Anti-ultraviolet nylon fiber applied to sunscreen clothes and preparation method of anti-ultraviolet nylon fiber

By irradiation grafting and cross-linking reaction on nylon 66 fibers, 2-hydroxybenzophenone is introduced to form anti-ultraviolet nylon fibers, which solves the problem of poor UV resistance of traditional nylon fiber fabrics and achieves efficient UV absorbs and shields, and ensures the fiber's long-lasting UV resistance.

CN119392398AInactive Publication Date: 2025-02-07YUNNAN MAIDING TECHNOLOGY CO LTD
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Patent Information

Application Number
CN202411775875.9
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-12-05
Publication Date
2025-02-07
Estimated Expiration
Not applicable · inactive patent

AI Technical Summary

Technical Problem

Traditional nylon fiber fabric apparel is not good in terms of UV radiation resistance, and UV absorbers are easily separated and dissolved during long-term wear and washing, resulting in a degradation in UV radiation resistance.

Method used

Glycidyl methacrylate was introduced on the surface of nylon 66 fibers by irradiation grafting, and 2-hydroxybenzophenone was chemically grafted onto nylon 66 fibers by crosslinking reaction to form 2-hydroxybenzophenone linkage Branch nylon 66 fibers were then prepared by melt spinning and traction stretching.

Benefits of technology

This method makes nylon 66 fiber have significant absorption and shielding effects in ultraviolet rays, and uses chemical graft to covalently bind the UV absorber to the fiber, avoiding the problem of separation and dissolution during washing and long-term wear. , thereby improving the fiber's long-lasting UV resistance.

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Abstract

The invention relates to the technical field of sunscreen clothes, and discloses an anti-ultraviolet nylon fiber applied to sunscreen clothes, glycidyl methacrylate is grafted and introduced on the surface of nylon 66 through an irradiation grafting method, so that abundant epoxy groups are introduced, and 2-hydroxybenzophenone is chemically grafted to the surface of nylon 66 under the crosslinking action of hexamethylenediamine, so that the anti-ultraviolet nylon fiber applied to the sunscreen clothes is obtained. 2-hydroxybenzophenone grafted nylon 66 is obtained, then the 2-hydroxybenzophenone grafted nylon 66 is compounded with nylon 66, the anti-ultraviolet nylon fiber is obtained through melt spinning and traction stretching treatment, the anti-ultraviolet nylon fiber serves as a garment material to be applied to sun protection garments, the 2-hydroxybenzophenone grafted with the nylon 66 fiber has very strong ultraviolet absorption and ultraviolet shielding effects, and the anti-ultraviolet nylon fiber is prepared through a chemical grafting method. 2-hydroxybenzophenone and nylon 66 fiber are combined through chemical covalent bonds, so that the nylon 66 fiber garment material is endowed with excellent ultraviolet protection performance and lasting ultraviolet resistance.
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Description

Technical Field

[0001] The invention relates to the technical field of sun-proof clothing, in particular to an anti-ultraviolet nylon fiber applied to sun-proof clothing and a preparation method thereof. Background Art

[0002] Sun protection clothing has excellent UV shielding and UV absorption effects. Usually, UV absorbers are added to the fabric to improve the reflection and shielding effect of the clothing surface on UV rays, thereby preventing UV rays from passing through the clothes and harming human skin. Traditional sun protection clothing is usually made of polyester fibers, nylon fibers, etc. Among them, nylon fibers have good elasticity, wear resistance, color fastness and other advantages, which makes nylon fibers have important applications in clothing and accessories.

[0003] Traditional nylon fibers do not have the function of UV absorption and UV shielding. The fabrics and clothing made of nylon fibers have low anti-UV radiation effect. Therefore, it is necessary to modify the nylon fibers and introduce functional small molecules with UV absorption and UV shielding effects, such as 2-dihydroxybenzophenone, salicylic acid ester and other UV absorbing small molecules. However, if these UV absorbers are added to nylon fiber fabrics and clothing only through physical blending, the UV absorbers will easily separate and dissolve from the fabrics and clothing during long-term wearing and washing, which greatly reduces the anti-UV radiation performance of nylon fiber fabrics and clothing. Summary of the invention

[0004] In view of the deficiencies in the prior art, the present invention provides an anti-ultraviolet nylon fiber for use in sun-protective clothing and a preparation method, which solves the problem that traditional nylon fiber fabric clothing has low anti-ultraviolet performance.

[0005] To achieve the above object, the present invention provides the following technical solution: an anti-ultraviolet nylon fiber used in sun protection clothing, wherein the preparation method of the anti-ultraviolet nylon fiber comprises the following steps: (1) Sodium hydroxide, 2,4-dihydroxybenzophenone and epichlorohydrin are added to distilled water, stirred to dissolve, reacted at 85-95°C for 2-6 hours, distilled under reduced pressure, washed with ethanol and purified by recrystallization to obtain epoxy 2-hydroxybenzophenone.

[0006] (2) Add nylon 66 and glycidyl methacrylate to distilled water and methanol solvents, stir evenly, place in an irradiation tube, and perform irradiation grafting in a nitrogen atmosphere. Distill the solution under reduced pressure to remove the solvent, then add acetone solvent, and extract and purify with a Soxhlet extractor to obtain glycidyl methacrylate grafted nylon 66.

[0007] (3) Adding glycidyl methacrylate grafted nylon 66, epoxy 2-hydroxybenzophenone and a crosslinking agent hexamethylenediamine to an N,N-dimethylformamide solvent to carry out a crosslinking reaction, adding distilled water for precipitation and washing, and then adding acetone solvent, extracting and purifying by a Soxhlet extractor to obtain 2-hydroxybenzophenone grafted nylon 66.

[0008] (4) placing nylon 66 and 2-hydroxybenzophenone grafted nylon 66 in a melt spinning machine for melt spinning to obtain primary nylon fibers, and then subjecting the primary nylon fibers to a traction, stretching and shaping treatment to obtain 2-hydroxybenzophenone grafted UV-resistant nylon fibers.

[0009] Preferably, the mass ratio of nylon 66 to glycidyl methacrylate in step (1) is 10:80-140.

[0010] Preferably, in step (3), the mass ratio of glycidyl methacrylate grafted nylon 66, epoxy 2-hydroxybenzophenone and hexamethylenediamine is 100:60-150:25-70.

[0011] Preferably, the temperature of the cross-linking reaction in step (3) is 35-60°C, and the reaction time is 6-12 h.

[0012] Preferably, the mass ratio of nylon 66 to 2-hydroxybenzophenone grafted nylon 66 in step (4) is 100:0.5-3.

[0013] Preferably, the melt spinning temperature in step (4) is 265-275° C., and the spinning rate is 8-15 m / s.

[0014] Preferably, the stretching ratio in step (4) is 2.5-4 times, and the stretching rate is 3-4 m / s.

[0015] Compared with the prior art, the present invention has the following beneficial technical effects: The invention discloses an anti-ultraviolet nylon fiber for sunscreen clothing. The invention introduces glycidyl methacrylate onto the surface of nylon 66 by irradiation grafting, thereby introducing abundant epoxy groups. Then, two amino groups of hexamethylenediamine react with epoxy 2-hydroxybenzophenone and epoxy groups grafted onto nylon 66 respectively. Thus, under the crosslinking effect of hexamethylenediamine, 2-hydroxybenzophenone is chemically grafted onto the surface of nylon 66 to obtain 2-hydroxybenzophenone grafted nylon 66. Then, 2-hydroxybenzophenone grafted nylon 66 is grafted onto nylon 66. The 2-hydroxybenzophenone grafted onto nylon 66 fiber has strong UV absorption and UV shielding effects, and the 2-hydroxybenzophenone is chemically covalently bonded to the nylon 66 fiber through a chemical grafting method, making it difficult to separate and dissolve 2-hydroxybenzophenone from the nylon 66 fiber clothing fabric, thereby giving the nylon 66 fiber clothing fabric excellent UV protection performance and lasting UV resistance. DETAILED DESCRIPTION

[0016] To achieve the above object, the present invention provides the following specific implementation methods and examples: A method for preparing UV-resistant nylon fiber comprises the following steps: (1) Sodium hydroxide, 2,4-dihydroxybenzophenone and epichlorohydrin are added to distilled water, stirred to dissolve, reacted at 85-95°C for 2-6 hours, distilled under reduced pressure, washed with ethanol and purified by recrystallization to obtain epoxy 2-hydroxybenzophenone.

[0017] (2) Add nylon 66 and glycidyl methacrylate in a mass ratio of 10:80-140 to distilled water and methanol solvent, stir evenly, place in an irradiation tube, and perform irradiation grafting in a nitrogen atmosphere. Distill the solution under reduced pressure to remove the solvent, then add acetone solvent, and extract and purify with a Soxhlet extractor to obtain glycidyl methacrylate grafted nylon 66.

[0018] (3) Add methacrylate-glycidyl grafted nylon 66, epoxy 2-hydroxybenzophenone and crosslinking agent hexamethylenediamine in a mass ratio of 100:60-150:25-70 to N,N-dimethylformamide solvent, carry out crosslinking reaction at 35-60 °C for 6-12 h, add distilled water for precipitation and washing, then add acetone solvent, extract and purify by Soxhlet extractor to obtain 2-hydroxybenzophenone grafted nylon 66.

[0019] (4) Nylon 66 and 2-hydroxybenzophenone grafted nylon 66 in a mass ratio of 100:0.5-3 are placed in a melt spinning machine for melt spinning at a temperature of 265-275 °C and a spinning rate of 8-15 m / s to obtain spun nylon fibers. The spun nylon fibers are then subjected to a drawing and stretching treatment with a drawing and stretching ratio of 2.5-4 times and a stretching rate of 3-4 m / s to obtain 2-hydroxybenzophenone grafted UV-resistant nylon fibers. Example 1

[0020] (1) Sodium hydroxide, 2,4-dihydroxybenzophenone and epichlorohydrin were added to distilled water, stirred to dissolve, reacted at 85 °C for 2 h, and distilled under reduced pressure. The mixture was washed with ethanol and purified by recrystallization to obtain epoxy 2-hydroxybenzophenone.

[0021] (2) Add nylon 66 and glycidyl methacrylate in a mass ratio of 10:80 to distilled water and methanol solvent, stir evenly, place in an irradiation tube, and perform irradiation grafting in a nitrogen atmosphere. Distill the solution under reduced pressure to remove the solvent, then add acetone solvent, and extract and purify with a Soxhlet extractor to obtain glycidyl methacrylate grafted nylon 66.

[0022] (3) Glycidyl methacrylate grafted nylon 66, epoxy 2-hydroxybenzophenone and crosslinking agent hexamethylenediamine in a mass ratio of 100:60:25 were added to N,N-dimethylformamide solvent, and the crosslinking reaction was carried out at 35 °C for 6 h. Distilled water was added for precipitation and washing, and then acetone solvent was added. The 2-hydroxybenzophenone grafted nylon 66 was extracted and purified by Soxhlet extractor to obtain 2-hydroxybenzophenone grafted nylon 66.

[0023] (4) Nylon 66 and 2-hydroxybenzophenone grafted nylon 66 in a mass ratio of 100:0.5 were placed in a melt spinning machine for melt spinning at a temperature of 265 °C and a spinning rate of 8 m / s to obtain spun nylon fibers. The spun nylon fibers were then subjected to a drawing and stretching treatment with a drawing and stretching ratio of 2.5 times and a stretching rate of 3 m / s to obtain 2-hydroxybenzophenone grafted UV-resistant nylon fibers. Example 2

[0024] (1) Sodium hydroxide, 2,4-dihydroxybenzophenone and epichlorohydrin were added to distilled water, stirred to dissolve, reacted at 85 °C for 6 h, and distilled under reduced pressure. The mixture was washed with ethanol and purified by recrystallization to obtain epoxy 2-hydroxybenzophenone.

[0025] (2) Add nylon 66 and glycidyl methacrylate in a mass ratio of 10:100 to distilled water and methanol solvent, stir evenly, place in an irradiation tube, and perform irradiation grafting in a nitrogen atmosphere. Distill the solution under reduced pressure to remove the solvent, then add acetone solvent, and extract and purify with a Soxhlet extractor to obtain glycidyl methacrylate grafted nylon 66.

[0026] (3) Glycidyl methacrylate grafted nylon 66, epoxy 2-hydroxybenzophenone and crosslinking agent hexamethylenediamine in a mass ratio of 100:80:35 were added to N,N-dimethylformamide solvent, and the crosslinking reaction was carried out at 50 °C for 6 h. Distilled water was added for precipitation and washing, and then acetone solvent was added. The 2-hydroxybenzophenone grafted nylon 66 was extracted and purified by Soxhlet extractor to obtain 2-hydroxybenzophenone grafted nylon 66.

[0027] (4) Nylon 66 and 2-hydroxybenzophenone grafted nylon 66 in a mass ratio of 100:1 were placed in a melt spinning machine for melt spinning at a temperature of 275 °C and a spinning rate of 8 m / s to obtain spun nylon fibers. The spun nylon fibers were then subjected to a drawing and stretching treatment with a drawing and stretching ratio of 3 times and a stretching rate of 3 m / s to obtain 2-hydroxybenzophenone grafted UV-resistant nylon fibers. Example 3

[0028] (1) Sodium hydroxide, 2,4-dihydroxybenzophenone and epichlorohydrin were added to distilled water, stirred to dissolve, reacted at 90 °C for 4 h, and distilled under reduced pressure. The mixture was washed with ethanol and purified by recrystallization to obtain epoxy 2-hydroxybenzophenone.

[0029] (2) Add nylon 66 and glycidyl methacrylate in a mass ratio of 10:110 to distilled water and methanol solvent, stir evenly, place in an irradiation tube, and perform irradiation grafting in a nitrogen atmosphere. Distill the solution under reduced pressure to remove the solvent, then add acetone solvent, and extract and purify with a Soxhlet extractor to obtain glycidyl methacrylate grafted nylon 66.

[0030] (3) Glycidyl methacrylate grafted nylon 66, epoxy 2-hydroxybenzophenone and crosslinking agent hexamethylenediamine in a mass ratio of 100:100:45 were added to N,N-dimethylformamide solvent, and the crosslinking reaction was carried out at 50 °C for 10 h. Distilled water was added for precipitation and washing, and then acetone solvent was added. The product was extracted and purified by Soxhlet extractor to obtain 2-hydroxybenzophenone grafted nylon 66.

[0031] (4) Nylon 66 and 2-hydroxybenzophenone grafted nylon 66 in a mass ratio of 100:2 were placed in a melt spinning machine for melt spinning at a temperature of 270 °C and a spinning rate of 10 m / s to obtain spun nylon fibers. The spun nylon fibers were then subjected to a drawing and stretching treatment with a drawing and stretching ratio of 3 times and a stretching rate of 3.5 m / s to obtain 2-hydroxybenzophenone grafted UV-resistant nylon fibers. Example 4

[0032] (1) Sodium hydroxide, 2,4-dihydroxybenzophenone and epichlorohydrin were added to distilled water, stirred to dissolve, reacted at 95 °C for 4 h, and distilled under reduced pressure. The mixture was washed with ethanol and purified by recrystallization to obtain epoxy 2-hydroxybenzophenone.

[0033] (2) Add nylon 66 and glycidyl methacrylate in a mass ratio of 10:125 to distilled water and methanol solvent, stir evenly, place in an irradiation tube, and perform irradiation grafting in a nitrogen atmosphere. Distill the solution under reduced pressure to remove the solvent, then add acetone solvent, and extract and purify with a Soxhlet extractor to obtain glycidyl methacrylate grafted nylon 66.

[0034] (3) Glycidyl methacrylate grafted nylon 66, epoxy 2-hydroxybenzophenone and crosslinking agent hexamethylenediamine in a mass ratio of 100:135:60 were added to N,N-dimethylformamide solvent, and the crosslinking reaction was carried out at 60 °C for 12 h. Distilled water was added for precipitation and washing, and then acetone solvent was added. The 2-hydroxybenzophenone grafted nylon 66 was extracted and purified by Soxhlet extractor to obtain 2-hydroxybenzophenone grafted nylon 66.

[0035] (4) Nylon 66 and 2-hydroxybenzophenone grafted nylon 66 in a mass ratio of 100:2.5 were placed in a melt spinning machine for melt spinning at a temperature of 275 °C and a spinning rate of 12 m / s to obtain spun nylon fibers. The spun nylon fibers were then subjected to a drawing and stretching treatment with a drawing and stretching ratio of 4 times and a stretching rate of 3.5 m / s to obtain 2-hydroxybenzophenone grafted UV-resistant nylon fibers. Example 5

[0036] (1) Sodium hydroxide, 2,4-dihydroxybenzophenone and epichlorohydrin were added to distilled water, stirred to dissolve, reacted at 95 °C for 6 h, distilled under reduced pressure, washed with ethanol and purified by recrystallization to obtain epoxy 2-hydroxybenzophenone.

[0037] (2) Add nylon 66 and glycidyl methacrylate in a mass ratio of 10:140 to distilled water and methanol solvent, stir evenly, place in an irradiation tube, and perform irradiation grafting in a nitrogen atmosphere. Distill the solution under reduced pressure to remove the solvent, then add acetone solvent, and extract and purify with a Soxhlet extractor to obtain glycidyl methacrylate grafted nylon 66.

[0038] (3) Glycidyl methacrylate grafted nylon 66, epoxy 2-hydroxybenzophenone and crosslinking agent hexamethylenediamine in a mass ratio of 100:150:70 were added to N,N-dimethylformamide solvent, and the crosslinking reaction was carried out at 35 °C for 12 h. Distilled water was added for precipitation and washing, and then acetone solvent was added. The 2-hydroxybenzophenone grafted nylon 66 was extracted and purified by Soxhlet extractor to obtain 2-hydroxybenzophenone grafted nylon 66.

[0039] (4) Nylon 66 and 2-hydroxybenzophenone grafted nylon 66 in a mass ratio of 100:3 were placed in a melt spinning machine for melt spinning at a temperature of 275 °C and a spinning rate of 15 m / s to obtain spun nylon fibers. The spun nylon fibers were then subjected to a drawing and stretching treatment with a drawing and stretching ratio of 4 times and a stretching rate of 4 m / s to obtain 2-hydroxybenzophenone grafted UV-resistant nylon fibers.

Claims

1. A UV-resistant nylon fiber, characterized in that: The preparation method of the anti-ultraviolet nylon fiber comprises the following steps: (1) Adding sodium hydroxide, 2,4-dihydroxybenzophenone and epichlorohydrin to distilled water, stirring to dissolve, reacting at 85-95°C for 2-6 hours, distilling under reduced pressure, washing with ethanol and purifying by recrystallization to obtain epoxy 2-hydroxybenzophenone; (2) Add nylon 66 and glycidyl methacrylate to distilled water and methanol solvents, stir evenly, place in an irradiation tube, and perform irradiation grafting in a nitrogen atmosphere. Distill the solution under reduced pressure to remove the solvent, then add acetone solvent, and perform extraction and purification by a Soxhlet extractor to obtain glycidyl methacrylate grafted nylon 66; (3) adding glycidyl methacrylate grafted nylon 66, epoxy 2-hydroxybenzophenone and crosslinking agent hexamethylenediamine to N,N-dimethylformamide solvent to carry out crosslinking reaction, adding distilled water for precipitation and washing, then adding acetone solvent, extracting and purifying by Soxhlet extractor to obtain 2-hydroxybenzophenone grafted nylon 66; (4) placing nylon 66 and 2-hydroxybenzophenone grafted nylon 66 in a melt spinning machine for melt spinning to obtain primary nylon fibers, and then subjecting the primary nylon fibers to a traction, stretching and shaping treatment to obtain 2-hydroxybenzophenone grafted UV-resistant nylon fibers.

2. The UV-resistant nylon fiber according to claim 1, characterized in that: The mass ratio of nylon 66 to glycidyl methacrylate in step (1) is 10:80-140.

3. The UV-resistant nylon fiber according to claim 1, characterized in that: The mass ratio of glycidyl methacrylate grafted nylon 66, epoxy 2-hydroxybenzophenone and hexamethylenediamine in the step (3) is 100:60-150:25-70.

4. The UV-resistant nylon fiber according to claim 1, characterized in that: The temperature of the cross-linking reaction in step (3) is 35-60°C, and the reaction time is 6-12 hours.

5. The UV-resistant nylon fiber according to claim 1, characterized in that: The mass ratio of nylon 66 to 2-hydroxybenzophenone grafted nylon 66 in step (4) is 100:0.5-3.

6. The UV-resistant nylon fiber according to claim 1, characterized in that: The melt spinning temperature in step (4) is 265-275°C, and the spinning rate is 8-15 m / s.

7. The UV-resistant nylon fiber according to claim 1, characterized in that: The stretching ratio in step (4) is 2.5-4 times, and the stretching rate is 3-4 m / s.

Citation Information

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