A polyester-cotton one-bath dyeing process

Abstract

The application discloses a polyester-cotton one-bath dyeing process, which comprises the following steps: immersing polyester-cotton blended fabric into a dye bath containing a zinc complex of disperse dye, adjusting the pH of the dye bath to 7-8, and dyeing cotton at a temperature of 80-90 DEG C; then adjusting the pH to 3-5, and dyeing polyester at a temperature of 100-130 DEG C to obtain dyed fabric; in the low-temperature alkaline cotton dyeing stage, the complex is stably suspended in the dye bath, and the hydrolysis of disperse dye is avoided; in the high-temperature acid polyester dyeing stage, the complex is dissociated to release disperse dye, and the disperse dye diffuses into the fiber to realize the dyeing of polyester. Further, the zinc ions remaining on the dyed fabric are complexed with amine-based polymers and dopamine hydrochloride in a finishing liquid and deposited on the surface of the fabric, so that the surface of the fabric is modified, and the fabric has good sunlight color fastness, antibacterial and antistatic properties.

Description

Technical Field

[0001] This invention relates to the field of dyeing technology, and more specifically, to a one-bath dyeing process for polyester-cotton blends. Background Technology

[0002] Polyester-cotton knitted fabrics possess both the moisture-wicking properties of cotton and the excellent abrasion resistance, wrinkle-free properties, and quick-drying properties of polyester, making them an important component of knitted apparel fabrics. However, the dyeing and finishing of polyester-cotton blends has always been a challenge. Because polyester has a highly compact crystalline structure and is hydrophobic, and lacks reactive dyeing groups, disperse dyes are often used for dyeing. The dyeing process involves the disperse dye entering the amorphous regions of the polyester fiber for recrystallization, thus requiring high-temperature, acidic conditions, which facilitate fiber swelling and disperse dye diffusion. Conversely, cotton fibers have numerous hydroxyl groups on their surface, requiring reactive dyes to react with them under alkaline conditions, chemically bonding to the fiber surface, typically at low temperatures. Due to the significant differences in dyeing conditions between the two fabrics, including pH and temperature, previous efforts have been made to develop efficient and energy-saving polyester-cotton dyeing processes. To save energy and improve efficiency, developing high-temperature, alkali-resistant disperse dyes to achieve one-bath dyeing of polyester-cotton is a research hotspot in this field.

[0003] In view of this, the present invention is proposed. Summary of the Invention

[0004] This invention proposes a one-bath dyeing process for polyester and cotton, aiming to provide a method to improve the high-temperature alkali resistance of traditional disperse dyes, thereby realizing one-bath dyeing of polyester and cotton.

[0005] This invention is implemented as follows:

[0006] A one-bath dyeing process for polyester-cotton includes the following steps:

[0007] (1) Prepare the dye bath according to the dye solution composition;

[0008] The dyeing solution component includes a disperse dye-zinc complex, wherein the disperse dye in the disperse dye-zinc complex comprises a structural segment of formula (A) or formula (B):

[0009] (A)Ar1-N=N-Ar2-OH; where Ar is an aromatic ring, and Ar1 and Ar2 are independently selected from one of the following: benzene ring, thiophene ring, benzothiophene ring, thiazole ring or carbazole;

[0010] (B)

[0011] (2) Immerse the polyester-cotton blended fabric in the dye bath, adjust the pH of the dye bath to 7-8, and perform heat preservation dyeing 1 at 80-90℃; then adjust the pH to 3-5 and perform heat preservation dyeing 2 at 100-130℃ to obtain the dyed fabric with liquid.

[0012] (3) The dyed fabric with liquid is washed and / or finished and dried to obtain the dyed fabric.

[0013] This invention involves adding a disperse dye-zinc complex to the dye bath. During the alkaline, low-temperature cotton dyeing stage, this complex remains stably suspended in the dye bath, preventing hydrolysis of the disperse dye. During the acidic, high-temperature polyester dyeing stage, the complex dissociates, releasing the disperse dye, which diffuses into the fiber to dye the polyester, thereby improving the alkali resistance of the disperse dye. Under alkaline conditions, the hydroxyl hydrogen ions of Ar-OH in the disperse dye readily dissociate, thus increasing the Zn... 2+ The strong complexation strength with Ar-O- increases the stability of disperse dyes under alkaline conditions, preventing dissociation and hydrolysis, thereby improving the dyeing rate in subsequent dyeing stages. Under acidic conditions, the Ar-OH in disperse dyes tends to protonate to form Ar-OH2. + Therefore, due to electrostatic repulsion with Zn 2+ The dye dissociates and releases the disperse dye, thus achieving the dyeing of polyester.

[0014] In some embodiments, step (3) includes immersing the liquid-dyed fabric in an alkaline solution, sonicating it, washing it with water, and finally drying it to obtain the dyed fabric.

[0015] In some embodiments, step (3) includes immersing the dyed fabric in a finishing solution, sonicating and heating it in a water bath to 85-95°C for 3-6 hours, removing the fabric, washing it with water, and drying it to obtain the finished fabric; the finishing solution includes dopamine hydrochloride and / or an amine polymer; the amine polymer is at least one of polyethyleneimine and polylysine.

[0016] The present invention further involves placing the liquid-dyed fabric in a specific finishing solution for finishing. The zinc ions remaining on the liquid-dyed fabric complex with amine polymers and dopamine hydrochloride in the finishing solution and deposit on the surface of the fabric, thereby performing surface finishing modification on the fabric and giving the fabric good light fastness, antibacterial and antistatic properties.

[0017] In some embodiments, the dye solution components include: 1-2% owf of reactive dye, 1-2% owf of disperse dye-zinc complex, 30-60 g / L of sodium sulfate, 0.5-1 g / L of high-temperature leveling agent, and pH buffer.

[0018] In some embodiments, the finishing solution comprises: 1–4 g / L of an amino polymer, 0.5–2 g / L of dopamine hydrochloride, and an alkaline agent.

[0019] In some embodiments, the pH buffer is a disodium hydrogen phosphate-citric acid buffer with a pH range of 2.2 to 8.

[0020] In some implementations, adjusting the pH refers to adding disodium hydrogen phosphate or citric acid to adjust the pH of the dye bath.

[0021] In some embodiments, the incubation staining time is 20 to 30 minutes.

[0022] In some embodiments, the incubation staining time is 20 to 30 minutes.

[0023] In some embodiments, the ratio of the dye bath to the polyester-cotton blended fabric is (10:1) to (20:1).

[0024] In some embodiments, the alkaline agent is ammonia or sodium hydroxide.

[0025] In some embodiments, the pH value of the finishing solution is 9 to 11.

[0026] Under alkaline conditions, the residual disperse dye on the fabric surface can be re-complexed with zinc ions, improving the dyeing rate while avoiding reduction cleaning, shortening the process and reducing energy consumption.

[0027] In some embodiments, the disperse dye-zinc complex is prepared as follows: the disperse dye is dissolved in solvent A, then an organic zinc salt is added, homogenized and concentrated to obtain a concentrated solution; the concentrated solution is added dropwise to solvent B, and after complete precipitation, it is filtered, washed and dried to obtain a crude product; the crude product is redispersed in solvent C for recrystallization to obtain the disperse dye-zinc complex.

[0028] In some embodiments, solvent A is selected from at least one of N,N-dimethylformamide, dimethyl sulfoxide, benzene, xylene, toluene, chloroform, and dichloromethane;

[0029] In some embodiments, solvent B is selected from one of cyclohexane, cyclopentane, n-heptane, n-hexane, and water;

[0030] In some embodiments, the solvent C is selected from acetone, ethanol, benzene, toluene, and N,N-dimethylformamide;

[0031] In some embodiments, the organic zinc salt is selected from at least one of zinc acetate, zinc propionate, zinc lactate, zinc gluconate, zinc citrate, zinc stearate, and zinc glycinate;

[0032] In some embodiments, the molar ratio of the disperse dye to the organozinc salt is 2 to 6:1;

[0033] In some embodiments, the ratio of the total mass of the disperse dye and the organozinc salt to solvent A is 1 g: 80-120 mL;

[0034] In some embodiments, homogenization refers to homogenizing at a speed of 1000–2000 rpm for 10–15 min;

[0035] In some embodiments, the solid content of the concentrate is 2% to 5%;

[0036] In some embodiments, the ratio of the crude product to solvent C is 1 g: 50-80 mL;

[0037] In some embodiments, the recrystallization includes standing at 5–10°C for 48 hours, filtering to obtain crystals, rinsing and drying.

[0038] In some embodiments, the disperse dye in the disperse dye-zinc complex has one of the following molecular structures:

[0039] (A-1)

[0040] (A-2)

[0041] (A-3)

[0042] (A-4)

[0043] (B-1)

[0044] The present invention has the following beneficial effects:

[0045] This invention provides a one-bath dyeing process for polyester-cotton blends. In this process, a disperse dye-zinc complex is added. During the alkaline, low-temperature cotton dyeing stage, the complex remains stably suspended in the dye bath, preventing hydrolysis of the disperse dye. During the acidic, high-temperature polyester dyeing stage, the complex dissociates, releasing the disperse dye, which diffuses into the fiber to dye the polyester. Furthermore, the zinc ions remaining on the dyed fabric are complexed with amine polymers and dopamine hydrochloride in the finishing solution and deposited on the fabric surface, performing a surface finishing modification that gives the fabric good lightfastness, antibacterial properties, and antistatic properties. Attached Figure Description

[0046] To more clearly illustrate the technical solutions of the embodiments of the present invention, the accompanying drawings used in the embodiments will be briefly introduced below. It should be understood that the following drawings only show some embodiments of the present invention and should not be regarded as a limitation on the scope. For those skilled in the art, other related drawings can be obtained based on these drawings without creative effort.

[0047] Figure 1 The XRD patterns are of the disperse dye-zinc complex and CI Disperse Orange 54 prepared in Examples 1, 7 and 8. Detailed Implementation

[0048] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. Where specific conditions are not specified in the embodiments, conventional conditions or conditions recommended by the manufacturer shall apply. Reagents or instruments whose manufacturers are not specified are all conventional products that can be purchased commercially.

[0049] In the description of the embodiments of this application, the technical terms "first" and "second" are used only to distinguish different objects and should not be construed as indicating or implying relative importance or implicitly indicating the number, specific order, or primary and secondary relationship of the indicated technical features.

[0050] The term "embodiment" in this document means that a particular feature, structure, or characteristic described in connection with an embodiment may be included in at least one embodiment of this application. The appearance of this phrase in various places in the specification does not necessarily refer to the same embodiment, nor is it a separate or alternative embodiment that is mutually exclusive with other embodiments.

[0051] In the embodiments of this application, the term "or / and" is only a description of the relationship between related objects, indicating that there can be three kinds of relationships. For example, A or / and B can represent three situations: A exists alone, A and B exist at the same time, and B exists alone.

[0052] Additionally, the character " / " in this article generally indicates that the objects before and after it are in an "or" relationship.

[0053] In this application embodiment, "multiple" means two or more (including two), similarly, "multiple groups" means two or more (including two groups), and "multiple layers" means two or more (including two layers), unless otherwise explicitly specified and limited.

[0054] In the embodiments of this application, "at least one" means one or more.

[0055] In the embodiments of this application, the technical terms "length," "width," "thickness," "upper," "lower," "front," "rear," "left," "right," "vertical," and "horizontal," etc., indicating the orientation or positional relationship, are based on the orientation or positional relationship shown in the accompanying drawings. They are only for the convenience of describing the embodiments of this application and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation or be constructed in a specific orientation, etc., and should not be construed as a limitation on the embodiments of this application. Those skilled in the art can understand the specific meaning of the above terms in the embodiments of this application according to the specific circumstances.

[0056] The features and performance of the present invention will be further described in detail below with reference to embodiments.

[0057] Example 1

[0058] A one-bath dyeing process for polyester-cotton includes the following steps:

[0059] (1) Prepare the dye bath according to the dye solution composition;

[0060] The dye liquor components include: Reactive Orange XGN 2% o.wf., Disperse Dye-Zinc Complex 2.2% owf., Sodium Sulfate 40 g / L, Disodium Hydrogen Phosphate 27.6 g / L, Citric Acid 0.5 g / L, and High Temperature Leveling Agent TYW-646 0.8 g / L.

[0061] The preparation method of disperse dye-zinc complex is as follows: CI Disperse Orange 54 is dissolved in toluene, then zinc acetate is added, and homogenization is carried out at 1000 rpm for 12 min. Then, the mixture is heated and concentrated to a solid content of 3.25% to obtain a concentrated solution. The concentrated solution is added dropwise to three times its volume of water. After precipitation is complete, the mixture is filtered, washed with water, and dried to obtain a crude product. The crude product is redispersed in N,N-dimethylformamide for recrystallization to obtain the disperse dye-zinc complex. Based on the amount of raw material CI Disperse Orange 54 added, the yield of disperse dye-zinc complex is 68.4%.

[0062] The molar ratio of disperse dye to organozinc salt is 4:1.

[0063] The ratio of the total mass of disperse dye and organozinc salt to solvent A is 1 g: 100 mL.

[0064] The ratio of crude product to N,N-dimethylformamide is 1g: 50-80mL.

[0065] Recrystallization involves standing at 10°C for 48 hours, filtering to obtain crystals, rinsing with DMF, and then vacuum drying at 80°C to constant weight.

[0066] The high-temperature leveling agent TYW-646 was purchased from Dongguan Taiyang New Material Technology Co., Ltd.

[0067] Reactive Orange XGN was purchased from Shanghai Dyestuff Chemical Plant No. 8.

[0068] CI Dispersible Orange 54 was purchased from Shaanxi Didu Pharmaceutical Chemical Co., Ltd., and its molecular structure is as follows:

[0069]

[0070] (2) Immerse the polyester-cotton blended fabric in the dye bath, add disodium hydrogen phosphate to adjust the pH of the dye bath to 8, keep the temperature at 80℃ for 20 minutes, then add citric acid to adjust the pH to 3, keep the temperature at 120℃ for 30 minutes, then cool down to 60℃, and the dyeing is completed, and the dyed fabric with liquid is obtained.

[0071] The ratio of dye bath to fabric is 1:10.

[0072] The polyester-cotton blended fabric is a 70 / 30 polyester-cotton blended bleached fabric (13tex×13tex, 614 threads / 10cm×283 threads / 10cm).

[0073] (3) The dyed fabric was immersed in ammonia water with pH 10 and ultrasonically cleaned at 60W for 15 minutes. Then it was placed in acetone and ultrasonically cleaned for 10 minutes to recover the disperse dye-zinc complex. Finally, it was dried at 120°C to obtain the fabric.

[0074] Example 2

[0075] The difference from Example 1 is that in step (3), the dyed fabric is immersed in ammonia water with pH=10, ultrasonically controlled at 60W for 20 minutes, the fabric is taken out and washed in water at 25°C (bath ratio of 1:20) for 10 minutes, and then dried at 120°C to obtain the finished fabric.

[0076] Example 3

[0077] A one-bath dyeing process for polyester-cotton includes the following steps:

[0078] (1) Prepare dye bath and finishing solution according to the dye bath components and finishing solution components respectively;

[0079] The dye solution composition is the same as in Example 1;

[0080] The finishing solution consists of 2.5 g / L polyethyleneimine, 1.5 g / L dopamine hydrochloride, and sodium hydroxide, with a pH of 10.

[0081] Polyethyleneimine with a viscosity of 12000 MPa·s (25℃) and an amine value of 18 mg·eq / g was purchased from Gongbike New Material Technology Co., Ltd.

[0082] (2) Same as in Example 1;

[0083] (3) Immerse the dyed fabric in the finishing solution, turn on the 60W ultrasonic and heat it to 90℃ in a water bath for 4 hours. After taking out the fabric, wash it in 25℃ water (bath ratio of 1:20) for 10 minutes and dry it at 120℃ to obtain the finished fabric.

[0084] Example 4

[0085] A one-bath dyeing process for polyester-cotton includes the following steps:

[0086] (1) Prepare dye bath and finishing solution according to the dye bath components and finishing solution components respectively;

[0087] The dyeing solution components include: 1% owf of RGB reactive red, 1.2% owf of disperse dye-zinc complex, 60 g / L of sodium sulfate, 26.5 g / L of disodium hydrogen phosphate, 1.2 g / L of citric acid, and 0.5 g / L of high-temperature leveling agent TYW-646.

[0088] The preparation method of disperse dye-zinc complex is as follows: CI Disperse Red 151 is dissolved in dichloromethane, then zinc lactate is added, and homogenization is carried out at 1000 rpm for 12 min. The mixture is then heated and concentrated to a solid content of 2.02%, yielding a concentrated solution. The concentrated solution is added dropwise to three times its volume of water, and after complete precipitation, it is filtered, washed with water, and dried to obtain a crude product. The crude product is redispersed in acetone for recrystallization to obtain the disperse dye-zinc complex. Based on the amount of CI Disperse Red 151 added, the yield of the disperse dye-zinc complex is 50.3%.

[0089] The molar ratio of disperse dye to organozinc salt is 2:1.

[0090] The ratio of the total mass of disperse dye and organozinc salt to solvent A is 1 g: 100 mL.

[0091] The ratio of crude product to acetone was 1g:80mL.

[0092] Recrystallization involved standing at 10°C for 48 hours, filtering to obtain crystals, rinsing with acetone, and then vacuum drying at 80°C to constant weight.

[0093] The finishing solution consists of 4 g / L polylysine, 2 g / L dopamine hydrochloride, and sodium hydroxide, with a pH of 11.

[0094] Polylysine was purchased from Shanghai Maclean Biochemical Technology Co., Ltd.

[0095] RGB reactive red was purchased from Shanghai Dyestuff Chemical Plant No. 8.

[0096] CI Disperse Red 151 was purchased from Shenzhen Ruijite Biotechnology Co., Ltd., and its molecular structure is as follows:

[0097]

[0098] (2) Immerse the polyester-cotton blended fabric in the dye bath, add disodium hydrogen phosphate to adjust the pH of the dye bath to 7.5, keep the temperature at 90℃ for 30 minutes, then add citric acid to adjust the pH to 5, keep the temperature at 130℃ for 20 minutes, then cool down to 60℃ to finish the dyeing process and obtain the dyed fabric with liquid.

[0099] The ratio of dye bath to fabric is 1:20.

[0100] (3) Immerse the dyed fabric in the finishing solution, turn on the 60W ultrasonic and heat it to 90℃ in a water bath for 4 hours. After taking out the fabric, wash it in 25℃ water (bath ratio of 1:20) for 10 minutes and dry it at 120℃ to obtain the finished fabric.

[0101] Example 5

[0102] A one-bath dyeing process for polyester-cotton includes the following steps:

[0103] (1) Prepare dye bath and finishing solution according to the dye bath components and finishing solution components respectively;

[0104] The dyeing solution components include: Reactive Brilliant Blue KN-R 1% owf, Disperse Dye-Zinc Complex 1.2% owf, Sodium Sulfate 30 g / L, Disodium Hydrogen Phosphate 27.6 g / L, Citric Acid 0.5 g / L, and High-Temperature Leveling Agent TYW-646 1 g / L.

[0105] The preparation method of disperse dye-zinc complex is as follows: Disperse Blue 72 is dissolved in DMF, then zinc glycine is added, and homogenization is carried out at 1000 rpm for 12 min. The mixture is then heated and concentrated to a solid content of 4.88%, yielding a concentrated solution. The concentrated solution is added dropwise to three times its volume of cyclohexane. After complete precipitation, the solution is filtered, washed with cyclohexane, and dried to obtain a crude product. The crude product is redispersed in benzene for recrystallization to obtain the disperse dye-zinc complex. Based on the amount of Disperse Blue 72 added, the yield of the disperse dye-zinc complex is 68.5%.

[0106] The molar ratio of disperse dye to organozinc salt is 6:1.

[0107] The ratio of the total mass of disperse dye and organozinc salt to solvent A is 1 g: 100 mL.

[0108] The ratio of crude product to benzene was 1 g: 80 mL.

[0109] Recrystallization involved standing at 10°C for 48 hours, filtering to obtain crystals, rinsing with benzene, and then drying under vacuum at 100°C to constant weight.

[0110] The finishing solution consists of 1 g / L polyethyleneimine, 2 g / L dopamine hydrochloride, and sodium hydroxide, with a pH of 9.

[0111] Reactive Brilliant Blue KN-R was purchased from Shanghai Dyestuff Chemical Plant No. 8.

[0112] Disperse Blue 72 was purchased from Wuhan Xinyang Ruihe Chemical Technology Co., Ltd., and its molecular structure is as follows:

[0113]

[0114] (2) Immerse the polyester-cotton blended fabric in the dye bath, add disodium hydrogen phosphate to adjust the pH of the dye bath to 8, keep the temperature at 90℃ for 20 minutes, then add citric acid to adjust the pH to 4, keep the temperature at 100℃ for 20 minutes, then cool down to 60℃, and the dyeing is completed, and the dyed fabric with liquid is obtained.

[0115] The ratio of dye bath to fabric is 1:10.

[0116] (3) Immerse the dyed fabric in the finishing solution, turn on the 60W ultrasonic and heat it to 90℃ in a water bath for 4 hours. After taking out the fabric, wash it in 25℃ water (bath ratio of 1:20) for 10 minutes and dry it at 120℃ to obtain the finished fabric.

[0117] Example 6

[0118] The difference from Example 3 is that solvent A was replaced with dichloromethane instead of toluene. Based on the amount of raw material CI Disperse Orange 54 added, the yield of the disperse dye-zinc complex was 46.7%.

[0119] Example 7

[0120] The difference from Example 3 is that solvent C was replaced with benzene instead of DMF. Based on the amount of raw material CI Disperse Orange 54 added, the yield of the disperse dye-zinc complex was 71.5%.

[0121] Example 8

[0122] The difference from Example 3 is that the crude product is not recrystallized.

[0123] Example 9

[0124] The difference from Example 3 is that the molar ratio of disperse dye to organozinc salt is 2:1. Based on the amount of raw material CI Disperse Orange 54 added, the yield of the disperse dye-zinc complex is 70.9%.

[0125] Example 10

[0126] The difference from Example 3 is that the molar ratio of disperse dye to organozinc salt is 6:1. Based on the amount of raw material CI Disperse Orange 54 added, the yield of the disperse dye-zinc complex is 52.4%.

[0127] Example 11

[0128] The difference from Example 3 is that dopamine hydrochloride was not added to the finishing solution.

[0129] Example 12

[0130] The difference from Example 3 is that polyethyleneimine was not added to the finishing solution.

[0131] Comparative Example 1

[0132] A one-bath dyeing process for polyester-cotton includes the following steps:

[0133] (1) Prepare dye bath and finishing solution according to the dye bath components and finishing solution components respectively;

[0134] The dyeing solution components include: Reactive Orange XGN 2% owf, CI Disperse Orange 542% owf, Sodium sulfate 40 g / L, disodium hydrogen phosphate 27.6 g / L, citric acid 0.5 g / L, and high-temperature leveling agent TYW-646 0.8 g / L.

[0135] The finishing solution consists of 2.5 g / L polyethyleneimine, 1.5 g / L dopamine hydrochloride, and sodium hydroxide, with a pH of 10.

[0136] (2) Same as Example 3.

[0137] (3) Same as Example 3.

[0138] Comparative Example 2

[0139] A one-bath dyeing process for polyester-cotton includes the following steps:

[0140] (1) Prepare the dye bath according to the dye solution composition;

[0141] The dyeing solution components include: Reactive Orange XGN 2% owf, CI Disperse Orange 542% owf, Sodium sulfate 40 g / L, disodium hydrogen phosphate 27.6 g / L, citric acid 0.5 g / L, and high-temperature leveling agent TYW-646 0.8 g / L.

[0142] (2) Same as Example 1.

[0143] (3) Same as Example 1.

[0144] Test Example 1: Properties of Complexes

[0145] The physical properties of the disperse dye-zinc complexes prepared in Examples 1, 7, and 8, as well as the raw material CI Disperse Orange 54, were investigated, including elemental analysis, X-ray diffraction (XRD) analysis, and melting point determination. The XRD patterns are attached. Figure 1 As shown in Table 1, the melting point and Zn elemental content percentage are as follows. XRD analysis was performed using a Dandong TD-3500 X-ray diffractometer at a scanning speed of 2° / min; melting point analysis was performed using a Digipol-M70 melting point apparatus; and Zn elemental content analysis was performed using inductively coupled plasma atomic emission spectrometry (ICP).

[0146] Table 1

[0147]

[0148] From the appendix Figure 1 As shown in Table 1, the complexes of Examples 1, 7, and 8 exhibited altered crystal forms compared to CI Disperse Orange 54, and elemental analysis revealed the presence of Zn, indicating the presence of Zn. 2+ The successful introduction of [the method / process] is noteworthy. Furthermore, Example 8 is an amorphous complex with the lowest melting point; Examples 7 and 1 have different crystal forms due to recrystallization using different solvents, and the complex in Example 7 has a higher melting point. Both excessively high and low melting points are detrimental to dyeing. This demonstrates that the preparation process of the complex affects its physical properties.

[0149] Test Example 2 Apparent Color Depth K / S Value

[0150] A Datacolor 650 colorimeter was used with a D65 light source and a 10° viewing angle to measure the K / S value at the maximum absorption wavelength of the fabric. Each sample was measured four times at different locations, and the average value was taken.

[0151] Test Example 3: Colorfastness Test

[0152] The color fastness to washing of dyed fabrics was tested according to GB / T 3921-2008 "Textiles - Tests for color fastness to washing"; the color fastness to rubbing of dyed fabrics was tested according to GB / T 3920-2008 "Textiles - Tests for color fastness to washing"; and the color fastness to sunlight of dyes was tested according to GB / T 8427-2008 "Textiles - Tests for color fastness to washing";

[0153] The results of Test Example 2 and Test Example 3 are listed in Table 2.

[0154] Table 2

[0155]

[0156] As can be seen from the table, the dyed fabrics provided in the embodiments of the present invention have better color depth and color fastness compared with Comparative Examples 1 and 2. The dye baths of Comparative Examples 1 and 2 used conventional disperse dyes, and the resulting fabrics had lower color depth K / S values, indicating that the formation of the complex improved the hydrolysis resistance of the disperse dyes, preventing them from hydrolyzing during the dyeing process, thereby improving the dye uptake rate.

[0157] Examples 1 and 2 were not finished, but different cleaning methods were used. In Example 1, the dyed fabric was cleaned successively with ammonia and acetone. In the ammonia environment, the floating disperse dye on the fabric surface recombines with zinc ions under alkaline conditions to form a complex, which is then washed out in acetone, resulting in a low K / S value. In Example 2, the dyed fabric was washed successively with ammonia and water. The floating disperse dye recombines with zinc ions to form a complex, which remains on the fabric surface, resulting in a higher K / S value, but lower color fastness to soaping. Example 1 shows that using disperse dye-zinc complex as a dyeing agent allows for the recovery of disperse dye through alkaline treatment without the need for reduction washing.

[0158] Compared to Example 2, Example 3 showed a significant improvement in color fastness due to the addition of an amine polymer and dopamine hydrochloride to the finishing solution. This is because the addition of the amine polymer and dopamine hydrochloride resulted in a greater increase in the color fastness of Zn. 2+ It can be fixed on the fabric surface, and the multi-component cross-linked network forms a film on the fabric surface, thereby improving color fastness.

[0159] Example 4 uses a red dye, resulting in a high color depth. Example 7 and Example 3 used different solvent C (recrystallization solvent), and Example 8 did not undergo recrystallization, leading to different properties of the resulting disperse dye-zinc complex (see Test Example 1), and therefore different dyeing effects on fabrics.

[0160] In Example 11, no dopamine hydrochloride was added to the finishing solution. The color fastness to washing and light was significantly lower than in Example 3. This is because dopamine hydrochloride polymerized under alkaline conditions, forming insoluble substances that adhered to the fabric surface. Furthermore, the catechol groups and amine polymers on dopamine hydrochloride jointly complexed with Zn. 2+ This forms diverse film-like substances covering the fabric surface, thereby improving wash fastness; polydopamine hydrochloride with a catechol structure and Zn 2+ Complexation increases the absorption and conversion of ultraviolet light by the complex, thereby resisting the decomposition of dye by light energy and thus improving the color fastness to sunlight.

[0161] No amine polymer was added to the finishing solution in Example 12. The resulting fabric had a K / S value that was not much different from that in Example 3, but the wash fastness was lower than that in Example 3. This is because the film-forming property of the amine polymer inhibited the washing out of the dye.

[0162] Test Example 3 Antibacterial Performance Test

[0163] The antimicrobial properties of textiles were tested according to GB / T 20944.3-2008 "Evaluation of antimicrobial properties of textiles: shaking method". The samples were disinfected with ethanol and ultraviolet light before testing. The results are listed in Table 3.

[0164] Test Example 4: Antistatic Performance Test

[0165] The triboelectric voltage of textiles was measured in accordance with GB / T 12703 "Evaluation of Antistatic Performance of Textiles", and the results are listed in Table 3.

[0166] Table 3

[0167]

[0168]

[0169] As shown in Table 3, Example 3 underwent finishing compared to Examples 1 and 2, resulting in a significantly higher antibacterial rate and a significantly lower triboelectric voltage. This indicates that finishing is beneficial for improving the antibacterial and antistatic properties of the fabric. In Example 11, no dopamine hydrochloride was added to the finishing solution, and the antibacterial rate was almost the same as in Example 2, but the triboelectric voltage increased significantly. In Example 12, no amine polymer was added to the finishing solution, resulting in a significantly lower antibacterial rate and a slightly lower triboelectric voltage. These findings indicate that the addition of amine polymers, due to their positive charge, helps to disrupt bacterial cell membranes, thus exerting antibacterial activity, while the addition of dopamine hydrochloride, due to its conjugated structure, makes it conductive, thus playing an antistatic role. Although Comparative Example 1 used the same finishing solution as Example 3 to finish the dyed fabric, it lacked Zn... 2+ Because the active substance polyethyleneimine could not be fixed to the fabric surface, it had almost no antibacterial activity, similar to Example 1. Example 2 had certain antibacterial activity and antistatic properties compared to Comparative Example 1. This is because the fabric in Example 2 still had a large number of zinc ions remaining, which endowed the fabric with certain antibacterial activity and conductivity.

[0170] The above are merely preferred embodiments of the present invention and are not intended to limit the present invention. Various modifications and variations can be made to the present invention by those skilled in the art. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the scope of protection of the present invention.

Claims

1. A one-bath dyeing process for polyester-cotton, characterized in that, Includes the following steps: (1) Prepare the dye bath according to the dye solution composition; The dyeing solution composition includes a disperse dye-zinc complex and a reactive dye, wherein the disperse dye in the disperse dye-zinc complex has one of the following molecular structures: （A-1） ； （A-2） ； （A-3） ； （A-4） ； （B-1） ； (2) Immerse the polyester-cotton blended fabric in the dye bath, adjust the pH of the dye bath to 7-8, and perform heat preservation dyeing 1 at 80-90℃; then adjust the pH to 3-5 and perform heat preservation dyeing 2 at 100-130℃ to obtain the dyed fabric with liquid. (3) Immerse the dyed fabric in the finishing solution, sonicate and heat it to 85~95℃ in a water bath for 3~6 hours. After taking out the fabric, wash it with water and dry it to obtain the finished fabric. The finishing solution includes: 1~4g / L amine polymer, 0.5~2g / L dopamine hydrochloride and alkali agent. The amine polymer is at least one of polyethyleneimine and polylysine; The preparation method of the disperse dye-zinc complex is as follows: the disperse dye is dissolved in solvent A, then an organozinc salt is added, homogenized, and concentrated to obtain a concentrated solution; the concentrated solution is added dropwise to solvent B, and after complete precipitation, it is filtered, washed, and dried to obtain a crude product; the crude product is redispersed in solvent C for recrystallization to obtain the disperse dye-zinc complex; the solvent A is selected from at least one of N,N-dimethylformamide, dimethyl sulfoxide, benzene, xylene, toluene, chloroform, and dichloromethane; And / or, the solvent B is selected from one of cyclohexane, cyclopentane, n-heptane, n-hexane, and water; And / or, the solvent C is selected from acetone, ethanol, benzene, toluene, and N,N-dimethylformamide; And / or, the organic zinc salt is selected from at least one of zinc acetate, zinc propionate, zinc lactate, zinc gluconate, zinc citrate, zinc stearate, and zinc glycinate; And / or, the recrystallization includes standing at 5~10°C for 48 hours, filtering to obtain crystals, rinsing and drying.

2. The one-bath dyeing process for polyester-cotton according to claim 1, characterized in that, The dyeing solution components include: 1-2% owf of reactive dye, 1-2% owf of disperse dye-zinc complex, 30-60 g / L of sodium sulfate, 0.5-1 g / L of high-temperature leveling agent, and pH buffer.

3. The one-bath dyeing process for polyester-cotton according to any one of claims 1 to 2, characterized in that, The pH buffer solution is a disodium hydrogen phosphate-citric acid buffer solution with a pH range of 2.2 to 8; And / or, the pH adjustment refers to adjusting the pH of the dye bath by adding disodium hydrogen phosphate or citric acid; And / or, the time for the heat preservation staining 1 is 20~30 min; And / or, the time for the heat preservation staining 2 is 20~30 min; And / or, the ratio of the dye bath to the polyester-cotton blended fabric is (10:1) to (20:1).

4. The one-bath dyeing process for polyester-cotton according to claim 1, characterized in that, The alkaline agent is ammonia or sodium hydroxide; And / or, the pH value of the finishing solution is 9~11.

5. The one-bath dyeing process for polyester-cotton according to claim 1, characterized in that, The molar ratio of the disperse dye to the organozinc salt is 2~6:1; And / or, the ratio of the total mass of the disperse dye and the organozinc salt to solvent A is 1g:80~120mL; And / or, the homogenization refers to homogenizing at a speed of 1000~2000 rpm for 10~15 min; And / or, the solid content in the concentrate is 2% to 5%; And / or, the ratio of the crude product to solvent C is 1g:50~80mL.

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