Flame-retardant acrylic yarn, preparation process thereof and flame-retardant fabric

Abstract

The invention provides a flame-retardant acrylic yarn, a preparation process thereof and a flame-retardant fabric, and belongs to the technical field of textiles. The preparation process of the flame-retardant acrylic yarn comprises the following steps: S01, preparing a flame-retardant solution containing modified chitosan; s02, dipping acrylic yarns in the flame-retardant solution prepared in S01; and S03, shaping, washing and drying. Chitosan usually does not release toxic gas during combustion, mainly generates water and carbon dioxide, and has small influence on the environment. When the modified chitosan is combusted, even if some additional gas is generated, the toxicity is relatively low. According to the flame-retardant acrylic yarn, the modified chitosan serves as the flame retardant, the flame retardant is green and causes little pollution during combustion, and the modified chitosan can remarkably improve the flame retardance of the acrylic yarn.

Description

Technical Field

[0001] The present invention relates to the field of textile technology, in particular to a flame-retardant acrylic yarn and a preparation process thereof, and a flame-retardant fabric. Background Art

[0002] Acrylic fiber has a wool-like feel, a soft texture, and excellent warmth retention. It is commonly used in sweaters, knitwear, sportswear, and outerwear. It also offers excellent abrasion and light resistance, making it suitable for outdoor wear. Acrylic fiber has a wide range of applications, from clothing to industrial products. While standard acrylic fiber exhibits some flame retardancy, its flame retardancy needs to be further enhanced to meet specialized needs. Through chemical modification and the addition of flame retardants, the flame retardancy of acrylic fiber can be significantly improved, thus playing a vital role in fire prevention and protection.

[0003] Chitosan is a multifunctional natural polymer material with good biocompatibility, biodegradability and multiple biological activities. It is widely used in medicine, food, agriculture, environmental protection and other fields. Summary of the Invention

[0004] In response to the above problems, the present invention proposes an improved flame-retardant acrylic yarn based on chitosan. The modified chitosan does not need to work together with phytic acid and does not include phosphorus components. The obtained flame-retardant acrylic yarn has excellent flame retardant properties.

[0005] The first aspect of the present invention is to disclose a preparation process of a flame retardant acrylic yarn, comprising the following steps:

[0006] S01, preparing a flame retardant solution containing modified chitosan;

[0007] S02, acrylic yarn impregnated with the flame retardant solution prepared in S01;

[0008] S03, setting, washing and drying.

[0009] In some embodiments of the present invention, in S01, chitosan is modified using nano-silica, a silane coupling agent, and epichlorohydrin as main raw materials;

[0010] Preferably, the active substance in the flame retardant solution does not include phytic acid and phosphorus.

[0011] In some embodiments of the present invention, in S02, acrylic yarn is taken and immersed in the flame retardant solution obtained in S01 at a weight-to-volume ratio of 1:(5-15), and then removed after being heated at 30-50° C. for 5-15 hours and drained.

[0012] In some embodiments of the present invention, in S03, the shaping is performed by dry steaming at 110-130° C. for 3-6 hours in a high temperature and high pressure steam setting pot.

[0013] In some embodiments of the present invention, in S01, the ratio of chitosan and nano-silica, silane coupling agent and epichlorohydrin is 80-120g:5-15g:10-20mL:30-150g, preferably 100g:5-15g:10-20mL:50-150g, and further preferably 100g:5-15g:10-20mL:80-120g.

[0014] In some embodiments of the present invention, in S01, in the flame retardant solution, the content of the modified chitosan is 1-10%, and the content of Tween 80 is 0.5-2%; preferably, the content of the modified chitosan is 3-8%, and the content of Tween 80 is 0.5-1%.

[0015] In some embodiments of the present invention, S01 further includes a brominated flame retardant.

[0016] In some embodiments of the present invention, in S01, in the flame retardant solution, the weight ratio of the modified chitosan to the brominated flame retardant is (0.5-1):(1-3), preferably 1:(1-2).

[0017] The second aspect of the present invention is to disclose the flame retardant acrylic yarn obtained according to the preparation process of the flame retardant acrylic yarn described in the first aspect.

[0018] The third aspect of the present invention is to disclose a flame-retardant fabric woven from the flame-retardant acrylic yarn according to the first aspect.

[0019] Chitosan itself typically does not release toxic gases when burned, primarily producing water and carbon dioxide, resulting in minimal environmental impact. Even if modified chitosan produces some additional gases when burned, these gases are relatively less toxic. The flame-retardant acrylic yarn of the present invention uses modified chitosan as a flame retardant. This environmentally friendly flame retardant produces minimal pollution when burned, and the modified chitosan can significantly improve the flame retardant properties of the acrylic yarn.

[0020] In research on the preparation of the flame-retardant acrylic yarn, the present invention also found that the combination of modified chitosan and a brominated flame retardant significantly improved flame retardancy compared to either alone, demonstrating a synergistic effect. This is likely because the modified chitosan forms a protective layer during combustion, while the brominated flame retardant promotes char formation, which together enhance flame retardancy.

[0021] In addition, the study also found that a specific proportion of modified chitosan and brominated flame retardants can also improve the antistatic properties of flame retardant acrylic yarn. DETAILED DESCRIPTION

[0022] The following describes the embodiments of the present invention through specific examples. Those skilled in the art will readily understand the other advantages and benefits of the present invention from the disclosure herein. The present invention may also be implemented or applied through various other specific embodiments, and the details in this specification may be modified or altered based on different viewpoints and applications without departing from the spirit of the present invention.

[0023] In the following examples and comparative examples, all reagents used are commercially available products.

[0024] Unless otherwise noted, the following examples and comparative examples represent parallel experiments with identical components, component amounts, preparation steps, and preparation parameters. The epichlorohydrin was acidified with HCl to a pH of 6.2±0.1. The chitosan pretreated with sodium hydroxide was dispersed in isopropanol, 10% by weight of sodium hydroxide was added, and the mixture was reacted at 50°C for 1 hour. In the flame retardant solution, the contents of modified chitosan and decabromodiphenylethane are expressed in weight percentage (w / w), and the content of Tween 80 is expressed in weight volume percentage (w / v, g / mL).

[0025] Example 1

[0026] A preparation process of flame retardant acrylic yarn:

[0027] (1) Preparation of modified chitosan:

[0028] KH-550 silane coupling agent 15mL Nanosilica 10g Epichlorohydrin 100g Chitosan 100g Sodium hydroxide 10g

[0029] Take KH-550 silane coupling agent and add it into a container. Add 10 times the volume of toluene and stir to dilute. Add nano-silica and stir to react at 70°C for 3 hours. Cool, filter, wash, dry and set aside.

[0030] Add anhydrous ethanol at a weight-to-volume ratio (g / mL) of 10 times that of the solid product, slowly add epichlorohydrin dropwise, stir and react at 45°C for 8 hours, cool, filter, wash, dry and set aside;

[0031] Isopropanol at a weight-to-volume ratio (g / mL) of 10 times that of the solid product was added, and chitosan pretreated with sodium hydroxide was added. The mixture was stirred and reacted at 45° C. for 8 h, cooled, filtered, washed, and dried for 5 h to obtain modified chitosan.

[0032] (2) Preparation of flame retardant solution

[0033] Take (1) to obtain modified chitosan, add purified water, add Tween 80, and stir;

[0034] The content of modified chitosan is 5%, and the content of Tween 80 is 1%;

[0035] (3) Impregnation

[0036] Take acrylic yarn and immerse it in the flame retardant solution obtained in (2) at a weight-to-volume ratio of 1:10. After immersing it at 40°C for 10 hours, remove it and drain it.

[0037] (4) Finalization

[0038] The impregnated acrylic yarn obtained in (3) was dry-steamed at 120° C. for 5 h in a high-temperature and high-pressure steam setting pot, washed with water, and dried to obtain a flame-retardant acrylic yarn.

[0039] Example 2

[0040] A preparation process of flame retardant acrylic yarn:

[0041] (1) Preparation of modified chitosan:

[0042]

[0043]

[0044] Take KH-550 silane coupling agent and add it into a container. Add 10 times the volume of toluene and stir to dilute. Add nano-silica and stir to react at 70°C for 3 hours. Cool, filter, wash, dry and set aside.

[0045] Add anhydrous ethanol at a weight-to-volume ratio (g / mL) of 15 times that of the solid product, slowly add epichlorohydrin dropwise, stir and react at 50°C for 8 hours, cool, filter, wash, dry and set aside;

[0046] Isopropanol at a weight-to-volume ratio (g / mL) of 15 times that of the solid product was added, and chitosan pretreated with sodium hydroxide was added. The mixture was stirred and reacted at 45° C. for 8 h, cooled, filtered, washed, and dried for 5 h to obtain modified chitosan.

[0047] (2) Preparation of flame retardant solution

[0048] Take (1) to obtain modified chitosan, add purified water, add Tween 80, and stir;

[0049] The content of modified chitosan is 5%, and the content of Tween 80 is 1%;

[0050] (3) Impregnation

[0051] Take acrylic yarn and immerse it in the flame retardant solution obtained in (2) at a weight-to-volume ratio of 1:10. After immersing it at 40°C for 10 hours, remove it and drain it.

[0052] (4) Finalization

[0053] The impregnated acrylic yarn obtained in (3) was dry-steamed at 120° C. for 5 h in a high-temperature and high-pressure steam setting pot, washed with water, and dried to obtain a flame-retardant acrylic yarn.

[0054] Example 3

[0055] A preparation process of flame retardant acrylic yarn:

[0056] (1) Preparation of modified chitosan:

[0057] KH-550 silane coupling agent 15mL Nanosilica 10g Epichlorohydrin 80g Chitosan 100g Sodium hydroxide 10g

[0058] Take KH-550 silane coupling agent and add it into a container. Add 10 times the volume of toluene and stir to dilute. Add nano-silica and stir to react at 70°C for 3 hours. Cool, filter, wash, dry and set aside.

[0059] Add anhydrous ethanol at a weight-to-volume ratio (g / mL) of 10 times that of the solid product, slowly add epichlorohydrin dropwise, stir and react at 45°C for 8 hours, cool, filter, wash, dry and set aside;

[0060] Isopropanol at a weight-to-volume ratio (g / mL) of 10 times that of the solid product was added, and chitosan pretreated with sodium hydroxide was added. The mixture was stirred and reacted at 45° C. for 8 h, cooled, filtered, washed, and dried for 5 h to obtain modified chitosan.

[0061] (2) Preparation of flame retardant solution

[0062] Take (1) to obtain modified chitosan, add purified water, add Tween 80, and stir;

[0063] The content of modified chitosan is 4%, and the content of Tween 80 is 1%;

[0064] (3) Impregnation

[0065] Take acrylic yarn and immerse it in the flame retardant solution obtained in (2) at a weight-to-volume ratio of 1:10. After immersing it at 40°C for 10 hours, remove it and drain it.

[0066] (4) Finalization

[0067] The impregnated acrylic yarn obtained in (3) was dry-steamed at 120° C. for 5 h in a high-temperature and high-pressure steam setting pot, washed with water, and dried to obtain a flame-retardant acrylic yarn.

[0068] Example 4

[0069] A preparation process of flame retardant acrylic yarn:

[0070] (1) Preparation of modified chitosan:

[0071] KH-550 silane coupling agent 15mL Nanosilica 5g Epichlorohydrin 50g Chitosan 100g Sodium hydroxide 10g

[0072] Take KH-550 silane coupling agent and add it into a container. Add 10 times the volume of toluene and stir to dilute. Add nano-silica and stir to react at 70°C for 3 hours. Cool, filter, wash, dry and set aside.

[0073] Add anhydrous ethanol at a weight-to-volume ratio (g / mL) of 10 times that of the solid product, slowly add epichlorohydrin dropwise, stir and react at 45°C for 8 hours, cool, filter, wash, dry and set aside;

[0074] Isopropanol at a weight-to-volume ratio (g / mL) of 10 times that of the solid product was added, and chitosan pretreated with sodium hydroxide was added. The mixture was stirred and reacted at 45° C. for 8 h, cooled, filtered, washed, and dried for 5 h to obtain modified chitosan.

[0075] (2) Preparation of flame retardant solution

[0076] Take (1) to obtain modified chitosan, add purified water, add Tween 80, and stir;

[0077] The content of modified chitosan is 5%, and the content of Tween 80 is 1%;

[0078] (3) Impregnation

[0079] Take acrylic yarn and immerse it in the flame retardant solution obtained in (2) at a weight-to-volume ratio of 1:10. After immersing it at 40°C for 10 hours, remove it and drain it.

[0080] (4) Finalization

[0081] The impregnated acrylic yarn obtained in (3) was dry-steamed at 120° C. for 5 h in a high-temperature and high-pressure steam setting pot, washed with water, and dried to obtain a flame-retardant acrylic yarn.

[0082] Example 5

[0083] A preparation process of flame retardant acrylic yarn:

[0084] (1) Preparation of modified chitosan:

[0085] KH-550 silane coupling agent 15mL Nanosilica 10g Epichlorohydrin 100g Chitosan 100g Sodium hydroxide 10g

[0086] Take KH-550 silane coupling agent and add it into a container. Add 10 times the volume of toluene and stir to dilute. Add nano-silica and stir to react at 70°C for 3 hours. Cool, filter, wash, dry and set aside.

[0087] Add anhydrous ethanol at a weight-to-volume ratio (g / mL) of 10 times that of the solid product, slowly add epichlorohydrin dropwise, stir and react at 45°C for 8 hours, cool, filter, wash, dry and set aside;

[0088] Isopropanol at a weight-to-volume ratio (g / mL) of 10 times that of the solid product was added, and chitosan pretreated with sodium hydroxide was added. The mixture was stirred and reacted at 45° C. for 8 h, cooled, filtered, washed, and dried for 5 h to obtain modified chitosan.

[0089] (2) Preparation of flame retardant solution

[0090] Take the modified chitosan obtained in (1), add purified water, add Tween 80, stir, add decabromodiphenylethane dissolved in N,N-dimethylformamide, stir for 30 minutes, ultrasonically treat for 20 minutes, and stir for another 30 minutes;

[0091] The content of modified chitosan is 5%, the content of Tween 80 is 1%, and the content of decabromodiphenylethane is 10%;

[0092] (3) Impregnation

[0093] Take acrylic yarn and immerse it in the flame retardant solution obtained in (2) at a weight-to-volume ratio of 1:10. After immersing it at 40°C for 10 hours, remove it and drain it.

[0094] (4) Finalization

[0095] The impregnated acrylic yarn obtained in (3) was dry-steamed at 120° C. for 5 h in a high-temperature and high-pressure steam setting pot, washed with water, and dried to obtain a flame-retardant acrylic yarn.

[0096] Example 6

[0097] A preparation process of flame retardant acrylic yarn:

[0098] (1) Preparation of modified chitosan:

[0099] KH-550 silane coupling agent 15mL Nanosilica 10g Epichlorohydrin 100g Chitosan 100g Sodium hydroxide 10g

[0100] Take KH-550 silane coupling agent and add it into a container. Add 10 times the volume of toluene and stir to dilute. Add nano-silica and stir to react at 70°C for 3 hours. Cool, filter, wash, dry and set aside.

[0101] Add anhydrous ethanol at a weight-to-volume ratio (g / mL) of 10 times that of the solid product, slowly add epichlorohydrin dropwise, stir and react at 45°C for 8 hours, cool, filter, wash, dry and set aside;

[0102] Isopropanol at a weight-to-volume ratio (g / mL) of 10 times that of the solid product was added, and chitosan pretreated with sodium hydroxide was added. The mixture was stirred and reacted at 45° C. for 8 h, cooled, filtered, washed, and dried for 5 h to obtain modified chitosan.

[0103] (2) Preparation of flame retardant solution

[0104] Take the modified chitosan obtained in (1), add purified water, add Tween 80, stir, add decabromodiphenylethane dissolved in N,N-dimethylformamide, stir for 30 minutes, ultrasonically treat for 20 minutes, and stir for another 30 minutes;

[0105] The content of modified chitosan is 5%, the content of Tween 80 is 1%, and the content of decabromodiphenylethane is 5%;

[0106] (3) Impregnation

[0107] Take acrylic yarn and immerse it in the flame retardant solution obtained in (2) at a weight-to-volume ratio of 1:10. After immersing it at 40°C for 10 hours, remove it and drain it.

[0108] (4) Finalization

[0109] The impregnated acrylic yarn obtained in (3) was dry-steamed at 120° C. for 5 h in a high-temperature and high-pressure steam setting pot, washed with water, and dried to obtain a flame-retardant acrylic yarn.

[0110] Example 7

[0111] A preparation process of flame retardant acrylic yarn:

[0112] (1) Preparation of modified chitosan:

[0113] KH-550 silane coupling agent 15mL Nanosilica 10g Epichlorohydrin 100g Chitosan 100g Sodium hydroxide 10g

[0114] Take KH-550 silane coupling agent and add it into a container. Add 10 times the volume of toluene and stir to dilute. Add nano-silica and stir to react at 70°C for 3 hours. Cool, filter, wash, dry and set aside.

[0115] Add anhydrous ethanol at a weight-to-volume ratio (g / mL) of 10 times that of the solid product, slowly add epichlorohydrin dropwise, stir and react at 45°C for 8 hours, cool, filter, wash, dry and set aside;

[0116] Isopropanol at a weight-to-volume ratio (g / mL) of 10 times that of the solid product was added, and chitosan pretreated with sodium hydroxide was added. The mixture was stirred and reacted at 45° C. for 8 h, cooled, filtered, washed, and dried for 5 h to obtain modified chitosan.

[0117] (2) Preparation of flame retardant solution

[0118] Take the modified chitosan obtained in (1), add purified water, add Tween 80, stir, add decabromodiphenylethane dissolved in N,N-dimethylformamide, stir for 30 minutes, ultrasonically treat for 20 minutes, and stir for another 30 minutes;

[0119] The content of modified chitosan is 5%, the content of Tween 80 is 1%, and the content of decabromodiphenylethane is 15%;

[0120] (3) Impregnation

[0121] Take acrylic yarn and immerse it in the flame retardant solution obtained in (2) at a weight-to-volume ratio of 1:10. After immersing it at 40°C for 10 hours, remove it and drain it.

[0122] (4) Finalization

[0123] The impregnated acrylic yarn obtained in (3) was dry-steamed at 120° C. for 5 h in a high-temperature and high-pressure steam setting pot, washed with water, and dried to obtain a flame-retardant acrylic yarn.

[0124] Comparative Example 1

[0125] A preparation process for flame-retardant acrylic yarn, which differs from Example 1 in that unmodified chitosan is directly used in (2).

[0126] Comparative Example 2

[0127] A preparation process for flame-retardant acrylic yarn, which differs from Example 5 in that unmodified chitosan is directly used in (2).

[0128] Flame retardant properties:

[0129] The flame-retardant acrylic yarns of the embodiment and the comparative example were used as the warp and weft threads, and the warp and weft threads were interwoven perpendicularly to each other to prepare a fabric, and the density of the warp and weft threads was 80 threads / cm.

[0130] The limiting oxygen index is determined according to the standard / LOI in FZT50017-2011. The results are shown in the table below.

[0131] LOI Example 1 35 Example 2 34 Example 3 32 Example 4 28 Example 5 48 Example 6 43 Example 7 44 Comparative Example 1 22 Comparative Example 2 36

[0132] The results show that the flame retardancy of the fabrics obtained in Examples 1-3 is significantly better than that of Comparative Example 1, demonstrating the flame retardancy of the modified chitosan. In addition, the flame retardancy of the fabrics obtained in Examples 1-3 is also significantly better than that of Example 4, demonstrating the significant impact of the chitosan modification method.

[0133] The results showed that the flame retardant properties of the fabrics obtained in Examples 5-7 were significantly better than those in Example 1, demonstrating the synergistic effect of the modified chitosan and the brominated flame retardant. However, there was no significant difference between Comparative Example 2 and Example 1, indicating that the unmodified chitosan and brominated flame retardant were simply superimposed and lacked a synergistic effect.

[0134] Antistatic properties:

[0135] The volume resistivity is used to characterize the antistatic properties of flame retardant fabrics.

[0136] The results show that the volume resistivity of Examples 5 and 6 is 5.1×10 8 Ω·cm and 5.8×10 8 Ω·cm, and the volume resistivity of Examples 5 and 6 is 6.1×10 8 Ω·cm, indicating that modified chitosan and brominated flame retardants not only affect the flame retardant properties of acrylic yarn, but also improve the antistatic properties.

[0137] The preferred specific implementation modes and embodiments of the present invention are described in detail above, but the present invention is not limited to the above implementation modes and embodiments. Various changes can be made within the scope of knowledge possessed by those skilled in the art without departing from the concept of the present invention.

Claims

1. A process for preparing a flame retardant acrylic yarn, characterized in that: The following steps are involved: S01, preparing a flame retardant solution containing modified chitosan; S02, acrylic yarn impregnated with the flame retardant solution prepared in S01; S03, setting, washing and drying.

2. The process for preparing the flame retardant acrylic yarn according to claim 1, wherein: In S01, chitosan was modified using nano-silica, silane coupling agent and epichlorohydrin as the main raw materials; Preferably, the active substance in the flame retardant solution does not include phytic acid and phosphorus.

3. The process for preparing the flame retardant acrylic yarn according to claim 1 or 2, wherein: In S02, take acrylic yarn and immerse it in the flame retardant solution obtained in S01 at a weight-to-volume ratio of 1:(5-15), then remove it from the solution at 30-50°C for 5-15 hours and drain it.

4. The process for preparing the flame retardant acrylic yarn according to any one of claims 1 to 3, wherein: In S03, the shaping is performed by dry steaming at 110-130°C for 3-6 hours in a high temperature and high pressure steam setting pot.

5. The process for preparing the flame retardant acrylic yarn according to any one of claims 1 to 4, characterized in that: In S01, the ratio of chitosan to nano-silica, silane coupling agent and epichlorohydrin is 80-120g:5-15g:10-20mL:30-150g, preferably 100g:5-15g:10-20mL:50-150g, and more preferably 100g:5-15g:10-20mL:80-120g.

6. The process for preparing the flame retardant acrylic yarn according to any one of claims 1 to 5, characterized in that: In S01, in the flame retardant solution, the content of the modified chitosan is 1-10%, and the content of Tween 80 is 0.5-2%; preferably, the content of the modified chitosan is 3-8%, and the content of Tween 80 is 0.5-1%.

7. The process for preparing the flame retardant acrylic yarn according to any one of claims 1 to 6, characterized in that: S01 also includes a brominated flame retardant.

8. The process for preparing the flame retardant acrylic yarn according to any one of claims 1 to 7, characterized in that: In S01, in the flame retardant solution, the weight ratio of the modified chitosan to the brominated flame retardant is (0.5-1):(1-3), preferably 1:(1-2).

9. A flame-retardant acrylic yarn obtained according to the preparation process of the flame-retardant acrylic yarn according to any one of claims 1 to 8.

10. A flame-retardant fabric woven from the flame-retardant acrylic yarn according to claim 9.

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