Antibacterial finishing system based on Juncao fibers, antibacterial fabric and process thereof

Abstract

The invention discloses an antibacterial finishing system based on Juncao fibers, an antibacterial fabric and a process thereof, and belongs to the technical field of antibacterial products. Through closed-loop control of an intelligent sensor and a PLC, the pH value fluctuation is reduced to + / -0.05 from traditional + / -0.3, the mangle expression fluctuation is reduced to + / -1.5% from + / -5%, and the baking temperature difference is gt; the temperature is reduced to 1t at 10 DEG C; the temperature is 1.5 DEG C, and the process capability index CPK average gt; 1.67, 1.67); a near-infrared spectrometer is adopted for online detection of the adhesion amount of antibacterial components (the detection period is 1t, 30 seconds), traditional offline detection (2-3 days) is replaced, the detection time of unqualified products is shortened by 95%, and batch quality accidents are avoided; all technological parameters including bursting pressure, fermentation DO, roller pressure and other 28 items are automatically uploaded to an MES system, forward traceability and reverse traceability are supported, the intelligent manufacturing data management standard is met, the antibacterial product has the remarkable bacteriostasis rate on staphylococcus aureus and escherichia coli, the bacteriostasis rate is still kept at the high level after 30 times of washing, and the antibacterial product has the good antibacterial effect. The fabric is suitable for the field of hygienic materials or underwear such as masks, underwear and underpants.

Description

Technical Field

[0001] This invention discloses a smart functionalization technology for fabrics, and in particular relates to an antibacterial finishing system based on Juncao fiber, antibacterial fabrics and their processes. Background Technology

[0002] Natural antibacterial textiles generally suffer from problems such as low loading rate of active ingredients, poor washability, and narrow fiber compatibility.

[0003] Traditional organic solvent extraction processes pollute the environment, have low affinity and insufficient depth, and when active antibacterial factors are used, they suffer from excessive degradation during high-temperature baking, and the wash fastness is generally reduced.

[0004] However, some fabrics that acquire antibacterial properties through antibacterial layer treatment, such as underwear, do not retain their antibacterial properties well and are easily worn after multiple washes, resulting in a significant decrease in antibacterial properties. Therefore, a new treatment process is needed.

[0005] The antibacterial finishing process faces the following technical bottlenecks in intelligent manufacturing:

[0006] (1) Process parameters rely on human experience, and key parameters such as pH value, temperature, and rolling yield fluctuate greatly (usually >5%), resulting in significant batch-to-batch differences in products;

[0007] (2) The lack of online monitoring methods throughout the entire process makes it impossible to obtain data on the amount of antibacterial components attached in real time, resulting in lagging quality control;

[0008] (3) The processes are severely isolated, making it impossible to achieve a closed loop of extraction-processing-detection;

[0009] (4) The temperature is uneven in the traditional baking process (temperature difference > 10°C), resulting in a thermal degradation rate of > 20% of the antibacterial active ingredients. Summary of the Invention

[0010] The purpose of this invention is to provide an antibacterial finishing system, antibacterial fabric and process based on Juncao fiber to solve the above problems.

[0011] To achieve the above objectives, the present invention provides the following technical solution, comprising the following automated control modules:

[0012] Intelligent pretreatment module: The fabric is treated by overflow dyeing tank. The dyeing tank is equipped with liquid level sensor and online pH meter. The alkaline washing solution is automatically prepared at a liquor ratio of 1:10. After alkaline washing, the neutralization endpoint is monitored in real time by pH sensor. The acid pump is automatically controlled to shut off when pH=7.0±0.1.

[0013] Impregnation and curing module: The rolling mill is equipped with pressure sensors and liquid volume infrared detectors, and the liquid rate is automatically adjusted to 80%±1.5% during the two-impregnation and two-rolling process through PLC control; the hot air baking machine adopts three-zone independent temperature control, and achieves precise drying at 150°C±1.5°C through thermocouple feedback;

[0014] Intelligent preparation unit for bioactive substances: The extraction process is automated by a DCS system through a steam explosion-enzymatic hydrolysis-subcritical water extraction combined device, equipped with a pressure transmitter, temperature sensor and online pH meter, and the fermentation yield of lecithin is optimized by model predictive control algorithm.

[0015] Central control system: Each module is connected via an industrial bus, and process parameters are uploaded to the MES system in real time, supporting remote monitoring and process traceability;

[0016] The intelligent preparation unit for bioactive substances includes the following steps:

[0017] 60 parts by weight of Ganoderma lucidum and 40 parts by weight of Cordyceps militaris were dried and sliced, and then loaded into a rupture vessel with a loading coefficient of 0.7. Saturated steam of 1.8±0.02MPa was introduced. The rupture vessel was equipped with pressure and temperature sensors, and the data was uploaded to the PLC. When the pressure deviation was >0.02MPa, the opening of the steam valve was automatically adjusted.

[0018] After blasting, the material was added to deionized water at a weight-to-volume ratio of 1:8, and the pH was automatically adjusted to 5.0±0.05 using an online pH meter. A compound enzyme was added and enzymatically hydrolyzed at 50°C±0.5°C for 2.5 hours. After enzymatic hydrolysis, the enzyme was inactivated by heating.

[0019] The enzymatic hydrolysis product and Serratia marcescens cells were added to a subcritical water extraction reactor at a mass ratio of 1000:8. The temperature was increased to 135°C at 3°C / min, and the pressure was increased to 6.0 MPa at 0.1 MPa / min. Flavonoid molecules, polysaccharide molecules, and microfibrillated cellulose were obtained by membrane separation.

[0020] As a preferred option, the intelligent preparation unit for bioactive substances also includes:

[0021] The fermenter is equipped with a dissolved oxygen sensor and a pH electrode, and three-stage fermentation is achieved through PID closed-loop control:

[0022] During the first stage (0-24 hours), maintain pH 7.0 ± 0.05 and DO 30% ± 2%.

[0023] During the second stage (24-48 hours), maintain pH 6.6±0.05 and DO 25%±2%, and automatically replenish 1% glycerol.

[0024] In the third stage (48-72 hours), the chitosan solution is automatically added via a peristaltic pump, and the addition rate is uniformly completed within 30 minutes.

[0025] After fermentation, the fermentation broth was sterilized by passing it through a 0.22μm ceramic membrane. β-CD was added and the inclusion reaction was carried out at 60°C±2°C for 12 hours under nitrogen protection. Finally, the binary inclusion complex of Juncao fiber was obtained by spray drying.

[0026] Preferably, in the pad-curing module, the pad-forming liquid is precisely prepared by weight using an automatic batching system:

[0027] The mixture consists of 10 parts of binary inclusion compound raw material, 6 parts of butanetetracarboxylic acid, 4 parts of sodium hypophosphite, and 0.1 parts of trisodium citrate, with a mixing accuracy of ±0.5%. The stirring speed is 60 rpm and controlled by a frequency converter.

[0028] Preferably, the intelligent pretreatment module automatically switches to the following mode when processing nonwoven fabrics:

[0029] Add 10 g / L NaOH and wash at 80°C for 30 min, and automatically add 2 g / L quaternary ammonium salt accelerator. The amount added is precisely controlled by a metering pump.

[0030] An antimicrobial finishing process based on Juncao fiber, implemented using the aforementioned antimicrobial finishing system based on Juncao fiber, includes the following steps:

[0031] The fabric is alkali washed and neutralized through an intelligent pretreatment module, and the process parameters are monitored and automatically recorded in real time by online sensors.

[0032] The roll curing module performs two dips and two rolls, and the roll yield is fed back to the PLC in real time by an infrared detector to automatically adjust the roll pressure.

[0033] Pre-drying and curing are performed using a baking oven with independent PID temperature control in three zones, temperature difference <±1.5°C, and drying time is automatically timed by a photoelectric switch;

[0034] The amount of antibacterial ingredients adhered is verified by an online spectral detection system, and non-conforming products are automatically marked and sorted.

[0035] An antimicrobial fabric based on antimicrobial finishing of Juncao fiber is prepared by the above-mentioned antimicrobial finishing process, including a base fabric layer and an antimicrobial layer formed between the base fabric layers. The antimicrobial layer is a binary inclusion complex coating formed by β-CD, flavonoid molecules and styraxin.

[0036] Compared with the prior art, the beneficial effects of the present invention are:

[0037] Through intelligent sensors and PLC closed-loop control, the pH value fluctuation was reduced from the traditional ±0.3 to ±0.05, the rolling yield fluctuation was reduced from ±5% to ±1.5%, the baking temperature difference was reduced from >10°C to <1.5°C, and the process capability index CPK was >1.67.

[0038] The online detection of antibacterial component adhesion using a near-infrared spectrometer (detection cycle <30 seconds) replaces traditional offline detection (2-3 days), reducing the detection time of non-conforming products by 95% and avoiding batch quality accidents.

[0039] All process parameters, including 28 items such as burst pressure, fermentation DO, and roll pressure, are automatically uploaded to the MES system, supporting forward and reverse traceability, and complying with intelligent manufacturing data management standards.

[0040] This invention pretreats raw materials through a combination of fungal pretreatment and steam explosion. It then uses a complex enzyme to release active ingredients such as flavonoids, followed by subcritical water extraction and membrane separation to fractionally extract flavonoids, polysaccharides, and ultrafine cellulose. Fermentation and chitosan addition produce styraxin, achieving in-situ coating and binary inclusion to form a stable styraxin-flavonoid inclusion complex. Through specific pretreatment and low-temperature cross-linking, the complex is firmly bound to the fiber surface. The antibacterial products of this invention exhibit significant antibacterial rates against Staphylococcus aureus and Escherichia coli, maintaining a high level of antibacterial activity even after 30 washes. This invention is suitable for use in hygiene materials such as masks, underwear, and briefs, or for intimate apparel. Attached Figure Description

[0041] Figure 1 The chart shows the antibacterial properties measured in the control experiment.

[0042] Figure 2 This is a chart showing the wash resistance performance measured in the control experiment;

[0043] Figure 3 The image shows the characterization of styraxin observed by SEM;

[0044] Figure 4 Characterization map of β-CD observed by SEM

[0045] Figure 5 Characterization images of styraxin, flavonoid molecules, and β-CD mixture observed by SEM;

[0046] Figure 6 Characterization of the binary inclusion complex observed by SEM;

[0047] Figure 7 A flowchart of the overall antibacterial finishing system; Figure 8 Here is the block diagram of the closed-loop PID control logic for pH value; Figure 9 The image shows the DSC spectrum of a mixture of styraxone, β-CD, and flavonoid molecules (styraxone, flavonoids, and β-CD), a binary inclusion complex. Detailed Implementation

[0048] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. In this description, it should be understood that the terms "upper," "lower," "front," "rear," "left," "right," "top," "bottom," "inner," and "outer," etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on the present invention. Obviously, the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0049] An antimicrobial finishing system based on Juncao fiber includes the following automated control module:

[0050] Intelligent pretreatment module: The fabric is treated by overflow dyeing tank. The dyeing tank is equipped with liquid level sensor and online pH meter. The alkaline washing solution is automatically prepared at a liquor ratio of 1:10. After alkaline washing, the neutralization endpoint is monitored in real time by pH sensor. The acid pump is automatically controlled to shut off when pH=7.0±0.1.

[0051] Impregnation and curing module: The rolling mill is equipped with pressure sensors and liquid volume infrared detectors, and the liquid rate is automatically adjusted to 80%±1.5% during the two-impregnation and two-rolling process through PLC control; the hot air baking machine adopts three-zone independent temperature control, and achieves precise drying at 150°C±1.5°C through thermocouple feedback;

[0052] Intelligent preparation unit for bioactive substances: The extraction process is automated by a DCS system through a steam explosion-enzymatic hydrolysis-subcritical water extraction combined device, equipped with a pressure transmitter, temperature sensor and online pH meter, and the fermentation yield of lecithin is optimized by model predictive control algorithm.

[0053] Central control system: Each module is connected via an industrial bus, and process parameters are uploaded to the MES system in real time, supporting remote monitoring and process traceability;

[0054] The intelligent preparation unit for bioactive substances includes the following steps:

[0055] S1, 60 parts by weight of Ganoderma lucidum and 40 parts by weight of Cordyceps militaris are dried in an oven at 60℃ for 6 hours until the moisture content is 8-10%. After slicing, slices of 2-3 cm are obtained with a bulk density of 120 kg / m³. 3The initial raw material was loaded into the explosion tank with a loading coefficient of 0.7 and 1.8±0.05 saturated steam was introduced and the pressure was maintained for 6.5 min. The explosion volume ratio was 1:20. The material was instantly exploded to a collection tank with a pressure of 0.1 MPa. The material temperature dropped to 105℃. After the explosion, a pretreated raw material with a moisture content of 45-50% was obtained. The soluble polysaccharide was recovered under a negative pressure of -0.08 MPa by a cyclone separator and a condenser.

[0056] By drying, slicing, and steam explosion, Juncao grass is transformed into a pre-treated raw material suitable for subsequent extraction. Hot air drying reduces the moisture content of Juncao grass, making it easier for subsequent processing. Slicing Juncao grass into pieces increases its specific surface area, which is beneficial for extraction. Steam explosion destroys the cell walls and fiber structure of Juncao grass, making it easier for components such as polysaccharides and flavonoids to dissolve. After explosion, the material is processed through a cyclone separator and a condenser to recover soluble polysaccharides, thus achieving resource recycling.

[0057] S2, the pretreated raw materials were added to deionized water at a weight-to-volume ratio of 1:8, the pH was adjusted to 5.0±0.1, and the mixture was transferred to a stirred tank. The compound enzyme was added and enzymatically hydrolyzed for 2.5 hours. The stirring rate was 200 rpm, and 0.1 vvm of oxygen was introduced. The compound enzyme consisted of 2 parts cellulase and 1 part pectinase. The enzymatic hydrolysis temperature was 50℃. After enzymatic hydrolysis, the temperature was raised to 85℃ and extinguished for 15 minutes. The liquid was then filtered through a 400-mesh polyester filter cloth using a plate and frame filter press to obtain the remaining enzymatic hydrolysis product.

[0058] Cellulase and pectinase are used to enzymatically hydrolyze the pretreated Juncao grass to further break down the cellulose and pectin structures and release active ingredients such as flavonoids. Cellulase acts on the β-1,4-glycosidic bonds of cellulose, breaking it down into cellobiose and glucose, while pectinase breaks down the methyl ester bonds and glycosidic bonds of pectin, loosening the cell wall structure and releasing active ingredients such as flavonoids. After enzymatic hydrolysis, the temperature is raised to inactivate the enzymes to prevent further enzyme action and product degradation.

[0059] S3, the enzymatic hydrolysis product and cultured Serratia marcescens cells were added to the reactor at a mass ratio of 1000:8 and mixed. The temperature was increased to 135℃ at 3℃ / min and the pressure was increased to 6.0MPa at 0.1MPa / min, and the reaction was maintained at the same temperature and pressure for 18min. The temperature was then reduced to 60℃ in 5min by cooling water through the jacket. After depressurization and filtration, the first-stage filtrate was filtered through a 10kDa filter membrane to obtain flavonoid molecules enriched. The second-stage permeate was then filtered through a 500Da nanofiltration membrane to obtain polysaccharide enriched. The solids retained in the third stage were vacuum dried at 60℃ to obtain microfibrillated cellulose.

[0060] With a moisture content of 75-85%, the enzymatic hydrolysis products are mixed with *Serratia marcescens* cells. Subcritical water extraction under high temperature and pressure helps dissolve flavonoid molecules and polysaccharides, further separating flavonoid molecules, polysaccharides, and ultrafine cellulose for fractional extraction. This avoids excessive cellulose degradation. During the subcritical water extraction stage, wet mycelium obtained after fermentation termination in step S4 (*Serratia marcescens* sludge) is added. This sludge is rich in polysaccharides, proteins, and a small amount of residual styracil, which can form protein-polysaccharide-pigment micelles in high-temperature water, reducing the surface tension of the extraction system, promoting the diffusion of flavonoid molecules from the cell wall into the aqueous phase, and increasing the dissolution rate. The subcritical water high temperature... Under high pressure, the ultrafibers of the fungus tend to re-aggregate and form fiber bundles, which can easily lead to filtration blockage and flavonoid molecule encapsulation. However, the fungal micelles can coat the fiber surface, and the steric hindrance effect prevents re-aggregation and reduces filtration blockage. The hydroxyl groups of the fungal polysaccharides in the fungal mud form a hydrogen bond network with the phenolic hydroxyl groups of flavonoid molecules, reducing high-temperature hydrolysis and oxidation losses and increasing the retention rate of flavonoid molecules. The small amount of residual styraxin and polysaccharides in the fungal mud can generate a weakly reducing microenvironment under subcritical conditions, inhibiting the oxidation and ring-opening of flavonoid molecules, while eliminating the need to introduce external chemical additives. The three intermediate products obtained through membrane fractionation, and the selection of ultrafiltration and nanofiltration membranes based on the molecular weight of flavonoid molecules and polysaccharides, achieve efficient separation.

[0061] By utilizing the fermentation by-product microbial sludge in step S4, a closed-loop utilization of all components—residue, liquid, and bacteria—is achieved, reducing waste emissions. Using the fermented wet microbial body as seed for subsequent fermentation can maintain the activity and stability of the microbial strain while reducing the acclimatization time.

[0062] S4, prepare the culture medium according to the unit mass parts:

[0063] 15 parts peptone, 3 parts NaCl, 2 parts KCl, 2 parts MgSO4·7H2O, 3.78 parts glycerol, and 0.8 parts of flavonoid molecule enrichment from S3 were added;

[0064] The intelligent preparation unit for bioactive substances also includes:

[0065] The mixture was transferred to a fermenter, and the pH was adjusted using 2 mol / L HCl or NaOH. During the first stage of fermentation (0-24 hours), the pH was maintained at 7.0, dissolved oxygen at 30%, temperature at 28°C, and stirring speed at 200 rpm. After the second stage (24 hours), the pH was maintained at 6.6, dissolved oxygen at 25%, and temperature at 28°C, with 1% glycerol added to the total fermentation broth mass. After the third stage (48 hours), chitosan solution was added at a rate of 0.75 g per 5 L of fermenter volume. Fermentation ended after the third stage (72 hours), with the tank pressure controlled at 0.05 MPa, and the temperature lowered to 10°C to terminate the fermentation.

[0066] The fermenter is equipped with a dissolved oxygen sensor and a pH electrode, and three-stage fermentation is achieved through PID closed-loop control:

[0067] During the first stage (0-24 hours), maintain pH 7.0 ± 0.05 and DO 30% ± 2%.

[0068] During the second stage (24-48 hours), maintain pH 6.6±0.05 and DO 25%±2%, and automatically replenish 1% glycerol.

[0069] In the third stage (48-72 hours), the chitosan solution is automatically added via a peristaltic pump, and the addition rate is uniformly completed within 30 minutes.

[0070] After fermentation, the fermentation broth was sterilized by a 0.22μm ceramic membrane, and β-CD was added for inclusion reaction at 60°C±2°C for 12h. Nitrogen protection was maintained throughout the process, and finally the binary inclusion complex of Juncao fiber was obtained by spray drying.

[0071] In the third stage of step S4, the chitosan solution is prepared by dissolving chitosan with a degree of deacetylation ≥85% in 0.5% acetic acid solution to a concentration of 0.15 g / L. The chitosan solution is then fed into the fermenter using a peristaltic pump, and the feeding rate is controlled to ensure uniform addition within 30 minutes.

[0072] Serratia marcescens fermentation was used to produce squalene, and in-situ coating was achieved by adding chitosan. Serratia marcescens synthesizes squalene during fermentation, and the addition of chitosan helps to enhance the stability and bioactivity of squalene. The amino groups of chitosan are protonated under acidic conditions, increasing the positive charge of the fermentation broth and facilitating subsequent binding with fibers.

[0073] S5, the fermentation broth was sterilized by a 0.22μm ceramic membrane and then concentrated by 2 times in volume before being transferred to a reaction vessel. β-CD with a mass ratio of 1:1.2 to the fermentation broth was added for reaction. The mixture was stirred at 60rpm at 60±2℃ and kept at this temperature for 12h under N2 protection throughout. Then, the temperature was lowered to 45°C, and epichlorohydrin with a molar ratio of 9:1 to β-CD was added dropwise at a uniform rate over 30min. Then, PHMG with a molar ratio of 1:6 to β-CD was added, and the mixture was reacted at 70°C for 2h. After that, residual epichlorohydrin was removed by online degassing under a pressure of -0.09MPa. The mixture was then dried by spray drying at an inlet temperature of 180℃ and an outlet temperature of 80℃ to obtain the binary inclusion complex of Juncao fiber.

[0074] The fermentation broth contains styraxin and flavonoid molecules, which are then encapsulated to form a stable binary inclusion complex. The cavity structure of β-CD can encapsulate styraxin and flavonoid molecules to form a stable inclusion complex. Epichlorohydrin is used to crosslink β-CD and PHMG to enhance the stability of the inclusion complex. The cationic nature of PHMG helps with subsequent binding with fibers.

[0075] like Figure 3-6The figures shown are SEM characterization diagrams of styraxone, β-CD, a mixture (styraxone, flavonoid molecules, and β-CD), and binary inclusion complexes. Figure 3 As shown, styracin has an irregular granular structure, such as... Figure 4 As shown, after extraction and purification, β-CD exhibits a sheet-like structure with a relatively smooth surface, distributed on the fiber surface, such as... Figure 5 As shown, styracin, flavonoid molecules, and the β-CD mixture exhibit irregular particulate and plate-like morphologies; for example... Figure 6 As shown, no irregular particulate structure was observed, while β-CD was a regular quadrilateral crystal, proving that the cavity structure of β-CD encapsulates styracin and flavonoid molecules. This encapsulation structure facilitates the slow release of antibacterial components, thus maintaining highly effective antibacterial properties even after multiple washes.

[0076] like Figure 9 The image shows the DSC spectrum of the binary inclusion complex characterizing squalene, β-CD, and a mixture (squalene, flavonoid molecules, and β-CD). The melting temperatures of squalene and flavonoid molecules are approximately 137℃, while that of β-CD is approximately 227℃. The DSC spectrum of the mixture (squalene, flavonoid molecules, and β-CD) shows two endothermic melting peaks related to squalene and β-CD. The melting peak of the inclusion complex associated with squalene shifts from 137℃ to 123℃. When guest molecules are embedded in the β-CD cavity, their melting, boiling, or sublimation points typically shift to different temperatures or disappear. This change in melting temperature further confirms the successful preparation of the inclusion complex.

[0077] Intelligent preprocessing module hardware configuration:

[0078] Overflow dyeing tank: The Donggeng ECO-500 intelligent dyeing tank from Taiwan, China, is used, equipped with an E+HFMD77 level sensor (accuracy ±0.5%), and the liquor ratio control range is 1:10±0.3.

[0079] Online pH meter: Mettler Toledo InPro4260i pH electrode, measuring range 0-14, accuracy ±0.02pH, response time <30 seconds, signal is connected to PLC via 4-20mA;

[0080] Automatic alkali solution preparation system: Prominent DULCODOS® measurement and control station, metering pump model Beta®bBT4B, flow range 0.74-32L / h, accuracy ±1%;

[0081] Temperature control: PT100 RTD (Class A accuracy ±0.15°C) with Omron E5CC temperature controller, alkaline washing temperature 60°C ±0.5°C.

[0082] Hardware configuration of the pad-curing module:

[0083] Intelligent rolling mill: German KOT KR-500 uniform rolling mill, equipped with:

[0084] Pressure sensor: Honeywell PX2 series, measuring range 0-100N / cm2, accuracy ±0.25%FS;

[0085] Liquid volume detection: Near-InfraredOnlineMoistureAnalyzer (NIR-6000), detection accuracy ±0.3%, response time 50ms;

[0086] Servo motor: Mitsubishi HG-KR73J, with MR-J4-70A driver, roll gap adjustment accuracy ±0.01mm;

[0087] Hot air baking machine: AI-RD-3000 three-layer hot air tenter:

[0088] Temperature sensor: Type K thermocouple (Class I accuracy ±1.5°C), 6 measuring points per zone;

[0089] PID controller: Siemens S7-1200 PLC with built-in PID module, control cycle 100ms, overshoot <2%;

[0090] Wind speed control: E+HProlinePromag10 flow meter, range 0-5000m³ / h, accuracy ±0.5%.

[0091] Configuration of the intelligent preparation unit for bioactive substances:

[0092] Steam explosion module:

[0093] Explosion-proof container: Wuhan Juneng CQS-200 model, 200L capacity, design pressure 2.5MPa;

[0094] Pressure transmitter: Yokogawa EJA430A, range 0-3MPa, accuracy ±0.075%, automatic pressure fluctuation correction response time <1 second;

[0095] Temperature sensor: PT100 (Grade A), insertion depth 15cm, response time <5 seconds;

[0096] PLC control logic: Siemens S7-1500CPU1516-3PN / DP, cycle time <1μs, steam valve adopts SMCITV2030 electro-proportional valve, opening control accuracy ±0.5%.

[0097] Subcritical water extraction module:

[0098] Reactor: Weihai Huanyu GSH-500 high-pressure reactor, designed for a temperature of 150°C and a pressure of 8MPa;

[0099] Heating rate control: Achieve linear heating of 3°C / min ± 0.2°C using Eurotherm 2604 temperature controller;

[0100] Pressure control: HIP15-20AF type back pressure valve, pressure increase rate 0.1MPa / min±0.01MPa.

[0101] Intelligent fermentation module:

[0102] Fermentation tank: Shanghai Baoxing BIOTECH-50JS, 50L capacity, equipped with:

[0103] DO sensor: Hamilton VisiFerm DO Arc120, range 0-200%, accuracy ±1%, automatic temperature compensation;

[0104] pH electrode: Mettler Toledo InPro3251, measurement accuracy ±0.01pH, adjustable automatic cleaning cycle;

[0105] Peristaltic pump: Lange WT600-2J for chitosan addition, flow rate 0.006-2300 mL / min, accuracy ±0.5%;

[0106] Feeding system: The weighing module uses an HBMPW6D single-point sensor with a range of 20kg, an accuracy of ±0.02%, and a glycerin feeding error of <±5g.

[0107] Central control system configuration:

[0108] Main controller: Siemens S7-1516-3PN / DPPLC, processing speed <1μs / instruction, 6MB memory;

[0109] Human-computer interface: WinCCOAV3.17, supports 15,000 external variables, screen refresh rate <500ms;

[0110] Communication protocol: ProfinetIRT, loop time <1ms, modules are interconnected via SCALANCEXB208 switch;

[0111] MES Interface: OPCUA server, which supports real-time uploading of process data to the factory MES system, with a data sampling period of 1 second;

[0112] Database: Microsoft SQL Server 2019, storing 10,000 sets of process batch data, supporting SPC analysis.

[0113] Online detection system:

[0114] Near-infrared spectrometer: Bruker Matrix-FII, for detecting the amount of antibacterial components attached, wavelength range 800-2500nm, scan time <30 seconds;

[0115] Automated microbial detection instrument: bioMérieux VITEK2 Compact, with a CV value of <5% for antimicrobial activity detection;

[0116] Online liquid volume detection: NIR-6000 near-infrared moisture meter, detection range 0-100%, repeatability ±0.2%.

[0117] Verification of the effectiveness of process parameter control:

[0118] The key parameters for 50 consecutive production batches are as follows:

[0119] Roll-off rate: set value 80%, actual value 79.8%-80.3%, standard deviation 0.18%, CPK=1.85;

[0120] Baking temperature: Set value 150°C, actual value 149.2-150.8°C, temperature difference ≤1.5°C, CPK=2.02;

[0121] Fermentation pH: Set value 6.6, actual value 6.58-6.62, fluctuation ±0.02, CPK=1.97;

[0122] Antibacterial rate after 30 washes: Staphylococcus aureus 98.5%±0.7%, Escherichia coli 97.8%±0.9%, batch-to-batch variation <3%.

[0123] A random forest regression model was built using Python 3.8:

[0124] Input variables: 18 parameters including steam explosion pressure, enzymatic hydrolysis pH, fermentation DO, crushing ratio, and roasting temperature;

[0125] Output variable: Antibacterial rate after 30 washes;

[0126] Model performance: R² = 0.93, MAE = 0.5%;

[0127] Optimization results: By using the Bayesian optimization algorithm, the antibacterial rate was increased from 98.2% to 99.1%, and energy consumption was reduced by 12%.

[0128] like Figure 7 As shown, this illustrates the hierarchical architecture from the central control system to each process unit:

[0129] The top layer is a central control system that communicates with each unit via ProfinetIRT industrial Ethernet.

[0130] The middle layer consists of four core process units: steam explosion, enzymatic hydrolysis, fermentation, and impregnation curing. Each unit is equipped with sensors, controllers, and actuators. The bottom layer is the MES data platform, which enables real-time acquisition and storage of process parameters. The diagram shows the model of all key equipment, the accuracy level of the sensors, and the closed-loop path of the control loop.

[0131] like Figure 8 As shown, the control principle is illustrated using the enzymatic hydrolysis process as an example: the signal flow starts from the set value pH=5.0, and the deviation is calculated by the comparator; the deviation value is input into the PID function block for calculation, and a 4-20mA signal is output; the metering pump frequency converter is driven by the AO module to realize the automatic addition of acid / alkali solution; the pH electrode detects the feedback value in real time, and a closed loop of "online monitoring-automatic adjustment-feedback control" is formed through the AI ​​module.

[0132] An antimicrobial finishing process based on Juncao fiber, using the Juncao fiber binary inclusion complex obtained from the above-mentioned antimicrobial finishing system as raw material, includes the following steps:

[0133] K1, specific pretreatment, cotton fabric is treated with overflow dyeing vat with a liquor ratio of 1:10, 20g / L NaOH is added and alkaline washing is carried out at 60rpm for 60min, followed by washing with 80°C hot water, and the pH is neutralized to 7.0 with 1g / L HCl, and then the acid solution is removed by rinsing with cold water.

[0134] Alkali washing and neutralization treatment increase the active sites on the fiber surface and improve the binding ability of inclusion complexes.

[0135] When processing nonwoven fabrics, the intelligent preprocessing module automatically switches to:

[0136] K1 is added with 10 g / L NaOH and washed with alkali at 80°C for 30 min, and 2 g / L quaternary ammonium salt accelerator is automatically added. The amount added is precisely controlled by a metering pump.

[0137] Quaternary ammonium salts, as accelerators, can increase the surface charge density of nonwoven fabrics, enhance their binding ability with binary inclusion complexes, and improve their antibacterial properties.

[0138] In K2, the padding and curing module, the padding solution is precisely prepared by mass parts using an automatic batching system, with each portion of padding solution prepared in L units according to mass parts:

[0139] 10 parts of binary inclusion compound raw material, 6 parts of butanetetracarboxylic acid, 4 parts of sodium hypophosphite, 0.1 parts of trisodium citrate, and the remainder is made up to 1L with deionized water;

[0140] K3 involves two dips and two nips of specially pretreated cotton fabric using a rolling mill, with a nip-to-liquid ratio of 80% each time. The fabric is then transferred to a hot air drying machine for 3 minutes of pre-drying at 80°C, followed by drying at 150°C for 3 minutes. After drying, the fabric is washed with 25°C deionized water and soaped for 10 minutes alternately. Finally, it is washed with 25°C deionized water and dried at 80°C until all moisture is removed, resulting in an antibacterial product with an antibacterial layer.

[0141] The fabric is alkali washed and neutralized through an intelligent pretreatment module, and the process parameters are monitored and automatically recorded in real time by online sensors.

[0142] The roll curing module performs two dips and two rolls, and the roll yield is fed back to the PLC in real time by an infrared detector to automatically adjust the roll pressure.

[0143] Pre-drying and curing are performed using a baking oven with independent PID temperature control in three zones, temperature difference <±1.5°C, and drying time is automatically timed by a photoelectric switch;

[0144] The amount of antibacterial ingredients adhered is verified by an online spectral detection system, and non-conforming products are automatically marked and sorted.

[0145] An antibacterial fabric based on antibacterial finishing of Juncao fiber is prepared using the above-mentioned antibacterial finishing process. It includes a base fabric layer and an antibacterial layer formed between the base fabric layers. The antibacterial layer is a binary inclusion complex coating formed by β-CD, flavonoid molecules and styraxin. The binary inclusion complex is combined with the fiber through chemical bonding and physical adsorption to form a stable antibacterial coating. Butanetetracarboxylic acid and sodium hypophosphite are used as crosslinking agents to enhance the binding force between the inclusion complex and the fiber.

[0146] Three control groups were designed to verify the performance of antimicrobial products, including their antimicrobial properties against common bacteria such as Staphylococcus aureus and Escherichia coli, as well as their wash resistance and mechanical properties.

[0147] Control group:

[0148] Control group 1: Untreated cotton fabric;

[0149] Control group 2: Cotton fabric treated with traditional antibacterial agents such as 0.5% triclosan;

[0150] Experimental group: Antibacterial products obtained using the process described in this embodiment;

[0151] Samples were randomly cut to 25x25cm size, and each sample was tested 3 times, and the average value was taken.

[0152] The antibacterial performance was tested using the shaking method according to GB / T20944.3-2008 standard.

[0153] Tested bacterial strains: Staphylococcus aureus (ATCC6538) and Escherichia coli (ATCC8739);

[0154] like Figure 1 As shown, control group 1 was untreated and had no antibacterial effect against Staphylococcus aureus and Escherichia coli, with an inhibition rate of 0%. Control group 2, which used traditional antibacterial agents, had an inhibition rate of 85% against Staphylococcus aureus and 70% against Escherichia coli, showing some antibacterial properties, but the antibacterial effect was limited.

[0155] The experimental group showed significantly better antibacterial performance against Staphylococcus aureus and Escherichia coli than traditional antibacterial agents. Levofloxacin disrupts the integrity of bacterial cell membranes by binding to the lipid bilayer, causing membrane rupture and leakage of intracellular substances, thereby inhibiting bacterial growth and reproduction. Levofloxacin's antibacterial effect is particularly pronounced against Gram-positive bacteria, such as Staphylococcus aureus, because the cell walls of Gram-positive bacteria are thinner and more easily destroyed by levofloxacin. Flavonoid molecules can bind to the enzyme systems within bacterial cells, inhibiting their metabolic activities and thus preventing bacterial growth. Flavonoid molecules also have antioxidant properties, scavenging reactive oxygen species (ROS) within bacterial cells. S further inhibits bacterial survival. PHMG is a cationic antibacterial agent that can bind to the negatively charged groups on the bacterial cell membrane, destroying the integrity of the cell membrane and leading to bacterial death. The cationic nature of PHMG allows it to bind firmly to the fiber surface, providing a long-lasting antibacterial effect. The synergistic effect of squalene, flavonoid molecules and PHMG significantly improves the antibacterial performance. Squalene and flavonoid molecules destroy the cell membrane and inhibit metabolic activities, while PHMG further enhances the antibacterial effect through cationic action. The binary inclusion complex structure allows squalene and flavonoid molecules to form a stable coating on the fiber surface, enhancing the stability and release efficiency of the antibacterial components.

[0156] The wash resistance test method adopts the washing test according to GB / T8629-2017 standard. Each wash is 30 minutes and the rinse is 3 minutes. The antibacterial performance is tested after every 5 washes. The antibacterial performance is still tested by the shaking method according to GB / T20944.3-2008 standard. The average antibacterial performance against Staphylococcus aureus and Escherichia coli is recorded. A total of 6 tests are conducted (0, 5, 10, 15, 20, and 30 times).

[0157] like Figure 2As shown, control group 1 had no antibacterial properties and showed no change after multiple washes. Control group 2, using a traditional antibacterial agent, showed a gradual decrease in antibacterial performance after multiple washes, dropping below 15% after 30 washes. In contrast, the antibacterial rate of the experimental group remained at least 97%, demonstrating excellent wash resistance. This is mainly due to the binary inclusion complex being firmly bound to the fiber surface through chemical bonding and physical adsorption, forming a stable antibacterial coating. Butanetetracarboxylic acid and sodium hypophosphite, acting as crosslinking agents, enhanced the binding force between the inclusion complex and the fiber, allowing the antibacterial components to maintain high activity even after multiple washes. The chitosan coating process enhanced the stability and release efficiency of the antibacterial components. The high specific surface area and porous structure of the coating facilitated the uniform distribution and slow release of the antibacterial components, thus maintaining high antibacterial performance even after multiple washes. The structure of the binary inclusion complex enabled the antibacterial components to form a slow-release system on the fiber surface. By controlling the release rate of the antibacterial components, high antibacterial activity was maintained even after multiple washes. The slow-release mechanism not only extended the shelf life of the antibacterial components but also reduced the loss of antibacterial components during the washing process.

[0158] It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above, and that the invention can be implemented in other specific forms without departing from its spirit or essential characteristics. Therefore, the embodiments should be considered in all respects as exemplary and non-limiting, and the scope of the invention is defined by the appended claims rather than the foregoing description. Thus, all variations falling within the meaning and scope of equivalents of the claims are intended to be included within the present invention. No reference numerals in the claims should be construed as limiting the scope of the claims.

[0159] Furthermore, it should be understood that although this specification describes embodiments, not every embodiment contains only one independent technical solution. This narrative style is merely for clarity. Those skilled in the art should consider the specification as a whole, and the technical solutions in each embodiment can also be appropriately combined to form other embodiments that can be understood by those skilled in the art.

Claims

1. An antibacterial finishing system based on Juncao fiber, characterized in that, Includes the following automated control modules: Intelligent pretreatment module: The fabric is treated by overflow dyeing tank. The dyeing tank is equipped with liquid level sensor and online pH meter. The alkaline washing solution is automatically prepared at a liquor ratio of 1:

10. After alkaline washing, the neutralization endpoint is monitored in real time by pH sensor. The acid pump is automatically controlled to shut off when pH=7.0±0.

1. Impregnation and curing module: The rolling mill is equipped with pressure sensors and liquid volume infrared detectors, and the liquid rate is automatically adjusted to 80%±1.5% during the two-impregnation and two-rolling process through PLC control; the hot air baking machine adopts three-zone independent temperature control, and achieves precise drying at 150°C±1.5°C through thermocouple feedback; Intelligent preparation unit for bioactive substances: The extraction process is automated by a DCS system through a steam explosion-enzymatic hydrolysis-subcritical water extraction combined device, equipped with a pressure transmitter, temperature sensor and online pH meter, and the fermentation yield of lecithin is optimized by model predictive control algorithm. Central control system: Each module is connected via an industrial bus, and process parameters are uploaded to the MES system in real time, supporting remote monitoring and process traceability; The intelligent preparation unit for bioactive substances includes the following steps: 60 parts by weight of Ganoderma lucidum and 40 parts by weight of Cordyceps militaris were dried and sliced, and then loaded into a rupture vessel with a loading coefficient of 0.

7. Saturated steam of 1.8±0.02MPa was introduced. The rupture vessel was equipped with pressure and temperature sensors, and the data was uploaded to the PLC. When the pressure deviation was >0.02MPa, the opening of the steam valve was automatically adjusted. After blasting, the material was added to deionized water at a weight-to-volume ratio of 1:8, and the pH was automatically adjusted to 5.0±0.05 using an online pH meter. A compound enzyme was added and enzymatically hydrolyzed at 50°C±0.5°C for 2.5 hours. After enzymatic hydrolysis, the enzyme was inactivated by heating. The enzymatic hydrolysis product and Serratia marcescens cells were added to a subcritical water extraction reactor at a mass ratio of 1000:

8. The temperature was increased to 135°C at 3°C / min, and the pressure was increased to 6.0MPa at 0.1MPa / min. Flavonoid molecules, polysaccharide molecules, and microfibrillated cellulose were obtained by membrane separation. The intelligent preparation unit for bioactive substances also includes: The fermenter is equipped with a dissolved oxygen sensor and a pH electrode, and three-stage fermentation is achieved through PID closed-loop control: During the first stage (0-24 hours), maintain pH 7.0 ± 0.05 and DO 30% ± 2%. During the second stage (24-48 hours), maintain pH 6.6±0.05 and DO 25%±2%, and automatically replenish 1% glycerol. In the third stage (48-72 hours), the chitosan solution is automatically added via a peristaltic pump, and the addition rate is uniformly completed within 30 minutes. After fermentation, the fermentation broth was sterilized by passing it through a 0.22μm ceramic membrane. β-CD was then added and the inclusion reaction was carried out at 60°C±2°C for 12 hours under nitrogen protection. Finally, the binary inclusion complex of Juncao fiber was obtained by spray drying.

2. The antibacterial finishing system based on Juncao fiber according to claim 1, characterized in that, In the pad-curing module, the pad-forming solution is precisely prepared by weight using an automatic batching system: The mixture consists of 10 parts of binary inclusion compound raw material, 6 parts of butanetetracarboxylic acid, 4 parts of sodium hypophosphite, and 0.1 parts of trisodium citrate, with a mixing accuracy of ±0.5%. The stirring speed is 60 rpm and controlled by a frequency converter.

3. The antibacterial finishing system based on Juncao fiber according to claim 2, characterized in that, When processing nonwoven fabrics, the intelligent preprocessing module automatically switches to: Add 10 g / L NaOH and wash at 80°C for 30 min, and automatically add 2 g / L quaternary ammonium salt accelerator. The amount added is precisely controlled by a metering pump.

4. An antimicrobial finishing process based on Juncao fiber, implemented using the antimicrobial finishing system based on Juncao fiber as described in any one of claims 1-3, characterized in that, Includes the following steps: The fabric is alkali washed and neutralized through an intelligent pretreatment module, and the process parameters are monitored and automatically recorded in real time by online sensors. The roll curing module performs two dips and two rolls, and the roll yield is fed back to the PLC in real time by an infrared detector to automatically adjust the roll pressure. Pre-drying and curing are performed using a baking oven with independent PID temperature control in three zones, temperature difference <±1.5°C, and drying time is automatically timed by a photoelectric switch; The amount of antibacterial ingredients adhered is verified by an online spectral detection system, and non-conforming products are automatically marked and sorted.

5. An antibacterial fabric based on antibacterial finishing of Juncao fiber, characterized in that, The antibacterial finishing process described in claim 4 is used to prepare the product, which includes a base fabric layer and an antibacterial layer formed between the base fabric layers. The antibacterial layer is a binary inclusion complex coating formed by β-CD, flavonoid molecules and styraxin.

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