Anti-wrinkle cross-linking agent based on sucralose as well as preparation method and application of anti-wrinkle cross-linking agent
An anti-wrinkle crosslinking agent is prepared by reacting sucralose with periodate in a non-aqueous solvent, which solves the problem of easy wrinkling of cotton and silk fabrics, achieves efficient anti-wrinkle finishing effect and environmental protection, and improves the strength and whiteness of the fabric.
Patent Information
- Application Number
- CN202510991510.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-07-18
- Publication Date
- 2025-09-23
AI Technical Summary
Existing cotton and silk fabrics are prone to wrinkles during dyeing and finishing and daily wear. Existing formaldehyde-free anti-wrinkle finishing agents generate formic acid during the reaction process, resulting in hydrolysis degradation and poor cross-linking effects, and residual oxidants affect the strength of the fabric.
Sucralose is used as raw material, and the anti-wrinkle crosslinking agent is prepared by periodate oxidation in a non-aqueous solvent and freezing treatment in the dark. Catalysts and non-aqueous solvents are used in the fabric finishing process to improve the crosslinking effect and environmental protection.
It achieves efficient multi-aldehyde cross-linking, with high fabric appearance grade and strength retention rate, no formaldehyde residue, high whiteness and low color difference.
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Figure CN120683710A_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of textile finishing, and in particular to a sucralose-based anti-wrinkle crosslinking agent, a preparation method and application thereof. Background Art
[0002] With the continuous development of society, people pay more attention to the quality of life and demand textiles that are not only good quality, affordable, and fashionable, but also comfortable and environmentally friendly. Cotton and silk fabrics are pollution-free and environmentally friendly materials that are both abundantly available in nature and fully degraded by microorganisms after use. They have the advantages of being soft to the touch, breathable and moisture-wicking, anti-static, comfortable to wear, and economical. However, due to the large number of hydrogen bonds formed between the macromolecules of cotton and silk fabrics, cotton and silk fabrics are prone to wrinkling during dyeing and finishing and daily wear, and their smooth appearance cannot be maintained, seriously affecting their application performance and the consumer's wearing experience. Therefore, it is urgent to address the wrinkling shortcomings of cotton and silk fabrics.
[0003] Chemical crosslinking can improve the water resistance of cotton and silk macromolecules, reduce the plasticizing effect of water molecules, and enhance their wrinkle resistance and ease of care. Currently, materials used for anti-wrinkle finishing of cotton and silk are divided into formaldehyde-based and formaldehyde-free anti-wrinkle finishing agents based on whether they contain formaldehyde. Etherified 2D lipid-based finishing agents are widely used in the former. These finishing processes require the use of high-efficiency catalysts and the presence of acids, which can significantly damage cotton fabrics. Furthermore, the finishing process releases formaldehyde, making them less environmentally friendly and safe. The latter primarily includes polycarboxylic acids and polyaldehydes. For example, the paper "Preparation and Performance Study of Sugar-Based Formaldehyde-Free Anti-Wrinkle Finishes for Cotton Fabrics, Lou Jiangfei, Jiangnan University" describes a formaldehyde-free anti-wrinkle finishing agent based on glucose, fructose, sucrose, trehalose, raffinose, and stachyose. Formaldehyde-based crosslinked polyaldehyde anti-wrinkle finishing agents are produced through selective oxidation with periodate to generate aldehyde groups. The paper "Research on the Application of Aldehyde Oxidized Sucrose in Anti-wrinkle Finishing of Cotton Fabrics, Liang Yajing, Tianjin University of Technology" discloses a formaldehyde-free anti-wrinkle finishing agent that uses sucrose as the main raw material. After oxidation with sodium periodate, an oxidized sucrose solution composed of tetraaldehyde oxidized sucrose, six-membered ring hemiacetal and its hydrate is prepared. The oxidized sucrose is used in the anti-wrinkle finishing of cotton fabrics. However, the preparation of polyaldehyde cross-linking agents using binary or ternary sugars as raw materials, periodate as oxidant, and water as solvent has the following problems: 1. Formic acid is generated during the reaction, which catalyzes the hydrolysis of ether bonds between sugar rings to degrade into monocyclic sugars, reducing the yield of the target product and thus affecting the cross-linking effect of the polyaldehyde. In addition, the oxidized binary or ternary sugar cross-linking agent is very likely to form hemiacetal or acetal under the catalysis of formic acid, thereby reducing the cross-linking effect between the polyaldehyde cross-linking agent and cotton fabrics and silk; 2. Iodate is generated during the reaction. The conventional method for recovering or removing iodate is to form barium iodate by adding barium salts. However, this method cannot completely remove the oxidant. The oxidant remaining on the fabric will destroy the macromolecular structure of cotton fabrics and silk under the action of high temperature (100-150°C), thereby reducing the strength of the fabric. Summary of the Invention
[0004] In view of this, the present invention provides a method for preparing an anti-wrinkle crosslinking agent based on sucralose, comprising the following steps:
[0005] (1) dissolving sucralose in a non-aqueous solvent and stirring uniformly to obtain a sucralose solution;
[0006] (2) Dissolve the oxidant in distilled water and stir evenly to obtain an oxidant aqueous solution;
[0007] (3) adding the aqueous oxidant solution dropwise to the sucralose solution, reacting at a temperature of -5 to 25°C in the dark for 30 minutes to 24 hours to obtain a preparation solution;
[0008] (4) The prepared liquid is placed in a -60°C to -20°C environment for freezing treatment for 1 to 12 hours, and filtered to obtain the anti-wrinkle crosslinking agent.
[0009] Furthermore, the non-aqueous solvent in step (1) is a solvent that can form hydrogen bonds with water molecules, and the non-aqueous solvent is selected from at least one of methanol, ethanol, and propanol.
[0010] Furthermore, the oxidant in step (2) is a periodate, and the periodate is selected from at least one of sodium periodate and potassium periodate.
[0011] Furthermore, the molar ratio of the oxidant to sucralose is 2.5-3.5:1.
[0012] Furthermore, an inert gas is introduced during the reaction process of step (3), and the inert gas is selected from at least one of nitrogen and helium.
[0013] Furthermore, the effective content of the diglycosyl crosslinking agent in the anti-wrinkle crosslinking agent in step (4) is 5% to 15%.
[0014] Furthermore, the main structural formula of the dibasic glycoside cross-linking agent is shown below: .
[0015] The present invention also provides an anti-wrinkle cross-linking agent prepared by the method and application of the anti-wrinkle cross-linking agent in anti-wrinkle finishing of fabrics.
[0016] Furthermore, the application includes the following steps:
[0017] (1) dissolving the anti-wrinkle crosslinking agent in a non-aqueous solvent, adding a catalyst, and preparing a working solution containing 5% to 8% of the anti-wrinkle crosslinking agent;
[0018] (2) Immerse the fabric in the working solution for 10 to 30 minutes, centrifuge and dehydrate for 10 to 30 seconds, control the amount of liquid on the fabric to be 50% to 80%, pre-dry, bake, remove impurities, wash, and dry to obtain the wrinkle-resistant fabric.
[0019] Furthermore, the catalyst in step (1) 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.
[0020] Furthermore, the pre-baking temperature in step (2) is 110-130°C, the pre-baking time is 10-30s, the baking temperature is 150-180°C, the baking time is 60-300s, 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 be 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.
[0021] Compared with the prior art, the present invention has the following beneficial effects:
[0022] The chlorine-containing polyaldehyde cross-linking agent prepared by the invention will not form intramolecular or intermolecular acetal.
[0023] No formic acid is generated during the reaction, so sucralose will not be hydrolyzed during the reaction, and the yield of the chlorinated polyaldehyde-based cross-linking agent is nearly 100%.
[0024] During the cross-linking process, the present invention effectively reduces the probability of hemiacetal formation between cross-linking agents by adding a non-aqueous solvent. The non-aqueous solvent can also act as a penetrant and prevent yellowing during the anti-wrinkle finishing process of the fabric.
[0025] The appearance grade of the fabric treated with the anti-wrinkle crosslinking agent provided by the present invention is greater than or equal to 4.0 before washing, and greater than or equal to 3.5 after 50 washes. The tear strength retention rate is greater than 80%, the whiteness retention rate is greater than 90%, and the wrinkle recovery angle is greater than 300 degrees. The fabric has the characteristics of high whiteness, high strength, low color difference, and formaldehyde-free. BRIEF DESCRIPTION OF THE DRAWINGS
[0026] Figure 1 This is the carbon NMR spectrum of the sucralose tetraaldehyde cross-linking agent prepared in Example 1 of the present invention.
[0027] Figure 2 This is the carbon nuclear magnetic resonance spectrum of the sucrose aldehyde cross-linking agent prepared in Comparative Example 1 of the present invention. DETAILED DESCRIPTION
[0028] In one embodiment of the present invention, the present invention provides a method for preparing a sucralose-based anti-wrinkle crosslinking agent, comprising the following steps:
[0029] (1) dissolving sucralose in a non-aqueous solvent and stirring uniformly to obtain a sucralose solution;
[0030] (2) Dissolve the oxidant in distilled water and stir evenly to obtain an oxidant aqueous solution;
[0031] (3) adding the aqueous oxidant solution dropwise to the sucralose solution, reacting at a temperature of -5 to 25°C in the dark for 30 minutes to 24 hours to obtain a preparation solution;
[0032] (4) The prepared liquid is placed in a -60°C to -20°C environment for freezing treatment for 1 to 12 hours, and filtered to obtain the anti-wrinkle crosslinking agent.
[0033] In one embodiment of the present invention, the non-aqueous solvent in step (1) 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 one embodiment of the present invention, the oxidant in step (2) is a periodate, preferably, the periodate is selected from at least one of sodium periodate and potassium periodate.
[0036] In one embodiment of the present invention, the molar ratio of the oxidant to sucralose is 2.5-3.5:1. Preferably, the molar ratio of the oxidant to sucralose is 3:1.
[0037] In one embodiment of the present invention, an inert gas is introduced during the reaction process of step (3). Preferably, the inert gas is selected from at least one of nitrogen and helium.
[0038] In one embodiment of the present invention, 5-20 wt% of a non-aqueous solvent is added to the prepared solution before the freezing treatment in step (4). The purpose of the freezing treatment in step (4) is to remove and recover the oxidant.
[0039] In one embodiment of the present invention, the temperature of the filtration in step (4) 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 (4) is controlled within the range of -30°C.
[0040] In one embodiment of the present invention, the effective content of the diglycosyl crosslinking agent in the anti-wrinkle crosslinking agent in step (4) is 5% to 15%.
[0041] In one embodiment of the present invention, the main structural formula of the diglycosyl cross-linking agent is shown below: .
[0042] The present invention also provides an anti-wrinkle cross-linking agent prepared by the method and application of the anti-wrinkle cross-linking agent in anti-wrinkle finishing of fabrics.
[0043] In one embodiment of the present invention, the application comprises the following steps:
[0044] (1) dissolving the anti-wrinkle crosslinking agent in a non-aqueous solvent, adding a catalyst, and preparing a working solution containing 5% to 8% of the anti-wrinkle crosslinking agent;
[0045] (2) Immerse the fabric in the working solution for 10 to 30 minutes, centrifuge and dehydrate for 10 to 30 seconds, control the amount of liquid on the fabric to be 50% to 80%, pre-dry, bake, remove impurities, wash, and dry to obtain the wrinkle-resistant fabric.
[0046] In one embodiment of the present invention, the catalyst in step (1) is selected from at least one of zinc sulfate, magnesium chloride, and zinc chloride, and the amount of the catalyst is 1-10 wt %. Preferably, the amount of the catalyst is 1-6 wt %. More preferably, the amount of the catalyst is 3 wt %. The pH value of the working solution is between 2 and 5.
[0047] In one embodiment of the present invention, the pre-baking temperature in step (2) 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.
[0048] In one embodiment of the present invention, the baking temperature is 150-180° C., and the baking time is 60s-300s. Preferably, the baking temperature is 150° C., and the baking time is 180s.
[0049] In one embodiment of the present invention, the impurity removal and washing step comprises: placing the baked fabric at 40-60°C, washing with water for 5-20 minutes, controlling the bath ratio to be 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. Preferably, the impurity removal and washing step comprises: placing the baked fabric at 50°C, washing with water for 5 minutes, controlling the bath ratio to be 5:1, and the amount of soap flakes used in the impurity removal and washing process is 0.5g / L, and the amount of sodium carbonate used is 0.1g / L.
[0050] 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.
[0051] 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.
[0052] Example 1
[0053] A method for preparing an anti-wrinkle crosslinking agent based on sucralose, comprising the following steps:
[0054] (1) 50 g of sucralose was added to 100 ml of methanol solution and dissolved by magnetic stirring at a speed of 600 rpm for 10 minutes to obtain a sucralose solution;
[0055] (2) 80.68 g of sodium periodate was added to 400 ml of distilled water, and the solution was dissolved by magnetic stirring at a speed of 800 rpm for 15 minutes to obtain a sodium periodate aqueous solution, which was then protected from light.
[0056] (3) The temperature of the sucralose solution in step (1) was controlled at 10° C., high-purity nitrogen was introduced as a protective gas, and the sucralose solution was protected from light. Then, a light-protected sodium periodate aqueous solution was added dropwise using a constant pressure separatory funnel at a rate of 20 ml / min. After the addition was completed, the solution was reacted in the dark for 2 hours to obtain a prepared solution;
[0057] (4) After the reaction, the prepared solution was transferred to a -30°C environment and frozen for 5 hours. The excess sodium periodate and the generated sodium iodate precipitated in the form of salt. The oxidant was recovered by vacuum filtration at -30°C, and the recovery rate was close to 100%. The residual oxidant was tested with starch potassium iodide test paper, and it was found that the test paper did not turn blue, indicating that the recovery rate was close to 100%. The liquid obtained after filtration was the anti-wrinkle crosslinking agent.
[0058] The aldehyde content of the anti-wrinkle crosslinking agent is 10.10 mmol / g, and the yield of the target product is calculated to be 99.2%.
[0059] 50 ml of the anti-wrinkle crosslinking 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.
[0060] 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.
[0061] The anti-wrinkle processing technology of non-ironing white silk fabric includes the following specific steps:
[0062] (1) 500 ml of the anti-wrinkle crosslinking agent was dissolved in 500 ml of methanol, a non-aqueous solvent, to prepare a working solution containing 5% of the effective content of the sucralose-based anti-wrinkle crosslinking agent, and zinc sulfate was added as a catalyst in an amount of 3%;
[0063] (2) Immerse the white silk fabric to be wrinkle-free in the working solution for 15 minutes, centrifuge and dehydrate for 10 seconds, control the amount of liquid on the fabric to be 70%, pre-bake at 110°C for 20 seconds, bake at 150°C for 180 seconds, wash the baked silk fabric 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 dry to obtain wrinkle-resistant silk fabric.
[0064] The performance test of the wrinkle-resistant silk fabric prepared in Example 1 was carried out, and the test results are as follows:
[0065] The appearance grade measured in accordance with GB / T18863-2002 is greater than or equal to 4.0 before washing, and greater than or equal to 3.5 after 50 washes.
[0066] The formaldehyde content measured according to GB / T18401 is 0.
[0067] According to the test of GB / T3923.1, the tear strength retention rate is 82.11%.
[0068] The wrinkle recovery angle (warp + weft) of the fabric tested according to GB / T319-1997 is 313 degrees.
[0069] The whiteness of the fabric was tested according to GB / T8424.2-2001, and the whiteness retention rate was 94.2%.
[0070] The fabric’s color fastness to dry rubbing tested in accordance with GB / T3920-2008 is ≥5.0, and its color fastness to wet rubbing is ≥5.0.
[0071] The light fastness of the fabric tested in accordance with GB / T8427-2019 is ≥3.5.
[0072] The color fastness to washing of fabrics tested in accordance with GB / T3921.1-2008 is ≥5.0.
[0073] Example 2
[0074] The preparation method of the anti-wrinkle crosslinking agent is the same as that of Example 1, except that:
[0075] The anti-wrinkle processing technology of permanent-iron dyed silk fabrics has the following specific steps:
[0076] (1) 500 ml of the anti-wrinkle crosslinking agent was dissolved in 500 ml of non-aqueous solvent ethanol to prepare a working solution with an effective content of 5% of the sucralose-based anti-wrinkle crosslinking agent, and zinc chloride was added as a catalyst in an amount of 5%;
[0077] (2) Immerse the silk fabric to be dyed without ironing in the working solution for 15 minutes, centrifuge and dehydrate for 10 seconds, control the amount of liquid on the fabric to be 70%, pre-bake at 110°C for 15 seconds, bake at 150°C for 180 seconds, wash the baked silk fabric 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 dry to obtain wrinkle-resistant silk fabric.
[0078] The performance test of the wrinkle-resistant silk fabric prepared in Example 2 was carried out, and the test results are as follows:
[0079] The appearance grade measured according to GB / T18863-2002 is greater than or equal to 3.8 before washing, and greater than or equal to 3.5 after 50 washes.
[0080] The formaldehyde content measured according to GB / T18401 is 0.
[0081] According to the test of GB / T3923.1, the tear strength retention rate is 91.5%.
[0082] The wrinkle recovery angle (warp + weft) of the fabric tested according to GB / T319-1997 is 302 degrees.
[0083] 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.
[0084] The light fastness of the fabric tested in accordance with GB / T8427-2019 is ≥3.0.
[0085] The color fastness to washing of fabrics tested in accordance with GB / T3921.1-2008 is ≥4.0.
[0086] Example 3
[0087] A method for processing a non-ironing pure cotton white twill fabric, comprising the following steps:
[0088] Cross-linker preparation: 500 ml of a diglycosylated cross-linker stock solution was prepared according to the method of Example 1, except that 82 g of sodium periodate was used. After preparation, the aldehyde content of the cross-linker was measured to be 10.15 mmol / g, and the yield of the desired product was calculated to be 99.6%.
[0089] Magnesium chloride was added as a catalyst in an amount of 3 wt %, and a weakly polar organic solvent, n-propanol, was added so that the effective content of the dibasic sugar-based cross-linking agent was 8%;
[0090] The white cotton fabric to be wrinkle-free was immersed in the working solution for 20 minutes, centrifuged and dehydrated for 20 seconds, the liquid content of the fabric was controlled to 70%, pre-baked at 110°C for 20 seconds, and baked at 150°C for 180 seconds. The baked 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 wrinkle-resistant cotton fabric.
[0091] The performance test of the wrinkle-resistant pure cotton fabric prepared in Example 3 was carried out, and the test results are as follows:
[0092] The appearance grade measured in accordance with GB / T18863-2002 is greater than or equal to 4.0 before washing, and greater than or equal to 3.5 after 50 washes.
[0093] The formaldehyde content was not detected according to GB / T18401.
[0094] According to the test of GB / T3923.1, the tear strength retention rate is 85.23%.
[0095] The wrinkle recovery angle (warp + weft) of the fabric tested according to GB / T319-1997 is 301 degrees.
[0096] The whiteness of the fabric was tested according to GB / T8424.2-2001, and the whiteness retention rate was 83%.
[0097] The fabric’s color fastness to dry rubbing is tested in accordance with GB / T3920-2008 and its color fastness to wet rubbing is ≥5.
[0098] The light fastness of the fabric tested in accordance with GB / T8427-2019 is ≥4.0.
[0099] The color fastness to washing of fabrics tested in accordance with GB / T3921.1-2008 is ≥5.
[0100] Example 4
[0101] A method for processing a non-ironing pure cotton solid color twill fabric, comprising the following steps:
[0102] Cross-linker preparation: 500 ml of a diglycosylated cross-linker stock solution was prepared according to the method of Example 1, except that 86.1 g of sodium periodate was used. After preparation, the aldehyde content of the cross-linker was measured to be 10.16 mmol / g, and the yield of the desired product was calculated to be 99.7%.
[0103] Zinc chloride was added as a catalyst in an amount of 3 wt %; isopropyl alcohol, a weakly polar organic solvent, was added so that the effective content of the dibasic sugar-based cross-linking agent was 8%;
[0104] The wrinkle-resistant pure cotton solid color fabric was immersed in the working solution for 15 minutes, centrifuged and dehydrated for 30 seconds, the liquid content of the fabric was controlled to 70%, pre-baked at 110°C for 30 seconds, and baked at 150°C for 200 seconds. The baked pure 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 wrinkle-resistant pure cotton solid color fabric.
[0105] The performance test of the wrinkle-resistant pure cotton fabric prepared in Example 4 was carried out, and the test results are as follows:
[0106] The appearance grade measured in accordance with GB / T18863-2002 is greater than or equal to 4.0 before washing, and greater than or equal to 3.5 after 50 washes.
[0107] The formaldehyde content was not detected according to GB / T18401.
[0108] The tear strength retention rate tested according to GB / T3923.1 is 81.0%.
[0109] The wrinkle recovery angle (warp + weft) of the fabric tested according to GB / T319-1997 is 309 degrees.
[0110] The whiteness of the fabric was tested according to GB / T8424.2-2001, and the whiteness retention rate was 82%.
[0111] 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.
[0112] Test the fabric's light fastness in accordance with GB / T8427-2019 to ensure it is ≥3.
[0113] The color fastness to washing of fabrics tested in accordance with GB / T3921.1-2008 is ≥4.0.
[0114] Example 5
[0115] A method for processing a non-ironing pure cotton plain weave fabric comprises the following steps:
[0116] The preparation method of the anti-wrinkle crosslinking agent and the application method of the crosslinking agent are the same as those in Example 4, the main difference being that the liquid carrying amount is 55%.
[0117] The performance test of the wrinkle-resistant pure cotton fabric prepared in Example 5 was carried out, and the test results are as follows:
[0118] The appearance grade measured in accordance with GB / T18863-2002 is greater than or equal to 4.0 before washing, and greater than or equal to 3.5 after 50 washes.
[0119] The formaldehyde content was not detected according to GB / T18401.
[0120] According to the test of GB / T3923.1, the tear strength retention rate is 80.3%.
[0121] The wrinkle recovery angle (warp + weft) of the fabric tested according to GB / T319-1997 is 302 degrees.
[0122] The whiteness of the fabric was tested according to GB / T8424.2-2001, and the whiteness retention rate was 81%.
[0123] The fabric’s color fastness to dry rubbing is tested in accordance with GB / T3920-2008 and its color fastness to wet rubbing is ≥4.0 and ≥4.
[0124] The light fastness of the fabric tested in accordance with GB / T8427-2019 is ≥4.
[0125] The color fastness to washing of fabrics tested in accordance with GB / T3921.1-2008 is ≥4.0.
[0126] Comparative Example 1
[0127] Sucrose and sodium periodate were dissolved in distilled water to prepare a reaction solution with a sucrose mass fraction of 5% and a molar ratio of sodium periodate to sucrose of 3:1. The reaction solution was reacted at 20°C for 26 hours, and then barium sulfate was added at a molar ratio of 1:2 to sodium periodate. After stirring for 1 hour, the solution was filtered to obtain a clear solution which was the sucrose aldehyde crosslinker.
[0128] After titration testing, the residual rate of sodium iodate was 13.2%, and the aldehyde content in the sucrose aldehyde crosslinker was 6.7 mmol / g, indicating that part of the sucrose was not oxidized or the oxidized sucrose formed intramolecular hemiacetal, resulting in a low aldehyde content in the crosslinker.
[0129] 10 ml of the sucrose aldehyde cross-linking agent was taken and dried under reduced pressure at -60°C and a pressure of 4 Pa for 3 hours to obtain anhydrous powder.
[0130] 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 2 As shown by Figure 2 The provided carbon NMR spectrum shows that there is only one aldehyde peak at 163 ppm. This is because under the catalysis of formic acid, sucrose aldehyde forms an intramolecular hemiacetal in aqueous solution.
[0131] The anti-wrinkle processing technology of cotton fabrics includes the following specific steps:
[0132] (1) The above-mentioned sucrose aldehyde crosslinking agent is mixed with magnesium chloride, JFC penetrant and polyethylene softener to obtain a mixed solution, wherein the concentration of magnesium chloride is 20g / L, JFC is 2g / L, polyethylene softener is 2g / L, and the pH of the mixed solution is 3.
[0133] (2) Immerse the cotton fabric in the mixed solution, perform double dipping and double rolling, control the liquid carrying rate of the cotton fabric to be 90%, pre-dry at 80°C for 10 minutes, bake at 120°C for 1 minute, and then wash and dry.
[0134] The performance of the anti-wrinkle treated cotton fabric of Comparative Example 1 was tested, and the test results are as follows:
[0135] The strength retention rate of torn cotton fabric tested according to GB / T3923.1 is 86.3%.
[0136] The wrinkle recovery angle (warp + weft) of the fabric tested according to GB / T319-1997 is 205 degrees.
[0137] The whiteness of the fabric was tested according to GB / T8424.2-2001, and the whiteness retention rate was 92.1%.
[0138] Since sucrose aldehyde forms hemiacetal in the molecule, the number of reactive groups on the cross-linking agent is reduced, thereby reducing the anti-wrinkle effect.
[0139] Comparative Example 2
[0140] The preparation method of the sucrose aldehyde crosslinking agent is the same as that of Comparative Example 1, except that:
[0141] The anti-wrinkle processing technology of silk fabrics includes the following specific steps:
[0142] (1) The above-mentioned sucrose aldehyde crosslinking agent is mixed with magnesium chloride, JFC penetrant and polyethylene softener to obtain a mixed solution, wherein the concentration of magnesium chloride is 20g / L, JFC is 2g / L, polyethylene softener is 2g / L, and the pH of the mixed solution is 3.
[0143] (2) Immerse the cotton fabric in the mixed solution, perform double dipping and double rolling, control the liquid carrying rate of the cotton fabric to be 90%, pre-dry at 80°C for 10 minutes, bake at 150°C for 5 minutes, and then wash and dry.
[0144] The performance of the silk fabric treated with anti-wrinkle treatment in Comparative Example 2 was tested, and the test results were as follows:
[0145] According to GB / T3923.1 test, the strength retention rate of torn silk fabric is 76.3%.
[0146] The wrinkle recovery angle (warp + weft) of the fabric tested according to GB / T319-1997 is 235 degrees.
[0147] The whiteness of the fabric was tested according to GB / T8424.2-2001, and the whiteness retention rate was 82.1%.
[0148] Since sucrose aldehyde forms hemiacetal in the molecule, the number of reactive groups on the cross-linking agent is reduced, thereby reducing the anti-wrinkle effect.
[0149] Comparative Example 3
[0150] 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.
[0151] Comparative Example 4
[0152] 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.
[0153] Comparative Example 5
[0154] 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.
[0155] Comparative Example 6
[0156] 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.
[0157] Comparative Example 7
[0158] 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.
[0159] The method of applying the anti-wrinkle crosslinking agent is the same as that of Example 1. The properties of the anti-wrinkle silk fabric prepared in Comparative Example 7 are tested, and the test results are as follows:
[0160] The appearance grade measured in accordance with GB / T18863-2002 is greater than or equal to 3.0 before washing, and greater than or equal to 2.5 after 50 washes.
[0161] The formaldehyde content was not detected according to GB / T18401.
[0162] According to the test of GB / T3923.1, the tear strength retention rate is 89.1%.
[0163] The wrinkle recovery angle (warp + weft) of the fabric tested according to GB / T319-1997 is 246 degrees.
[0164] The whiteness of the fabric was tested according to GB / T8424.2-2001, and the whiteness retention rate was 92%.
[0165] The fabric’s color fastness to dry rubbing is tested in accordance with GB / T3920-2008 and its color fastness to wet rubbing is ≥4.0 and ≥4.
[0166] The light fastness of the fabric tested in accordance with GB / T8427-2019 is ≥4.
[0167] The color fastness to washing of fabrics tested in accordance with GB / T3921.1-2008 is ≥4.0.
[0168] 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 method for preparing an anti-wrinkle crosslinking agent based on sucralose, characterized in that: The following steps are involved: (1) dissolving sucralose in a non-aqueous solvent and stirring uniformly to obtain a sucralose solution; (2) Dissolve the oxidant in distilled water and stir evenly to obtain an oxidant aqueous solution; (3) adding the aqueous oxidant solution dropwise to the sucralose solution, reacting at a temperature of -5 to 25°C in the dark for 30 minutes to 24 hours to obtain a preparation solution; (4) The prepared liquid is placed in a -60°C to -20°C environment for freezing treatment for 1 to 12 hours, and filtered to obtain the anti-wrinkle crosslinking agent.
2. The method for preparing the anti-wrinkle crosslinking agent based on sucralose according to claim 1, characterized in that: The non-aqueous solvent in step (1) is a solvent that can form hydrogen bonds with water molecules.
3. The method for preparing the anti-wrinkle crosslinking agent based on sucralose according to claim 1, characterized in that: The oxidant in step (2) is periodate.
4. The method for preparing the anti-wrinkle crosslinking agent based on sucralose according to claim 1, characterized in that: The molar ratio of the oxidant to sucralose is 2.5-3.5:
1.
5. The method for preparing the anti-wrinkle crosslinking agent based on sucralose according to claim 1, characterized in that: Inert gas is introduced during the reaction process of step (3).
6. The method for preparing the anti-wrinkle crosslinking agent based on sucralose according to claim 1, characterized in that: The effective content of the diglycosyl crosslinking agent in the anti-wrinkle crosslinking agent in step (4) is 5% to 15%.
7. An anti-wrinkle crosslinking agent, characterized in that Prepared by the method according to any one of claims 1 to 6.
8. Use of the anti-wrinkle crosslinking agent prepared by the method according to any one of claims 1 to 6 or the anti-wrinkle crosslinking agent according to claim 7 in anti-wrinkle finishing of fabrics, characterized in that: The following steps are involved: (1) dissolving the anti-wrinkle crosslinking agent in a non-aqueous solvent, adding a catalyst, and preparing a working solution containing 5% to 8% of the anti-wrinkle crosslinking agent; (2) Immerse the fabric in the working solution for 10 to 30 minutes, centrifuge and dehydrate for 10 to 30 seconds, control the amount of liquid on the fabric to be 50% to 80%, pre-dry, bake, remove impurities, wash, and dry to obtain the wrinkle-resistant fabric.
9. The application according to claim 8, characterized in that: The catalyst in step (1) 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.
10. The use according to claim 8, characterized in that: The pre-baking temperature in step (2) is 110-130°C, and the pre-baking time is 10-30s. The baking temperature is 150-180°C, and the baking time is 60s-300s. The impurity removal and washing step comprises: placing the baked fabric at 40-60°C, washing with water for 5-20min, controlling the bath ratio to be 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.