed oil phase pump flow rate control sequence, if it encounters high-resistance materials with initial dynamic viscosity at the upper limit critical state, the excessively high local shear resistance causes the introduced oil phase material to experience local overload, disrupting the spatial symmetry of the layered liquid crystal three-dimensional network in the continuous phase substrate. This leads to a lag in the adsorption mass transfer rate of emulsifier molecules, resulting in the median average particle size of the final washing and care emulsion product diverging to over 1.50 μm and accompanied by an increase in the stratification rate.

[0044] To eliminate processing uncertainties caused by batch-to-batch material property differences, the control system initiates a pre-calibration procedure. A viscosity sensor located at the bottom of the reactor measures the viscosity of the aqueous dispersion containing soybean lecithin and tea saponin at an initial temperature of 30°C. The average viscosity measurement from five consecutive samples with a variance less than 0.05 is used as the input parameter to the parameter calibration module. This module fine-tunes the initial speed increment of the stirring system according to a preset first-order linear compensation rule. When the measured initial dynamic viscosity deviates from the normal reference dynamic viscosity, the speed correction unit adjusts the speed according to the formula... Calculate and output the corresponding stirring speed correction amount. The specific values, among which, This is the adjustment amount for the stirring speed. The variable frequency gain coefficient for the flow field is fixed at 2.5. The initial dynamic viscosity is the measured value obtained from the online viscosity sensor. The standard dynamic viscosity reference value set for the process is fixed at 55 mPa·s. When the measured initial dynamic viscosity value changes to the upper limit scalar endpoint of 65 mPa·s, the control unit calculates the output stirring speed correction. The value is 25 rpm, and the drive frequency of the stirring motor in the reactor is increased in situ, so that the initial speed is automatically aligned from 200 rpm to 225 rpm, thereby making the mechanical shear rate adaptively matched to the low mass transfer rate of the current batch of materials in the initial state of oil-water contact.

[0045] After the high-precision metering pump completes the oil injection operation, to counteract the uneven flow resistance of the dispersed phase generated by the high-viscosity material in the reactor, an ultrasonic generator applies a transient pulse energy field with a power of 1500W to the oil-water mixture system. The stirring system generates a dynamic retraction action, and its rotation speed is stepped down to 250rpm within 0.6s to avoid shear damage to the assembled interface caused by the continuous high shear energy field. When the material temperature is slowly cooled to 22℃ in two stages through a gradient temperature control jacket, the hydrophobic segments in the finished washing and conditioning emulsion fix the lattice arrangement structure. Test data shows that when faced with the initial... When the dynamic viscosity is at the critical fluctuations of 45 mPa·s and 65 mPa·s respectively, the flow attenuation coefficient is dynamically adjusted through the above parameter calibration process. The median average particle size of the final produced washing and care emulsion product is maintained in the range of 0.262 μm to 0.285 μm. After the washing and care emulsion product is placed at 40℃ for 180 days, the phase boundary stratification rate is less than 0.008 mm / d. The three-dimensional steric grid structure provides spatial steric constraint on the dispersed phase droplets, and the stability and long-term storage quality of the material system are not affected by the fluctuations in the physical properties of the initial raw materials.

[0046] Example 4: In the continuous processing flow of washing and care emulsion, the batch-to-batch physicochemical properties of natural emulsifiers soybean lecithin and tea saponin cause deviations in their swelling rate and interfacial tension equilibrium time in the continuous aqueous dispersion phase. To ensure the long-term stability of emulsion particle size, before executing the continuous injection process of oil phase materials, the system first discretizes and calibrates the swelling kinetic characteristics of different batches of natural emulsifiers. The initial dynamic viscosity of the dispersed aqueous phase after stirring to apparent homogeneity at room temperature is used as the physical property benchmark. The initial dynamic viscosity is measured using an online rotational viscometer and used as an input parameter in the preset shear energy field compensation function to determine the attenuation sequence of the oil phase pumping flow rate.

[0047] The shear energy field compensation function is ,in, for Oil phase pump flow rate at all times The initial pump flow rate is set to 80 mL / min; The viscosity-adaptive decay constant is... Current running time The total duration of the oil injection process is set to 600 seconds; the control unit calculates the initial dynamic viscosity based on the real-time viscosity measured by the online viscosity sensor. Dynamic calculation of viscosity-adaptive decay constant Its calculation logic is as follows: ,in, The normal reference attenuation constant has a value of 0.5; This is the viscosity fluctuation compensation coefficient. The initial dynamic viscosity was measured by an online viscosity sensor. The reference dynamic viscosity of the standard batch emulsifier is 60 mPa·s. When the measured initial dynamic viscosity deviates from the reference value, the flow rate decay curve is adaptively corrected through this compensation function to keep the phase interface expansion rate of newly generated droplets and the diffusion rate of emulsifier molecules to the interface within the kinetic equilibrium window.

[0048] To eliminate shear energy field deviations caused by impeller wear or mechanical clearances in the transmission system due to long-term system operation, the system automatically triggers a kinetic response calibration process after every 100 batches of product. This involves injecting a standard test fluid with known physical properties into the reactor, measuring the current fluctuations and torque changes of the stirring motor under a preset speed gradient, and comparing this with the output particle size data recorded by the online particle size monitor at the reactor outlet. A multiple linear regression algorithm is then used to update the stirring motor's speed compensation mapping table. When the system detects a decrease in the unit shear output efficiency of the impeller exceeding 5.0%, the control unit automatically injects a compensating speed increment into the stirring motor. This increment is calculated using the following method: ,in, For speed compensation increment, This is the speed compensation weighting coefficient, with a value of 120.0. The real-time median particle size measured by the online monitoring instrument. The target median particle size for the process is preset to 0.28 μm. An online laser particle size analyzer installed on the reactor's discharge pipeline is connected to an automatic bypass continuous dilution mechanism. A high-pressure metering pump continuously draws material from the reactor at a flow rate of 2 mL / min into a mixing chamber with a quartz jacket. Deionized water at a flow rate of 2000 mL / min is introduced for bubble-free online static mixing. After diluting the material volume fraction to the single-transmittance light scattering range, it is introduced into a flow measurement cell to obtain the real-time median particle size. The system adjusts the motor drive frequency in real time according to the particle size deviation to ensure that the emulsion system still maintains the target particle size convergence range of 0.25μm to 0.32μm under the condition of agitator blade wear. Through the above offline calibration and online compensation mechanism, the stability of the preparation process of the washing and care emulsion is locked within the preset engineering parameter boundaries.

[0049] 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 natural material emulsification process in the processing of personal care products, characterized in that, Includes the following steps: Step S101: Under the temperature conditions of 30℃ to 42℃, the material flow containing the oil phase is injected into the dispersed aqueous phase containing tea saponin and soybean lecithin at a pumping flow rate that decreases hourly. At the same time, the speed of the stirring system is continuously increased at a speed rate of 15 rpm / min to 35 rpm / min to form a dispersion flow field inside the dispersed aqueous phase in which the oil-water phase interface expansion rate matches the adsorption rate of natural material molecules. Step S102: Apply an ultrasonic pulse with a duration of 3s to 8s and a power of 1200W to 1800W to the oil-water mixture system in the dispersed flow field to break up the droplets. After the ultrasonic pulse stops, adjust the speed of the stirring system to be reduced by 40% to 60% instantly to generate a dynamic yielding action, and control the tea saponin and soybean lecithin to arrange on the surface of the oil droplets to form a transversely reorganized phase interface film. Step S103: Maintain the reduced rotation speed and continuously stir the oil-water mixture system at a low speed, and control the oil-water mixture system to cool down in two stages. In the first stage, control the cooling rate to 0.6℃ / min to 1.2℃ / min to cool down to 30℃ to release the residual shear stress in the oil-water mixture system. In the second stage, control the cooling rate to 0.2℃ / min to 0.5℃ / min to continue cooling down to 22℃ to lock the lattice arrangement of hydrophobic hydrocarbon segments in the phase interface film and form a three-dimensional steric network.

2. The natural material emulsification process in the processing of personal care products according to claim 1, characterized in that, In step S101, the initial value of the pump flow rate that decreases hourly is 40 mL / min to 60 mL / min, the initial speed of the stirring system is 200 rpm to 300 rpm, and the speed after adjustment is 800 rpm to 1200 rpm.

3. The natural material emulsification process in the processing of personal care products according to claim 1, characterized in that, The total weight of the system is 100%, with tea saponin accounting for 1.5% to 3.5%, soybean lecithin accounting for 2.0% to 5.0%, oil phase accounting for 15% to 35%, and the dispersed aqueous phase containing 0.5% to 1.5% hydrolyzed wheat protein, with the balance being water.

4. The natural material emulsification process in the processing of personal care products according to claim 1, characterized in that, In step S101, dynamic torque data is collected by an online torque sensor. When the rate of change of the dynamic torque data over time exceeds the critical threshold of 0.8 N·m / s, the control unit reduces the cooling rate of the first stage and extends the low-speed stirring time in step S103.

5. The natural material emulsification process in the processing of personal care products according to claim 1, characterized in that, Step S102 includes the following sub-steps: Step S1021, applying an ultrasonic pulse of 20 kHz to 28 kHz to the oil-water mixture system; Step S1022, controlling the rotation speed of the stirring system to be reduced to 200 rpm to 400 rpm within 0.5 s to 1.2 s.

6. The natural material emulsification process in the processing of personal care products according to claim 1, characterized in that, In step S103, step S1031 involves cooling the oil-water mixture system to 30°C at a rate of 0.6°C / min to 1.2°C / min; step S1032 involves cooling the oil-water mixture system to 22°C at a rate of 0.2°C / min to 0.5°C / min.

7. The natural material emulsification process in the processing of personal care products according to claim 1, characterized in that, In step S101, the total time for injecting the material flow containing the oil phase is controlled to be 30 min to 50 min, and the pumping flow rate is gradually reduced from 50 mL / min to 10 mL / min; at the same time, the rotation speed of the stirring system is gradually increased from 200 rpm to 1000 rpm.

8. The natural material emulsification process in the processing of personal care products according to claim 1, characterized in that, It also includes step S104, where after the temperature of the oil-water mixture system drops to 22°C and is kept at a constant temperature for 10 to 15 minutes, the stirring system is stopped and the material is discharged to obtain the final washing and care emulsion product.

9. The natural material emulsification process in the processing of personal care products according to claim 8, characterized in that, Step S105: Record the phase separation thickness data of the final shampoo and conditioner product after 180 days at 40°C; Step S106: Determine the separation rate based on the data; Step S107: When the separation rate is less than 0.01 mm / d, the product is deemed to have met the factory standard.

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