Textile dye as well as preparation method and dyeing method thereof

Abstract

The invention provides a textile dye as well as a preparation method and a dyeing method thereof, the preparation method of the textile dye comprises the following specific steps: S1, carrying out superfine grinding on a natural extract until the particle size is 2-10 microns to obtain extract powder; s2, uniformly mixing the extract powder with modified glucan, metal salt grafted cellulose whiskers and polylactic acid microspheres to obtain a material; s3, adding the materials into water, stirring, curing, drying and crushing to obtain the dye. The natural extract powder, the modified glucan, the metal salt grafted cellulose whiskers and the polylactic acid microspheres are compounded, the dye is green, environmentally friendly and safe, the obtained dye is high in stability, has the effects of being high in dye uptake and uniform in dyeing and is high in affinity to textiles, and the obtained dyed textiles are good in color fastness, high in light stability, not prone to fading and good in color fastness. And the method has important popularization and application values.

Description

Technical Field

[0001] The invention relates to the technical field of textile chemical industry, and in particular to a textile dye and a preparation method and a dyeing method thereof. Background Art

[0002] Most natural dyes are extracted from plants and have the advantages of being non-toxic, harmless, environmentally friendly, regenerable, and pollution-free. Using natural pigments to dye fabrics is an ancient method, but due to its poor washing fastness and lack of bright color, it has gradually been replaced by synthetic dyes. At present, with the development of economy and culture, environmental protection, health, and green awareness have gradually gained popularity. The potential unsafe factors of synthetic dyes have caused widespread concern among people. More and more people are pursuing the naturalness of textile raw materials, and are also increasingly concerned about the safety of using dyes. Natural dyes have regained attention for their advantages such as environmental protection and health, so it is imperative to develop safe, economical, and effective natural dyes.

[0003] Therefore, the current dyeing of textiles with natural dyes needs to overcome the problems of low natural dye uptake, poor dyeing uniformity, low dyeing fastness of finished products, poor light stability, and unsuitability for actual industrial production. Summary of the invention

[0004] In view of this, the present invention provides a textile dye and a preparation method and a dyeing method thereof, which comprehensively solve the above technical problems.

[0005] The technical solution of the present invention is achieved in this way:

[0006] A method for preparing a textile dye, the specific steps comprising:

[0007] S1, ultrafinely grinding the natural extract into a particle size of 2-10 μm to obtain extract powder;

[0008] S2, mixing the extract powder, modified dextran, metal salt grafted cellulose whiskers, and polylactic acid microspheres uniformly to obtain a material;

[0009] The metal salt grafted cellulose whiskers are prepared by ultrasonically stirring the cellulose whiskers and the metal salt solution;

[0010] The modified dextran is prepared by mixing dextran, 3-aminopropyltriethoxysilane and hexadecyltriethoxysilane at 40-60° C. for 4-6 hours;

[0011] S3, adding the material into water, stirring, solidifying, drying and crushing to obtain the dye.

[0012] Furthermore, in step S1, the method for preparing the natural extract comprises:

[0013] (1) subjecting the raw material to steam explosion treatment, adding the mixture after explosion into phosphate buffer solution to adjust the pH to 6.8-7.4, and obtaining a slurry;

[0014] (2) subjecting the slurry to ultrasonic hypoxia extraction to obtain a filter residue and an extract, concentrating the extract to obtain a powder a, and storing it at a low temperature;

[0015] (3) adding the filter residue to the bacterial liquid for mixed fermentation, adding ethanol to the fermentation liquid, performing low-temperature alcohol precipitation, filtering and concentrating to obtain powder b, and mixing powder a and powder b uniformly to obtain a natural extract.

[0016] Furthermore, in step (1), the raw material is any one of red beet, cocoa peel, blue grass or orange peel; the steam explosion is carried out at 130-150° C. and 0.2-0.4 MPa for 30-60 s;

[0017] In step (2), the ultrasonic hypoxic extraction is performed at an oxygen content of 2% to 4%, 30 to 45° C., and 20 to 30 kHz for 20 to 30 minutes;

[0018] In step (3), the material-liquid ratio of the filter residue to the bacterial solution is 1:5-7 g / mL; the bacterial solution is composed of Bacillus subtilis and Candida oliveri in a mass ratio of 1-3:1; and the fermentation is carried out at 25-28° C. for 6-10 hours.

[0019] Furthermore, in step S2, the mass ratio of the extract powder to the modified dextran, the metal salt grafted cellulose whisker, and the polylactic acid microspheres is 1:0.2-0.4:1-3:0.1-0.3.

[0020] Furthermore, in step S2, the solid-to-liquid ratio of the cellulose whiskers and the metal salt solution is 1:6-8 mg / mL; the concentration of the metal salt solution is 1-3 mol / L, including zinc chloride, cerium nitrate and silver nitrate in a mass ratio of 1:2-4:0.2-0.5; and the ultrasonic stirring is at 200-300 W and 50-70° C. for 5-7 hours.

[0021] Furthermore, in step S2, the solid-liquid ratio of the dextran and 3-aminopropyltriethoxysilane and hexadecyltriethoxysilane is (10-30) mg:(4-6) mL:(3-5) mL.

[0022] A textile dye is prepared by the above preparation method.

[0023] A dyeing method for textile dyes, the specific steps comprising:

[0024] (1) pre-treating the textile to be dyed for standby use;

[0025] (2) dissolving the dye in water to obtain a dye slurry, immersing the pretreated textile to be dyed in the dye slurry, padding, baking, and setting aside;

[0026] (3) The textile treated in step (2) is subjected to ultrahigh pressure treatment, and after completion, the textile is allowed to stand at normal pressure and then soap-washed.

[0027] Furthermore, in step (1), the pretreatment is carried out at 40-60° C. and a relative humidity of 40-55% for 1-2 hours.

[0028] Furthermore, in step (3), the ultrahigh pressure treatment is carried out at 100 MPa for 60-80 min, at 300 MPa for 40-50 min, or at 500 MPa for 20-30 min.

[0029] Compared with the prior art, the present invention has the following beneficial effects:

[0030] 1. The present invention is green, environmentally friendly and safe by compounding natural extract powder, modified dextran, metal salt grafted cellulose whiskers and polylactic acid microspheres. The obtained dye has strong stability, high dyeing rate, uniform dyeing effect, strong affinity for textiles, and the obtained dyed textiles have good color fastness, high light stability, and are not easy to fade, and have important promotion and application value.

[0031] 2. The natural extract powder of the present invention is processed by steam explosion of raw materials, and ultrasonic hypoxia and bacterial fermentation are used to extract the required natural extract to the maximum extent. The powder obtained by ultrafine grinding can effectively increase the solubility and stability of the dye, can be dyed evenly, and dyed with bright colors.

[0032] 3. The reactive groups on the modified polysaccharide of the present invention can be combined with the surface of textile fibers to enhance the adhesion and stability of the dye. At the same time, the modified polysaccharide can be better dispersed without precipitation, making the dyeing more uniform. The cellulose whiskers grafted with metals Zn, Ce, and Ag of the present invention can increase the light stability, deodorization, and antibacterial ability of dyed textiles. The metal-grafted cellulose whiskers have a high specific surface area and excellent mechanical properties, forming a stable complex on the surface of textile fibers to increase durability. The polylactic acid microspheres of the present invention have good biodegradability, can control the dyeing speed of the dye, improve uniformity, and enhance the dyeing effect.

[0033] 4. The dyeing method of the dye of the present invention improves the color fastness of the dyeing, and the ultra-high pressure treatment allows the dye to evenly penetrate the interior of the fiber, shortens the dyeing time and the amount of dye used, can achieve a good dyeing effect at a lower temperature, improves production efficiency, saves energy, and improves color stability, and has good promotion value. DETAILED DESCRIPTION

[0034] In order to better understand the technical content of the present invention, specific embodiments are provided below to further illustrate the present invention.

[0035] Unless otherwise specified, the experimental methods used in the embodiments of the present invention are all conventional methods.

[0036] Unless otherwise specified, the materials, reagents, etc. used in the embodiments of the present invention can be obtained from commercial sources.

[0037] The polylactic acid microspheres of the present invention are one or more of PLGA, PLGA-PEG, and PLLG-PEG microspheres;

[0038] The Bacillus subtilis of the present invention was purchased from Guangzhou Weiyuan Biotechnology Co., Ltd.; the olive Candida was purchased from Noan Gene Technology Co., Ltd.;

[0039] The raw material of the natural extract of the present invention can be any one of red beet, cocoa peel, blue grass or orange peel.

[0040] Example 1

[0041] The preparation method of the textile dye of this embodiment comprises the following specific steps:

[0042] S1, ultrafinely grinding the natural extract into a particle size of 2-10 μm to obtain extract powder;

[0043] The preparation method of the natural extract comprises:

[0044] (1) subjecting the raw material to steam explosion treatment, specifically: treating at 140° C. and 0.3 MPa for 45 s, adding the mixture after explosion into phosphate buffer to adjust the pH to 7±0.2, and obtaining a slurry;

[0045] (2) subjecting the slurry to ultrasonic hypoxic extraction, specifically: extracting for 25 min at an oxygen content of 3%, 40° C., and 25 kHz, extracting to obtain a filter residue and an extract, concentrating the extract to obtain powder a, and storing at low temperature;

[0046] (3) adding the filter residue to the bacterial solution (Bacillus subtilis and Candida olivetica in a mass ratio of 2:1) at a solid-liquid ratio of 1:6 g / mL, fermenting at 27°C for 8 h, adding ethanol to the fermentation solution, precipitating with low-temperature alcohol, filtering and concentrating to obtain powder b, and mixing powder a and powder b to obtain a natural extract;

[0047] S2, mixing the extract powder, modified dextran, metal salt grafted cellulose whiskers, and polylactic acid microspheres in a mass ratio of 1:0.3:2:0.2 to obtain a material;

[0048] The preparation method of the metal salt grafted cellulose whiskers is as follows: according to the solid-liquid ratio of 1:7 mg / mL, cellulose whiskers are added into a 2 mol / L metal salt solution (zinc chloride, cerium nitrate and silver nitrate in a mass ratio of 1:3:0.4) and ultrasonically stirred at 250W and 60°C for 6 hours;

[0049] The preparation method of the modified dextran is as follows: adding dextran to 3-aminopropyltriethoxysilane and hexadecyltriethoxysilane at a solid-liquid ratio of 20 mg:5 mL:4 mL, and mixing at 50° C. for 5 hours;

[0050] S3, adding the material into water, stirring, solidifying, drying and crushing to obtain a dye;

[0051] The dyeing method of the textile dye comprises the following specific steps:

[0052] (1) The textile to be dyed is pretreated at 50° C. and 45% relative humidity for 1.5 h and set aside;

[0053] (2) dissolving the dye in water to obtain a dye slurry, immersing the pretreated textile to be dyed in the dye slurry, and baking at 50° C. for 4 h for later use;

[0054] (3) The textile treated in step (2) is subjected to ultrahigh pressure treatment, specifically: the treatment is carried out at 100 MPa for 60-80 min, and the textile is allowed to stand at normal pressure after completion, and then the textile is soap-washed.

[0055] Example 2

[0056] The preparation method of the textile dye of this embodiment comprises the following specific steps:

[0057] S1, ultrafinely grinding the natural extract into a particle size of 2-10 μm to obtain extract powder;

[0058] The preparation method of the natural extract comprises:

[0059] (1) steam explosion treatment of the raw material, specifically: treatment at 130° C. and 0.2 MPa for 30 s, adding the mixture after explosion into phosphate buffer to adjust the pH to 7±0.2, and obtaining a slurry;

[0060] (2) subjecting the slurry to ultrasonic hypoxic extraction, specifically: extracting for 20 min at an oxygen content of 2%, 30° C., and 20 kHz, extracting to obtain a filter residue and an extract, concentrating the extract to obtain a powder a, and storing at low temperature;

[0061] (3) adding the filter residue to the bacterial solution (Bacillus subtilis and Candida olivetica in a mass ratio of 1:1) at a solid-liquid ratio of 1:5 g / mL, fermenting at 25° C. for 6 h, adding ethanol to the fermentation solution, precipitating with low-temperature alcohol, filtering and concentrating to obtain powder b, and mixing powder a and powder b to obtain a natural extract;

[0062] S2, mixing the extract powder, modified dextran, metal salt grafted cellulose whiskers, and polylactic acid microspheres in a mass ratio of 1:0.2:1:0.1 to obtain a material;

[0063] The preparation method of the metal salt grafted cellulose whiskers is as follows: according to the solid-liquid ratio of 1:6 mg / mL, cellulose whiskers are added into a 1 mol / L metal salt solution (zinc chloride, cerium nitrate and silver nitrate in a mass ratio of 1:2:0.2) and ultrasonically stirred at 200 W and 50° C. for 5 h.

[0064] The preparation method of the modified dextran is as follows: adding dextran to 3-aminopropyltriethoxysilane and hexadecyltriethoxysilane at a solid-liquid ratio of 10 mg:4 mL:3 mL, and mixing at 40° C. for 4 hours;

[0065] S3, adding the material into water, stirring, solidifying, drying and crushing to obtain a dye;

[0066] The dyeing method of the textile dye comprises the following specific steps:

[0067] (1) The textile to be dyed is pretreated at 40° C. and 40% relative humidity for 1 h and set aside;

[0068] (2) dissolving the dye in water to obtain a dye slurry, immersing the pretreated textile to be dyed in the dye slurry, and baking at 60° C. for 5 h for later use;

[0069] (3) The textile treated in step (2) is subjected to ultrahigh pressure treatment, specifically: treating at 300 MPa for 40-50 min, leaving it to stand at normal pressure, and then soap washing the textile.

[0070] Example 3

[0071] The preparation method of the textile dye of this embodiment comprises the following specific steps:

[0072] S1, ultrafinely grinding the natural extract into a particle size of 2-10 μm to obtain extract powder;

[0073] The preparation method of the natural extract comprises:

[0074] (1) subjecting the raw material to steam explosion treatment, specifically: treating at 150° C. and 0.4 MPa for 60 s, adding the mixture after explosion into phosphate buffer to adjust the pH to 7±0.2, and obtaining a slurry;

[0075] (2) subjecting the slurry to ultrasonic hypoxic extraction, specifically: extracting for 30 min at an oxygen content of 4%, 45°C, and 30kHz to obtain a filter residue and an extract, concentrating the extract to obtain powder a, and storing at low temperature;

[0076] (3) adding the filter residue to the bacterial solution (Bacillus subtilis and Candida olivetica in a mass ratio of 3:1) at a solid-liquid ratio of 1:7 g / mL, fermenting at 28°C for 10 h, adding ethanol to the fermentation solution, precipitating with low-temperature alcohol, filtering and concentrating to obtain powder b, and mixing powder a and powder b to obtain a natural extract;

[0077] S2, mixing the extract powder, modified dextran, metal salt grafted cellulose whiskers, and polylactic acid microspheres in a mass ratio of 1:0.4:3:0.3 to obtain a material;

[0078] The preparation method of the metal salt grafted cellulose whiskers is as follows: according to the solid-liquid ratio of 1:8 mg / mL, cellulose whiskers are added into a 3 mol / L metal salt solution (zinc chloride, cerium nitrate and silver nitrate in a mass ratio of 1:4:0.5) and ultrasonically stirred at 300 W and 70° C. for 7 h.

[0079] The preparation method of the modified dextran is as follows: adding dextran to 3-aminopropyltriethoxysilane and hexadecyltriethoxysilane at a solid-liquid ratio of 30 mg:6 mL:5 mL, and mixing at 60° C. for 6 hours;

[0080] S3, adding the material into water, stirring, solidifying, drying and crushing to obtain a dye;

[0081] The dyeing method of the textile dye comprises the following specific steps:

[0082] (1) The textile to be dyed is pretreated at 60° C. and 55% relative humidity for 2 h and set aside;

[0083] (2) dissolving the dye in water to obtain a dye slurry, immersing the pretreated textile to be dyed in the dye slurry, padding, baking, and setting aside;

[0084] (3) The textile treated in step (2) is subjected to ultrahigh pressure treatment, specifically: treating at 500 MPa for 20-30 min, leaving it to stand at normal pressure, and then soaping the textile.

[0085] Comparative Example 1

[0086] The difference from Example 1 is that conventional commercially available dyes (purchased from Haitongyuan Fine Chemical Processing Factory, Bao'an District, Shenzhen City) are used and conventional dyeing methods are used for dyeing.

[0087] Comparative Example 2

[0088] The difference from Example 1 is that the preparation method of the natural extract lacks ultrasonic low-oxygen extraction, and the rest is consistent with Example 1.

[0089] That is, the preparation method of the textile dye of this comparative example comprises the following specific steps:

[0090] S1, ultrafinely grinding the natural extract into a particle size of 2-10 μm to obtain extract powder;

[0091] The preparation method of the natural extract comprises:

[0092] (1) subjecting the raw material to steam explosion treatment, specifically: treating at 140° C. and 0.3 MPa for 45 s, adding the mixture after explosion into phosphate buffer to adjust the pH to 7±0.2, and obtaining a slurry;

[0093] (2) according to the material-liquid ratio of the mixture after explosion to the bacterial solution of 1:6 g / mL, the slurry was added to the bacterial solution (Bacillus subtilis and Candida olivetica in a mass ratio of 2:1), and the mixture was fermented at 27°C for 8 h, ethanol was added to the fermentation solution, low-temperature alcohol precipitation was performed, and powder b was obtained by filtration and concentration, and powder a and powder b were mixed uniformly to obtain a natural extract;

[0094] S2, mixing the extract powder, modified dextran, metal salt grafted cellulose whiskers, and polylactic acid microspheres in a mass ratio of 1:0.3:2:0.2 to obtain a material;

[0095] The preparation method of the metal salt grafted cellulose whiskers is as follows: according to the solid-liquid ratio of 1:7 mg / mL, cellulose whiskers are added into a 2 mol / L metal salt solution (zinc chloride, cerium nitrate and silver nitrate in a mass ratio of 1:3:0.4) and ultrasonically stirred at 250W and 60°C for 6 hours;

[0096] The preparation method of the modified dextran is as follows: adding dextran to 3-aminopropyltriethoxysilane and hexadecyltriethoxysilane at a solid-liquid ratio of 20 mg:5 mL:4 mL, and mixing at 50° C. for 5 hours;

[0097] S3, adding the material into water, stirring, solidifying, drying and crushing to obtain a dye;

[0098] The dyeing method of the textile dye comprises the following specific steps:

[0099] (1) The textile to be dyed is pretreated at 50° C. and 45% relative humidity for 1.5 h and set aside;

[0100] (2) dissolving the dye in water to obtain a dye slurry, immersing the pretreated textile to be dyed in the dye slurry, and baking at 50° C. for 4 h for later use;

[0101] (3) The textile treated in step (2) is subjected to ultrahigh pressure treatment, specifically: the treatment is carried out at 100 MPa for 60-80 min, and the textile is allowed to stand at normal pressure after completion, and then the textile is soap-washed.

[0102] Comparative Example 3

[0103] The difference from Example 1 is that the metal salt grafted cellulose whiskers are replaced by metal salts, and the rest is the same as Example 1.

[0104] That is, the preparation method of the textile dye of this comparative example comprises the following specific steps:

[0105] S1, ultrafinely grinding the natural extract into a particle size of 2-10 μm to obtain extract powder;

[0106] The preparation method of the natural extract comprises:

[0107] (1) subjecting the raw material to steam explosion treatment, specifically: treating at 140° C. and 0.3 MPa for 45 s, adding the mixture after explosion into phosphate buffer to adjust the pH to 7±0.2, and obtaining a slurry;

[0108] (2) subjecting the slurry to ultrasonic hypoxic extraction, specifically: extracting for 25 min at an oxygen content of 3%, 40° C., and 25 kHz, extracting to obtain a filter residue and an extract, concentrating the extract to obtain powder a, and storing at low temperature;

[0109] (3) adding the filter residue to the bacterial solution (Bacillus subtilis and Candida olivetica in a mass ratio of 2:1) at a solid-liquid ratio of 1:6 g / mL, fermenting at 27°C for 8 h, adding ethanol to the fermentation solution, precipitating with low-temperature alcohol, filtering and concentrating to obtain powder b, and mixing powder a and powder b to obtain a natural extract;

[0110] S2, mixing the extract powder, modified dextran, metal salt (zinc chloride, cerium nitrate and silver nitrate in a mass ratio of 1:3:0.4), and polylactic acid microspheres in a mass ratio of 1:0.3:2:0.2 to obtain a material;

[0111] The preparation method of the modified dextran is as follows: adding dextran to 3-aminopropyltriethoxysilane and hexadecyltriethoxysilane at a solid-liquid ratio of 20 mg:5 mL:4 mL, and mixing at 50° C. for 5 hours;

[0112] S3, adding the material into water, stirring, solidifying, drying and crushing to obtain a dye;

[0113] The dyeing method of the textile dye comprises the following specific steps:

[0114] (1) The textile to be dyed is pretreated at 50° C. and 45% relative humidity for 1.5 h and set aside;

[0115] (2) dissolving the dye in water to obtain a dye slurry, immersing the pretreated textile to be dyed in the dye slurry, and baking at 50° C. for 4 h for later use;

[0116] (3) The textile treated in step (2) is subjected to ultrahigh pressure treatment, specifically: the treatment is carried out at 100 MPa for 60-80 min, and the textile is allowed to stand at normal pressure after completion, and then the textile is soap-washed.

[0117] Comparative Example 4

[0118] The difference from Example 1 is that the modified glucan is missing, and the other aspects are the same as Example 1.

[0119] The preparation method of the textile dye of this comparative example comprises the following specific steps:

[0120] S1, ultrafinely grinding the natural extract into a particle size of 2-10 μm to obtain extract powder;

[0121] The preparation method of the natural extract comprises:

[0122] (1) subjecting the raw material to steam explosion treatment, specifically: treating at 140° C. and 0.3 MPa for 45 s, adding the mixture after explosion into phosphate buffer to adjust the pH to 7±0.2, and obtaining a slurry;

[0123] (2) subjecting the slurry to ultrasonic hypoxic extraction, specifically: extracting for 25 min at an oxygen content of 3%, 40° C., and 25 kHz, extracting to obtain a filter residue and an extract, concentrating the extract to obtain powder a, and storing at low temperature;

[0124] (3) adding the filter residue to the bacterial solution (Bacillus subtilis and Candida olivetica in a mass ratio of 2:1) at a solid-liquid ratio of 1:6 g / mL, fermenting at 27°C for 8 h, adding ethanol to the fermentation solution, precipitating with low-temperature alcohol, filtering and concentrating to obtain powder b, and mixing powder a and powder b to obtain a natural extract;

[0125] S2, mixing the extract powder, metal salt grafted cellulose whiskers, and polylactic acid microspheres in a mass ratio of 1:2:0.2 to obtain a material;

[0126] The preparation method of the metal salt grafted cellulose whiskers is as follows: according to the solid-liquid ratio of 1:7 mg / mL, cellulose whiskers are added into a 2 mol / L metal salt solution (zinc chloride, cerium nitrate and silver nitrate in a mass ratio of 1:3:0.4) and ultrasonically stirred at 250W and 60°C for 6 hours;

[0127] S3, adding the material into water, stirring, solidifying, drying and crushing to obtain a dye;

[0128] The dyeing method of the textile dye comprises the following specific steps:

[0129] (1) The textile to be dyed is pretreated at 50° C. and 45% relative humidity for 1.5 h and set aside;

[0130] (2) dissolving the dye in water to obtain a dye slurry, immersing the pretreated textile to be dyed in the dye slurry, and baking at 50° C. for 4 h for later use;

[0131] (3) The textile treated in step (2) is subjected to ultrahigh pressure treatment, specifically: the treatment is carried out at 100 MPa for 60-80 min, and the textile is allowed to stand at normal pressure after completion, and then the textile is soap-washed.

[0132] Comparative Example 5

[0133] The difference from Example 1 is that polylactic acid microspheres are missing, and the rest is the same as Example 1.

[0134] The preparation method of the textile dye of this embodiment comprises the following specific steps:

[0135] S1, ultrafinely grinding the natural extract into a particle size of 2-10 μm to obtain extract powder;

[0136] The preparation method of the natural extract comprises:

[0137] (1) subjecting the raw material to steam explosion treatment, specifically: treating at 140° C. and 0.3 MPa for 45 s, adding the mixture after explosion into phosphate buffer to adjust the pH to 7±0.2, and obtaining a slurry;

[0138] (2) subjecting the slurry to ultrasonic hypoxic extraction, specifically: extracting for 25 min at an oxygen content of 3%, 40° C., and 25 kHz, extracting to obtain a filter residue and an extract, concentrating the extract to obtain powder a, and storing at low temperature;

[0139] (3) adding the filter residue to the bacterial solution (Bacillus subtilis and Candida olivetica in a mass ratio of 2:1) at a solid-liquid ratio of 1:6 g / mL, fermenting at 27°C for 8 h, adding ethanol to the fermentation solution, precipitating with low-temperature alcohol, filtering and concentrating to obtain powder b, and mixing powder a and powder b to obtain a natural extract;

[0140] S2, mixing the extract powder, modified dextran, and metal salt grafted cellulose whiskers in a mass ratio of 1:0.3:2 to obtain a material;

[0141] The preparation method of the metal salt grafted cellulose whiskers is as follows: according to the solid-liquid ratio of 1:7 mg / mL, cellulose whiskers are added into a 2 mol / L metal salt solution (zinc chloride, cerium nitrate and silver nitrate in a mass ratio of 1:3:0.4) and ultrasonically stirred at 250W and 60°C for 6 hours;

[0142] The preparation method of the modified dextran is as follows: adding dextran to 3-aminopropyltriethoxysilane and hexadecyltriethoxysilane at a solid-liquid ratio of 20 mg:5 mL:4 mL, and mixing at 50° C. for 5 hours;

[0143] S3, adding the material into water, stirring, solidifying, drying and crushing to obtain a dye;

[0144] The dyeing method of the textile dye comprises the following specific steps:

[0145] (1) The textile to be dyed is pretreated at 50° C. and 45% relative humidity for 1.5 h and set aside;

[0146] (2) dissolving the dye in water to obtain a dye slurry, immersing the pretreated textile to be dyed in the dye slurry, and baking at 50° C. for 4 h for later use;

[0147] (3) The textile treated in step (2) is subjected to ultrahigh pressure treatment, specifically: the treatment is carried out at 100 MPa for 60-80 min, and the textile is allowed to stand at normal pressure after completion, and then the textile is soap-washed.

[0148] Comparative Example 6

[0149] The difference from Example 1 is that no ultrahigh pressure treatment is used, and the rest is the same as Example 1.

[0150] The preparation method of the textile dye of this comparative example comprises the following specific steps:

[0151] S1, ultrafinely grinding the natural extract into a particle size of 2-10 μm to obtain extract powder;

[0152] The preparation method of the natural extract comprises:

[0153] (1) subjecting the raw material to steam explosion treatment, specifically: treating at 140° C. and 0.3 MPa for 45 s, adding the mixture after explosion into phosphate buffer to adjust the pH to 7±0.2, and obtaining a slurry;

[0154] (2) subjecting the slurry to ultrasonic hypoxic extraction, specifically: extracting for 25 min at an oxygen content of 3%, 40° C., and 25 kHz, extracting to obtain a filter residue and an extract, concentrating the extract to obtain powder a, and storing at low temperature;

[0155] (3) adding the filter residue to the bacterial solution (Bacillus subtilis and Candida olivetica in a mass ratio of 2:1) at a solid-liquid ratio of 1:6 g / mL, fermenting at 27°C for 8 h, adding ethanol to the fermentation solution, precipitating with low-temperature alcohol, filtering and concentrating to obtain powder b, and mixing powder a and powder b to obtain a natural extract;

[0156] S2, mixing the extract powder, modified dextran, metal salt grafted cellulose whiskers, and polylactic acid microspheres in a mass ratio of 1:0.3:2:0.2 to obtain a material;

[0157] The preparation method of the metal salt grafted cellulose whiskers is as follows: according to the solid-liquid ratio of 1:7 mg / mL, cellulose whiskers are added into a 2 mol / L metal salt solution (zinc chloride, cerium nitrate and silver nitrate in a mass ratio of 1:3:0.4) and ultrasonically stirred at 250W and 60°C for 6 hours;

[0158] The preparation method of the modified dextran is as follows: adding dextran to 3-aminopropyltriethoxysilane and hexadecyltriethoxysilane at a solid-liquid ratio of 20 mg:5 mL:4 mL, and mixing at 50° C. for 5 hours;

[0159] S3, adding the material into water, stirring, solidifying, drying and crushing to obtain a dye;

[0160] The dyeing method of the textile dye comprises the following specific steps:

[0161] (1) The textile to be dyed is pretreated at 50° C. and 45% relative humidity for 1.5 h and set aside;

[0162] (2) The dye is dissolved in water to obtain a dye slurry, the pretreated textile to be dyed is immersed in the dye slurry for padding, baked at 50° C. for 6 h, and the textile is then soap-washed.

[0163] Test example

[0164] The dyed textile fabrics obtained in Examples 1-3 and Comparative Examples 1-6 were subjected to performance testing tests;

[0165] Among them, 1. Color fastness to rubbing: refer to GB / T3920-2008 for color fastness to rubbing test, and analyze and record the test results;

[0166] 2. Water fastness: refer to GB / T5713-2013 for water fastness test (water temperature is set at 60℃, test samples are placed in water for 30 minutes, and gray card is used to evaluate the color change grade of the test samples);

[0167] 3. Light fastness: According to GB / T1710-2008 "Comparison of light fastness of similar coloring pigments", the light source is a xenon lamp with a quartz cover, the wavelength is 300-400nm, and the irradiance is 50±2W / m 2 , the color contrast between the unexposed part and the fully exposed part of the test sample is evaluated using a gray scale to obtain the light fastness of the test sample;

[0168] 4. Antibacterial ability test: according to GB / T 20944.3-2008 "Evaluation of antibacterial properties of textiles";

[0169] 5. Other indicators: color fixation rate, solubility, K / S value (absorption coefficient / scattering coefficient) and UPF value (ultraviolet protection factor).

[0170] The results are shown in Table 1-2.

[0171] Table 1

[0172]

[0173] Table 2

[0174]

[0175] It can be seen from Table 1-2 that, compared with Comparative Examples 1-6, the textiles obtained by the dyes and dyeing methods of Examples 1-3 of the present invention have high color fixation rate, uniform dyeing, high color fastness, and high color depth K / S value, indicating high dye uptake rate and excellent antibacterial performance.

[0176] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

Claims

1. A method for preparing a textile dye, characterized in that: The specific steps include: S1, ultrafinely grinding the natural extract into a particle size of 2-10 μm to obtain extract powder; S2, mixing the extract powder, modified dextran, metal salt grafted cellulose whiskers, and polylactic acid microspheres uniformly to obtain a material; The metal salt grafted cellulose whiskers are prepared by ultrasonically stirring the cellulose whiskers and the metal salt solution; The modified dextran is prepared by mixing dextran, 3-aminopropyltriethoxysilane and hexadecyltriethoxysilane at 40-60° C. for 4-6 hours; S3, adding the material into water, stirring, solidifying, drying and crushing to obtain the dye.

2. The method for preparing a textile dye according to claim 1, characterized in that: In step S1, the method for preparing the natural extract comprises: (1) subjecting the raw material to steam explosion treatment, adding the mixture after explosion into phosphate buffer solution to adjust the pH to 6.8-7.4, and obtaining a slurry; (2) subjecting the slurry to ultrasonic hypoxia extraction to obtain a filter residue and an extract, concentrating the extract to obtain a powder a, and storing it at a low temperature; (3) adding the filter residue to the bacterial liquid for mixed fermentation, adding ethanol to the fermentation liquid, performing low-temperature alcohol precipitation, filtering and concentrating to obtain powder b, and mixing powder a and powder b uniformly to obtain a natural extract.

3. The method for preparing a textile dye according to claim 2, characterized in that: In step (1), the raw material is any one of red beet, cocoa peel, blue grass or orange peel; the steam explosion is carried out at 130-150° C. and 0.2-0.4 MPa for 30-60 s; In step (2), the ultrasonic hypoxic extraction is performed at an oxygen content of 2% to 4%, 30 to 45° C., and 20 to 30 kHz for 20 to 30 minutes; In step (3), the material-liquid ratio of the filter residue to the bacterial solution is 1:5-7 g / mL; the bacterial solution is composed of Bacillus subtilis and Candida oliveri in a mass ratio of 1-3:1; and the fermentation is carried out at 25-28° C. for 6-10 hours.

4. The method for preparing a textile dye according to claim 1, characterized in that: In step S2, the mass ratio of the extract powder to the modified dextran, the metal salt grafted cellulose whisker, and the polylactic acid microspheres is 1:0.2-0.4:1-3:0.1-0.

3.

5. The method for preparing a textile dye according to claim 1, characterized in that: In step S2, the solid-to-liquid ratio of the cellulose whiskers to the metal salt solution is 1:6-8 mg / mL; the concentration of the metal salt solution is 1-3 mol / L, and the solution includes zinc chloride, cerium nitrate and silver nitrate in a mass ratio of 1:2-4:0.2-0.5; and the ultrasonic stirring is performed at 200-300 W and 50-70° C. for 5-7 hours.

6. The method for preparing a textile dye according to claim 1, characterized in that: In step S2, the solid-to-liquid ratio of the dextran, 3-aminopropyltriethoxysilane, and hexadecyltriethoxysilane is (10-30) mg: (4-6) mL: (3-5) mL.

7. A textile dye, prepared by the preparation method according to any one of claims 1 to 6.

8. A dyeing method for textile dyes according to claim 7, characterized in that: The specific steps include: (1) pre-treating the textile to be dyed for standby use; (2) dissolving the dye in water to obtain a dye slurry, immersing the pretreated textile to be dyed in the dye slurry, padding, baking, and setting aside; (3) The textile treated in step (2) is subjected to ultrahigh pressure treatment, and after completion, the textile is allowed to stand at normal pressure and then soap-washed.

9. A dyeing method for textile dyes according to claim 8, characterized in that: In step (1), the pretreatment is carried out at 40-60° C. and a relative humidity of 40%-55% for 1-2 hours.

10. A dyeing method for textile dyes according to claim 8, characterized in that: In step (3), the ultrahigh pressure treatment is carried out at 100 MPa for 60-80 min, at 300 MPa for 40-50 min, or at 500 MPa for 20-30 min.

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