Anti-ultraviolet moisture-absorbing fiber and preparation method and fabric thereof

Abstract

The invention relates to the technical field of fibers, and discloses an anti-ultraviolet moisture-absorbing fiber, a preparation method thereof and a fabric, and the anti-ultraviolet moisture-absorbing fiber is obtained by adding polyethylene glycol terephthalate and a polymer ultraviolet absorbent into a screw melt spinning machine for spinning and drawing by a drawing machine. The compatibility between the polymer ultraviolet absorbent and polyethylene glycol terephthalate is very good, adverse effects on the mechanical properties of polyester fibers are avoided after spinning, and a polymer molecular chain contains a 2-hydroxybenzophenone ultraviolet absorbing group, so that very good ultraviolet aging resistance is achieved, and the service life of the polyester fibers is prolonged. And the fiber after ultraviolet aging still has very high breaking strength and breaking elongation. The molecular side chain of the polymer ultraviolet absorbent contains a large number of carboxyl groups, so that the hydrophilicity and the moisture absorption rate of a fiber fabric can be improved by adding the polymer ultraviolet absorbent into polyester fibers, and the polymer ultraviolet absorbent shows higher moisture regain.

Description

Technical Field

[0001] The invention relates to the technical field of fibers, in particular to an anti-ultraviolet and moisture-absorbing fiber and a preparation method and fabric thereof. Background Art

[0002] Polyester fibers and their fabrics have good strength, elasticity and wrinkle resistance, and are widely used in clothing, building interior decoration, transportation interior decoration, etc. Traditional polyester fibers have poor hydrophilicity and low moisture absorption rate. Adding functional additives to polyester fibers can give polyester fibers and fabrics anti-ultraviolet, hydrophilic moisture absorption, antibacterial, flame retardant and other properties.

[0003] The invention patent with announcement number CN105442326B discloses a nano-composite anti-ultraviolet organic coating finishing agent and its preparation method, using polyether-based methylsiloxane-co-benzophenone derivative-based methylsiloxane-co-dimethylsiloxane copolymer, hydroxyl polyether-terminated polyethylene terephthalate, water-dispersible phenyl-modified silicon / titanium sol, etc. as raw materials to obtain a nano-composite anti-ultraviolet organic coating finishing agent, which gives polyester and other fabrics anti-ultraviolet effect and smooth and elastic feel. However, the organic coating finishing agent in this patent does not give polyester and other fabrics hydrophilic and hygroscopic properties. Summary of the invention

[0004] The invention solves the problem that the polyester fiber and the fabric have poor anti-ultraviolet performance and poor hydrophilic moisture absorption performance.

[0005] The technical solution of the present invention is: a method for preparing a fiber resistant to ultraviolet light and moisture absorption comprises:

[0006] (1) Add 4-(4,6-dichloro-1,3,5-triazine-2-oxy)-2-hydroxyphenyl benzophenone, terephthalyline ester, and N,N-diisopropylethylamine to N,N-dimethylformamide, heat and stir to react, pour the obtained solution into ethanol, precipitate, filter, wash with ethanol, and dry to obtain a polymer ultraviolet absorber. The reaction formula is:

[0007]

[0008] (2) Adding polyethylene terephthalate and a polymer UV absorber into a screw melt spinning machine for spinning, wherein the temperature of zones 1 to 4 is 275-300° C. and the spinning rate is 1800-2500 m / min; stretching is performed by a stretching machine at a stretching speed of 500-800 m / min and a stretching ratio of 2-3; and obtaining a fiber that is resistant to UV light and moisture absorption.

[0009] Preferably, in (1), the molar ratio of 4-(4,6-dichloro-1,3,5-triazine-2-oxy)-2-hydroxyphenyl benzophenone, terephthalylidene ester, and N,N-diisopropylethylamine is 1:(0.9-1.2):(2-2.4).

[0010] Preferably, in (1), the reaction temperature is 45-60°C and the reaction time is 8-12h.

[0011] Preferably, in (2), the mass ratio of polyethylene terephthalate to polymer UV absorber is 100:(1-8).

[0012] Preferably, the preparation method of terephthaloyl bisserine ester comprises: adding Boc-DL-serine (CAS registration number is 3850-40-6) at a molar ratio of (1.8-2.2): 1: (2-2.2) to dichloromethane at 0-5°C, then stirring and reacting at 15-30°C for 6-10h, distilling under reduced pressure, dissolving the product after washing with water in dichloromethane, adding trifluoroacetic acid, stirring and reacting at 20-30°C for 3-5h, distilling under reduced pressure, washing with saturated sodium bicarbonate solution, then dissolving in dichloromethane, recrystallizing and purifying to obtain terephthaloyl bisserine ester. The reaction formula is:

[0013]

[0014] Preferably, the anti-ultraviolet and moisture-absorbing Kapol fabric is made of anti-ultraviolet and moisture-absorbing fibers.

[0015] The technical effect produced by the present invention is as follows: the present invention uses Boc-DL-serine and terephthaloyl chloride as reactants to prepare terephthaloyl serine ester, which is then polymerized with 4-(4,6-dichloro-1,3,5-triazine-2-oxy)-2-hydroxyphenyl benzophenone to obtain a novel polymer ultraviolet absorber, which is then blended with polyethylene terephthalate for melt spinning to obtain ultraviolet resistant and moisture absorbing polyester fiber.

[0016] The polymer ultraviolet absorber of the present invention contains terephthalate structural units in the polymer molecular chain, has good compatibility with polyethylene terephthalate, does not cause adverse effects on the mechanical properties of polyester fibers after spinning, and has good breaking strength and breaking elongation before ultraviolet aging.

[0017] The polymer ultraviolet absorber of the present invention is a macromolecular polymer with good thermal stability. In the high-temperature melt spinning process, thermal decomposition will not occur, and the anti-ultraviolet aging performance of the ultraviolet absorber will not be affected. The polymer molecular chain contains 2-hydroxybenzophenone ultraviolet absorption groups, which can convert light energy into heat energy through the rupture of intramolecular hydrogen bonds and tautomerism, and play a good anti-ultraviolet aging performance. The fiber after ultraviolet aging still has high breaking strength and breaking elongation, and the decline is very small.

[0018] The molecular side chain of the polymer ultraviolet absorber of the present invention contains a large number of carboxyl groups, which can be added into polyester fibers to improve the hydrophilicity and moisture absorption rate of the fiber fabrics and show a higher moisture regain. DETAILED DESCRIPTION

[0019] The chemical structure of 4-(4,6-dichloro-1,3,5-triazine-2-oxy)-2-hydroxyphenylbenzophenone is:

[0020] The preparation was carried out according to the method of the literature journal "Journal of Textile Research", February 2014, Volume 35, Issue 2, "Synthesis of New Ultraviolet Absorbers and Their Application in Cotton Fabrics".

[0021] Example 1

[0022] (1) At 0°C, add 30 mmol Boc-DL-serine, 15 mmol terephthaloyl chloride, and 30 mmol triethylamine to 80 mL dichloromethane, and then stir and react at 25°C for 10 hours, evaporate under reduced pressure, wash the product with water, dissolve it in 70 mL dichloromethane, add 40 mL trifluoroacetic acid, stir and react at 25°C for 4 hours, evaporate under reduced pressure, wash with saturated sodium bicarbonate solution, and then dissolve it in dichloromethane, recrystallize and purify to obtain terephthalide serine ester.

[0023] (2) Add 30 mmol 4-(4,6-dichloro-1,3,5-triazine-2-oxy)-2-hydroxyphenyl benzophenone, 33 mmol p-phenylenedisyl ester, and 60 mmol N,N-diisopropylethylamine to 150 mL N,N-dimethylformamide, heat to 45°C, stir and react for 12 hours, pour the obtained solution into ethanol, precipitate, filter, wash with ethanol, and dry to obtain a polymer UV absorber.

[0024] (3) Add 100g of polyethylene terephthalate and 1g of a polymer UV absorber into a screw melt spinning machine for spinning. The temperatures of zones 1 to 4 are 275°C, 290°C, 300°C and 295°C, and the spinning rate is 2000m / min. The fibers are stretched in a stretching machine at a speed of 800m / min and a stretching ratio of 2.6 to obtain fibers that are resistant to UV light and moisture absorption.

[0025] Example 2

[0026] (1) Add 33 mmol Boc-DL-serine, 15 mmol terephthaloyl chloride, and 33 mmol triethylamine to 90 mL dichloromethane at 5°C, and then stir and react for 10 hours at 15°C. Distill under reduced pressure, wash the product with water, dissolve it in 70 mL dichloromethane, add 30 mL trifluoroacetic acid, stir and react for 5 hours at 20°C, distill under reduced pressure, wash with saturated sodium bicarbonate solution, and then dissolve it in dichloromethane. Recrystallize and purify to obtain terephthalide serine ester.

[0027] (2) Add 30 mmol 4-(4,6-dichloro-1,3,5-triazine-2-oxy)-2-hydroxyphenyl benzophenone, 36 mmol p-phenylenedisyl ester, and 72 mmol N,N-diisopropylethylamine to 200 mL N,N-dimethylformamide, heat to 60°C, stir and react for 8 hours, pour the obtained solution into ethanol, precipitate, filter, wash with ethanol, and dry to obtain a polymer UV absorber.

[0028] (3) Add 100 g of polyethylene terephthalate and 3 g of a polymer UV absorber into a screw melt spinning machine for spinning. The temperatures of zones 1 to 4 are 275°C, 290°C, 300°C and 295°C, and the spinning rate is 2500 m / min. The fibers are stretched in a stretching machine at a speed of 500 m / min and a stretching ratio of 2.6. The fibers are resistant to UV light and moisture absorption.

[0029] Example 3

[0030] (1) At 0°C, add 27 mmol Boc-DL-serine, 15 mmol terephthaloyl chloride, and 30 mmol triethylamine to 70 mL dichloromethane, then stir and react at 30°C for 6 h, distill under reduced pressure, wash the product with water, dissolve it in 70 mL dichloromethane, add 40 mL trifluoroacetic acid, stir and react at 30°C for 3 h, distill under reduced pressure, wash with saturated sodium bicarbonate solution, then dissolve it in dichloromethane, and purify it by recrystallization to obtain terephthalide serine ester.

[0031] (2) Add 30 mmol 4-(4,6-dichloro-1,3,5-triazine-2-oxy)-2-hydroxyphenyl benzophenone, 27 mmol p-phenylenedisyl ester, and 60 mmol N,N-diisopropylethylamine to 150 mL N,N-dimethylformamide, heat to 50°C, stir and react for 12 hours, pour the obtained solution into ethanol, precipitate, filter, wash with ethanol, and dry to obtain a polymer UV absorber.

[0032] (3) Add 100 g of polyethylene terephthalate and 5 g of a polymer UV absorber into a screw melt spinning machine for spinning. The temperatures of zones 1 to 4 are 275°C, 290°C, 300°C and 295°C, and the spinning rate is 1800 m / min. The fibers are stretched in a stretching machine at a speed of 500 m / min and a stretching ratio of 3. Thus, fibers resistant to UV and moisture absorption are obtained.

[0033] Example 4

[0034] (1) Prepare a polymer UV absorber according to the method of Example 1.

[0035] (2) Add 100 g of polyethylene terephthalate and 8 g of a polymer UV absorber into a screw melt spinning machine for spinning, wherein the temperatures of zones 1 to 4 are 275° C., 290° C., 300° C., and 295° C., and the spinning rate is 2500 m / min; the fibers are stretched by a stretching machine at a stretching speed of 600 m / min and a stretching ratio of 2; and fibers resistant to UV and moisture absorption are obtained.

[0036] Comparative Example 1

[0037] (1) Add 100 g of polyethylene terephthalate into a screw melt spinning machine for spinning, with the temperatures of zones 1 to 4 being 275° C., 290° C., 300° C., and 295° C., and the spinning rate being 2000 m / min; and stretching by a stretching machine at a stretching speed of 800 m / min and a stretching ratio of 2.6; and obtain polyester fiber.

[0038] Comparative Example 2

[0039] (1) Add 100 g of polyethylene terephthalate and 1 g of 4-(4,6-dichloro-1,3,5-triazine-2-oxy)-2-hydroxyphenyl benzophenone into a screw melt spinning machine for spinning, wherein the temperatures of zones 1 to 4 are 275° C., 290° C., 300° C., and 295° C., and the spinning rate is 2000 m / min; the fiber is stretched by a stretching machine at a stretching speed of 800 m / min and a stretching ratio of 2.6; and a fiber resistant to ultraviolet light and moisture absorption is obtained.

[0040] Comparative Example 3

[0041] (1) Add 30 mmol 4-(4,6-dichloro-1,3,5-triazine-2-oxy)-2-hydroxyphenyl benzophenone, 33 mmol p-phenylenediamine, and 60 mmol N,N-diisopropylethylamine to 150 mL N,N-dimethylformamide, heat to 45°C, stir and react for 12 hours, pour the obtained solution into ethanol, precipitate, filter, wash with ethanol, and dry to obtain a polymer UV absorber.

[0042] (2) Add 100g of polyethylene terephthalate and 1g of a polymer UV absorber into a screw melt spinning machine for spinning. The temperatures of zones 1 to 4 are 275°C, 290°C, 300°C and 295°C, and the spinning rate is 2000m / min. The fibers are stretched in a stretching machine at a speed of 800m / min and a stretching ratio of 2.6. The fibers are resistant to UV light and moisture absorption.

[0043] The mechanical properties of the fiber were tested using an electronic single fiber strength tester with a clamping distance of 10 mm and a tensile speed of 20 mm / min. Each sample was tested 10 times and the average value was taken.

[0044] The fiber was placed in a UV aging accelerated testing machine for UV aging test, with an irradiation intensity of 0.72 W / m 2 , time is 120h, wavelength is 340nm. Then the mechanical properties are tested.

[0045] Table 1 Fiber mechanical properties test

[0046]

[0047] After testing, the polyester fiber of Comparative Example 1 did not have any UV absorber added, and its breaking strength and breaking elongation before UV aging were 3.31 cN / dtex and 20.5%, with good mechanical properties. However, after UV aging, the breaking strength and breaking elongation were 2.56 cN / dtex and 17.3%, a significant decrease.

[0048] In Comparative Example 2, 4-(4,6-dichloro-1,3,5-triazine-2-oxy)-2-hydroxyphenyl benzophenone was added as a UV absorber. This substance is a small molecule compound with poor thermal stability. During the high-temperature melt spinning process, thermal decomposition occurs, which affects the UV resistance of the fiber, and the breaking strength and elongation at break decrease significantly.

[0049] Polymer ultraviolet absorbers are added to the polyester fibers of Examples 1-4. The polymer molecular chains of the ultraviolet absorbers contain terephthalate structural units, and the compatibility with polyethylene terephthalate is very good. After spinning, the mechanical properties of the polyester fibers will not be adversely affected. The breaking strength and elongation at break before ultraviolet aging are very similar to those of the polyester fibers of Comparative Example 1. In addition, as a macromolecular polymer, the polymer ultraviolet absorber has very good thermal stability. During the high-temperature melt spinning process, thermal decomposition will not occur, and the anti-ultraviolet aging performance of the ultraviolet absorber will not be affected. The polymer molecular chains contain 2-hydroxybenzophenone ultraviolet absorbing groups, which can convert light energy into heat energy through the rupture of intramolecular hydrogen bonds and tautomerism, and have good anti-ultraviolet aging performance. The fibers after ultraviolet aging still have very high breaking strength and elongation at break, and the decline is very small.

[0050] Comparative Example 3 uses 4-(4,6-dichloro-1,3,5-triazine-2-oxy)-2-hydroxyphenyl benzophenone and p-phenylenediamine as raw materials. The polymer UV absorber obtained by polymerization does not contain terephthalate structural units, and has poor compatibility with polyethylene terephthalate. After spinning, it will have an adverse effect on the mechanical properties of polyester fibers. Compared with Comparative Example 1 and Example 1, the fiber of Comparative Example 1 has significantly lower breaking strength and breaking elongation before UV aging.

[0051] The polyester fiber is woven into fabrics, and the moisture regain of the fabrics is tested according to the method of GB / T 9995-1997.

[0052] Table 2 Moisture regain test of fiber fabrics

[0053] Moisture regain (%) Example 1 0.482 Example 2 0.605 Example 3 0.982 Example 4 1.159 Comparative Example 1 0.421 Comparative Example 2 0.427 Comparative Example 3 0.405

[0054] After testing, compared with comparative example 1, the moisture regain of the fiber fabrics of Examples 1-4 is significantly increased. This is because the molecular side chains of the added polymer UV absorbers contain a large number of carboxyl groups, which can be added to the fibers to improve the hydrophilicity and moisture absorption of the fiber fabrics, thereby improving the moisture regain.

[0055] The 4-(4,6-dichloro-1,3,5-triazine-2-oxy)-2-hydroxyphenyl benzophenone added in Comparative Example 2 and the polymer UV absorber added in Comparative Example 3 do not contain hydrophilic carboxyl groups, and the hydrophilicity and moisture absorption rate of the fiber are poor, and the moisture regain is low.

Claims

1. A method for preparing a fiber that resists ultraviolet light and moisture absorption, characterized in that: The preparation method comprises: (1) Add 4-(4,6-dichloro-1,3,5-triazine-2-oxy)-2-hydroxyphenyl benzophenone, terephthalyline ester and N,N-diisopropylethylamine to N,N-dimethylformamide, heat and stir to react, pour the obtained solution into ethanol, precipitate, filter, wash and dry the precipitate to obtain a polymer ultraviolet absorber; The chemical structural formula of the terephthalate is as follows: (2) Adding polyethylene terephthalate and a polymer UV absorber into a screw melt spinning machine for spinning, and then drawing the fibers with UV resistance and moisture absorption resistance.

2. The method for preparing the fiber resistant to ultraviolet light and moisture absorption according to claim 1, characterized in that: In the above (1), the molar ratio of 4-(4,6-dichloro-1,3,5-triazine-2-oxy)-2-hydroxyphenyl benzophenone, terephthalylidene ester, and N,N-diisopropylethylamine is 1:(0.9-1.2):(2-2.4).

3. The method for preparing the fiber resistant to ultraviolet light and moisture absorption according to claim 1, characterized in that: In the step (1), the reaction temperature is 45-60°C and the reaction time is 8-12h.

4. The method for preparing the fiber resistant to ultraviolet light and moisture absorption according to claim 1, characterized in that: In the above (2), the mass ratio of polyethylene terephthalate to polymer ultraviolet absorber is 100:(1-8).

5. The method for preparing the fiber resistant to ultraviolet light and moisture absorption according to claim 1, characterized in that: In the above (2), the temperature of zones 1 to 4 of the screw melt spinning machine is 275-300° C., and the spinning rate is 1800-2500 m / min.

6. The method for preparing the fiber resistant to ultraviolet light and moisture absorption according to claim 1, characterized in that: In the above (2), the drawing speed is 500-800 m / min, and the drawing ratio is 2-3.

7. The method for preparing the fiber resistant to ultraviolet light and moisture absorption according to claim 1, characterized in that: The preparation method of the terephthalide serine ester comprises: adding Boc-DL-serine, terephthaloyl chloride and triethylamine to dichloromethane at 0-5°C, stirring and reacting for 6-10 hours at 15-30°C, distilling under reduced pressure, dissolving the product after washing in dichloromethane, adding trifluoroacetic acid, stirring and reacting for 3-5 hours at 20-30°C, distilling under reduced pressure, washing, and purifying by recrystallization to obtain the terephthalide serine ester.

8. The method for preparing the fiber resistant to ultraviolet light and moisture absorption according to claim 7, characterized in that: The molar ratio of Boc-DL-serine, terephthaloyl chloride and triethylamine is (1.8-2.2):1:(2-2.2).

9. A fiber resistant to ultraviolet light and moisture absorption prepared according to the preparation method according to any one of claims 1 to 8.

10. An anti-ultraviolet moisture absorption fabric made of the anti-ultraviolet moisture absorption fiber as claimed in claim 9.

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