Preparation method of anti-ultraviolet modified polyester fabric

Abstract

The present invention relates to the technical field of fabrics, and discloses a preparation method of an anti-ultraviolet modified polyester fabric. The present invention uses bis(3-chloropropyl)amine and allyltriethoxysilane as raw materials, undergoes Michael addition to obtain intermediate 1, and then undergoes ring-opening reaction with 1,3-propane sultone to obtain intermediate 2. Intermediate 2 is used twice to successively carry out substitution reaction and quaternization reaction with 2,4-dihydroxybenzophenone and modified ferulic acid to obtain bisbenzophenone quaternary salt and ferulic acid ester triple quaternary salt. The anti-ultraviolet modified polyester fabric is obtained by condensing the siloxy groups contained in the ferulic acid ester triple quaternary salt and the bisbenzophenone quaternary salt with the hydroxyl groups contained in the polyester fabric treated with alkali.

Description

Technical Field

[0001] The present invention relates to the technical field of fabrics, and particularly to a preparation method of an anti-ultraviolet modified polyester fabric. Background Art

[0002] With the increasing awareness of ultraviolet protection among people, the demand for anti-ultraviolet functional fabrics is becoming more and more urgent. Textiles can resist ultraviolet radiation to protect the human body. However, high-intensity or long-term ultraviolet radiation will induce the photodegradation reaction of textile materials, reduce the mechanical properties, and shorten the service life. Based on this, anti-ultraviolet fabrics are favored by people. Polyester fabrics have anti-ultraviolet ability, but with the development of society, traditional polyester fabrics cannot meet people's needs.

[0003] Polyester fabrics have good physical and chemical stability and low cost, but they have poor hygroscopicity, giving people a stuffy feeling, which seriously affects their application in the clothing field. Therefore, it is necessary to modify their surface to improve the hydrophilic and moisture-absorbing properties. In addition, polyester fabrics are prone to generating static electricity, and due to the static electricity, a large amount of bacteria in the air are adsorbed, which is harmful to human health. Therefore, it is necessary to modify polyester fabrics to solve the above problems.

[0004] Ferulic acid is a phenolic acid widely present in plants, widely present in important plants such as corn, beet, and angelica, and has strong antioxidant, anti-ultraviolet, antibacterial and other properties. However, the poor water solubility of ferulic acid limits its application in the fields of food, cosmetics, medicine, etc. Therefore, it can be modified to enhance its hydrophilicity to expand the application range of ferulic acid. Summary of the Invention

[0005] (I) Technical Problems to be Solved

[0006] In view of the deficiencies of the prior art, the present invention provides a preparation method of an anti-ultraviolet modified polyester fabric, and the prepared polyester fabric has excellent anti-ultraviolet effect, antibacterial ability and hydrophilic property.

[0007] (II) Technical Solutions

[0008] A preparation method of an anti-ultraviolet modified polyester fabric, the preparation method comprising the following steps:

[0009] (1) Add bis(3-chloropropyl)amine and allyl triethoxysilane to a flask containing methanol solvent, stir and disperse, heat up to 30-40 °C, react for 3-6 h, after the reaction is completed, extract with ether, distill under reduced pressure, and dry to obtain intermediate 1;

[0010] (2) Add intermediate 1 to isopropanol solvent, stir and mix evenly. Control the temperature at 60 - 70 °C, add 1,3 - propane sultone thereto, and react at a constant temperature for 3 - 5 h. After the reaction is completed, perform rotary evaporation, wash with petroleum ether, filter by suction, and dry to obtain intermediate 2;

[0011] (3) Add 2,4 - dihydroxybenzophenone to an aqueous sodium hydroxide solution, stir to dissolve. Under a nitrogen atmosphere, add intermediate 2 thereto, control the reaction temperature at 80 - 90 °C, react for 3 - 5 h. After the reaction is completed, wash with deionized water and dry to obtain bis - benzophenone - based quaternary ammonium salt;

[0012] (4) Prepare an 80% ethanol - aqueous solution, add 2.5 - 5 wt% of ferulic acid ester tri - quaternary ammonium salt and 2.5 - 5 wt% of bis - benzophenone - based quaternary ammonium salt thereto, adjust the pH to 3 - 4 using glacial acetic acid, stir at room temperature for 30 - 60 min. Immerse the alkali - treated polyester fabric in it for 10 min according to a bath ratio of 50:1, take it out and dry to obtain the anti - ultraviolet modified polyester fabric.

[0013] Preferably, in the step (1), the molar ratio of bis(3 - chloropropyl)amine to allyl triethoxysilane is 1:1 - 1.2.

[0014] Preferably, in the step (2), the molar ratio of intermediate 1 to 1,3 - propane sultone is 1:1 - 1.2.

[0015] Preferably, in the step (3), the molar ratio of 2,4 - dihydroxybenzophenone to intermediate 2 is 2 - 2.4:1.

[0016] Preferably, in the step (4), the preparation method of the ferulic acid ester tri - quaternary ammonium salt includes the following steps:

[0017] A1. Add ferulic acid and p - toluenesulfonic acid to a flask equipped with cyclohexane solvent, stir and disperse, then add triethanolamine thereto, control the reaction temperature at 85 - 95 °C, react for 2 - 5 h. After the reaction is completed, neutralize to neutral with a 10% mass - fraction sodium bicarbonate solution, wash with saturated brine, separate the liquid, extract, and perform rotary evaporation to obtain modified ferulic acid;

[0018] A2. Add intermediate 2 and modified ferulic acid to a flask equipped with N,N - dimethylformamide solvent, stir and disperse, control the reaction temperature at 70 - 80 °C, react for 6 - 10 h. After the reaction is completed, perform vacuum distillation, wash successively with a 10% mass - fraction hydrochloric acid and deionized water, and dry to obtain the ferulic acid ester tri - quaternary ammonium salt.

[0019] Further preferably, in A1, the molar ratio of ferulic acid to triethanolamine is 4 - 6:1.

[0020] Further preferably, in A1, the dosage of p-toluenesulfonic acid is 10% of the mass of ferulic acid.

[0021] Further preferably, in A2, the molar ratio of intermediate 2 to modified ferulic acid is 1:2 - 2.4.

[0022] (III) Beneficial technical effects

[0023] In the present invention, using bis(3-chloropropyl)amine and allyltriethoxysilane as raw materials, through Michael addition, intermediate 1 is obtained. Then, it undergoes a ring-opening reaction with 1,3-propane sultone to obtain intermediate 2. Intermediate 2 is used twice to successively carry out substitution reactions and quaternization reactions with 2,4-dihydroxybenzophenone and modified ferulic acid to obtain bisbenzophenone quaternary salt and ferulic acid ester triquaternary salt. The siloxy groups contained in the ferulic acid ester triquaternary salt and bisbenzophenone quaternary salt are condensed with the hydroxyl groups contained in the polyester fabric treated with alkali to obtain an anti-ultraviolet modified polyester fabric.

[0024] In the present invention, the siloxy groups contained in the ferulic acid ester triquaternary salt and bisbenzophenone quaternary salt are condensed with the hydroxyl groups contained in the polyester fabric treated with alkali, grafting the ferulic acid ester triquaternary salt and bisbenzophenone quaternary salt onto the surface of the polyester fabric. The unreacted siloxane bonds are condensed with each other to form a cross-linked network structure on the fabric surface. When subjected to external stress, the stress can be dispersed through the cross-linking sites, thereby improving the mechanical properties of the polyester fabric.

[0025] The polyester fabric prepared in the present invention has a quaternary ammonium salt structure on its surface. The positively charged quaternary ammonium salt can be adsorbed onto negatively charged bacteria through electrostatic interaction, disturbing the charge distribution on the surface of the bacteria, affecting the normal activity of the cell membrane, and hindering the synthesis of bacterial proteins, achieving the effect of sterilization and antibacterial. The ferulic acid structure contained therein can destroy the permeability of the bacterial cell membrane, resulting in the leakage of the contents, achieving the effect of sterilization and antibacterial. The two work together to improve the sterilization and antibacterial performance of the polyester fabric.

[0026] In addition, the polyester fabric prepared in the present invention contains many hydrophilic groups such as hydroxyl groups, sulfonic acid groups, and quaternary ammonium salt groups, which can absorb moisture and improve the hydrophilic and moisture-absorbing effect of the polyester fabric. The ferulic acid structure and benzophenone structure contained therein, as ultraviolet absorption structures, can absorb high-energy ultraviolet rays and convert the energy into harmless heat energy, chemical energy, etc. for release, thereby improving the anti-ultraviolet effect of the fabric. Description of the drawings

[0027] Figure 1 is the reaction route of intermediate 2;

[0028] Figure 2 is the reaction route of bisbenzophenone quaternary salt;

[0029] Figure 3 It is the reaction route of ferulic acid ester triple quaternary ammonium salt. Specific implementation manners

[0030] To make the objectives, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. Apparently, the described embodiments are some but not all of the embodiments of the present invention. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without making creative efforts shall fall within the protection scope of the present invention.

[0031] Preparation method of alkali-treated polyester fabric: Prepare a 200 g / L sodium hydroxide solution according to a bath ratio of 50:1, control the temperature at 80 °C, add the polyester fabric thereto, stir for 30 min, take it out, wash it with deionized water until the pH is 7, and dry it to obtain the alkali-treated polyester fabric.

[0032] Example 1

[0033] (1) Add 50 mmol of bis(3-chloropropyl)amine and 60 mmol of allyl triethoxysilane to a flask containing methanol solvent, stir and disperse, heat up to 35 °C, react for 3 h. After the reaction, extract with ether, distill under reduced pressure, and dry to obtain Intermediate 1.

[0034] (2) Add 50 mmol of Intermediate 1 to isopropanol solvent, stir and mix evenly, control the temperature at 60 °C, add 60 mmol of 1,3-propane sultone thereto, react at a constant temperature for 4 h. After the reaction, perform rotary evaporation, wash with petroleum ether, filter by suction, and dry to obtain Intermediate 2.

[0035] (3) Add 48 mmol of 2,4-dihydroxybenzophenone to a 10% aqueous sodium hydroxide solution, stir to dissolve, and under a nitrogen atmosphere, add 20 mmol of Intermediate 2 thereto, control the reaction temperature at 85 °C, react for 5 h. After the reaction, wash with deionized water and dry to obtain bisbenzophenone-based quaternary ammonium salt.

[0036] (4) Add 100 mmol of ferulic acid and 10% of p-toluenesulfonic acid based on the mass of ferulic acid to a flask containing cyclohexane solvent, stir and disperse, then add 20 mmol of triethanolamine thereto, control the reaction temperature at 90 °C, react for 3 h. After the reaction, neutralize to neutral with a 10% sodium bicarbonate solution, wash with saturated brine, separate the liquid, extract, and perform rotary evaporation to obtain modified ferulic acid.

[0037] (5) 20 mmol of intermediate 2 and 45 mmol of modified ferulic acid were added to a flask containing N,N-dimethylformamide solvent, stirred and dispersed, the reaction temperature was controlled at 80 °C, and the reaction was carried out for 10 h. After the reaction, distillation under reduced pressure was carried out, and washing was carried out successively with 10% hydrochloric acid by mass and deionized water, and then drying was carried out to obtain ferulic acid ester triple quaternary ammonium salt.

[0038] (6) An 80% ethanol aqueous solution was prepared, 2.5 wt% of ferulic acid ester triple quaternary ammonium salt and 2.5 wt% of bisbenzophenone quaternary ammonium salt were added thereto, the pH was adjusted to 4 with glacial acetic acid, and stirring was carried out at room temperature for 40 min. The alkali-treated polyester fabric was immersed therein at a bath ratio of 50:1 for 10 min, taken out and dried to obtain an anti-ultraviolet modified polyester fabric.

[0039] Example 2

[0040] (1) 50 mmol of bis(3-chloropropyl)amine and 50 mmol of allyl triethoxysilane were added to a flask containing methanol solvent, stirred and dispersed, heated to 35 °C, and the reaction was carried out for 4 h. After the reaction, extraction with ether was carried out, distillation under reduced pressure was carried out, and drying was carried out to obtain intermediate 1.

[0041] (2) 50 mmol of intermediate 1 was added to isopropanol solvent, stirred and mixed evenly, the temperature was controlled at 70 °C, 50 mmol of 1,3-propane sultone was added thereto, and the reaction was carried out at a constant temperature for 5 h. After the reaction, rotary evaporation was carried out, washing with petroleum ether was carried out, suction filtration was carried out, and drying was carried out to obtain intermediate 2.

[0042] (3) 40 mmol of 2,4-dihydroxybenzophenone was added to a 10% sodium hydroxide aqueous solution by mass, stirred and dissolved, and 20 mmol of intermediate 2 was added thereto under a nitrogen atmosphere, the reaction temperature was controlled at 80 °C, and the reaction was carried out for 5 h. After the reaction, washing with deionized water was carried out, and drying was carried out to obtain bisbenzophenone quaternary ammonium salt.

[0043] (4) 120 mmol of ferulic acid and 10% of p-toluenesulfonic acid by the mass of ferulic acid were added to a flask containing cyclohexane solvent, stirred and dispersed, and then 20 mmol of triethanolamine was added thereto, the reaction temperature was controlled at 90 °C, and the reaction was carried out for 2 h. After the reaction, neutralization was carried out to neutrality with a 10% sodium bicarbonate solution by mass, washing with saturated brine was carried out, liquid separation was carried out, extraction was carried out, and rotary evaporation was carried out to obtain modified ferulic acid.

[0044] (5) 20 mmol of intermediate 2 and 48 mmol of modified ferulic acid were added to a flask containing N,N-dimethylformamide solvent, stirred and dispersed, the reaction temperature was controlled at 75 °C, and the reaction was carried out for 8 h. After the reaction, distillation under reduced pressure was carried out, and washing was carried out successively with 10% hydrochloric acid by mass and deionized water, and then drying was carried out to obtain ferulic acid ester triple quaternary ammonium salt.

[0045] (6) Prepare an 80% ethanol aqueous solution, add 3 wt% of ferulic acid ester triple quaternary ammonium salt and 3 wt% of bisbenzophenone quaternary ammonium salt thereto, adjust the pH to 3 with glacial acetic acid, stir at room temperature for 60 min, immerse the alkali-treated polyester fabric in it at a bath ratio of 50:1 for 10 min, take it out, and dry it to obtain an anti-ultraviolet modified polyester fabric.

[0046] Example 3

[0047] (1) Add 50 mmol of bis(3-chloropropyl)amine and 55 mmol of allyl triethoxysilane to a flask containing methanol solvent, stir and disperse, heat up to 40 °C, react for 5 h. After the reaction, extract with ether, distill under reduced pressure, and dry to obtain Intermediate 1.

[0048] (2) Add 50 mmol of Intermediate 1 to isopropanol solvent, stir and mix evenly, control the temperature at 65 °C, add 55 mmol of 1,3-propanesultone thereto, react at a constant temperature for 3 h. After the reaction, perform rotary evaporation, wash with petroleum ether, filter by suction, and dry to obtain Intermediate 2.

[0049] (3) Add 45 mmol of 2,4-dihydroxybenzophenone to a 10% sodium hydroxide aqueous solution by mass, stir to dissolve, under a nitrogen atmosphere, add 20 mmol of Intermediate 2 thereto, control the reaction temperature at 85 °C, react for 4 h. After the reaction, wash with deionized water and dry to obtain bisbenzophenone quaternary ammonium salt.

[0050] (4) Add 100 mmol of ferulic acid and 10% of p-toluenesulfonic acid by the mass of ferulic acid to a flask containing cyclohexane solvent, stir and disperse, then add 20 mmol of triethanolamine thereto, control the reaction temperature at 85 °C, react for 5 h. After the reaction, neutralize to neutral with a 10% sodium bicarbonate solution by mass, wash with saturated brine, separate the liquid, extract, and perform rotary evaporation to obtain modified ferulic acid.

[0051] (5) Add 20 mmol of Intermediate 2 and 40 mmol of modified ferulic acid to a flask containing N,N-dimethylformamide solvent, stir and disperse, control the reaction temperature at 80 °C, react for 8 h. After the reaction, distill under reduced pressure, wash successively with a 10% hydrochloric acid solution by mass and deionized water, and dry to obtain ferulic acid ester triple quaternary ammonium salt.

[0052] (6) Prepare an 80% ethanol aqueous solution, add 4 wt% of the ferulic acid ester triple quaternary ammonium salt and 4 wt% of the bisbenzophenone quaternary ammonium salt thereto, adjust the pH to 4 using glacial acetic acid, stir at room temperature for 30 min, immerse the alkali-treated polyester fabric therein at a bath ratio of 50:1 for 10 min, take it out, and dry it to obtain the anti-ultraviolet modified polyester fabric.

[0053] Example 4

[0054] (1) Add 50 mmol of bis(3-chloropropyl)amine and 60 mmol of allyl triethoxysilane to a flask containing methanol solvent, stir and disperse, heat up to 30 °C, react for 6 h, after the reaction is completed, extract with diethyl ether, distill under reduced pressure, and dry to obtain Intermediate 1.

[0055] (2) Add 50 mmol of Intermediate 1 to isopropanol solvent, stir and mix evenly, control the temperature at 65 °C, add 60 mmol of 1,3-propane sultone thereto, react at a constant temperature for 4 h, after the reaction is completed, perform rotary evaporation, wash with petroleum ether, filter by suction, and dry to obtain Intermediate 2.

[0056] (3) Add 48 mmol of 2,4-dihydroxybenzophenone to a 10% sodium hydroxide aqueous solution, stir to dissolve, under a nitrogen atmosphere, add 20 mmol of Intermediate 2 thereto, control the reaction temperature at 90 °C, react for 3 h, after the reaction is completed, wash with deionized water and dry to obtain the bisbenzophenone quaternary ammonium salt.

[0057] (4) Add 80 mmol of ferulic acid and 10% of p-toluenesulfonic acid by mass of ferulic acid to a flask containing cyclohexane solvent, stir and disperse, then add 20 mmol of triethanolamine thereto, control the reaction temperature at 95 °C, react for 4 h, after the reaction is completed, neutralize to neutral with a 10% sodium bicarbonate solution, wash with saturated brine, separate the liquid, extract, and perform rotary evaporation to obtain the modified ferulic acid.

[0058] (5) Add 20 mmol of Intermediate 2 and 45 mmol of the modified ferulic acid to a flask containing N,N-dimethylformamide solvent, stir and disperse, control the reaction temperature at 80 °C, react for 9 h, after the reaction is completed, distill under reduced pressure, wash successively with 10% hydrochloric acid by mass and deionized water, and dry to obtain the ferulic acid ester triple quaternary ammonium salt.

[0059] (6) Prepare an 80% ethanol aqueous solution, add 5 wt% of the ferulic acid ester triple quaternary ammonium salt and 5 wt% of the bisbenzophenone quaternary ammonium salt thereto, adjust the pH to 4 using glacial acetic acid, stir at room temperature for 50 min, immerse the alkali-treated polyester fabric therein at a bath ratio of 50:1 for 10 min, take it out, and dry it to obtain the anti-ultraviolet modified polyester fabric.

[0060] Comparative Example 1

[0061] (1) 50 mmol of bis(3-chloropropyl)amine and 60 mmol of allyltriethoxysilane were added to a flask containing methanol solvent, stirred and dispersed, heated to 35 °C, and reacted for 3 h. After the reaction, extraction was carried out with ether, followed by distillation under reduced pressure and drying to obtain Intermediate 1.

[0062] (2) 50 mmol of Intermediate 1 was added to isopropanol solvent, stirred and mixed evenly, the temperature was controlled at 60 °C, and 60 mmol of 1,3-propane sultone was added thereto. The reaction was carried out at a constant temperature for 4 h. After the reaction, rotary evaporation was carried out, followed by washing with petroleum ether, suction filtration and drying to obtain Intermediate 2.

[0063] (3) 48 mmol of 2,4-dihydroxybenzophenone was added to an aqueous sodium hydroxide solution with a mass fraction of 10%, stirred and dissolved. Under a nitrogen atmosphere, 20 mmol of Intermediate 2 was added thereto, and the reaction temperature was controlled at 85 °C. After the reaction for 5 h, washing was carried out with deionized water and drying to obtain bisbenzophenone quaternary ammonium salt.

[0064] (4) An 80% ethanol aqueous solution was prepared, 2.5 wt% of bisbenzophenone quaternary ammonium salt was added thereto, the pH was adjusted to 4 with glacial acetic acid, and it was stirred at room temperature for 40 min. The alkali-treated polyester fabric was immersed therein for 10 min according to a bath ratio of 50:1, taken out and dried to obtain a modified polyester fabric.

[0065] Comparative Example 2

[0066] (1) 50 mmol of bis(3-chloropropyl)amine and 60 mmol of allyltriethoxysilane were added to a flask containing methanol solvent, stirred and dispersed, heated to 35 °C, and reacted for 3 h. After the reaction, extraction was carried out with ether, followed by distillation under reduced pressure and drying to obtain Intermediate 1.

[0067] (2) 50 mmol of Intermediate 1 was added to isopropanol solvent, stirred and mixed evenly, the temperature was controlled at 60 °C, and 60 mmol of 1,3-propane sultone was added thereto. The reaction was carried out at a constant temperature for 4 h. After the reaction, rotary evaporation was carried out, followed by washing with petroleum ether, suction filtration and drying to obtain Intermediate 2.

[0068] (3) 100 mmol of ferulic acid and 10% of p-toluenesulfonic acid based on the mass of ferulic acid were added to a flask containing cyclohexane solvent, stirred and dispersed, and then 20 mmol of triethanolamine was added thereto. The reaction temperature was controlled at 90 °C, and the reaction was carried out for 3 h. After the reaction, it was neutralized to neutral with a 10% sodium bicarbonate solution, washed with saturated brine, separated, extracted, and rotary evaporated to obtain modified ferulic acid.

[0069] (4) 20 mmol of intermediate 2 and 45 mmol of modified ferulic acid were added to a flask containing N,N-dimethylformamide solvent, stirred and dispersed, the reaction temperature was controlled at 80 °C, and the reaction was carried out for 10 h. After the reaction, distillation under reduced pressure was carried out, and washing was carried out successively with 10% hydrochloric acid by mass and deionized water, and then dried to obtain ferulic acid ester triquaternary ammonium salt.

[0070] (5) An 80% ethanol aqueous solution was prepared, 2.5 wt% of ferulic acid ester triquaternary ammonium salt was added thereto, the pH was adjusted to 4 with glacial acetic acid, and the mixture was stirred at room temperature for 40 min. The polyester fabric after alkali treatment was immersed therein at a bath ratio of 50:1 for 10 min, taken out, and dried to obtain a modified polyester fabric.

[0071] Referring to the GB / T18830-2009 standard, the ultraviolet protection factor (UPF) was tested;

[0072] Referring to the GB / T20944.3-2008 standard, the antibacterial properties of the polyester fabric were tested, and the test strains were Escherichia coli (Ecoli, ATTCC25922) and Staphylococcus aureus (Saureus, ATCC6538).

[0073] Table 1:

[0074]

[0075] The larger the ultraviolet protection factor, the better the anti-ultraviolet effect. As can be seen from the table, the polyester fabric prepared by the present invention has good anti-ultraviolet effect and antibacterial properties.

[0076] According to the GB / T3923-1997 standard, the polyester fabric was cut into a cloth sample of 150×50 mm 2 and the breaking strength of the fabric was measured at a rate of 100 mm / min by an electronic fabric strength tester. The polyester fabrics before and after modification were subjected to ultraviolet aging experiments in an accelerated aging test machine using a fluorescent ultraviolet lamp to simulate sunlight at 60 °C and a UV radiation of 0.89 W / m 2 / nm. The polyester fabric samples were clamped in the instrument tray, taken out after being exposed to ultraviolet irradiation for 100 h, and the breaking strength was measured again.

[0077] The polyester fabric was fixed on a glass slide, and 5 μL of water droplets were injected onto the sample surface using a syringe of a contact angle measuring instrument, and the contact angle at 30 s was measured.

[0078] Table 2:

[0079]

[0080] Comparative example 3 was an unmodified polyester fabric.

[0081] The smaller the contact angle, the better the hydrophilicity. As can be seen from the table, the polyester fabric prepared by the present invention has good mechanical properties and hydrophilic effect. After 100 h of ultraviolet light irradiation, compared with Comparative Example 3 without modification, it has better anti-ultraviolet effect. And from Comparative Examples 1-2 and Examples 1-4, the polyester fabric containing both benzophenone structure and ferulic acid structure has better anti-ultraviolet effect, and with the increase of the dosage of both, the anti-ultraviolet ability and mechanical properties increase.

[0082] The above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, those of ordinary skill in the art should understand that: they can still modify the technical solutions recorded in the foregoing embodiments, or perform equivalent replacements on some of the technical features; and these modifications or replacements will not make the essence of the corresponding technical solutions deviate from the spirit and scope of the technical solutions of the embodiments of the present invention.

Claims

1. A method for preparing an anti-ultraviolet modified polyester fabric, characterized in that: The preparation method comprises the following steps: (1) Add bis(3-chloropropyl)amine and allyltriethoxysilane to a flask containing methanol solvent, stir and disperse, heat to 30-40°C, react for 3-6 hours, and after the reaction is completed, extract with ether, distill under reduced pressure, and dry to obtain intermediate 1; (2) Add intermediate 1 to isopropanol solvent, stir and mix evenly, control the temperature to 60-70°C, add 1,3-propane sultone, react at constant temperature for 3-5 hours, after the reaction is completed, rotary evaporate, wash with petroleum ether, filter and dry to obtain intermediate 2; (3) Add 2,4-dihydroxybenzophenone to a sodium hydroxide aqueous solution, stir to dissolve, add intermediate 2 thereto under a nitrogen atmosphere, control the reaction temperature to 80-90° C., react for 3-5 hours, and after the reaction is completed, wash with deionized water and dry to obtain a dibenzophenone-based quaternary ammonium salt; (4) preparing an 80% ethanol aqueous solution, adding 2.5-5wt% of ferulate triple quaternary ammonium salt and 2.5-5wt% of dibenzophenone quaternary ammonium salt thereto, adjusting the pH to 3-4 with glacial acetic acid, stirring for 30-60 minutes at room temperature, immersing the alkali-treated polyester fabric therein at a bath ratio of 50:1 for 10 minutes, taking out, and drying to obtain an anti-ultraviolet modified polyester fabric; The preparation method of the triple quaternary ammonium salt of ferulate comprises the following steps: A1. Add ferulic acid and p-toluenesulfonic acid into a flask filled with cyclohexane solvent, stir and disperse, then add triethanolamine, control the reaction temperature to 85-95° C., react for 2-5 hours, and after the reaction is completed, neutralize to neutrality with a 10% mass fraction sodium bicarbonate solution, wash with saturated brine, separate, extract, and rotary evaporate to obtain modified ferulic acid; A2. Add intermediate 2 and modified ferulic acid into a flask filled with N,N-dimethylformamide solvent, stir and disperse, control the reaction temperature to 70-80°C, react for 6-10 hours, and after the reaction is completed, distill under reduced pressure, wash with 10% hydrochloric acid and deionized water in turn, and dry to obtain a triple quaternary ammonium salt of ferulic acid ester.

2. The method for preparing the UV-resistant modified polyester fabric according to claim 1, characterized in that: In the above (1), the molar ratio of bis(3-chloropropyl)amine to allyltriethoxysilane is 1:1-1.

2.

3. The method for preparing the UV-resistant modified polyester fabric according to claim 1, characterized in that: In the above (2), the molar ratio of the intermediate 1 to 1,3-propane sultone is 1:1-1.

2.

4. The method for preparing the UV-resistant modified polyester fabric according to claim 1, characterized in that: In the above (3), the molar ratio of 2,4-dihydroxybenzophenone to intermediate 2 is 2-2.4:

1.

5. The method for preparing the UV-resistant modified polyester fabric according to claim 1, characterized in that: In the A1, the molar ratio of ferulic acid to triethanolamine is 4-6:

1.

6. The method for preparing the UV-resistant modified polyester fabric according to claim 1, characterized in that: In A1, the amount of p-toluenesulfonic acid used is 10% of the mass of ferulic acid.

7. The method for preparing the UV-resistant modified polyester fabric according to claim 1, characterized in that: In A2, the molar ratio of the intermediate 2 to the modified ferulic acid is 1:2-2.4.

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