Polyester large biofiber containing lavender active ingredient and preparation method thereof

Abstract

The present invention relates to the technical field of polyester fiber modification, specifically disclosing a polyester biofiber containing a lavender active ingredient and a preparation method thereof. The polyester biofiber containing a lavender active ingredient comprises the following raw materials in parts by weight: 100-300 parts of polyester chips, 5-10 parts of a lavender active ingredient, 10-20 parts of a modified mica sheet, 10-20 parts of a coupling agent, and 1-3 parts of a dispersant. Furthermore, the present invention first enzymatically hydrolyzes lavender leaves using a composite enzyme and then extracts them using a deep eutectic solvent. The two steps are combined to fully extract the active ingredient from the lavender leaves. The polyester fiber of the present invention has excellent aging resistance and antibacterial properties and has broad market prospects.

Description

Technical Field

[0001] The present invention relates to the technical field of polyester fiber modification, and more particularly to a polyester large biological fiber containing lavender active ingredients and a preparation method thereof. Background Art

[0002] In the textile industry, polyester fiber is widely popular due to its high modulus, high strength, excellent elasticity, good shape retention and heat resistance, making it one of the most widely used and consumed fiber varieties.

[0003] While polyester fibers possess excellent chemical stability and weather resistance, long-term exposure to harsh environments such as ultraviolet light, high temperatures, and oxidation can easily lead to molecular chain breakage and degradation, resulting in a decrease in fiber performance and even loss of usefulness. Ultraviolet light is a major factor in the aging of polyester fibers, breaking down chemical bonds and causing problems such as reduced strength, color fading, and increased brittleness. Furthermore, oxygen and moisture in the air can react with polyester fibers, further accelerating the aging process. Furthermore, the dense molecular structure and smooth surface of polyester fibers make them less susceptible to bacterial adhesion and growth. However, in actual use, polyester fiber products often have poor air and moisture permeability, leading to the accumulation of sweat and oil, creating favorable conditions for bacterial growth. These bacteria not only affect wear comfort and aesthetics but can also pose health risks, such as causing skin allergies and infections. Therefore, maintaining the inherent excellent properties of polyester fibers while further improving their aging resistance and antibacterial properties has become a pressing technical challenge for the textile industry.

[0004] At present, CN117987954A provides a polyester large biofiber containing mint active ingredients and a preparation method thereof. The preparation method includes preparing mint extract, loading, coating, preparing functional masterbatch, and spinning steps; the polyester polyester chip pretreatment step is to mix sodium dodecylbenzene sulfonate, sodium lignin sulfonate and deionized water to obtain a dispersion; the polyester polyester chip is placed in 2.5-3.5 times the volume of the dispersion and subjected to microwave treatment for 8-12 minutes at a microwave power of 192-204W. After the microwave treatment, the temperature is raised to 80-84°C at a rate of 0.4-0.6°C / min, and the fiber is allowed to stand at 80-84°C for 30-35 minutes. After the standing period, the fiber is dried to obtain the pretreated polyester polyester chip; although the antibacterial properties of the fiber obtained by this invention have been improved to a certain extent, its aging resistance has not been improved.

[0005] Based on the above statements, the present invention proposes a novel polyester large biofiber containing lavender active ingredients. Summary of the Invention

[0006] In order to improve the aging resistance and antibacterial properties of existing polyester fibers, the present invention provides a polyester large biofiber containing lavender active ingredients and a preparation method thereof.

[0007] In a first aspect, the present invention provides a polyester large biofiber containing lavender active ingredients, comprising the following raw materials in parts by weight: 100-300 parts of polyester chips, 5-10 parts of lavender active ingredients, 10-20 parts of modified mica sheets, 10-20 parts of coupling agents, and 1-3 parts of dispersants.

[0008] Preferably, the lavender active ingredient is prepared by the following method:

[0009] S1. Wash fresh lavender leaves, dry them, crush them, and sieve them to obtain powder;

[0010] S2. Add water and complex enzyme to the powder, perform enzymatic hydrolysis at 30-45°C for 30-40 minutes, and then inactivate the enzyme in a water bath at 100-120°C for 2-4 minutes to obtain an enzymatic hydrolyzate;

[0011] S3, adding the enzymatic hydrolysate to a deep eutectic solvent, soaking the solution at 60-70°C for 12-24 hours, filtering, and collecting the filtrate to obtain an extract;

[0012] S4. Add the extract to water / ethyl acetate, heat to 60-70° C., stir for 30-40 minutes, allow to stand and separate into layers, cool to room temperature, collect the organic layer, and freeze-dry to obtain the lavender active ingredient.

[0013] Preferably, in step S2, the mass ratio of powder, water and complex enzyme is 1:10:0.06-0.1; the mass ratio of the complex enzyme including cellulase, β-glucanase and pectinase is 10:4:7.

[0014] Preferably, in step S3, the mass ratio of the enzymatic hydrolysate to the deep eutectic solvent is 10:2-3; the hydrogen bond acceptor in the deep eutectic solvent is glucose, the hydrogen bond donor is one of β-hydroxybutyric acid, citric acid, malic acid, and sorbitol, and the molar ratio of the hydrogen bond acceptor to the hydrogen bond donor is 3:1-3.

[0015] Preferably, in step S4, the mass ratio of the extract, water and ethyl acetate is 10:5:5-7.

[0016] Preferably, the modified mica sheet is prepared by the following method:

[0017] Mica sheets, ionic liquid and water are uniformly mixed in a mass ratio of 50:8-15:100, stirred and reacted at 60-80° C. for 2-4 hours, filtered, washed and dried to obtain modified mica sheets.

[0018] Preferably, the ionic liquid is 1-hydroxyethyl-3-methylimidazole chloride and / or 1-butyl-3-methylimidazole dicyanamide.

[0019] Preferably, the coupling agent is obtained by mixing N-phenyl-3-aminopropyltrimethoxysilane and γ-aminopropyltriethoxysilane in a mass ratio of 2-5:7.

[0020] Preferably, the dispersant is at least one of sodium lignin sulfonate, polyethylene glycol, sodium dodecylbenzene sulfonate, Tween, and Span.

[0021] In a second aspect, the present invention provides a method for preparing a polyester biofiber containing lavender active ingredients, using the following technical solution:

[0022] A method for preparing a large polyester biofiber containing lavender active ingredients comprises the following steps:

[0023] The lavender active ingredient, the modified mica flakes, the coupling agent, and the dispersant are uniformly mixed to obtain a mixture;

[0024] The polyester chips are first melted at a temperature of 245-250°C and a screw speed of 250-280 r / min for 50-60 minutes, and then the mixture is added and melt-blended for 8-10 minutes at a melting temperature of 245-250°C and a screw speed of 250-280 r / min; then extruded, cooled, pelletized, and dried to obtain a polyester masterbatch containing lavender active ingredients;

[0025] The polyester masterbatch containing lavender active ingredients is heated, melted, and measured before spinning at a spinning temperature of 260-270°C and a spinning speed of 3440-3460 m / min. After spinning, the fiber is subjected to primary drawing, oiling, secondary drawing, and winding to obtain a polyester large biofiber containing lavender active ingredients.

[0026] Preferably, the temperature of the primary stretching is 175-180° C., the stretching ratio is 3.4-3.6 times, the temperature of the secondary stretching is 115-120° C., and the stretching ratio is 1.7-2.3 times.

[0027] In summary, the present invention has the following beneficial effects:

[0028] 1. The polyester large biofiber containing lavender active ingredients of the present invention includes polyester chips, lavender active ingredients, modified mica sheets, coupling agents, dispersants and other raw materials, and strictly controls the weight of each component to promote the interaction between the components, which can effectively improve the aging resistance and antibacterial properties of the polyester fiber.

[0029] 2. The present invention selects lavender blades, and first performs enzymolysis with a composite enzyme obtained by mixing cellulase, beta-glucanase and pectinase. The composite enzyme can selectively degrade cellulose, beta-glucan and pectin, which helps the lavender blades to release active ingredients without damaging the active ingredients; then extracts through a deep eutectic solvent, and the hydrogen bond acceptor in the deep eutectic solvent is glucose, and the hydrogen bond donor is one of beta-hydroxybutyric acid, citric acid, malic acid and sorbitol. The deep eutectic solvent can dissolve more lavender active ingredients; the present invention combines enzymolysis with deep eutectic solvent extraction to extract lavender active ingredients, better maintains the quality of lavender active ingredients, reduces their degradation or loss, thereby improving the quality and stability of lavender active ingredients. The lavender active ingredient of the present invention has excellent antibacterial and antioxidant properties, and thus greatly improves the aging resistance and antibacterial properties of polyester fiber.

[0030] 3. The present invention loads ionic liquid on the surface of the mica sheet, and the ionic liquid is 1-hydroxyethyl-3-methylimidazole chloride and / or 1-butyl-3-methylimidazole dicyanamide salt, which can not only adsorb lavender active ingredients through hydrogen bonding, maintain the stability of lavender active ingredients, thereby enhancing the aging resistance and antibacterial properties of polyester fibers, but also greatly improve the mechanical properties of polyester fibers.

[0031] 4. The lavender active ingredient and the modified mica flakes of the present invention interact with each other and synergistically enhance the thermal stability and UV resistance of polyester fibers, and improve their aging resistance, thereby enabling the polyester fibers to maintain excellent mechanical properties for a long time.

[0032] 5. The preparation method of the polyester large biofiber containing lavender active ingredients of the present invention has simple steps, low cost, and is suitable for industrial production. The obtained polyester large biofiber has better comprehensive performance and can meet higher market demands. DETAILED DESCRIPTION

[0033] The present invention is further described in detail below with reference to the examples.

[0034] Preparation Examples 1-3 and Comparative Preparation Examples 1-2 provide methods for preparing lavender active ingredients.

[0035] Preparation Example 1

[0036] Lavender active ingredient, prepared by the following method:

[0037] S1. Wash fresh lavender leaves, dry them, crush them, and sieve them to obtain 100-mesh powder;

[0038] S2. Add 100 g of water and 0.6 g of complex enzyme to 10 g of powder, perform enzymatic hydrolysis at 30°C for 40 min, and then inactivate the enzyme in a water bath at 100°C for 2 min to obtain an enzymatic hydrolyzate;

[0039] The mass ratio of the complex enzymes, cellulase, β-glucanase and pectinase, is 10:4:7;

[0040] S3, adding 100 g of the enzymatic hydrolysate to 20 g of a deep eutectic solvent, soaking the mixture at 60° C. for 24 h, filtering, and collecting the filtrate to obtain an extract;

[0041] The hydrogen bond acceptor in the deep eutectic solvent is glucose, the hydrogen bond donor is β-hydroxybutyric acid, and the molar ratio of the hydrogen bond acceptor to the hydrogen bond donor is 3:1;

[0042] S4. Add 100 g of the extract to water / ethyl acetate (50 g / 50 g), heat to 60° C., stir for 40 min, allow to stand and separate, cool to room temperature, collect the organic layer, and freeze-dry to obtain the lavender active ingredient.

[0043] Preparation Example 2

[0044] Lavender active ingredient, prepared by the following method:

[0045] S1. Wash fresh lavender leaves, dry them, crush them, and sieve them to obtain 150-mesh powder.

[0046] S2. Add 100 g of water and 0.8 g of complex enzyme to 10 g of powder, perform enzymatic hydrolysis at 40°C for 35 min, and then inactivate the enzyme in a water bath at 110°C for 3 min to obtain an enzymatic hydrolyzate;

[0047] The mass ratio of the complex enzymes, cellulase, β-glucanase and pectinase, is 10:4:7;

[0048] S3, adding 100 g of the enzymatic hydrolysate to 25 g of a deep eutectic solvent, soaking the mixture at 65° C. for 18 h, filtering, and collecting the filtrate to obtain an extract;

[0049] The hydrogen bond acceptor in the deep eutectic solvent is glucose, the hydrogen bond donor is citric acid, and the molar ratio of the hydrogen bond acceptor to the hydrogen bond donor is 3:2;

[0050] S4. Add 100 g of the extract to water / ethyl acetate (50 g / 60 g), heat to 65° C., stir for 35 min, allow to stand and separate, cool to room temperature, collect the organic layer, and freeze-dry to obtain the lavender active ingredient.

[0051] Preparation Example 3

[0052] Lavender active ingredient, prepared by the following method:

[0053] S1. Wash fresh lavender leaves, dry them, crush them, and sieve them to obtain 200-mesh powder.

[0054] S2. Add 100 g of water and 1 g of complex enzyme to 10 g of powder, perform enzymatic hydrolysis at 45°C for 30 min, and then inactivate the enzyme in a water bath at 120°C for 4 min to obtain an enzymatic hydrolyzate;

[0055] The mass ratio of the complex enzymes, cellulase, β-glucanase and pectinase, is 10:4:7;

[0056] S3, adding 100 g of the enzymatic hydrolysate to 30 g of a deep eutectic solvent, soaking the mixture at 70° C. for 12 h, filtering, and collecting the filtrate to obtain an extract;

[0057] The hydrogen bond acceptor in the deep eutectic solvent is glucose, the hydrogen bond donor is malic acid, and the molar ratio of the hydrogen bond acceptor to the hydrogen bond donor is 3:3;

[0058] S4. Add 100 g of the extract to water / ethyl acetate (50 g / 70 g), heat to 70° C., stir for 30 min, allow to stand and separate, cool to room temperature, collect the organic layer, and freeze-dry to obtain the lavender active ingredient.

[0059] Comparative Preparation Example 1

[0060] Lavender active ingredient, prepared by the following method:

[0061] S1. Wash fresh lavender leaves, dry them, crush them, and sieve them to obtain 100-mesh powder;

[0062] S2. Add 100 g of water and 0.6 g of complex enzyme to 10 g of powder, perform enzymatic hydrolysis at 30°C for 40 min, and then inactivate the enzyme in a water bath at 100°C for 2 min to obtain an enzymatic hydrolyzate;

[0063] S3. Add 100 g of the enzymatic hydrolysate to water / ethyl acetate (50 g / 50 g), heat to 60° C., stir for 40 min, allow to stand for stratification, cool to room temperature, collect the organic layer, and freeze-dry to obtain the lavender active ingredient.

[0064] Comparative Preparation Example 2

[0065] Lavender active ingredient, prepared by the following method:

[0066] S1. Wash fresh lavender leaves, dry them, crush them, and sieve them to obtain 100-mesh powder;

[0067] S2. Add 100 g of water and 20 g of a deep eutectic solvent to 10 g of the powder, soak at 60° C. for 24 h, filter, and collect the filtrate to obtain an extract;

[0068] The hydrogen bond acceptor in the deep eutectic solvent is glucose, the hydrogen bond donor is β-hydroxybutyric acid, and the molar ratio of the hydrogen bond acceptor to the hydrogen bond donor is 3:1;

[0069] S3. Add 100 g of the extract to water / ethyl acetate (50 g / 50 g), heat to 60° C., stir for 40 min, allow to stand and separate, cool to room temperature, collect the organic layer, and freeze-dry to obtain the lavender active ingredient.

[0070] Preparation Examples 4-6 provide methods for preparing modified mica sheets.

[0071] Preparation Example 4

[0072] Modified mica flakes are prepared by the following method:

[0073] Mica flakes, ionic liquid and water were mixed uniformly in a mass ratio of 25:4:50, stirred and reacted at 60°C for 2 hours, filtered, washed and dried to obtain modified mica flakes;

[0074] Wherein, the ionic liquid is 1-hydroxyethyl-3-methylimidazole chloride.

[0075] Preparation Example 5

[0076] Modified mica flakes are prepared by the following method:

[0077] Mica flakes, ionic liquid and water were mixed uniformly in a mass ratio of 5:1:10, stirred and reacted at 70°C for 3 hours, filtered, washed and dried to obtain modified mica flakes;

[0078] Wherein, the ionic liquid is 1-butyl-3-methylimidazole dicyanamide salt.

[0079] Preparation Example 6

[0080] Modified mica flakes are prepared by the following method:

[0081] Mica flakes, ionic liquid and water were mixed uniformly in a mass ratio of 25:3:50, stirred and reacted at 80°C for 4 hours, filtered, washed and dried to obtain modified mica flakes;

[0082] The ionic liquid is obtained by mixing 1-hydroxyethyl-3-methylimidazole chloride and 1-butyl-3-methylimidazole dicyanamide in a mass ratio of 1:1.

[0083] Examples 1-3 provide a polyester large biofiber containing lavender active ingredients and a preparation method thereof.

[0084] Example 1

[0085] A polyester biofiber containing lavender active ingredients, comprising the following raw materials in parts by weight: 100 parts of polyester chips, 5 parts of lavender active ingredients, 10 parts of modified mica sheets, 10 parts of coupling agents, and 1 part of dispersant;

[0086] The lavender active ingredient was prepared according to Preparation Example 1; the modified mica flakes were prepared according to Preparation Example 4; the coupling agent was prepared by mixing N-phenyl-3-aminopropyltrimethoxysilane and γ-aminopropyltriethoxysilane in a mass ratio of 2:7; and the dispersant was sodium lignin sulfonate.

[0087] A method for preparing a large polyester biofiber containing lavender active ingredients comprises the following steps:

[0088] The lavender active ingredient, the modified mica flakes, the coupling agent, and the dispersant are uniformly mixed to obtain a mixture;

[0089] The polyester chips were first melted at a temperature of 245°C and a screw speed of 250 r / min for 50 minutes, and then the mixture was added and melt-blended for 8 minutes at a melting temperature of 245°C and a screw speed of 250 r / min. The mixture was then extruded, cooled, pelletized, and dried to obtain a polyester masterbatch containing the lavender active ingredient.

[0090] The polyester masterbatch containing lavender active ingredients is heated, melted, and metered before spinning at a spinning temperature of 260°C and a spinning speed of 3440 m / min. After the spinning is completed, the fibers are subjected to primary drawing, oiling, secondary drawing, and winding to obtain a polyester biofiber containing lavender active ingredients.

[0091] The temperature of the first drawing was 175° C., the drawing ratio was 3.6 times, and the temperature of the second drawing was 115° C., the drawing ratio was 1.7 times.

[0092] Example 2

[0093] A polyester large biofiber containing lavender active ingredients, comprising the following raw materials in parts by weight: 200 parts of polyester chips, 8 parts of lavender active ingredients, 15 parts of modified mica sheets, 15 parts of coupling agents, and 2 parts of dispersants;

[0094] The lavender active ingredient was prepared according to Preparation Example 2; the modified mica flakes were prepared according to Preparation Example 5; the coupling agent was prepared by mixing N-phenyl-3-aminopropyltrimethoxysilane and γ-aminopropyltriethoxysilane in a mass ratio of 4:7; and the dispersant was polyethylene glycol.

[0095] A method for preparing a large polyester biofiber containing lavender active ingredients comprises the following steps:

[0096] The lavender active ingredient, the modified mica flakes, the coupling agent, and the dispersant are uniformly mixed to obtain a mixture;

[0097] The polyester chips were first melted at a temperature of 248°C and a screw speed of 265 r / min for 55 minutes, and then the mixture was added and melt-blended for 9 minutes at a melting temperature of 248°C and a screw speed of 265 r / min. The mixture was then extruded, cooled, pelletized, and dried to obtain a polyester masterbatch containing the lavender active ingredient.

[0098] The polyester masterbatch containing lavender active ingredients is heated, melted, and metered before spinning at a spinning temperature of 265°C and a spinning speed of 3450 m / min. After the spinning is completed, the masterbatch is subjected to primary drawing, oiling, secondary drawing, and winding to obtain a polyester biofiber containing lavender active ingredients.

[0099] The temperature of the first drawing was 178° C., the drawing ratio was 3.5 times, and the temperature of the second drawing was 117° C., the drawing ratio was 1.9 times.

[0100] Example 3

[0101] A polyester biofiber containing lavender active ingredients, comprising the following raw materials in parts by weight: 300 parts of polyester chips, 10 parts of lavender active ingredients, 20 parts of modified mica sheets, 20 parts of coupling agents, and 3 parts of dispersants;

[0102] The lavender active ingredient was prepared according to Preparation Example 1; the modified mica flakes were prepared according to Preparation Example 6; the coupling agent was prepared by mixing N-phenyl-3-aminopropyltrimethoxysilane and γ-aminopropyltriethoxysilane in a mass ratio of 5:7; and the dispersant was sodium dodecylbenzenesulfonate.

[0103] A method for preparing a large polyester biofiber containing lavender active ingredients comprises the following steps:

[0104] The lavender active ingredient, the modified mica flakes, the coupling agent, and the dispersant are uniformly mixed to obtain a mixture;

[0105] The polyester chips were first melted at a temperature of 250°C and a screw speed of 280 r / min for 60 minutes, and then the mixture was added and melt-blended for 10 minutes at a melting temperature of 250°C and a screw speed of 280 r / min. The mixture was then extruded, cooled, pelletized, and dried to obtain a polyester masterbatch containing the lavender active ingredient.

[0106] The polyester masterbatch containing lavender active ingredients is heated, melted, and metered before spinning at a spinning temperature of 270°C and a spinning speed of 3460 m / min. After the spinning is completed, the fibers are subjected to primary drawing, oiling, secondary drawing, and winding to obtain a polyester biofiber containing lavender active ingredients.

[0107] The temperature of the first drawing was 180° C., the drawing ratio was 3.6 times, and the temperature of the second drawing was 120° C., the drawing ratio was 2.3 times.

[0108] In order to verify the performance of the polyester large biofiber containing lavender active ingredients provided by the present invention, the inventors set up comparative examples 1-6, in which:

[0109] Comparative Example 1

[0110] Comparative Example 1 is different from Example 1 only in that the lavender active ingredient is prepared by Comparative Preparation Example 1, specifically as follows:

[0111] A polyester biofiber containing lavender active ingredients, comprising the following raw materials in parts by weight: 100 parts of polyester chips, 5 parts of lavender active ingredients, 10 parts of modified mica sheets, 10 parts of coupling agents, and 1 part of dispersant;

[0112] The lavender active ingredient was prepared by Comparative Preparation Example 1; the modified mica flakes were prepared by Preparation Example 4; the coupling agent was prepared by mixing N-phenyl-3-aminopropyltrimethoxysilane and γ-aminopropyltriethoxysilane in a mass ratio of 2:7; and the dispersant was sodium lignin sulfonate.

[0113] A method for preparing a large polyester biofiber containing lavender active ingredients comprises the following steps:

[0114] The lavender active ingredient, the modified mica flakes, the coupling agent, and the dispersant are uniformly mixed to obtain a mixture;

[0115] The polyester chips were first melted at a temperature of 245°C and a screw speed of 250 r / min for 50 minutes, and then the mixture was added and melt-blended for 8 minutes at a melting temperature of 245°C and a screw speed of 250 r / min. The mixture was then extruded, cooled, pelletized, and dried to obtain a polyester masterbatch containing the lavender active ingredient.

[0116] The polyester masterbatch containing lavender active ingredients is heated, melted, and metered before spinning at a spinning temperature of 260°C and a spinning speed of 3440 m / min. After the spinning is completed, the fibers are subjected to primary drawing, oiling, secondary drawing, and winding to obtain a polyester biofiber containing lavender active ingredients.

[0117] The temperature of the first drawing was 175° C., the drawing ratio was 3.6 times, and the temperature of the second drawing was 115° C., the drawing ratio was 1.7 times.

[0118] Comparative Example 2

[0119] Comparative Example 2 is different from Example 1 only in that the lavender active ingredient is prepared by Comparative Preparation Example 2, specifically as follows:

[0120] A polyester biofiber containing lavender active ingredients, comprising the following raw materials in parts by weight: 100 parts of polyester chips, 5 parts of lavender active ingredients, 10 parts of modified mica sheets, 10 parts of coupling agents, and 1 part of dispersant;

[0121] The lavender active ingredient was prepared by comparative preparation example 2; the modified mica flakes were prepared by preparation example 4; the coupling agent was prepared by mixing N-phenyl-3-aminopropyltrimethoxysilane and γ-aminopropyltriethoxysilane in a mass ratio of 2:7; and the dispersant was sodium lignin sulfonate.

[0122] A method for preparing a large polyester biofiber containing lavender active ingredients comprises the following steps:

[0123] The lavender active ingredient, the modified mica flakes, the coupling agent, and the dispersant are uniformly mixed to obtain a mixture;

[0124] The polyester chips were first melted at a temperature of 245°C and a screw speed of 250 r / min for 50 minutes, and then the mixture was added and melt-blended for 8 minutes at a melting temperature of 245°C and a screw speed of 250 r / min. The mixture was then extruded, cooled, pelletized, and dried to obtain a polyester masterbatch containing the lavender active ingredient.

[0125] The polyester masterbatch containing lavender active ingredients is heated, melted, and metered before spinning at a spinning temperature of 260°C and a spinning speed of 3440 m / min. After the spinning is completed, the fibers are subjected to primary drawing, oiling, secondary drawing, and winding to obtain a polyester biofiber containing lavender active ingredients.

[0126] The temperature of the first drawing was 175° C., the drawing ratio was 3.6 times, and the temperature of the second drawing was 115° C., the drawing ratio was 1.7 times.

[0127] Comparative Example 3

[0128] Comparative Example 3 is the same as Example 1, except that the lavender active ingredient is replaced with an equal mass of lavender extract, as follows:

[0129] A polyester biofiber containing lavender extract, comprising the following raw materials in parts by weight: 100 parts of polyester chips, 5 parts of lavender extract, 10 parts of modified mica sheets, 10 parts of coupling agents, and 1 part of dispersant;

[0130] The modified mica flakes were prepared according to Preparation Example 4; the coupling agent was obtained by mixing N-phenyl-3-aminopropyltrimethoxysilane and γ-aminopropyltriethoxysilane in a mass ratio of 2:7; the dispersant was sodium lignin sulfonate; and the lavender extract was purchased from Wuhan Lanabai Pharmaceutical Chemical Co., Ltd. under the brand name Lanabai, with a purity of 99%.

[0131] A method for preparing a large polyester biofiber containing lavender extract comprises the following steps:

[0132] uniformly mixing the lavender extract, modified mica flakes, a coupling agent, and a dispersant to obtain a mixture;

[0133] The polyester chips were first melted at a temperature of 245°C and a screw speed of 250 r / min for 50 minutes, and then the mixture was added and melt-blended for 8 minutes at a melting temperature of 245°C and a screw speed of 250 r / min; then extruded, cooled, pelletized, and dried to obtain a polyester masterbatch containing lavender extract;

[0134] The polyester masterbatch containing lavender extract is heated, melted, and metered before spinning at a spinning temperature of 260°C and a spinning speed of 3440 m / min. After the spinning is completed, the fiber is subjected to primary drawing, oiling, secondary drawing, and winding to obtain a polyester large bio-fiber containing lavender extract.

[0135] The temperature of the first drawing was 175° C., the drawing ratio was 3.6 times, and the temperature of the second drawing was 115° C., the drawing ratio was 1.7 times.

[0136] Comparative Example 4

[0137] Comparative Example 4 is the same as Example 1, except that mica sheets of equal mass are used to replace the modified mica sheets, as follows:

[0138] A polyester biofiber containing lavender active ingredients, comprising the following raw materials in parts by weight: 100 parts of polyester chips, 5 parts of lavender active ingredients, 10 parts of mica flakes, 10 parts of coupling agents, and 1 part of dispersant;

[0139] The lavender active ingredient is prepared according to Preparation Example 1; the coupling agent is obtained by mixing N-phenyl-3-aminopropyltrimethoxysilane and γ-aminopropyltriethoxysilane in a mass ratio of 2:7; and the dispersant is sodium lignin sulfonate.

[0140] A method for preparing a large polyester biofiber containing lavender active ingredients comprises the following steps:

[0141] The lavender active ingredient, mica flakes, coupling agent, and dispersant are uniformly mixed to obtain a mixture; polyester chips are first melted at a temperature of 245°C and a screw speed of 250 r / min for 50 minutes, and then the mixture is added and melt-blended for 8 minutes at a melting temperature of 245°C and a screw speed of 250 r / min; then, the mixture is extruded, cooled, pelletized, and dried to obtain a polyester masterbatch containing the lavender active ingredient;

[0142] The polyester masterbatch containing lavender active ingredients is heated, melted, and metered before spinning at a spinning temperature of 260°C and a spinning speed of 3440 m / min. After the spinning is completed, the fibers are subjected to primary drawing, oiling, secondary drawing, and winding to obtain a polyester biofiber containing lavender active ingredients.

[0143] The temperature of the first drawing was 175° C., the drawing ratio was 3.6 times, and the temperature of the second drawing was 115° C., the drawing ratio was 1.7 times.

[0144] Comparative Example 5

[0145] Comparative Example 5 is the same as Example 1, except that the modified mica sheet is replaced with an equal mass of lavender active ingredient, as follows:

[0146] A polyester biofiber containing lavender active ingredients, comprising the following raw materials in parts by weight: 100 parts of polyester chips, 15 parts of lavender active ingredients, 10 parts of coupling agents, and 1 part of dispersants;

[0147] The lavender active ingredient is prepared according to Preparation Example 1; the coupling agent is obtained by mixing N-phenyl-3-aminopropyltrimethoxysilane and γ-aminopropyltriethoxysilane in a mass ratio of 2:7; and the dispersant is sodium lignin sulfonate.

[0148] A method for preparing a large polyester biofiber containing lavender active ingredients comprises the following steps:

[0149] uniformly mixing the lavender active ingredient, the coupling agent, and the dispersant to obtain a mixture;

[0150] The polyester chips were first melted at a temperature of 245°C and a screw speed of 250 r / min for 50 minutes, and then the mixture was added and melt-blended for 8 minutes at a melting temperature of 245°C and a screw speed of 250 r / min. The mixture was then extruded, cooled, pelletized, and dried to obtain a polyester masterbatch containing the lavender active ingredient.

[0151] The polyester masterbatch containing lavender active ingredients is heated, melted, and metered before spinning at a spinning temperature of 260°C and a spinning speed of 3440 m / min. After the spinning is completed, the fibers are subjected to primary drawing, oiling, secondary drawing, and winding to obtain a polyester biofiber containing lavender active ingredients.

[0152] The temperature of the first drawing was 175° C., the drawing ratio was 3.6 times, and the temperature of the second drawing was 115° C., the drawing ratio was 1.7 times.

[0153] Comparative Example 6

[0154] Comparative Example 6 is the same as Example 1, except that the lavender active ingredient is replaced with modified mica sheets of equal mass, as follows:

[0155] A polyester fiber comprises the following raw materials in parts by weight: 100 parts of polyester chips, 15 parts of modified mica sheets, 10 parts of coupling agents, and 1 part of dispersing agent;

[0156] The modified mica flakes were prepared according to Preparation Example 4; the coupling agent was prepared by mixing N-phenyl-3-aminopropyltrimethoxysilane and γ-aminopropyltriethoxysilane in a mass ratio of 2:7; and the dispersant was sodium lignin sulfonate.

[0157] A method for preparing a large polyester biofiber containing lavender active ingredients comprises the following steps:

[0158] uniformly mixing the modified mica flakes, the coupling agent, and the dispersant to obtain a mixture;

[0159] The polyester chips were first melted at a temperature of 245°C and a screw speed of 250 r / min for 50 minutes, and then added to the mixture and melt-blended for 8 minutes at a melting temperature of 245°C and a screw speed of 250 r / min; then extruded, cooled, pelletized, and dried to obtain polyester masterbatch;

[0160] The polyester masterbatch is heated, melted, and metered before spinning at a spinning temperature of 260°C and a spinning speed of 3440 m / min. After spinning, the polyester fiber is obtained through primary drawing, oiling, secondary drawing, and winding.

[0161] The temperature of the first drawing was 175° C., the drawing ratio was 3.6 times, and the temperature of the second drawing was 115° C., the drawing ratio was 1.7 times.

[0162] The properties of the polyester fibers obtained in Examples 1-3 and Comparative Examples 1-6 were tested respectively, and the following parameters were obtained, as shown in Table 1:

[0163] The breaking strength and elongation of the fiber are tested in accordance with GB / T14344-2022 "Test method for tensile properties of chemical fiber filaments";

[0164] The fiber aging performance test is carried out in accordance with GB / T35256-2017 "Textiles - Tests for Colour Fastness - Artificial Weathering - Exposure to Filtered Xenon Arc Radiation", where the exposure conditions are the 7.1A conditions in the standard.

[0165] The antibacterial performance test of the fiber is carried out in accordance with GB / T20944.3-2008 "Evaluation of antibacterial properties of textiles Part 3: Oscillation method".

[0166] Table 1:

[0167]

[0168] The data shown in Table 1 above show that the comprehensive performance of the polyester fibers obtained in Examples 1-3 is significantly better than that in Comparative Examples 1-6. They have higher breaking strength and elongation at break, significant aging resistance, and good antibacterial effect, which fully demonstrates that the polyester large biofiber containing lavender active ingredients of the present invention has excellent comprehensive performance and broad application prospects.

[0169] By comparing Example 1 with Comparative Examples 1 and 2, it can be seen that the lavender active ingredient of the present invention is first enzymatically hydrolyzed by a composite enzyme and then extracted using a deep eutectic solvent. The combination of the two steps can fully extract the active ingredient in the lavender leaves; further comparing Example 1 with Comparative Example 3 shows that the lavender active ingredient of the present invention is superior to the lavender extract, can effectively improve the aging resistance of polyester fiber, and improve its antibacterial performance.

[0170] By comparing Example 1 and Comparative Example 4, it can be seen that the modified mica sheet of the present invention is obtained by modifying the hydrophilic ionic liquid. Compared with the mica sheet, the modified mica sheet can not only improve the mechanical properties of the polyester fiber, but also enhance the aging resistance and antibacterial properties of the polyester fiber.

[0171] Comparison of Example 1 with Comparative Examples 5 and 6 shows that the lavender active ingredient of the present invention and the modified mica flakes interact with each other and synergize to improve the aging resistance and antibacterial properties of the polyester fiber.

[0172] This specific embodiment is merely an explanation of the present invention and is not intended to limit the present invention. After reading this specification, those skilled in the art may make non-creative modifications to this embodiment as needed. However, as long as such modifications are within the scope of the claims of the present invention, they are protected by patent law.

Claims

1. A polyester biofiber containing lavender active ingredients, characterized in that: The invention comprises the following raw materials in parts by weight: 100-300 parts of polyester chips, 5-10 parts of lavender active ingredients, 10-20 parts of modified mica sheets, 10-20 parts of coupling agents, and 1-3 parts of dispersants; The lavender active ingredient is prepared by the following method: S1. Wash fresh lavender leaves, dry them, crush them, and sieve them to obtain powder; S2. Add water and complex enzyme to the powder, perform enzymatic hydrolysis at 30-45°C for 30-40 minutes, and then inactivate the enzyme in a water bath at 100-120°C for 2-4 minutes to obtain an enzymatic hydrolyzate; S3, adding the enzymatic hydrolysate to a deep eutectic solvent, soaking the solution at 60-70°C for 12-24 hours, filtering, and collecting the filtrate to obtain an extract; S4. Add the extract to water / ethyl acetate, heat to 60-70°C, stir for 30-40 minutes, allow to stand and separate, cool to room temperature, collect the organic layer, and freeze-dry to obtain the lavender active ingredient; The modified mica sheet is prepared by the following method: mica sheet, ionic liquid and water are uniformly mixed in a mass ratio of 50:8-15:100, stirred and reacted at 60-80°C for 2-4 hours, filtered, washed and dried to obtain the modified mica sheet; the ionic liquid is 1-hydroxyethyl-3-methylimidazole chloride and / or 1-butyl-3-methylimidazole dicyanamide salt.

2. The polyester large biofiber containing lavender active ingredients according to claim 1, characterized in that: In step S2, the mass ratio of powder, water and complex enzyme is 1:10:0.06-0.1; the mass ratio of the complex enzyme including cellulase, β-glucanase and pectinase is 10:4:

7.

3. The polyester large biofiber containing lavender active ingredients according to claim 1, characterized in that: In step S3, the mass ratio of the enzymatic hydrolysate to the deep eutectic solvent is 10:2-3; the hydrogen bond acceptor in the deep eutectic solvent is glucose, the hydrogen bond donor is one of β-hydroxybutyric acid, citric acid, malic acid, and sorbitol, and the molar ratio of the hydrogen bond acceptor to the hydrogen bond donor is 3:1-3.

4. The polyester large biofiber containing lavender active ingredient according to claim 1, characterized in that: The mass ratio of the extract, water and ethyl acetate in step S4 is 10:5:5-7.

5. The polyester large biofiber containing lavender active ingredient according to claim 1, characterized in that: The coupling agent is obtained by mixing N-phenyl-3-aminopropyltrimethoxysilane and gamma-aminopropyltriethoxysilane in a mass ratio of 2-5:

7.

6. The polyester large bio-fiber containing lavender active ingredient according to claim 1, characterized in that: The dispersant is at least one of sodium lignin sulfonate, polyethylene glycol, sodium dodecylbenzene sulfonate, Tween, and Span.

7. A method for preparing a polyester large biofiber containing lavender active ingredients according to any one of claims 1 to 6, characterized in that: The following steps are involved: The lavender active ingredient, the modified mica flakes, the coupling agent, and the dispersant are uniformly mixed to obtain a mixture; The polyester chips are first melted at a temperature of 245-250°C and a screw speed of 250-280 r / min for 50-60 minutes, and then the mixture is added and melt-blended for 8-10 minutes at a melting temperature of 245-250°C and a screw speed of 250-280 r / min; then extruded, cooled, pelletized, and dried to obtain a polyester masterbatch containing lavender active ingredients; The polyester masterbatch containing lavender active ingredients is heated, melted, and measured before spinning at a spinning temperature of 260-270°C and a spinning speed of 3440-3460 m / min. After spinning, the fiber is subjected to primary drawing, oiling, secondary drawing, and winding to obtain a polyester large biofiber containing lavender active ingredients.

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