A health-care silk fabric and its preparation method

Abstract

The present invention discloses a health care silk fabric and a preparation method thereof, relating to the technical field of textiles. When preparing the health care silk fabric, a nano-titanium dioxide composite silk fiber fabric is used as the fabric base layer. First, a modified silane coupling agent is used to carry out ultrasonic swelling modification on the fabric base layer. The two ends of the modified silane coupling agent are respectively grafted onto the nano-titanium dioxide and silk fiber molecules, and a pyrrole compound is used to crosslink between the nano-titanium dioxide and the silk fiber to form a network structure, enhancing the air permeability of the fabric base layer; then, through constant voltage electric treatment, the pyrrole compound is polymerized to form a polypyrrole conductive path, enhancing the antistatic property of the health care silk fabric; then, through low-frequency ultrasonic technology, the dye is embedded and grafted inside the fabric base layer, increasing the color fastness of the moisturizing silk fabric; finally, through orthogonal electrostatic field microwave treatment, a metal complex film layer is formed on the surface of the fabric base layer to enhance the ultraviolet resistance of the moisturizing silk fabric.

Description

Technical Field

[0001] It relates to the technical field of textiles, specifically a health silk fabric and its preparation method. Background Art

[0002] Silk is mainly composed of animal protein and has the beautiful names of "the second skin of the human body" and "the queen of fibers". According to the "Compendium of Materia Medica" records: Silk protein powder can eliminate skin dark spots and treat suppurative dermatitis. Modern medical experiments further prove that the protein content of silk is much higher than that of pearls, with the nitrogen content 37 times higher than that of pearls and the main amino acid content more than 10 times higher. These amino acids can be directly absorbed and adsorbed by human hair and skin, can promote the vitality of skin cells, prevent blood vessel sclerosis, prevent skin aging after long-term use, have a special antipruritic effect on certain skin diseases, and have a certain health care effect on arthritis, scapulohumeral periarthritis, and asthma.

[0003] Since 2000, under the advocacy of returning to nature and the green revolution, silk has received more and more attention and pursuit. From expensive silk quilts to silk pillows, silk underwear, and then to silk medical suture lines and silk protein artificial skin in the medical field, the role of silk is becoming more and more important. However, the disadvantages of poor antibacterial performance, poor antistatic performance, poor water washing resistance, and poor ultraviolet resistance of silk have become a major problem on the road of its wide application.

[0004] The present invention has noticed this phenomenon and solves this problem by preparing a health silk fabric. Summary of the Invention

[0005] The purpose of the present invention is to provide a health silk fabric and its preparation method to solve the problems existing in the prior art.

[0006] To solve the above technical problems, the present invention provides the following technical solutions:

[0007] A health silk fabric, by weight, mainly includes 10 - 20 parts of fabric base layer, 16 - 32 parts of modified silane coupling agent, and 70 - 80 parts of dyeing agent.

[0008] Further, the fabric base layer is obtained by the silk spinning of silkworms fed with mulberry leaves coated with nano-titanium dioxide on the surface to obtain nano-titanium dioxide composite silk fibers, followed by cocoon cooking, reeling, and weaving.

[0009] Further, the modified silane coupling agent is prepared by the condensation of aminolevulinic acid and trimethoxysilyl chloride.

[0010] Further, the dyeing agent is prepared by the esterification reaction of shikonin and 2-carboxy-3-hydroxyglutaric acid.

[0011] A preparation method of a health care silk fabric mainly includes the following preparation steps:

[0012] (1) Ultrasonic swelling modification: Immerse the fabric base layer in calcium nitrate and carry out ultrasonic treatment. After fishing out, wash it with deionized water and dry it, then soak it in a modified silane coupling agent and continue ultrasonic treatment to obtain a pretreated fabric base layer;

[0013] (2) Constant voltage electroprocessing: Soak the pretreated fabric base layer with a lithium perchlorate solution, and pass a constant voltage current under nitrogen protection to obtain a modified fabric base layer;

[0014] (3) Low-frequency ultrasonic dyeing: Immerse the modified fabric base layer in a dyeing agent for low-frequency ultrasonic treatment. After washing, drying, and padding, obtain a dyed fabric base layer;

[0015] (4) Orthogonal electrostatic field microwave treatment: Place the dyed fabric base layer in an orthogonal electrostatic field for microwave treatment, and then carry out washing, drying, soaping, washing, and drying to obtain a health care silk fabric.

[0016] Further, the preparation method of the health care silk fabric mainly includes the following preparation steps:

[0017] (1) Ultrasonic swelling modification: Under the ultrasonic conditions of 80 - 85 °C and 30 - 40 kHz, immerse the fabric base layer in a calcium nitrate solution with a mass fraction of 30 - 45% and 100 times the mass of the fabric base layer for ultrasonic treatment for 6 - 10 s. After fishing out, wash it with deionized water 3 - 4 times, place it in an oven at 60 °C and dry it for 1 - 1.2 h, then naturally cool it to room temperature. Subsequently, add it to a mixed solution obtained by stirring 2 - 2.4 times the mass of the fabric base layer of ethyl acetate and 1.6 - 1.8 times the mass of the fabric base layer of the modified silane coupling agent at 25 - 26 °C and 140 - 180 r / min for 10 - 20 min, heat it up to 83 - 87 °C, and carry out ultrasonic treatment for 30 - 40 s under the ultrasonic conditions of 30 - 40 kHz to obtain a pretreated fabric base layer;

[0018] (2) Constant voltage electroprocessing: Under the ultrasonic conditions of 30 - 40 kHz, immerse the pretreated fabric base layer in a lithium perchlorate solution with a mass fraction of 40% and 10 - 12 times the mass of the pretreated fabric base layer for ultrasonic treatment for 6 - 8 s. Pass nitrogen at room temperature and 0.14 - 0.15 m 3 / s. After 9 - 10 min, apply a constant voltage of 0.6 - 0.9 V and energize for 9 - 11 min. Subsequently, wash it with deionized water 3 - 4 times, and then dry it naturally to obtain a modified fabric base layer;

[0019] (3) Low-frequency ultrasonic dyeing: Immerse the modified fabric base layer in a dyeing agent that is 7 to 8 times the mass of the modified fabric base layer under ultrasonic conditions of 60 - 70°C and 20 - 25 kHz for 30 - 36 s, then take it out, wash it 3 - 4 times with deionized water, put it in an oven at 40 - 60°C for 1 - 1.5 h, then take it out and cool it to room temperature. Then, pad it under the conditions of a padding temperature of 30 - 35°C and a liquor pickup rate of 85% - 92% to obtain the dyed fabric base layer;

[0020] (4) Orthogonal electrostatic field microwave treatment: Under the conditions of an orthogonal electrostatic field of 220 kV / m, microwave of 2400 - 2500 MHz and 700 - 900 W, microwave-treat the dyed fabric base layer for 28 - 32 min, then wash it 3 - 4 times with deionized water, put it in an oven at 40 - 60°C for 1 h - 1.5 h, then take it out and cool it to room temperature. Then, stir and wash it for 10 min at a speed of 100 - 120 r / min with a soap detergent that is 0.01 - 0.03 times the mass of the dyed fabric base layer, then wash it 3 - 4 times with deionized water, continue to put it in an oven at 40 - 60°C for 1 h - 1.5 h, then take it out and cool it to room temperature to obtain the health care silk fabric.

[0021] Furthermore, the preparation method of the fabric base layer in step (1) is as follows: Uniformly coat the surface of mulberry leaves with nano-titanium dioxide sol that is 0.006 - 0.01 times the mass of the mulberry leaves, let it dry naturally, then feed it to silkworms to obtain cocoons. Add the cocoons to deionized water that is 3 - 5 times the mass of the cocoons, then add sodium carbonate that is 0.1 - 0.2 times the mass of the cocoons, stir at 120 - 180 r / min for 10 - 12 min, heat up to boiling, continue to stir for 40 - 60 min, take it out and wash it 4 - 6 times with deionized water, reel the silk to obtain silk threads, and use the silk threads as warp and weft to weave in a plain weave to obtain the fabric base layer; The silkworms selected are Jing Song Hao Yue.

[0022] Furthermore, the preparation method of the modified silane coupling agent in step (1) is as follows: Add trimethoxysilane chloride to ethyl acetate that is 5 - 6 times the mass of trimethoxysilane chloride, carry out oil bath reflux at 77 - 78°C and 600 - 800 r / min for 1 h, then add aminolevulinic acid that is 1.2 - 1.4 times the mass of trimethoxysilane chloride, and continue to stir and carry out oil bath reflux for 1 h under the protection of nitrogen and at 110°C to obtain the modified silane coupling agent.

[0023] Furthermore, the preparation method of the dyeing agent in step (3) is as follows: Under the stirring conditions of 75 - 85°C and 600 - 800 r / min, reflux the shikonin, 2-carboxy-3-hydroxyglutaric acid and concentrated sulfuric acid in an oil bath at a mass ratio of 1:1.2 - 1.6:0.3 - 0.4 for 1 - 2 h to obtain the dyeing agent.

[0024] Furthermore, the soap detergent in step (4) is industrial soap.

[0025] Compared with the prior art, the beneficial effects achieved by the present invention are as follows:

[0026] When preparing the health care silk fabric, the present invention uses the nano-titanium dioxide composite silk fiber fabric as the fabric base layer, and successively performs steps such as ultrasonic swelling modification, constant voltage electro-treatment, low-frequency ultrasonic dyeing, and orthogonal electrostatic field microwave treatment on the fabric base layer to obtain the health care silk fabric; among them, the modified silane coupling agent is prepared by mixing aminolevulinic acid and trimethoxysilyl chloride; the dyeing agent is prepared by mixing shikonin and 2-carboxy-3-hydroxyglutaric acid.

[0027] First, immerse the fabric base layer in the modified silane coupling agent. Under the action of ultrasonic swelling, the structure of the nano-titanium dioxide composite silk fiber becomes loose, and the molecular chain of the modified silane coupling agent is quickly embedded into the structure of the nano-titanium dioxide composite silk fiber. At this time, one end of the modified silane coupling agent removes the methoxy group and reacts with the hydroxyl group on the surface of nano-titanium dioxide to form a covalent bond crosslinking, and the other end, aminolevulinic acid, reacts with the amino group on the fibroin fiber to generate a pyrrole compound, and molecular chain crosslinking occurs between the fibroin fiber and nano-titanium dioxide to form a network structure, which not only strengthens the fiber strength of the fabric base layer but also improves the air permeability of the fabric base layer; then, perform constant voltage electro-treatment on the fabric to obtain a pre-treated fabric base layer. The pyrrole compound in the fabric base layer oxidizes and polymerizes under the action of current to form a polypyrrole compound, forming a conductive path inside the pre-treated fabric base layer, making the fabric base layer have antistatic performance.

[0028] Secondly, immerse the pre-treated fabric base layer in the dyeing agent. Under the action of low-frequency ultrasound, the molecular chain of the dyeing agent is embedded into the fiber gaps of the fabric base layer. The molecular chain of shikonin modified by 2-carboxy-3-hydroxyglutaric acid has a carboxyl group, which can react with the hydroxyl group on the fiber fabric to form a stable covalent bond crosslinking, firmly grafting the dyeing agent molecules in the fabric base layer and increasing the color fastness of the health care silk fabric; moreover, under the acoustic cavitation action of low-frequency ultrasound, the hydroxyl group in 2-carboxy-3-hydroxyglutaric acid on the molecular chain of the dyeing agent is oxidized to a carbonyl group and reacts with the amino group of the fabric base layer fiber to generate a Schiff base compound, increasing the antibacterial property of the health care silk fabric; subsequently, under the action of the orthogonal electrostatic field microwave, some titanium ions, hydrogen ions, etc. in the fabric base layer are ionized, the carbon-carbon double bond inside the dyeing agent breaks and polymerizes and crosslinks to form a polymer film, exposing the phenolic hydroxyl group and carbonyl group in the dyeing agent on the film surface to quickly capture the free titanium ions to form a coordination bond crosslinking, forming a stable metal complex film layer on the surface of the fabric base layer and increasing the ultraviolet resistance of the fabric base layer. Detailed implementation manners

[0029] Next, in combination with the embodiments of the present invention, the technical solutions in the embodiments of the present invention will be clearly and completely described. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present invention.

[0030] In order to more clearly illustrate the method provided by the present invention, the following embodiments are used for detailed description. The test methods for each index of the health silk fabric prepared in the following embodiments are as follows:

[0031] Air permeability: Take the health silk fabrics prepared in the embodiments and comparative examples with the same length and width, and test the air permeability according to the GB / T5453 standard method.

[0032] Color fastness: Take the health silk fabrics prepared in the embodiments and comparative examples with the same length and width, and test the color fastness according to the GB / T3921 standard method.

[0033] Antistatic property: Take the health silk fabrics prepared in the embodiments and comparative examples with the same length and width, and test the antistatic property according to the GB / T24249 standard method.

[0034] Anti-ultraviolet performance: Take the health silk fabrics prepared in the embodiments and comparative examples with the same length and width, and test the anti-ultraviolet performance according to the GB / T17032 standard method.

[0035] Example 1

[0036] A health silk fabric mainly includes 10 parts of fabric base layer, 16 parts of modified silane coupling agent, and 70 parts of dye by weight.

[0037] A preparation method of a health silk fabric, the preparation method of the health silk fabric mainly includes the following preparation steps:

[0038] (1) Ultrasonic swelling modification: Uniformly coat the surface of mulberry leaves with nano-titanium dioxide sol at 0.006 times the mass of the mulberry leaves. After natural drying, feed them to the silkworms Jing Song Hao Yue to obtain cocoons. Add the cocoons to deionized water at 3 times the mass of the cocoons, then add sodium carbonate at 0.1 times the mass of the cocoons and stir at 120 r / min for 10 min. Heat up to boiling, continue stirring for 40 min, fish out and wash 4 times with deionized water, reel the silk to obtain silk threads. Use the silk threads as warp and weft to perform plain weaving to obtain the fabric base layer; Add trimethoxysilane to ethyl acetate at 5 times the mass of trimethoxysilane, carry out oil bath reflux at 77 °C and 600 r / min for 1 h, then add aminolevulinic acid at 1.2 times the mass of trimethoxysilane, and under the protection of nitrogen and at 110 °C, continue stirring and oil bath reflux for 1 h to obtain the modified silane coupling agent; Under the conditions of 80 °C and 30 kHz ultrasonic, immerse the fabric base layer in a 30% calcium nitrate solution at 100 times the mass of the fabric base layer and ultrasonic for 6 s. Fish out and wash 3 times with deionized water, put it in an oven at 60 °C and dry for 1 h, then naturally cool to room temperature. Subsequently, add it to a mixed solution obtained by stirring ethyl acetate at 2 times the mass of the fabric base layer and the modified silane coupling agent at 1.6 times the mass of the fabric base layer at 25 °C and 140 r / min for 10 min, heat up to 83 °C, and ultrasonic for 30 s under the conditions of 30 kHz ultrasonic to obtain the pretreated fabric base layer;

[0039] (2) Constant voltage treatment: Under the conditions of 30 kHz ultrasonic, immerse the pretreated fabric base layer in a 40% lithium perchlorate solution at 10 times the mass of the pretreated fabric base layer and ultrasonic for 6 s. Pass nitrogen at room temperature and 0.14 m 3 / s, after 9 min, apply a constant voltage of 0.6 V and energize for 9 min. Subsequently, wash 3 times with deionized water, then naturally dry to obtain the modified fabric base layer;

[0040] (3) Low-frequency ultrasonic dyeing: Under the conditions of stirring at 75 °C and 600 r / min, reflux the shikonin, 2-carboxy-3-hydroxyglutaric acid and concentrated sulfuric acid in an oil bath at a mass ratio of 1:1.2:0.3 for 1 h to obtain the dyeing agent; Under the conditions of 60 °C and 20 kHz ultrasonic, immerse the modified fabric base layer in the dyeing agent at 7 times the mass of the modified fabric base layer and ultrasonic for 30 s, then fish out. Subsequently, wash 3 times with deionized water, then put it in an oven at 40 °C and dry for 1 h, then take it out and cool to room temperature. Then, impregnate and roll at an impregnating and rolling temperature of 30 °C and a pick-up rate of 85% to obtain the dyed fabric base layer;

[0041] (4) Orthogonal electrostatic field microwave treatment: Under the conditions of an orthogonal electrostatic field of 220 kV / m, microwaves of 2400 and 700 W, the dyed fabric base layer was microwave-treated for 28 min, then washed 3 times with deionized water, placed in an oven at 40 °C for 1 h, then taken out and cooled to room temperature. Subsequently, industrial soap 0.01 times the mass of the dyed fabric base layer was used to stir and wash at a rotation speed of 100 r / min for 10 min, then washed 3 times with deionized water, and continued to be placed in an oven at 40 °C for 1 h, taken out and cooled to room temperature to obtain the health silk fabric.

[0042] Example 2

[0043] A health silk fabric mainly includes 15 parts of fabric base layer, 24 parts of modified silane coupling agent, and 75 parts of dye by weight.

[0044] A preparation method of a health silk fabric, the preparation method of the health silk fabric mainly includes the following preparation steps:

[0045] (1) Ultrasonic swelling modification: Uniformly coat 0.008 times the mass of mulberry leaves with nano-titanium dioxide sol on the surface of mulberry leaves, air-dry naturally and feed them to the silkworms Jing Song Hao Yue to obtain cocoons. Add the cocoons to 4 times the mass of deionized water of the cocoons, then add 0.15 times the mass of sodium carbonate of the cocoons and stir at 150 r / min for 11 min, heat up to boiling, continue to stir for 50 min, fish out and wash 5 times with deionized water, reel the silk to obtain silk. Use the silk as warp and weft and weave by plain weave to obtain the fabric base layer; Add trimethoxysilane chloride to ethyl acetate 5.5 times the mass of trimethoxysilane chloride, carry out oil bath reflux at 77 °C and 700 r / min for 1 h, then add aminolevulinic acid 1.3 times the mass of trimethoxysilane chloride, and continue to stir and carry out oil bath reflux for 1 h under the protection of nitrogen and at 110 °C to obtain the modified silane coupling agent; Under the ultrasonic condition of 83 °C and 35 kHz, immerse the fabric base layer in a calcium nitrate solution with a mass fraction of 38% 100 times the mass of the fabric base layer and ultrasonic for 8 s, fish out and wash 3 times with deionized water, place in an oven at 60 °C and dry for 1.1 h, then naturally cool to room temperature, and then add it to a mixed solution obtained by stirring 2.2 times the mass of ethyl acetate of the fabric base layer and 1.7 times the mass of the modified silane coupling agent of the fabric base layer at 25 °C and 160 r / min for 15 min, heat up to 85 °C, and ultrasonic for 35 s under the ultrasonic condition of 35 kHz to obtain the pretreated fabric base layer;

[0046] (2) Constant voltage electric treatment: Under the ultrasonic condition of 35 kHz, immerse the pretreated fabric base layer in a lithium perchlorate solution with a mass fraction of 40% 11 times the mass of the pretreated fabric base layer and ultrasonic for 7 s, at room temperature, 0.14 m 3Under the condition of / s, nitrogen gas was introduced. After 9.5 minutes, an electric current was applied for 10 minutes under a constant voltage condition of 0.8 V. Subsequently, it was washed 3 times with deionized water and then naturally air-dried to obtain the modified fabric base layer;

[0047] (3) Low-frequency ultrasonic dyeing: Under the stirring conditions of 80 °C and 700 r / min, shikonin, 2-carboxy-3-hydroxyglutaric acid, and concentrated sulfuric acid were refluxed in an oil bath for 1.5 h according to a mass ratio of 1:1.4:0.35 to obtain a dyeing agent; Under the ultrasonic condition of 65 °C and 23 kHz, the modified fabric base layer was immersed in a dyeing agent 7.5 times the mass of the modified fabric base layer and ultrasonicated for 34 s and then fished out. Subsequently, it was washed 3 times with deionized water, then placed in an oven at 50 °C and baked for 1.3 h, then taken out and cooled to room temperature. Then, it was pad-dyed under the conditions of a padding temperature of 33 °C and a liquor pickup rate of 90% to obtain the dyed fabric base layer;

[0048] (4) Orthogonal electrostatic field microwave treatment: Under the conditions of an orthogonal electrostatic field of 220 kV / m, a microwave of 2450 MHz, and 800 W, the dyed fabric base layer was microwave-treated for 30 min, then washed 3 times with deionized water, then placed in an oven at 50 °C and baked for 1.2 h. Subsequently, it was taken out and cooled to room temperature. Then, industrial soap 0.02 times the mass of the dyed fabric base layer was used to stir and wash at a rotation speed of 110 r / min for 10 min, then washed 3 times with deionized water, and continued to be placed in an oven at 50 °C and baked for 1.2 h, then taken out and cooled to room temperature to obtain the health-care silk fabric.

[0049] Example 3

[0050] A health-care silk fabric mainly includes 20 parts of fabric base layer, 32 parts of modified silane coupling agent, and 80 parts of dyeing agent by weight.

[0051] A preparation method of a health-care silk fabric, the preparation method of the health-care silk fabric mainly includes the following preparation steps:

[0052] (1) Ultrasonic swelling modification: Uniformly coat the surface of mulberry leaves with nano-titanium dioxide sol at 0.01 times the mass of the mulberry leaves. After natural drying, feed them to the silkworms Jing Song Hao Yue to obtain cocoons. Add the cocoons to 5 times the mass of deionized water, then add sodium carbonate at 0.2 times the mass of the cocoons and stir at 180 r / min for 12 min. Heat to boiling and continue stirring for 60 min. Scoop out and wash 6 times with deionized water, then reel to obtain silk. Use the silk as warp and weft and weave in plain weave to obtain the fabric base layer; Add trimethoxysilane to ethyl acetate at 6 times the mass of trimethoxysilane, reflux in an oil bath at 78 °C and 800 r / min for 1 h, then add aminolevulinic acid at 1.4 times the mass of trimethoxysilane. Under the protection of nitrogen and at 110 °C, continue stirring and refluxing in an oil bath for 1 h to obtain a modified silane coupling agent; Under the conditions of 85 °C and 40 kHz ultrasonic, immerse the fabric base layer in a 45% calcium nitrate solution at 100 times the mass of the fabric base layer and ultrasonic for 10 s. Scoop out and wash 4 times with deionized water, then place in an oven at 60 °C and dry for 1.2 h. Then naturally cool to room temperature, and then add it to a mixed solution obtained by stirring ethyl acetate at 2.4 times the mass of the fabric base layer and the modified silane coupling agent at 1.8 times the mass of the fabric base layer at 26 °C and 180 r / min for 20 min. Heat to 87 °C and ultrasonic for 40 s under the conditions of 40 kHz ultrasonic to obtain a pretreated fabric base layer;

[0053] (2) Constant voltage treatment: Under the conditions of 40 kHz ultrasonic, immerse the pretreated fabric base layer in a 40% lithium perchlorate solution at 12 times the mass of the pretreated fabric base layer and ultrasonic for 8 s. Pass nitrogen at room temperature and 0.15 m 3 / s. After 10 min, apply a constant voltage of 0.9 V and energize for 11 min. Then wash 4 times with deionized water and then dry naturally to obtain a modified fabric base layer;

[0054] (3) Low-frequency ultrasonic dyeing: Under the conditions of stirring at 85 °C and 800 r / min, reflux shikonin, 2-carboxy-3-hydroxyglutaric acid and concentrated sulfuric acid in an oil bath at a mass ratio of 1:1.6:0.4 for 2 h to obtain a dyeing agent; Under the conditions of 70 °C and 25 kHz ultrasonic, immerse the modified fabric base layer in a dyeing agent at 8 times the mass of the modified fabric base layer and ultrasonic for 36 s, then scoop out. Then wash 4 times with deionized water, then place in an oven at 60 °C and bake for 1.5 h, then take out and cool to room temperature. Then pad at a padding temperature of 35 °C and a liquor pickup of 92% to obtain a dyed fabric base layer;

[0055] (4) Orthogonal electrostatic field microwave treatment: Under the conditions of an orthogonal electrostatic field of 220 kV / m, microwave of 2500 MHz and 900 W, the dyed fabric base layer was microwave-treated for 32 min, then washed 4 times with deionized water, then placed in an oven at 60 °C for 1.5 h, then taken out and cooled to room temperature. Then, industrial soap 0.03 times the mass of the dyed fabric base layer was used to stir and wash at a rotation speed of 120 r / min for 10 min, then washed 4 times with deionized water, and continued to be placed in an oven at 60 °C for 1.5 h. After taking out and cooling to room temperature, a health silk fabric was obtained.

[0056] Comparative Example 1

[0057] A health silk fabric, by weight, mainly includes 10 parts of fabric base layer, 16 parts of modified silane coupling agent, and 70 parts of dyeing agent.

[0058] A preparation method of a health silk fabric, the preparation method of the health silk fabric mainly includes the following preparation steps:

[0059] (1) Swelling modification: Uniformly coat 0.006 times the mass of mulberry leaves with nano-titanium dioxide sol on the surface of mulberry leaves, air-dry naturally and feed them to the silkworms Jing Song Hao Yue to obtain cocoons. Add the cocoons to 3 times the mass of deionized water of the cocoons, then add 0.1 times the mass of sodium carbonate of the cocoons and stir at 120 r / min for 10 min, heat up to boiling, continue to stir for 40 min, fish out and wash 4 times with deionized water, reel the silk to obtain silk. Use the silk as warp and weft and weave by plain weave to obtain a fabric base layer; Add trimethoxysilane to ethyl acetate 5 times the mass of trimethoxysilane, and carry out oil bath reflux at 77 °C and 600 r / min for 1 h, then add 1.2 times the mass of aminolevulinic acid of trimethoxysilane, and continue to stir and carry out oil bath reflux for 1 h under the protection of nitrogen and at 110 °C to obtain a modified silane coupling agent; Under the stirring condition of 80 °C and 180 r / min, immerse the fabric base layer in a 30% calcium nitrate solution 100 times the mass of the fabric base layer and stir for 3 h, fish out and wash 3 times with deionized water, place in an oven at 60 °C and dry for 1 h, then naturally cool to room temperature. Then add ethyl acetate 2 times the mass of the fabric base layer, carry out oil bath reflux at 80 °C and 200 r / min for 1 h, then add 1.6 times the mass of the modified silane coupling agent of the fabric base layer, and continue to carry out oil bath reflux at 90 °C and 200 r / min for 1 h to obtain a pretreated fabric base layer;

[0060] (2) Constant voltage electric treatment: Under the condition of 30 kHz ultrasonic wave, immerse the pretreated fabric base layer in a 40% lithium perchlorate solution 10 times the mass of the pretreated fabric base layer and ultrasonic for 6 s, at room temperature, 0.14 m 3Under the condition of / s, nitrogen gas was introduced. After 9 minutes, an electric current was applied for 9 minutes under a constant voltage of 0.6 V. Subsequently, it was washed 3 times with deionized water and then air-dried naturally to obtain the modified fabric base layer;

[0061] (3) Low-frequency ultrasonic dyeing: Under the conditions of stirring at 75 °C and 600 r / min, shikonin, 2-carboxy-3-hydroxyglutaric acid, and concentrated sulfuric acid were refluxed in an oil bath for 1 h according to a mass ratio of 1:1.2:0.3 to obtain a dyeing agent; Under the conditions of 60 °C and 20 kHz ultrasonic wave, the modified fabric base layer was immersed in a dyeing agent 7 times the mass of the modified fabric base layer and ultrasonically treated for 30 s and then fished out. Subsequently, it was washed 3 times with deionized water, then placed in an oven at 40 °C and dried for 1 h, and then taken out and cooled to room temperature. Then, it was padded under the conditions of a padding temperature of 30 °C and a liquor pickup of 85% to obtain the dyed fabric base layer;

[0062] (4) Orthogonal electrostatic field microwave treatment: Under the conditions of an orthogonal electrostatic field of 220 kV / m, 2400 and 700 W microwave, the dyed fabric base layer was microwave-treated for 28 min, then washed 3 times with deionized water, then placed in an oven at 40 °C and dried for 1 h, and then taken out and cooled to room temperature. Then, industrial soap 0.01 times the mass of the dyed fabric base layer was used to stir and wash at a rotation speed of 100 r / min for 10 min, then washed 3 times with deionized water, and continued to be placed in an oven at 40 °C and dried for 1 h, and then taken out and cooled to room temperature to obtain the health-care silk fabric.

[0063] Comparative Example 2

[0064] A health-care silk fabric, by weight, mainly includes 10 parts of fabric base layer, 16 parts of modified silane coupling agent, and 70 parts of dyeing agent.

[0065] A preparation method of a health-care silk fabric, the preparation method of the health-care silk fabric mainly includes the following preparation steps:

[0066] (1) Ultrasonic swelling modification: Uniformly coat the surface of mulberry leaves with nano-titanium dioxide sol at 0.006 times the mass of the mulberry leaves. After natural drying, feed them to the silkworms Jing Song Hao Yue to obtain cocoons. Add the cocoons to deionized water at 3 times the mass of the cocoons, then add sodium carbonate at 0.1 times the mass of the cocoons and stir at 120 r / min for 10 min. Heat to boiling and continue stirring for 40 min. Scoop out and wash 4 times with deionized water, then reel the silk. Use the silk as warp and weft to perform plain weaving to obtain the fabric base layer; Add trimethoxysilane to ethyl acetate at 5 times the mass of trimethoxysilane, and carry out oil bath reflux at 77 °C and 600 r / min for 1 h. Then add aminolevulinic acid at 1.2 times the mass of trimethoxysilane, and under the protection of nitrogen and at 110 °C, continue stirring and oil bath reflux for 1 h to obtain the modified silane coupling agent; Under the conditions of 80 °C and 30 kHz ultrasonic, immerse the fabric base layer in a 30% calcium nitrate solution at 100 times the mass of the fabric base layer and ultrasonicate for 6 s. Scoop out and wash 3 times with deionized water, put it in an oven at 60 °C and dry for 1 h, then naturally cool to room temperature. Subsequently, add it to a mixed solution obtained by stirring ethyl acetate at 2 times the mass of the fabric base layer and the modified silane coupling agent at 1.6 times the mass of the fabric base layer at 25 °C and 140 r / min for 10 min. Heat to 83 °C and ultrasonicate for 30 s under the condition of 30 kHz ultrasonic. Then wash 3 times with deionized water and then naturally dry to obtain the modified fabric base layer;

[0067] (2) Low-frequency ultrasonic dyeing: Under the conditions of stirring at 75 °C and 600 r / min, reflux the shikonin, 2-carboxy-3-hydroxyglutaric acid and concentrated sulfuric acid in an oil bath at a mass ratio of 1:1.2:0.3 for 1 h to obtain the dyeing agent; Under the conditions of 60 °C and 20 kHz ultrasonic, immerse the modified fabric base layer in the dyeing agent at 7 times the mass of the modified fabric base layer and ultrasonicate for 30 s, then scoop out, wash 3 times with deionized water, then put it in an oven at 40 °C and bake for 1 h, then take it out and cool to room temperature. Then pad it under the conditions of a padding temperature of 30 °C and a liquor pickup of 85% to obtain the dyed fabric base layer;

[0068] (3) Orthogonal electrostatic field microwave treatment: Under the orthogonal electrostatic field of 220 kV / m, 2400 and 700 W microwave conditions, microwave-treat the dyed fabric base layer for 28 min, then wash 3 times with deionized water, then put it in an oven at 40 °C and bake for 1 h, then take it out and cool to room temperature. Then use industrial soap at 0.01 times the mass of the dyed fabric base layer and stir and wash at 100 r / min for 10 min, then wash 3 times with deionized water, continue to put it in an oven at 40 °C and bake for 1 h, then take it out and cool to room temperature to obtain the health-care silk fabric.

[0069] Comparative Example 3

[0070] A health care silk fabric, by weight, mainly includes 10 parts of fabric base layer, 16 parts of modified silane coupling agent, and 70 parts of dyeing agent.

[0071] A preparation method of a health care silk fabric, the preparation method of the health care silk fabric mainly includes the following preparation steps:

[0072] (1) Ultrasonic swelling modification: Uniformly coat 0.006 times the mass of mulberry leaves with nano-titanium dioxide sol on the surface of mulberry leaves, let it dry naturally, and feed it to the silkworms Jing Song Hao Yue to obtain cocoons. Add the cocoons to 3 times the mass of deionized water of the cocoons, then add 0.1 times the mass of sodium carbonate of the cocoons, stir at 120 r / min for 10 min, heat up to boiling, continue to stir for 40 min, fish out and wash 4 times with deionized water, reel the silk to obtain silk. Use the silk as warp and weft to carry out plain weave to make the fabric base layer; Under the ultrasonic condition of 80 °C and 30 kHz, immerse the fabric base layer in a calcium nitrate solution with a mass fraction of 30% and 100 times the mass of the fabric base layer for 6 s by ultrasonic wave, fish out and wash 3 times with deionized water, put it in an oven at 60 °C and dry for 1 h, then naturally cool to room temperature. Then add it to 2 times the mass of ethyl acetate of the fabric base layer and 1.6 times the mass of trimethoxysilane chloride of the fabric base layer, and stir in the mixed solution obtained by stirring at 25 °C and 140 r / min for 10 min, heat up to 83 °C, and ultrasonically wave for 30 s under the ultrasonic condition of 30 kHz to obtain a pretreated fabric base layer;

[0073] (2) Constant voltage electro-treatment: Under the ultrasonic condition of 30 kHz, immerse the pretreated fabric base layer in a lithium perchlorate solution with a mass fraction of 40% and 10 times the mass of the pretreated fabric base layer for 6 s by ultrasonic wave, and introduce nitrogen at room temperature and a condition of 0.14 m 3 / s. After 9 min, apply an electric current at a constant voltage of 0.6 V for 9 min, then wash 3 times with deionized water, and then dry naturally to obtain a modified fabric base layer;

[0074] (3) Low-frequency ultrasonic dyeing: Under the stirring conditions of 75 °C and 600 r / min, reflux the shikonin, 2-carboxy-3-hydroxyglutaric acid and concentrated sulfuric acid in an oil bath at a mass ratio of 1:1.2:0.3 for 1 h to obtain a dyeing agent; Under the ultrasonic condition of 60 °C and 20 kHz, immerse the modified fabric base layer in a dyeing agent with 7 times the mass of the modified fabric base layer for 30 s by ultrasonic wave, then fish out, then wash 3 times with deionized water, then put it in an oven at 40 °C and dry for 1 h, then take it out and cool to room temperature. Then pad at a padding temperature of 30 °C and a liquor pickup of 85% to obtain a dyed fabric base layer;

[0075] (4) Orthogonal electrostatic field microwave treatment: Under the conditions of an orthogonal electrostatic field of 220 kV / m, microwave powers of 2400 and 700 W, the dyed fabric substrate was microwave-treated for 28 min, then washed 3 times with deionized water, placed in an oven at 40 °C for 1 h, taken out and cooled to room temperature. Subsequently, industrial soap at 0.01 times the mass of the dyed fabric substrate was used to stir and wash at a rotation speed of 100 r / min for 10 min, then washed 3 times with deionized water, and continued to be placed in an oven at 40 °C for 1 h, taken out and cooled to room temperature to obtain the health care silk fabric.

[0076] Comparative Example 4

[0077] A health care silk fabric, by weight, mainly includes 10 parts of fabric substrate, 16 parts of modified silane coupling agent, and 70 parts of dye.

[0078] A preparation method of a health care silk fabric, the preparation method of the health care silk fabric mainly includes the following preparation steps:

[0079] (1) Ultrasonic swelling modification: Uniformly coat nano-titanium dioxide sol at 0.006 times the mass of mulberry leaves on the surface of mulberry leaves, air-dry naturally and feed them to the silkworms Jing Song Hao Yue to obtain cocoons. Add the cocoons to deionized water at 3 times the mass of the cocoons, then add sodium carbonate at 0.1 times the mass of the cocoons, stir at 120 r / min for 10 min, heat up to boiling, continue to stir for 40 min, fish out and wash 4 times with deionized water, reel the silk to obtain silk threads. Use the silk threads as warp and weft to perform plain weaving to obtain the fabric substrate; Add trimethoxysilane to ethyl acetate at 5 times the mass of trimethoxysilane, carry out oil bath reflux at 77 °C and 600 r / min for 1 h, then add aminolevulinic acid at 1.2 times the mass of trimethoxysilane, and continue to stir and carry out oil bath reflux for 1 h under the protection of nitrogen and at 110 °C to obtain the modified silane coupling agent; Under the conditions of 80 °C and 30 kHz ultrasonic wave, immerse the fabric substrate in a calcium nitrate solution with a mass fraction of 30% at 100 times the mass of the fabric substrate and ultrasonically treat for 6 s, fish out and wash 3 times with deionized water, place in an oven at 60 °C and dry for 1 h, then naturally cool to room temperature. Subsequently, add it to a mixed solution obtained by stirring 2 times the mass of the fabric substrate of ethyl acetate and 1.6 times the mass of the fabric substrate of the modified silane coupling agent at 25 °C and 140 r / min for 10 min, heat up to 83 °C, and ultrasonically treat for 30 s under the conditions of 30 kHz ultrasonic wave to obtain the pretreated fabric substrate;

[0080] (2) Constant voltage treatment: Under the conditions of 30 kHz ultrasonic wave, immerse the pretreated fabric substrate in a lithium perchlorate solution with a mass fraction of 40% at 10 times the mass of the pretreated fabric substrate and ultrasonically treat for 6 s, at room temperature, 0.14 m 3Under the condition of / s, nitrogen gas was introduced. After 9 minutes, an electric current was applied at a constant voltage of 0.6V for 9 minutes. Subsequently, it was washed 3 times with deionized water and then naturally air-dried to obtain the modified fabric base layer;

[0081] (3) Dyeing: Under the conditions of stirring at 75°C and 600 r / min, shikonin, 2-carboxy-3-hydroxyglutaric acid, and concentrated sulfuric acid were refluxed in an oil bath at a mass ratio of 1:1.2:0.3 for 1 hour to obtain a dyeing agent; Under the conditions of a padding temperature of 30°C and a liquor ratio of 85%, the modified fabric base layer was immersed in a dyeing agent 7 times the mass of the modified fabric base layer for padding to obtain the dyed fabric base layer;

[0082] (4) Orthogonal electrostatic field microwave treatment: Under the conditions of an orthogonal electrostatic field of 220 kV / m, microwaves of 2400 and 700 W, the dyed fabric base layer was microwave-treated for 28 minutes, then washed 3 times with deionized water, placed in an oven at 40°C for 1 hour, then taken out and cooled to room temperature. Then, industrial soap 0.01 times the mass of the dyed fabric base layer was used to stir and wash at a rotation speed of 100 r / min for 10 minutes, then washed 3 times with deionized water, and continued to be placed in an oven at 40°C for 1 hour and then taken out and cooled to room temperature to obtain the health care silk fabric.

[0083] Comparative Example 5

[0084] A health care silk fabric, by weight, mainly includes 10 parts of fabric base layer, 16 parts of modified silane coupling agent, and 70 parts of dyeing agent.

[0085] A preparation method of a health care silk fabric, the preparation method of the health care silk fabric mainly includes the following preparation steps:

[0086] (1) Ultrasonic swelling modification: Uniformly coat the surface of mulberry leaves with nano-titanium dioxide sol at 0.006 times the mass of the mulberry leaves. After natural drying, feed them to the silkworms Jing Song Hao Yue to obtain cocoons. Add the cocoons to deionized water at 3 times the mass of the cocoons, then add sodium carbonate at 0.1 times the mass of the cocoons and stir at 120 r / min for 10 min. Heat to boiling, continue stirring for 40 min, fish out and wash 4 times with deionized water, and reel the silk to obtain silk. Use the silk as warp and weft and weave in plain weave to obtain the fabric base layer; Add trimethoxysilane to ethyl acetate at 5 times the mass of trimethoxysilane, carry out oil bath reflux at 77 °C and 600 r / min for 1 h, then add aminolevulinic acid at 1.2 times the mass of trimethoxysilane, and continue stirring and oil bath reflux for 1 h under the protection of nitrogen and at 110 °C to obtain a modified silane coupling agent; Under ultrasonic conditions of 80 °C and 30 kHz, immerse the fabric base layer in a 30% calcium nitrate solution at 100 times the mass of the fabric base layer and ultrasonically treat for 6 s. Fish out, wash 3 times with deionized water, place in an oven at 60 °C and dry for 1 h, then naturally cool to room temperature. Subsequently, add it to a mixed solution obtained by stirring ethyl acetate at 2 times the mass of the fabric base layer and the modified silane coupling agent at 1.6 times the mass of the fabric base layer at 25 °C and 140 r / min for 10 min, heat to 83 °C, and ultrasonically treat for 30 s under ultrasonic conditions of 30 kHz to obtain a pretreated fabric base layer;

[0087] (2) Constant voltage treatment: Under ultrasonic conditions of 30 kHz, immerse the pretreated fabric base layer in a 40% lithium perchlorate solution at 10 times the mass of the pretreated fabric base layer and ultrasonically treat for 6 s. Pass nitrogen at room temperature and 0.14 m 3 / s, after 9 min, apply a constant voltage of 0.6 V and energize for 9 min, then wash 3 times with deionized water, and then dry naturally to obtain a modified fabric base layer;

[0088] (3) Low-frequency ultrasonic dyeing: At 60 °C and under ultrasonic conditions of 20 kHz, immerse the modified fabric base layer in a shikonin dyeing agent at 7 times the mass of the modified fabric base layer and ultrasonically treat for 30 s, then fish out. Subsequently, wash 3 times with deionized water, then place in an oven at 40 °C and bake for 1 h, then take out and cool to room temperature. Then, carry out padding at a padding temperature of 30 °C and a liquor pickup of 85% to obtain a dyed fabric base layer;

[0089] (4)Orthogonal electrostatic field microwave treatment: Under the conditions of an orthogonal electrostatic field of 220 kV / m, microwaves of 2400 and 700 W, the dyed fabric base layer was microwave-treated for 28 min, then washed 3 times with deionized water, placed in an oven at 40 °C for 1 h, then taken out and cooled to room temperature. Subsequently, industrial soap 0.01 times the mass of the dyed fabric base layer was used to stir and wash at a speed of 100 r / min for 10 min, then washed 3 times with deionized water, and continued to be placed in an oven at 40 °C for 1 h, taken out and cooled to room temperature to obtain the health care silk fabric.

[0090] Comparative Example 6

[0091] A health care silk fabric, by weight, mainly includes 10 parts of fabric base layer, 16 parts of modified silane coupling agent, and 70 parts of dye.

[0092] A preparation method of a health care silk fabric, the preparation method of the health care silk fabric mainly includes the following preparation steps:

[0093] (1)Ultrasonic swelling modification: Uniformly coat nano-titanium dioxide sol 0.006 times the mass of mulberry leaves on the surface of mulberry leaves, let it dry naturally, and feed it to the silkworms Jing Song Hao Yue to obtain cocoons. Add the cocoons to deionized water 3 times the mass of the cocoons, then add sodium carbonate 0.1 times the mass of the cocoons, stir at 120 r / min for 10 min, heat up to boiling, continue to stir for 40 min, fish out and wash 4 times with deionized water, reel the silk to obtain silk. Use the silk as warp and weft to weave by plain weave to obtain the fabric base layer; Add trimethoxy chlorosilane to ethyl acetate 5 times the mass of trimethoxy chlorosilane, carry out oil bath reflux at 77 °C and 600 r / min for 1 h, then add aminolevulinic acid 1.2 times the mass of trimethoxy chlorosilane, under the protection of nitrogen and at 110 °C, continue to stir and carry out oil bath reflux for 1 h to obtain the modified silane coupling agent; Under the conditions of 80 °C and 30 kHz ultrasonic, immerse the fabric base layer in a calcium nitrate solution with a mass fraction of 30% 100 times the mass of the fabric base layer and ultrasonically treat for 6 s, fish out and wash 3 times with deionized water, place in an oven at 60 °C and dry for 1 h, then naturally cool to room temperature. Subsequently, add it to a mixed solution obtained by stirring ethyl acetate 2 times the mass of the fabric base layer and the modified silane coupling agent 1.6 times the mass of the fabric base layer at 25 °C and 140 r / min for 10 min, heat up to 83 °C, and ultrasonically treat for 30 s under the conditions of 30 kHz ultrasonic to obtain the pretreated fabric base layer;

[0094] (2)Constant voltage electric treatment: Under the conditions of 30 kHz ultrasonic, immerse the pretreated fabric base layer in a lithium perchlorate solution with a mass fraction of 40% 10 times the mass of the pretreated fabric base layer and ultrasonically treat for 6 s, at room temperature, 0.14 m 3Under the condition of / s, nitrogen gas was introduced. After 9 minutes, an electric current was applied at a constant voltage of 0.6 V for 9 minutes. Subsequently, it was washed 3 times with deionized water and then air-dried naturally to obtain the modified fabric base layer;

[0095] (3) Low-frequency ultrasonic dyeing: Under the conditions of stirring at 75 °C and 600 r / min, shikonin, 2-carboxy-3-hydroxyglutaric acid, and concentrated sulfuric acid were refluxed in an oil bath for 1 h according to a mass ratio of 1:1.2:0.3 to obtain a dyeing agent; Under the conditions of 60 °C and 20 kHz ultrasonic wave, the modified fabric base layer was immersed in a dyeing agent 7 times the mass of the modified fabric base layer and ultrasonicated for 30 s and then fished out. Subsequently, it was washed 3 times with deionized water, then placed in an oven at 40 °C and baked for 1 h, then taken out and cooled to room temperature. Then, it was padded under the conditions of a padding temperature of 30 °C and a liquor pickup of 85% to obtain the dyed fabric base layer;

[0096] (4) Microwave treatment: Under the conditions of 2400 and 700 W microwave, the dyed fabric base layer was microwave-treated for 28 min, then washed 3 times with deionized water, then placed in an oven at 40 °C and baked for 1 h. Subsequently, it was taken out and cooled to room temperature. Then, industrial soap 0.01 times the mass of the dyed fabric base layer was used to stir and wash at a rotation speed of 100 r / min for 10 min, then washed 3 times with deionized water, and continued to be placed in an oven at 40 °C and baked for 1 h, and then taken out and cooled to room temperature to obtain the health care silk fabric.

[0097] Comparative Example 7

[0098] A health care silk fabric mainly includes 10 parts of fabric base layer, 16 parts of modified silane coupling agent, and 70 parts of dyeing agent by weight.

[0099] A preparation method of a health care silk fabric, the preparation method of the health care silk fabric mainly includes the following preparation steps:

[0100] (1) Ultrasonic swelling modification: Uniformly coat the surface of mulberry leaves with nano-titanium dioxide sol at 0.006 times the mass of the mulberry leaves. After natural drying, feed them to the silkworms Jing Song Hao Yue to obtain cocoons. Add the cocoons to deionized water at 3 times the mass of the cocoons, then add sodium carbonate at 0.1 times the mass of the cocoons and stir at 120 r / min for 10 min. Heat to boiling and continue stirring for 40 min. Scoop out and wash 4 times with deionized water, then reel the silk. Use the silk as warp and weft and weave in plain weave to obtain the fabric base layer; Add trimethoxysilane to ethyl acetate at 5 times the mass of trimethoxysilane, and carry out oil bath reflux at 77 °C and 600 r / min for 1 h. Then add aminolevulinic acid at 1.2 times the mass of trimethoxysilane, and under the protection of nitrogen and at 110 °C, continue stirring and carry out oil bath reflux for 1 h to obtain the modified silane coupling agent; Under ultrasonic conditions of 80 °C and 30 kHz, immerse the fabric base layer in a 30% calcium nitrate solution at 100 times the mass of the fabric base layer and ultrasonicate for 6 s. Scoop out, wash 3 times with deionized water, place in an oven at 60 °C and dry for 1 h, then naturally cool to room temperature. Then add it to a mixed solution obtained by stirring ethyl acetate at 2 times the mass of the fabric base layer and the modified silane coupling agent at 1.6 times the mass of the fabric base layer at 25 °C and 140 r / min for 10 min. Heat to 83 °C and ultrasonicate for 30 s under ultrasonic conditions of 30 kHz to obtain the pretreated fabric base layer;

[0101] (2) Constant voltage treatment: Under ultrasonic conditions of 30 kHz, immerse the pretreated fabric base layer in a 40% lithium perchlorate solution at 10 times the mass of the pretreated fabric base layer and ultrasonicate for 6 s. Pass nitrogen at room temperature and 0.14 m 3 / s. After 9 min, apply a constant voltage of 0.6 V and energize for 9 min. Then wash 3 times with deionized water and then naturally dry to obtain the modified fabric base layer;

[0102] (3) Low-frequency ultrasonic dyeing: Under stirring conditions of 75 °C and 600 r / min, reflux shikonin, 2-carboxy-3-hydroxyglutaric acid and concentrated sulfuric acid in an oil bath at a mass ratio of 1:1.2:0.3 for 1 h to obtain the dyeing agent; Under ultrasonic conditions of 60 °C and 20 kHz, immerse the modified fabric base layer in the dyeing agent at 7 times the mass of the modified fabric base layer and ultrasonicate for 30 s, then scoop out, wash 3 times with deionized water, then place in an oven at 40 °C and bake for 1 h, and then take out and cool to room temperature to obtain the dyed fabric base layer;

[0103] (4)Orthogonal electrostatic field treatment: Pad under the conditions of an orthogonal electrostatic field of 220 kV / m, a padding temperature of 30 °C, and a liquor ratio of 85%, then wash 3 times with deionized water, put it in an oven at 40 °C and bake for 1 h, then take it out and cool to room temperature. Then, stir and wash with industrial soap 0.01 times the mass of the dyed fabric base at a rotation speed of 100 r / min for 10 min, then wash 3 times with deionized water, continue to put it in an oven at 40 °C and bake for 1 h, take it out and cool to room temperature to obtain the health care silk fabric.

[0104] Comparative Example 8

[0105] A health care silk fabric, by weight, mainly includes 10 parts of fabric base, 16 parts of modified silane coupling agent, and 70 parts of dye.

[0106] A preparation method of a health care silk fabric, the preparation method of the health care silk fabric mainly includes the following preparation steps:

[0107] (1) Swelling modification: Uniformly coat 0.006 times the mass of mulberry leaves with nano-titanium dioxide sol on the surface of mulberry leaves, air-dry naturally and feed them to the silkworms Jing Song Hao Yue to obtain cocoons. Add the cocoons to 3 times the mass of deionized water of the cocoons, then add 0.1 times the mass of sodium carbonate of the cocoons and stir at 120 r / min for 10 min, heat up to boiling, continue to stir for 40 min, fish out and wash 4 times with deionized water, reel the silk to obtain silk threads. Use the silk threads as warp and weft to weave in plain weave to make the fabric base; Add trimethoxysilane chloride to ethyl acetate 5 times the mass of trimethoxysilane chloride, carry out oil bath reflux at 77 °C and 600 r / min for 1 h, then add aminolevulinic acid 1.2 times the mass of trimethoxysilane chloride, and continue to stir and carry out oil bath reflux for 1 h under the protection of nitrogen and at 110 °C to obtain the modified silane coupling agent; Under the stirring conditions of 80 °C and 180 r / min, immerse the fabric base in a 30% calcium nitrate solution 100 times the mass of the fabric base and stir for 3 h, fish out and wash 3 times with deionized water, put it in an oven at 60 °C and dry for 1 h, then naturally cool to room temperature. Then add ethyl acetate 2 times the mass of the fabric base, carry out oil bath reflux at 80 °C and 200 r / min for 1 h, and then add the modified silane coupling agent 1.6 times the mass of the fabric base, and continue to carry out oil bath reflux at 90 °C and 200 r / min for 1 h to obtain the pretreated fabric base;

[0108] (2) Dyeing: Under the conditions that the padding temperature is 30°C and the liquor ratio is 85%, immerse the modified fabric base layer in shikonin dyeing agent which is 7 times the mass of the modified fabric base layer by padding, then wash it 3 times with deionized water, put it into an oven at 40°C and bake for 1 h, then take it out and cool it to room temperature. Then, use industrial soap which is 0.01 times the mass of the dyed fabric base layer to stir and wash at a rotation speed of 100 r / min for 10 min, then wash it 3 times with deionized water, continue to put it into an oven at 40°C and bake for 1 h, take it out and cool it to room temperature to obtain the health care silk fabric.

[0109] Effect Example

[0110] Table 1 below gives the analysis results of the color fastness, air permeability, ultraviolet resistance and antistatic properties of the health care silk fabrics prepared by using Examples 1 to 3 and Comparative Examples 1 to 8 of the present invention.

[0111] Table 1

[0112]

[0113] From the comparison of the experimental data of Examples 1, 2, 3 and Comparative Example 1 in Table 1, it can be found that without ultrasonic treatment during swelling modification, the molecular chains between nano-titanium dioxide and silk fiber molecules inside the fabric substrate cannot crosslink into a network structure, resulting in poor air permeability of the health care silk fabric; from the comparison of the experimental data of Examples 1, 2, 3 and Comparative Example 2, it can be found that during the preparation of the health care silk fabric, without constant voltage treatment on the modified fabric substrate, a polypyrrole conductive path cannot be formed between the fibers of the fabric substrate, resulting in poor antistatic performance of the health care silk fabric; from the comparison of the experimental data of Examples 1, 2, 3 and Comparative Example 3, it can be found that during the preparation of the health care silk fabric, using a modified silane coupling agent can form pyrrole compounds inside the fabric substrate, and polymerize to form a polypyrrole conductive path during subsequent constant voltage treatment, resulting in strong antistatic performance of the health care silk fabric; from the comparison of the experimental data of Examples 1, 2, 3 and Comparative Example 4, it can be found that for the health care silk fabric dyed without the low-frequency ultrasonic dyeing process, the molecular chains of the dyeing agent cannot be embedded inside the nano-titanium dioxide composite silk fiber, and the dyeing agent only adheres to the surface of the fabric substrate, resulting in a decrease in the color fastness of the health care silk fabric; from the comparison of the experimental data of Examples 1, 2, 3 and Comparative Example 5, it can be found that when using a shikonin dyeing agent not modified by 2-carboxy-3-hydroxypentanedioic acid for dyeing, the dyeing agent cannot be grafted onto the fabric substrate through stable covalent bonds, resulting in a decrease in the color fastness of the health care silk fabric; from the comparison of the experimental data of Examples 1, 2, 3 and Comparative Example 6, it can be found that without the treatment of an orthogonal electrostatic field, metal complexes are not formed on the film on the surface of the health care silk fabric, resulting in poor ultraviolet resistance of the health care silk fabric; from the comparison of the experimental data of Examples 1, 2, 3 and Comparative Example 7, it can be found that in the orthogonal electrostatic field, without microwave treatment, the dyeing agent cannot polymerize into a film on the silk surface, and the hydroxyl and carbonyl groups in the dyeing agent cannot quickly capture free titanium ions to form a large number of metal complexes, thereby reducing the color fastness of the health care silk fabric and weakening the antistatic performance of the health care silk fabric; from the comparison of the experimental data of Examples 1, 2, 3 and Comparative Example 8, it can be found that during the preparation of the health care silk fabric with the fabric substrate, when using a shikonin dyeing agent not modified by 2-carboxy-3-hydroxypentanedioic acid for dyeing under the process conditions without ultrasonic swelling modification, constant voltage treatment, low-frequency ultrasonic dyeing, and orthogonal electrostatic field microwave treatment, the obtained health care silk fabric has poor air permeability, weak antistatic performance, low color fastness and poor ultraviolet resistance.

[0114] It is obvious to those skilled in the art that the present invention is not limited to the details of the above-described exemplary embodiments, and that the present invention can be implemented in other specific forms without departing from the spirit or essential characteristics of the present invention. Therefore, from any point of view, the embodiments should be regarded as exemplary and non-restrictive. The scope of the present invention is defined by the appended claims rather than the above description. Therefore, all changes falling within the meaning and scope of the equivalent elements of the claims are intended to be embraced within the present invention. Any reference signs in the claims should not be construed as limiting the claim concerned.

Claims

1. A health care silk fabric, characterized in that, By weight parts, it mainly includes 10-20 parts of fabric base layer, 16-32 parts of modified silane coupling agent, and 70-80 parts of dyeing agent; The preparation method of the health silk fabric includes the following preparation steps: (1) Ultrasonic swelling modification: Add trimethoxysilane chloride to ethyl acetate with a mass 5-6 times that of trimethoxysilane chloride, and carry out oil bath reflux at 77-78 °C and 600-800 r / min for 1 h. Then add aminolevulinic acid with a mass 1.2-1.4 times that of trimethoxysilane chloride, and continue to stir and carry out oil bath reflux for 1 h under the protection of nitrogen and at 110 °C to obtain a modified silane coupling agent; Under ultrasonic conditions of 80-85 °C and 30-40 kHz, immerse the fabric base layer in a calcium nitrate solution with a mass fraction of 30-45% and a mass 100 times that of the fabric base layer for ultrasonic treatment for 6-10 s. After fishing out, wash it with deionized water 3-4 times, put it in an oven at 60 °C and dry it for 1-1.2 h, then naturally cool it to room temperature. Subsequently, add it to a mixed solution obtained by stirring 2-2.4 times the mass of ethyl acetate of the fabric base layer and 1.6-1.8 times the mass of the modified silane coupling agent of the fabric base layer at 25-26 °C and 140-180 r / min for 10-20 min, raise the temperature to 83-87 °C, and carry out ultrasonic treatment for 30-40 s under ultrasonic conditions of 30-40 kHz to obtain a pretreated fabric base layer; (2) Constant voltage electro-treatment: Under ultrasonic conditions of 30 - 40 kHz, immerse the pretreated fabric substrate into a lithium perchlorate solution with a mass fraction of 40% and a mass 10 - 12 times that of the pretreated fabric substrate, and perform ultrasonic treatment for 6 - 8 s. Then, introduce nitrogen gas at room temperature and a condition of 0.14 - 0.15 m 3 / s. After 9 - 10 min, apply a constant voltage of 0.6 - 0.9 V and conduct electricity for 9 - 11 min. Subsequently, wash it 3 - 4 times with deionized water and then air dry naturally to obtain the modified fabric substrate; (3) Low-frequency ultrasonic dyeing: Under stirring conditions of 75-85 °C and 600-800 r / min, reflux shikonin, 2-carboxy-3-hydroxypentanedioic acid and concentrated sulfuric acid in an oil bath at a mass ratio of 1:1.2-1.6:0.3-0.4 for 1-2 h to obtain a dyeing agent; Under ultrasonic conditions of 60-70 °C and 20-25 kHz, immerse the modified fabric base layer in a dyeing agent with a mass 7-8 times that of the modified fabric base layer for ultrasonic treatment for 30-36 s, then fish it out, wash it with deionized water 3-4 times, put it in an oven at 40-60 °C and bake it for 1-1.5 h, then take it out and cool it to room temperature. Then, carry out padding under the conditions of a padding temperature of 30-35 °C and a liquor pickup rate of 85%-92% to obtain a dyed fabric base layer; (4) Orthogonal electrostatic field microwave treatment: Under an orthogonal electrostatic field of 220 kV / m, microwave conditions of 2400-2500 MHz and 700-900 W, microwave-treat the dyed fabric base layer for 28-32 min, then wash it with deionized water 3-4 times, put it in an oven at 40-60 °C and bake it for 1 h-1.5 h, then take it out and cool it to room temperature. Then, use a soaping agent with a mass 0.01-0.03 times that of the dyed fabric base layer to stir and wash it at a rotation speed of 100-120 r / min for 10 min, then wash it with deionized water 3-4 times, continue to put it in an oven at 40-60 °C and bake it for 1 h-1.5 h, then take it out and cool it to room temperature to obtain the health silk fabric.

2. The health care silk fabric according to claim 1, characterized in that, The preparation method of the fabric base layer in step (1) is as follows: Uniformly coat the surface of mulberry leaves with nano-titanium dioxide sol at 0.006 to 0.01 times the mass of the mulberry leaves, let it dry naturally, feed it to silkworms to obtain cocoons, add the cocoons to deionized water at 3 to 5 times the mass of the cocoons, then add sodium carbonate at 0.1 to 0.2 times the mass of the cocoons, stir at 120 to 180 r / min for 10 to 12 min, heat up to boiling, continue stirring for 40 to 60 min, fish out and wash with deionized water 4 to 6 times, reel the silk, use the silk as warp and weft and carry out plain weaving to obtain the fabric base layer; The silkworms selected are Jing Song Hao Yue.

3. The health care silk fabric according to claim 1, characterized in that, The soaping agent in step (4) is industrial soap.

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