Polyester BI fiber containing active ingredients of lemon balm and valerian and preparation method of polyester BI fiber

Abstract

The invention relates to the technical field of functional fibers, and particularly discloses a polyester BI fiber containing lemon balm and valerian active ingredients and a preparation method of the polyester BI fiber containing the lemon balm and valerian active ingredients. Comprising the following raw materials in parts by weight: 100-300 parts of polyester chips, 10-20 parts of microspheres containing lemon balm and valerian active ingredients, and 2-5 parts of a dispersing agent. According to the microspheres containing the active ingredients of the lemon balm and the valerian, the active ingredients of the lemon balm and the valerian are stably included in a cavity of beta-cyclodextrin, and guar gum assists in dissolution and emulsification, so that the microspheres with stable performance are formed; active ingredients of the lemon balm and the valerian are slowly released from the interiors of the microspheres, so that the polyester BI fiber is endowed with a long-term antibacterial function and a remarkable soothing and calming function.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of functionalized fibers, more particularly, it relates to a polyester BI fiber containing active ingredients of lemon balm and valerian and a preparation method thereof. BACKGROUND

[0002] The appearance of polyester BI fiber (BI for Bioactives Inside) greatly improves the skin-friendly performance of polyester fiber, which is an intelligent fiber that integrates biologically active substances (such as plant extracts, minerals, prebiotics, etc.) into the fiber through special technology, allowing it to have long-lasting, stable health functions. Lemon balm is rich in volatile essential oils, flavonoids, phenolic acids, terpenes and other active ingredients throughout the plant, with a fresh lemon scent, and also has significant soothing, anti-anxiety, antibacterial and other biological activities. Valerian is a traditional medicinal plant, and its roots and rhizomes are rich in sesquiterpenes, flavonoids, alkaloids and other active ingredients, which have significant effects of calming the nerves, anti-anxiety and improving sleep disorders. In addition, the active ingredients of valerian also have certain antibacterial and anti-inflammatory effects, and can inhibit common pathogenic bacteria, thereby enhancing the health protection performance of textiles.

[0003] Introducing lemon balm and valerian active ingredients into polyester fibers can give textiles natural antibacterial and soothing functions to meet the high demands of consumers. Currently, existing technologies mostly apply lemon balm and valerian active ingredients to textiles through post-finishing methods such as coating and dipping. However, the thermal stability of the active ingredients of both is poor, and direct addition to the polyester melt spinning system can cause thermal degradation, resulting in loss of function and difficulty in achieving long-term stable functional attachment. At the same time, the compatibility of lemon balm and valerian active ingredients with polyester fibers is poor, and direct blending spinning can cause aggregation, leading to a decrease in fiber mechanical properties. These defects are key technical obstacles that restrict the application of lemon balm and valerian active ingredients in polyester fibers.

[0004] Based on the above statement, the present application proposes a new type of polyester BI fiber containing lemon balm and valerian active ingredients. SUMMARY

[0005] In view of the deficiencies of the prior art, the present application provides a polyester BI fiber containing lemon balm and valerian active ingredients and a preparation method thereof, so that the polyester BI fiber can stably release lemon balm and valerian active ingredients for a long time to achieve long-term antibacterial purposes, and the mechanical properties of the polyester BI fiber are excellent, thereby making the polyester BI fiber have significant soothing, antibacterial functions.

[0006] In a first aspect, the present application provides a polyester BI fiber containing lemon balm and valerian active ingredients, which adopts the following technical scheme: A polyester BI fiber containing active ingredients of lemon balm and valerian, comprising the following raw materials in parts by weight: polyester chips 100-300 parts, microspheres containing active ingredients of lemon balm and valerian 10-20 parts, dispersing agent 2-5 parts.

[0007] Preferably, the preparation method of the microspheres containing active ingredients of lemon balm and valerian comprises the following steps: After dissolving lemon balm extract, valerian extract and β-cyclodextrin in ethanol, adding a guar gum aqueous solution, ultrasonic dispersion, and adding polyvinyl alcohol dropwise under stirring, continuing to stir after the end of dropwise addition to form an emulsion, vacuum drying, and grinding to obtain microspheres containing active ingredients of lemon balm and valerian.

[0008] Preferably, the mass ratio of the lemon balm extract, valerian extract, β-cyclodextrin, ethanol, guar gum aqueous solution, and polyvinyl alcohol is 1-4:2:10-20:40-60:5-15:2-5; and the concentration of the guar gum aqueous solution is 1-5wt%.

[0009] Preferably, the preparation method of the lemon balm extract comprises the following steps: The plasma pretreated lemon balm dry leaves are crushed to obtain lemon balm powder; The lemon balm powder is added into a eutectic solvent, stirred uniformly, vacuum packaged, placed in an ultrahigh pressure treatment device for extraction, centrifuged, and the supernatant is taken, vacuum concentrated to obtain lemon balm extract.

[0010] Preferably, the plasma pretreatment conditions are: working gas is air, power is 10-50W, treatment time is 20-60s, and treatment distance is 2-5cm.

[0011] Preferably, the extraction conditions of the ultrahigh pressure treatment device are: extraction pressure is 300-400MPa, and extraction time is 10-15min.

[0012] Preferably, the solid-liquid ratio of the lemon balm powder and the eutectic solvent is 1g:20-30mL; and the water content of the eutectic solvent is 35-50wt%, including ethylene glycol and oxalic acid in a molar ratio of 1:2-4.

[0013] Preferably, the preparation method of the valerian extract comprises the following steps: The valerian dry rhizome is crushed to obtain valerian dry powder; the valerian dry powder is added into an ethanol solution, ultrasonic extracted, filtered, reduced pressure concentrated, and dried to obtain valerian extract.

[0014] Preferably, the material-liquid ratio of the valerian dry powder and the ethanol solution is 1g:10-30mL; the concentration of the ethanol solution is 30-70wt%; the ultrasonic extraction conditions are: power 100-200W, time 20-60min, and temperature 30-70°C.

[0015] Preferably, the dispersant is polyethylene glycol with a molecular weight of 2000-6000.

[0016] In a second aspect, the present application provides a preparation method of polyester BI fiber containing lemon balm and valerian active ingredients, which adopts the following technical scheme: A preparation method of polyester BI fiber containing lemon balm and valerian active ingredients, comprising the following steps: S1, uniformly mixing microspheres containing lemon balm and valerian active ingredients and a dispersant to obtain a mixture; S2, melting the polyester chips at a temperature of 235-240°C and a screw rotation speed of 250-280r / min for 1-1.5h, then adding the mixture, melt blending for 3-5min, the melt temperature is 235-240°C, and the screw rotation speed is 255-275r / min; then extruding, cooling, granulating, and drying to obtain polyester granules; S3, extruding and melting the polyester granules at 255-265°C, spinning, controlling the spinning speed to be 1700-1750m / min, then drawing, oiling, and winding to obtain polyester BI fiber containing lemon balm and valerian active ingredients.

[0017] In summary, the present application has the following beneficial effects: (1) The polyester BI fiber containing lemon balm and valerian active ingredients of the present application comprises polyester chips, microspheres containing lemon balm and valerian active ingredients, and a dispersant, and the components interact with each other, which not only improves the antibacterial performance stability and durability of the polyester BI fiber, but also improves the mechanical properties of the polyester BI fiber.

[0018] (2) The microspheres containing lemon balm and valerian active ingredients of the present application can stably encapsulate lemon balm and valerian active ingredients in the cavity of β-cyclodextrin, and form stable microspheres with the help of guar gum solubilization and emulsification; the lemon balm and valerian active ingredients are slowly released from the inside of the microspheres, so that the polyester BI fiber has long-term stable antibacterial performance; in addition, the microspheres can better compatibilize with polyester molecules, which is conducive to enhancing the mechanical properties of the polyester BI fiber.

[0019] (3) In this invention, the dried leaves of lemon balm are first pretreated with plasma to form micropores on the leaf surface and destroy the cell wall structure. Then, they are mixed with a eutectic solvent and extracted under ultra-high pressure to force the eutectic solvent to penetrate and dissolve the active ingredients. The preparation method of lemon balm extract of this invention not only has high extraction efficiency, but also can protect the active ingredients from being destroyed to a great extent, thereby making the polyester BI fiber have excellent antibacterial properties.

[0020] (4) This invention contains lemon balm extract and valerian extract, which work synergistically to enhance the stability and durability of the antibacterial properties of polyester BI fiber, and the mechanical properties of polyester BI fiber are also superior.

[0021] (5) The preparation method of polyester BI fiber containing lemon balm and valerian active ingredients of the present invention is simple, low in cost, and suitable for industrial production. The resulting polyester BI fiber has significant soothing and calming and antibacterial functions, which can meet higher market demands. Detailed Implementation

[0022] The present invention will be further described in detail below with reference to the embodiments.

[0023] Examples 1-3 provide a polyester BI fiber containing lemon balm and valerian active ingredients and its preparation method.

[0024] Example 1 A polyester BI fiber containing lemon balm and valerian active ingredients comprises the following raw materials in parts by weight: 100 parts of polyester chips (semi-dull SD501, China Petroleum & Chemical Corporation), 10 parts of microspheres containing lemon balm and valerian active ingredients, and 2 parts of dispersant. A method for preparing microspheres containing active ingredients from lemon balm and valerian includes the following steps: Lemon balm extract, valerian extract, and β-cyclodextrin were dissolved in ethanol and stirred at 300 rpm for 15 min. Then, guar gum aqueous solution (1 wt%) was added and dispersed under ultrasonication at 150 W for 10 min. Polyvinyl alcohol was then added dropwise at 1 mL / min while stirring at 60 rpm. After the addition was completed, stirring was continued at the same speed for 30 min to form an emulsion. The emulsion was then vacuum dried at 40℃ and 0.09 MPa for 24 h, ground, and passed through a 200-mesh sieve to obtain microspheres containing the active ingredients of lemon balm and valerian. The mass ratio of lemon balm extract, valerian extract, β-cyclodextrin, ethanol, guar gum aqueous solution, and polyvinyl alcohol was 1:2:10:40:5:2. The preparation method of lemon balm extract includes the following steps: The lemon balm dry leaves are subjected to plasma pretreatment with air as working gas, power of 10 W, processing time of 20 s and processing distance of 2 cm, and then are crushed to obtain lemon balm powder; The lemon balm powder is added into a eutectic solvent (35wt% of water content, including ethylene glycol and oxalic acid in a molar ratio of 1:2) at a solid-liquid ratio of 1g:20mL, uniformly stirred, vacuum packaged, and subjected to extraction in an ultrahigh pressure treatment device, with an extraction pressure of 300 MPa and an extraction time of 10 min, centrifuged at a speed of 10000 rpm, and the supernatant is taken, vacuum concentrated to obtain lemon balm extract; A preparation method of valerian extract, comprising the following steps: The valerian dry rhizome is crushed to obtain valerian dry powder; the valerian dry powder is added into an ethanol solution (30wt%) at a solid-liquid ratio of 1g:30mL, ultrasonically extracted at a power of 100 W and a temperature of 30°C for 20 min, filtered, concentrated under reduced pressure, and dried to obtain valerian extract; The dispersant is polyethylene glycol with a molecular weight of 2000; A preparation method of polyester BI fiber containing active ingredients of lemon balm and valerian, comprising the following steps: S1, uniformly mixing microspheres containing active ingredients of lemon balm and valerian and a dispersant to obtain a mixture; S2, melting the polyester chips at a temperature of 235°C and a screw rotation speed of 250r / min for 1h, then adding the mixture, and melt blending for 3min at a melt temperature of 235°C and a screw rotation speed of 255r / min; then extruding, cooling, granulating, and drying to obtain polyester granules; S3, extruding and melting the polyester granules at 255°C, spinning, controlling the spinning speed to be 1700m / min, and then drawing, oiling, and winding to obtain polyester BI fiber containing active ingredients of lemon balm and valerian.

[0025] Example 2 A polyester BI fiber containing active ingredients of lemon balm and valerian, comprising the following raw materials by weight: polyester chips (semi-dull SD501, China Petroleum Chemical Corporation) 200 parts, microspheres containing active ingredients of lemon balm and valerian 15 parts, and dispersant 4 parts; A preparation method of microspheres containing active ingredients of lemon balm and valerian, comprising the following steps: The lemon balm extract, valerian extract and β-cyclodextrin are dissolved in ethanol, after stirring at a rotation speed of 400 rpm for 13 min, a guar gum aqueous solution (3 wt%) is added, and is dispersed under ultrasonic waves at a power of 180 W for 20 min, and then polyvinyl alcohol is added dropwise at a speed of 1.5 mL / min under stirring at a rotation speed of 700 rpm, after the dropwise addition is completed, the stirring is continued at the same rotation speed for 40 min to form an emulsion, and the emulsion is vacuum dried at a temperature of 40°C and a vacuum degree of 0.09 MPa for 30 h, ground, and sieved through a 200-mesh sieve to obtain microspheres containing active ingredients of lemon balm and valerian; wherein the mass ratio of the lemon balm extract, the valerian extract, the β-cyclodextrin, the ethanol, the guar gum aqueous solution and the polyvinyl alcohol is 3:2:15:50:10:4; A preparation method of lemon balm extract, comprising the following steps: The dried leaf blades of lemon balm are subjected to plasma pretreatment with air as working gas, a power of 30 W, a treatment time of 40 s and a treatment distance of 4 cm, and then are crushed to obtain lemon balm powder; The lemon balm powder is added into a eutectic solvent (containing 40 wt% of water, including ethylene glycol and oxalic acid at a molar ratio of 1:3) at a solid-liquid ratio of 1 g:25 mL, is uniformly stirred, vacuum packaged, placed in an ultrahigh pressure treatment device, and subjected to extraction at an extraction pressure of 350 MPa and an extraction time of 13 min, and then is subjected to centrifugation at a speed of 10,000 rpm, and the supernatant is taken, vacuum concentrated, to obtain lemon balm extract; A preparation method of valerian extract, comprising the following steps: The dried rhizomes of valerian are crushed to obtain dried valerian powder; the dried valerian powder is added into an ethanol solution (50 wt%) at a solid-liquid ratio of 1 g:20 mL, and is subjected to ultrasonic extraction at a power of 150 W and a temperature of 50°C for 40 min, filtered, concentrated under reduced pressure, and dried to obtain valerian extract; The dispersant is polyethylene glycol with a molecular weight of 6,000; A preparation method of polyester BI fiber containing active ingredients of lemon balm and valerian, comprising the following steps: S1, uniformly mixing the microspheres containing active ingredients of lemon balm and valerian and the dispersant to obtain a mixture; S2, melting the polyester chips at a temperature of 238°C and a screw rotation speed of 260 r / min for 1 h, then adding the mixture, and melt blending for 4 min at a melt temperature of 238°C and a screw rotation speed of 265 r / min; and then extruding, cooling, pelletizing and drying to obtain polyester pellets; S3, extruding and melting the polyester pellets at 260°C, spinning, controlling the spinning speed to be 1,725 m / min, and then drawing, oiling and winding to obtain polyester BI fiber containing active ingredients of lemon balm and valerian.

[0026] Example 3 A polyester BI fiber containing lemon balm and valerian active ingredients, comprising the following raw materials by weight: polyester chips (semi-dull SD501, China Petroleum Chemical Corporation) 300 parts, microspheres containing lemon balm and valerian active ingredients 20 parts, dispersant 5 parts; A method for preparing microspheres containing lemon balm and valerian active ingredients, comprising the following steps: The lemon balm extract, valerian extract and β-cyclodextrin are dissolved in ethanol, and after stirring at a speed of 500 rpm for 10 min, a guar gum aqueous solution (5 wt%) is added, dispersed under ultrasonic power of 200 W for 30 min, and polyvinyl alcohol is added dropwise at a speed of 2 mL / min under stirring at a speed of 800 rpm. After the dropwise addition is completed, the stirring is continued at the same speed for 45 min to form an emulsion. The emulsion is vacuum dried at a temperature of 40°C and a vacuum degree of 0.09 MPa for 36 h, ground, and sieved through a 200-mesh sieve to obtain the microspheres containing lemon balm and valerian active ingredients. The mass ratio of the lemon balm extract, valerian extract, β-cyclodextrin, ethanol, guar gum aqueous solution, and polyvinyl alcohol is 4:2:20:60:15:5. A method for preparing lemon balm extract, comprising the following steps: The dried leaf blades of lemon balm are subjected to plasma pretreatment with air as the working gas, a power of 50 W, a treatment time of 60 s, and a treatment distance of 5 cm, and then crushed to obtain lemon balm powder. The lemon balm powder is added into a eutectic solvent (containing 50 wt% water, including ethylene glycol and oxalic acid at a molar ratio of 1:4) at a solid-liquid ratio of 1 g:30 mL, uniformly stirred, vacuum packaged, and subjected to extraction in an ultrahigh-pressure treatment device at an extraction pressure of 400 MPa and an extraction time of 115 min. Centrifugation is performed at a speed of 10,000 rpm, and the supernatant is collected, vacuum concentrated, and subjected to drying to obtain the lemon balm extract. A method for preparing valerian extract, comprising the following steps: The dried rhizome of valerian is crushed to obtain dried valerian powder. The dried valerian powder is added into an ethanol solution (70 wt%) at a solid-liquid ratio of 1 g:30 mL, subjected to ultrasonic extraction at a power of 200 W and a temperature of 70°C for 60 min, filtered, concentrated under reduced pressure, and dried to obtain the valerian extract. The dispersant is polyethylene glycol with a molecular weight of 4000. A method for preparing a polyester BI fiber containing lemon balm and valerian active ingredients, comprising the following steps: S1, uniformly mixing the microspheres containing lemon balm and valerian active ingredients and the dispersant to obtain a mixture; S2, melt the polyester chip at a temperature of 240℃ and a screw rotation speed of 280r / min for 1.5h, then add the mixture, melt blend for 5min, the melt temperature is 240℃, the screw rotation speed is 275r / min; then extrude, cool, cut and dry to obtain polyester master granules; S3, melt the polyester master granules at 265℃, spin, control the spinning speed to be 1750m / min, then stretch, oil, and wind to obtain polyester BI fiber containing active ingredients of lemon balm and valerian.

[0027] In order to verify the comprehensive performance of the polyester BI fiber obtained in embodiments 1-3, comparative examples 1-5 are set, as follows: Comparative example 1 Comparative example 1 is different from embodiment 1 in that the lemon balm extract and the valerian extract are directly added to the polyester BI fiber as raw materials, as follows: A polyester BI fiber containing active ingredients of lemon balm and valerian, comprising the following raw materials by weight: polyester chip (semi-dull SD501, China Petroleum Chemical Corporation) 100 parts, lemon balm extract 4 parts, valerian extract 6 parts, dispersant 2 parts; A preparation method of lemon balm extract, comprising the following steps: The lemon balm dry leaves are pretreated by plasma with air as working gas, power of 10W, processing time of 20s, and processing distance of 2cm, and then are crushed to obtain lemon balm powder; The lemon balm powder is added into a eutectic solvent (containing 35wt% of water, including ethylene glycol and oxalic acid in a molar ratio of 1:2) at a solid-liquid ratio of 1g:20mL, is uniformly stirred, vacuum packaged, placed in an ultrahigh pressure treatment device, extracted at an extraction pressure of 300MPa for 10min, centrifuged at a speed of 10000rpm, and the supernatant is taken, vacuum concentrated to obtain lemon balm extract; A preparation method of valerian extract, comprising the following steps: The valerian dry rhizome is crushed to obtain valerian dry powder; the valerian dry powder is added into an ethanol solution (30wt%) at a solid-liquid ratio of 1g:30mL, ultrasonically extracted at a power of 100W and a temperature of 30°C for 20min, filtered, reduced pressure concentrated, and dried to obtain valerian extract; The dispersant is polyethylene glycol with a molecular weight of 2000; A preparation method of a polyester BI fiber containing active ingredients of lemon balm and valerian, comprising the following steps: S1, mix the lemon balm extract, the valerian extract, and the dispersant uniformly to obtain a mixture; S2, melt the polyester chip at 235℃ for 1h at a screw speed of 250r / min, then add the mixture and melt blend for 3min, the melt temperature is 235℃ and the screw speed is 255r / min; then extrude, cool, cut and dry to obtain polyester master batch; S3, melt the polyester master batch at 255℃, spin, control the spinning speed at 1700m / min, then draw, oil, and wind to obtain the polyester BI fiber containing active ingredients of lemon balm and valerian.

[0028] Comparative Example 2 Comparative Example 2, the difference from Example 1 is that the preparation method of lemon balm extract is different, which is as follows: A polyester BI fiber containing active ingredients of lemon balm and valerian, comprising the following raw materials by weight: polyester chip (semi-dull SD501, China Petroleum Chemical Corporation) 100 parts, microspheres containing active ingredients of lemon balm and valerian 10 parts, dispersing agent 2 parts; The preparation method of the microspheres containing active ingredients of lemon balm and valerian comprises the following steps: The lemon balm extract, valerian extract and β-cyclodextrin are dissolved in ethanol, stirred at a speed of 300rpm for 15min, then the aqueous guar gum solution (1wt%) is added, dispersed under ultrasonic power of 150W for 10min, and the polyvinyl alcohol is added dropwise at a speed of 1mL / min under stirring at a speed of 60rpm. After the dropwise addition is completed, continue to stir at the same speed for 30min to form an emulsion. Vacuum drying is carried out at a temperature of 40℃ and a vacuum degree of 0.09MPa for 24h, grinding, and sieving through a 200 mesh sieve to obtain the microspheres containing active ingredients of lemon balm and valerian; wherein the mass ratio of lemon balm extract, valerian extract, β-cyclodextrin, ethanol, aqueous guar gum solution and polyvinyl alcohol is 1:2:10:40:5:2; The preparation method of the lemon balm extract comprises the following steps: The lemon balm dry leaves are crushed to obtain lemon balm powder; The lemon balm powder is added into the eutectic solvent (containing water at a rate of 35wt%, including ethylene glycol and oxalic acid at a molar ratio of 1:2) at a material to liquid ratio of 1g:20mL, stirred uniformly, vacuum packaged, placed in an ultrahigh pressure treatment device for extraction, the extraction pressure is 300MPa and the extraction time is 10min, centrifuged at a speed of 10000rpm, take the supernatant, vacuum concentrated to obtain the lemon balm extract; The preparation method of the valerian extract comprises the following steps: Valerian dry root rhizome is crushed to obtain valerian dry powder; the valerian dry powder is added into an ethanol solution (30 wt%) according to a material-liquid ratio of 1 g:30 mL, ultrasonic extraction is carried out at a power of 100 W and a temperature of 30°C for 20 min, filtration is carried out, concentration is carried out under reduced pressure, and drying is carried out to obtain a valerian extract; The dispersant is polyethylene glycol with a molecular weight of 2000; A preparation method of a polyester BI fiber containing active ingredients of lemon balm and valerian, comprising the following steps: S1, uniformly mixing microspheres containing active ingredients of lemon balm and valerian and a dispersant to obtain a mixture; S2, melting the polyester chips at a temperature of 235°C and a screw rotation speed of 250 r / min for 1 h, then adding the mixture, melt blending for 3 min, the melt temperature is 235°C, and the screw rotation speed is 255 r / min; then extruding, cooling, granulating, and drying to obtain polyester granules; S3, extruding and melting the polyester granules at 255°C, spinning, controlling the spinning speed to be 1700 m / min, then drawing, oiling, and winding to obtain the polyester BI fiber containing active ingredients of lemon balm and valerian.

[0029] Comparative Example 3 Comparative Example 3 is the same as Example 1 except that the preparation method of the lemon balm extract is different, which is as follows: A polyester BI fiber containing active ingredients of lemon balm and valerian, comprising the following raw materials by weight: polyester chips (semi-dull SD501, China Petroleum Chemical Corporation) 100 parts, microspheres containing active ingredients of lemon balm and valerian 10 parts, and a dispersant 2 parts; A preparation method of microspheres containing active ingredients of lemon balm and valerian, comprising the following steps: The lemon balm extract, the valerian extract, and β-cyclodextrin are dissolved in ethanol, stirring at a rotation speed of 300 rpm for 15 min, then adding a guar gum aqueous solution (1 wt%), dispersing under ultrasonic waves at a power of 150 W for 10 min, adding polyvinyl alcohol at a speed of 1 mL / min under stirring at a rotation speed of 60 rpm, continuing to stir at the same rotation speed for 30 min after the addition is completed to form an emulsion, vacuum drying at a temperature of 40°C and a vacuum degree of 0.09 MPa for 24 h, grinding, and passing through a 200-mesh sieve to obtain the microspheres containing active ingredients of lemon balm and valerian; wherein the mass ratio of the lemon balm extract, the valerian extract, β-cyclodextrin, ethanol, the guar gum aqueous solution, and polyvinyl alcohol is 1:2:10:40:5:2; A preparation method of a lemon balm extract, comprising the following steps: The lemon balm dry leaves are subjected to plasma pretreatment with air as working gas, power of 10 W, processing time of 20 s and processing distance of 2 cm, and then are crushed to obtain lemon balm powder; The lemon balm powder is added into a eutectic solvent (35wt% of water content, including ethylene glycol and oxalic acid in a molar ratio of 1:2) at a solid-liquid ratio of 1g:20mL, stirred uniformly, and then subjected to ultrasonic extraction at a power of 100 W and a temperature of 30°C for 30 min, filtered, concentrated under reduced pressure, and dried to obtain a lemon balm extract; A preparation method of valerian extract, comprising the following steps: The valerian dry rhizome is crushed to obtain valerian dry powder; the valerian dry powder is added into an ethanol solution (30wt%) at a solid-liquid ratio of 1g:30mL, subjected to ultrasonic extraction at a power of 100 W and a temperature of 30°C for 20 min, filtered, concentrated under reduced pressure, and dried to obtain a valerian extract; The dispersant is polyethylene glycol with a molecular weight of 2000; A preparation method of a polyester BI fiber containing active ingredients of lemon balm and valerian, comprising the following steps: S1, uniformly mixing microspheres containing active ingredients of lemon balm and valerian and a dispersant to obtain a mixture; S2, melting the polyester chips at a temperature of 235°C and a screw rotation speed of 250r / min for 1h, then adding the mixture, melt blending for 3min, the melting temperature is 235°C, and the screw rotation speed is 255r / min; then extruding, cooling, granulating, and drying to obtain polyester granules; S3, extruding and melting the polyester granules at 255°C, spinning, controlling the spinning speed to be 1700m / min, and then drawing, oiling, and winding to obtain the polyester BI fiber containing active ingredients of lemon balm and valerian.

[0030] Comparative Example 4 Comparative Example 4 is the same as Example 1 except that the microspheres containing active ingredients of lemon balm are used to replace the microspheres containing active ingredients of lemon balm and valerian, and the specific steps are as follows: A polyester BI fiber containing active ingredients of lemon balm, comprising the following raw materials by weight: polyester chips (semi-dull SD501, China Petroleum Chemical Corporation) 100 parts, microspheres containing active ingredients of lemon balm 10 parts, and dispersant 2 parts; A preparation method of microspheres containing active ingredients of lemon balm, comprising the following steps: The lemon balm extract and the beta-cyclodextrin are dissolved in ethanol, after stirring at a rotation speed of 300 rpm for 15 min, a guar gum aqueous solution (1 wt%) is added, and dispersed under ultrasonic waves at a power of 150 W for 10 min, and then polyvinyl alcohol is added dropwise at a speed of 1 mL / min under stirring at a rotation speed of 60 rpm, after the dropwise addition is completed, the stirring is continued at the same rotation speed for 30 min to form an emulsion, and then vacuum drying is performed at a temperature of 40 DEG C and a vacuum degree of 0.09 MPa for 24 h, grinding and sieving through a 200 mesh sieve to obtain the microspheres containing the active ingredients of lemon balm; wherein the mass ratio of the lemon balm extract, the beta-cyclodextrin, the ethanol, the guar gum aqueous solution and the polyvinyl alcohol is 3:10:40:5:2; A preparation method of lemon balm extract, comprising the following steps: The dried lemon balm leaves are subjected to plasma pretreatment with air as the working gas, a power of 10 W, a treatment time of 20 s and a treatment distance of 2 cm, and then are crushed to obtain lemon balm powder; The lemon balm powder is added into a eutectic solvent (containing 35 wt% of water, including ethylene glycol and oxalic acid at a molar ratio of 1:2) at a solid-liquid ratio of 1 g:20 mL, is uniformly stirred, vacuum packaged, and subjected to extraction in an ultrahigh pressure treatment device at an extraction pressure of 300 MPa for 10 min, and then is subjected to centrifugation at a speed of 10000 rpm, and the supernatant is taken, vacuum concentrated to obtain the lemon balm extract; The dispersant is polyethylene glycol with a molecular weight of 2000; A preparation method of polyester BI fiber containing active ingredients of lemon balm, comprising the following steps: S1, uniformly mixing the microspheres containing active ingredients of lemon balm and the dispersant to obtain a mixture; S2, melting the polyester chips at a temperature of 235 DEG C and a screw rotation speed of 250 r / min for 1 h, then adding the mixture, and melt blending for 3 min at a melt temperature of 235 DEG C and a screw rotation speed of 255 r / min; and then extruding, cooling, pelletizing and drying to obtain polyester pellets; S3, extruding and melting the polyester pellets at 255 DEG C, spinning, controlling the spinning speed to be 1700 m / min, and then drawing, oiling and winding to obtain polyester BI fiber containing active ingredients of lemon balm.

[0031] Comparative Example 5 Comparative Example 5 is the same as Example 1 except that the microspheres containing active ingredients of valerian are used to replace the microspheres containing active ingredients of lemon balm and valerian in equal mass, and the specific steps are as follows: A polyester BI fiber containing lemon balm and valerian active ingredients, comprising the following raw materials by weight: polyester chips (semi-dull SD501, China Petroleum Chemical Corporation) 100 parts, microspheres containing valerian active ingredients 10 parts, dispersing agent 2 parts; A method for preparing microspheres containing valerian active ingredients, comprising the following steps: The valerian extract and β-cyclodextrin are dissolved in ethanol, after stirring at a speed of 300 rpm for 15 min, an aqueous guar gum solution (1 wt%) is added, and dispersed under ultrasonic power of 150 W for 10 min; polyvinyl alcohol is added dropwise at a speed of 1 mL / min under stirring at a speed of 60 rpm, and after the dropwise addition is completed, the stirring is continued at the same speed for 30 min to form an emulsion; the emulsion is vacuum dried at a temperature of 40°C and a vacuum degree of 0.09 MPa for 24 h, and then ground to obtain the microspheres containing valerian active ingredients; wherein the mass ratio of the valerian extract, β-cyclodextrin, ethanol, aqueous guar gum solution, and polyvinyl alcohol is 3:10:40:5:2; A method for preparing valerian extract, comprising the following steps: The valerian dry rhizome is crushed to obtain valerian dry powder; the valerian dry powder is added into an ethanol solution (30 wt%) at a material-liquid ratio of 1 g:30 mL, and ultrasonic extraction is performed at a power of 100 W and a temperature of 30°C for 20 min; filtration, vacuum concentration, and drying are performed to obtain the valerian extract; The dispersing agent is polyethylene glycol with a molecular weight of 2000; A method for preparing a polyester BI fiber containing valerian active ingredients, comprising the following steps: S1, uniformly mixing the microspheres containing valerian active ingredients and the dispersing agent to obtain a mixture; S2, melting the polyester chips at a temperature of 235°C and a screw speed of 250 r / min for 1 h, then adding the mixture, and melt blending for 3 min at a melt temperature of 235°C and a screw speed of 255 r / min; then extruding, cooling, granulating, and drying to obtain polyester granules; S3, extruding and melting the polyester granules at 255°C, spinning, controlling the spinning speed to be 1700 m / min, and then performing drawing, oiling, and winding to obtain the polyester BI fiber containing valerian active ingredients.

[0032] The polyester BI fibers obtained in Examples 1-3 and Comparative Examples 1-5 are respectively tested for various performance tests, and the following results are obtained: (1) The test is performed according to GB / T 20944.3-2008 "Evaluation of antibacterial properties of textiles Part 3: oscillation method". In addition, the 50-time standard washing is performed according to the method of GB / T 8629-2017, and the antibacterial rate is tested again, as shown in Table 1.

[0033] Table 1: From the data shown in Table 1 above, it can be seen that the polyester BI fibers obtained in Examples 1-3 have significantly improved antibacterial effect on the three common pathogenic bacteria, and can maintain excellent antibacterial performance after multiple washing, indicating that the polyester BI fibers of the present application have long-acting and stable antibacterial performance, thereby indicating that the polyester BI fibers can release active ingredients and maintain soothing and calming functions for a long time.

[0034] As can be seen from Comparative Example 1 and Comparative Example 1, the β-cyclodextrin molecules of the present application have a cavity structure, which can wrap the lemon balm extract and valerian extract in the cavity, and the guar gum and polyvinyl alcohol further promote the formation of stable microspheres, greatly maintaining the active ingredients in the lemon balm extract and valerian extract, thereby enabling the polyester BI fibers to have long-acting antibacterial performance.

[0035] As can be seen from Comparative Example 1 and Comparative Examples 2 and 3, the lemon balm extract of the present application is pretreated by plasma pretreatment and then extracted by ultrahigh pressure low eutectic solvent, which significantly improves the dissolution efficiency of the active ingredients of the lemon balm, thereby improving the antibacterial performance of the polyester BI fibers.

[0036] As can be seen from Comparative Example 1 and Comparative Examples 4 and 5, the interaction between the lemon balm extract and the valerian extract in the present application helps to improve the stability and durability of the antibacterial performance of the polyester BI fibers.

[0037] (2) The YG009 monofilament strength tester was used to test the mechanical properties of the fibers, the tensile rate was 400 mm / min, the clamping length was 200 mm, and the pre-tension was 5 cN. Five parallel samples were prepared for each fiber, the mechanical properties of each parallel sample were tested 15 times, and the average value was taken, as shown in Table 2.

[0038] Table 2: From the data shown in Table 2 above, it can be seen that the mechanical properties of the polyester BI fibers obtained in Examples 1-3 are significantly improved. As can be seen from Comparative Example 1 and Comparative Example 1, the microspheres of the active ingredients of lemon balm and valerian of the present application can be well compatible with the polyester molecules, significantly enhancing the mechanical properties of the polyester BI fibers.

[0039] The specific embodiments are merely an explanation of the present application, and are not a limitation of the present application. Those skilled in the art can make modifications to the embodiments without creative contribution after reading the specification, as long as the modifications are within the scope of the claims of the present application.

Claims

1. A polyester BI fiber containing active ingredients of lemon balm and valerian, characterized in that, The preparation method of the microspheres containing active ingredients of lemon balm and valerian includes the following steps:

2. The poly-ester BI fibres containing active ingredients of Monarda and Valerian according to claim 1, characterized in that, The preparation method of the microspheres containing active ingredients of lemon balm and valerian includes the following steps: The lemon balm extract, the valerian extract and the beta-cyclodextrin are dissolved in ethanol, then a guar gum aqueous solution is added, ultrasonic dispersion is performed, polyvinyl alcohol is added dropwise under stirring, after the dropwise addition is completed, stirring is continued to form an emulsion, vacuum drying is performed, grinding is performed, and the microspheres containing active ingredients of lemon balm and valerian are obtained.

3. The poly-ester BI fibres containing active ingredients of lemon balm and valerian according to claim 2, characterized in that, The mass ratio of the lemon balm extract, the valerian extract, the beta-cyclodextrin, the ethanol, the guar gum aqueous solution and the polyvinyl alcohol is 1-4:2:10-20:40-60:5-15:2-5; and the concentration of the guar gum aqueous solution is 1-5 wt%.

4. The poly-ester BI fibres containing active ingredients of Monarda and Valerian according to claim 2, characterized in that, The preparation method of the lemon balm extract includes the following steps: The plasma pretreated lemon balm dried leaves are crushed to obtain lemon balm powder; The lemon balm powder is added into a eutectic solvent, stirring is uniformly performed, vacuum packaging is performed, extraction is performed in an ultrahigh pressure treatment device, centrifugation is performed, the supernatant is taken, vacuum concentration is performed, and the lemon balm extract is obtained.

5. The poly-ester BI fibres containing active ingredients of lemon balm and valerian according to claim 4, characterised in that, The plasma pretreatment conditions are as follows: the working gas is air, the power is 10-50 W, the treatment time is 20-60 s, and the treatment distance is 2-5 cm.

6. The poly-ester BI fibres containing active ingredients of Monarda and Valerian according to claim 4, characterized by, The extraction conditions of the ultrahigh pressure treatment device are as follows: the extraction pressure is 300-400 MPa, and the extraction time is 10-15 min.

7. The poly-ester BI fibres containing active ingredients of Monarda and Valerian according to claim 4, characterized by, The solid-liquid ratio of the lemon balm powder and the eutectic solvent is 1 g:20-30 mL; and the water content of the eutectic solvent is 35-50 wt%, including ethylene glycol and oxalic acid in a molar ratio of 1:2-4.

8. The poly-ester BI fibres containing active ingredients of Monarda and Valerian according to claim 2, characterized by, The preparation method of the valerian extract includes the following steps: The valerian dried rhizome is crushed to obtain valerian dry powder; the valerian dry powder is added into an ethanol solution, ultrasonic extraction is performed, filtration is performed, vacuum concentration is performed, and drying is performed, and the valerian extract is obtained.

9. The poly-ester BI fibres containing active ingredients of lemon balm and valerian according to claim 8, characterised in that, The solid-liquid ratio of the valerian dry powder and the ethanol solution is 1 g:10-30 mL; the concentration of the ethanol solution is 30-70 wt%; and the ultrasonic extraction conditions are as follows: the power is 100-200 W, the time is 20-60 min, and the temperature is 30-70 °C.

10. A process for the preparation of the polyester BI fibres containing the active ingredients of Monarda citriodora and Valeriana officinalis according to any one of claims 1 to 9, characterised in that, The preparation method includes the following steps: S1, the microspheres containing active ingredients of lemon balm and valerian and the dispersant are uniformly mixed to obtain a mixture; S2, the polyester chips are first melted at a temperature of 235-240 °C and a screw rotation speed of 250-280 r / min for 1-1.5 h, then the mixture is added, melt blending is performed for 3-5 min, the melt temperature is 235-240 °C, and the screw rotation speed is 255-275 r / min; then extrusion, cooling, granulation and drying are performed to obtain polyester master granules; S3, the polyester master granules are extruded and melted at 255-265 °C, spinning is performed, the spinning speed is controlled to be 1700-1750 m / min, then drawing, oiling and winding are performed, and the polyester BI fiber containing active ingredients of lemon balm and valerian is obtained.

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