Pad dyeing process capable of preventing lyocell woven fabric from fibrillation

Abstract

The invention discloses a pad dyeing process capable of preventing fibrillation of a lyocell woven fabric, which is characterized in that dye and a cross-linking agent are used for preparing dye liquor in one bath, and the dye and the cross-linking agent enter the fabric by padding the belt liquor. After being pre-dried, the fabric is padded with a fixation liquid, salt and alkali are brought into the surface of the fabric, and then the fabric is fed into a steaming box for steaming fixation. Meanwhile, the cross-linking agent is subjected to a cross-linking reaction in the fiber at the steaming temperature under the action of salt and alkali. By using the dichlorotriazine cross-linking agent, the antifibrillated lyocell woven fabric can be simply prepared through a rolling-drying-rolling-steaming process.

Description

Technical Field

[0001] The invention relates to the field of textile production technology and processing, and in particular to a pad dyeing process capable of preventing lyocell woven fabric from fibrillation. Background Art

[0002] Lyocell fiber is a regenerated cellulose fiber spun from a cellulose solution dissolved in N-methylmorpholine oxide (NMMO). The fiber production process is environmentally friendly and pollution-free. It has the comfort of cotton fiber, the strength of polyester fiber, the drape of viscose fiber and the silk-like feel. Therefore, it is called the new green fiber of the 21st century.

[0003] Lyocell knitted and woven fabrics that have not been cross-linked will fibrillate during daily wear and washing, resulting in lighter color or "white frost" or pilling, which will affect the feel and gloss of the fabric. Currently, the main way to solve the problem of Lyocell fiber fibrillation is to cross-link the fibers or fabrics.

[0004] At present, most of the anti-fibrillation treatment for lyocell fabrics is for lyocell fibers, including the spinning process and post-spinning treatment process. After cross-linking, the fibers still need to go through multiple processes such as spinning, weaving, pre-treatment, printing and dyeing, and finishing. The cross-linking agent is faced with the consumption of chemical reagents such as acids and alkalis, and there is more friction between the fibers and the equipment, so they are still prone to fibrillation.

[0005] Compared with the dip dyeing process of knitted fabrics, the pad dyeing process of woven fabrics is simple, consumes less water and energy, and has a fast production speed. For the pad dyeing process of Lyocell woven fabrics, the crosslinking agent concentration needs to reach 30-50g / L; how to prevent and control the fibrillation of Lyocell woven fabrics during the dyeing and finishing process, and the crosslinking technology that can be carried out in the same bath as the dyeing process has become a difficult problem that needs to be solved in the field of textile dyeing and finishing. Summary of the invention

[0006] Aiming at the phenomenon that lyocell fabric is prone to fibrillation during production and use, resulting in light color or pilling, the present invention designs a method for preventing and controlling the fibrillation of lyocell woven fabric during dyeing and finishing, and proposes a pad dyeing process that can prevent the fibrillation of lyocell woven fabric.

[0007] The present invention adopts a liquid crosslinking agent, and the dye and the high-solubility crosslinking agent are mixed in the same bath to prepare a dye solution, and the dye and the crosslinking agent are allowed to enter the interior of the fabric by padding with the solution. After the fabric is pre-dried, the fabric is padded with a color fixing solution, and salt and alkali are brought into the fabric surface, and then the fabric is sent to a steamer for steaming and color fixing. At the same time, the crosslinking agent undergoes a crosslinking reaction inside the fiber under the steaming temperature and the action of salt and alkali. Since the dye and the crosslinking agent are padded in the same bath in the pad dyeing process, the two enter the interior of the fabric by padding with the solution, and the crosslinking agent does not affect the amount of dye brought in, and therefore does not affect the color of the fabric.

[0008] The technical solution of the present invention is to provide a pad dyeing process that can prevent the fibrillation of lyocell woven fabrics, and the specific operating steps are as follows: 1) preparing dye solution: the dye solution comprises 4-40 g / L of reactive dye, 30-50 g / L of cross-linking agent, 2 g / L of penetrant, and 10 g / L of anti-migration agent; the rolling rate is 60%-90%, preferably 75%; The cross-linking agent structure is as follows: , X is Cl; R has a water-soluble group. R can be formed by dehydrogenation of one of ethylene glycol, diethylene glycol, diethylene glycol methyl ether, aminoethanol, diethanolamine, triethanolamine, glycerol, polyethylene glycol, polypropylene glycol, polyethylene glycol monomethyl ether, polypropylene glycol monomethyl ether, and polyetheramine;

[0009] 2) Pad-dye the lyocell woven fabric in the dye solution with a padding rate of 60%-90%; 3) Drying in a drying drum at 100°C; 4) Padding alkaline color fixing solution, soda ash: 40g / L; sodium sulfate: 200g / L; rolling rate 60%-90%, preferably 80%; 5) Steam fixation, temperature 100℃, time 2min; 6) Wash with water 6 times; wash with hot water at 95℃ for 2 times (add soap detergent 1g / L), wash with hot water at 80℃ for 2 times, wash with warm water at 60℃ for 1 time, wash with cold water at 25℃ for 1 time (add glacial acetic acid 1g / L); 7) Dry in a drying drum at 100°C.

[0010] Furthermore, the preparation method of the cross-linking agent is as follows: cyanuric chloride and liquid water-soluble organic matter are subjected to a substitution reaction under anhydrous alkaline conditions, so that the liquid water-soluble organic matter replaces one of the Cl groups on cyanuric chloride.

[0011] The liquid phase water-soluble organic matter includes one of ethylene glycol, diethylene glycol, diethylene glycol methyl ether, aminoethanol, diethanolamine, triethanolamine, glycerol, polyethylene glycol, polypropylene glycol, polyethylene glycol monomethyl ether, polypropylene glycol monomethyl ether, and polyetheramine.

[0012] The basic conditions were established by the addition of triethylamine.

[0013] Furthermore, the penetrant in step 1 is a non-ionic scouring penetrant, and the anti-migration agent is sodium alginate.

[0014] Furthermore, the reactive dye in step 1 includes one or more of monochloro-s-triazine type, dichloro-s-triazine type, vinyl sulfone type, monochloro-s-triazine-based and vinyl sulfone-based dual-active group type.

[0015] Furthermore, the neutralizing acid is glacial acetic acid, and the soaping agent may be TF-231H.

[0016] The beneficial effects of the present invention are: 1) Anti-fibrillation treatment is carried out during the pad dyeing process to improve the anti-fibrillation ability of Lyocell fabric during the dyeing, wearing and washing processes. The pad dyeing process is short in time and high in efficiency, and is suitable for large-scale continuous production of anti-fibrillation Lyocell woven fabrics.

[0017] 2) Use highly soluble liquid cyanuric chloride derivatives as cross-linking agents, which can be used in the same bath as the dye during the pad dyeing process without affecting the color of the fabric. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] Figure 1 This is an optical microscope image of Lyocell twill (30 count) after five washes without a crosslinking agent. Figure 2 This is an optical microscope image of Lyocell twill (30 count) after five washes with 30 g / L crosslinking agent; Figure 3 This is an optical microscope image of Lyocell plain weave (40 count) after five washes without a crosslinking agent. Figure 4 This is an optical microscope image of Lyocell plain weave (40 count) after five washes with water at 30 g / L crosslinking agent.

[0019] The following examples are used to further illustrate the present invention, and their purpose is to illustrate the present invention and should not be construed as limiting the scope of the present invention. Unless otherwise specified, all parts by weight and weight percentages are used below.

[0020] The raw materials used in the present invention, unless otherwise specified, are conventional commercially available products; the methods used in the present invention, unless otherwise specified, are conventional methods in the art.

[0021] The embodiments of the present invention are further described below with reference to a plurality of embodiments.

[0022] It should be clear that the described embodiments are only part of the embodiments of the present application, rather than all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by ordinary technicians in the field without creative work are within the scope of protection of the present application.

[0023] The terms used in the embodiments of the present application are only for the purpose of describing specific embodiments, and are not intended to limit the present application. The singular forms "a", "said" and "the" used in the embodiments of the present application and the appended claims are also intended to include plural forms, unless the context clearly indicates other meanings.

[0024] In the present invention, the pad dyeing is specifically a pad-dry-pad-steam process, in which the fabric is dipped into a solution containing the dye, and after drying, the fabric is dipped into a solution containing a color fixing alkali agent (usually soda ash) and an electrolyte (usually sodium sulfate), and then steamed to fix the color.

[0025] Example 1 (1) Preparation of a cross-linking agent: At 0°C, polyethylene glycol 400, cyanuric chloride and alkali (triethylamine) in a molar ratio of 1:1:1 were added to a reaction apparatus and reacted for 6 hours to obtain an anti-fibrillation cross-linking agent.

[0026] (2) Use reactive dyes to prepare dye solution, dye: 4g / L; penetrant: 2g / L; anti-migration agent: 10g / L; cross-linking agent added in the same bath: 30g / L; rolling rate is 75%. The penetrant used is a non-ionic scouring penetrant, and the anti-migration agent is sodium alginate.

[0027] (3) Drying: Dry at 100℃.

[0028] (4) Immersing in alkaline color fixing solution: soda ash: 40g / L; sodium sulfate: 200g / L; the rolling rate is 80%.

[0029] (5) Steam fixation at 100°C for 2 min.

[0030] (6) Washing: Wash twice with 95℃ hot water (add 1g / L soap detergent), wash twice with 80℃ hot water, wash once with 60℃ warm water, and wash once with 25℃ cold water (add 1g / L glacial acetic acid).

[0031] (7) Drum drying: drying at 100°C.

[0032] Anti-fibrillation evaluation method: refer to standard AATCC 135, use a standard washing machine, wash 5 times in total, take out, dry, and observe the fibrillation of the fabric surface with an optical microscope or a scanning electron microscope.

[0033] Dyeing evaluation method: Use a colorimeter to test the dyeing of the fabric samples.

[0034] As shown in Table 1, the anti-fibrillation effect of the lyocell fabric can reach level 4 when the cross-linking agent is used at a dosage of 30 g / L. And as shown in Table 2, the present invention has no significant effect on the dyeing effect of the fabric.

[0035]

[0036] Example 2 (1) Preparation of a cross-linking agent: Add polyethylene glycol monomethyl ether 350, cyanuric chloride and alkali (triethylamine) in a molar ratio of 1:1:1 into a reaction apparatus at 5°C and react for 6 hours to obtain an anti-fibrillation cross-linking agent.

[0037] (2) Use reactive dyes to prepare dye solution, dye: 40g / L; penetrant: 2g / L; anti-migration agent: 10g / L; cross-linking agent added in the same bath: 50g / L; rolling rate is 60%. (The penetrant used is a non-ionic scouring penetrant, and the anti-migration agent is sodium alginate)

[0038] (3) Drying: Dry at 100℃.

[0039] (4) Immersing in alkaline color fixing solution: soda ash: 40 g / L; sodium sulfate: 200 g / L; the rolling rate is 60%.

[0040] (5) Steam fixation at 100°C for 2 min.

[0041] (6) Washing: Wash twice with 95℃ hot water (add 1g / L soap detergent), wash twice with 80℃ hot water, wash once with 60℃ warm water, and wash once with 25℃ cold water (add 1g / L glacial acetic acid).

[0042] (7) Drum drying: drying at 100°C.

[0043] Anti-fibrillation evaluation method: refer to standard AATCC 135, use a standard washing machine, wash 5 times in total, take out, dry, and use an optical microscope to observe the fibrillation of the fabric surface.

[0044] Dyeing evaluation method: Use a colorimeter to test the dyeing of the fabric samples.

[0045] The evaluation results are similar to those of Example 1. When the cross-linking agent is used at a dosage of 50 g / L, the anti-fibrillation effect of the lyocell fabric can reach level 5, and has no significant effect on the dyeing effect of the fabric.

[0046] Example 3 (1) Preparation of a cross-linking agent: Add polyethylene glycol monomethyl ether 350, cyanuric chloride and alkali (triethylamine) in a molar ratio of 1:1:1 into a reaction apparatus at 5°C and react for 6 hours to obtain an anti-fibrillation cross-linking agent.

[0047] (2) Use reactive dyes to prepare dye solution, dye: 40g / L; penetrant: 2g / L; anti-migration agent: 10g / L; cross-linking agent added in the same bath: 50g / L; rolling rate is 90%. (The penetrant used is a non-ionic scouring penetrant, and the anti-migration agent is sodium alginate)

[0048] (3) Drying: Dry at 100℃.

[0049] (4) Immersing in alkaline color fixing solution: soda ash: 40 g / L; sodium sulfate: 200 g / L; the rolling rate is 90%.

[0050] (5) Steam fixation at 100°C for 2 min.

[0051] (6) Washing: Wash twice with 95℃ hot water (add 1g / L soap detergent), wash twice with 80℃ hot water, wash once with 60℃ warm water, and wash once with 25℃ cold water (add 1g / L glacial acetic acid).

[0052] (7) Drum drying: drying at 100°C.

[0053] Anti-fibrillation evaluation method: refer to standard AATCC 135, use a standard washing machine, wash 5 times in total, take out, dry, and use an optical microscope to observe the fibrillation of the fabric surface.

[0054] Dyeing evaluation method: Use a colorimeter to test the dyeing of the fabric samples.

[0055] The evaluation results are similar to those of Example 1. When the cross-linking agent is used at a dosage of 50 g / L, the anti-fibrillation effect of the lyocell fabric can reach level 5, and has no significant effect on the dyeing effect of the fabric.

[0056] Comparative Example --- Crosslinking agent of CN116926971B (1) Preparation of anti-fibrillation composition: 1) Select raw materials according to the following weight percentages of each component:

[0057] The structural formula of cross-linking agent A is as follows: .

[0058] 2) The preparation method of the anti-fibrillation composition is specifically as follows: first, the pH of the cross-linking agent A slurry after the reaction to the end point is adjusted to 5-6 with sodium carbonate, and then sodium dodecylbenzene sulfonate, sodium methylene dinaphthalene sulfonate NNO, succinic acid, and caprolactam are added to the reaction solution with a content of 22% of the cross-linking agent A, and the mixture is stirred at 15-20° C. for 1 hour, and then the slurry is transferred to a spray tower storage tank, spray-dried, and packaged to obtain the anti-fibrillation composition.

[0059] (2) Anti-fibrillation cross-linking finishing: Bath ratio 1:8, after pre-treatment of fabric, add 30g / L of anti-fibrillation composition, run evenly, add 3.5g / L of Reactive Yellow 3RS and 2g / L of Reactive Black KN-B, run evenly, add 40g / L of sodium sulfate, continue running for 20min, heat to 60℃, add 20g / L of soda ash three times, continue running for 40min, take out of the vat, wash, neutralize and dry to obtain anti-fibrillation lyocell fabric.

[0060] Anti-fibrillation evaluation method: refer to standard AATCC 135, use a standard washing machine, wash 5 times in total, take out, dry, and use a scanning electron microscope to observe the fibrillation of the fabric surface.

[0061] Dyeing evaluation method: Use a colorimeter to test the dyeing of the fabric samples.

[0062] During the dyeing operation, it can be seen that the working solution can only remain clear and transparent for one hour, that is, the aqueous solution state of the composition is unstable and has a low solubility. The rolling solution prepared at a concentration of 30 g / L is relatively turbid and produces precipitation, resulting in color spots during roller dyeing, which makes it difficult to apply to roller dyeing of lyocell woven fabrics.

[0063] Moreover, the multifunctional triazine compounds in the composition described in the patent are anionic, and interact with the dye during the dyeing and cross-linking bath, resulting in insufficient dyeing. The non-ionic cross-linking agent used in this application will not affect the dyeing effect during the roller dyeing process, and has better water solubility, and can achieve better cross-linking effect during use.

[0064] Although the embodiments of the present invention are disclosed for illustrative purposes, those skilled in the art will appreciate that various substitutions, changes and modifications are possible without departing from the spirit and scope of the present invention and the appended claims. Therefore, the scope of the present invention is not limited to the contents disclosed in the embodiments.

Claims

1. A pad dyeing process for preventing fibrillation of lyocell woven fabrics, characterized in that: The following steps are involved: (1) preparing a dye solution: the dye solution comprises a reactive dye, a cross-linking agent, a penetrant, and an anti-migration agent; the cross-linking agent has the following structure: , wherein X is Cl; R has a water-soluble group, and R is formed by dehydrogenating one of ethylene glycol, diethylene glycol, diethylene glycol methyl ether, aminoethanol, diethanolamine, triethanolamine, glycerol, polyethylene glycol, polypropylene glycol, polyethylene glycol monomethyl ether, polypropylene glycol monomethyl ether, and polyetheramine; (2) pad-dyeing the lyocell woven fabric in a dye solution with a padding rate of 60% to 90%; (3) Drying in a drying drum at 100°C; (4) Immersing in alkaline fixing solution, with a rolling rate of 60%-90%; (5) Steam fixation, temperature 100°C, time 2 min; (6) 6 washes; (7) Drying in a drying drum at 100°C.

2. The pad dyeing process according to claim 1, characterized in that: In step 1, the concentration of the active dye is 4-40 g / L, the concentration of the penetrant is 2 g / L, the concentration of the anti-migration agent is 10 g / L, and the concentration of the cross-linking agent is 30-50 g / L.

3. The pad dyeing process according to claim 1, characterized in that: The reactive dye in step 1 includes one or more of monochloro-s-triazine type, dichloro-s-triazine type, vinyl sulfone type, monochloro-s-triazine-based and vinyl sulfone-based dual-active group type.

4. The pad dyeing process according to claim 1, wherein the anti-migration agent in step 1 is sodium alginate.

5. The pad dyeing process according to claim 1, wherein the penetrant in step 1 is a non-ionic refining penetrant.

6. The pad dyeing process according to claim 1, characterized in that: The alkaline color fixing solution in step 4 includes 40 g / L soda ash and 200 g / L sodium sulfate.

7. The pad dyeing process according to claim 1, characterized in that: The six water washes in step 6 include two washes at 95° C., two washes at 80° C., one wash at 60° C., and one wash at 25° C. with 1 g / L of neutralizing acid added.

8. The pad dyeing process according to claim 7, characterized in that: The neutralizing acid is glacial acetic acid.

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