A method for synergistic dyeing of Lyocell fabrics using pyrrolizin and reactive red dye.

By using a synergistic dyeing method combining pre-dyeing with reactive red dye and styraxanthin nano-suspension, the problem of low dyeing rate of styraxanthin was solved, achieving synergistic enhancement of dark color dyeing and functionality in Lyocell fabrics, and improving the color depth and functional performance of the dyed fabrics.

CN118563581BActive Publication Date: 2026-03-10QINGDAO UNIV
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-06-12
Publication Date
2026-03-10

AI Technical Summary

Technical Problem

In the existing technology, the dyeing rate of pyroxene on lyocell fabrics is low, resulting in a lighter color after dyeing. Furthermore, the functional performance of pyroxene is weak, making it difficult to achieve synergistic effects between dark-colored dyeing and functional enhancement.

Method used

Reactive red dyes were used to pre-dye Lyocell fabrics, increasing the negative charge of the fibers by introducing a large number of anionic groups. Then, styraxin nano-suspension was used for dyeing under acidic conditions, which utilized electrostatic attraction to increase the dye uptake of styraxin and achieved dark color dyeing and functional enhancement through synergistic effects.

Benefits of technology

It significantly improves the dyeing rate of styrax rubigin, achieving dark-colored dyeing effects, while enhancing the antibacterial and UV-protective properties of fabrics, breaking the technical barrier that styrax rubigin can only dye medium and light colors.

✦ Generated by Eureka AI based on patent content.

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Abstract

This invention discloses a method for synergistic dyeing of Lyocell fabric using styraxanthin and reactive red dye, comprising: (1) immersing the Lyocell fabric in reactive red dye solution, adding a dyeing accelerator and continuing to keep it warm for a certain period of time; (2) heating the dye solution to 60°C at a certain heating rate, adding a fixing agent and keeping it warm for 60 minutes, then cooling and removing the fabric; (3) washing the fabric with hot water first, then soaping for 10 minutes, removing the Lyocell fabric after soaping, cleaning and drying; (4) adjusting the pH value of the styraxanthin nano-suspension dye solution to 3; (5) immersing the Lyocell fabric in the styraxanthin nano-suspension dye solution for dyeing; (6) cleaning and soaping after dyeing; (7) removing the Lyocell fabric after soaping, cleaning and drying. This invention significantly improves the dyeing rate of styraxanthin, achieves synergistic enhancement of color and function after dyeing, greatly improves the color depth of the dyed fabric, and realizes the dark color dyeing effect of bacterial dye.
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Description

TECHNICAL FIELD

[0001] The present application belongs to the technical field of lyocell fabric dyeing, and particularly relates to a method for synergistically dyeing lyocell fabric with prodigiosin and reactive red dye. BACKGROUND

[0002] With more and more attention paid to the green environmental protection, safety and other aspects of dyes, biomass dyes have been re-attained attention due to their advantages such as environmental protection and health. Microbial pigments are rich in resources, low in cost, short in production cycle, and widely sourced, and belong to renewable resources, and are gradually becoming a research hotspot in the field of textile dyeing. Textiles dyed with the same are soft in color, good in environmental compatibility, biodegradable, and non-toxic and harmless, meeting the ecological requirements of textiles.

[0003] As a potential microbial pigment, prodigiosin has attracted much attention due to its bright color and good thermal stability. Prodigiosin has antibacterial and ultraviolet protection functions, and can impart high added value to textiles when used as a dye, and is extremely valuable for development. The microbial pigment is a red pigment, which is almost insoluble in water under neutral conditions and easily soluble in organic solvents.

[0004] Lyocell fiber is a regenerated cellulose fiber prepared by using N-methylmorpholine-N-oxide (NMMO) as a solvent and adopting a unique dry-jet wet spinning process. The production process is simple, short in cycle, and uses raw materials widely distributed in nature and abundant in reserves. The solvent used is non-toxic, and the solvent recovery rate can reach 99.7%. No harmful substances are released during the production process, and the environment is not polluted. The clothes made of the fiber are smooth in hand feeling, natural in color, high in strength, and good in moisture permeability and air permeability, and are known as green fiber in the 21st century.

[0005] At present, lyocell fabric is generally dyed with reactive dyes, and some bacterial pigments can also color the same. There are two dyeing processes, namely, dip dyeing and padding dyeing, and each process has advantages and disadvantages. As a known technology, prodigiosin is insoluble in water under neutral conditions, and its solubility in water increases under acidic conditions. By utilizing this property, the pH of the prodigiosin nanoparticle suspension dyeing solution is adjusted to be acidic, and under the high-temperature conditions of dyeing, the prodigiosin will be partially dissolved. In addition, prodigiosin is at the nanometer level, which also contributes to its dissolution under the acidic and hot conditions. During the dyeing process, the dissolved pigment molecules enter the interior of the fiber, and after the dyeing is completed, the acidic and alkaline environment on the cotton fiber is changed to neutral through water washing and soaping, and the prodigiosin changes from the dissolved state to the insoluble state, thereby depositing in the interior of the fiber, achieving dyeing, and obtaining good fastness. The techniques for dyeing lyocell fabric with bacterial dyes and reactive dyes are as follows:

[0006] CN116497614A discloses a method for improving the dyeing depth of bacterial dye prodigiosin on lyocell fabric, comprising: (1) weighing 1,2,3,4-butanetetracarboxylic acid (BTCA) solid particles and sodium hypophosphite solid particles, adding water to obtain a modified finishing liquor; (2) lyocell fabric is immersed in the modified finishing liquor, bath ratio is 1:30, temperature is set to 40℃, and immersion treatment time is set to 20min; (3) the excess modified finishing liquor on the fabric is removed by a mangle, and a modified lyocell fabric is obtained; (4) a dyeing liquor is obtained and is ready for use; (5) the pH value of the dyeing liquor is adjusted to 3; (6) the dyeing temperature is 80-100℃, the bath ratio is 1:30, and the time is 10-30min; (7) warm water is used for rinsing, and then soaping is carried out; (8) the fabric is washed with warm water first, then cold water, and is dried. The dyeing process does not need to involve organic solvents, greatly reduces the production cost, and effectively improves the dyeing depth of prodigiosin on lyocell fabric.

[0007] CN105507028A discloses a method for dyeing cellulose fiber fabric with reactive dyes, and relates to the field of textile printing and dyeing. The method comprises the following steps: (1) preparing a dyeing working solution according to 0.1-100g / L of reactive dyes and 10-30g / L of fixing alkali agent; (2) impregnating the fabric with the dyeing working solution; (3) treating at 10-90℃ for 30-36000s; and (4) steaming in saturated steam for 20-600s. The dyeing method has the advantages of high dye utilization rate, low production cost, simple operation, stable product quality and the like.

[0008] From the above patent technologies, when lyocell fabric is dyed with prodigiosin, the affinity of prodigiosin to lyocell fiber is low, resulting in low dyeing rate of prodigiosin on lyocell fabric, light color of dyed fabric and weak functional performance of pigments. Even if the K / S value of the modified fabric after dyeing is 2.71 at most, the dyeing standard of deep color series of lyocell fabric cannot be met. Although the dyeing with reactive dyes has good dyeing rate, color fastness and dyeing depth, the reactive dyes have no antibacterial activity and other functions. Therefore, how to dye lyocell fabric with bacterial dye prodigiosin, further improve the dyeing rate of prodigiosin, improve the color depth of the fabric after dyeing, realize the deep color series dyeing effect of bacterial dyes, and make the lyocell fabric have the functions of antibacterial property and ultraviolet resistance at the same time, has become a difficult problem that technicians in the field of dyeing and finishing of lyocell fabric need to solve. SUMMARY

[0009] In view of the deficiencies of the prior art, the technical problem to be solved by the present application is to provide a method for synergistically dyeing lyocell fabric with prodigiosin and reactive red dye, which can significantly improve the dyeing rate of prodigiosin, realize the synergistic effect of color and function after dyeing, greatly improve the color depth of the dyed fabric, and realize the deep color system dyeing effect of bacterial dye.

[0010] To solve the above technical problems, the technical solution adopted by the present application is: a method for synergistically dyeing lyocell fabric with prodigiosin and reactive red dye, comprising the following steps:

[0011] I. Pre-dyeing with reactive dyes:

[0012] (1) The lyocell fabric is immersed in the reactive red dyeing solution, and is kept at a certain temperature for a certain time, and then the dyeing is continued for a certain time after adding a dyeing accelerator;

[0013] (2) The dyeing solution is heated at a certain heating rate to 60 DEG C, and then is kept for 60 min after adding a fixing agent, and then is cooled and the fabric is taken out;

[0014] (3) The pre-dyed fabric is first washed with hot water, and then is soaped in a soaping solution at 90 DEG C for 10 min, and then the lyocell fabric is taken out after soaping, and is washed and dried;

[0015] II. Dyeing with prodigiosin nanosuspension:

[0016] (4) The pH value of the prodigiosin nanosuspension dyeing solution is adjusted to 3 by using an organic acid;

[0017] (5) The pre-dyed lyocell fabric is immersed in the prodigiosin nanosuspension dyeing solution for dyeing, and the dyeing temperature is 90 DEG C and the dyeing time is 20 min;

[0018] (6) After the dyeing is completed, the fabric is first washed with hot water, and then is soaped;

[0019] (7) The lyocell fabric is taken out after soaping, and is washed and dried.

[0020] The method for synergistically dyeing lyocell fabric with prodigiosin and reactive red dye, in the step (1), the amount of reactive red dye is 0.3%-3% owf, the bath ratio is 1:15, the temperature is kept at 30 DEG C for 15 min, the amount of dyeing accelerator is 40 g / L, and the dyeing is continued for 15 min at 30 DEG C after adding the dyeing accelerator.

[0021] The method for synergistically dyeing lyocell fabric with prodigiosin and reactive red dye, in the step (2), the heating rate is 2 DEG C / min, and the amount of fixing agent is 20 g / L.

[0022] The method for synergistically dyeing lyocell fabric with prodigiosin and reactive red dye, in the step (3), the soap concentration in the soap solution used for soaping is 2 g / L, the fabric is first washed with hot water and then with cold water, and the drying temperature of the oven is 70 DEG C.

[0023] The method for synergistically dyeing lyocell fabric with prodigiosin and reactive red dye, in the step (4), the organic acid is citric acid or glacial acetic acid.

[0024] The method for synergistically dyeing lyocell fabric with prodigiosin and reactive red dye, in the step (4), the concentration of prodigiosin pigment particles in the prodigiosin nano-suspension dyeing solution is 82.1 mg / L, and the average particle size is 240.7 nm.

[0025] The method for synergistically dyeing lyocell fabric with prodigiosin and reactive red dye, in the step (6), the soap concentration in the soap solution used for soaping is 2 g / L, the soaping temperature is 50 DEG C, and the soaping time is 10 min.

[0026] The method for synergistically dyeing lyocell fabric with prodigiosin and reactive red dye, in the step (7), after soaping, the lyocell fabric is first washed with hot water and then with cold water, and then dried in an oven, and the drying temperature of the oven is 70 DEG C.

[0027] The method for synergistically dyeing lyocell fabric with prodigiosin and reactive red dye, in the step (1), the reactive red dye solution used for pre-dyeing is any one of reactive red KD-8B, reactive red 3BS or reactive red 195 dye solution, and the dyeing accelerator is sodium sulfate or sodium chloride.

[0028] The method for synergistically dyeing lyocell fabric with prodigiosin and reactive red dye, in the step (2), the fixing agent is soda ash.

[0029] The advantages of this invention's method for synergistic dyeing of Lyocell fabrics using styraxanthin and reactive red dye are: first, the Lyocell fabric is pre-dyed with reactive red dye, and then over-dyed with styraxanthin. Directly using styraxanthin to dye Lyocell fabric results in a lighter color and lower pigment uptake due to the poor affinity between the pigment and Lyocell fibers. This invention pre-dyes Lyocell with reactive red dye. Because reactive dyes have a large number of anionic sulfonic acid groups, they introduce numerous anionic groups into the Lyocell fibers, significantly increasing their negative charge. Since styraxanthin is positively charged in acidic dye solutions, electrostatic attraction causes a large amount of styraxanthin to be applied to the Lyocell fabric, thus significantly increasing the styraxanthin uptake. Furthermore, since both reactive red dye and styraxanthin are red, they have a synergistic effect on the color of the Lyocell fabric. Furthermore, the increased dyeing amount of styraxone allows its functionality (including antibacterial and UV protection) to be well manifested, thus exhibiting a synergistic effect on the functionality of the dyed Lyocell fabric. The dyed fabric can reach dark shades, breaking the technical limitation that styraxone can only dye Lyocell to medium and light shades. Attached Figure Description

[0030] Figure 1 This is a process flow diagram of the synergistic staining method of the present invention. Detailed Implementation

[0031] The present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments.

[0032] In this invention, unless otherwise stated, directional terms such as "upper" and "lower" generally refer to the upper and lower positions of the device in its actual use or operating state, specifically the drawing directions in the accompanying drawings; while "inner" and "outer" refer to the outline of the device. Furthermore, in the description of this application, the term "comprising" means "including but not limited to". The terms first, second, third, etc., are used merely as illustrative purposes and do not impose numerical requirements or establish an order. The term "multiple" means "two or more".

[0033] like Figure 1 As shown, a method for synergistic dyeing of Lyocell fabric using erythromycin and reactive red dye includes the following steps:

[0034] I. Pre-dyeing with reactive dyes:

[0035] (1) Use reactive red dyeing solution to immerse Lyocell fabric, keep it at a certain temperature for a certain time, add dyeing accelerator and continue to keep it at a certain temperature for a certain time.

[0036] (2) Heat the dye liquor to 60°C at a certain heating rate, add the fixing agent and keep it warm for 60 minutes, then cool it down and take out the fabric.

[0037] (3), the fabric after pre-dyeing is washed with hot water first, and then is soaped in a soaping solution at a temperature of 90 DEG C for 10 min, and the lyocell fabric is taken out after soaping, washed, and dried;

[0038] II. Proflavine nanosuspension dyeing:

[0039] (4), the pH value of the proflavine nanosuspension dyeing solution is adjusted to 3 using an organic acid;

[0040] (5), the lyocell fabric after pre-dyeing is immersed in the proflavine nanosuspension dyeing solution for dip dyeing, the dyeing temperature is 90 DEG C, and the dyeing time is 20 min;

[0041] (6), after the dyeing is completed, the fabric is first washed with hot water, and then is soaped;

[0042] (7), the lyocell fabric is taken out after soaping, washed, and dried.

[0043] The organic acid is citric acid or glacial acetic acid, the reactive red dyeing solution is any one of reactive red KD-8B, reactive red 3BS, or reactive red 195 dyeing solution, the dyeing accelerating agent is anhydrous sodium sulfate or sodium chloride, and the color fixing agent is sodium carbonate.

[0044] The preparation process of the proflavine nanosuspension dyeing solution used in the application is as follows: ATCC 8100 Serratia marcescens is activated, and the Serratia marcescens colony with the largest colony and the deepest color in the third generation strain is inoculated into a seed culture solution (seed culture solution formula: 5 g / L of yeast powder, 10 g / L of peptone, 3 g / L of sodium chloride, and 2 g / L of potassium chloride), and is cultured in a constant-temperature culture oscillator for 12 h, at a temperature of 30 DEG C, a shaking bed speed of 160 rpm, and indoor natural light. Then, the seed culture solution is taken out using a pipette gun and is fermented in a fermentation medium for 72 h, at a temperature of 28 DEG C, a shaking bed speed of 200 rpm, and dark culture during the fermentation process (fermentation liquid formula: 15 g / L of peptone, 3 g / L of sodium chloride, 2 g / L of potassium chloride, 2 g / L of magnesium sulfate, 3 g / L of glycerol, and 18 g / L of Tween 80). After the fermentation is completed, the bacterial bodies in the fermentation liquid are removed by high-speed low-temperature centrifugation using a high-speed refrigerated centrifuge, and thus a proflavine pigment particle concentration of 82.1 mg / L and a proflavine nanosuspension dyeing solution with an average particle size of 240.7 nm are obtained.

[0045] Nanoscale prodigiosin is dispersed in the dyeing liquor in the form of small particles, in a stable and uniform suspension state, and the size of the prodigiosin particles is in the nanometer level. In addition, the nanoscale prodigiosin obtained by the fermentation method is coated by surfactant micelles, with the hydrophilic end of the surfactant facing outward and the nanoscale prodigiosin inside the micelles. The small size of the pigment and the coating of the surfactant can ensure the stability and uniformity of the dyeing liquor, which is conducive to the uniformity of the color of the dyed fabric. Prodigiosin is insoluble in water under neutral conditions, and the solubility increases with the increase of the acidity of the solution. During the dip dyeing process, the pH value of the dyeing liquor is first adjusted to 3, and during the dip dyeing process at 90°C, the solubility of the small prodigiosin particles increases under the condition of high temperature and acidity. Due to the small size, which is in the nanometer level, the dissolution of the small prodigiosin particles is facilitated, and the more prodigiosin is dissolved, the better the dyeing effect on the lyocell fabric.

[0046] The present application will be described in detail below through specific examples. The following examples are only part of the examples of the present application and are not a limitation of the present application.

[0047] Example 1:

[0048] Lyocell fabric was dip dyed with 0.3% (owf) active red KD-8B dyeing liquor, bath ratio 1:15, 30°C for 15 min, then 40 g / L sodium sulfate was added and the temperature was kept at 30°C for another 15 min, then the temperature was increased to 60°C at a rate of 2°C / min, 20 g / L sodium carbonate was added and the temperature was kept at 60°C for 60 min, then the temperature was decreased and the fabric was taken out. After dyeing, the fabric was first washed with hot water, then soaped at 90°C for 10 min, the soap concentration in the soaping liquor was 2 g / L. After soaping, the lyocell fabric was first washed with hot water, then with cold water, and then dried in an oven, the drying temperature was 70°C.

[0049] The pH value of the prodigiosin suspension dyeing liquor was adjusted to 3 with citric acid solid particles, the dyeing method was dip dyeing, the dyeing temperature was 90°C, and the dyeing time was 20 min. After dyeing, the fabric was first washed with hot water, then soaped, the soap concentration in the soaping liquor was 2 g / L, the soaping temperature was 50°C, and the soaping time was 10 min. After soaping, the lyocell fabric was first washed with hot water, then with cold water, and then dried in an oven, the drying temperature was 70°C.

[0050] Example 2:

[0051] Lycell fabric was dip dyed with 1.5% (owf) Reactive Red KD-8B dye liquor, bath ratio 1:15, 30°C for 15 min, then 40 g / L sodium sulphate was added and the temperature was kept at 30°C for another 15 min, then the temperature was raised to 60°C at a rate of 2°C / min, 20 g / L sodium carbonate was added and the temperature was kept at 60°C for 60 min, then the temperature was lowered and the fabric was taken out. After dyeing, the fabric was first washed with hot water, then soaped at 90°C for 10 min, the soap concentration in the soaping bath was 2 g / L. After soaping, the Lycell fabric was first washed with hot water, then cold water, and then dried in an oven, the drying temperature was 70°C.

[0052] Lycell fabric was dip dyed with 1.5% (owf) Reactive Red KD-8B dye liquor, bath ratio 1:15, 30°C for 15 min, then 40 g / L sodium sulphate was added and the temperature was kept at 30°C for another 15 min, then the temperature was raised to 60°C at a rate of 2°C / min, 20 g / L sodium carbonate was added and the temperature was kept at 60°C for 60 min, then the temperature was lowered and the fabric was taken out. After dyeing, the fabric was first washed with hot water, then soaped at 90°C for 10 min, the soap concentration in the soaping bath was 2 g / L. After soaping, the Lycell fabric was first washed with hot water, then cold water, and then dried in an oven, the drying temperature was 70°C.

[0053] Example 3:

[0054] Lycell fabric was dip dyed with 1.5% (owf) Reactive Red KD-8B dye liquor, bath ratio 1:15, 30°C for 15 min, then 40 g / L sodium sulphate was added and the temperature was kept at 30°C for another 15 min, then the temperature was raised to 60°C at a rate of 2°C / min, 20 g / L sodium carbonate was added and the temperature was kept at 60°C for 60 min, then the temperature was lowered and the fabric was taken out. After dyeing, the fabric was first washed with hot water, then soaped at 90°C for 10 min, the soap concentration in the soaping bath was 2 g / L. After soaping, the Lycell fabric was first washed with hot water, then cold water, and then dried in an oven, the drying temperature was 70°C.

[0055] Lycell fabric was dip dyed with 1.5% (owf) Reactive Red KD-8B dye liquor, bath ratio 1:15, 30°C for 15 min, then 40 g / L sodium sulphate was added and the temperature was kept at 30°C for another 15 min, then the temperature was raised to 60°C at a rate of 2°C / min, 20 g / L sodium carbonate was added and the temperature was kept at 60°C for 60 min, then the temperature was lowered and the fabric was taken out. After dyeing, the fabric was first washed with hot water, then soaped at 90°C for 10 min, the soap concentration in the soaping bath was 2 g / L. After soaping, the Lycell fabric was first washed with hot water, then cold water, and then dried in an oven, the drying temperature was 70°C.

[0056] The principle of this invention for synergistic dyeing of Lyocell fabrics is as follows: First, Lyocell fabrics are pre-dyed with reactive dyes. Since Lyocell fibers are cellulose fibers, their hydroxyl groups have a low degree of ionization and a small amount of negative charge. Pre-dyeing (colored modification) with reactive dyes containing a large number of anionic sulfonic acid groups introduces a large number of anionic groups into the Lyocell fibers. After the reactive dyes covalently bond with the hydroxyl groups on the fibers, the negative charge of the Lyocell fibers increases significantly. During the dyeing process using a styraxin nano-suspension dye solution, in an acidic environment, the styraxin nanoparticles dissolve into a small amount of molecular form and a large amount of ionic form of styraxin pigment. These ionic pigments are positively charged in the acidic dye solution. Under the action of electrostatic attraction, a large amount of styraxin ionic pigments adsorb onto the surface of the Lyocell fibers and enter the fiber interior, resulting in a large amount of styraxin dyeing the Lyocell fabric, thus significantly increasing the amount of styraxin dye. Since both reactive red dyes and styraxin are red, they have a synergistic effect on the color of the Lyocell fabric. In addition, the increased amount of pyroxene dyeing allows the functionality of pyroxene to be well manifested, thus also showing a synergistic effect on the functionality of dyed Lyocell fabrics.

[0057] This invention cleverly borrows the traditional technique of "over-dyeing" with synthetic dyes to obtain fabrics of different color schemes. It first pre-dyes with reactive red dye, then further dyes with microbial erythromycin, applying the concept of synergistic color enhancement to the dyeing of Lyocell fabrics with bacterial dyes. Since both reactive red dye and erythromycin are red, the further dyeing with erythromycin on the pre-dyed fabric results in a synergistic color enhancement effect, allowing for deep color depths. Simultaneously, the significantly increased erythromycin uptake enhances its antibacterial and UV-protective functions, ultimately achieving a synergistic effect of both color and function in the dyed Lyocell fabric. This overcomes the technical challenge that erythromycin can only dye Lyocell to light and medium shades, unable to achieve deep color ranges.

[0058] The performance test results of the method for synergistic dyeing of Lyocell fabrics using erythromycin and reactive red dye obtained in Examples 1-3 of this invention are as follows:

[0059] I. Testing Method:

[0060] The owf of reactive dye usage refers to the amount of dye used relative to the weight of the fabric. For example, 1% owf means that 0.01g of dye is used for 1g of fabric.

[0061] Method for testing the staining rate of styraxanthin: Dilute the initial styraxanthin staining solution and the residual staining solution 100 times with a 90% acidic ethanol aqueous solution at pH 3, and measure the absorbance at 535 nm using a spectrophotometer. Calculate the styraxanthin staining rate using the following formula (where A0 and A represent the absorbance at 535 nm of the initial staining solution and the residual staining solution after 100-fold dilution, respectively).

[0062]

[0063] After dyeing, the K / S value of the dyed fabric is measured using a Datacolor colorimeter. The K / S value indicates the depth of color of the fabric; the higher the value, the deeper the color.

[0064] Color fastness to rubbing was determined according to GB / T 3920—2008 "Textiles - Tests for Color Fastness to Rubbing". Color fastness to washing with soap was determined according to GB / T 3921—2008 "Textiles - Tests for Color Fastness to Washing with Soap". Color fastness to perspiration was tested according to GB / T 3922-2013 "Textiles - Tests for Color Fastness to Perspiration". Antibacterial properties of the fabric were tested according to GB / T 20944.3-2008 "Evaluation of Antibacterial Properties of Textiles - Part 3: Vibration Method". The ultraviolet protection factor (UPF) of the dyed fabric was tested according to AATCC 183-2004 test method.

[0065] II. Test Results:

[0066] 1. The test results of the dyeing uptake rate of the erythromycin suspension on Lyocell fabric pre-dyed with reactive red dye are shown in Table 1:

[0067] Table 1:

[0068]

[0069] Note: The smaller the Zeta potential (the larger the absolute value of the negative number), the more negative charge the fabric carries. As shown in Table 1, the Lyocell fabric pre-dyed with reactive red dye introduces a large number of anionic sulfonic acid groups, resulting in a significant increase in negative charge. In Example 3, using 3% (owf) Reactive Red KD-8B dye solution, the Zeta potential of the pre-dyed Lyocell fabric reached -18.0 mV. Under the influence of electrostatic attraction, a large amount of pyrogallol ion pigment is adsorbed onto the surface of the Lyocell fiber and enters the fiber interior, resulting in a large amount of pyrogallol dyeing the Lyocell fabric, thus significantly increasing the pyrogallol dyeing amount, with a pyrogallol dyeing rate reaching 62.3%.

[0070] 2. The dyeing effect and functional test results of the erythromycin suspension on Lyocell fabrics pre-dyed with reactive red dye are shown in Tables 2 and 3:

[0071] Table 2:

[0072]

[0073] Note: The K / S value indicates the depth of color in the fabric; the higher the value, the deeper the color. As shown in Table 2, the K / S value of the fabric after pre-dyeing with reactive red dye followed by dyeing with styraxanthin is significantly higher than that after dyeing with reactive red dye alone or dyeing with styraxanthin alone. This demonstrates that the "reactive red pre-dyeing + styraxanthin dyeing" method of this invention achieves a synergistic color enhancement effect. Therefore, the "colored modification + bacterial dyeing" technique of this invention can achieve the goal of dyeing lyocell in darker shades using styraxanthin.

[0074] Table 3:

[0075] Example 1 Example 2 Example 3 Dry rubbing fastness 5 5 5 Wet rubbing fastness 4-5 4-5 4-5 Fastness to soaping-off colour change 4 4 4 Fastness to soaping-off cotton staining 5 5 5 Fastness to soaping-off wool staining 5 5 5 Fastness to perspiration (acidic) colour change 4-5 4-5 4-5 Fastness to perspiration (alkaline) colour change 4 4 4 Bacteriostatic rate 33.3% 71.0% 96.1% UPF value 105.5 503.8 885.3

[0076] Colorfastness description: The colorfastness grades listed in the table range from 1 to 5, with 5 indicating the best colorfastness and 1 indicating the worst. UPF value represents the ultraviolet protection index; the higher the value, the better the UV protection performance. A higher antibacterial rate indicates better antibacterial performance. Therefore, the dyeing process of this invention demonstrates a functional synergistic effect.

[0077] In summary, as shown in Tables 1-3, pre-dyeing with reactive red dyes has a synergistic effect on the dyeing of erythromycin and the imparting of functionality to Lyocell fabrics, resulting in increased erythromycin dyeing rate, increased fabric color depth, and improved antibacterial and UV protection properties of the fabric.

[0078] Of course, the above description is not intended to limit the present invention, and the present invention is not limited to the examples given above. Any changes, modifications, additions or substitutions made by those skilled in the art within the scope of the present invention should be protected by the present invention.

Claims

1. A method for synergistic dyeing of Lyocell fabric with Proflavine and Reactive Red dyes, characterized in that, The method comprises the following steps: I. Pre-dyeing with reactive dyes: (1) Immersing the lyocell fabric in a reactive red dyeing solution, keeping the temperature constant for a certain period of time, and then adding a dyeing accelerator and keeping the temperature constant for a certain period of time; (2) Raising the temperature of the dyeing solution at a certain rate until reaching 60℃, adding a fixing agent and keeping the temperature constant for 60 minutes, and then lowering the temperature and taking out the fabric; (3) Washing the pre-dyed fabric with hot water first, and then soaping the fabric in a soaping solution at a temperature of 90℃ for 10 minutes, taking out the lyocell fabric after soaping, and then washing and drying the fabric; II. Dyeing with a nanosuspension of prodigiosin: (4) Adjusting the pH value of the nanosuspension of prodigiosin to 3 using an organic acid; (5) Immersing the pre-dyed lyocell fabric in the nanosuspension of prodigiosin for dyeing, and the dyeing temperature is 90℃ and the dyeing time is 20 minutes; (6) Washing the fabric with hot water after dyeing, and then soaping the fabric; (7) Taking out the lyocell fabric after soaping, and then washing and drying the fabric.

2. The method for synergistic dyeing of Lyocell fabric with Proflavine and Reactive Red dyes according to claim 1, characterized in that: In the step (1), the amount of the reactive red dye is 0.3%-3% owf, the bath ratio is 1:15, the temperature is kept constant at 30℃ for 15 minutes, the amount of the dyeing accelerator is 40g / L, and the temperature is kept constant at 30℃ for 15 minutes after adding the dyeing accelerator.

3. The method for synergistic dyeing of Lyocell fabric with Proflavine and Reactive Red dyes according to claim 1, characterized in that: In the step (2), the temperature raising rate is 2℃ / min, and the amount of the fixing agent is 20g / L.

4. The method for synergistic dyeing of Lyocell fabric with Proflavine and Reactive Red dyes according to claim 1, characterized in that: In the step (3), the concentration of the soap flakes in the soaping solution is 2g / L, the fabric is first washed with hot water and then with cold water, and the drying temperature in the oven is 70℃.

5. The method of synergistic dyeing of Lyocell fabric with Proflavine and Reactive Red dyes according to claim 1, characterized in that: In the step (4), the organic acid is citric acid or glacial acetic acid.

6. The method of synergistic dyeing of Lyocell fabric with Proflavine and Reactive Red dyes according to claim 1, characterized in that: In the step (4), the concentration of the prodigiosin pigment particles in the nanosuspension of prodigiosin is 82.1mg / L, and the average particle size is 240.7nm.

7. A process for synergistic dyeing of Lyocell fabric with Proflavine and Reactive Red dyes as claimed in claim 1, wherein: In the step (6), the concentration of the soap flakes in the soaping solution is 2g / L, the soaping temperature is 50℃, and the soaping time is 10 minutes.

8. A process for synergistic dyeing of Lyocell fabric with Proflavine and Reactive Red dyes as claimed in claim 1, wherein: In the step (7), the lyocell fabric is first washed with hot water and then with cold water after being taken out after soaping, and then the fabric is dried in an oven, and the drying temperature is 70℃.

9. A process for synergistic dyeing of Lyocell fabric with Proflavine and Reactive Red dyes as claimed in claim 1, wherein: In the step (1), the reactive red dyeing solution used for pre-dyeing is any one of reactive red KD-8B, reactive red 3BS or reactive red 195 dyeing solution, and the dyeing accelerator is sodium sulfate or sodium chloride.

10. The method of synergistic dyeing of Lyocell fabric with Proflavine and Reactive Red dyes according to claim 4, characterized in that: In the step (2), the fixing agent is soda ash.

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