阅读说明：本技术 一种高吸水性芳香涤纶织物的制备方法 (Preparation method of high-water-absorption aromatic polyester fabric ) 是由 廖国庆 于 2020-06-29 设计创作，主要内容包括：本发明公开了一种高吸水性芳香涤纶织物的制备方法,步骤为：(1)制备含有丙烯酸、N,N-亚甲基双丙烯酰胺和过硫酸铵的改性溶液；(2)将涤纶织物水洗烘干后置于紫外灯下辐照；(3)将辐照后的织物在改性溶液中浸渍并通氮气；(4)将浸渍后的织物置于紫外灯下辐照反应；(5)将反应后的织物经水和氢氧化钠溶液处理；(6)用含有pH响应芳香缓释粒子的涂层剂对改性后的织物进行涂覆；(7)将涂覆后的织物在碳酸铵溶液中浸渍后水洗烘干。本发明对涤纶织物进行吸水改性,并将pH响应芳香缓释粒子内并整理在吸水改性后的涤纶织物上,利用涤纶织物改性后的高吸水性实现通过pH的变化控制芳香抑菌剂的释放,提高了释香持久性。(The invention discloses a preparation method of a high-water-absorption aromatic polyester fabric, which comprises the following steps: (1) preparing a modified solution containing acrylic acid, N-methylene-bisacrylamide and ammonium persulfate; (2) washing and drying the polyester fabric, and then placing the polyester fabric under an ultraviolet lamp for irradiation; (3) dipping the irradiated fabric in a modified solution and introducing nitrogen; (4) placing the impregnated fabric under an ultraviolet lamp for irradiation reaction; (5) treating the reacted fabric with water and sodium hydroxide solution; (6) coating the modified fabric with a coating agent containing pH-responsive aromatic slow-release particles; (7) and soaking the coated fabric in an ammonium carbonate solution, washing with water and drying. According to the invention, the polyester fabric is subjected to water absorption modification, the pH response aromatic slow-release particles are arranged in the polyester fabric subjected to water absorption modification, and the release of the aromatic bacteriostatic agent is controlled through the change of pH by utilizing the high water absorption of the modified polyester fabric, so that the fragrance release durability is improved.)

1. The preparation method of the high-water-absorption aromatic polyester fabric is characterized by comprising the following steps of:

(1) dissolving acrylic acid and N, N-methylene bisacrylamide in water, adding ammonium persulfate, and uniformly stirring to obtain a modified solution;

(2) washing and drying the polyester fabric, and then irradiating for 20-30 min under an ultraviolet lamp;

(3) soaking the irradiated polyester fabric in a modified solution, and introducing nitrogen for 10-20 min;

(4) taking the polyester fabric out of the modified solution, and placing the polyester fabric under an ultraviolet lamp for irradiation reaction for 20-30 min;

(5) placing the polyester fabric after the irradiation reaction in water, boiling for 1-2 h, then placing in a sodium hydroxide solution, soaking for 20-30 min, washing with water and drying to obtain a water-absorbing modified polyester fabric;

(6) dispersing the pH response aromatic slow-release particles in polyacrylate emulsion to obtain a coating agent, coating the water absorption modified polyester fabric with the coating agent, and drying to obtain the polyester fabric with the sun-proof coating;

(7) putting the polyester fabric with the sun-proof coating in 0.5-1.5 g/L of Na₂CO₃And soaking the fabric in the solution for 1-2 min, and then washing and drying the fabric to obtain the high-water-absorptivity aromatic polyester fabric.

2. The preparation method of the high-water-absorption aromatic polyester fabric according to claim 1, wherein the mass fraction of acrylic acid in the modified solution in the step (1) is 6-10%, the mass fraction of N, N-methylene bisacrylamide is 2-6% o, and the mass fraction of ammonium persulfate is 1-3%.

3. The preparation method of the high water absorption aromatic polyester fabric according to claim 1, wherein the ultraviolet lamp power in the steps (2) and (4) is 400-1000W, and the irradiation distance is 10-15 cm.

4. The method for preparing the aromatic polyester fabric with high water absorption according to claim 1, wherein the concentration of the sodium hydroxide solution in the step (5) is 0.02-0.05 mol/L.

5. The method for preparing a high water absorption aromatic polyester fabric according to claim 1, wherein the method for preparing the pH response aromatic slow release particles in the step (6) comprises the following steps:

(a) dissolving hexadecylamine in absolute ethyl alcohol at the temperature of 25-30 ℃, adding 0.1-0.2 mol/L potassium chloride solution and deionized water, and uniformly stirring to obtain a guiding agent solution;

(b) dropwise adding titanium isopropoxide into the guiding agent solution under the stirring state, standing for 15-24 h, centrifuging, washing the product with ethanol, and drying to obtain TiO₂The molar ratio of the added titanium isopropoxide to the hexadecylamine in the guiding agent solution is 1: (0.1 to 0.5);

(c) adding TiO into the mixture₂Dispersing the precursor in a mixed solution of ammonia water, absolute ethyl alcohol and deionized water, reacting at 150-180 ℃ for 12-24 h, centrifuging, washing the product with ethanol, drying, and roasting at 500-510 ℃ for 2-3 h to obtain mesoporous TiO₂；

(d) Downward mesoporous TiO under the protection of nitrogen₂Adding toluene, gamma-chloropropyltrimethoxysilane and 3-glycidyl ether oxypropyltriethoxysilane, stirring at 80-120 ℃ and reacting for 20-30 h to obtain surface-modified mesoporous TiO₂Mesoporous TiO₂The mass volume ratio of the mixture to toluene, gamma-chloropropyltrimethoxysilane and 3-glycidyl ether oxypropyltriethoxysilane is 1 g: (20-30 mL): (20-30 mL): (400-600 mL);

(e) adding alanine into phosphate buffer solution with pH of 7.0, stirring uniformly, and adding surface modified mesoporous TiO₂Oscillating and reacting for 20-30 h at 50-60 ℃, filtering, washing the product with ethanol, and drying in vacuum to obtain alanine-modified mesoporous TiO₂Wherein the concentration of alanine in phosphate buffer solution is 2-4 mg/mL, and surface modified mesoporous TiO is added₂The mass volume ratio of the phosphate buffer solution to the phosphate buffer solution is 1 g: (100-200 mL);

(f) alanine modified mesoporous TiO₂Dispersing in an aromatic bacteriostatic agent, stirring at room temperature for reaction for 8-12 h, filtering, and washing with deionized water to obtain the aromatic bacteriostatic agent-loaded mesoporous TiO₂；

(g) Loading mesoporous TiO with aromatic bacteriostat₂Dispersing in N, N-dimethylformamide, stirring for 30-40 min, adding octadecyl dimethyl tertiary amine and potassium iodide under the protection of nitrogen, stirring at 40-60 ℃ for reaction for 24-36 h, filtering, washing the product with N, N-dimethylformamide, and drying in vacuum to obtain the pH response aromatic slow-release particles.

6. The method for preparing the aromatic polyester fabric with high water absorbability according to claim 5, wherein the mass-to-volume ratio of the hexadecylamine to the added absolute ethyl alcohol, the potassium chloride solution and the deionized water in the step (a) is 1 g: (80-120 mL): (0.3-0.5 mL): (1-2 mL).

7. The method for preparing the aromatic polyester fabric with high water absorbability according to claim 5, wherein the concentration of the ammonia water in the mixed solution in the step (c) is 0.1-0.2 mol/L, and the volume ratio of the absolute ethyl alcohol to the deionized water is (1-2): 1; TiO 2₂The mass volume ratio of the precursor to the mixed solution is 1 g: (18-22 mL).

8. The method for preparing the fragrant dacron fabric with high water absorbability according to claim 5, wherein the fragrant bacteriostatic agent in step (f) is rose essential oil, lemon essential oil, mint essential oil,One or more than one of blumea oil, and the alanine-modified mesoporous TiO₂The mass volume ratio of the aromatic bacteriostatic agent to the aromatic bacteriostatic agent is 1 g: (20-50 mL).

9. The method for preparing the aromatic polyester fabric with high water absorption according to claim 5, wherein the mesoporous TiO loaded with the aromatic bacteriostatic agent in the step (g)₂The mass-to-volume ratio of N, N-dimethylformamide is 1 g: (200-400 mL) of mesoporous TiO loaded with aromatic bacteriostatic agent₂The mass ratio of the organic solvent to the octadecyl dimethyl tertiary amine and the potassium iodide is 5: (9-11): (0.1-0.5).

10. The preparation method of the aromatic polyester fabric with high water absorption according to claim 1 or 5, wherein the coating agent in the step (6) comprises 10-30% of pH-responsive aromatic slow-release particles by mass, and 1-2 coating agents are coated, wherein the coating amount of the pH-responsive aromatic slow-release particles in each coating is 1-3% of the weight of the polyester fabric.

Technical Field

The invention relates to the technical field of functional fabrics, in particular to a preparation method of a high-water-absorptivity aromatic polyester fabric.

Background

Polyester is a synthetic fiber obtained by spinning polyester formed by polycondensation of organic dibasic acid and dihydric alcohol, has light weight, good corrosion resistance, good mechanical property and chemical stability, and good crease elasticity and stiffness, and is widely used as textile fabrics. However, because only two hydroxyl groups are arranged at two ends of the polyester macromolecules, the polyester fabric is hydrophobic, does not absorb moisture and conduct moisture, and is poor in wearing comfort.

In order to prolong the fragrance releasing time of the fragrant fabric in the prior art, the fragrance is generally coated in the microcapsule and is finished on the fabric, and the volatilization of the fragrance is protected by the microcapsule, so that the fragrance has a slow release effect, and the fragrance releasing durability of the fabric is prolonged. However, the method of prolonging the fragrance release durability of the fragrance in the fabric by the microcapsule is difficult to control and regulate the release of the fragrance, the fragrance is continuously volatilized even if the clothes are not put on, the fragrance is lost, and the effect of prolonging the fragrance retention time is still limited.

Disclosure of Invention

The invention provides a preparation method of a high-water-absorption aromatic polyester fabric, aiming at overcoming the problems of poor moisture absorption of the polyester fabric, poor wearing comfort, more volatilization loss of an aromatic agent in the aromatic fabric and pending improvement of fragrance release durability in the prior art, the invention polymerizes a water absorption layer with a three-dimensional net structure on the surface of the polyester fabric, so that the polyester fabric has good moisture absorption performance, and loads a fragrant bacteriostatic agent in pH response fragrant slow-release particles and arranges the fragrant bacteriostatic agent on the polyester fabric after water absorption modification, and the release of the fragrant bacteriostatic agent is controlled by the change of pH by utilizing the high water absorption of the modified polyester fabric, thereby avoiding the volatilization loss of the fragrant bacteriostatic agent when clothes are not worn, and improving the fragrance release durability of the polyester fabric.

In order to achieve the purpose, the invention adopts the following technical scheme:

a preparation method of a high-water-absorption aromatic polyester fabric comprises the following steps:

(1) dissolving acrylic acid and N, N-methylene bisacrylamide in water, adding ammonium persulfate, and uniformly stirring to obtain a modified solution;

(2) washing and drying the polyester fabric, and then irradiating for 20-30 min under an ultraviolet lamp;

(3) soaking the irradiated polyester fabric in a modified solution, and introducing nitrogen for 10-20 min;

(4) taking the polyester fabric out of the modified solution, and placing the polyester fabric under an ultraviolet lamp for irradiation reaction for 20-30 min;

(5) placing the polyester fabric after the irradiation reaction in water, boiling for 1-2 h, then placing in a sodium hydroxide solution, soaking for 20-30 min, washing with water and drying to obtain a water-absorbing modified polyester fabric;

(6) dispersing the pH response aromatic slow-release particles in polyacrylate emulsion to obtain a coating agent, coating the water absorption modified polyester fabric with the coating agent, and drying to obtain the polyester fabric with the sun-proof coating;

(7) putting the polyester fabric with the sun-proof coating in 0.5-1.5 g/L of Na₂CO₃And soaking the fabric in the solution for 1-2 min, and then washing and drying the fabric to obtain the high-water-absorptivity aromatic polyester fabric.

Preferably, in the modifying solution in the step (1), the mass fraction of acrylic acid is 6-10%, the mass fraction of N, N-methylene bisacrylamide is 2-6 per mill, and the mass fraction of ammonium persulfate is 1-3%.

Preferably, the power of the ultraviolet lamp in the steps (2) and (4) is 400-1000W, and the irradiation distance is 10-15 cm.

Preferably, the concentration of the sodium hydroxide solution in the step (5) is 0.02-0.05 mol/L.

Preferably, the method for preparing the pH-responsive aromatic sustained-release particles described in the step (6) comprises the steps of:

(a) dissolving hexadecylamine in absolute ethyl alcohol at the temperature of 25-30 ℃, adding 0.1-0.2 mol/L potassium chloride solution and deionized water, and uniformly stirring to obtain a guiding agent solution;

(b) dropwise adding isopropanol into the guiding agent solution under stirringTitanium is kept stand for 15-24 h and then centrifuged, and the product is washed by ethanol and dried to obtain TiO₂The molar ratio of the added titanium isopropoxide to the hexadecylamine in the guiding agent solution is 1: (0.1 to 0.5);

(c) adding TiO into the mixture₂Dispersing the precursor in a mixed solution of ammonia water, absolute ethyl alcohol and deionized water, reacting at 150-180 ℃ for 12-24 h, centrifuging, washing the product with ethanol, drying, and roasting at 500-510 ℃ for 2-3 h to obtain mesoporous TiO₂；

(d) Downward mesoporous TiO under the protection of nitrogen₂Adding toluene, gamma-chloropropyltrimethoxysilane and 3-glycidyl ether oxypropyltriethoxysilane, stirring at 80-120 ℃ and reacting for 20-30 h to obtain surface-modified mesoporous TiO₂Mesoporous TiO₂The mass volume ratio of the mixture to toluene, gamma-chloropropyltrimethoxysilane and 3-glycidyl ether oxypropyltriethoxysilane is 1 g: (20-30 mL): (20-30 mL): (400-600 mL);

(e) adding alanine into phosphate buffer solution with pH of 7.0, stirring uniformly, and adding surface modified mesoporous TiO₂Oscillating and reacting for 20-30 h at 50-60 ℃, filtering, washing the product with ethanol, and drying in vacuum to obtain alanine-modified mesoporous TiO₂Wherein the concentration of alanine in phosphate buffer solution is 2-4 mg/mL, and surface modified mesoporous TiO is added₂The mass volume ratio of the phosphate buffer solution to the phosphate buffer solution is 1 g: (100-200 mL);

(f) alanine modified mesoporous TiO₂Dispersing in an aromatic bacteriostatic agent, stirring at room temperature for reaction for 8-12 h, filtering, and washing with deionized water to obtain the aromatic bacteriostatic agent-loaded mesoporous TiO₂；

(g) Loading mesoporous TiO with aromatic bacteriostat₂Dispersing in N, N-dimethylformamide, stirring for 30-40 min, adding octadecyl dimethyl tertiary amine and potassium iodide under the protection of nitrogen, stirring at 40-60 ℃ for reaction for 24-36 h, filtering, washing the product with N, N-dimethylformamide, and drying in vacuum to obtain the pH response aromatic slow-release particles.

Preferably, the mass-to-volume ratio of the hexadecylamine to the added absolute ethyl alcohol, the potassium chloride solution and the deionized water in the step (a) is 1 g: (80-120 mL): (0.3-0.5 mL): (1-2 mL).

Preferably, the concentration of ammonia water in the mixed solution in the step (c) is 0.1-0.2 mol/L, and the volume ratio of the absolute ethyl alcohol to the deionized water is (1-2): 1; TiO 2₂The mass volume ratio of the precursor to the mixed solution is 1 g: (18-22 mL).

Preferably, the aromatic bacteriostatic agent in the step (f) is one or more of rose essential oil, lemon essential oil, mint essential oil and argy wormwood oil, and the alanine-modified mesoporous TiO is₂The mass volume ratio of the aromatic bacteriostatic agent to the aromatic bacteriostatic agent is 1 g: (20-50 mL).

Preferably, the mesoporous TiO loaded with the aromatic bacteriostatic agent in the step (g)₂The mass-to-volume ratio of N, N-dimethylformamide is 1 g: (200-400 mL) of mesoporous TiO loaded with aromatic bacteriostatic agent₂The mass ratio of the organic solvent to the octadecyl dimethyl tertiary amine and the potassium iodide is 5: (9-11): (0.1-0.5).

Preferably, the coating agent in the step (6) contains 10-30% of pH response aromatic slow-release particles by mass, and is coated by 1-2 coating agents, wherein the coating amount of the pH response aromatic slow-release particles in each coating is 1-3% of the weight of the polyester fabric.

The polyester fabric is pre-irradiated under an ultraviolet lamp, molecular chains on the surface of the polyester fabric are cracked under the ultraviolet irradiation, oxygen molecules in the air are converted into ozone and active oxygen, the surface of the polyester fabric is promoted to be oxidized, and therefore abundant polar groups such as hydroxyl groups are introduced to the surface of the polyester fabric, and the hydrophilicity of the polyester fabric is preliminarily improved. And then, soaking the polyester fabric subjected to pre-irradiation in a modification solution, then placing the polyester fabric under an ultraviolet lamp for irradiation, so that a hydrophilic acrylic monomer and an N, N-methylene bisacrylamide crosslinking agent in the modification solution are subjected to crosslinking polymerization under the initiation of an initiator ammonium persulfate and ultraviolet light to form a three-dimensional network structure on the surface of the polyester fabric, and after the polyester fabric is treated by boiling water and a sodium hydroxide solution, unreacted monomers, homopolymers and other impurities are removed, so that the polyester fabric subjected to water absorption modification is obtained, and due to the hydrophilicity of the crosslinked copolymer and the capillary action of the three-dimensional network structure, the modified polyester fabric obtains good water absorption performance.

Then, the invention coats a coating containing pH response aromatic slow release particles on the surface of the polyester fabric after water absorption modification, so that the polyester fabric obtains aromatic slow release performance. In the preparation process of the pH response aromatic slow-release particles, mesoporous TiO is prepared firstly₂，TiO₂Is a common ultraviolet resistant agent in the fabric, can effectively absorb and reflect ultraviolet rays, and leads the fabric to have the sun-proof function, and the TiO with the mesoporous structure is prepared in the invention₂Making TiO into₂The fabric has a sun-screening function and good adsorption performance, so that the aromatic bacteriostatic agent can be loaded in the pore channels, and the fabric has aromatic slow-release performance. The invention also relates to mesoporous TiO₂Alanine and long carbon chain quaternary ammonium salt are modified on the surface, and as the quaternary ammonium group in the long carbon chain quaternary ammonium salt is positively charged and the isoelectric point of the alanine is 6.02, the alanine is negatively charged under neutral and alkaline conditions and is attracted with the quaternary ammonium salt group, and the long carbon chain covers the mesoporous TiO under the attraction action₂The pore structure is closed, and the aromatic bacteriostatic agent loaded in the pore cannot be released; under the acidic condition that the pH value is less than 6.02, alanine is positively charged and is repelled with quaternary ammonium salt groups, and long carbon chains leave the mesoporous TiO under the repelling action₂The surface is unfolded, the pore structure is opened, and the aromatic bacteriostatic agent loaded in the pore can be released. Due to mesoporous TiO₂The closing and opening of the pore structure can be controlled along with the change of pH, so that the release of the loaded aromatic bacteriostatic agent can also be controlled by the external pH.

In the preparation process, firstly, the mesoporous TiO is prepared by the steps (a) to (c) and the hexadecylamine is used as a guiding agent₂Then, through the step (d), gamma-chloropropyltrimethoxysilane and 3-glycidoxypropyltriethoxysilane are utilized to prepare the mesoporous TiO₂Modifying the surface with chloropropyl and epoxy; then, through the step (e), the epoxy group is utilized to open loop and graft alanine on the mesoporous TiO₂Introducing alanine on the surface; then loading the aromatic bacteriostatic agent in the mesoporous TiO through the step (f)₂In the duct of (2); finally, the step (g) of utilizing the mesoporous TiO under the reaction condition of neutral condition₂The surface gamma-chloropropyltrimethoxysilane and octadecyl dimethyl tertiary amine are subjected to quaternization reaction, and long carbon chain quaternary ammonium salt is introduced into the mesoporous TiO₂And (3) sealing the pore channel on the surface.

The sweat of a human body is generally weakly acidic, the pH value is about 5.5, when the pH response aromatic slow-release particles are loaded on the polyester fabric and worn on the human body, when the human body generates sweat, the sweat can be quickly absorbed due to good hygroscopicity of the polyester fabric after water absorption modification, so that the pH response aromatic slow-release particles are under an acidic condition, the pore structure is opened, the aromatic bacteriostatic agent loaded in the pH response aromatic slow-release particles can be slowly released to kill bacteria on the skin, the phenomenon that the bacteria decompose organic matters in the sweat to generate peculiar smell is avoided, meanwhile, the peculiar smell can be covered by the fragrance of the aromatic bacteriostatic agent, and the deodorization effect is achieved. After the fabric stained with sweat is cleaned, under the washing action of neutral water, the pore structure in the pH response aromatic slow-release particles is closed again, and the aromatic bacteriostatic agent stops releasing. Therefore, the aromatic bacteriostatic agent can not be released to cause loss when the fabric is placed, and only when the fabric is worn on a human body and sweats, the aromatic bacteriostatic agent can be released to eliminate peculiar smell, and the fragrance release duration is good.

Therefore, the invention has the following beneficial effects:

(1) acrylic acid and N, N-methylene bisacrylamide are subjected to crosslinking copolymerization on the surface of the polyester fabric under the action of ultraviolet irradiation to form a three-dimensional net structure, so that the polyester fabric obtains good water absorption performance, human sweat can be effectively absorbed, wearing comfort is improved, pH response of the pH response aromatic slow-release particles can be realized under the action of the sweat, and an aromatic bacteriostatic agent is released;

(2) using mesoporous TiO₂The aromatic bacteriostatic agent is loaded, so that the pH response aromatic slow-release particles have the sun-screening function and the loading function at the same time;

(3) in the mesoporous TiO₂Alanine and long carbon chain quaternary ammonium salt are modified on the surface, and the attraction or repulsion performance of alanine and quaternary ammonium group under different pH conditions is utilized to enable the sun-proof particles to have a pH response slow release function, so that the sun-proof deodorizing fabric can be made to have aromatic fragrance when placedThe fragrant bacteriostatic agent can not be released, and only when the fragrant bacteriostatic agent is worn on a human body and sweats, the fragrant bacteriostatic agent can be released to eliminate peculiar smell, and the fragrance release duration is good.

Detailed Description

The invention is further described with reference to specific embodiments.

The reagents used in the present invention are as follows:

polyacrylate emulsion: the solid content is 40 percent, Shanghai Jiehun new material company;

rose essential oil: purity is more than or equal to 99 percent, Shanghai Zhengnzhen nanometer science and technology Limited company;

lemon essential oil: purity is more than or equal to 99 percent, Shanghai Zhengnzhi nano science and technology Limited company.

Other reagents used in the present invention are those commonly used in the art or commercially available.