Disperse dye one-bath dyeing method for cross-linked polyester-cotton fabric based on sucralose oxide

Abstract

The invention provides a cross-linked polyester-cotton fabric disperse dye one-bath dyeing method based on sucralose oxide, and belongs to the technical field of textile dyeing. The method comprises the following steps: S1, preparing a binary glycosyl cross-linking agent mother solution; s2, cross-linking modification of the polyester-cotton fabric; and one-bath dyeing of disperse dye. The polyester-cotton fabric modified by the chlorine-containing multi-aldehyde group cross-linking agent prepared by the invention is suitable for being dyed by a disperse dye, and the effect of carrying out one-bath dyeing on the polyester-cotton fabric by only using one disperse dye is realized. The color fastness and the wrinkle resistance of the polyester-cotton fabric modified by the chlorine-containing multi-aldehyde group cross-linking agent are improved to a certain extent.

Description

Technical Field

[0001] The invention relates to the technical field of textile dyeing, in particular to a disperse dye one-bath dyeing method for cross-linked polyester-cotton fabric based on sucralose oxide. Background Art

[0002] Cotton fiber is a common natural fiber. Textile products made from cotton fiber are widely used due to their excellent moisture absorption, warmth retention, breathability, and anti-static properties. However, the large number of hydrogen bonds formed between the macromolecules of cotton fabrics causes cotton fiber fabrics to wrinkle easily after machine washing, affecting consumers' wearing experience. Polyester fiber has the characteristics of good elasticity, high strength, and low moisture absorption. Polyester fiber also has good shape retention, can maintain a good appearance, and is not prone to wrinkling and deformation. However, polyester fiber has poor moisture absorption. During wear, sweat cannot be absorbed in time, causing the body to feel stuffy and uncomfortable. If sweating is excessive, it will adhere to the skin surface, easily breeding bacteria and causing skin itching and other problems.

[0003] Polyester-cotton blended fabrics are textiles made by mixing polyester and cotton fibers in a specific ratio. They combine the advantages of both polyester and cotton fibers while overcoming their respective shortcomings, making them very popular among consumers. However, the polyester fibers in polyester-cotton blends are thermoplastic fibers, while cotton fabrics are thermosetting fibers. Furthermore, polyester fibers are suitable for dyeing with disperse dyes under weakly acidic conditions, while cotton fibers are dyed with reactive dyes under alkaline conditions. This makes it impossible to dye both with the same dye. This significantly increases the number of steps, increases processing time, and reduces production efficiency. For example, invention patent application number 201310452306.6 discloses a one-bath, two-step exhaust dyeing method for polyester-cotton fabrics using disperse / reactive dyes, and invention patent application number 201610592627.X discloses a one-bath, two-step exhaust dyeing method for polyester-cotton fabrics using disperse / reactive dyes. These patents shorten the dyeing time by replacing the traditional two-bath method with a one-bath method, but still cannot achieve the effect of dyeing polyester-cotton fabrics with the same dye. Although the papers "Study on Pretreatment of Polyester / Cotton Fabrics and One-Bath Dyeing Process of Disperse Dyes, Liu Chong, Donghua University" and "Research on One-Bath Process of Scouring, Bleaching and Dyeing of Polyester-Cotton Knitted Fabrics, Liang Guoliang, Donghua University" both disclose a one-bath dyeing method for polyester-cotton fabrics, these methods use a large variety of reagents and have complex treatment processes.

[0004] Sucralose, also known as sucralose, is a non-nutritive, intense sweetener made from sucrose via chlorination. Its chemical name is 4,1',6'-trichloro-4,1',6'-trideoxygalactosucrose. It is a white powder that is highly soluble in water (solubility 28.2 g at 20°C), and its aqueous solution is clear and transparent. Its sweetness is 400-800 times that of sucrose. The use of sucralose in the dyeing process of polyester-cotton fabrics has important practical significance in addressing the difficulty of using a single dye simultaneously in the fabric processing, resulting in complex procedures, lengthy processing times, and low production efficiency. Summary of the Invention

[0005] In view of this, the present invention provides a one-bath dyeing method for cross-linked polyester-cotton fabric with disperse dyes based on sucralose oxide, comprising the following steps:

[0006] S1. Preparation of diglycoside cross-linking agent mother solution:

[0007] Dissolve sucralose in a non-aqueous solvent and stir evenly to obtain a sucralose solution; dissolve an oxidant in distilled water and stir evenly to obtain an oxidant aqueous solution; add the oxidant aqueous solution dropwise to the sucralose solution, and react at a temperature of -5 to 25° C. in the dark for 30 minutes to 24 hours to obtain a prepared solution; freeze the prepared solution at -60° C. to -20° C. for 1 to 12 hours, and filter to obtain a liquid that is a mother solution of a diglycosyl cross-linking agent;

[0008] S2. Cross-linking modification of polyester-cotton fabric:

[0009] The mother liquor of the dibasic sugar-based crosslinking agent is dissolved in a non-aqueous solvent, and a catalyst is added to prepare a working solution with a dibasic sugar-based crosslinking agent content of 5% to 8%. The polyester-cotton fabric is immersed in the working solution for 10 to 30 minutes, centrifuged for 10 to 30 seconds, and the amount of liquid carried by the polyester-cotton fabric is controlled to be 50% to 80%. The fabric is pre-baked, baked, washed with water to remove impurities, and dried to obtain the modified polyester-cotton fabric.

[0010] S3, dyeing: mixing disperse dye with water to obtain a dyeing solution, adjusting the pH value of the dyeing solution to between 3 and 5, immersing the modified polyester-cotton fabric described in step S2 in the dyeing solution, and sequentially performing dyeing and post-processing to obtain the processed polyester-cotton fabric.

[0011] Furthermore, the amount of sucralose in step S1 accounts for 5% to 20% of the initial total mass of the reaction system, and the non-aqueous solvent is a solvent that can form hydrogen bonds with water molecules.

[0012] Furthermore, the oxidant in step S1 is periodate, and the molar ratio of the oxidant to sucralose is 2.5-3.5:1.

[0013] Furthermore, inert gas is introduced during the reaction process in step S1, and 5% to 20% of a non-aqueous solvent is added to the prepared solution before freezing the prepared solution. The effective content of the diglycosyl crosslinking agent in the diglycosyl crosslinking agent mother solution is 5% to 15%.

[0014] Furthermore, in step S2, the catalyst is selected from at least one of zinc sulfate, magnesium chloride, and zinc chloride, the amount of the catalyst is 1-10 wt%, and the pH value of the working solution is between 2 and 5.

[0015] Furthermore, the pre-baking temperature in step S2 is 110~130°C, the pre-baking time is 10~30s, the baking temperature is 150~180°C, the baking time is 60s~300s, and the impurity removal and washing step includes: placing the baked fabric at 40~60°C, washing with water for 5~20min, controlling the bath ratio to 3~6:1, and the amount of soap flakes used in the impurity removal and washing process is 0.5~1g / L, and the amount of sodium carbonate used is 0.1~2g / L.

[0016] Furthermore, the mass fraction of the disperse dye in the dyeing solution in step S3 is 0.01% to 10%, acetic acid is used to adjust the pH of the dyeing solution, and the bath ratio of the modified polyester-cotton fabric to the dyeing solution is 1:5 to 10.

[0017] Furthermore, the dyeing process parameters of step S3 are as follows: the initial dyeing temperature is 30-50°C, then the temperature is increased to between 110-130°C at a rate of 1-10°C / min, kept at this temperature for 10-90 minutes, cooled to below 50°C, and the dye liquor is drained.

[0018] Furthermore, the post-treatment in step S3 includes placing the dyed modified polyester-cotton fabric in a solution containing hydrosulfite and sodium hydroxide, and keeping the solution at 50-80° C. for 10-30 minutes.

[0019] Furthermore, the dosage of the hydrosulfite is 0.5-10 g / L, and the dosage of sodium hydroxide is 0.1-5 g / L.

[0020] Compared with the prior art, the present invention has the following beneficial effects:

[0021] The chlorine-containing polyaldehyde cross-linking agent prepared by the invention will not form intramolecular or intermolecular acetals, and will not reduce the yield of the target product.

[0022] Each chlorine-containing polyaldehyde cross-linking agent molecule prepared by the present invention can form carboxaldehyde with 8 hydroxyl groups, thereby greatly reducing the amount of the cross-linking agent used.

[0023] The chlorine-containing polyaldehyde cross-linking agent prepared by the present invention has three chlorine elements on each molecule, and the chlorine elements cannot form hydrogen bonds with the hydroxyl groups on the fibers, thereby reducing the number of hydrogen bonds formed between the cellulose fiber macromolecules due to the hydroxyl groups. Therefore, the modified polyester-cotton fabric is suitable for dyeing with disperse dyes, achieving the effect of dyeing the polyester-cotton fabric in one bath using only one disperse dye.

[0024] The polyester-cotton fabric modified with the chlorine-containing polyaldehyde cross-linking agent prepared in the present application has a certain anti-wrinkle effect. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] Figure 1 This is the carbon NMR spectrum of the sucralose tetraaldehyde cross-linking agent prepared in Example 1 of the present invention. DETAILED DESCRIPTION

[0026] The present invention provides a one-bath dyeing method for cross-linked polyester-cotton fabric using disperse dyes based on sucralose oxide, comprising the following steps:

[0027] S1. Preparation of diglycoside cross-linking agent mother solution:

[0028] Dissolve sucralose in a non-aqueous solvent and stir evenly to obtain a sucralose solution; dissolve an oxidant in distilled water and stir evenly to obtain an oxidant aqueous solution; add the oxidant aqueous solution dropwise to the sucralose solution, and react at a temperature of -5 to 25° C. in the dark for 30 minutes to 24 hours to obtain a prepared solution; freeze the prepared solution at -60° C. to -20° C. for 1 to 12 hours, and filter to obtain a liquid that is a mother solution of a diglycosyl cross-linking agent;

[0029] S2. Cross-linking modification of polyester-cotton fabric:

[0030] The mother liquor of the dibasic sugar-based crosslinking agent is dissolved in a non-aqueous solvent, and a catalyst is added to prepare a working solution with a dibasic sugar-based crosslinking agent content of 5% to 8%. The polyester-cotton fabric is immersed in the working solution for 10 to 30 minutes, centrifuged for 10 to 30 seconds, and the amount of liquid carried by the polyester-cotton fabric is controlled to be 50% to 80%. The fabric is pre-baked, baked, washed with water to remove impurities, and dried to obtain the modified polyester-cotton fabric.

[0031] S3, dyeing: mixing disperse dye with water to obtain a dyeing solution, adjusting the pH value of the dyeing solution to between 3 and 5, immersing the modified polyester-cotton fabric described in step S2 in the dyeing solution, and sequentially performing dyeing and post-processing to obtain the processed polyester-cotton fabric.

[0032] In some embodiments of the present invention, the amount of sucralose used in step S1 accounts for 5% to 20% of the initial total mass of the reaction system.

[0033] In some embodiments of the present invention, the non-aqueous solvent in step S1 is a solvent that can form hydrogen bonds with water molecules. Preferably, the non-aqueous solvent is selected from at least one of methanol, ethanol, propanol, n-propanol, and isopropanol.

[0034] The present invention adds an alcohol non-aqueous solvent to form hydrogen bonds with the hydroxyl groups in the molecular structure of sucralose, thereby slowing down the rapid temperature rise of the reaction system after the addition of the oxidant solution, which triggers a series of adverse reactions such as runaway reaction, decomposition or structural destruction of the target product, and increase of by-products. At the same time, the sucralose molecules are protected from thermal decomposition or oxidation.

[0035] In some embodiments of the present invention, the oxidant in step S1 is periodate, and the molar ratio of the oxidant to sucralose is 2.5-3.5:1.

[0036] In some embodiments of the present invention, an inert gas is introduced during the reaction process of step S1. Preferably, the inert gas is selected from at least one of nitrogen and helium.

[0037] In some embodiments of the present invention, in step S1, 5% to 20% of a non-aqueous solvent is added to the preparation solution before freezing the preparation solution. The purpose of freezing is to remove and recover the oxidant.

[0038] In one embodiment of the present invention, the temperature of the filtration in step S1 is controlled within the range of -60°C to -20°C. Preferably, the temperature of the filtration in step (4) is controlled within the range of -40°C to -20°C. More preferably, the temperature of the filtration in step S1 is controlled within the range of -30°C.

[0039] In some embodiments of the present invention, the effective content of the diglycosyl cross-linking agent in the diglycosyl cross-linking agent mother solution in step S1 is 5% to 15%.

[0040] In some embodiments of the present invention, the main structural formula of the diglycosyl cross-linking agent is shown below: .

[0041] In some embodiments of the present invention, the content of cotton fiber in the polyester-cotton fabric in step S2 is 20%-80%, and the content of polyester is 80%-20%.

[0042] In some embodiments of the present invention, the catalyst in step S2 is selected from at least one of zinc sulfate, magnesium chloride, and zinc chloride. The amount of the catalyst in step S2 is 1-10 wt %, preferably 1-5 wt %, more preferably 3 wt %, and the pH value of the working solution in step S2 is between 2 and 5.

[0043] In some embodiments of the present invention, the pre-baking temperature in step S2 is 110-130° C., and the pre-baking time is 10-30 seconds. Preferably, the pre-baking temperature in step (2) is 110° C., and the pre-baking time is 20 seconds.

[0044] In some embodiments of the present invention, the baking temperature in step S2 is 150-180° C., and the baking time is 60s-300s. Preferably, the baking temperature is 150° C., and the baking time is 180s.

[0045] In some embodiments of the present invention, the impurity removal and washing step in step S2 includes: placing the baked fabric at 40-60° C., washing with water for 5-20 minutes, and controlling the bath ratio to be 3-6:1.

[0046] In some embodiments of the present invention, the amount of soap flakes used in the impurity removal and washing process in step S2 is 0.5-1 g / L, and the amount of sodium carbonate used is 0.1-2 g / L. Preferably, the amount of soap flakes used in the impurity removal and washing process is 0.5 g / L, and the amount of sodium carbonate used is 0.1 g / L.

[0047] In some embodiments of the present invention, the mass fraction of the disperse dye in the dyeing solution in step S3 is 0.01% to 10%, and acetic acid is used to adjust the pH of the dyeing solution.

[0048] In some embodiments of the present invention, the bath ratio of the modified polyester-cotton fabric to the dyeing solution in step S3 is 1:5-10. Preferably, the bath ratio of the modified polyester-cotton fabric to the dyeing solution is 1:8.

[0049] In some embodiments of the present invention, the dyeing process parameters of step S3 are as follows: the initial dyeing temperature is 30~50°C, then the temperature is increased to between 110~130°C at a rate of 1~10°C / min, kept warm for 10~90 minutes, cooled to below 50°C, and the dye liquor is drained. Preferably, the dyeing process parameters of step S3 are as follows: the initial dyeing temperature is 50°C, then the temperature is increased to 120°C at a rate of 5°C / min, kept warm for 30 minutes, cooled to below 50°C, and the dye liquor is drained.

[0050] In some embodiments of the present invention, the post-treatment in step S3 includes: placing the dyed modified polyester-cotton fabric in a solution containing hydrosulfur powder and sodium hydroxide, and keeping it warm at 50-80°C for 10-30 minutes. Preferably, the post-treatment includes: placing the dyed modified polyester-cotton fabric in a solution containing hydrosulfur powder and sodium hydroxide, and keeping it warm at 80°C for 30 minutes.

[0051] In some embodiments of the present invention, the dosage of the sodium hydrosulfite is 0.5-10 g / L, and the dosage of the sodium hydroxide is 0.1-5 g / L. Preferably, the dosage of the sodium hydrosulfite is 2 g / L, and the dosage of the sodium hydroxide is 0.5 g / L.

[0052] To make the objectives, technical solutions, and advantages of the present invention more clear, the technical solutions of the present invention are described clearly and completely below. Obviously, the embodiments described are only some of the embodiments of the present invention, not all of them. All other embodiments derived by persons of ordinary skill in the art based on the embodiments of the present invention without inventive effort are also within the scope of protection of the present invention.

[0053] Unless otherwise specified, the experimental methods or test methods described in the following examples are all conventional methods; the raw materials and auxiliary agents, unless otherwise specified, are all obtained from conventional commercial channels or prepared by conventional methods.

[0054] Example 1

[0055] A one-bath dyeing method for cross-linked polyester-cotton fabric using disperse dyes based on sucralose oxide, comprising the following steps:

[0056] S1. Preparation of diglycoside cross-linking agent mother solution:

[0057] S1.1. Take 50 g of sucralose and add it to 100 ml of methanol solution. Dissolve it by magnetic stirring at 600 rpm for 10 minutes to obtain a sucralose solution.

[0058] S1.2, take 83.4 g of sodium periodate, add it to 400 ml of distilled water, and dissolve it by magnetic stirring at a speed of 800 rpm for 15 minutes to obtain an aqueous solution of sodium periodate, and protect the aqueous solution of sodium periodate from light;

[0059] S1.3. Control the temperature of the sucralose solution in step (1) at 10°C, introduce high-purity nitrogen as a protective gas, and protect the sucralose solution from light. Then, use a constant pressure separatory funnel to dropwise add the light-protected sodium periodate aqueous solution at a rate of 20 ml / min. After the addition is complete, react in the dark for 2 hours to obtain a prepared solution.

[0060] S1.4. After the reaction, the prepared solution was transferred to a -30°C environment and frozen for 5 hours. Excess sodium periodate and generated sodium iodate precipitated as salt. The oxidant was recovered by vacuum filtration at -30°C, with a recovery rate of nearly 100%. The residual oxidant was tested with starch potassium iodide test paper. If the test paper did not turn blue, the recovery rate was close to 100%. The liquid obtained after filtration was the mother liquor of the diglycosyl cross-linking agent.

[0061] S2, cross-linking modification of polyester-cotton fabric (cotton content is 80%, polyester content is 20%):

[0062] S2.1. Dissolve 500 ml of the dibasic sugar-based crosslinker mother solution in 500 ml of the non-aqueous solvent methanol to prepare a working solution containing 5% effective content of the sucralose-based crosslinker. Add zinc sulfate as a catalyst at a catalyst dosage of 3%;

[0063] S2.2. Immerse a polyester-cotton fabric in the working solution for 15 minutes, centrifuge for 10 seconds, control the amount of liquid on the polyester-cotton fabric to 70%, pre-bake at 110°C for 20 seconds, bake at 150°C for 180 seconds, and wash the baked polyester-cotton fabric with water at 50°C for 5 minutes with a bath ratio of 5:1, using 0.5 g / L soap flakes and 0.1 g / L sodium carbonate, and then dry to obtain a modified polyester-cotton fabric.

[0064] S3. Staining:

[0065] Take disperse blue 56 in an amount of 1% of the mass of the dyeing solution. The structure of the disperse blue 56 is anthraquinone type. Mix the disperse blue 56 with water, add acetic acid to adjust the pH value of the dyeing solution to 4, immerse the modified polyester-cotton fabric prepared in step S2.2 in the dyeing solution, and control the bath ratio of the modified polyester-cotton fabric and the dyeing solution to be 1:8; the initial dyeing temperature is 50°C, then increase the temperature to 120°C at 5°C / min, keep warm for 30 minutes, cool to below 50°C, drain the dyeing solution, take it out, and place the polyester-cotton fabric in a solution containing hydrosulfite and sodium hydroxide, wherein the amount of hydrosulfite is 2 g / L and the amount of sodium hydroxide is 0.5 g / L, and keep warm at 80°C for 30 minutes to obtain the processed polyester-cotton fabric.

[0066] Performance testing:

[0067] 1) Testing revealed that the aldehyde content of the dibasic saccharide cross-linking agent mother liquor prepared in step S1 was 10.10 mmol / g, and calculations indicated that the yield of the target product reached 99.2%.

[0068] 50 ml of the mother solution of the dibasic sugar-based cross-linking agent was taken and dried under reduced pressure at -60°C and a pressure of 4 Pa ​​for 6 hours to obtain a water-free and organic solvent-free powder.

[0069] Take the above powder and use the nuclear magnetic resonance carbon spectroscopy (CNMR) technology to track the structure of the oxidant. The results are as follows Figure 1 As shown by Figure 1The provided C-NMR spectrum reveals two aldehyde peaks at 163 ppm and 166 ppm. Previously reported C-NMR spectra of sucrose-based tetraaldehyde crosslinkers exhibit only a single aldehyde peak, while the characterization results of the present invention show two aldehyde peaks in the C-NMR spectrum of the sucralose tetraaldehyde crosslinker. This may be because traditional sucrose-based tetraaldehyde crosslinkers are typically prepared in aqueous solution. The hydrogen ions generated by the oxidation byproduct, formic acid, readily catalyze the reaction between the aldehyde and hydroxyl groups within the sucrose ring molecule to form hemiacetals, slowing the selective oxidation rate of the ortho-hydroxyl groups in the sucrose molecule by the oxidant and reducing the yield of the sucrose-based tetraaldehyde crosslinker. Consequently, only a single aldehyde peak is detected. In contrast, the present invention pre-dissolves sucralose in a non-aqueous monohydric alcohol solvent and dissolves periodate in distilled water. After the two solutions are mixed, the monohydric alcohol forms hydrogen bonds with hydrogen atoms in water molecules, and no byproduct, formic acid, is generated. Therefore, the preparation method provided by the present invention does not catalyze the formation of intramolecular and intermolecular hemiacetals by the sucralose tetraaldehyde cross-linker, and does not reduce the yield of the target product.

[0070] II) Testing the properties of the processed polyester-cotton fabric prepared in step S3. The results are as follows:

[0071] The appearance grade measured according to GB / T18863-2002 before washing is greater than or equal to 3.5.

[0072] The formaldehyde content measured according to GB / T18401 is 0.

[0073] According to the test of GB / T3923.1, the tear strength retention rate is 80.11%.

[0074] The wrinkle recovery angle (warp + weft) of the fabric tested according to GB / T319-1997 is 303 degrees.

[0075] The fabric’s color fastness to dry rubbing tested in accordance with GB / T3920-2008 is ≥4.0, and its color fastness to wet rubbing is ≥4.0.

[0076] The light fastness of the fabric tested in accordance with GB / T8427-2019 is ≥5.

[0077] According to GB / T3921.1-2008, the washing color fastness of the fabric is basically ≥4, the dyeing depth of the polyester-cotton fabric is 15.1, and the color difference is 0.2.

[0078] Example 2

[0079] The difference from Example 1 is that the Disperse Blue 56 in step S3 is replaced by an equal amount of Disperse Red 54, and the structure of Disperse Red 54 is azo type.

[0080] The obtained polyester-cotton fabric was subjected to performance test, and the results were as follows:

[0081] The appearance grade before washing measured according to GB / T18863-2002 is greater than or equal to 3.5.

[0082] The formaldehyde content measured according to GB / T18401 is 0.

[0083] According to GB / T3923.1 test, the tear strength retention rate is 81.5%.

[0084] According to GB / T319-1997, the wrinkle recovery angle (warp + weft) of the fabric tested is 292 degrees.

[0085] According to GB / T3920-2008, the fabric’s dry rubbing color fastness is ≥4.0, and the wet rubbing color fastness is ≥3.5.

[0086] According to GB / T8427-2019, the light fastness of the fabric is ≥6.0.

[0087] According to GB / T3921.1-2008 test, the washing color fastness of the fabric is basically ≥4.0, the dyeing depth of the polyester-cotton fabric is 18.2, and the color difference is 0.4.

[0088] Example 3

[0089] The difference from Example 1 is that the Disperse Blue 56 in step S3 is replaced by an equal amount of Disperse Yellow 42, and the structure of Disperse Yellow 42 is a heterocyclic type.

[0090] The obtained polyester-cotton fabric was subjected to performance test, and the results were as follows:

[0091] The appearance grade measured according to GB / T18863-2002 before washing is greater than or equal to 3.5.

[0092] The formaldehyde content measured according to GB / T18401 is 0.

[0093] According to the test of GB / T3923.1, the tear strength retention rate is 82.3%.

[0094] The wrinkle recovery angle (warp + weft) of the fabric tested according to GB / T319-1997 is 295 degrees.

[0095] The fabric’s color fastness to dry rubbing is tested according to GB / T3920-2008 and its color fastness to wet rubbing is ≥4.

[0096] The light fastness of the fabric tested in accordance with GB / T8427-2019 is ≥6.

[0097] According to GB / T3921.1-2008, the washing color fastness of the fabric is basically ≥4, the dyeing depth of the polyester-cotton fabric is 14.3, and the color difference is 0.3.

[0098] Example 4

[0099] The difference from Example 1 is that the methanol solution in step S1.1 is replaced with an equal amount of ethanol solution, and the amount of sodium periodate used in step S1.2 is 82g. After the preparation is completed, the aldehyde content of the crosslinker is measured to be 10.15mmol / g, and the yield of the target product is calculated to reach 99.6%. In step S2.1, the weakly polar organic solvent n-propanol is added to the mother liquor of the dibasic sugar-based crosslinker to prepare a working solution with an effective content of 6% sucralose-based crosslinker. In step S2.1, magnesium chloride is used as the catalyst instead of zinc sulfate, and the amount used is 3wt%.

[0100] A polyester-cotton fabric (cotton content: 50%; polyester content: 50%) was immersed in the working solution for 20 minutes, centrifuged for 20 seconds, the fabric liquid content was controlled to be 70%, pre-dried at 110°C for 20 seconds, and baked at 150°C for 180 seconds. The baked polyester-cotton fabric was washed with water at 50°C for 5 minutes with a bath ratio of 5:1, a soap flake dosage of 0.5 g / L, a sodium carbonate dosage of 0.1 g / L, and dried to obtain a modified polyester-cotton fabric.

[0101] The dyeing process is the same as in Example 1. The properties of the processed polyester-cotton fabric are as follows:

[0102] The appearance grade measured according to GB / T18863-2002 before washing is greater than or equal to 3.5.

[0103] The formaldehyde content measured according to GB / T18401 is 0.

[0104] According to the test of GB / T3923.1, the tear strength retention rate is 83.1%.

[0105] The wrinkle recovery angle (warp + weft) of the fabric tested in accordance with GB / T319-1997 is 290 degrees.

[0106] The fabric’s color fastness to dry rubbing tested in accordance with GB / T3920-2008 is ≥4.0, and its color fastness to wet rubbing is ≥4.0.

[0107] The light fastness of the fabric tested in accordance with GB / T8427-2019 is ≥5.

[0108] According to GB / T3921.1-2008 test, the washing color fastness of the fabric is basically ≥4, the dyeing depth of the polyester-cotton fabric is 14.3, and the color difference is 0.2.

[0109] Example 5

[0110] The difference from Example 1 was that the methanol solution in step S1.1 was replaced with an equal amount of ethanol solution, and the amount of sodium periodate used in step S1.2 was 86.1 g. After the preparation, the aldehyde content of the cross-linking agent was measured to be 10.16 mmol / g, and the calculated yield of the target product reached 99.7%.

[0111] In step S2.1, a weakly polar organic solvent, isopropanol, is added to the mother liquor of the dibasic sugar-based cross-linking agent to prepare a working solution with an effective content of 5% of the sucralose-based cross-linking agent. In step S2.1, zinc chloride is used instead of zinc sulfate as a catalyst in an amount of 2.8 wt%.

[0112] A polyester-cotton fabric (cotton content: 20% and polyester content: 80%) was immersed in the working solution for 20 minutes, centrifuged for 20 seconds, the fabric carrying liquid amount was controlled to be 70%, pre-dried at 110°C for 20 seconds, and baked at 150°C for 200 seconds. The baked polyester-cotton fabric was washed with water at 50°C for 5 minutes with a bath ratio of 5:1, a soap flake dosage of 0.5 g / L, a sodium carbonate dosage of 0.1 g / L, and dried to obtain a modified polyester-cotton fabric.

[0113] The dyeing process is the same as in Example 1. The properties of the processed polyester-cotton fabric are as follows:

[0114] The appearance grade measured according to GB / T18863-2002 before washing is greater than or equal to 3.5.

[0115] The formaldehyde content measured according to GB / T18401 is 0.

[0116] According to the test of GB / T3923.1, the tear strength retention rate is 80.1%.

[0117] The wrinkle recovery angle (warp + weft) of the fabric tested according to GB / T319-1997 is 299 degrees.

[0118] The fabric’s color fastness to dry rubbing tested in accordance with GB / T3920-2008 is ≥4.0, and its color fastness to wet rubbing is ≥4.0.

[0119] The light fastness of the fabric tested in accordance with GB / T8427-2019 is ≥5.

[0120] According to GB / T3921.1-2008, the washing color fastness of the fabric is basically ≥4, the dyeing depth of the polyester-cotton fabric is 16.3, and the color difference is 0.1.

[0121] Comparative Example 1

[0122] The difference from Example 1 is that step S1 and step S2 are not included;

[0123] The staining process of step S3 is as follows:

[0124] First bath: Dyeing polyester with disperse dyes

[0125] Disperse blue 56 is taken in an amount of 1% by mass of the dyeing solution. The structure of the disperse blue 56 is anthraquinone type. The disperse blue 56 is mixed with water, and acetic acid is added to adjust the pH value of the dyeing solution to 4. The polyester-cotton fabric is immersed in the dyeing solution, and the bath ratio of the polyester-cotton fabric to the dyeing solution is controlled to be 1:8. The initial dyeing temperature is 50°C, then the temperature is increased to 120°C at a rate of 5°C / min, kept at this temperature for 30 minutes, and then cooled to below 50°C. The dyeing solution is drained and taken out. The polyester-cotton fabric is placed in a solution containing hydrosulfite and sodium hydroxide, wherein the amount of hydrosulfite is 2g / L and the amount of sodium hydroxide is 0.5g / L. The solution is kept at 80°C for 30 minutes to obtain a first bath of polyester-cotton fabric.

[0126] Second bath: reactive dyes for cellulosic dyeing

[0127] Reactive blue 19 is taken in an amount of 2.2% by mass of a dyeing solution, wherein the structure of the reactive blue 19 is anthraquinone type. The reactive blue 19 is mixed with water, acetic acid is added to adjust the pH value of the dyeing solution to 4, and a first bath polyester-cotton fabric is immersed in the dyeing solution, and the bath ratio of the first bath polyester-cotton fabric to the dyeing solution is controlled to be 1:8. The initial dyeing temperature is 30° C., then the temperature is raised to 60° C. at a rate of 5° C. / min, 5 g / L of sodium carbonate is added, and the temperature is kept at this temperature for 30 minutes, and then the temperature is lowered to below 40° C., the dyeing solution is drained, and a soaping solution is added, wherein the amount of sodium carbonate is 0.5 g / L and the amount of soap flakes is 2 g / L. The fabric is washed at 80° C. for 30 minutes to obtain a processed polyester-cotton fabric.

[0128] The obtained polyester-cotton fabric was subjected to performance test, and the results were as follows:

[0129] The appearance grade measured according to GB / T18863-2002 before washing is greater than or equal to 2.5.

[0130] The formaldehyde content measured according to GB / T18401 is 0.

[0131] According to the test of GB / T3923.1, the tear strength retention rate is 98.11%.

[0132] The wrinkle recovery angle (warp + weft) of the fabric tested according to GB / T319-1997 is 203 degrees.

[0133] The fabric’s color fastness to dry rubbing is tested according to GB / T3920-2008 and its color fastness to wet rubbing is ≥4.

[0134] The light fastness of the fabric tested in accordance with GB / T8427-2019 is ≥5.

[0135] According to GB / T3921.1-2008 test, the washing color fastness of the fabric is basically ≥4, the dyeing depth of the polyester-cotton fabric is 14.9, and the color difference is 0.2.

[0136] Comparative Example 2

[0137] The difference from Comparative Example 1 is that an equal amount of Disperse Red 54 is used to replace Disperse Blue 56 in the first bath; and an equal amount of Reactive Red 195 is used to replace Reactive Blue 19 in the second bath.

[0138] The obtained polyester-cotton fabric was subjected to performance test, and the results were as follows:

[0139] The appearance grade measured according to GB / T18863-2002 before washing is greater than or equal to 2.5.

[0140] The formaldehyde content measured according to GB / T18401 is 0.

[0141] According to the test of GB / T3923.1, the tear strength retention rate is 99.2%.

[0142] The wrinkle recovery angle (warp + weft) of the fabric tested according to GB / T319-1997 is 198 degrees.

[0143] The fabric’s color fastness to dry rubbing tested in accordance with GB / T3920-2008 is ≥4.0, and its color fastness to wet rubbing is ≥3.5.

[0144] The light fastness of the fabric tested in accordance with GB / T8427-2019 is ≥3.0.

[0145] According to GB / T3921.1-2008, the washing color fastness of the fabric is basically ≥4.0, the dyeing depth of the polyester-cotton fabric is 18.3, and the color difference is 0.3.

[0146] Comparative Example 3

[0147] The difference from Example 1 is that step S1 and step S2 are not included.

[0148] The obtained polyester-cotton fabric was subjected to performance test, and the results were as follows:

[0149] The appearance grade measured in accordance with GB / T18863-2002 before washing is greater than or equal to 2.0.

[0150] The formaldehyde content measured according to GB / T18401 is 0.

[0151] According to the test of GB / T3923.1, the tear strength retention rate is 99.5%.

[0152] The wrinkle recovery angle (warp + weft) of the fabric tested according to GB / T319-1997 is 168 degrees.

[0153] According to GB / T3920-2008, the fabric’s color fastness to dry rubbing is ≥5, and its color fastness to wet rubbing is ≥4.

[0154] The light fastness of the fabric tested in accordance with GB / T8427-2019 is ≥4.

[0155] According to GB / T3921.1-2008, the fabric's color fastness to washing is ≥4. The dyeing depth of the polyester-cotton fabric is 1.3, and the color difference is 2.5. The reason for the lighter color and larger color difference is that disperse dyes can only dye the polyester fiber, but not the cotton fiber.

[0156] Comparative Example 4

[0157] The difference from Example 1 is that the amount of sodium periodate used is 31.25 g, and the remaining steps are the same as Example 1. The aldehyde content of the obtained anti-wrinkle crosslinking agent is 6.75 mmol / g.

[0158] Comparative Example 5

[0159] The difference from Example 1 is that the amount of sodium periodate used is 62.49 g, and the remaining steps are the same as Example 1. The aldehyde content of the obtained anti-wrinkle crosslinking agent is 8.14 mmol / g.

[0160] Comparative Example 6

[0161] The difference from Example 1 is that the amount of sodium periodate used is 110 g, and the remaining steps are the same as Example 1. The aldehyde content of the obtained anti-wrinkle crosslinking agent is 7.8 mmol / g.

[0162] Comparative Example 7

[0163] The difference from Example 1 is that the sucralose in step (1) is replaced by an equal amount of sucrose, and the aldehyde content in the obtained anti-wrinkle crosslinking agent is 6.9 mmol / g.

[0164] Comparative Example 8

[0165] The difference from Example 1 is that the methanol solution in step (1) is replaced by an equal amount of distilled water, and the aldehyde content in the obtained anti-wrinkle crosslinking agent is 7.3 mmol / g.

[0166] The above is only a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principles of the present invention. These improvements and modifications should also be regarded as within the scope of protection of the present invention.

Claims

1. A one-bath dyeing method for cross-linked polyester-cotton fabrics using disperse dyes based on sucralose oxide, characterized in that: The following steps are involved: S1. Preparation of diglycoside cross-linking agent mother solution: Dissolve sucralose in a non-aqueous solvent and stir evenly to obtain a sucralose solution; dissolve an oxidant in distilled water and stir evenly to obtain an oxidant aqueous solution; add the oxidant aqueous solution dropwise to the sucralose solution, and react at a temperature of -5 to 25° C. in the dark for 30 minutes to 24 hours to obtain a prepared solution; freeze the prepared solution at -60° C. to -20° C. for 1 to 12 hours, and filter to obtain a liquid that is a mother solution of a diglycosyl cross-linking agent; S2. Cross-linking modification of polyester-cotton fabric: The mother liquor of the dibasic sugar-based crosslinking agent is dissolved in a non-aqueous solvent, and a catalyst is added to prepare a working solution with a dibasic sugar-based crosslinking agent content of 5% to 8%. The polyester-cotton fabric is immersed in the working solution for 10 to 30 minutes, centrifuged for 10 to 30 seconds, and the amount of liquid carried by the polyester-cotton fabric is controlled to be 50% to 80%. The fabric is pre-baked, baked, washed with water to remove impurities, and dried to obtain the modified polyester-cotton fabric. S3, dyeing: mixing disperse dye with water to obtain a dyeing solution, adjusting the pH value of the dyeing solution to between 3 and 5, immersing the modified polyester-cotton fabric described in step S2 in the dyeing solution, and sequentially performing dyeing and post-processing to obtain the processed polyester-cotton fabric.

2. The one-bath dyeing method for cross-linked polyester-cotton fabric using disperse dyes based on sucralose oxide according to claim 1, characterized in that: The amount of sucralose used in step S1 accounts for 5% to 20% of the initial total mass of the reaction system, and the non-aqueous solvent is a solvent that can form hydrogen bonds with water molecules.

3. The one-bath dyeing method of disperse dyes for cross-linked polyester-cotton fabrics based on sucralose oxide according to claim 1, characterized in that: The oxidant in step S1 is periodate, and the molar ratio of the oxidant to sucralose is 2.5-3.5:

1.

4. The one-bath dyeing method of disperse dyes for cross-linked polyester-cotton fabrics based on sucralose oxide according to claim 1, characterized in that: In the reaction process of step S1, an inert gas is introduced, and 5% to 20% of a non-aqueous solvent is added to the prepared solution before freezing the prepared solution. The effective content of the diglycosyl crosslinking agent in the diglycosyl crosslinking agent mother solution is 5% to 15%.

5. The one-bath dyeing method of disperse dyes for cross-linked polyester-cotton fabrics based on sucralose oxide according to claim 1, characterized in that: In step S2, the catalyst is selected from at least one of zinc sulfate, magnesium chloride, and zinc chloride, the amount of the catalyst is 1-10 wt%, and the pH value of the working solution is between 2 and 5.

6. The one-bath dyeing method of disperse dyes for cross-linked polyester-cotton fabrics based on sucralose oxide according to claim 1, characterized in that: The pre-baking temperature in step S2 is 110-130°C, the pre-baking time is 10-30s, the baking temperature is 150-180°C, the baking time is 60s-300s, and the impurity removal and washing step includes: placing the baked fabric at 40-60°C, washing it with water for 5-20min, controlling the bath ratio to 3-6:1, and using 0.5-1g / L of soap flakes and 0.1-2g / L of sodium carbonate during the impurity removal and washing process.

7. The one-bath dyeing method of disperse dyes for cross-linked polyester-cotton fabrics based on sucralose oxide according to claim 1, characterized in that: The mass fraction of the disperse dye in the dyeing solution in step S3 is 0.01% to 10%, acetic acid is used to adjust the pH of the dyeing solution, and the bath ratio of the modified polyester-cotton fabric to the dyeing solution is 1:5 to 10.

8. The one-bath dyeing method of disperse dyes for cross-linked polyester-cotton fabrics based on sucralose oxide according to claim 1, characterized in that: The dyeing process parameters of step S3 are as follows: the initial dyeing temperature is 30-50°C, then the temperature is increased to between 110-130°C at a rate of 1-10°C / min, kept at this temperature for 10-90 minutes, cooled to below 50°C, and the dye liquor is drained.

9. The one-bath dyeing method of disperse dyes for cross-linked polyester-cotton fabrics based on sucralose oxide according to claim 1, characterized in that: The post-treatment in step S3 includes placing the dyed modified polyester-cotton fabric in a solution containing hydrosulfite and sodium hydroxide, and keeping the solution at 50-80° C. for 10-30 minutes.

10. The one-bath dyeing method for cross-linked polyester-cotton fabric using disperse dyes based on sucralose oxide according to claim 9, characterized in that: The dosage of the hydrosulfite is 0.5-10 g / L, and the dosage of the sodium hydroxide is 0.1-5 g / L.

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