阅读说明：本技术 一种含橄榄的es纤维及其制备方法 (Olive-containing ES fiber and preparation method thereof ) 是由 黄效华 刘浩林 刘洁 甄丽 穆伟华 于 2020-10-31 设计创作，主要内容包括：本发明提供一种含橄榄的ES纤维及其制备方法,包括：橄榄提取液的制备、分子巢颗粒的制备、含橄榄提取物的分子巢颗粒的制备、制备皮层材料、制备芯层材料、纺丝、后处理。本发明的有益效果为：本发明的含橄榄的ES纤维对金黄色葡萄球菌抑菌率≥99.3%,对大肠杆菌抑菌率≥96.8%,对白色念珠菌抑菌率≥95.2%；在1.2×10-2w/in2紫外线照射50h,其物理性能仍能够保持96.1%以上；模量为163-170N/tex。(The invention provides olive-containing ES fibers and a preparation method thereof, wherein the preparation method comprises the following steps: preparing olive extracting solution, preparing molecular nest particles containing olive extracts, preparing skin layer materials, preparing core layer materials, spinning and carrying out post-treatment. The invention has the beneficial effects that: the olive-containing ES fiber has the bacteriostatic rate of more than or equal to 99.3 percent on staphylococcus aureus, the bacteriostatic rate of more than or equal to 96.8 percent on escherichia coli and the bacteriostatic rate of more than or equal to 95.2 percent on candida albicans; the physical property of the material can still keep more than 96.1 percent after the ultraviolet irradiation of 1.2 multiplied by 10 < -2 > w/in2 for 50 hours; the modulus is 163-170N/tex.)

1. A method for preparing olive-containing ES fibers, which is characterized by comprising the following steps: preparing olive extracting solution, preparing molecular nest particles containing olive extracts, preparing skin layer materials, preparing core layer materials, spinning and post-treating;

preparing the olive extracting solution, namely preparing a mixture of olive leaf extract and olive fruit extract by ultrasonic extraction;

the preparation of the molecular nest particle comprises the following steps: preparing and forming a precursor;

the preparation of the precursor comprises the steps of mixing absolute ethyl alcohol and deionized water, then adding a predetermined part of hexadecyl trimethyl ammonium bromide and ammonia water, stirring at 200-300RPM for 5-10min, dropwise adding a predetermined part of tetraethoxysilane, continuously stirring for 1-1.5h, heating to 35-45 ℃, preserving heat for 2-4h, standing for gel aging, and preparing the precursor;

the precursor is molded, dried and calcined to prepare molecular nest particles; the molecular nest particles are porous nano SiO₂The particle size is 300-360nm, the pore diameter is 5-12nm, and the specific surface is 650-800m³/g。

2. The method of claim 1, wherein the step of preparing the molecular nest particles comprises: activating;

the activation is carried out, the formed molecular nest particles are placed in a closed container, the pressure is increased to 11-12MPa within 30s, the pressure is maintained for 10min, and the pressure is quickly released to normal pressure within 1.5 s; and then pressurizing to 15-20MPa within 30s, maintaining the pressure for 5min, and quickly relieving the pressure to normal pressure within 1.5s to finish the activation step.

3. The method for preparing the olive-containing ES fiber according to claim 1, wherein the preparation of the olive extract-containing molecular nest particles comprises the steps of preparing a molecular nest particle dispersion liquid and loading;

preparing the molecular nest particle dispersion, namely putting the molecular nest particles into absolute ethyl alcohol, and uniformly dispersing to obtain the molecular nest particle dispersion;

the molecular nest particle: the volume ratio of the absolute ethyl alcohol is 1: 1-2;

the loading step, mixing the olive extract and the molecular nest particle dispersion liquid with a surfactant and a stabilizer, and dispersing at 500-600RPM for 20-30 min;

the olive extracting solution: molecular nest particle dispersion liquid: surfactant (b): the mass ratio of the stabilizer is 50:10:2: 1.

4. The method of preparing olive-containing ES fiber according to claim 1, wherein the olive leaf extract: the weight ratio of the olive fruit extract is 2-4: 1;

the olive leaf extract has oleuropein content of more than 30% and hydroxytyrosol content of 10-20%;

the olive fruit extract has an olive polyphenol content of more than 8%.

5. The method of claim 1, wherein the preparation of the precursor comprises the steps of: deionized water: cetyl trimethylammonium bromide: ammonia water: the volume ratio of the ethyl orthosilicate is 90-100: 5-10: 5-10: 8-12: 20-25.

6. The method for preparing the ES fiber containing the olive as claimed in claim 1, wherein the skin layer material is prepared by uniformly mixing the molecular nest particles containing the olive extract, the PE slices, the polyethylene oxide, the silicone emulsion, the titanate coupling agent, the maleic anhydride grafted compatilizer and the diisooctyl sebacate, and carrying out banburying granulation to obtain the skin layer material;

the preparation method comprises the steps of uniformly mixing PP slices, titanate coupling agent and glass fiber, and carrying out banburying granulation to obtain the core layer material.

7. The method for preparing the olive-containing ES fiber according to claim 6, wherein the prepared skin layer material comprises the olive extract-containing molecular nest particles, PE slices, polyethylene oxide, silicone emulsion, titanate coupling agent, maleic anhydride grafting compatilizer and diisooctyl sebacate, and the weight ratio of the olive extract-containing molecular nest particles to the PE slices to the diisooctyl sebacate is 30-35: 200-220: 5-8:8-10:5-10:3-10: 2-5;

and banburying is carried out at the banburying pressure of 12MPa and the banburying temperature of 110 ℃ for 40 min.

8. The method for preparing the ES fibers containing the olives as claimed in claim 6, wherein the core material is prepared by mixing PP slices, titanate coupling agent and modified glass fibers at a weight ratio of 100:2: 5;

and banburying is carried out at the banburying pressure of 14MPa, the banburying temperature of 200 ℃ and the banburying time of 30 min.

9. The method for preparing the olive-containing ES fiber according to claim 1, wherein the spinning comprises drying, melting and filtering the skin layer material and the core layer material, respectively, and then performing composite spinning after metering to obtain the fiber;

the volume part ratio of the skin layer material to the core layer material is 1: 1-1.2;

the melting temperature of the skin layer material is 120 ℃, and the melting temperature of the core layer material is 220 ℃;

the pressure of a nozzle of a spinneret plate is 3.2-3.5kg/cm in the spinning process²The die temperature was 200 ℃.

10. An olive-containing ES fiber, which is produced by the production method according to any one of claims 1 to 9.

Technical Field

The invention relates to the field of ES fibers, in particular to olive-containing ES fibers and a preparation method thereof.

Background

Olive, a plant of the genus Olea of the family Burseraceae. The height can reach 35 m, and the diameter at breast height can reach 150 cm. 3-6 pairs of small leaves, paper to leather, 12-16 pairs of lateral veins, 1.5-15 cm long infructescence and 1-6 fruits. Oval to spindle-shaped, yellow-green at maturity, thick outer peel, hard core, pointed ends at both ends, and coarsened core surface. The flowering period is 4-5 months, and the fruit is mature in 10-12 months. The olive is native to southern China, and cultivated in areas such as Fujian, Taiwan, Guangdong, Guangxi, Yunnan, Japan (Kawasaki, Okinawa) and Malaysia, and wild olive is cultivated in valley and hillside miscellaneous tree forest with elevation below 1300 m, or cultivated beside garden and village.

The olive is a good windproof tree species and a street tree. The wood can be used for shipbuilding, making sleepers, making furniture, making farm implements, making building materials and the like. The olive leaves, the olive fruits and the olive stones can be used as medicines, and have the effects of clearing heat and removing toxicity, eliminating phlegm and relieving cough, eliminating diseases and killing insects, reducing swelling and relieving pain and the like. Wherein the fructus Canarii albi can be eaten raw or soaked, and can be used for treating laryngitis, hemoptysis, polydipsia, enteritis and diarrhea.

As early as the 15 th-16 th century, there was evidence that drinking olive leaf-brewed tea was the traditional treatment for discomfort such as cough, sore throat, cystitis and fever in the middle east. However, olive leaves have not started to attract the attention of the medical community until the early 18 th century. The main components of olive leaf mainly comprise iridoid, flavone and its glycoside, biflavone and its glycoside, low molecular tannin, etc., and the most active components are oleuropein and hydroxytyrosol. Oleuropein in the olive leaves can protect skin cells from being damaged by ultraviolet rays, prevent ultraviolet rays from decomposing skin membrane lipid, promote fibroblasts to generate collagen, reduce secretion of fibroblast collagen enzyme, and prevent glycan resistant reaction of cell membranes, so that the fibroblasts are highly protected, the skin is naturally prevented from being damaged by oxidation, the skin is further prevented from being damaged by the ultraviolet rays, the skin is effectively kept tender and elastic, and the effects of strengthening and tendering the skin are achieved.

The ES fiber is a polyolefin fiber developed by japanese wisdom corporation, and is a novel thermal bonding conjugate fiber. The fiber is a bi-component skin-core structure composite fiber, the skin tissue has low melting point and good flexibility, and the core tissue has high melting point and high strength. After the fiber is subjected to heat treatment, a part of the skin layer is melted to play a bonding role, and the rest of the skin layer still keeps a fiber state and has the characteristic of small heat shrinkage rate. Is particularly suitable for producing products such as sanitary materials, warm-keeping filling materials, filtering materials and the like by a hot air penetration process.

After the ES fibers are heat-treated, the fibers are bonded to each other to form a nonwoven fabric molding without using a binder. Such as a through-air bonded nonwoven fabric and a hot-rolled bonded nonwoven fabric. The ES fiber is formed by combining two resins having different melting points, and bonding between fibers can be achieved by heat treatment only by utilizing the difference in melting point between the two resins. The section form of the ES fiber is a sheath-core type or a side-by-side type, and the non-woven fabric processed by the ES fiber has good fluffiness, softness and wet elasticity.

With the development and progress of the times and the improvement of the living standard of people, the functional improvement of the ES fiber is more and more. Because the ES fiber has certain irritation to the skin, people with allergic constitution are easy to have allergic reaction of different degrees when using ES fiber products. Thus, the demand for the antiallergic function of ES fiber is more and more urgent today as the use of ES fiber is more and more widespread.

At present, there are two main methods for modifying ES fiber: one is to directly add a functional modifier into the raw material of the skin layer in the spinning process to prepare the functional ES fiber. Another approach is to attach functional ingredients to the fiber surface by post-treatment processes, thereby imparting a degree of functional properties to the ES fiber. The first method described above is a key direction in the research of functional modification, because the functional auxiliary agent can be effectively dispersed inside the sheath layer of the ES fiber, and the fiber can be made permanently functional.

In the prior art of producing ES fiber by the first production process, there are reports of loading a functional additive on porous nano-silica particles, preparing a functional masterbatch, and finally performing a hybrid spinning process. The applicant finds that in the process of preparing the ES fiber by adopting the process, due to the characteristic that nano-silica porous particles tend to agglomerate, when the nano-silica porous particles are used as a carrier loaded with functional components, the nano-silica porous particles are not well distributed in the cortex of the ES fiber, the modification effect is not ideal, and the functional components cannot fully exert the modification effect on the fiber.

Further, in the research process of modifying ES fibers by using olives as plant modification materials, the applicant finds that when the effective components extracted from olives are loaded on a common carrier, the loading effect is not ideal and the process requirements cannot be met. When the active ingredients are loaded on the nano-silica porous particles, although the loading effect is good, the olive active ingredients are easy to lose due to the influence of the process in the fiber processing and forming process, and the processing stability is not ideal.

Disclosure of Invention

In order to solve the technical problems in the prior art, the invention provides olive-containing ES fibers and a preparation method thereof, so as to achieve the following aims:

(1) the distribution of the nano-silica porous particles loaded with the olive active ingredients in the ES fiber cortex is improved;

(2) improving the processing stability of the nano silicon dioxide porous particles containing the olive effective components;

(3) reducing the irritation of ES fibers to the skin.

In order to solve the technical problems, the technical scheme adopted by the invention is as follows:

a method for preparing olive-containing ES fibers, comprising: preparing olive extracting solution, preparing molecular nest particles containing olive extracts, preparing skin layer materials, preparing core layer materials, spinning and post-treating;

preparing the olive extracting solution, namely preparing a mixture of olive leaf extract and olive fruit extract by ultrasonic extraction;

the preparation of the molecular nest particle comprises the following steps: preparing and forming a precursor;

the preparation of the precursor comprises the steps of mixing absolute ethyl alcohol and deionized water, then adding a predetermined part of hexadecyl trimethyl ammonium bromide and ammonia water, stirring at 200-300RPM for 5-10min, dropwise adding a predetermined part of tetraethoxysilane, continuously stirring for 1-1.5h, heating to 35-45 ℃, preserving heat for 2-4h, standing for gel aging, and preparing the precursor;

the precursor is molded, dried and calcined to prepare molecular nest particles; the molecular nest particles are porous nano SiO₂The particle size is 300-360nm, the pore diameter is 5-12nm, and the specific surface is 650-800m³/g；

Further, the preparation of the molecular nest particle comprises the following steps: activating;

the activation is carried out, the formed molecular nest particles are placed in a closed container, the pressure is increased to 11-12MPa within 30s, the pressure is maintained for 10min, and the pressure is quickly released to normal pressure within 1.5 s; and then pressurizing to 15-20MPa within 30s, maintaining the pressure for 5min, and quickly relieving the pressure to normal pressure within 1.5s to finish the activation step.

Further, the preparation of the molecular nest particles containing the olive extract comprises the preparation and loading of a molecular nest particle dispersion liquid;

preparing the molecular nest particle dispersion, namely putting the molecular nest particles into absolute ethyl alcohol, and uniformly dispersing to obtain the molecular nest particle dispersion;

the molecular nest particle: the volume ratio of the absolute ethyl alcohol is 1: 1-2;

the loading step, mixing the olive extract and the molecular nest particle dispersion liquid with a surfactant and a stabilizer, and dispersing at 500-600RPM for 20-30 min;

the olive extracting solution: molecular nest particle dispersion liquid: surfactant (b): the mass ratio of the stabilizer is 50:10:2: 1.

Further, the olive leaf extract: the weight ratio of the olive fruit extract is 2-4: 1;

the olive leaf extract has oleuropein content of more than 30% and hydroxytyrosol content of 10-20%;

the olive fruit extract has an olive polyphenol content of more than 8%.

Further, the preparation of the precursor, the absolute ethyl alcohol: deionized water: cetyl trimethylammonium bromide: ammonia water: the volume ratio of the ethyl orthosilicate is 90-100: 5-10: 5-10: 8-12: 20-25.

Further, preparing a skin layer material, namely uniformly mixing the molecular nest particles containing the olive extract, the PE slices, the polyethylene oxide, the emulsified silicone oil, the titanate coupling agent, the maleic anhydride grafted compatilizer and the diisooctyl sebacate, and carrying out banburying granulation to prepare the skin layer material;

the preparation method comprises the steps of uniformly mixing PP slices, titanate coupling agent and glass fiber, and carrying out banburying granulation to obtain the core layer material.

Further, the skin layer material is prepared by mixing the olive extract-containing molecular nest particles, the PE slices, polyethylene oxide, emulsified silicone oil, a titanate coupling agent, a maleic anhydride grafting compatilizer and diisooctyl sebacate in parts by weight of 30-35: 200-220: 5-8:8-10:5-10:3-10: 2-5; carrying out internal mixing, wherein the internal mixing pressure is 12MPa, the internal mixing temperature is 110 ℃, and the internal mixing time is 40 min;

the core layer material is prepared, wherein the ratio of the PP slices, the titanate coupling agent and the modified glass fiber in parts by weight is 100:2: 5; and banburying is carried out at the banburying pressure of 14MPa, the banburying temperature of 200 ℃ and the banburying time of 30 min.

Further, in the spinning, the skin layer material and the core layer material are respectively dried, melted and filtered, and then composite spinning is carried out after metering to prepare fibers;

the volume part ratio of the skin layer material to the core layer material is 1: 1-1.2;

the melting temperature of the skin layer material is 120 ℃, and the melting temperature of the core layer material is 220 ℃;

the pressure of a nozzle of a spinneret plate is 3.2-3.5kg/cm in the spinning process²The die temperature was 200 ℃.

Compared with the prior art, the invention has the beneficial effects that:

(1) according to the preparation method of the olive-containing ES fiber, the prepared olive extract-containing molecular nest particles are good in processing stability and cannot be influenced by a fiber preparation process; meanwhile, the molecular nest particles are good in distribution in the fiber cortex, the modification effect of the effective components of the olive can be fully exerted, the inhibition rate of the ES fibers on staphylococcus aureus is more than or equal to 99.3%, the inhibition rate on escherichia coli is more than or equal to 96.8%, and the inhibition rate on candida albicans is more than or equal to 95.2%.

(2) In the olive-containing ES fiber prepared by the olive extract-containing molecular nest particles, the olive effective component load is stable, the modification effect on the ES fiber is stable and durable, and the antibacterial performance of the ES fiber is reduced by less than 8.1% after 100 times of standard washing.

(3) The olive-containing ES fiber has the functions of skin care, skin moistening and ultraviolet protection, and the physical performance of the olive-containing ES fiber can still be kept above 96.1% after 1.2 x 10-2w/in2 ultraviolet irradiation for 50 hours.

(4) The ES fiber containing olive can effectively reduce the irritation to the skin and the anaphylactic reaction of people with allergic constitution to ES fiber products.

(5) The olive-containing ES fiber has good physical properties, and the modulus is 163-170N/tex.

Detailed Description

In order to more clearly understand the technical features, objects, and effects of the present invention, specific embodiments of the present invention will now be described.

Example 1

A method for preparing olive-containing ES fibers, comprising: preparing olive extracting solution, preparing molecular nest particles containing olive extracts, preparing skin layer materials, preparing core layer materials, spinning and carrying out post-treatment.

Preparing the olive extracting solution, namely mixing a predetermined part of olive leaf extract and an olive fruit extract, and grinding the mixture to 150 meshes; adding into 10 times volume of anhydrous ethanol, stirring at 100RPM for 10min, heating to 40 deg.C, performing ultrasonic extraction for 2 hr, and filtering to obtain solid substance.

The ultrasonic extraction has the ultrasonic frequency of 22kHz and the ultrasonic intensity of 10W/cm²And the ultrasonic power is 350W.

The olive leaf extract: the olive fruit extract has a weight ratio of 2: 1.

The olive leaf extract contains oleuropein 33.4%, hydroxytyrosol 17.1%, and 80 mesh.

The olive fruit extract has the olive polyphenol content of 10.5 percent and the mesh number of 60 meshes.

The preparation of the molecular nest particle comprises precursor preparation, molding and activation.

Preparing the precursor, mixing absolute ethyl alcohol and deionized water in a predetermined part, adding Cetyl Trimethyl Ammonium Bromide (CTAB) and ammonia water in a predetermined part, stirring at 200RPM for 5min, dropwise adding Tetraethoxysilane (TEOS) in a predetermined part, and continuously stirring for 1 h; heating to 35 ℃, preserving heat for 2 hours, and standing the gel for aging until the gel is complete; and preparing the precursor.

The absolute ethyl alcohol: deionized water: cetyl trimethylammonium bromide: ammonia water: the volume ratio of the ethyl orthosilicate is 90: 5: 5: 12: 25.

the forming is carried out, the precursor is placed at 260 ℃ under the condition of 15MPa, and supercritical drying is carried out until the moisture content is less than 0.5%; then calcining at 500 ℃ for 3h to obtain the molecular nest particles.

The molecular nest particles are porous nano SiO₂The particle diameter D50 is 360nm, the pore diameter is 8-12nm, and the specific surface is 750m³/g。

The activation is carried out, the molecular nest particles are placed in a closed container, the pressure is increased to 11MPa within 30s, the pressure is maintained for 10min, and the pressure is quickly released to normal pressure within 1.5 s; and then pressurizing to 15MPa within 30s, maintaining the pressure for 5min, and quickly relieving the pressure to normal pressure within 1.5s to finish the activation step.

The preparation of the molecular nest particles containing the olive extract comprises the preparation and loading of a molecular nest particle dispersion liquid.

And (3) preparing the molecular nest particle dispersion, namely putting the molecular nest particles into absolute ethyl alcohol, and uniformly dispersing to obtain the molecular nest particle dispersion.

The molecular nest particle: the volume ratio of the absolute ethyl alcohol is 1:1.

The loading step, mixing the olive extract and the molecular nest particle dispersion liquid with a surfactant and a stabilizer, and dispersing for 20min at 500RPM to obtain molecular nest particles containing olive extracts; filtering out said molecular nest particles, and then evaporating the solvent to remove the ethanol to obtain dried molecular nest particles containing olive extract.

The olive extracting solution: molecular nest particle dispersion liquid: surfactant (b): the mass ratio of the stabilizer is 50:10:2: 1;

the surfactant is polyethylene glycol; the stabilizer is sodium stearate.

The preparation method comprises the steps of preparing a skin layer material, uniformly mixing the olive extract-containing molecular nest particles, PE slices, polyethylene oxide, emulsified silicone oil, a titanate coupling agent, a maleic anhydride grafting compatilizer and diisooctyl sebacate, and carrying out banburying granulation to obtain the skin layer material.

The olive extract-containing molecular nest particles, the PE slices, the polyethylene oxide, the emulsified silicone oil, the titanate coupling agent, the maleic anhydride grafted compatilizer and the diisooctyl sebacate have the weight ratio of 30: 220: 5:8: 10: 10: 5.

and banburying is carried out at the banburying pressure of 12MPa and the banburying temperature of 110 ℃ for 40 min.

The preparation method comprises the steps of uniformly mixing PP slices, titanate coupling agent and glass fiber, and carrying out banburying granulation to obtain the core layer material.

And banburying is carried out at the banburying pressure of 14MPa, the banburying temperature of 200 ℃ and the banburying time of 30 min.

The weight ratio of the PP slices to the titanate coupling agent to the modified glass fiber is 100:2: 5.

The modified glass fiber is prepared by hydroxylating and silanizing ground glass fiber and polymerizing. The method specifically comprises the following steps: firstly, grinding glass fiber to 260nm, mixing hydrogen peroxide and the glass fiber, heating to 80 ℃, and mixing for 2 h; adding acetone and gamma-aminopropyltriethoxysilane, mixing and reacting for 3 h; filtering out solid matters and drying; then putting the mixture into N, N-dimethylformamide, adding phthalic anhydride and pentaerythritol, heating to 120 ℃, and reacting for 5 hours; adding diethylenetriamine and reacting for 2 h; drying to obtain the product.

The hydrogen peroxide solution: glass fiber: acetone: gamma-aminopropyltriethoxysilane: n, N-dimethylformamide: phthalic anhydride: pentaerythritol: the weight ratio of the diethylenetriamine is 30:1:40:15:20:2:2: 10.

And in the spinning step, the skin layer material and the core layer material are respectively dried until the moisture content is less than 0.02%, and are respectively melted and filtered, and then the fibers are obtained by carrying out composite spinning after metering.

The volume part ratio of the skin layer material to the core layer material is 1: 1.2.

The melting temperature of the skin layer material is 120 ℃, and the melting temperature of the core layer material is 220 ℃.

In the composite spinning, the pressure of a nozzle of a spinneret plate is 3.5kg/cm²The die temperature was 200 ℃.

The fiber is a skin-core layer structure fiber.

And after the post-treatment, the fiber obtained after the spinning is wound, drawn, oiled and curled, the olive-containing ES fiber is obtained.

The drafting is carried out by 3.1 times of drafting multiple, and the drafting speed is 50 m/min.

Through detection, the olive-containing ES fiber of the embodiment has 99.3 percent of bacteriostasis rate on staphylococcus aureus, 96.8 percent of bacteriostasis rate on escherichia coli and 95.2 percent of bacteriostasis rate on candida albicans; after 100 times of standard washing, the antibacterial performance of the ES fiber is reduced by 7.9 percent; has skin caring, and ultraviolet preventing effects, and its physical properties can be maintained at 96.4% after ultraviolet irradiation of 1.2 × 10-2w/in2 for 50 h; the modulus was 163N/tex.

Example 2

A method for preparing olive-containing ES fibers, comprising: preparing olive extracting solution, preparing molecular nest particles containing olive extracts, preparing skin layer materials, preparing core layer materials, spinning and carrying out post-treatment.

Preparing the olive extracting solution, namely mixing a predetermined part of olive leaf extract and an olive fruit extract, and grinding the mixture to 200 meshes; adding into 10 times volume of anhydrous ethanol, stirring at 200RPM for 15min, heating to 45 deg.C, performing ultrasonic extraction for 2.5h, and filtering to obtain solid substance.

The ultrasonic extraction has the ultrasonic frequency of 22kHz and the ultrasonic intensity of 10W/cm²And the ultrasonic power is 350W.

The olive leaf extract: the olive fruit extract has a weight ratio of 4: 1.

The olive leaf extract contains oleuropein 33.4%, hydroxytyrosol 17.1%, and 80 mesh.

The olive fruit extract has the olive polyphenol content of 10.5 percent and the mesh number of 60 meshes.

The preparation of the molecular nest particle comprises precursor preparation, molding and activation.

Preparing the precursor, mixing absolute ethyl alcohol and deionized water in a predetermined part, adding Cetyl Trimethyl Ammonium Bromide (CTAB) and ammonia water in a predetermined part, stirring at 250RPM for 10min, dropwise adding Tetraethoxysilane (TEOS) in a predetermined part, and continuously stirring for 1.5 h; heating to 40 ℃, and preserving heat for 3 hours; standing the gel and aging until the gel is complete; and preparing the precursor.

The absolute ethyl alcohol: deionized water: cetyl trimethylammonium bromide: ammonia water: the volume ratio of the ethyl orthosilicate is 90: 10: 10: 10: 25.

the forming is carried out, the precursor gel is placed at 260 ℃ and under the condition of 16MPa, and supercritical drying is carried out until the moisture content is less than 0.5%; then calcining at 530 ℃ for 4h to obtain the molecular nest particles.

The molecular nest particles are porous nano SiO₂The particle diameter D50 is 300nm, the pore diameter is 7-10nm, and the specific surface is 800m³/g。

The activation is carried out, the molecular nest particles are placed in a closed container, the pressure is increased to 12MPa within 30s, the pressure is maintained for 10min, and the pressure is quickly released to normal pressure within 1.5 s; and then pressurizing to 18MPa within 30s, maintaining the pressure for 5min, and quickly relieving the pressure to normal pressure within 1.5s to finish the activation step.

The preparation of the molecular nest particles containing the olive extract comprises the preparation and loading of a molecular nest particle dispersion liquid.

And (3) preparing the molecular nest particle dispersion, namely putting the molecular nest particles into absolute ethyl alcohol, and uniformly dispersing to obtain the molecular nest particle dispersion.

The molecular nest particle: the volume ratio of the absolute ethyl alcohol is 1: 1.5.

The loading step, mixing the olive extract and the molecular nest particle dispersion with a surfactant and a stabilizer, and dispersing for 30min at 550RPM to obtain molecular nest particles containing olive extracts; filtering out said molecular nest particles, and then evaporating the solvent to remove the ethanol to obtain dried molecular nest particles containing olive extract.

The olive extracting solution: molecular nest particle dispersion liquid: surfactant (b): the mass ratio of the stabilizer is 50:10:2: 1;

the surfactant is polyethylene glycol; the stabilizer is sodium stearate.

The preparation method comprises the steps of preparing a skin layer material, uniformly mixing the olive extract-containing molecular nest particles, PE slices, polyethylene oxide, emulsified silicone oil, a titanate coupling agent, a maleic anhydride grafting compatilizer and diisooctyl sebacate, and carrying out banburying granulation to obtain the skin layer material.

The olive extract-containing molecular nest particles, the PE slices, the polyethylene oxide, the emulsified silicone oil, the titanate coupling agent, the maleic anhydride grafted compatilizer and the diisooctyl sebacate have the weight ratio of 35: 200: 5:8:5:3:2.

And banburying is carried out at the banburying pressure of 12MPa and the banburying temperature of 110 ℃ for 40 min.

The preparation method comprises the steps of uniformly mixing PP slices, titanate coupling agent and glass fiber, and carrying out banburying granulation to obtain the core layer material.

And banburying is carried out at the banburying pressure of 14MPa, the banburying temperature of 200 ℃ and the banburying time of 30 min.

The weight ratio of the PP slices to the titanate coupling agent to the modified glass fiber is 100:2: 5.

The modified glass fiber is prepared by hydroxylating and silanizing ground glass fiber and polymerizing. The method specifically comprises the following steps: firstly, grinding glass fiber to 260nm, mixing hydrogen peroxide and the glass fiber, heating to 80 ℃, and mixing for 2 h; adding acetone and gamma-aminopropyltriethoxysilane, mixing and reacting for 3 h; filtering out solid matters and drying; then putting the mixture into N, N-dimethylformamide, adding phthalic anhydride and pentaerythritol, heating to 120 ℃, and reacting for 5 hours; adding diethylenetriamine and reacting for 2 h; drying to obtain the product.

The hydrogen peroxide solution: glass fiber: acetone: gamma-aminopropyltriethoxysilane: n, N-dimethylformamide: phthalic anhydride: pentaerythritol: the weight ratio of the diethylenetriamine is 30:1:40:15:20:2:2: 10.

And in the spinning step, the skin layer material and the core layer material are respectively dried until the moisture content is less than 0.02%, and are respectively melted and filtered, and then the fibers are obtained by carrying out composite spinning after metering.

The volume part ratio of the skin layer material to the core layer material is 1: 1.05.

The melting temperature of the skin layer material is 120 ℃, and the melting temperature of the core layer material is 220 ℃.

In the composite spinning, the pressure of a nozzle of a spinneret plate is 3.5kg/cm²The die temperature was 200 ℃.

The fiber is a skin-core layer structure fiber.

And after the post-treatment, the fiber obtained after the spinning is wound, drawn, oiled and curled, the olive-containing ES fiber is obtained.

The drafting is carried out by 3.1 times of drafting multiple, and the drafting speed is 60 m/min.

Through detection, the olive-containing ES fiber has 99.7% of inhibition rate on staphylococcus aureus, 97.8% of inhibition rate on escherichia coli and 97.2% of inhibition rate on candida albicans; after 100 times of standard washing, the antibacterial performance of the ES fiber is reduced by 5.4 percent; has skin caring, and ultraviolet preventing effects, and its physical properties can be maintained at 96.9% after ultraviolet irradiation of 1.2 × 10-2w/in2 for 50 h; the modulus was 170N/tex.

Comparative example 1

The technical scheme of the embodiment 2 is adopted, and the difference is that: the step of 'preparation of molecular nest particles' is deleted, and the molecular nest particles adopted in the step of 'preparation of molecular nest particles containing olive extract' are replaced by bentonite particles with the same particle size specification.

Through detection, the olive-containing ES fiber of the comparative example has 73.2 percent of bacteriostasis rate on staphylococcus aureus, 69.1 percent of bacteriostasis rate on escherichia coli and 60.8 percent of bacteriostasis rate on candida albicans; after 100 times of standard washing, the antibacterial performance of the ES fiber is reduced by 42.9 percent; has skin caring, and ultraviolet preventing effects, and its physical properties are maintained at 70.4% under ultraviolet irradiation of 1.2 × 10-2w/in2 for 50 h; the modulus was 161N/tex.

All percentages used in the present invention are mass percentages unless otherwise indicated.

Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.