阅读说明：本技术 一种防晒除臭纯棉织物及其制备方法 (Sun-proof deodorant pure cotton fabric and preparation method thereof ) 是由 廖国庆 于 2020-06-24 设计创作，主要内容包括：本发明公开了一种防晒除臭纯棉织物及其制备方法,制备步骤为：(1)将pH响应缓释防晒粒子分散在聚丙烯酸酯乳液中得到涂层剂；(2)纯棉基布经预洗、烘干后,用涂层剂进行涂覆并烘干得到具有防晒涂层的织物；(3)将具有防晒涂层的织物Na<Sub>2</Sub>CO<Sub>3</Sub>溶液中浸渍并水洗,烘干后得到防晒除臭纯棉织物。本发明将芳香抑菌剂负载在pH响应缓释防晒粒子内并整理在纯棉织物上,使纯棉织物具有防晒效果的同时,可以通过pH的变化控制芳香抑菌剂的释放,使织物在接触人体汗液后才释放出芳香抑菌剂杀菌并遮掩异味,水洗后芳香抑制剂又停止释放,避免衣物在放置不穿时芳香抑菌剂的挥发损失,提高了织物的释香持久性。(The invention discloses a sun-proof deodorant pure cotton fabric and a preparation method thereof, wherein the preparation method comprises the following steps: (1) dispersing the pH response slow-release sunscreen particles in polyacrylate emulsion to obtain a coating agent; (2) after the pure cotton base cloth is pre-washed and dried, coating the pure cotton base cloth with a coating agent and drying the pure cotton base cloth to obtain a fabric with a sun-proof coating; (3) the fabric with the sun-proof coating Na 2 CO 3 Soaking and washing the fabric in the solution, and drying the fabric to obtain the sun-proof deodorant pure cotton fabric. The aromatic bacteriostatic agent is loaded in the pH response slow-release sunscreen particles and is arranged on the pure cotton fabric, so that the pure cotton fabric has a sunscreen effect, the release of the aromatic bacteriostatic agent can be controlled through the change of pH, the aromatic bacteriostatic agent is released to sterilize and cover peculiar smell after the fabric contacts human sweat, the aromatic bacteriostatic agent stops releasing after the fabric is washed, the volatilization loss of the aromatic bacteriostatic agent when the fabric is not worn is avoided, and the fragrance release durability of the fabric is improved.)

1. A sun-proof deodorant pure cotton fabric is characterized by comprising pure cotton base cloth and a sun-proof coating loaded on the pure cotton base cloth, wherein the sun-proof coating comprises pH-responsive slow-release sun-proof particles, and the preparation method of the pH-responsive slow-release sun-proof particles comprises the following steps:

(a) dissolving hexadecylamine in absolute ethyl alcohol at 25-30 ℃, adding a 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 TiO₂A precursor;

(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 and gamma-chlorineStirring and reacting propyl trimethoxy silane and 3-glycidyl ether oxypropyl triethoxy silane at 80-120 ℃ for 20-30 h to obtain surface modified mesoporous TiO₂；

(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 TiO₂；

(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 slow-release sunscreen particles.

2. The sun-screening deodorant pure cotton fabric according to claim 1, wherein the concentration of the potassium chloride solution in the step (a) is 0.1-0.2 mol/L, and the mass-volume ratio of the hexadecylamine to the added absolute ethyl alcohol, the potassium chloride solution and the deionized water is 1 g: (80-120 mL): (0.3-0.5 mL): (1-2 mL).

3. The sun-screening deodorant pure cotton fabric according to claim 1, wherein the molar ratio of the titanium isopropoxide added in the step (b) to the hexadecylamine in the directing agent solution is 1: (0.1-0.5).

4. The sun-proof deodorant pure cotton fabric according to claim 1, wherein 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).

5. The sun-screening deodorant pure cotton fabric according to claim 1, wherein the mesoporous TiO in step (d) is selected from the group consisting of₂The 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).

6. The sun-screening deodorant pure cotton fabric according to claim 1, wherein the concentration of alanine in phosphate buffer solution in step (e) 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).

7. The sun-screening deodorant pure cotton fabric according to claim 1, wherein the aromatic bacteriostatic agent in step (f) is one or more of rose essential oil, lemon essential oil, mint essential oil and blumea 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).

8. The sun-screening deodorant pure cotton fabric according to claim 1, wherein the mesoporous TiO loaded with aromatic bacteriostatic agent in 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)。

9. a method for preparing a sun-screening deodorant pure cotton fabric according to any one of claims 1 to 8, characterized by comprising the steps of:

(1) dispersing the pH-responsive slow-release sunscreen particles in polyacrylate emulsion to obtain a coating agent, wherein the mass fraction of the pH-responsive slow-release sunscreen particles in the coating agent is 10-30%;

(2) pre-washing pure cotton base cloth at 80-90 ℃ for 25-35 min, drying at 100-105 ℃ for 2-3 min, coating with a coating agent, and drying at 80-90 ℃ for 2-3 min to obtain a fabric with a sun-proof coating;

(3) the fabric with the sun-proof coating is coated with 0.5-1.5 g/L of Na₂CO₃Soaking the fabric in the solution for 1-2 min, washing with water, and drying at 100-105 ℃ for 2-3 min to obtain the sun-proof deodorant pure cotton fabric.

10. The sun-screening deodorant pure cotton fabric according to claim 1, wherein 1-2 coating layers are applied in step (2), and the amount of the pH-responsive slow-release sun-screening particles applied in each coating layer is 1-3% of the weight of the pure cotton base fabric.

Technical Field

The invention relates to the technical field of functional fabrics, in particular to a sun-proof deodorant pure cotton fabric and a preparation method thereof.

Background

The fabric is added with the aromatic, so that pleasant aroma can be brought, and meanwhile, a plurality of aromatic also have the effects of calming, sterilizing, health care and the like, so that the fabric has the additional functions of bacteriostasis, deodorization and the like when being worn. However, if the aromatic is directly sprayed on the fabric, the aroma retention time of the aromatic is short and the aromatic is not washable, so that the aromatic is usually coated in the microcapsule and is finished on the fabric in the prior art, volatilization of the aromatic is protected by the microcapsule, the aromatic has a slow release effect, and the aroma release durability of the fabric is prolonged. For example, patent document CN105603765A, "a method for preparing a rose essential oil microcapsule finishing agent and its application", discloses a rose essential oil microcapsule with semipermeable capsule wall, where the rose essential oil can be slowly released through the capsule wall, and the rose essential oil can be made into a finishing agent which can exert a lasting health care effect after being finished on pure cotton fabric.

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 aims to overcome the problems that in the prior art, the fragrance release is difficult to control and regulate by a method for prolonging the fragrance release durability of a fragrance in a fabric through microcapsules, the fragrance is continuously volatilized even if clothes are not worn, so that the fragrance is lost, and the fragrance retention time prolonging effect is still limited.

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

a sun-proof deodorization pure cotton fabric comprises a pure cotton base cloth and a sun-proof coating loaded on the pure cotton base cloth, wherein the sun-proof coating comprises pH-responsive slow-release sun-proof particles, and the preparation method of the pH-responsive slow-release sun-proof particles comprises the following steps:

(a) dissolving hexadecylamine in absolute ethyl alcohol at 25-30 ℃, adding a 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 TiO₂A precursor;

(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 TiO₂；

(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 TiO₂；

(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 slow-release sunscreen particles.

In the preparation process of the pH response slow-release sunscreen 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 into₂Has sun-screening function and good adsorption performance, so as to load the aromatic bacteriostatic agent in the pore canal. The invention also relates to mesoporous TiO₂Surface modified with alanine and lengthThe quaternary ammonium group in the long carbon chain quaternary ammonium salt is positively charged, and the isoelectric point of the alanine is 6.02, so that the alanine is negatively charged under neutral and alkaline conditions, is attracted with the quaternary ammonium salt group, and the long carbon chain covers the mesoporous TiO under the action of attraction₂The 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.

When the sweat of a human body is generally weakly acidic, the pH value is about 5.5, and the sun-proof and deodorizing fabric prepared by loading the pH response slow-release sun-proof particles on the pure cotton base cloth is worn on the human body, when the human body generates sweat, the sweat can be quickly absorbed due to good water absorption of the pure cotton base cloth, so that the pH response slow-release sun-proof particles are in an acidic condition, the pore structure is opened, the aromatic bacteriostatic agent loaded in the pH response slow-release sun-proof particles can be slowly released to kill bacteria on the skin, the bacteria are prevented from decomposing organic matters in the sweat to generate peculiar smell, and the peculiar smell can be covered by the fragrance of the aromatic bacteriostatic agent to play a deodorizing effect. After the fabric stained with sweat is cleaned, under the washing action of neutral water, the pore structure in the pH response slow-release sunscreen particles is closed again, and the aromatic bacteriostatic agent stops releasing. Therefore, the sun-proof deodorant fabric does not release the aromatic bacteriostatic agent to cause loss when being placed, and the aromatic bacteriostatic agent can be released to eliminate peculiar smell only when the sun-proof deodorant fabric is worn on a human body and sweats, so that the fragrance release duration is good.

The sun-proof deodorant pure cotton fabric adopts the pure cotton fabric as the base fabric, has good sweat absorption and moisture absorption performance and high wearing comfort, can remove and cover the body odor generated by sweating, and is suitable for being made into underwear, socks and other close-fitting clothes; meanwhile, the fabric provided by the invention also has good sun-proof performance and is suitable for making clothes in summer.

Preferably, the concentration of the potassium chloride solution in the step (a) is 0.1-0.2 mol/L, and the mass-to-volume ratio of the hexadecylamine to the added absolute ethyl alcohol, the potassium chloride solution and the deionized water is 1 g: (80-120 mL): (0.3-0.5 mL): (1-2 mL).

Preferably, the molar ratio of titanium isopropoxide added in step (b) to hexadecylamine in the directing agent solution is 1:

(0.1～0.5)。

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:

(18～22mL)。

preferably, the mesoporous TiO in step (d)₂The 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).

Preferably, the concentration of alanine in the phosphate buffer solution in the step (e) is 2-4 mg/mL, and the 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).

Preferably, step (f) is performedThe aromatic bacteriostatic agent is one or more of rose essential oil, lemon essential oil, mint essential oil and blumea 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).

The invention also provides a preparation method of the sun-proof deodorizing pure cotton fabric, which comprises the following steps:

(1) dispersing the pH-responsive slow-release sunscreen particles in polyacrylate emulsion to obtain a coating agent, wherein the mass fraction of the pH-responsive slow-release sunscreen particles in the coating agent is 10-30%;

(2) pre-washing pure cotton base cloth at 80-90 ℃ for 25-35 min, drying at 100-105 ℃ for 2-3 min, coating with a coating agent, and drying at 80-90 ℃ for 2-3 min to obtain a fabric with a sun-proof coating;

(3) the fabric with the sun-proof coating is coated with 0.5-1.5 g/L of Na₂CO₃Soaking the fabric in the solution for 1-2 min, washing with water, and drying at 100-105 ℃ for 2-3 min to obtain the sun-proof deodorant pure cotton fabric.

Preferably, 1-2 coating layers are coated in the step (2), and the coating amount of the pH response slow-release sunscreen particles in each coating layer is 1-3% of the weight of the pure cotton base cloth.

After the sun-proof coating containing the pH response slow-release sun-proof particles is coated on the pure cotton base cloth, Na is added₂CO₃The solution is soaked, washed and dried, so that the pore channel of the pH response slow-release sunscreen particles is ensured to be in a closed state, and the aromatic inhibitor is not released to cause loss in the process of placing the fabric.

Therefore, the invention has the following beneficial effects:

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

(2) betweenPorous 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 ensure that the sun-proof particles have a pH response slow release function, so that the aromatic bacteriostatic agent can not be released when the sun-proof deodorant fabric is placed, and only when the sun-proof deodorant fabric is worn on a human body and sweats, the aromatic bacteriostatic agent can be released to eliminate peculiar smell, and the fragrance release durability is good;

(3) the pure cotton fabric is used as the base fabric material, so that the wearing comfort is good, the sweat absorption and moisture absorption performance is good, and the pH response of the pH response slow-release sunscreen particles to sweat is facilitated.

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.