A dyeing process for preventing fibrillation of lyocell woven fabric

By combining enzyme cold pad-batch desizing and bleaching with a one-bath two-step dyeing process, along with anti-fibrillation treatment, the problem of fibrillation caused by mechanical external forces in wet Lyocell fabrics has been solved. This achieves efficient prevention of fibrillation and improved dye utilization, making it suitable for continuous production of Lyocell fabrics.

CN119352317BActive Publication Date: 2025-10-21BEIJING CTA TEX CHEM
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Patent Information

Application Number
CN202411643112.9
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-11-18
Publication Date
2025-10-21
Estimated Expiration
2044-11-18

AI Technical Summary

Technical Problem

Lyocell woven fabrics are susceptible to fibrillation under mechanical force or friction when wet, leading to quality problems such as abrasions and white frost. Existing technologies are unable to effectively prevent this phenomenon in continuous production.

Method used

The greige fabric is treated with a one-step enzymatic cold pad-batch desizing and bleaching process, combined with a one-bath two-step roll dyeing process. After dyeing, it is treated with antifibrillation. A stable suspension of antifibrillation crosslinking agent, leveling agent and dispersant is used to reduce friction between the fabric and the equipment, improve dye utilization, and avoid uneven dyeing and color difference.

Benefits of technology

It effectively prevents fibrillation of Lyocell fabrics in continuous production, reduces abrasion and white bloom, improves dye uptake, reduces energy consumption, and is suitable for industrial applications.

✦ Generated by Eureka AI based on patent content.

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Abstract

The application discloses a dyeing process for preventing fibrillation of lyocell woven fabric. The process comprises the following steps: singeing, desizing and bleaching of lyocell grey cloth; preparation of a dyeing working solution, including dyes, anti-wrinkle agent, anhydrous sodium sulfate and soda ash, mixing the working solution uniformly, and carrying out first-step pad dyeing on the pretreated lyocell fabric; preparation of an anti-fibrillation working solution, including anti-fibrillation crosslinking agent, leveling agent and dispersing agent, high-speed stirring of the solution to prepare a stable suspension, and adding the dyeing working solution into the suspension; after heating, second-step pad dyeing is started; and washing, soaping, softening and drying of the treated lyocell woven fabric. The pad dyeing process is suitable for continuous long-drum production of lyocell woven fabric and its blended fabric, and through one-bath two-step dyeing process, the effect of preventing fibrillation can be achieved, the utilization rate of dyes is improved, the risk of light dyeing and color deviation of lyocell woven fabric is avoided, and the process has great application prospect.
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Description

Technical Field

[0001] The invention belongs to the technical field of textile production and processing, and particularly relates to a jig dyeing process for preventing lyocell woven fabrics from fibrillating. Background Art

[0002] Lyocell woven fabrics offer advantages such as high strength, a rich feel, good drape, excellent moisture absorption, vibrant colors, and excellent wrinkle resistance. They can be blended, composited, or interwoven with other fibers to create fabrics with a smooth, finished finish. However, Lyocell fibers exhibit a unique fibrillation property. When wet, fiber swelling and mechanical forces cause the original individual fibers to split axially, splitting into tiny fibrils. This can lead to problems such as pale color, "frost," white lines, and scratches on the fabric. Lyocell woven fabrics are typically dyed using an open-width continuous process. Under conditions of damp heat, alkalinity, and mechanical friction, the lateral swelling of the fibers makes the rigid fabric more susceptible to fibrillation, resulting in serious fabric quality issues.

[0003] Currently, the main approaches to addressing the fibrillation problem of Lyocell woven fabrics are through cold pad-batch dyeing, pad-dye steaming, or pad-dye baking processes. Patent CN 115772811A utilizes a cold pad-batch dyeing process to produce a fibrillation-resistant Lyocell fabric. However, this process is relatively cumbersome and requires repeated baking of the fabric, which consumes a lot of energy. Furthermore, the low temperature of the cold pad-batch process can easily lead to incomplete crosslinking agent reaction. Patent CN 117364512A discloses an anti-fibrillation treatment process for dyed Lyocell fabrics. This process is not intended for finishing from grey fabrics but is only suitable for repairing colored fabrics. Furthermore, the anti-fibrillation treatment process in this process is a static impregnation process, unsuitable for the continuous production requirements of large-scale production.

[0004] At present, the fibrillation problem of Lyocell woven fabrics in the dyeing and finishing process causes abrasions and white frost on the fabric. This is an industry problem that urgently needs to be solved. It is also a difficulty in improving the quality of Lyocell woven fabrics. Therefore, it is urgent to develop a Lyocell fabric anti-fibrillation jig dyeing process that is suitable for continuous production, does not add additional steps, and is simple to operate. Summary of the Invention

[0005] The present invention addresses the drawback of Lyocell fabrics, which are susceptible to fibrillation when exposed to mechanical forces or friction in a wet state. The present invention provides a jig-dyeing process for preventing fibrillation of Lyocell woven fabrics. This method reduces scratches on Lyocell fabrics during dyeing and finishing, making it suitable for continuous production. It not only does not affect dye application but also produces Lyocell fabrics with excellent anti-fibrillation properties, without incurring additional equipment costs, and is energy-efficient and environmentally friendly.

[0006] The jig dyeing process for preventing fibrillation of lyocell woven fabrics provided by the present invention comprises the following steps:

[0007] (1) Singeing, desizing and bleaching the Lyocell fabric;

[0008] (2) preparing a dyeing working solution, wherein the dyeing working solution includes a dye, an anti-wrinkle agent, sodium sulfate and soda ash, and mixing the dyeing working solution evenly. After the working solution is heated to a certain temperature, performing the first step of roller dyeing on the lyocell fabric treated in step (1);

[0009] (3) preparing an anti-fibrillation working solution, wherein the anti-fibrillation working solution comprises an anti-fibrillation cross-linking agent, a leveling agent and a dispersant, stirring the anti-fibrillation working solution at a high speed to obtain a stable suspension, adding the dyeing working solution of step (2) to carry out the second step of roller dyeing;

[0010] (4) Wash, soap, soften and dry the treated lyocell fabric.

[0011] In step (1) of the above method, the singeing is to remove the fuzz from the cloth surface by through-singing, and the process conditions are two positive and two negative, a speed of 100 m / min, and a temperature of 1000-1100°C;

[0012] The desizing and bleaching process in step (1) adopts a cold pad-batch desizing and bleaching one-step process: amylase, penetrant, alkali, hydrogen peroxide, refining agent, oxygen bleaching stabilizer, and dispersing chelating agent are added to water and mixed to obtain a treatment bath, and the grey cloth is padded with the treatment bath, rolled up, and then wrapped, sealed, and stacked at room temperature.

[0013] Among them, the dosage of amylase is 5-10g / L (amylase activity 4000U / ml), penetrant 1-5g / L, alkali (NaOH) dosage 6-10g / L, hydrogen peroxide 4-5g / L, refining agent 5-6g / L, oxygen bleaching stabilizer 4-5g / L, dispersing chelating agent 1-2g / L, cold stacking condition is room temperature stacking, and stacking time is 16-20h.

[0014] In step (2), the dye is one or more of s-triazine type reactive dyes, vinyl sulfone type reactive dyes, and halogenated pyrimidine type reactive dyes;

[0015] The anti-wrinkle agent is one or more of urea-formaldehyde resin, dimethylolethylene urea resin, dimethylol dihydroxyethylene urea resin, high polymer chitosan, waterborne polyurethane resin, epoxy compound, citric acid, and polymaleic acid;

[0016] The dyeing working solution is prepared by adding dye, anti-wrinkle agent, sodium sulfate and soda ash into water and mixing them evenly, wherein the amount of dye is 5-20g / L; the amount of anti-wrinkle agent is 1-2g / L; the amount of sodium sulfate is 40-60g / L; and the amount of soda ash is 15-20g / L;

[0017] In step (2), the first step of the jig dyeing process is to gradually add the dyeing working solution in four times, adding 1 / 4 of the dye solution each time, the dyeing temperature is 60-80°C, and the dyeing time is 15-20 minutes.

[0018] In step (3), the anti-fibrillation cross-linking agent is one or more of a dichlorotriazine compound, a dibromotriazine compound, and 1,3,5-triacryloylhexahydro-1,3,5-triazine, and the amount used is 30-80 g / L;

[0019] The leveling agent is one or more of fatty alkyl sulfate, alkylbenzene sulfonate, polyethylene glycol alkyl ether sulfate, naphthalenesulfonic acid-formaldehyde condensate, polyethylene glycol ether of fatty amine, polyethylene polyamine, and oxyethylated nitrogen-containing fatty alkyl compound, and the amount used is 1-5 g / L;

[0020] The dispersant is one or more of alkylphenol polyoxyethylene ether, fatty amine polyoxyethylene ether, fatty alcohol polyoxyethylene ether, fatty alcohol polyoxyethylene ether sodium sulfate, fatty alcohol polyoxyethylene ether sodium carboxylate, and isomeric alcohol polyoxyethylene ether, and the dosage is 3-5 g / L;

[0021] In step (3), the process for preparing the anti-fibrillation working solution is to add the anti-fibrillation crosslinking agent, the leveling agent, and the dispersant into water according to the added amount, mix them evenly, and stir them in a high-speed stirrer for 1-2 hours to obtain a stable suspension, wherein the stirrer speed is 2000-5000 r / min;

[0022] In step (3), the second step of roller dyeing process conditions are dyeing temperature 60-80°C and dyeing time 45-60min.

[0023] In step (4), the soaping agent is a mixture of aralkyl polyglycol ester and fatty acid amine, the soaping temperature is 95-100°C, the soaping time is 20-30 minutes, the drying temperature is 110-120°C, and the drying time is 1-2 minutes.

[0024] The jig dyeing process is suitable for lyocell woven fabrics and lyocell blended fabrics with other fabrics.

[0025] The lyocell woven fabric produced by the above process and its blended fabric with other fabrics also fall within the protection scope of the present invention.

[0026] Compared with the prior art, the present invention has the following beneficial effects:

[0027] (1) The present invention uses an enzyme cold pad-batch desizing and bleaching one-step process to treat Lyocell woven fabric, which shortens the pre-treatment process flow, reduces the friction time between the fabric and the equipment, and reduces the risk of fibrillation.

[0028] (2) The present invention adopts a one-bath two-step roller dyeing process to carry out an anti-fibrillation treatment on lyocell woven fabrics, which does not increase the investment in additional equipment, is simple in process and easy to operate; in addition, the one-bath two-step roller dyeing process separates the time before and after the dyeing working solution and the anti-fibrillation working solution act on the woven fabric, allowing a part of the dye to be stage-dyed first and then subjected to the anti-fibrillation treatment, which can improve the utilization rate of the dye, ensure the dye uptake rate, reduce the competitive dyeing effect between the cross-linking agent and the dye, and thus avoid the risk of light dyeing of the fabric.

[0029] (3) The present invention prepares a dyeing working solution and adds an anti-wrinkle agent to the dyeing working solution, thereby preventing the lyocell woven fabric from becoming hard after contact with water and becoming prone to fibrillation due to friction between equipment; at the same time, when preparing the anti-fibrillation working solution, a leveling agent and a dispersant are added, and high-speed dispersion is performed to obtain a uniform suspension, thereby ensuring the stability of the entire dyeing and finishing liquid, and avoiding the dyeing phenomenon and color difference of the front and back of the fabric that occur in the production of lyocell woven fabrics in long-roll dyeing machines.

[0030] (4) The jig dyeing process of the present invention is suitable for the continuous production of anti-fibrillation of lyocell fabrics in factories. The treated fabrics have good anti-fibrillation effect and good washability. No fibrillation occurs after washing 10 times. At the same time, no formaldehyde is released during the finishing process, which avoids harm to the human body and the environment. The process has great application prospects. BRIEF DESCRIPTION OF THE DRAWINGS

[0031] Figure 1 The surface of the lyocell fabric of Example 1 after washing 10 times (microscope magnification 1600 times).

[0032] Figure 2 The surface of the lyocell fabric of Comparative Example 1 after washing 10 times (microscope magnification 1600 times).

[0033] Figure 3 The surface of the Lyocell fabric of Comparative Example 2 after washing 10 times (microscope magnification 1600 times).

[0034] Figure 4 This is a comparison of the white frost on the surface of the lyocell fabric prepared in Example 1 before and after washing, a is before washing, and b is after washing.

[0035] Figure 5 This is a comparison of the white frost on the surface of the lyocell fabric prepared in Example 2 before and after washing, a is before washing, and b is after washing.

[0036] Figure 6This is a comparison of the white frost on the surface of the lyocell fabric prepared in Example 3 before and after washing, a is before washing, and b is after washing.

[0037] Figure 7 This is a comparison of the white frost on the surface of the lyocell fabric prepared in Example 4 before and after washing, a is before washing, and b is after washing.

[0038] Figure 8 This is a comparison of the white frost on the surface of the lyocell fabric prepared in Example 5 before and after washing, a is before washing, and b is after washing.

[0039] Figure 9 This is a comparison of the white frost on the surface of the lyocell fabric prepared in Comparative Example 1 before and after washing, a is before washing, and b is after washing.

[0040] Figure 10 This is a comparison of the white frost on the surface of the Lyocell fabric prepared in Comparative Example 2 before and after washing, a is before washing, and b is after washing. DETAILED DESCRIPTION

[0041] The present invention will be further described in detail below in conjunction with specific embodiments. The examples provided are only for illustrating the present invention and are not intended to limit the scope of the present invention. The examples provided below can serve as a guide for further improvements by those skilled in the art and are not intended to limit the present invention in any way.

[0042] Unless otherwise specified, the experimental methods in the following examples are conventional methods and were performed according to the techniques or conditions described in the literature in the field or according to the product instructions. The materials and reagents used in the following examples, unless otherwise specified, were all commercially available.

[0043] In the desizing and bleaching processes in the following examples and comparative examples, the amylase used was amylase 2D-BG purchased from Novozymes, the penetrant was FK-ST20, the refining agent was FK-ST1218H, the oxygen bleaching stabilizer was FK-601, and the dispersing chelating agent was FK-422 purchased from Beijing Zhongfang Chemical Co., Ltd.

[0044] The anti-wrinkle agents were purchased from Zibo Lurui Fine Chemical Company, including AC-L and LUK.

[0045] The anti-fibrillation crosslinking agents were purchased from Beijing Zhongfang Chemical Co., Ltd., products CB-3 and CB-4, and from Nantong Jiangtian Chemical Co., Ltd., product 1,3,5-triacryloylhexahydro-1,3,5-triazine (TAHT).

[0046] The leveling agent was FK-482 purchased from Beijing Zhongfang Chemical Co., Ltd. and LA-RK purchased from Zibo Lurui Fine Chemical Co., Ltd.

[0047] The dispersants were purchased from Hangzhou Kecheng Chemical Co., Ltd., including JFC-4 and AH-30.

[0048] The soaping agent was FK-9500 purchased from Beijing Zhongfang Chemical Co., Ltd.

[0049] Example 1

[0050] The jig-dyeing process to prevent fibrillation of lyocell woven fabrics includes the following steps:

[0051] (1) Singeing the lyocell grey fabric, which is a through-burning method to remove the fluff on the fabric, is carried out under the following process conditions: two positive and two negative, a speed of 100 m / min, and a temperature of 1000°C; the desizing and bleaching process adopts a cold pad-batch desizing and bleaching one-step process: amylase, penetrant, alkali, hydrogen peroxide, refining agent, oxygen bleaching stabilizer, and dispersing chelating agent are added to water and mixed to obtain a treatment bath, and the grey fabric is padded with the treatment bath, rolled up, and then wrapped, sealed, and stacked at room temperature;

[0052] Among them, the dosage of amylase 2D-BG is 5g / L (4000U / ml), the dosage of penetrant FK-ST20 is 2g / L, the dosage of NaOH is 10g / L, the dosage of hydrogen peroxide is 5g / L, the dosage of refining agent FK-ST1218H is 5g / L, the dosage of oxygen bleaching stabilizer FK-601 is 5g / L, the dosage of dispersing chelating agent FK-422 is 2g / L, the cold stacking condition is room temperature stacking, and the stacking time is 20h.

[0053] (2) preparing a dyeing working solution comprising a dye, an anti-wrinkle agent, sodium sulfate and soda ash, mixing the working solution uniformly, and subjecting the lyocell fabric treated in step (1) to the first step of jig dyeing; the dye is triazine type reactive dye black B, the amount of which is 5 g / L, the amount of sodium sulfate is 60 g / L, and the amount of soda ash is 15 g / L; the anti-wrinkle agent is AC-L, the amount of which is 2 g / L;

[0054] The dyeing working solution was added gradually in four times, with 1 / 4 of the dyeing working solution added each time. The dyeing temperature was 60°C and the dyeing time was 15 minutes (the first step of roller dyeing was 15 minutes).

[0055] (3) Prepare an anti-fibrillation working solution, wherein the anti-fibrillation crosslinking agent is CB-3, the dosage is 40g / L; the leveling agent is FK-482, the dosage is 2g / L; the dispersant is JFC-4, the dosage is 3g / L, the anti-fibrillation crosslinking agent, the leveling agent and the dispersant are mixed evenly according to the added amount, stirred in a high-speed stirrer for 1h, the stirrer speed is 2000r / min, to prepare a stable suspension, add the dyeing working solution of step (2), and start the second step of roller dyeing; the process conditions of the second step of roller dyeing are dyeing temperature 60℃ and dyeing time 60min.

[0056] (4) The treated lyocell fabric was washed, soaped, softened, and dried. The soaping agent was FK-9500, the soaping temperature was 95°C, the soaping time was 30 minutes, the drying temperature was 110°C, and the drying time was 1 minute.

[0057] Example 2

[0058] The jig-dyeing process to prevent fibrillation of lyocell woven fabrics includes the following steps:

[0059] (1) Singeing the lyocell grey fabric, which is a through-burning method to remove the fluff on the fabric, is carried out under the following process conditions: two positive and two negative, a speed of 100 m / min, and a temperature of 1000°C; the desizing and bleaching process adopts a cold pad-batch desizing and bleaching one-step process: amylase, penetrant, alkali, hydrogen peroxide, refining agent, oxygen bleaching stabilizer, and dispersing chelating agent are added to water and mixed to obtain a treatment bath, and the grey fabric is padded with the treatment bath, rolled up, and then wrapped, sealed, and stacked at room temperature;

[0060] Among them, the dosage of amylase 2D-BG is 5g / L (4000U / ml), the dosage of penetrant FK-ST20 is 2g / L, the dosage of NaOH is 10g / L, the dosage of hydrogen peroxide is 5g / L, the dosage of refining agent FK-ST1218H is 5g / L, the dosage of oxygen bleaching stabilizer FK-601 is 5g / L, the dosage of dispersing chelating agent FK-422 is 2g / L, the cold stacking condition is room temperature stacking, and the stacking time is 20h.

[0061] (2) preparing a dyeing working solution comprising a dye, an anti-wrinkle agent, sodium sulfate and soda ash, mixing the working solution uniformly, and performing the first step of roller dyeing on the lyocell fabric treated in step (1); the dye is a triazine type reactive dye black B, the amount of which is 5 g / L, the amount of sodium sulfate is 60 g / L, and the amount of soda ash is 15 g / L; the anti-wrinkle agent is LUK, the amount of which is 2 g / L;

[0062] The dyeing working solution was gradually added in four times, with 1 / 4 of the dyeing working solution added each time. The dyeing temperature was 60°C and the dyeing time was 15 minutes.

[0063] (3) Prepare an anti-fibrillation working solution, wherein the anti-fibrillation crosslinking agent is CB-4, the dosage is 40g / L; the leveling agent is LA-RK, the dosage is 2g / L; the dispersant is AH-30, the dosage is 3g / L, the anti-fibrillation crosslinking agent, the leveling agent and the dispersant are mixed evenly according to the added amount, stirred in a high-speed stirrer for 1h, the stirrer speed is 2000r / min, to prepare a stable suspension, add the dyeing working solution of step (2), and start the second step of roller dyeing; the process conditions of the second step of roller dyeing are dyeing temperature 60℃ and dyeing time 60min.

[0064] (4) The treated lyocell fabric was washed, soaped, softened, and dried. The soaping agent was FK-9500, the soaping temperature was 95°C, the soaping time was 30 minutes, the drying temperature was 110°C, and the drying time was 1 minute.

[0065] Example 3

[0066] The jig-dyeing process to prevent fibrillation of lyocell woven fabrics includes the following steps:

[0067] (1) Singeing the lyocell grey fabric, which is a through-burning method to remove the fluff on the fabric, is carried out under the following process conditions: two positive and two negative, a speed of 100 m / min, and a temperature of 1000°C; the desizing and bleaching process adopts a cold pad-batch desizing and bleaching one-step process: amylase, penetrant, alkali, hydrogen peroxide, refining agent, oxygen bleaching stabilizer, and dispersing chelating agent are added to water and mixed to obtain a treatment bath, and the grey fabric is padded with the treatment bath, rolled up, and then wrapped, sealed, and stacked at room temperature;

[0068] Among them, the dosage of amylase 2D-BG is 5g / L (4000U / ml), the dosage of penetrant FK-ST20 is 2g / L, the dosage of NaOH is 10g / L, the dosage of hydrogen peroxide is 5g / L, the dosage of refining agent FK-ST1218H is 5g / L, the dosage of oxygen bleaching stabilizer FK-601 is 5g / L, the dosage of dispersing chelating agent FK-422 is 2g / L, the cold stacking condition is room temperature stacking, and the stacking time is 20h.

[0069] (2) preparing a dyeing working solution comprising a dye, an anti-wrinkle agent, sodium sulfate and soda ash, mixing the working solution uniformly, and performing the first step of roller dyeing on the lyocell fabric treated in step (1); the dye is a triazine type reactive dye black B, the amount of which is 5 g / L, the amount of sodium sulfate is 60 g / L, and the amount of soda ash is 15 g / L; the anti-wrinkle agent is LUK, the amount of which is 2 g / L;

[0070] The dyeing working solution was gradually added in four times, with 1 / 4 of the dyeing working solution added each time. The dyeing temperature was 60°C and the dyeing time was 15 minutes.

[0071] (3) Prepare an anti-fibrillation working solution, wherein the anti-fibrillation crosslinking agent is TAHT, the dosage is 40g / L; the leveling agent is LA-RK, the dosage is 2g / L; the dispersant is AH-30, the dosage is 3g / L, the anti-fibrillation crosslinking agent, the leveling agent and the dispersant are mixed evenly according to the added amount, stirred in a high-speed stirrer for 1h, the stirrer speed is 2000r / min, to prepare a stable suspension, add the dyeing working solution of step (2), and start the second step of roller dyeing; the process conditions of the second step of roller dyeing are dyeing temperature 60℃ and dyeing time 60min.

[0072] (4) The treated lyocell fabric was washed, soaped, softened, and dried. The soaping agent was FK-9500, the soaping temperature was 95°C, the soaping time was 30 minutes, the drying temperature was 110°C, and the drying time was 1 minute.

[0073] Example 4

[0074] The jig-dyeing process to prevent fibrillation of lyocell woven fabrics includes the following steps:

[0075] (1) Singeing the lyocell grey fabric, which is a through-burning method to remove the fluff on the fabric, is carried out under the following process conditions: two positive and two negative, a speed of 100 m / min, and a temperature of 1000°C; the desizing and bleaching process adopts a cold pad-batch desizing and bleaching one-step process: amylase, penetrant, alkali, hydrogen peroxide, refining agent, oxygen bleaching stabilizer, and dispersing chelating agent are added to water and mixed to obtain a treatment bath, and the grey fabric is padded with the treatment bath, rolled up, and then wrapped, sealed, and stacked at room temperature;

[0076] Among them, the dosage of amylase 2D-BG is 5g / L (4000U / ml), the dosage of penetrant FK-ST20 is 2g / L, the dosage of NaOH is 10g / L, the dosage of hydrogen peroxide is 5g / L, the dosage of refining agent FK-ST1218H is 5g / L, the dosage of oxygen bleaching stabilizer FK-601 is 5g / L, the dosage of dispersing chelating agent FK-422 is 2g / L, the cold stacking condition is room temperature stacking, and the stacking time is 20h.

[0077] (2) preparing a dyeing working solution comprising a dye, an anti-wrinkle agent, sodium sulfate and soda ash, mixing the working solution uniformly, and performing the first step of roller dyeing on the lyocell fabric treated in step (1); the dye is a triazine type reactive dye black B, the amount of which is 5 g / L, the amount of sodium sulfate is 60 g / L, and the amount of soda ash is 15 g / L; the anti-wrinkle agent is LUK, the amount of which is 2 g / L;

[0078] The dyeing working solution was gradually added in four times, with 1 / 4 of the dyeing working solution added each time. The dyeing temperature was 60°C and the dyeing time was 15 minutes.

[0079] (3) Prepare an anti-fibrillation working solution, wherein the anti-fibrillation crosslinking agents are CB-3 and CB-4, with a dosage of 20 g / L respectively; the leveling agent is LA-RK, with a dosage of 2 g / L; and the dispersant is AH-30, with a dosage of 3 g / L. The anti-fibrillation crosslinking agent, leveling agent, and dispersant are mixed evenly according to the added amount, stirred in a high-speed stirrer for 1 hour at a stirrer speed of 2000 r / min to prepare a stable suspension, and the dyeing working solution of step (2) is added to start the second step of roller dyeing; the process conditions of the second step of roller dyeing are dyeing temperature of 60°C and dyeing time of 60 min.

[0080] (4) The treated lyocell fabric was washed, soaped, softened, and dried. The soaping agent was FK-9500, the soaping temperature was 95°C, the soaping time was 30 minutes, the drying temperature was 110°C, and the drying time was 1 minute.

[0081] Example 5

[0082] The jig-dyeing process to prevent fibrillation of lyocell woven fabrics includes the following steps:

[0083] (1) Singeing the lyocell grey fabric, which is a through-burning method to remove the fluff on the fabric, is carried out under the following process conditions: two positive and two negative, a speed of 100 m / min, and a temperature of 1000°C; the desizing and bleaching process adopts a cold pad-batch desizing and bleaching one-step process: amylase, penetrant, alkali, hydrogen peroxide, refining agent, oxygen bleaching stabilizer, and dispersing chelating agent are added to water and mixed to obtain a treatment bath, and the grey fabric is padded with the treatment bath, rolled up, and then wrapped, sealed, and stacked at room temperature;

[0084] Among them, the dosage of amylase 2D-BG is 5g / L (4000U / ml), the dosage of penetrant FK-ST20 is 2g / L, the dosage of NaOH is 10g / L, the dosage of hydrogen peroxide is 5g / L, the dosage of refining agent FK-ST1218H is 5g / L, the dosage of oxygen bleaching stabilizer FK-601 is 5g / L, the dosage of dispersing chelating agent FK-422 is 2g / L, the cold stacking condition is room temperature stacking, and the stacking time is 20h.

[0085] (2) preparing a dyeing working solution comprising a dye, an anti-wrinkle agent, sodium sulfate and soda ash, mixing the working solution uniformly, and performing the first step of roller dyeing on the lyocell fabric treated in step (1); the dye is a triazine type reactive dye black B, the amount of which is 5 g / L, the amount of sodium sulfate is 60 g / L, and the amount of soda ash is 15 g / L; the anti-wrinkle agent is LUK, the amount of which is 2 g / L;

[0086] The dyeing working solution was gradually added in four times, with 1 / 4 of the dyeing working solution added each time. The dyeing temperature was 80°C and the dyeing time was 15 minutes.

[0087] (3) Prepare an anti-fibrillation working solution, wherein the anti-fibrillation crosslinking agent is CB-4, the dosage is 40g / L; the leveling agent is LA-RK, the dosage is 2g / L; the dispersant is AH-30, the dosage is 3g / L, the anti-fibrillation crosslinking agent, the leveling agent and the dispersant are mixed evenly according to the added amount, stirred in a high-speed stirrer for 1h, the stirrer speed is 2000r / min, to prepare a stable suspension, add the dyeing working solution of step (2), and start the second step of roller dyeing; the process conditions of the second roller dyeing are dyeing temperature 80℃ and dyeing time 60min.

[0088] (4) The treated lyocell fabric was washed, soaped, softened, and dried. The soaping agent was FK-9500, the soaping temperature was 95°C, the soaping time was 30 minutes, the drying temperature was 110°C, and the drying time was 1 minute.

[0089] Comparative Example 1 (without adding anti-fibrillation crosslinking agent)

[0090] The jig-dyeing process to prevent fibrillation of lyocell woven fabrics includes the following steps:

[0091] (1) Singeing the lyocell grey fabric, which is a through-burning method to remove the fluff on the fabric, is carried out under the following process conditions: two positive and two negative, a speed of 100 m / min, and a temperature of 1000°C; the desizing and bleaching process adopts a cold pad-batch desizing and bleaching one-step process: amylase, penetrant, alkali, hydrogen peroxide, refining agent, oxygen bleaching stabilizer, and dispersing chelating agent are added to water and mixed to obtain a treatment bath, and the grey fabric is padded with the treatment bath, rolled up, and then wrapped, sealed, and stacked at room temperature;

[0092] Among them, the dosage of amylase 2D-BG is 5g / L (4000U / ml), the dosage of penetrant FK-ST20 is 2g / L, the dosage of NaOH is 10g / L, the dosage of hydrogen peroxide is 5g / L, the dosage of refining agent FK-ST1218H is 5g / L, the dosage of oxygen bleaching stabilizer FK-601 is 5g / L, the dosage of dispersing chelating agent FK-422 is 2g / L, the cold stacking condition is room temperature stacking, and the stacking time is 20h. (2) Prepare a dyeing working solution, which includes dye, anti-wrinkle agent, sodium sulfate and soda ash, mix the above working solution evenly, and perform the first step of roller dyeing on the lyocell fabric treated in step (1); the dye is triazine type reactive dye black B, the dosage is 5g / L, the dosage of sodium sulfate is 60g / L, and the dosage of soda ash is 15g / L; the anti-wrinkle agent is AC-L, the dosage is 2g / L;

[0093] The dyeing working solution was gradually added in four times, with 1 / 4 of the dyeing working solution added each time. The dyeing temperature was 60°C and the dyeing time was 15 minutes.

[0094] (3) Prepare an anti-fibrillation working solution, wherein no anti-fibrillation crosslinking agent is added; the leveling agent is FK-482, the dosage is 2 g / L; the dispersant is JFC-4, the dosage is 3 g / L, the leveling agent and the dispersant are mixed evenly according to the added amount, stirred in a high-speed stirrer for 1 hour, the stirrer speed is 2000 r / min, to prepare a stable suspension, add the dyeing working solution of step (2), and start the second step of roller dyeing; the process conditions of the second step of roller dyeing are dyeing temperature 60°C and dyeing time 60 minutes.

[0095] (4) The treated lyocell fabric was washed, soaped, softened, and dried. The soaping agent was FK-9500, the soaping temperature was 95°C, the soaping time was 30 minutes, the drying temperature was 110°C, and the drying time was 1 minute.

[0096] Comparative Example 2 (cross-linking before dyeing)

[0097] The jig-dyeing process to prevent fibrillation of lyocell woven fabrics includes the following steps:

[0098] (1) Singeing the lyocell grey fabric, which is a through-burning method to remove the fluff on the fabric, is carried out under the following process conditions: two positive and two negative, a speed of 100 m / min, and a temperature of 1000°C; the desizing and bleaching process adopts a cold pad-batch desizing and bleaching one-step process: amylase, penetrant, alkali, hydrogen peroxide, refining agent, oxygen bleaching stabilizer, and dispersing chelating agent are added to water and mixed to obtain a treatment bath, and the grey fabric is padded with the treatment bath, rolled up, and then wrapped, sealed, and stacked at room temperature;

[0099] Among them, the dosage of amylase 2D-BG is 5g / L (4000U / ml), the dosage of penetrant FK-ST20 is 2g / L, the dosage of NaOH is 10g / L, the dosage of hydrogen peroxide is 5g / L, the dosage of refining agent FK-ST1218H is 5g / L, the dosage of oxygen bleaching stabilizer FK-601 is 5g / L, the dosage of dispersing chelating agent FK-422 is 2g / L, the cold stacking condition is room temperature stacking, and the stacking time is 20h.

[0100] (2) Prepare an anti-fibrillation working solution, wherein the anti-fibrillation crosslinker is CB-3, the dosage is 40 g / L; the leveling agent is FK-482, the dosage is 2 g / L; the dispersant is JFC-4, the dosage is 3 g / L, and the anti-fibrillation crosslinker, leveling agent, and dispersant are mixed evenly according to the added amount, stirred in a high-speed mixer for 1 hour at a mixer speed of 2000 r / min to prepare a stable suspension, and start the first step of roller dyeing; the process conditions for the first step of roller dyeing are dyeing temperature 60 ° C and dyeing time 15 min.

[0101] (3) preparing a dyeing working solution comprising a dye, an anti-wrinkle agent, sodium sulfate and soda ash, mixing the working solution uniformly, and performing a second step of roller dyeing on the lyocell fabric treated in step (2); the dye is triazine type reactive dye black B, the amount of which is 5 g / L, the amount of sodium sulfate is 60 g / L, and the amount of soda ash is 15 g / L; the anti-wrinkle agent is AC-L, the amount of which is 2 g / L;

[0102] The dyeing working solution was gradually added in four times, with 1 / 4 of the dyeing working solution added each time. The dyeing temperature was 60°C and the dyeing time was 60 minutes.

[0103] (4) The treated lyocell fabric was washed, soaped, softened, and dried. The soaping agent was FK-9500, the soaping temperature was 95°C, the soaping time was 30 minutes, the drying temperature was 110°C, and the drying time was 1 minute.

[0104] Anti-fibrillation performance test of lyocell fabric before and after treatment:

[0105] The present invention provides a method for determining the degree of fibrillation of lyocell fabrics. The method involves testing the lyocell fabric's pilling resistance and examining the surface frost after washing the fabric five times and ten times before and after treatment. The pilling resistance was tested according to GB / T 4802.1-1997, and the lyocell textiles were washed according to GB 12799-91. The results are shown in Table 1.

[0106] Table 1 Comparison of surface conditions of Lyocell fabric before and after washing

[0107]

[0108] As shown in Table 1, the anti-pilling grade of the lyocell fabrics (Examples 1-5) treated with the anti-fibrillation jig dyeing process is relatively good after washing 5 and 10 times. The anti-pilling grade of the comparative example 1 is reduced after washing 5 times, and the anti-pilling grade of the comparative example 1 is reduced after washing 5 times. Figure 4-10 It can be seen that the Lyocell fabric of Comparative Example 1 (without anti-fibrillation crosslinking agent) showed white frost on the surface after washing 5 times, and the white frost was serious after washing 10 times. The Lyocell fabric of Comparative Example 2 (crosslinked before dyeing) showed a phenomenon of light dyeing. The Lyocell fabrics treated by the jig dyeing process all showed excellent anti-fibrillation properties on the surface. Figure 1-3 It can be seen that the anti-fibrillation effect of Example 1 is the most prominent, and there is no phenomenon of competing with the dye.

[0109] The present invention has been described in detail above. For those skilled in the art, without departing from the purpose and scope of the present invention, and without the need to carry out unnecessary experimental conditions, the present invention can be implemented in a wide range under equivalent parameters, concentrations and conditions. Although the present invention provides specific embodiments, it should be understood that further improvements can be made to the present invention. In short, according to the principles of the present invention, this application is intended to include any changes, uses or improvements to the present invention, including changes that depart from the disclosed scope in this application and are made using conventional techniques known in the art.

Claims

1. A jig dyeing process for preventing fibrillation of lyocell woven fabrics, comprising the following steps: (1) Singeing, desizing and bleaching the Lyocell fabric; The desizing and bleaching process adopts a cold pad-batch desizing and bleaching one-step process: amylase, penetrant, alkali, hydrogen peroxide, refining agent, oxygen bleaching stabilizer, and dispersing chelating agent are added to water and mixed to obtain a treatment bath, and the grey fabric is padded with the treatment bath, rolled up, and then wrapped, sealed, and stacked at room temperature. (2) preparing a dyeing working solution, wherein the dyeing working solution includes a dye, an anti-wrinkle agent, sodium sulfate and soda ash, and mixing the dyeing working solution evenly. After the working solution is heated to a certain temperature, performing the first step of roller dyeing on the lyocell fabric treated in step (1); (3) preparing an anti-fibrillation working solution, wherein the anti-fibrillation working solution comprises an anti-fibrillation cross-linking agent, a leveling agent and a dispersant, stirring the anti-fibrillation working solution at a high speed to obtain a stable suspension, adding the dyeing working solution of step (2) to carry out the second step of roller dyeing; (4) Wash, soap, soften and dry the treated lyocell fabric.

2. The jig dyeing process according to claim 1, characterized in that: In step (1), the singeing is to remove the fuzz from the cloth surface by a through-singing method, the process conditions are two positive and two negative, the speed is 100m / min, and the temperature is 1000-1100℃.

3. The jig dyeing process according to claim 1, characterized in that: In step (1), the dosage of amylase is 5-10 g / L, and the dosage of osmotic agent is 1-5 g / L. The alkali is NaOH, the dosage of NaOH is 6-10 g / L, the hydrogen peroxide is 4-5 g / L, the refining agent is 5-6 g / L, the oxygen bleaching stabilizer is 4-5 g / L, the dispersing chelating agent is 1-2 g / L, and the stacking time is 16-20 hours.

4. The jig dyeing process according to claim 1, characterized in that: In step (2), the dye is one or more of s-triazine type reactive dyes, vinyl sulfone type reactive dyes, and halogenated pyrimidine type reactive dyes; The anti-wrinkle agent is one or more of urea-formaldehyde resin, dimethylolethylene urea resin, dimethylol dihydroxyethylene urea resin, high polymer chitosan, waterborne polyurethane resin, epoxy compound, citric acid, and polymaleic acid; The dyeing working solution is prepared by adding dye, anti-wrinkle agent, sodium sulfate and soda ash into water and mixing them evenly. The amount of dye is 5-20g / L; the amount of anti-wrinkle agent is 1-2g / L; the amount of sodium sulfate is 40-60g / L; and the amount of soda ash is 15-20g / L.

5. The jig dyeing process according to claim 1, characterized in that: In step (2), the first step of the jig dyeing process is to gradually add the dyeing working solution in four times, adding 1 / 4 of the dye solution each time, the dyeing temperature is 60-80°C, and the dyeing time is 15-20 minutes.

6. The jig dyeing process according to claim 1, wherein: In step (3), the anti-fibrillation cross-linking agent is one or more of a dichlorotriazine compound, a dibromotriazine compound, and 1,3,5-triacryloylhexahydro-1,3,5-triazine, and the amount used is 30-80 g / L; The leveling agent is one or more of fatty alkyl sulfate, alkylbenzene sulfonate, polyethylene glycol alkyl ether sulfate, naphthalenesulfonic acid-formaldehyde condensate, polyethylene glycol ether of fatty amine, polyethylene polyamine, and oxyethylated nitrogen-containing fatty alkyl compound, and the amount used is 1-5 g / L; The dispersant is one or more of alkylphenol polyoxyethylene ether, fatty amine polyoxyethylene ether, fatty alcohol polyoxyethylene ether, fatty alcohol polyoxyethylene ether sodium sulfate, and fatty alcohol polyoxyethylene ether sodium carboxylate, and the dosage is 3-5 g / L.

7. The jig dyeing process according to claim 1, characterized in that: In step (3), the process for preparing the anti-fibrillation working liquid is to add the anti-fibrillation crosslinking agent, the leveling agent, and the dispersant into water according to the added amount, mix them evenly, and stir them in a high-speed stirrer for 1-2 hours to obtain a stable suspension, wherein the stirrer speed is 2000-5000 r / min.

8. The jig dyeing process according to claim 1, characterized in that: In step (3), the second step of roller dyeing process conditions are dyeing temperature 60-80°C and dyeing time 45-60min.

9. The jig dyeing process according to claim 1, characterized in that: In step (4), the soaping agent is a mixture of aralkyl polyglycol ester and fatty acid amine, the soaping temperature is 95-100°C, the soaping time is 20-30 minutes, the drying temperature is 110-120°C, and the drying time is 1-2 minutes.

10. The jig dyeing process according to claim 1, characterized in that: The jig dyeing process is suitable for lyocell woven fabrics and lyocell blended fabrics with other fabrics.

Citation Information

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