Camellia oil fiber and preparation method thereof

By preparing camellia oil microcapsules and blending them with viscose liquid, the problem of low retention and utilization of camellia oil in viscose fibers was solved, achieving efficient preparation of functional cellulose fibers with good antibacterial and antioxidant properties.

CN121896743APending Publication Date: 2026-04-21YIBIN SPARK NEW FIBER CO LTD
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
YIBIN SPARK NEW FIBER CO LTD
Filing Date
2024-10-18
Publication Date
2026-04-21

AI Technical Summary

Technical Problem

Existing technologies are insufficient to effectively increase the retention and utilization rate of camellia oil in viscose fibers while maintaining the spinnability and functionality of the fibers.

Method used

Camellia oil was prepared into microcapsules and blended with a viscose solution. Through specific dispersants, emulsifiers and gelling agents, a stable spinning solution was formed. After spinning, coagulation and curing processes, camellia oil fiber was finally prepared.

Benefits of technology

It increases the retention of camellia oil in viscose fibers, enhances the fibers' antibacterial, antioxidant, and free radical scavenging properties, and the preparation method is easy to operate.

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Abstract

The invention provides a camellia oil fiber and a preparation method thereof, and belongs to the field of functional cellulose fiber preparation. Wherein the camellia oil is prepared into microcapsules, then the microcapsules are prepared into dispersion liquid, the dispersion liquid is blended with a viscose spinning solution, and finally, the degradable camellia oil fibers which have the characteristics of regenerated fibers, the content of the camellia oil component in the camellia oil fibers is ensured, and the camellia oil fibers are endowed with good functions of resisting oxidation, scavenging free radicals and the like; therefore, the requirements and choices of people on functional cellulose fibers are met.
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Description

Technical Field

[0001] This invention relates to a camellia oil fiber and its preparation method, belonging to the field of functional cellulose fiber preparation. Background Technology

[0002] Camellia oil is obtained from the seeds of the Camellia oleifera Abel tree (family Camelliaceae). It is one of the oldest woody edible plant oils in China. Camellia oleifera trees generally grow in the subtropical humid climate zone of the Nanling Mountains. The entire growth process involves almost no pesticides or fertilizers. The latitude, longitude, soil, and climate are suitable, resulting in high nutritional content and no harmful substances such as erucic acid, cholesterol, or aflatoxin. Furthermore, camellia oil contains more than 90% unsaturated fatty acids, with oleic acid content of 80-83% and linoleic acid content of 7-13%.

[0003] Regenerated cellulose fiber is made from natural cellulose (cotton, hemp, bamboo, trees, shrubs, etc.) as raw material. Its chemical structure is not altered; only the physical structure of the natural cellulose is changed to produce regenerated cellulose fiber with better performance. The presence of active hydroxyl groups on the cellulose molecule allows regenerated cellulose fiber to be grafted and copolymerized with many other functional molecules during production, undergoing combination modification.

[0004] However, ensuring the effective retention of functional molecules, improving their utilization rate, and maintaining the spinnability and ease of operation of the fiber are urgent technical problems that need to be solved. Although existing technologies "CN110396729A - A High Moisturizing Health Regenerated Cellulose Fiber and Its Preparation Method" and "CN114182380A - A Tea Tree Oil Antibacterial Health Cellulose Fiber and Its Preparation Method" disclose camellia oil fiber, CN110396729A directly uses a spinning process without preparing microcapsules, thus failing to improve the purity and addition amount of camellia oil; CN114182380A uses tea tree oil, collagen, and titanium dioxide as active ingredients to prepare an antibacterial cellulose fiber, but this method does not involve cross-linking tea tree oil and collagen, resulting in a high content that is lost. Summary of the Invention

[0005] This invention aims to improve the retention of camellia oil in viscose fibers, i.e., to increase the utilization rate of camellia oil and viscose liquid, by proposing a camellia oil fiber and its preparation method. Camellia oil is prepared into microcapsules, then formulated into a dispersion and blended with viscose liquid. The resulting biodegradable camellia oil fiber not only possesses the characteristics of regenerated fibers but also ensures the presence of sufficient camellia oil content. Furthermore, it endows the camellia oil fiber with excellent antioxidant and free radical scavenging functions, thus meeting the demand and selection criteria for functional cellulose fibers.

[0006] To achieve the above technical objectives, the following technical solution is proposed:

[0007] The primary objective of this technical solution is to provide: a camellia oil fiber, which is made from camellia oil microcapsules and viscose liquid as raw materials through blending, spinning, coagulation, curing and post-treatment;

[0008] The finished product indicators of the camellia oil fiber include: Candida albicans ≥85.0%, Escherichia coli ≥90.0%, Staphylococcus aureus ≥90.0%, free radical scavenging ≥40%; dry breaking strength ≥2.10 cN / dtex, strength >2.08 dtex, wet breaking strength ≥1.00 cN / dtex, dry breaking elongation 17±4.5%, residual sulfur ≤20mg / 100g, defects ≤4mg / 100g, oily yellow fibers ≤1mg / 100g, and dry breaking strength coefficient of variation CV ≤20%.

[0009] Furthermore, the camellia oil microcapsules contain ≥50% camellia oil, have a particle size ≤10μm, and contain 50-90% camellia oil microcapsules with a particle size of 4-7μm; the camellia oil microcapsules are either powdered or granular. They are commercially available.

[0010] Furthermore, the cellulose content in the adhesive liquid is 89–94 g / L.

[0011] Furthermore, the weight ratio of the camellia oil microcapsules to the adhesive liquid is 10-20:80-90.

[0012] The second objective of this technical solution is to provide a method for preparing camellia oil fiber, comprising the following steps:

[0013] Preparation of S1 Camellia Oil Microcapsules

[0014] S1.1 Dissolve gelatin, alginate and β-cyclodextrin in water according to the ratio. First, make full contact between the encapsulation material and water to ensure that the encapsulation material can be evenly dispersed, which will facilitate the subsequent dissolution rate. Increase the temperature to 50°C at 5°C / min, and then increase the temperature to 80-90°C at 10°C / min to completely dissolve the encapsulation material solution.

[0015] Gelatin, alginate, and β-cyclodextrin serve as the encapsulation materials (wall materials) for camellia oil microcapsules, effectively encapsulating the camellia oil while ensuring particle uniformity. For the formulation, taking 1000g of camellia oil microcapsule powder as an example, the amount of gelatin is 8-12g, alginate is 10-130g, β-cyclodextrin is 20-100g, camellia oil is 80-400g, and the remainder is water, with a pH of 7-9. The aforementioned limitations on the types and proportions of encapsulation materials, heating rate, and temperature ensure the uniformity of the encapsulation material solution, facilitating subsequent preparation of the camellia oil microcapsules.

[0016] S1.2 Add the directly purchased camellia oil to the encapsulation material solution at a feeding rate of 5-10 g / min, stir evenly, so that the camellia oil is fully dispersed in the encapsulation material solution to obtain mixture I;

[0017] S1.3 Add a gelling agent (e.g., aluminum sulfate; aluminum sulfate dissolves in water to generate aluminum ions, which carry a positive charge and can attract and collide with negatively charged suspended matter in the water, forming larger particles that then precipitate) to mixture I. The dripping speed should be moderate to ensure that the resulting microcapsules are of uniform size (controlling the size ≤10μm). Let it stand for 1–3 hours. Then, using an atomizing device, pass this material liquid through a dry hot air stream (water content <5mg / kg, temperature 120–200℃, hot air flow rate 600–900L / h). The solution is atomized into fine droplets. The solvent in the droplet wall material evaporates rapidly upon heating, thus forming a mesh-like membrane structure with a sieving function around the micronized core material. The larger molecules of the core material are trapped in the formed membrane, while small molecules such as water or other solvents in the wall material are easily removed through the "mesh" due to thermal evaporation. The membrane is then further dried and cured (drying temperature is 80-100℃, curing time is 0.5-2h), resulting in powdered or granular camellia oil microcapsules with a camellia oil content ≥50% and a particle size ≤10μm.

[0018] Preparation of S2 Camellia Oil Dispersion

[0019] Camellia oil microcapsules were dissolved in a 5-20% (w / w) ethanol-water solution (pH 7-9, adjusted with 1-5% (w / w) sodium hydroxide). This reagent removes impurities from the surface of the camellia oil microcapsules, ensuring the effective content of camellia oil; it also prevents the microcapsules from agglomerating, resulting in more uniform dispersion. Regarding concentration, pure ethanol solution can damage some of the camellia oil microcapsule powder, reducing its performance and uniformity; too low a concentration cannot guarantee uniform distribution of the microcapsules; too high a concentration… To ensure the stability of the camellia oil microcapsules, the solution was continuously stirred (stirring rate 800–4000 r / min, time 0.5–2 h) at a dissolution temperature of 20–60℃. 1–10% of polyethylene glycol 200 was added (because the camellia oil microcapsule powder has a small particle size and is prone to aggregation in the solution, polyethylene glycol 200 disperses the aggregated camellia oil microcapsules, ensuring uniform dispersion. Insufficient polyethylene glycol 200 will cause microcapsule powder agglomeration and uneven dispersion). Adding too much alcohol 200 will affect the homogeneity and stability of the overall solution. Stir at 1000–6000 rpm for 0.5–2 hours (to ensure the stability, uniform distribution, and dissolution of the camellia oil microcapsules. Too low a speed will prevent uniform dispersion; too high a speed will damage the microcapsules). Add 0.5–1‰ of emulsifier (the emulsifier is one or a mixture of two or more of polyoxyethylene fatty alcohol ether, polyoxyethylene alkylphenol ether, and dodecyl alcohol amide phosphate; through emulsification and dispersion, it ensures the stability of the camellia oil microcapsules). Uniform dispersion of the capsules. Insufficient emulsifier will not achieve the desired emulsification effect; excessive emulsifier will affect the stability of the dispersion. After thorough stirring, add 1-8% aerogel (such as silica-based aerogel, which is low-cost and directly water-soluble). Using aerogel with microporous mesh properties as a carrier for camellia oil microcapsules ensures that more camellia oil substances are retained in the pores, reducing damage and loss during subsequent spinning, improving camellia oil utilization, and prolonging the release of effective substances within the camellia oil microcapsules, thus obtaining a camellia oil dispersion.

[0020] S3 blend

[0021] A mixture of sodium alginate and β-cyclodextrin (sodium alginate:β-cyclodextrin mass ratio of 5:1; used as a thickener for camellia oil dispersion to ensure a certain viscosity for easy mixing with viscous liquid) was added to the camellia oil dispersion using a metering pump and continuously stirred (stirring rate of 1000-3000 r / min, time of 0.5-1 h) to ensure thorough mixing, resulting in mixture II.

[0022] The weight ratio of sodium alginate and β-cyclodextrin mixture to camellia oil dispersion is 0.02-0.08:1, primarily to ensure that mixture II has sufficient viscosity. If the weight ratio is too small, the viscosity is not significant; if the weight ratio is too large, the viscosity is too high, increasing costs and resulting in poor flowability, which is inconvenient for subsequent spinning. Sodium alginate and β-cyclodextrin in the camellia oil dispersion act as a protective film, reducing damage to the camellia oil microcapsules. On one hand, sodium alginate and β-cyclodextrin impart a certain viscosity to the camellia oil dispersion, enabling better mixing with the viscous liquid, thus reducing direct contact and protecting the camellia oil microcapsules. On the other hand, sodium alginate powder becomes wet upon contact with water; the hydration of the particles makes their surface sticky, and then the particles quickly adhere together to form clumps. These clumps slowly and completely hydrate and dissolve, re-encapsulating the camellia oil microcapsules and releasing them slowly, thus providing protection.

[0023] Mixture II and viscose solution are degassed separately, and then the two are transported to the pre-spinning process by metering pump and supply system for static mixing. Then, they are degassed again to obtain spinning solution containing camellia oil.

[0024] In the spinning solution containing camellia oil, the mass of camellia oil is 5-20% of the mass of cellulose fiber;

[0025] S4 spinning

[0026] The two-bath wet spinning method is adopted. The spinning solution containing camellia oil is sent to the spinning machine through the glue supply pipeline, quantitatively fed in by the metering pump, and filtered again through the candle filter to remove particulate impurities. Then it is fed into the spinneret assembly through the curved tube.

[0027] Under pressure, the spinning solution containing camellia oil passes through numerous spinnerets, forming numerous viscous fine streams.

[0028] S5 Solidification and Curing

[0029] After the adhesive filaments flow out, the specific gravity is 1.25-1.32. They enter the coagulation bath and solidify in a coagulation bath containing 250-360 g / L sodium sulfate, 80-130 g / L sulfuric acid and 10-50 g / L zinc sulfate at a temperature of 40-60°C, thus becoming the nascent filaments.

[0030] Among them, for the coagulation bath, the amount of acid bath substance used is lower than that of the existing coagulation bath, which reduces the damage to the effective substances of camellia oil, while ensuring that the fiber forming is not affected.

[0031] Then, the nascent filaments are fed to the bundle stretching stage by the guide disc. In the curing bath, the nascent filaments undergo stretching while ultimately completing the decomposition and regeneration process, and the structure and properties of the fibers are basically fixed, forming a stable core-sheath structure;

[0032] S6 Post-processing

[0033] The obtained fiber bundles are cut, and after one acid washing, desulfurization, one water washing, two acid washing, two water washing, oiling, dehydration and drying, the camellia oil viscose fiber product is obtained.

[0034] The beneficial technical effects of adopting this technical solution are as follows:

[0035] This invention provides a camellia oil fiber that not only possesses the characteristics of regenerated cellulose fiber (FZ / T01057.2—2007 "Textile Fiber Test Methods Part 2: Combustion Method"), but also ensures the camellia oil content in the fiber (≥500mg / kg). Furthermore, it endows the camellia oil fiber with excellent antibacterial properties (GB / T 20944.3-2008 "Evaluation of Antibacterial Properties of Textiles Part 3: Shaking Method"), antioxidant and free radical scavenging properties (FB-DFHHWDCD-Determination of Polyphenolic Compounds 2024*, FB-FZPZZFSHL-Fatty Acid Content 2024*), thus meeting people's needs and preferences for functional cellulose fibers.

[0036] Among them, it effectively increased the retention of camellia oil in viscose fiber, improved the utilization rate of camellia oil and viscose liquid, and the preparation method involved is easy to control and has strong spinnability.

[0037] Composing the functional ingredient camellia oil into microcapsules allows for uniform distribution of the oil in the solution, ensuring even mixing with the viscose solution and facilitating further spinning. Treatment with ethanol-water solution, polyethylene glycol 200, emulsifiers, and aerogels ensures the uniform dispersion of the extremely small camellia oil microcapsules, facilitating subsequent blending. For example, the addition of aerogel utilizes its unique porous network properties to store a large amount of camellia oil microcapsule powder within the pores, further ensuring the retention of the effective components of the camellia oil, better binding with the subsequent viscose solution, and improving utilization. Attached Figure Description

[0038] Figure 1 This is a photograph of the camellia oil viscose fiber used in this invention.

[0039] Figure 2 This is a test report on the antibacterial properties of the camellia oil viscose fiber in this invention;

[0040] Figure 3 This is a test report on the polyphenol compound content of camellia oil viscose fiber in this invention;

[0041] Figure 4 This is a test report on the total fatty acid content of camellia oil viscose fiber in this invention. Detailed Implementation

[0042] The technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are only a part of the embodiments of the present invention, and not all of them. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.

[0043] Camellia oil (also known as wild camellia oil, tea seed oil, or oil-tea seed oil) is extracted from the seeds of the camellia tree (Camellia oleifera), belonging to the Theaceae family. The production process of camellia oil includes: shelling, drying, crushing, steaming, pressing, and filtering. Camellia oil does not contain erucic acid or cholesterol. Tests show that camellia oil contains over 90% unsaturated fatty acids, with oleic acid reaching 80-83% and linoleic acid reaching 7-13%, but the content of linolenic acid is extremely low.

[0044] Camellia oil is rich in nutrients, containing fatty acids (93% unsaturated fatty acids, including 82% oleic acid and 11% linoleic acid), camelliaside, tea polyphenols, saponins, tannins, and squalene, which is rich in antioxidants and has anti-inflammatory effects. Squalene and flavonoids have excellent anti-cancer effects. Camellia oil is also rich in vitamin E and trace elements such as calcium, iron, and zinc. The zinc content, hailed as the "flower of life" by medical and nutrition experts, is 10 times that of soybean oil. Camellia oil also contains the most diverse range of amino acids of all edible oils.

[0045] However, due to the inherent characteristics of camellia oil (insoluble in water), it cannot be well mixed with viscose (in terms of uniformity and fiber bonding), resulting in poor spinnability and fiber properties, thus hindering its utilization. To address this, camellia oil is prepared into microcapsules (commercially available, with specifications including camellia oil content ≥50% and particle size ≤10μm). After treatment with specific dispersants, emulsifiers, and gelling agents, it can be well mixed with viscose and then spun stably.

[0046] The preparation of camellia oil microcapsules includes the following steps:

[0047] 1. Dissolve 10g of gelatin, 100g of alginate and 60g of β-cyclodextrin in 630g of pure water. First, heat the solution to 50°C at 5°C / min, then heat it to 85°C at 10°C / min until completely dissolved. Adjust the pH to 8 with sodium hydroxide to obtain the encapsulation material solution.

[0048] 2. Add 200g of camellia oil to the encapsulation material solution at a rate of 8g / min, stir evenly to fully disperse the camellia oil in the encapsulation material solution, and obtain mixture I;

[0049] 3. Add aluminum sulfate to mixture I at a rate of 1.2 ml / min to ensure uniform capsule size, and let stand for 1.5 h. Then, use an atomizing device to atomize the microcapsules into fine droplets in a dry hot airflow (water content < 5 mg / kg, temperature 120-200℃, hot air flow rate 600-900 L / h). The solvent in the droplet wall material evaporates rapidly upon heating, thus forming a mesh membrane structure with sieving function around the micronized core material. Larger molecules of the core material are trapped in the formed membrane, while smaller molecules such as water or other solvents in the wall material are easily removed through the "mesh" due to thermal evaporation. The outlet temperature is 90℃. Then, solidify at 80-100℃ for 45 min to obtain 1000 g of camellia oil microcapsules.

[0050] The following example will then be used to illustrate this.

[0051] Example 1

[0052] This embodiment provides: a camellia oil fiber, which is made from camellia oil microcapsules and viscose liquid as raw materials through blending, spinning, coagulation, curing and post-treatment;

[0053] Among them, the camellia oil microcapsules contain ≥50% camellia oil, with a particle size ≤10μm, and the proportion of camellia oil microcapsules with a particle size of 4~7μm is 50~90%;

[0054] The cellulose content in the adhesive is 89–94 g / L;

[0055] The finished product indicators of the camellia oil fiber include: Candida albicans ≥85.0%, Escherichia coli ≥80.0%, Staphylococcus aureus ≥90.0%, free radical scavenging ≥40%; dry breaking strength ≥2.10 cN / dtex, strength >2.08 dtex, wet breaking strength ≥1.00 cN / dtex, dry breaking elongation 17±4.5%, residual sulfur ≤20mg / 100g, defects ≤4mg / 100g, oily yellow fibers ≤1mg / 100g, and dry breaking strength coefficient of variation CV ≤20%.

[0056] Camellia oil microcapsules are either powdered or granular.

[0057] The weight ratio of camellia oil microcapsules to adhesive liquid is 10-20:80-90.

[0058] Example 2

[0059] This embodiment produces 50 kg of camellia oil viscose fiber, including the following steps:

[0060] 1) Camellia oil dispersion preparation process

[0061] Camellia oil microcapsules were added to an ethanol-water solution with a mass fraction of 12% and a pH of 9 at 45°C and mixed until uniformly dispersed. Then, 4% polyethylene glycol 200 was added and mixed until uniformly dispersed. Next, 0.7‰ polyoxyethylene fatty alcohol ether was added and mixed until uniformly dispersed. Finally, 8% silica aerogel was added and mixed until uniformly dispersed to obtain a camellia oil dispersion.

[0062] 2) Blending process

[0063] With a weight ratio of 0.04:1 between the mixture of sodium alginate and β-cyclodextrin and the camellia oil dispersion, the mixture of sodium alginate and β-cyclodextrin was added to the camellia oil dispersion, mixed evenly, and degassed; then, it was added to the degassed viscose solution, mixed evenly, and degassed again to obtain a spinning solution containing camellia oil.

[0064] Among them, the quality of camellia oil is controlled to be 15% of the quality of cellulose.

[0065] 3) Spinning process

[0066] The two-bath wet spinning method is adopted. The spinning solution containing camellia oil is sent to the spinning machine through the glue supply pipeline, quantitatively fed in by the metering pump, and filtered again through the candle filter to remove particulate impurities. Then it is fed into the spinneret assembly through the curved tube.

[0067] Under pressure, the spinning solution containing camellia oil passes through numerous spinnerets, forming numerous viscous fine streams.

[0068] 4) Solidification and curing process

[0069] The viscose stream is controlled to enter the coagulation bath with a specific gravity of 1.25-1.32. It is then coagulated and formed in a coagulation bath containing 250-360 g / L sodium sulfate, 80-130 g / L sulfuric acid and 10-50 g / L zinc sulfate, and at a temperature of 40-60°C, thus becoming the nascent filaments.

[0070] Then, the nascent filaments are fed to the bundle stretching stage by the guide disc. In the curing bath, the nascent filaments undergo stretching while ultimately completing the decomposition and regeneration process, and the structure and properties of the fibers are basically fixed, forming a stable core-sheath structure;

[0071] 5) Post-processing steps,

[0072] The resulting fiber bundles are cut, and after one acid wash, desulfurization, one water wash, a second acid wash, a second water wash, oiling, dehydration, and drying, camellia oil viscose fiber products are obtained (e.g., Figure 1 (As shown).

[0073] The antibacterial properties, polyphenol content, and total fatty acid content of camellia oil viscose fiber were tested, and the results are as follows: Figure 2-4 As shown.

[0074] The finished product specifications of the obtained camellia oil viscose fiber are shown in Table 1 below.

[0075] Table 1

[0076]

[0077] Example 3

[0078] Based on Example 2, camellia oil viscose fiber was prepared. The difference from Example 2 is that in step 1), the mass fraction of ethanol-water solution is 8%, the amount of polyethylene glycol 200 added is 4%, and the amount of silicone aerogel added is 5%; in the spinning solution containing camellia oil in step 2), the mass of camellia oil is 10% of the mass of the viscose fiber, and the rest is the same as in Example 2.

[0079] The finished product specifications of the obtained camellia oil viscose fiber are shown in Table 2 below.

[0080] Table 2

[0081]

[0082]

[0083] Example 4

[0084] Based on Example 2, camellia oil viscose fiber was prepared, the difference being that in step 1), the mass fraction of ethanol-water solution was 20%, the amount of polyethylene glycol 200 added was 2%, and the amount of silica aerogel added was 8%; in step 2), the weight ratio of the mixture of sodium alginate and β-cyclodextrin to the camellia oil dispersion was 0.06:1, and in the spinning solution containing camellia oil, the mass of camellia oil was 5% of the mass of viscose fiber, the rest being the same as in Example 2.

[0085] The finished product specifications of the obtained camellia oil viscose fiber are shown in Table 3 below.

[0086] Table 3

[0087]

[0088] Example 5

[0089] Based on Example 2, camellia oil viscose fiber was prepared, the difference being that in step 1), the mass fraction of ethanol-water solution was 10%, the amount of polyethylene glycol 200 added was 2%, and the amount of silica aerogel added was 1%; in step 2), the weight ratio of the mixture of sodium alginate and β-cyclodextrin to the camellia oil dispersion was 0.02:1, and in the spinning solution containing camellia oil, the mass of camellia oil was 20% of the mass of viscose fiber, the rest being the same as in Example 2.

[0090] The finished product specifications of the obtained camellia oil viscose fiber are shown in Table 4 below.

[0091] Table 4

[0092]

[0093] Comparative Example 1

[0094] Based on Example 2, camellia oil viscose fiber was prepared. The difference from Example 2 is that in step 1), ethanol-water solution was not added. Instead, camellia oil microcapsules were directly added to 4% polyethylene glycol 200. The rest was the same as in Example 2.

[0095] The finished product specifications of the obtained camellia oil viscose fiber are shown in Table 5 below.

[0096] Table 5

[0097]

[0098] Comparative Example 2

[0099] Based on Example 2, camellia oil viscose fiber was prepared. The difference from Example 2 is that in step 1), polyethylene glycol 200 was not added, and the rest was the same as in Example 2.

[0100] The finished product specifications of the obtained camellia oil viscose fiber are shown in Table 6 below.

[0101] Table 6

[0102]

[0103] Comparative Example 3

[0104] Based on Example 2, camellia oil viscose fiber was prepared. The difference from Example 2 is that in step 1), polyoxyethylene fatty alcohol ether was not added, and the rest was the same as in Example 2.

[0105] The finished product specifications of the obtained camellia oil viscose fiber are shown in Table 7 below.

[0106] Table 7

[0107]

[0108] From Table 1-7, we can see that:

[0109] Compared with Example 2, Comparative Example 1 showed a significant decrease in antibacterial properties, free radical scavenging properties, and camellia oil content (total fatty acids). It can be seen that using ethanol to dissolve camellia oil microcapsules can effectively increase the total fatty acid content in camellia oil fiber and improve its utilization rate. This is because using ethanol removes impurities from the surface of camellia oil microcapsules, reduces agglomeration, and makes them easier to disperse and more uniform. During use, they can be better distributed in the fiber, reducing the large amount of loss caused by uneven distribution.

[0110] 2. Compared with Example 2, Comparative Example 2 showed a significant decrease in antibacterial properties, free radical scavenging properties, and camellia oil content (total fatty acids). It can be seen that the use of aerogel can effectively increase the total fatty acid content in the fiber and improve the utilization rate. This is because the porous network structure of aerogel itself allows more effective components of camellia oil to enter the network under the same volume. In the subsequent spinning process, it is not easily destroyed by strong acid and alkali environments, thus becoming a protective layer and improving the utilization rate of raw materials. At the same time, it slows down the release process of camellia oil microcapsules.

[0111] 3. Compared with Example 2, Comparative Example 3 showed a significant decrease in antibacterial properties, free radical scavenging properties, and camellia oil content (total fatty acids). This is because sodium alginate and β-cyclodextrin are homologous substances in camellia oil microcapsule powder. Sodium alginate has a solubilizing effect on hydrophobic molecules and a certain sustained-release effect on small molecule organic matter. β-cyclodextrin has the characteristics of a hydrophilic outer wall and a hydrophobic inner cavity, which can encapsulate hydrophobic substances and protect camellia oil to a certain extent, thereby improving the utilization rate of camellia oil.

[0112] The above description is merely a preferred embodiment of the present invention and is not intended to limit the present invention in any way. Any simple modifications, equivalent changes, and alterations made to the above embodiments based on the technical essence of the present invention shall fall within the protection scope of the present invention.

Claims

1. A camellia oil fiber, characterized in that, It is prepared by blending, spinning, coagulation, curing and post-treatment of camellia oil microcapsules and adhesive liquid as raw materials; Among them, the camellia oil microcapsules contain ≥50% camellia oil, have a particle size ≤10μm, and the proportion of camellia oil microcapsules with a particle size of 4~7μm is 50~90%; The cellulose content in the adhesive is 89–94 g / L; The finished product indicators of the camellia oil fiber include: Candida albicans ≥85.0%, Escherichia coli ≥90.0%, Staphylococcus aureus ≥90.0%, and free radical scavenging ≥40%.

2. The camellia oil fiber according to claim 1, characterized in that, The camellia oil microcapsules are either powdered or granular.

3. The camellia oil fiber according to claim 1, characterized in that, The weight ratio of the camellia oil microcapsules to the adhesive liquid is 10-20:80-90.

4. A method for preparing camellia oil fiber according to any one of claims 1-3, characterized in that, The process includes, in sequence, the preparation of camellia oil dispersion, blending, spinning, coagulation and solidification, and post-treatment. Camellia oil dispersion preparation process: Camellia oil microcapsules are added to an ethanol-water solution with a mass fraction of 5-20% and a pH of 7-9, and mixed until uniformly dispersed; then, 1-10% of polyethylene glycol 200 is added and mixed until uniformly dispersed; then, 0.5-1‰ of emulsifier is added and mixed until uniformly dispersed; finally, 1-8% of aerogel is added and mixed until uniformly dispersed to obtain the camellia oil dispersion. Blending process: Assuming a weight ratio of sodium alginate and β-cyclodextrin to camellia oil dispersion of 0.02-0.08:1, the sodium alginate and β-cyclodextrin mixture is added to the camellia oil dispersion, mixed evenly, and degassed; then, it is added to the degassed viscose solution, mixed evenly, and degassed again to obtain a spinning solution containing camellia oil. Spinning process: Two-bath wet spinning method is adopted; Coagulation and solidification process: The adhesive fine stream is controlled to enter the coagulation bath with a specific gravity of 1.25 to 1.

32. It is solidified and formed in the coagulation bath containing sodium sulfate 250 to 360 g / L, sulfuric acid 80 to 130 g / L and zinc sulfate 10 to 50 g / L, and the temperature is 40 to 60°C, thus becoming the nascent filaments.

5. The method for preparing camellia oil fiber according to claim 4, characterized in that, Camellia oil microcapsules were added to an ethanol-water solution and stirred at 800–4000 r / min for 0.5–2 h at 20–60 °C. After adding polyethylene glycol 200, the mixture was stirred at 1000–6000 r / min for 0.5–2 h.

6. The method for preparing camellia oil fiber according to claim 4, characterized in that, The emulsifier is one or a mixture of any two or more of polyoxyethylene fatty alcohol ether, polyoxyethylene alkylphenol ether, and dodecyl alcohol phosphate. The aerogel is a silica-based aerogel.

7. The method for preparing camellia oil fiber according to claim 4, characterized in that, In the mixture of sodium alginate and β-cyclodextrin, the weight ratio of sodium alginate to β-cyclodextrin is 4 to 5:

1.

8. The method for preparing camellia oil fiber according to claim 4, characterized in that, In the spinning solution containing camellia oil, the mass of camellia oil is 5-20% of the mass of cellulose fiber.

9. The method for preparing camellia oil fiber according to claim 4, characterized in that, The preparation of the camellia oil microcapsules includes: 1) Dissolve gelatin, alginate and β-cyclodextrin in water, heat to 50°C at 5°C / min, and then heat to 80-90°C at 10°C / min until completely dissolved to obtain a solution of encapsulation material; For example, in 1000g of camellia oil microcapsule powder, the amount of gelatin is 8-12g, the amount of alginate is 10-130g, the amount of β-cyclodextrin is 20-100g, the amount of camellia oil is 80-400g, and the remainder is water, with a pH of 7-9. 2) Add camellia oil to the encapsulation material solution at a feeding rate of 5-10 g / min, disperse evenly, and obtain mixture I; 3) Add aluminum sulfate to mixture I and let it stand for 1-3 hours; then, using an atomizing device, atomize it into droplets under the conditions of water content <5mg / kg, temperature 120-200℃, and hot gas flow rate 600-900L / h; then, solidify it for 0.5-2 hours at a temperature of 80-100℃ to obtain camellia oil microcapsules with a camellia oil content ≥50% and a particle size ≤10μm.

10. The method for preparing camellia oil fiber according to claim 9, characterized in that, In the encapsulation material solution, the weight ratio of gelatin, alginate, and β-cyclodextrin is 0.8–1.2:1–13:2–10.

Citation Information

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