A process optimization scheme for wrapping adsorbing pellitory extract with porous ceramic balls adapted to pillow sachet fillers

Abstract

This invention relates to an optimized process for encapsulating and adsorbing Eupatorium fortunei extract using porous ceramic balls in pillow fillings, belonging to the field of functional home textile materials technology. It aims to solve the problems of imbalance between pillow feel and adsorption, uncontrolled slow release, and safety deficiencies associated with traditional processes. Key technical points: Select ceramic balls with a porosity of 2-3mm and 50-55%, and activate them with sodium bicarbonate; air-dry Eupatorium fortunei stems and leaves in a 3:1 ratio, ultrasonically extract with 95% ethanol at a 1:25 ratio, and concentrate under reduced pressure; adsorb the concentrate using ceramic balls at a 1:2 ratio, and encapsulate with beeswax solution at a 1:0.8 ratio; after sieving, allow to air dry, and prepare 80-count cotton / linen filling bags (4 zones, 30-35g / 100cm²). This process produces a filling with a slow release of 6-8 hours (concentration 0.1-0.3mg / m³), with solvent residue ≤0.01mg / kg, primarily for use in sleep-aid pillows, improving comfort and safety.

Description

Technical Field

[0001] This invention belongs to the field of functional home textile materials technology, specifically involving an optimized process for encapsulating and adsorbing agastache extract in porous ceramic balls suitable for pillow pouch fillings. The process includes the design of all parameters of the process, the optimized filling characteristics, and its application in sleep-aid pillows. It focuses on solving the technical problems of "uncontrolled slow release, insufficient safety, and poor pillow feel" in traditional processes. Background Technology

[0002] Perrin ( Eupatorium fortunei Turcz. volatile oil contains active ingredients such as eucalyptol and nerol acetate, which have calming and sleep-improving effects, and are often used as a core functional ingredient in functional pillow fillings. Porous ceramic balls, due to their large specific surface area and high mechanical strength, have become the mainstream carrier for Eupatorium fortunei volatile oil. However, the traditional process of encapsulating and adsorbing Eupatorium fortunei extract with porous ceramic balls has the following core defects, making it difficult to adapt to the close-fitting use of pillows: 1. The pretreatment parameters of ceramic balls are too crude, resulting in an imbalance between pillow feel and adsorption capacity: Traditional processes use ceramic balls with a general particle size of 1-5mm and a porosity controlled at 40-60%. Particles <2mm are prone to leakage into the sac, causing respiratory discomfort; particles >3mm result in a hard pillow feel and poor scalp comfort; when the porosity is <50%, the adsorption capacity is insufficient (<0.1mg per gram), and when it is >55%, the ceramic balls are prone to pulverization (pulverization rate exceeds 15% within 6 months), making it impossible to balance "adsorption capacity" and "pillow feel durability".

[0003] 2. The extraction process of Eupatorium fortunei has high losses and fails to meet safety standards: The traditional method uses a mixed solvent of ethyl acetate and ethanol (high risk of residue), high-temperature ultrasound at 50-80℃ (15% decomposition rate of heat-sensitive components), and concentration at 70℃ and normal pressure (retention rate of volatile oil <85%), resulting in solvent residue in the final product exceeding 0.05mg / kg (5 times the standard). In addition, Eupatorium fortunei has a bitter odor and a skin irritation rate of 8%, which does not meet the safety standards for intimate apparel in GB 4806.1-2016.

[0004] 3. Uncontrolled adsorption and slow-release cycle do not match sleep requirements: Traditional adsorption processes have large fluctuations in the solid-liquid ratio (1:1-4), lack ultrasonic assistance or full-process ultrasonication (the former results in uneven adsorption, the latter in 20% evaporation loss), and the encapsulation material is mostly sodium carboxymethyl cellulose (which is prone to moisture absorption and clumping). This leads to an initial burst of release of the volatile oil of Perilla frutescens (concentration >0.5mg / m³ in 0-2 hours, pungent smell) and rapid decay in the later stage (concentration <0.05mg / m³ after 4 hours, ineffective), which cannot match the 6-8 hour sleep cycle.

[0005] 4. Poor compatibility between the pouch and the filling, resulting in a poor user experience: Traditional pouches use ordinary cotton fabric (air permeability <100mm / s, hindering the release of volatile oils), have no zoning design (the clay balls pile up on one side, resulting in uneven pillow feel), and the filling amount is controlled by experience (20-40g per 100cm²), which leads to insufficient loft (compression rebound rate <75%) or poor support, further exacerbating the imbalance of slow release.

[0006] Therefore, designing a process optimization scheme that "precisely optimizes ceramic ball parameters, ensures safe extraction processes, controls encapsulation and adsorption, and synergistically adapts the sac to the product" has become the key to solving the pain points of traditional processes and promoting the industrialization of Peilan functional pillows. Summary of the Invention

[0007] I. Technical problems to be solved This invention aims to overcome the shortcomings of traditional porous ceramic ball encapsulation and adsorption processes for Eupatorium fortunei extract, such as "imbalance between pillow feel and adsorption, poor safety, uncontrolled sustained release, and poor capsule fit," and achieves the following objectives: 1. Ceramic ball parameters suitable for pillow scenarios: particle size 2-3mm, porosity 50-55%, balancing "0.15-0.2mg adsorption per gram" and "no pulverization for 6 months"; 2. Perilla extract is safe and efficient: solvent residue ≤0.01mg / kg, heat-sensitive component retention rate ≥95%, mild odor and no off-odor; 3. Slow-release cycle precisely matched to sleep: stable release over 6-8 hours, concentration 0.1-0.3mg / m³, with no burst release or premature decay; 4. Synergistic effect of pouch and filling: air permeability ≥150mm / s, compression rebound rate after filling ≥85%, and uniform and comfortable pillow feel.

[0008] II. Technical Solution This solution optimizes the process through five steps: "pretreatment of ceramic balls → extraction of agastache rugosa → encapsulation and adsorption → post-treatment → capsule adaptation," forming a fully controllable technical system, as detailed below: (I) Optimization of pretreatment process for porous ceramic balls (optimization of core carrier):

[0009] Select spherical porous ceramic balls with a particle size of 2-3 mm and a porosity of 50-55% (purchased from Yixing Ceramics Factory, model TC-23). ​​Detect the particle size distribution (D50=2.5 ​​mm) using a laser particle size analyzer and the porosity (52.3%) using a mercury porosimeter. Ensure a specific surface area of ​​28-32 m² / g (to meet adsorption requirements) and a compressive strength ≥1.2 MPa (to prevent pulverization).

[0010] 2. Cleaning and sterilization process: Step 1: Ultrasonic cleaning with 300W deionized water for 20 minutes (frequency 40kHz) to remove dust from the surface of the ceramic balls (dust removal rate ≥98%, preventing dust from being stirred up during sleep). Step 2: Soak in boiling water for 30 minutes (100℃, 100% sterilization rate, eliminates microorganisms in pores, and avoids odors). Step 3: Dry at 80℃ for 2 hours with forced air, controlling the moisture content to ≤2% (avoid over-drying to prevent shrinkage of the ceramic ball structure).

[0011] 3. Mild activation process: Instead of using traditional strong alkaline sodium hydroxide, a 0.5 mol / L sodium bicarbonate solution (pH 8.0-8.5) was used for activation at 50℃ for 40 minutes (water bath temperature control, temperature difference ±1℃). The weakly alkaline solution gently etched the pore walls of the ceramic balls, forming "hydrophobic microchannels" (slowing down the release of volatile oils). After activation, the balls were rinsed with deionized water until the pH reached 6.8-7.2 (neutral, no skin irritation), and then dried at 80℃ for 3 hours to obtain pretreated ceramic balls. (II) Optimization of the extraction process of Perilla frutescens volatile oil (optimization of core functional components):

[0012] Select the above-ground parts of the current year's Eupatorium fortunei (from Bozhou Medicinal Materials Market, Anhui Province, batch number 202503), mix them with stems and leaves in a ratio of 3:1, and air-dry them naturally in the shade (25℃, 40% RH, to avoid loss of volatile oils due to high temperature from direct sunlight). After pulverizing them with a high-speed pulverizer, pass them through a 60-mesh sieve (sieve aperture 0.25mm, powder uniformity ≥90%, to ensure full contact with solvent).

[0013] 2. Ultrasonic extraction parameters: Solvent: 95% food-grade ethanol (compliant with GB 1886.187-2021, high safety, volatile oil solubility 1.8g / 100mL, 15% higher than traditional mixed solvents); Solid-liquid ratio: 1:25 (g:mL) (Eupatorium fortunei powder: ethanol; verified by single-factor experiments, the extract concentration is stable at 5-6 mg / mL under this ratio, with no excess residue during adsorption). Ultrasonic conditions: 45℃ (constant temperature water bath), 300W (power density 0.5W / cm²), 60 minutes (extraction time), decomposition rate of heat-sensitive component (neroli acetate) <5% (HPLC detection, retention time 8.2min, peak area ratio ≥12%).

[0014] 3. Reduced pressure concentration process: A rotary evaporator was used to concentrate the volatile oil at 45℃ and -0.09MPa (vacuum fluctuation ±0.005MPa) to remove 75% ethanol. The solid content of the concentrate was controlled at 25% (detected by refractometer), and the volatile oil retention rate was ≥95% (detected by GC-MS, total peak area loss <5%), to obtain a concentrated volatile oil of Perilla frutescens (purity ≥90%). (III) Optimization of Encapsulation and Adsorption Process (Core of Precision Sustained Release): Mixed (250mL three-necked flask, stirrer speed 150r / min), the adsorption rate reached 94% at this ratio (measured by UV spectrophotometer, absorbance change rate at 283nm). Ultrasonic assistance: Only turn on 300W ultrasound in the initial adsorption stage (0-30 minutes) (to promote the penetration of volatile oil into the deep pores of the ceramic ball, forming a gradient adsorption structure of "surface layer - transition layer - core layer". The surface layer is responsible for the release in the first 2 hours, and the deep layer is responsible for the release in the last 6 hours). After that, turn off the ultrasound (to avoid volatilization loss, the volatilization loss rate is <5%). Adsorption time: 2.5 hours (adsorption equilibrium time, after which the concentration of the concentrate no longer decreases as determined by HPLC). (Complies with GB 1886.87-2015, melting point 62-64℃, good biocompatibility, non-irritating), melt in a 70℃ water bath (just dissolves, prevents high temperature from damaging volatile oils), add 95% ethanol to make a 5% beeswax-ethanol solution (ethanol is volatile and leaves no residue); Stir at low speed for 30 minutes at 30℃ (80r / min to avoid damaging the ceramic balls), and let it cool naturally to 25℃ (to prevent the loss of volatile oils due to heating). A 0.5-1μm thick beeswax coating layer will form on the surface of the ceramic balls (scanning electron microscopy shows that the thickness uniformity is ≥90%). This coating layer softens and releases oil at 33-35℃ (scalp temperature) and hardens and retains oil at 20-25℃ (room temperature), achieving temperature-responsive slow release. (iv) Post-process optimization (safety and filling compatibility):

[0015] A double-layer stainless steel sieve (3mm upper layer, 2mm lower layer) is used. First, the 3mm sieve removes oversized particles (to prevent hardening), then the 2mm sieve removes undersized particles / powder (to prevent leakage). Finally, broken ceramic balls are manually removed (breakage rate <1%). The qualified rate of ceramic balls after sieving is ≥99%.

[0016] 2. Natural ventilation and drying: Instead of traditional high-temperature drying, natural ventilation drying at 25℃ and 40-50% RH for 48 hours (controlled by a constant temperature and humidity chamber) was adopted, with moisture content controlled at ≤3% (detected by Karl Fischer moisture analyzer) and ethanol residue at ≤0.01mg / kg (GC detection, DB-624 column, FID detector).

[0017] 3. Safety and odor testing: pH test: Soak 10g of ceramic balls in 100mL of deionized water for 24 hours. The pH of the soaking solution was measured to be 6.8-7.2 (neutral, meeting the standards for close-fitting products). Odor blind test: 20 volunteers aged 25-55 (10 men and 10 women) were placed in a 25℃ closed space (10m³) with 50g of ceramic balls. The rating scale was 1-5 points (1 = pungent, 5 = mild). " Mild and odorless" (score ≥4 points) had a satisfaction rate of ≥90%. (V) Pillowcase Fitting Design (Scenario Implementation Optimization):

[0018] It uses 80-count cotton-linen blended fabric (70% cotton, 30% linen), with an air permeability of ≥150mm / s as tested by an air permeability meter (to ensure the release of volatile oils), no pilling after 500 cycles of abrasion test by a Martindale abrasion tester (to prevent the leakage of ceramic powder), and a wash fastness of ≥4 grade (GB / T 3921-2008).

[0019] 2. Structural and infill design: Pocket specifications: Fits 40cm×60cm pillows, the interior is divided into 3-4 independent sections (20cm×20cm / section, to prevent the accumulation of clay balls), and the sections are sewn together with 1cm wide cotton thread (tensile strength ≥5N). Filling amount: 30-35g of optimized ceramic balls per 100cm² (passed pillow feel test, compression rebound rate ≥85% (GB / T 26706-2011) at this filling amount, balancing support and fluffiness); Usage cycle: It is recommended to replace it every 6 months (accelerated aging test: after 6 months, the residual volatile oil of Perilla is ≤20%, the peak area ratio detected by GC-MS is <2%, and the sleep aid effect is ineffective). Before replacement, ventilating and sun-drying at 25℃ for 2 hours can temporarily restore the scent.

[0020] III. Beneficial Effects Compared with traditional processes, this optimized solution has the following significant advantages: 1. Balance between pillow comfort and adsorption: 2-3mm ceramic balls + 50-55% porosity, no pulverization after 6 months, adsorbs 0.15-0.2mg of volatile oil per gram, which is 50% higher than the traditional process, and the pillow comfort score (out of 10) reaches 8.5 points; 2. Safety meets standards: 95% food-grade ethanol + 45℃ low-temperature process, solvent residue ≤0.01mg / kg, skin irritation rate 0%, mild odor with a satisfaction rate ≥90%, fully compliant with intimate apparel standards; 3. Precise sustained release: Gradient adsorption + beeswax coating, stable release for 6-8 hours, concentration 0.1-0.3mg / m³, no burst release or premature decay, matching the needs of sleep cycles; 4. High feasibility: Using conventional equipment such as ultrasonic instruments and rotary evaporators, the pouches are adapted to existing pillow sizes, and a single production line can produce 100,000 grams of filling material per day, reducing costs by 15% compared to traditional processes (increased pass rate + reduced waste). Attached Figure Description

[0021] Figure 1: Flow chart of the process for encapsulating and adsorbing Eupatorium extract with porous ceramic balls adapted to pillow pouches; 1. Label each step as “1. Pretreatment of ceramic balls → 2. Eupatorium extract → 3. Encapsulation and adsorption → 4. Post-treatment → 5. Encapsulation and bag filling”, and label key parameters (such as ceramic ball particle size, solid-liquid ratio, drying conditions) next to each step. Use arrows to connect each process to ensure logical coherence. Figure 2: Scanning electron microscope image of the pretreated porous ceramic balls (500x magnification); 1. Label the surface pores of the ceramic ball (5-10μm) and the hydrophobic microchannels. The scale bar (10μm) is marked on the right to show the pore structure after activation. Figure 3: Schematic diagram of the assembly of the sleep aid pillow's sac and filling; 1. Label the bag as “80 count cotton and linen blend bag”, “independent filling area (4)”, and “porous ceramic ball filling”. The size is labeled as “40cm×60cm” to show the partitioned filling structure. Detailed Implementation

[0022] The effectiveness of this solution is verified through examples and comparative examples. The raw materials and equipment used are all commercially available conventional products, and the testing methods comply with national standards.

[0023] 1. Example 1: Optimized process for preparing porous ceramic balls encapsulating and adsorbing Eupatorium fortunei extract filler Pretreatment of ceramic balls: Take 100g of ceramic balls with a particle size of 2-3mm and a porosity of 52%, ultrasonically clean them at 300W for 20 minutes, soak them in boiling water for 30 minutes, and dry them at 80℃ until the moisture content is 1.8%; immerse them in 0.5mol / L sodium bicarbonate solution (pH 8.2), activate them at 50℃ for 40 minutes, rinse them until the pH is 7.0, and dry them at 80℃ for 3 hours to obtain 98g of pretreated ceramic balls (yield 98%).

[0024] Eupatorium extract: Eupatorium stems and leaves (300g stems, 100g leaves) were dried in the shade, pulverized and passed through a 60-mesh sieve, 10L of 95% ethanol was added, and the mixture was sonicated at 45℃ and 300W for 60 minutes. The mixture was then concentrated at 45℃ and -0.09MPa to a solid content of 25%, yielding 400mL of concentrated solution (volatile oil purity 91.5%, yield 1.4%).

[0025] Encapsulation and adsorption: 98g of pretreated ceramic balls were mixed with 196mL of concentrated solution (1:2), stirred at 30℃ and 150r / min, and ultrasonically assisted for the first 30 minutes. After 2.5 hours, 78.4g of 5% beeswax-ethanol solution (1:0.8) was added, stirred at 30℃ for 30 minutes, and then cooled to 25℃.

[0026] Post-processing: After double-layer sieving, 97g of qualified ceramic balls were obtained (qualification rate 99%). They were dried at 25℃ for 48 hours with a moisture content of 2.5%, ethanol residue of 0.008mg / kg, pH 6.9, and a blind odor test satisfaction rate of 95%.

[0027] 2. Example 2: Preparation of a sleep-aid pillow with optimized filling Bag preparation: 40cm×60cm bags are sewn from 80-count cotton-linen blend fabric, divided into 4 independent 20cm×20cm sections.

[0028] Filling assembly: Each area is filled with 35g of the filler from Example 1, for a total of 140g. After encapsulation, the pillow has a compression resilience of 88% and an air permeability of 155mm / s.

[0029] 3. Example 3: Performance Testing (Laboratory + User Verification) Sustained-release performance (35℃ constant temperature oven, GC-MS detection):

[0030] User test (30 volunteers with difficulty falling asleep, aged 18-55): After using the pillow from Example 2 for 14 consecutive days, the results were as follows: Objective indicators: time to fall asleep decreased from 38 minutes to 18 minutes (-52.6%), and the number of awakenings during the night decreased from 2.5 times to 0.8 times (-68%). Subjective feedback: Pillow comfort score 8.6, odor satisfaction 93%, 0 cases of skin discomfort.

[0031] 4. Comparative Example: Filler prepared using traditional methods (control group) Process parameters: ceramic balls with a particle size of 1-5 mm and a porosity of 45%, activated with sodium hydroxide, using ethyl acetate-ethanol mixed solvent, ultrasonicated at 55℃, concentrated at 70℃, coated with sodium carboxymethyl cellulose, without sieving, and dried at 60℃.

[0032] Performance comparison:

[0033] In summary, this optimized process solution is significantly superior to traditional processes in terms of adsorption capacity, safety, sustained release period, and user experience, and is fully adapted to the usage requirements of pillow pouch fillings.

Claims

1. A process for encapsulating and adsorbing Eupatorium fortunei extract using porous ceramic balls adapted to pillowcase fillings, characterized in that, Includes the following steps: (1) Pretreatment of porous ceramic balls: Select spherical porous ceramic balls with a particle size of 2-3 mm and a porosity of 50-55%, and clean them sequentially with 300W deionized water for 20 minutes, soak them in boiling water for 30 minutes, and dry them at 80℃ until the moisture content is ≤2%; immerse the dried ceramic balls in 0.5 mol / L sodium bicarbonate solution (pH 8.0-8.5), activate them at 50℃ for 40 minutes, rinse them until the pH is 6.8-7.2, and dry them at 80℃ for 3 hours to obtain pretreated porous ceramic balls; (2) Extraction of Eupatorium fortunei volatile oil: Take the stems and leaves of Eupatorium fortunei from the current year (stem:leaf = 3:1), air dry naturally, crush and pass through a 60-mesh sieve, mix with 95% food grade ethanol at a solid-liquid ratio of 1:25, extract by ultrasonication at 45℃ and 300W for 60 minutes, and concentrate under reduced pressure at 45℃ and -0.09MPa to a solid content of 25% to obtain concentrated Eupatorium fortunei volatile oil (purity ≥90%). (3) Encapsulation and adsorption: The pretreated porous ceramic balls and the concentrated volatile oil of Eupatorium fortunei were mixed at a solid-liquid ratio of 1:2 and stirred at 30°C and 150r / min for 2.5 hours (with 300W ultrasonic assistance for the first 30 minutes); Food-grade beeswax with a purity of ≥99% was melted at 70°C and then mixed with 95% ethanol to make a 5% beeswax-ethanol solution. The solution was added to the adsorption system at a mass ratio of ceramic balls:solution = 1:0.8 and stirred at low speed at 30°C for 30 minutes, and then naturally cooled to 25°C. (4) Post-processing: The product from step (3) is sieved through a 3mm sieve and a 2mm sieve in sequence. Damaged ceramic balls are manually removed. The product is then naturally dried at 25℃ and 40-50% RH for 48 hours until the moisture content is ≤3%, resulting in a porous ceramic ball-encapsulated filling material for adsorbing Eupatorium extract that is suitable for pillow pouches.

2. The process according to claim 1, characterized in that, The specific surface area of ​​the pretreated porous ceramic balls in step (1) is 28-32 m² / g, and the adsorption capacity of each gram of ceramic ball for the volatile oil of Eupatorium fortunei is 0.15-0.2 mg.

3. The process according to claim 1, characterized in that, In step (2), the yield of the concentrated volatile oil of Eupatorium fortunei was 1.2-1.5%, and the retention rate of heat-sensitive components such as neroli acetate was ≥95% as detected by high performance liquid chromatography (HPLC).

4. The process according to claim 1, characterized in that, In step (3), the ultrasonic-assisted adsorption power is 300W and the duration is 15 minutes, which is used to promote the penetration of the volatile oil of Perilla into the deep pores of the ceramic ball to form a gradient adsorption structure of "surface layer - transition layer - core layer".

5. The process according to claim 1, characterized in that, In step (3), the ethanol concentration of the beeswax-ethanol solution is 95%. After coating, a beeswax coating layer with a thickness of 0.5-1μm is formed on the surface of the ceramic ball. The coating layer softens and releases oil at 33-35℃ and hardens and retains oil at 20-25℃.

6. The process according to claim 1, characterized in that, The pass rate of the sieved ceramic balls in step (4) is ≥99%, and the residual ethanol content is ≤0.01mg / kg as detected by gas chromatography (GC).

7. The process according to claim 1, characterized in that, In step (4), the dried ceramic balls were soaked in 10g of water for 24 hours. The pH of the soaking solution was 6.8-7.2, which met the requirements of GB 4806.1-2016 "General Safety Requirements for Food Contact Materials and Articles".

8. The process according to claim 1, characterized in that, In step (4), the dried ceramic balls need to be subjected to a blind odor test: 20 volunteers aged 25-55 rated the balls, with a satisfaction rate of ≥90% for "mild and odorless" and no bitter, pungent or other abnormal odors.

9. A porous ceramic ball-encapsulated filling material for adsorbing agrimony extract, adapted for use in pillowcases, characterized in that... The filler is prepared by any one of the processes described in claims 1-8; under conditions of 33-35℃, the release cycle of the volatile oil from the filler is 6-8 hours, with a release amount of 0.04-0.05 mg / h in 0-2 hours, 0.03-0.04 mg / h in 2-6 hours, and 0.02-0.03 mg / h in 6-8 hours, and the concentration is stable at 0.1-0.3 mg / m³.

10. A sleep-aid pillow containing porous ceramic balls encapsulating a filling of agastache extract, characterized in that, It includes 80 cotton-linen blended pouches (air permeability ≥150mm / s, no pilling after 500 rubs) and the filling material as described in claim 9; the pouches are suitable for 40cm×60cm pillows, and the interior is divided into 3-4 independent areas, each area is filled with 30-35g of filling material per 100cm², and the pillow compression resilience after filling is ≥85%.

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