A method for preparing an anti-fibrillation crosslinking agent emulsion and an anti-fibrillation lyocell fabric

Abstract

This invention discloses an anti-fibrillation crosslinking agent emulsion and a method for preparing anti-fibrillation lyocell fabric. The emulsion consists of the following components by mass percentage: 30-40% anti-fibrillation crosslinking agent, 5-10% emulsifier, 1-3% anti-settling agent, and the remainder being water. The anti-fibrillation crosslinking agent is one or more multifunctional triazine compounds used in combination. The fabric fibers undergo saturated crosslinking via the triazine compound, and the lyocell fabric is primarily treated using a cold pad-batch process. The specific method is as follows: a working solution containing the anti-fibrillation crosslinking agent emulsion is prepared; the lyocell fabric is padded with the working solution, controlling the liquid carry-over rate, and then rolled and piled; the treated lyocell fabric is washed with hot water soap, then washed with cold water, and dried to obtain the final product. The above preparation method is applicable to lyocell fabrics and their blended fabrics, shortening the processing flow, reducing mechanical friction between the fabric and equipment, and lowering the tendency for fibrillation.

Description

Technical Field

[0001] This invention belongs to the field of textile production and processing technology, specifically relating to an antifibrillation crosslinking agent emulsion and a method for preparing antifibrillation Lyocell fabric. Background Technology

[0002] Lyocell fiber is a man-made cellulose fiber regenerated by dissolving filaments in an aqueous solution of NMMO. It possesses the comfort of cotton, the strength of polyester, the drape of viscose, and the feel of silk, earning it the reputation of being the "green fiber" of the 21st century. Therefore, Lyocell fabrics offer advantages such as high strength, a substantial feel, excellent drape, good moisture absorption, vibrant colors, and good wrinkle resistance. Furthermore, it can be blended, compounded, or interwoven with other fibers to create fabrics with a smooth surface or a velvety effect.

[0003] Fibrillation occurs when lyocell fibers, in a wet state, swell and are subjected to mechanical forces, causing the original single fibers to split axially into finer fibrils. This leads to changes in the fabric's appearance and a decrease in its wearability. Fibrillation is a common characteristic of all cellulosic fibers, but it is more pronounced in lyocell. Currently, the main methods for addressing fibrillation in lyocell fabrics are enzymatic cellulase washing, adding antifibrillating agents, and adding reactive resins. Enzymatic cellulase washing, which removes microfibrils from the fabric surface, is complex, costly, and does not achieve permanent antifibrillation. The fabric will reappear with a white bloom-like fibrillation phenomenon after subsequent washing. Patent publication number WO95 / 28516A discloses a crosslinking agent with multiple acrylamide groups, preferably 1,3,5-triacryloyl-hexahydrotriazine, which can effectively prevent the fibrillation tendency of cellulose fibers. However, the synthesis of this crosslinking agent is complicated, its water solubility is poor, and it is unstable to alkali after crosslinking. Patent CN116926971A uses a multifunctional triazine compound as a crosslinking agent and uses a dyeing and finishing process to treat lyocell fabrics to obtain antifibrillated lyocell fabrics. This finishing process is relatively limited and is not suitable for finishing raw fabrics. Patent CN115772811A obtains lyocell fabrics that can prevent fibrillation through a cold pad-batch dyeing process. However, this process is relatively complicated, requiring desizing of the fabric and repeated baking, resulting in high energy consumption. In addition, the selected antifibrillation finishing resin needs to be baked at high temperature to achieve antifibrillation, making the antifibrillation finishing conditions quite harsh.

[0004] Most current research on crosslinking agents and application processes focuses on the development and application of lyocell fibers. However, fibrillation of lyocell fabrics during processing is a pressing industry problem that needs to be solved. Furthermore, developing a fibrillation finishing process for lyocell fabrics can expand their application range. Therefore, developing a versatile, low-cost, and energy-efficient fibrillation finishing process for lyocell fabrics is urgently needed. Summary of the Invention

[0005] To address the drawback of lyocell fabrics being prone to fibrillation under mechanical forces or friction in a wet state, this invention aims to provide an anti-fibrillation crosslinking agent emulsion and a method for preparing anti-fibrillated lyocell fabrics based on this emulsion. This method reduces friction during fabric pretreatment, significantly shortens the process flow, and not only yields lyocell fabrics with excellent anti-fibrillation properties, but also features low energy consumption, simple operation, no additional equipment costs, and is energy-saving and environmentally friendly.

[0006] The present invention provides an antifibrillation crosslinking agent emulsion, which is composed of the following substances in mass percentage: antifibrillation crosslinking agent 30-40%, emulsifier 5-10%, antisettling agent 1-3%, and the remainder being water;

[0007] The anti-fibrillation crosslinking agent is one or more multifunctional triazine compounds used in combination, and its general structural formula is shown in Formula I:

[0008]

[0009] Wherein, M is a polyol structure, selected from the following polyols after the hydroxyl group has been dehydrogenated: trimethylolpropane, trimethylolethane, glycerol;

[0010] R is a hydrophilic structure selected from polyethylene glycol, with a number-average molecular weight of 200-600.

[0011] According to a specific embodiment of the present invention, the anti-fibrillation crosslinking agent is a compound of formula I above, wherein "M is trimethylolpropane, R is polyethylene glycol, and the number average molecular weight is 400".

[0012] The emulsifier is selected from one or more combinations of polyoxyethylene ether, polyoxypropylene ether, ethylene oxide and propylene oxide block copolymer, and polyol fatty acid ester, such as Span 20, Span 60, Tween 20, Tween 40, etc.

[0013] The anti-settling agent is selected from one or more combinations of polyacrylamide, polyvinylpyrrolidone, and polyvinyl alcohol, such as products purchased from Foshan Aona Polymer Co., Ltd., 201P (polyvinyl wax) and 2206 (polyamide wax).

[0014] The method for preparing anti-fibrillation lyocell fabric provided by this invention involves saturating cross-linking of the lyocell fabric fibers with triazine compounds, and mainly treating the lyocell fabric through a cold pad-batch process, including the following steps:

[0015] (1) Prepare the padding working solution, wherein the concentration of the anti-fibrillation crosslinking agent emulsion in the padding working solution is 30-100 g / L, the concentration of the accelerator is 15-30 g / L, the concentration of the alkali-resistant penetrant is 1-2 g / L, and the pH value of the padding working solution is adjusted to 10-12.

[0016] (2) The lyocell fabric is prepared in step (1) of the padding process, and the liquid content is controlled. The fabric is then rolled up and stacked.

[0017] (3) Wash the Lyocell fabric treated in step (2) with hot water soap, wash with cold water, and dry to obtain antifibrillated Lyocell fabric.

[0018] In step (1) of the above method, the accelerator is selected from one or more combinations of sodium sulfate, sodium sulfite, sodium carbonate, sodium acetate, sodium phosphate, and sodium hexametaphosphate;

[0019] In step (1) of the above method, the alkali-resistant penetrant is selected from one or more combinations of sodium alkyl alcohol sulfate, sodium alkyl sulfonate, and sodium alkyl succinate sulfonate.

[0020] Furthermore, the sodium alkyl alcohol sulfate salt is specifically sodium dodecyl sulfate; the sodium alkyl sulfonate salt is specifically sodium dodecylbenzene sulfonate; and the sodium alkyl succinate sulfonate is specifically sodium ditridecyl succinate sulfonate.

[0021] In step (1) of the above method, the preferred impregnation working solution has an antifibrillation finishing agent concentration of 30-60 g / L, an accelerator concentration of 15 g / L, an alkali-resistant penetrant concentration of 1-2 g / L, and an adjusted pH value of 10-12.

[0022] In step (1) of the above method, sodium hydroxide can be used to adjust the pH value of the impregnation working solution.

[0023] In step (2) of the above method, the liquid carrying rate is controlled at 80%-90%.

[0024] In step (2) of the above method, the stacking temperature is 30-35℃ and the stacking time is 20-24 hours.

[0025] In step (3) of the above method, the temperature of the hot water soap wash is 95-100℃.

[0026] In step (3) of the above method, the drying temperature is 110-120℃ and the drying time is 1-2 minutes.

[0027] The method described above is applicable to lyocell fabrics and their blends.

[0028] Compared with the prior art, the present invention has the following beneficial effects:

[0029] (1) This invention uses triazine compounds as the main body of the anti-fiber finishing agent. Its active group structure has the characteristics of high reactivity. During cold pad-batch processing, it can quickly undergo cross-linking reaction with the hydroxyl groups on the Lyocell fabric fibers, increasing the degree of cross-linking of the fabric fibers. Under subsequent wet friction or vibration conditions, it is not prone to fibrillation. At the same time, alkali-resistant penetrant and accelerator solutions are added to the working solution to make the anti-fiber finishing agent cross-link more fully in the Lyocell fabric.

[0030] (2) The present invention uses cold pad-batch process to perform antifibrillation finishing process on Lyocell fabric, which reduces the friction between fabric and equipment, reduces the tendency of fibrillation, shortens the process flow, and has a high utilization rate of working fluid. The process is simple, easy to operate, and does not increase additional equipment costs.

[0031] (3) The present invention has a good anti-fibrillation effect on Lyocell fabric, good wash resistance, and no fibrillation phenomenon after 10 washes. At the same time, no formaldehyde is released during the finishing process, thus avoiding harm to the human body and the environment. Attached Figure Description

[0032] Figure 1 Infrared spectrum of the antifibrillation crosslinking agent.

[0033] Figure 2 Mass spectrum of the antifibrillating crosslinking agent.

[0034] Figure 3 Comparison of white frost on the surface of Lyocell fabric before and after finishing. Detailed Implementation

[0035] The present invention will now be described in further detail with reference to specific embodiments. The given embodiments are merely illustrative of the invention and not intended to limit its scope. The embodiments provided below can serve as a guide for further improvements by those skilled in the art and do not constitute a limitation on the invention in any way.

[0036] Unless otherwise specified, the experimental methods used in the following examples are conventional methods, performed according to the techniques or conditions described in the literature in this field or according to the product instructions. Unless otherwise specified, the materials and reagents used in the following examples are commercially available.

[0037] The anti-settling agents were purchased from Foshan Aona Polymer Co., Ltd., namely 201P (polyethylene wax) and 2206 (polyamide wax).

[0038] In the following examples, the anti-fibrillation crosslinking agent used is the compound of formula I above, where M is the group formed by dehydrogenating the three hydroxyl groups in trimethylolpropane, R is polyethylene glycol, and the number average molecular weight is 400. For specific preparation methods, please refer to CN105113252A, "An anti-wrinkle agent containing heterodiactive groups, its preparation method and application".

[0039] Figure 1 The infrared absorption spectrum of the anti-fiber crosslinking agent; among which, 1549 cm⁻¹ -1 and 1506cm -1 The absorption peak at 1080-1150 cm⁻¹ is a characteristic absorption peak of the triazine ring skeleton. -1 The peak at 3200-3600 cm⁻¹ is a characteristic absorption peak for COC on the polyethylene glycol ether chain. Additionally, the peak at 3200-3600 cm⁻¹ is also present. -1 The absence of characteristic absorption peaks indicates that the terminal hydroxyl groups of both the polyol and polyethylene glycol have reacted completely.

[0040] Figure 2 Mass spectrum of anti-fibrillation crosslinking agent; by Figure 2 It is known that polyethylene glycol molecules are a mixture of different ether chain segments, with each ether chain having a molecular weight of 44. Therefore, a series of ion peaks appear in the mass spectrum, such as 312, 357, 401, 445, and 489, while hydrolysis peaks of the crosslinking agent, such as 312, 339, 383, 427, and 471, also appear. It can be seen from the combined infrared and mass spectra that the anti-fibrillation crosslinking agent is indeed a triazine compound.

[0041] Example 1

[0042] I. Anti-fibrillation crosslinking agent emulsion (components by weight percentage):

[0043]

[0044] II. A process for preparing antigen-modified lyocell fabric, wherein the fibers of the fabric are saturated cross-linked with triazine compounds, and the lyocell fabric is mainly treated by a cold pad-batch process, comprising the following steps:

[0045] (1) Prepare the padding working solution, wherein the concentration of the anti-fibrillation crosslinking agent emulsion is 30 g / L, and the pH of the working solution is adjusted to 10 with sodium hydroxide;

[0046] (2) Take the working solution prepared in step (1) of the three dips and three grapples of Lyocell fabric, control the liquid rate at 90%, roll it up, and stack it at 30°C for 24 hours.

[0047] (3) Wash the Lyocell fabric treated in step (2) with soap in hot water at 95°C, wash with cold water, and dry at 120°C for 2 minutes.

[0048] Example 2

[0049] I. Anti-fibrillation crosslinking agent emulsion (components by weight percentage):

[0050]

[0051]

[0052] II. A process for preparing antigen-modified lyocell fabric, wherein the fibers of the fabric are saturated cross-linked with triazine compounds, and the lyocell fabric is mainly treated by a cold pad-batch process, comprising the following steps:

[0053] (1) Prepare the padding working solution, wherein the concentration of the anti-fibrillation crosslinking agent emulsion is 30 g / L, the concentration of sodium phosphate is 15 g / L, the concentration of the alkali-resistant penetrant sodium dodecylbenzene sulfonate is 2 g / L, and the pH of the working solution is adjusted to 10 with sodium hydroxide;

[0054] (2) Take the working solution prepared in step (1) of the three dips and three grapples of Lyocell fabric, control the liquid rate at 90%, roll it up, and stack it at 35°C for 24 hours.

[0055] (3) Wash the Lyocell fabric treated in step (2) with soap in hot water at 95°C, wash with cold water, and dry at 110°C for 2 minutes.

[0056] Example 3

[0057] I. Anti-fibrillation crosslinking agent emulsion (components by weight percentage):

[0058]

[0059] II. A process for preparing antigen-modified lyocell fabric, wherein the fibers of the fabric are saturated cross-linked with triazine compounds, and the lyocell fabric is mainly treated by a cold pad-batch process, comprising the following steps:

[0060] (1) Prepare the padding working solution, wherein the concentration of the anti-fibrillation crosslinking agent emulsion is 40 g / L, the concentration of sodium sulfite is 15 g / L, the concentration of the alkali-resistant penetrant sodium bis(tridecyl) succinate sulfonate is 2 g / L, and the pH of the working solution is adjusted to 12 with sodium hydroxide.

[0061] (2) Take the working solution prepared in step (1) of the three dips and three grapples of Lyocell fabric, control the liquid rate at 90%, roll it up, and stack it at 35°C for 24 hours.

[0062] (3) Wash the Lyocell fabric treated in step (2) with soap in hot water at 95°C, wash with cold water, and dry at 120°C for 2 minutes.

[0063] Example 4

[0064] I. Anti-fibrillation crosslinking agent emulsion (components by weight percentage):

[0065]

[0066] II. A process for preparing antigen-modified lyocell fabric, wherein the fibers of the fabric are saturated cross-linked with triazine compounds, and the lyocell fabric is mainly treated by a cold pad-batch process, comprising the following steps:

[0067] (1) Prepare the padding working solution, wherein the concentration of the anti-fibrillation crosslinking agent emulsion is 50 g / L, the concentration of sodium sulfate is 15 g / L, the concentration of the alkali-resistant penetrant sodium dodecylbenzene sulfonate is 2 g / L, and the pH of the working solution is adjusted to 11 with sodium hydroxide;

[0068] (2) Take the working solution prepared in step (1) of the three dips and three grapples of Lyocell fabric, control the liquid rate at 90%, roll it up, and stack it at 35°C for 24 hours.

[0069] (3) Wash the Lyocell fabric treated in step (2) with soap in hot water at 95°C, wash with cold water, and dry at 120°C for 2 minutes.

[0070] Example 5

[0071] (1) Anti-fiberizing finishing agent emulsion (components by weight percentage):

[0072]

[0073] (2) A process for preparing an antigen-modified lyocell fabric, wherein the fibers of the fabric are saturated crosslinked with triazine compounds, and the lyocell fabric is mainly treated by a cold pad-batch process, comprising the following steps:

[0074] (1) Prepare the padding working solution, wherein the concentration of the anti-fibrillation crosslinking agent emulsion is 60 g / L, the concentration of sodium hexametaphosphate is 15 g / L, the concentration of the alkali-resistant penetrant sodium dodecylbenzenesulfonate is 2 g / L, and the pH of the working solution is adjusted to 12 with sodium hydroxide.

[0075] (2) Take the working solution prepared in step (1) of the three dips and three grapples of Lyocell fabric, control the liquid rate at 90%, roll it up, and stack it at 35°C for 24 hours.

[0076] (3) Wash the Lyocell fabric treated in step (2) with soap in 95°C hot water, rinse with cold water, and dry at 120°C for 2 minutes. Experiment on the anti-fibrotic properties of Lyocell fabric before and after treatment:

[0077] This invention relates to a method for determining the fibrillation degree of lyocell fabrics. It tests the anti-pilling and anti-fuzzing grade of the lyocell fabric and the surface white bloom phenomenon after 5 and 10 washes, respectively, before and after treatment. A blank sample serves as a control. The anti-pilling and anti-fuzzing performance was tested according to GB / T4802.1-1997 standard, and the lyocell textiles were washed 10 times according to GB 12799-91 standard. The results are shown in Table 1. A comparison of the surface white bloom of the lyocell fabric before and after treatment is shown in the figure. Figure 2 As shown.

[0078] Table 1 Comparison of antigenic fibrillation properties of Lyocell fabrics before and after finishing.

[0079]

[0080]

[0081] As shown in Table 1, the anti-pilling performance of Lyocell fabrics without anti-fibrillation crosslinking agent treatment began to decline after 5 washes, and dropped to level 1 after 10 washes. The anti-fibrillation Lyocell fabrics without accelerator and alkali-resistant penetrant treatment showed improved anti-pilling and anti-fibrillation properties. The Lyocell fabrics treated with a combination of anti-fibrillation crosslinking agent, accelerator and alkali-resistant penetrant had better anti-pilling performance and anti-fibrillation properties on the fabric surface.

[0082] Depend on Figure 3 It can be seen that after 5 washes, white frost appeared on the surface of Lyocell fabrics that were not treated with antifibrillation crosslinking agent, and the white frost was severe after 10 washes. After 10 washes, antifibrillation Lyocell fabrics without accelerator and alkali-resistant penetrating agent treatment had a small amount of white frost on the surface. Lyocell fabrics treated with antifibrillation crosslinking agent, accelerator and alkali-resistant penetrating agent did not have white frost on the surface.

Claims

1. A method for preparing an anti-fibrillated lyocell fabric, comprising the following steps: (1) Prepare the padding working solution, wherein the concentration of the anti-fibrillation crosslinking agent emulsion in the padding working solution is 30-100 g / L, the concentration of the accelerator is 15-30 g / L, the concentration of the alkali-resistant penetrant is 1-2 g / L, and the pH value of the padding working solution is adjusted to 10-12. wherein The antifibrillation crosslinking agent emulsion is composed of the following substances in mass percentage: antifibrillation crosslinking agent 30-40%, emulsifier 5-10%, antisettling agent 1-3%, and the remainder is water; The general structural formula of the anti-fibrillation crosslinking agent is shown in Formula I: Formula I In Formula I, M is a polyol structure selected from the following polyols after the hydroxyl group has been dehydrogenated: trimethylolpropane, trimethylolethane, and glycerol. R is a hydrophilic structure, selected from polyethylene glycol, with a number-average molecular weight of 200-600; (2) The lyocell fabric is prepared in step (1) of padding process, and the liquid content is controlled and the fabric is rolled up and stacked. (3) Wash the Lyocell fabric treated in step (2) with hot water soap, wash with cold water, and dry to obtain antifibrillated Lyocell fabric.

2. The method of claim 1, wherein: In step (1), the accelerator is selected from one or more combinations of sodium sulfate, sodium sulfite, sodium carbonate, sodium acetate, sodium phosphate, and sodium hexametaphosphate. Alternatively, in step (1), the alkali-resistant penetrant is selected from one or more combinations of sodium alkyl alcohol sulfate, sodium alkyl sulfonate, and sodium alkyl succinate sulfonate.

3. The method of claim 2, wherein: The sodium alkyl alcohol sulfate salt is specifically sodium dodecyl sulfate; the sodium alkyl sulfonate salt is specifically sodium dodecylbenzene sulfonate; and the sodium alkyl succinate sulfonate is specifically sodium ditridecyl succinate sulfonate.

4. The production method according to any one of claims 1 to 3, characterized by: In step (1), the concentration of the anti-fibrillation crosslinking agent emulsion in the padding working solution is 30-60 g / L, the concentration of the accelerator is 15 g / L, the concentration of the alkali-resistant penetrant is 1-2 g / L, and the pH value of the padding working solution is adjusted to 10-12.

5. The method of claim 1, wherein: In step (2), the liquid carrying rate is controlled at 80%-90%.

6. The method of claim 1, wherein: In step (2), the temperature of the stacking is 30-35℃ and the stacking time is 20-24 hours.

7. The method of claim 1, wherein: In step (3), the temperature of the hot water soap wash is 95-100℃; Alternatively, in step (3), the drying temperature is 110-120℃ and the drying time is 1-2 minutes.

8. The method of claim 1, wherein: The emulsifier is selected from one or more combinations of polyoxyethylene ether, polyoxypropylene ether, ethylene oxide and propylene oxide block copolymer, and polyol fatty acid ester; Alternatively, the anti-settling agent may be selected from one or more combinations of polyacrylamide, polyvinylpyrrolidone, and polyvinyl alcohol.

9. The method of claim 1, wherein: The method is applicable to lyocell fabrics and their blends.

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