CN112251835A

CN112251835A - Olive-containing polyamide fiber and preparation method thereof

Info

Publication number: CN112251835A
Application number: CN202011196388.9A
Authority: CN
Inventors: 黄效华; 甄丽; 刘潇; 黄效龙; 穆伟华
Original assignee: Qingdao Baicao New Material Co ltd; Zhongke Textile Research Institute Qingdao Co ltd; Bestee Material Qingdao Co ltd
Current assignee: Qingdao Baicao New Material Co ltd; Zhongke Textile Research Institute Qingdao Co ltd; Bestee Material Qingdao Co ltd
Priority date: 2020-10-31
Filing date: 2020-10-31
Publication date: 2021-01-22

Abstract

The invention provides a polyamide fiber containing olive and a preparation method thereof, wherein the preparation method comprises the following steps: preparing olive extracting solution, preparing porous nano particles, preparing the porous nano particles containing the olive extract, and preparing the functional master batch. The invention has the beneficial effects that: the prepared porous nanoparticles containing the olive extract have good distribution in the fiber, the inhibition rate of the polyamide fiber to staphylococcus aureus is more than or equal to 99.8%, the inhibition rate to escherichia coli is more than or equal to 95.4%, and the inhibition rate to candida albicans is more than or equal to 92.7%; the breaking strength is more than or equal to 6.2cN/dtex, the elongation at break is more than or equal to 39 percent, and the yellowing resistance grade is 5 grade.

Description

Olive-containing polyamide fiber and preparation method thereof

Technical Field

The invention relates to the field of polyamide fiber, in particular to polyamide fiber containing olive 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 taking olive leaf infused tea was the traditional treatment of 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 effective components in olive leaf include iridoid, flavone and its glycoside, biflavone and its glycoside, and low molecular tannin, and the most active components are oleuropein and hydroxytyrosol. The active ingredients in the olive leaves can protect skin cells from being damaged by ultraviolet rays, prevent the ultraviolet rays from decomposing skin membrane lipid, promote the fibroblast to generate collagen, reduce the secretion of fibroblast collagen enzyme, prevent the anti-glycan reaction of cell membranes, naturally resist the damage of the skin caused by oxidation, prevent the damage of the UV ultraviolet rays, effectively maintain the tenderness and the elasticity of the skin and achieve the effects of strengthening and tendering the skin.

The nylon fiber, also called nylon, has the most outstanding advantages that the abrasion resistance is higher than that of all other fibers, 10 times higher than that of cotton and 20 times higher than that of wool, and the abrasion resistance can be greatly improved by slightly adding some nylon fibers into the blended fabric; when the stretch is extended to 3-6%, the elastic recovery rate can reach 100%; can withstand ten thousand times of bending without breaking.

The nylon fiber product has wide application, uses plastic to replace good materials of steel, iron, copper and other metals, and is important engineering plastic; the cast nylon can be used to replace antiwear parts of mechanical equipment and copper and alloy. The lead screw is suitable for manufacturing wear-resistant parts, transmission structural parts, household appliance parts, automobile manufacturing parts, lead screw prevention mechanical parts, chemical equipment and the like.

Along with the development and progress of the times and the improvement of the living standard of people, the functional improvement of the nylon fiber is more and more. The common functional fiber preparation methods mainly comprise two methods: one is to directly add functional auxiliary agent in the spinning process to prepare functional fiber. Another approach is to attach functional ingredients to the fiber surface by post-treatment, thereby imparting a degree of functionality to the fiber. In the first method, the functional aid can be effectively dispersed in the fiber, and the fiber can be provided with permanent functionality. In the second method, the functional additives on the surface of the fiber are easy to lose and the functionality is not durable.

In the prior art of producing nylon fiber by adopting the first production process, the processes of loading a functional additive on nano silica particles, preparing functional master batches and finally mixing and spinning are reported. The applicant finds that in the process of preparing the polyamide fiber by adopting the process, due to the characteristic that nano silicon dioxide particles tend to agglomerate, when the polyamide fiber is used as a carrier loaded with functional components, the distribution of the polyamide fiber in the fiber is poor, the modification effect is not ideal, and the characteristic of the functional components cannot fully play a modifying role on the fiber.

Furthermore, in the research process of modifying chinlon by using olive as a plant modification material, the applicant finds that when the effective components extracted from olive are loaded on a common carrier, the loading effect is not ideal and the process requirements cannot be met. When the effective components are loaded on the nano silicon dioxide particles, although the loading effect is good, the processing stability is not ideal, and the performance of polyamide fiber products in different batches is inconsistent, so that the large-scale and standardized production of functional polyamide fiber products is influenced.

Disclosure of Invention

In order to solve the technical problems in the prior art, the invention provides a polyamide fiber containing olive and a preparation method thereof, so as to realize the following purposes:

(1) the distribution of the nanometer silicon dioxide particles loaded with the olive effective components in the nylon fiber is improved;

(2) improving the processing stability of the nano-silica particles loaded with olive active ingredients.

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

a preparation method of olive-containing polyamide fiber comprises the following steps: preparing olive extracting solution, preparing porous nano particles containing olive extracts, and preparing functional master batches;

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

the preparation of the porous nano-particles comprises the following steps: preparing and molding silicon dioxide sol;

the preparation of the silica sol comprises the steps of mixing absolute ethyl alcohol with deionized water, then adding hexadecyl trimethyl ammonium bromide and ammonia water, stirring at 200-300RPM for 5-10min, dropwise adding tetraethoxysilane, and continuously stirring for 1-1.5h to prepare the silica sol;

the forming is carried out, the silicon dioxide sol is placed at the temperature of 210 ℃ and 220 ℃ and under the condition of 15-18MPa for supercritical drying until the moisture content is less than 0.5 percent; then calcining at the temperature of 500-600 ℃ for 3-5h to obtain the porous nano-particles.

The particle size of the porous nano-particles is 500-600nm, the pore diameter is 20-30nm, and the specific surface is 700-800m²/g。

Further, the preparation of the porous nanoparticles further comprises: activating;

the activation is carried out, the molded porous nano 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 s; and then pressurizing to 15-20MPa within 30s, maintaining the pressure for 5min, and rapidly relieving the pressure to normal pressure within 1.5s to complete the activation step of the porous nanoparticles.

Further, the preparation of the olive extract-containing porous nanoparticles comprises the preparation, loading and modification of a porous nanoparticle dispersion liquid;

preparing the porous nano-particle dispersion liquid, namely putting the porous nano-particles into absolute ethyl alcohol, and grinding and dispersing to obtain the porous nano-particle dispersion liquid;

and the loading step comprises the steps of mixing the olive extracting solution and the porous nano-particle dispersion liquid with a surfactant and a stabilizer, and repeatedly grinding and dispersing for 3-5 times, wherein the grinding time is 20-30min each time.

Further, the preparation of the olive extract comprises the following steps: the weight ratio of the olive fruit extract is 1: 5-6;

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%.

Preferably, the preparation of the silica sol, the absolute ethanol: 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, the modification is carried out, namely, the loaded porous nano particles are put into a composite modification liquid with the volume of 3-4 times, the temperature is raised to 40-50 ℃, and the mixture is stirred;

the composite modifying solution comprises the following components: butyl titanate, neodecanoic acid glycidyl ester, polyethylene glycol, polyvinylpyrrolidone, pentaerythritol, methyl nicotinate and absolute ethyl alcohol.

Further, preparing the functional master batch, namely mixing nylon 66 slices, the porous nanoparticles containing olive extracts, an antioxidant SEED, triisodecyl phosphite, polycaprolactone and a silane coupling agent KH-570, heating to 280 ℃, preserving heat, mixing and melting for 30-40min, and granulating to obtain the functional master batch.

Preferably, the weight ratio of the chinlon 66 slices, the porous nanoparticles containing the olive extracts, the antioxidant SEED, the triisodecyl phosphite, the polycaprolactone and the silane coupling agent KH-570 is 180-fold and 200:25-30:5-8:1-3:1-3: 1-3.

Further, in the spinning, common chinlon 66 chips and the functional mother particles are mixed, extruded and melted at 260 ℃, and spun after metering to prepare fibers;

the common chinlon 66 slices: the ratio of the functional master batch to the functional master batch is 100:1-8 by weight.

The porous nanoparticles containing olive extracts, which are adopted by the invention, contain functional groups of olive iridoid substances, flavone and flavonoid glycoside, biflavone and biflavone glycoside and the like on the surfaces, and functional groups of lipids and alcohols, and can be grafted with functional groups of polyamide fibers. Therefore, the porous nanoparticles containing the olive extract are tightly and firmly combined with the polyamide fiber, are not easy to run off or lose efficacy, can fully exert the modification effect of the olive active ingredients on the polyamide fiber, have stable and lasting modification effect, and can effectively avoid performance attenuation and yellowing phenomenon of the polyamide fiber or products after long-term storage or long-term use.

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

(1) according to the preparation method of the polyamide fiber containing the olive, the prepared porous nanoparticles containing the olive extract have good distribution in the fiber, the modification effect of the active ingredients of the olive on the polyamide fiber can be fully exerted, the bacteriostasis rate of the polyamide fiber on staphylococcus aureus is more than or equal to 99.8%, the bacteriostasis rate on escherichia coli is more than or equal to 95.4%, and the bacteriostasis rate on candida albicans is more than or equal to 92.7%.

(2) In the porous nanoparticles containing the olive extracts prepared from the olive-containing polyamide fibers, the active ingredients are stably loaded on the porous nanoparticles, the long-term stability is good, the modification effect on the polyamide fibers is stable and durable, and the antibacterial performance of the polyamide fibers is reduced by less than 7.4% after 100 times of standard washing.

(3) The olive-containing nylon fiber has the functions of skin care, skin moistening and ultraviolet resistance, and can effectively reduce the anaphylactic reaction of people who are easy to be allergic to nylon fiber products.

(4) The olive-containing polyamide fiber has an anti-oxidation function, and can effectively avoid the yellowing phenomenon and the performance attenuation phenomenon of the polyamide fiber or a product after long-term storage or use.

(5) The olive-containing polyamide fiber has the breaking strength of more than or equal to 6.2cN/dtex, the elongation at break of more than or equal to 39 percent and the yellowing resistance grade of 5.

(6) The preparation method of the olive-containing polyamide fiber effectively improves the processing stability of the porous nanoparticles containing the olive extract, and can meet the large-scale and standardized production requirements of functional polyamide fiber products.

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 preparation method of olive-containing polyamide fiber comprises the steps of preparing olive extract, preparing porous nanoparticles containing olive extract, preparing functional master batches, spinning and post-processing.

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 1h, and filtering to obtain solid substance.

The ultrasonic frequency is 20kHz, and the ultrasonic intensity is 10W/cm²And the ultrasonic power is 350W.

The olive leaf extract: the olive fruit extract has a weight ratio of 1: 5.

The olive leaf extract has oleuropein content of 33%, hydroxytyrosol content of 16%, and mesh number of 80 mesh.

The olive fruit extract has the olive polyphenol content of 17 percent and the mesh number of 80 meshes.

The preparation of the porous nano-particles comprises the steps of silica sol preparation, molding and activation.

The preparation method of the silica sol comprises the steps of mixing anhydrous ethanol and deionized water in a preset portion, then adding Cetyl Trimethyl Ammonium Bromide (CTAB) and ammonia water in a preset portion, stirring at 200RPM for 5min, dropwise adding Tetraethoxysilane (TEOS) in a preset portion, and continuously stirring for 1h to obtain the silica sol.

The absolute ethyl alcohol: deionized water: cetyl trimethylammonium bromide: ammonia water: the volume ratio of the ethyl orthosilicate is 90: 5: 5: 8: 20.

the forming is carried out, the silicon dioxide sol is placed at the temperature of 210 ℃ and under the pressure 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 porous nano-particles.

The porous nano-particles are SiO₂A particle diameter of 600nm, a pore diameter of 20nm and a specific surface area of 700m²/g。

The activation is carried out, the porous nano 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 s; and then pressurizing to 15MPa within 30s, maintaining the pressure for 5min, and rapidly relieving the pressure to normal pressure within 1.5s to complete the activation step of the porous nanoparticles.

The preparation of the porous nanoparticles containing the olive extract comprises the preparation, loading and modification of a porous nanoparticle dispersion liquid.

And (2) preparing the porous nano-particle dispersion liquid, namely putting the porous nano-particles into absolute ethyl alcohol, adding the absolute ethyl alcohol into a ball mill, grinding, shearing and dispersing the absolute ethyl alcohol, and uniformly mixing the absolute ethyl alcohol and the porous nano-particles to obtain the porous nano-particle dispersion liquid.

The porous nanoparticles are: the volume ratio of the absolute ethyl alcohol is 1: 1.5.

The loading step, mixing the olive extract and the porous nanoparticle dispersion liquid with a surfactant and a stabilizer, and repeatedly grinding and dispersing for 3 times, wherein the grinding speed is 500RPM, and the grinding time is 20min each time, so as to prepare the porous nanoparticles containing the olive extract; then evaporating the solvent to remove the ethanol, and obtaining the dried porous nanoparticles containing olive extract.

The olive extracting solution: porous nanoparticle dispersion liquid: the mass ratio of the surfactant to the stabilizer is 20:10:1: 1;

the surfactant is glycerol trioleate.

The stabilizer is sodium stearate.

And in the modification step, the loaded porous nano particles are put into 3 times of volume of composite modification liquid, the temperature is raised to 40 ℃, the stirring speed is 200RPM, the stirring is carried out for 2 hours, and the porous nano particles are separated.

The composite modified liquid comprises butyl titanate, glycidyl neodecanoate, polyethylene glycol, polyvinylpyrrolidone, pentaerythritol, methyl nicotinate and absolute ethyl alcohol.

The weight ratio of the butyl titanate to the glycidyl neodecanoate to the polyethylene glycol to the polyvinylpyrrolidone to the pentaerythritol to the methyl nicotinate to the absolute ethyl alcohol is 2:5:3:1:4:3: 20.

The preparation method of the functional master batch comprises the steps of mixing nylon 66 slices, porous nanoparticles containing olive extracts, an antioxidant SEED, triisodecyl phosphite, polycaprolactone and a silane coupling agent KH-570, heating to 280 ℃, keeping the temperature, mixing and melting for 30min, and granulating to obtain the functional master batch.

The weight ratio of the chinlon 66 slices, the porous nanoparticles containing the olive extracts, the antioxidant SEED, the triisodecyl phosphite, the polycaprolactone and the silane coupling agent KH-570 is 180:25: 8:1:1: 1.

And in the spinning step, common chinlon 66 chips and the functional mother particles are mixed, extruded and melted at 260 ℃, and spun after metering to prepare the fiber.

The common chinlon 66 slices: the ratio of the functional master batch to the functional master batch by weight is 100: 1.

And extruding and melting, wherein the pressure of a screw is 70kg/cm, and the rotating speed of the screw is 18 r/min.

And the post-treatment comprises oiling, winding and drafting.

And carrying out post-treatment on the fiber to obtain the olive-containing polyamide fiber.

The winding speed is 550 m/min.

The drafting is carried out by 3.3 times of drafting times and the drafting temperature is 105 ℃.

Through detection, the olive-containing polyamide fiber of the embodiment has 99.8% of inhibition rate on staphylococcus aureus, 95.4% of inhibition rate on escherichia coli and 92.7% of inhibition rate on candida albicans; after 100 times of standard washing, the antibacterial performance of the nylon fiber is reduced by 7.2 percent; the breaking strength is 6.2cN/dtex, the elongation at break is 39%, and the yellowing resistance grade is 5.

Example 2

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 150RPM for 15min, heating to 50 deg.C, performing ultrasonic extraction for 1.5h, and filtering to obtain solid substance.

The olive leaf extract: the weight ratio of the olive fruit extract is 1: 6.

The preparation of the silica sol comprises the steps of mixing absolute ethyl alcohol and deionized water in a preset portion, then adding Cetyl Trimethyl Ammonium Bromide (CTAB) and ammonia water in a preset portion, stirring at 300RPM for 10min, dropwise adding Tetraethoxysilane (TEOS) in a preset portion, and continuously stirring for 1.5h to obtain the silica sol.

The absolute ethyl alcohol: deionized water: cetyl trimethylammonium bromide: ammonia water: the volume ratio of the ethyl orthosilicate is 100: 8: 10: 10: 25.

the forming is carried out, the silicon dioxide sol is placed at 210 ℃ and under the condition of 16MPa, and supercritical drying is carried out until the moisture content is less than 0.5%; then calcining at 600 ℃ for 4h to obtain the porous nano-particles.

The porous nano-particles are SiO₂Particle size of 500nm, pore diameter of 30nm, and specific surface area of 800m²/g。

The activation is carried out, the porous nano 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 s; and then pressurizing to 16MPa within 30s, maintaining the pressure for 5min, and rapidly relieving the pressure to normal pressure within 1.5s to complete the activation step of the porous nanoparticles.

The porous nanoparticles are: the volume ratio of the absolute ethyl alcohol is 1: 2.0.

The loading step, mixing the olive extract and the porous nanoparticle dispersion liquid with a surfactant and a stabilizer, and repeatedly grinding and dispersing for 4 times, wherein the grinding speed is 550RPM, and the grinding time is 25min each time, so as to prepare the porous nanoparticles containing the olive extract; then evaporating the solvent to remove the ethanol, and obtaining the dried porous nanoparticles containing olive extract.

the surfactant is glycerol trioleate.

The stabilizer is sodium stearate.

And in the modification step, the loaded porous nano particles are put into a composite modification solution with 4 times of volume, the temperature is raised to 45 ℃, the stirring speed is 300RPM, the stirring is carried out for 3 hours, and the porous nano particles are separated.

The weight ratio of the butyl titanate to the glycidyl neodecanoate to the polyethylene glycol to the polyvinylpyrrolidone to the pentaerythritol to the methyl nicotinate to the absolute ethyl alcohol is 3:5:1:1:4:3: 25.

The preparation method of the functional master batch comprises the steps of mixing nylon 66 slices, porous nanoparticles containing olive extracts, an antioxidant SEED, triisodecyl phosphite, polycaprolactone and a silane coupling agent KH-570, heating to 280 ℃, keeping the temperature, mixing and melting for 40min, and granulating to obtain the functional master batch.

The weight ratio of the chinlon 66 slices, the porous nanoparticles containing the olive extracts, the antioxidant SEED, the triisodecyl phosphite, the polycaprolactone and the silane coupling agent KH-570 is 190: 30:6:2:3: 1.

The common chinlon 66 slices: the ratio of the functional master batch to the functional master batch in parts by weight is 100: 7.

And extruding and melting, wherein the pressure of a screw is 80kg/cm, and the rotating speed of the screw is 22 r/min.

And the post-treatment comprises oiling, winding and drafting.

And the winding speed is 600 m/min.

Through detection, the olive-containing polyamide fiber of the embodiment has 99.9% of inhibition rate on staphylococcus aureus, 96.8% of inhibition rate on escherichia coli and more than 94.1% of inhibition rate on candida albicans; after 100 times of standard washing, the antibacterial performance of the nylon fiber is reduced by 5.1 percent; the breaking strength is 6.6cN/dtex, the elongation at break is 44%, and the yellowing resistance grade is 5.

Example 3

The olive leaf extract: the weight ratio of the olive fruit extract is 1: 6.

The preparation of the porous nano-particles comprises the steps of molecular nest pretreatment, silica sol preparation, loading, forming and activation.

And (3) pretreating the molecular nest, namely grinding a predetermined part of molecular nest particles until the mesh number range D50 is mum, then placing the molecular nest particles in a vacuum environment, heating to 260 ℃, preserving heat for 2 hours, and naturally cooling to the normal temperature.

The molecular nest particleIs diatomite granule with particle size of 350 meshes and density of 0.35-0.4g/cm³。

loading, namely putting a predetermined part of molecular nest particles into silica sol, stirring at 150RPM, and standing for gel aging until the molecular nest particles absorb more than 80% of the silica sol until the gel is completely gelled; finally separating out the molecular nest particles.

The molecular nest particle: the silica sol had a weight ratio of 1: 2.5.

And (3) forming, namely placing the loaded molecular nest particles at 210 ℃ under the condition of 16MPa, performing supercritical drying until the moisture content is less than 0.5%, and naturally cooling to room temperature to obtain the porous nano particles.

The porosity of the porous nano-particles is 96%, and the specific surface area is 800m²/g。

the surfactant is glycerol trioleate.

The stabilizer is sodium stearate.

And (3) modifying, namely putting the activated porous nanoparticles into a composite modification solution with 4 times of volume, heating to 45 ℃, stirring at 300RPM for 3h, and separating the porous nanoparticles.

And the post-treatment comprises oiling, winding and drafting.

And the winding speed is 600 m/min.

Through detection, the olive-containing polyamide fiber of the embodiment has 99.9% of inhibition rate on staphylococcus aureus, 98.9% of inhibition rate on escherichia coli and more than 96.7% of inhibition rate on candida albicans; after 100 times of standard washing, the antibacterial performance of the nylon fiber is reduced by 4.8 percent; the breaking strength is 6.9cN/dtex, the elongation at break is 46 percent, and the yellowing resistance grade is 5 grade.

Comparative example 1

The technical scheme of the embodiment 2 is adopted, and the difference is that: the step of preparing porous nanoparticles is eliminated, and the porous nanoparticles used in the step of preparing porous nanoparticles containing olive extract are replaced by porous nanoparticles having a particle size range of 350 mesh and a density range of 0.35-0.4g/cm³Diatomaceous earth particles of (1).

Through detection, the olive-containing polyamide fiber of the comparative example has the bacteriostasis rate of 84.3 percent on staphylococcus aureus, 80.2 percent on escherichia coli and more than 79.6 percent on candida albicans; after 100 times of standard washing, the antibacterial performance of the nylon fiber is reduced by 29.8 percent; the breaking strength is 6.0cN/dtex, the elongation at break is 38%, and the anti-yellowing grade is 3.

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.

Claims

1. A preparation method of olive-containing polyamide fiber is characterized by comprising the following steps: preparing olive extracting solution, preparing porous nano particles containing olive extracts, and preparing functional master batches;

the forming is carried out, the silicon dioxide sol is placed at the temperature of 210 ℃ and 220 ℃ and under the condition of 15-18MPa for supercritical drying until the moisture content is less than 0.5 percent; then calcining at the temperature of 500-600 ℃ for 3-5h to obtain the porous nano-particles;

2. The method for preparing olive-containing polyamide fiber according to claim 1, wherein the preparation of the porous nanoparticles further comprises: activating;

3. The preparation method of olive-containing polyamide fiber according to claim 1, wherein the preparation of the olive extract-containing porous nanoparticles comprises preparation, loading and modification of a porous nanoparticle dispersion liquid;

4. The method for preparing olive-containing polyamide fiber according to claim 1, wherein the preparation of the olive extract comprises the following steps: the weight ratio of the olive fruit extract is 1: 5-6;

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

5. The method for preparing olive-containing polyamide fiber according to claim 1, wherein the preparation of the silica sol is carried out by mixing the following components in percentage by weight: 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 preparation method of olive-containing polyamide fiber according to claim 3, wherein the modification comprises putting the loaded porous nanoparticles into a 3-4 times volume of composite modification liquid, heating to 40-50 ℃, and stirring;

7. The method for preparing polyamide fiber containing olive according to claim 1, wherein the preparation of the functional masterbatch is that polyamide 66 slices, porous nanoparticles containing olive extract, antioxidant SEED, triisodecyl phosphite, polycaprolactone, silane coupling agent KH-570 are mixed, heated to 280 ℃ for heat preservation, mixed and melted for 30-40min, and granulated to obtain the functional masterbatch.

8. The method for preparing polyamide fiber containing olive as claimed in claim 7, wherein the weight ratio of polyamide 66 slices, porous nanoparticles containing olive extract, antioxidant SEED, triisodecyl phosphite, polycaprolactone, silane coupling agent KH-570 is 180-.

9. The preparation method of olive-containing nylon fiber according to claim 1, wherein the spinning is carried out by mixing common nylon 66 chips with the functional mother particles, extruding and melting at 260 ℃, metering, and spinning to obtain fiber;

10. An olive-containing polyamide fiber, characterized by being produced according to the production method of any one of claims 1 to 9.