A waterproof elastic non-woven fabric mask and a preparation method thereof

Abstract

The application discloses a waterproof elastic non-woven fabric mask, which comprises, from top to bottom, an outer non-woven fabric layer, an activated carbon non-woven fabric layer and an inner non-woven fabric layer; the waterproof elastic non-woven fabric mask is prepared through the following steps: in the first step, polyester non-woven fabric is soaked in an impregnation solution for 10-20 seconds, the excess impregnation solution is rolled off by using a vertical small rolling machine, the rolling residual rate is 50%, two-time impregnation and two-time rolling are adopted, then the polyester non-woven fabric is placed into a blowing drying box, pre-dried at 80 DEG C for 5 min, baked at 150 DEG C for 20 min, taken out, washed, dried at 60 DEG C until the weight is constant, and the outer non-woven fabric layer is obtained; in the second step, the inner non-woven fabric layer, the activated carbon non-woven fabric layer and the outer non-woven fabric layer are sequentially stacked, and then one-time composite molding is carried out to obtain the waterproof elastic non-woven fabric mask; the outer non-woven fabric layer has the characteristics of high hydrophobicity, air permeability, antibiosis and fragrance, and the safety and practicability of the mask are improved.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of mask preparation, and particularly relates to a waterproof elastic non-woven fabric mask and a preparation method thereof. BACKGROUND

[0002] In recent years, due to the acceleration of industrialization and the aggravation of various pollutions, the environment for human survival is deteriorating, the potential entry of infectious viruses and bacteria is increasing, and respiratory infectious diseases are transmitted through droplets and air, which has the characteristics of fast speed, wide susceptible population and high incidence, and thus poses a great threat to public health and social stability. Meanwhile, a certain degree of haze weather appears in many cities.

[0003] PM2.5 is medically referred to as inhalable particles, which are pollutants with a particle diameter less than or equal to 2.5 microns in the atmosphere. The general masks on the market have poor PM2.5 filtering effect and cannot effectively block PM2.5. Wearing a protective mask can effectively filter PM2.5 particles and block the invasion of pathogenic microorganisms into the human body, which is an effective means to prevent the spread of respiratory infectious diseases and protect the health of personnel. Related researchers found through investigation and research that persistent wearing of masks can reduce the infection of influenza. Protective masks, as a non-drug intervention means, can control the spread of pathogenic microorganisms. Antibacterial and mildew-resistant masks play an increasingly important role in reducing diseases and responding to sudden biological pollution incidents.

[0004] In order to achieve the purposes of antibiosis and mildew resistance, the masks on the market or reported in related patents are usually composed of multiple layers of gauze or cotton cloth. However, the existing non-woven fabric has poor waterproofness, is prone to bacterial growth and dust adsorption, and has poor antibacterial and mildew-resistant performance. Therefore, it is necessary to improve the waterproof elastic non-woven fabric mask with good antibacterial performance and high comfort. SUMMARY

[0005] The application aims to provide a waterproof elastic non-woven fabric mask and a preparation method thereof.

[0006] The technical problem to be solved by the application is:

[0007] In the prior art, the waterproofness of the non-woven fabric mask is poor, bacteria are prone to grow, dust is prone to be adsorbed, and an odor is prone to be generated after long wearing.

[0008] The object of the application can be achieved by the following technical scheme:

[0009] A waterproof elastic non-woven fabric mask comprises, from top to bottom, an outer non-woven fabric layer, an activated carbon non-woven fabric layer and an inner non-woven fabric layer.

[0010] The waterproof elastic non-woven fabric mask is prepared by the following steps:

[0011] The first step, the polyester non-woven fabric is soaked in the impregnating solution for 10-20 seconds, the excess impregnating solution is rolled off by using a vertical small roller, the rolling rate is 50%, two-dip-two-roll is adopted, then it is put into a blowing drying box, pre-dried at 80℃ for 5min, then baked at 150℃ for 20min, then taken out, washed, dried at 60℃ to constant weight, to obtain the outer non-woven fabric layer;

[0012] The second step, the inner non-woven fabric layer, the activated carbon non-woven fabric layer and the outer non-woven fabric layer are stacked in turn, then one-time composite molding is carried out, to obtain the waterproof elastic non-woven fabric mask.

[0013] Further, the carbon content of the activated carbon non-woven fabric layer is 30-40%, and the inner non-woven fabric layer is a hot air non-woven fabric.

[0014] Further, the impregnating solution is prepared by the following steps:

[0015] Polyethylene glycol and polydimethylsiloxane are added into a reaction kettle, heated to 85℃, stirred at a speed of 200r / min for 20min under nitrogen protection, then isophorone diisocyanate is added dropwise into the reaction kettle, after the dropwise addition is completed, dibutyltin dilaurate is added, and the reaction is kept for 30min, then dimethylol acrylic acid is added, and the reaction is kept for 2h, after the reaction is completed, acetone is added to adjust the viscosity to 1000-1500 centipoise, then cooled to room temperature, triethylamine is added to adjust the pH value of the system to 7-8, finally deionized water and composite filler are added, and high-speed dispersion is carried out at a speed of 1500r / min for 30-50min, to obtain the impregnating solution.

[0016] Further, the amount ratio of polyethylene glycol, polydimethylsiloxane, isophorone diisocyanate, dibutyltin dilaurate, dimethylol acrylic acid, deionized water and composite filler is 11g:69g:38g:1-3mL:30g:20mL:3-5g.

[0017] Further, the composite filler is prepared by the following steps:

[0018] Step A1, peppermint essential oil was added into a three-necked flask, the rotation speed was controlled at 80-120 r / min, and the emulsifier was added into the three-necked flask by a constant pressure dropping funnel while stirring, after the dropping was completed, the stirring was continued for 5-10 min to obtain a core solution, gelatin, gum arabic and deionized water were added into the reaction kettle, and the temperature was increased to 90℃, and the stirring was carried out at a rotation speed of 60-100 r / min for 20 min, and the core solution was added, and the rotation speed was increased to 200-300 r / min under the condition of a constant temperature water bath at 50℃, and after the stirring reaction was carried out for 20 min, the pH value of the system was adjusted to 4.4-4.5 by using a 10% acetic acid solution, then the rotation speed was controlled at 80 r / min, and the temperature was decreased to below 10℃, and a 25% glutaraldehyde solution was added into the reaction kettle by dripping, and the stirring was continued for 30 min, then the temperature was increased to 50℃, and the pH value of the system was adjusted to 9-10 by using a 10% sodium hydroxide solution, and the stirring was continued for 30 min to obtain a microcapsule solution;

[0019] Step A2, cetyltrimethylammonium bromide, a 1 mol / L hydrochloric acid solution, anhydrous ethanol, distilled water, tetraethyl orthosilicate and ammonium chloride were added into a reaction kettle, and the stirring was carried out at a rotation speed of 100-200 r / min for 2-4 h to obtain a mixture, the mixture was filtered, the filter cake was washed with a 40% ethanol solution until the washing liquid was neutral, and then the filter cake was calcined in a muffle furnace at 500℃ for 5 h to obtain carrier particles;

[0020] Step A3, the microcapsule solution obtained in step A1 was diluted 5-10 times with a 60% ethanol solution, and then was transferred into a centrifuge tube, the carrier particles obtained in step A2 were added into the centrifuge tube, and after ultrasonic dispersion was carried out at a temperature of 60℃ and a frequency of 25-45 kHz for 30 min, the temperature was decreased to 4℃, and the ultrasonic dispersion was continued at the same frequency for 30 min, finally, the centrifugal treatment was carried out at a rotation speed of 9000 r / min for 10-15 min under the condition of room temperature, the precipitate was washed with deionized water for 3-5 h, and then was freeze-dried at-45℃ until the weight was constant to obtain an intermediate;

[0021] Step A4, epichlorohydrin was added into a reactor, and the temperature was increased to 80℃ and kept for 2 h, then a mixed solution a composed of 5,5-dimethylhydantoin and a sodium hydroxide solution was added into the reactor by dripping, the dripping speed was controlled at 1-3 drops / s, after the dripping was completed, the temperature was kept unchanged, the stirring was carried out at a rotation speed of 100 r / min for 20 min, and then the system was statically placed for 1 h to obtain a solution a;

[0022] The reaction process was as follows:

[0023]

[0024] Step A5, N,N'-dimethyl dodecyl tertiary amine and tetramethyl dichloropropyl disiloxane are added into a three-necked flask, then methanol and potassium iodide are added into the three-necked flask, stirring at 60 r / min for 3-5 min, then the three-necked flask is placed in a magnetic heating stirrer, under nitrogen protection, the reaction temperature is controlled at 70°C, and magnetic stirring is carried out for 24 h, after the reaction is completed, the solvent methanol is removed by rotary evaporation under reduced pressure, then recrystallization is carried out in a solution mixed according to a volume ratio of 1:1 of acetone and anhydrous ethanol, filtration is carried out, the filter cake is washed with deionized water for 3-5 times, and finally drying is carried out at 50°C until the constant weight, to obtain solid b;

[0025] The reaction process is as follows:

[0026] Step A6, solid b and tetrahydrofuran are added into a reaction kettle, 2-aminobutanol and triethylamine are uniformly mixed according to a volume ratio of 1:3, and then the mixture is added into the reaction kettle through a constant-pressure dropping funnel, the dropping speed is controlled at 1 drop / s, after the dropping is completed, the reaction is carried out at 0°C for 2.5 h under the condition of a rotating speed of 100 r / min, then the reaction is carried out at 30°C for 2.5 h under the same rotating speed, and finally the reaction is carried out at 50°C for 18 h, after the reaction is completed, filtration is carried out, the filter cake is washed with a 35% ethanol solution for 3-5 times, and finally drying is carried out in an oven at 50-60°C until the constant weight, to obtain solid c; the reaction process is as follows:

[0027] Step A7, solid c and toluene are added into a three-necked flask, ultrasonic dispersion is carried out at a frequency of 20-40 kHz for 10 min, then solution a is added dropwise into the three-necked flask, after the dropping is completed, the reaction is carried out at 40°C for 24 h under the condition of a rotating speed of 100-200 r / min, to obtain solution d, then the intermediate is added into the three-necked flask, and reflux reaction is carried out at 100°C for 4 h, after the reaction is completed, centrifugal treatment is carried out at a rotating speed of 6000-8000 r / min for 10 min, the filter cake is washed with toluene for 3 times, and finally drying is carried out in a vacuum drying oven at 60°C for 24 h, to obtain a composite filler.

[0028] Part of the reaction process is as follows:

[0029] Further, the ratio of the use amount of the core solution, gelatin, gum arabic, deionized water and glutaraldehyde solution in step A1 is 0.5 mL: 1.25 g: 1 g: 30-50 mL: 2.5 mL, wherein the use amount of the emulsifier in the core solution is 1% of the mass of the peppermint essential oil, and the emulsifier is Span-80; the mass ratio of cetyltrimethylammonium bromide, hydrochloric acid solution, anhydrous ethanol, distilled water, tetraethyl orthosilicate and ammonium chloride in step A2 is 4: 1.12: 22.8: 50-60: 10.4: 4; the ratio of the use amount of the carrier particles and the microcapsule solution in step A3 is 0.5 g: 3-5 mL; the mass ratio of epichlorohydrin, 5,5-dimethylhydantoin and sodium hydroxide solution in step A4 is 1: 8: 1, wherein the mass fraction of the sodium hydroxide solution is 50%.

[0030] Further, the ratio of the use amount of the N,N'-dimethyl dodecyl tertiary amine, tetramethyldichloropropyl disiloxane, methanol and potassium iodide in step A5 is 0.1 mol: 0.1 mol: 20 mL: 0.005 mol, the ratio of the use amount of the solid b, tetrahydrofuran and 2-aminobutanol in step A6 is 0.1 mol: 80-120 mL: 0.1 mol; the ratio of the use amount of the solid c, toluene, a solution and intermediate in step A7 is 0.5 g: 20-30 mL: 3 g: 4 g.

[0031] Further, the primary composite molding in the second step is ultrasonic welding.

[0032] Further, a preparation method of a waterproof elastic non-woven fabric mask comprises the following steps:

[0033] In the first step, the polyester non-woven fabric is soaked in the impregnation solution for 10-20 seconds, the excess impregnation solution is rolled off by using a vertical small roller, the rolling rate is 50%, two-dip-two-roll is adopted, then it is placed into a blowing drying box, pre-dried at 80°C for 5 min, then baked at 150°C for 20 min, then taken out, washed with water, dried at 60°C to constant weight, to obtain the outer non-woven fabric layer;

[0034] In the second step, the inner non-woven fabric layer, the activated carbon non-woven fabric layer and the outer non-woven fabric layer are stacked in turn, then primary composite molding is carried out, to obtain the waterproof elastic non-woven fabric mask.

[0035] The beneficial effects of the present application are as follows: the present application is formed by ultrasonic welding of the inner non-woven fabric layer, the activated carbon non-woven fabric layer and the outer non-woven fabric layer to obtain a waterproof and elastic non-woven fabric mask, the peppermint essential oil is used as a core material, the gum arabic and the gelatin are used as wall materials, the peppermint essential oil microcapsule solution is prepared, the cetyltrimethylammonium bromide is used as a template agent, the tetraethyl orthosilicate is used as a silicon source, the mesoporous silica carrier particles are prepared by high-temperature calcination, the carrier particles are dispersed in the microcapsule solution, the microcapsule molecules enter the inside of the carrier particles through the gap structure on the carrier particle molecules to obtain an intermediate, a substitution reaction of 5,5-dimethylhydantoin and epichlorohydrin is carried out to obtain a solution a, the N,N'-dimethyldodecyl tertiary amine and the tetramethyldichlorodisiloxane are used as raw materials, the solid b with a halamine structure is generated under the catalysis of potassium iodide, the solid b is chemically reacted with 2-aminobutanol in a tetrahydrofuran solvent to obtain the solid c containing -NH2, finally, the solid c is subjected to ring-opening reaction with the solution a to obtain the substance d containing the halamine structure, the hydantoin ring, the epoxy group, the secondary amine group, the Si-O bond and the alcohol hydroxyl group, finally, the substance d is subjected to hydrolysis, the intermediate is modified, the N-halamine hydrophobic antibacterial alkyl long chain and the hydantoin ring antibacterial structure are grafted on the intermediate, the composite filler is endowed with excellent hydrophobicity and antibacterial property, the secondary amine group can participate in the curing reaction of the impregnating solution, the excellent hydrophobicity, the antibacterial property, the wear resistance and the aromatic and cool odor of the impregnating coating are endowed by combining the slow-release performance of the peppermint essential oil microcapsules in the intermediate, the polydimethylsiloxane is added in the impregnating solution, which can effectively improve the hydrophobicity of the non-woven fabric material, and further improve the cleanliness of the mask, and the polyester non-woven fabric is subjected to impregnation treatment in the present application, the original elasticity of the non-woven fabric is ensured, and the non-woven fabric is endowed with high hydrophobicity, air permeability, antibacterial property and fragrance, so that the safety and practicability of the mask are improved. DETAILED DESCRIPTION

[0036] The technical solutions in the embodiments of the present application will be described below in a clear and complete manner. Obviously, the described embodiments are only some of the embodiments of the present application, rather than all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative labor fall within the protection scope of the present application.

[0037] Embodiment 1

[0038] The composite filler is prepared by the following steps:

[0039] Step A1, peppermint essential oil was added into a three-necked flask, the stirring speed was controlled at 80 r / min, and the emulsifier was added into the three-necked flask through a constant pressure dropping funnel while stirring. After the dropping was completed, the stirring was continued for 5 min to obtain a core solution. Gelatin, gum arabic and deionized water were added into the reaction kettle, and the temperature was increased to 90℃. The stirring was carried out at a speed of 60 r / min for 20 min. The core solution was added. The stirring speed was increased to 200 r / min under the condition of a constant temperature water bath at 50℃. After the stirring reaction was carried out for 20 min, the pH value of the system was adjusted to 4.4 by using a 10% acetic acid solution. Then the stirring speed was controlled at 80 r / min, and the temperature was decreased to below 10℃. A 25% glutaraldehyde solution was added into the reaction kettle. After the stirring was continued for 30 min, the temperature was increased to 50℃. The pH value of the system was adjusted to 9 by using a 10% sodium hydroxide solution. The stirring was continued for 30 min to obtain a microcapsule solution.

[0040] Step A2, cetyltrimethylammonium bromide, a 1 mol / L hydrochloric acid solution, anhydrous ethanol, distilled water, tetraethyl orthosilicate and ammonium chloride were added into a reaction kettle. The stirring was carried out at a speed of 100 r / min for 2 h to obtain a mixture. The mixture was filtered. The filter cake was washed with a 40% ethanol solution until the washing liquid was neutral. Then the filter cake was calcined in a muffle furnace at 500℃ for 5 h to obtain carrier particles.

[0041] Step A3, the microcapsule solution obtained in step A1 was diluted 5 times with a 60% ethanol solution. Then the solution was transferred into a centrifuge tube. The carrier particles obtained in step A2 were added into the centrifuge tube. After the ultrasonic dispersion was carried out at a temperature of 60℃ and a frequency of 25 kHz for 30 min, the temperature was decreased to 4℃. The ultrasonic dispersion was continued at the same frequency for 30 min. Finally, the centrifugal treatment was carried out at a speed of 9000 r / min for 10 min at room temperature. The precipitate was washed with deionized water for 3 h. The freeze-drying was carried out at -45℃ until the weight was constant to obtain an intermediate.

[0042] Step A4, epichlorohydrin was added into a reactor. After the temperature was increased to 80℃ and kept for 2 h, a mixed solution a composed of 5,5-dimethylhydantoin and a sodium hydroxide solution was added into the reactor at a dropping speed of 1 drop / s. After the dropping was completed, the temperature was kept unchanged. The stirring was carried out at a speed of 100 r / min for 20 min. Then the system was statically placed for 1 h to obtain a solution a.

[0043] Step A5, N,N'-dimethyl dodecyl tertiary amine and tetramethyl dichloro propyl disiloxane were added into a three-necked flask, then methanol and potassium iodide were added into the three-necked flask, stirring at 60 r / min for 3 min, then the three-necked flask was put into a magnetic heating stirrer, under the protection of nitrogen, the reaction temperature was controlled at 70℃, and the reaction was carried out under magnetic stirring for 24 h, after the reaction was completed, the solvent methanol was removed by rotary evaporation under reduced pressure, then recrystallization was carried out in a solution mixed by acetone and anhydrous ethanol at a volume ratio of 1:1, the filter cake was washed with deionized water for 3 times, and finally dried at 50℃ until the weight was constant, to obtain solid b;

[0044] Step A6, solid b and tetrahydrofuran were added into a reaction kettle, 2-aminobutanol and triethylamine were mixed uniformly at a volume ratio of 1:3, and then added into the reaction kettle by a constant pressure dropping funnel, the dropping speed was controlled at 1 drop / s, after the dropping was completed, the reaction was carried out at 0℃ for 2.5 h under the condition of 100 r / min, then the reaction was carried out at 30℃ for 2.5 h under the same rotation speed, and finally the reaction was carried out at 50℃ for 18 h, after the reaction was completed, filtration was carried out, the filter cake was washed with a 35% ethanol solution for 3 times, and finally dried in an oven at 50℃ until the weight was constant, to obtain solid c;

[0045] Step A7, solid c and toluene were added into a three-necked flask, ultrasonic dispersion was carried out at a frequency of 20 kHz for 10 min, then solution a was added dropwise into the three-necked flask, after the dropping was completed, the reaction was carried out at 40℃ for 24 h under the condition of 100 r / min, to obtain solution d, then the intermediate was added into a three-necked flask, and the reaction was carried out at 100℃ under reflux for 4 h, after the reaction was completed, centrifugal treatment was carried out at a rotation speed of 6000 r / min for 10 min, the filter cake was washed with toluene for 3 times, and finally dried in a vacuum drying oven at 60℃ for 24 h, to obtain the composite filler.

[0046] Example 2

[0047] The composite filler was prepared by the following steps:

[0048] Step A1, peppermint essential oil was added into a three-necked flask, the stirring speed was controlled at 100 r / min, and the emulsifier was added into the three-necked flask through a constant pressure dropping funnel while stirring. After the dropping was completed, the stirring was continued for 8 min to obtain a core solution. Gelatin, gum arabic and deionized water were added into the reaction kettle, and the temperature was increased to 90℃. The stirring was carried out at a speed of 80 r / min for 20 min. The core solution was added. The stirring speed was increased to 250 r / min under the condition of a constant temperature water bath at 50℃. After the stirring reaction was carried out for 20 min, the pH value of the system was adjusted to 4.4 by using a 10% acetic acid solution. Then the stirring speed was controlled at 80 r / min, and the temperature was decreased to below 10℃. A 25% glutaraldehyde solution was added into the reaction kettle dropwise. After the stirring was continued for 30 min, the temperature was increased to 50℃. The pH value of the system was adjusted to 9 by using a 10% sodium hydroxide solution. The stirring was continued for 30 min to obtain a microcapsule solution.

[0049] Step A2, cetyltrimethylammonium bromide, a 1 mol / L hydrochloric acid solution, anhydrous ethanol, distilled water, tetraethyl orthosilicate and ammonium chloride were added into a reaction kettle. The stirring was carried out at a speed of 150 r / min for 3 h to obtain a mixture. The mixture was filtered. The filter cake was washed with a 40% ethanol solution until the washing liquid was neutral. Then the filter cake was calcined in a muffle furnace at 500℃ for 5 h to obtain carrier particles.

[0050] Step A3, the microcapsule solution obtained in step A1 was diluted 8 times with a 60% ethanol solution. Then the solution was transferred into a centrifuge tube. The carrier particles obtained in step A2 were added into the centrifuge tube. After the ultrasonic dispersion was carried out at a temperature of 60℃ and a frequency of 30 kHz for 30 min, the temperature was decreased to 4℃. The ultrasonic dispersion was continued at the same frequency for 30 min. Finally, the centrifugal treatment was carried out at a speed of 9000 r / min for 12 min at room temperature. The precipitate was washed with deionized water for 4 h. The freeze-drying was carried out at -45℃ until the weight was constant to obtain an intermediate.

[0051] Step A4, epichlorohydrin was added into a reactor. After the temperature was increased to 80℃ and kept for 2 h, a mixed solution a composed of 5,5-dimethylhydantoin and a sodium hydroxide solution was added into the reactor dropwise. The dropping speed was controlled at 2 drops / s. After the dropping was completed, the temperature was kept unchanged, and the stirring was carried out at a speed of 100 r / min for 20 min. Then the system was statically placed for 1 h to obtain a solution a.

[0052] Step A5, N,N'-dimethyl dodecyl tertiary amine and tetramethyl dichloro propyl disiloxane were added into a three-necked flask, then methanol and potassium iodide were added into the three-necked flask, stirring at 60 r / min for 4 min, then the three-necked flask was put into a magnetic heating stirrer, under the protection of nitrogen, the reaction temperature was controlled at 70℃, and the reaction was carried out under magnetic stirring for 24 h, after the reaction was completed, the solvent methanol was removed by rotary evaporation under reduced pressure, then recrystallization was carried out in a solution mixed by acetone and anhydrous ethanol at a volume ratio of 1:1, the filter cake was washed with deionized water for 4 times, and finally dried at 50℃ until the weight was constant, to obtain solid b;

[0053] Step A6, solid b and tetrahydrofuran were added into a reaction kettle, 2-aminobutanol and triethylamine were mixed uniformly at a volume ratio of 1:3, and then added into the reaction kettle by a constant pressure dropping funnel, the dropping speed was controlled at 1 drop / s, after the dropping was completed, the reaction was carried out at 0℃ for 2.5 h under stirring at 100 r / min, then the reaction was carried out at 30℃ for 2.5 h under the same stirring speed, and finally the reaction was carried out at 50℃ for 18 h, after the reaction was completed, filtration was carried out, the filter cake was washed with a 35% ethanol solution for 4 times, and finally dried in an oven at 55℃ until the weight was constant, to obtain solid c.

[0054] Step A7, solid c and toluene were added into a three-necked flask, ultrasonic dispersion was carried out at a frequency of 30 kHz for 10 min, then solution a was added dropwise into the three-necked flask, after the dropping was completed, the reaction was carried out at 40℃ for 24 h under stirring at 150 r / min, to obtain solution d, then the intermediate was added into a three-necked flask, and the reaction was carried out at 100℃ for 4 h under reflux, after the reaction was completed, centrifugal treatment was carried out at a speed of 7000 r / min for 10 min, the filter cake was washed with toluene for 3 times, and finally dried in a vacuum drying oven at 60℃ for 24 h, to obtain the composite filler.

[0055] Example 3

[0056] The composite filler was prepared by the following steps:

[0057] Step A1, peppermint essential oil was added into a three-necked flask, the stirring speed was controlled at 120 r / min, and the emulsifier was added into the three-necked flask by a constant pressure dropping funnel while stirring. After the dropping was completed, the stirring was continued for 10 min to obtain a core solution. Gelatin, gum arabic and deionized water were added into the reaction kettle, and the temperature was increased to 90℃. The stirring was carried out at a speed of 100 r / min for 20 min. The core solution was added. The stirring speed was increased to 300 r / min under the condition of a constant temperature water bath at 50℃. After the stirring reaction was carried out for 20 min, the pH value of the system was adjusted to 4.5 by using a 10% acetic acid solution. Then the stirring speed was controlled at 80 r / min, and the temperature was decreased to below 10℃. A 25% glutaraldehyde solution was added into the reaction kettle dropwise. The stirring was continued for 30 min. The temperature was increased to 50℃. The pH value of the system was adjusted to 10 by using a 10% sodium hydroxide solution. The stirring was continued for 30 min to obtain a microcapsule solution.

[0058] Step A2, cetyltrimethylammonium bromide, a 1 mol / L hydrochloric acid solution, anhydrous ethanol, distilled water, tetraethyl orthosilicate and ammonium chloride were added into a reaction kettle. The stirring was carried out at a speed of 200 r / min for 4 h to obtain a mixture. The mixture was filtered. The filter cake was washed with a 40% ethanol solution until the washing liquid was neutral. Then the filter cake was calcined in a muffle furnace at 500℃ for 5 h to obtain carrier particles.

[0059] Step A3, the microcapsule solution obtained in step A1 was diluted 10 times with a 60% ethanol solution. Then the solution was transferred into a centrifuge tube. The carrier particles obtained in step A2 were added into the centrifuge tube. The ultrasonic dispersion was carried out at a temperature of 60℃ and a frequency of 45 kHz for 30 min. The temperature was decreased to 4℃. The ultrasonic dispersion was continued at the same frequency for 30 min. Finally, the centrifugal treatment was carried out at a speed of 9000 r / min for 15 min at room temperature. The precipitate was washed with deionized water for 5 h. The freeze-drying was carried out at -45℃ until the weight was constant to obtain an intermediate.

[0060] Step A4, epichlorohydrin was added into a reactor. The temperature was increased to 80℃ and kept for 2 h. Then a mixed solution a composed of 5,5-dimethylhydantoin and a sodium hydroxide solution was added into the reactor dropwise. The dropping speed was controlled at 3 drops / s. After the dropping was completed, the temperature was kept unchanged. The stirring was carried out at a speed of 100 r / min for 20 min. Then the system was statically placed for 1 h to obtain a solution a.

[0061] Step A5, N,N'-dimethyl dodecyl tertiary amine and tetramethyl dichloropropyl disiloxane are added into a three-necked flask, then methanol and potassium iodide are added into the three-necked flask, stirring at 60 r / min for 5 min, then the three-necked flask is placed in a magnetic heating stirrer, the reaction temperature is controlled at 70℃ under nitrogen protection, and the reaction is stirred at a magnetic speed for 24 h, after the reaction is completed, the solvent methanol is removed by rotary evaporation under reduced pressure, then recrystallization is performed in a solution mixed according to a volume ratio of 1:1 of acetone and anhydrous ethanol, filtration is performed, the filter cake is washed with deionized water for 5 times, and finally drying is performed at 50℃ until the weight is constant to obtain solid b;

[0062] Step A6, solid b and tetrahydrofuran are added into a reaction kettle, 2-aminobutanol and triethylamine are uniformly mixed according to a volume ratio of 1:3, and then the mixture is added into the reaction kettle through a constant pressure dropping funnel, the dropping speed is controlled at 1 drop / s, after the dropping is completed, the reaction is performed at 0℃ for 2.5 h under stirring at 100 r / min, the stirring speed is unchanged, then the reaction is performed at 30℃ for 2.5 h, and finally the reaction is performed at 50℃ for 18 h, after the reaction is completed, filtration is performed, the filter cake is washed with a 35% ethanol solution for 3-5 times, and finally drying is performed in an oven at 60℃ until the weight is constant to obtain solid c;

[0063] Step A7, solid c and toluene are added into a three-necked flask, ultrasonic dispersion is performed at a frequency of 40 kHz for 10 min, then solution a is added dropwise into the three-necked flask, after the dropping is completed, the reaction is performed at 40℃ for 24 h under stirring at 200 r / min to obtain solution d, the intermediate is added into a three-necked flask, then reflux reaction is performed at 100℃ for 4 h, after the reaction is completed, centrifugal treatment is performed at a speed of 8000 r / min for 10 min, the filter cake is washed with toluene for 3 times, and finally drying is performed in a vacuum drying box at 60℃ for 24 h to obtain the composite filler.

[0064] Example 4

[0065] A waterproof and elastic non-woven fabric mask is prepared by the following steps:

[0066] First step, the polyester non-woven fabric is soaked in the impregnating solution for 10 seconds, the excess impregnating solution is rolled off by using a vertical small roller, the rolling rate is 50%, two-impregnation and two-rolling are adopted, then the non-woven fabric is placed in a blowing drying box, pre-drying is performed at 80℃ for 5 min, then baking is performed at 150℃ for 20 min, after that, the non-woven fabric is taken out, washed with water, and dried at 60℃ until the weight is constant to obtain the outer non-woven fabric layer;

[0067] Second step, the inner non-woven fabric layer, the activated carbon non-woven fabric layer and the outer non-woven fabric layer are stacked in sequence, and then one-time composite molding is performed to obtain the waterproof and elastic non-woven fabric mask.

[0068] The impregnating solution is prepared by the following steps:

[0069] Polyethylene glycol and polydimethylsiloxane were added into a reaction kettle, and the temperature was raised to 85°C. After stirring at 200 r / min for 20 min under nitrogen protection, isophorone diisocyanate was added dropwise into the reaction kettle. After the dropwise addition was completed, dibutyltin dilaurate was added, and the reaction was kept for 30 min. Then dimethylol acrylamide was added, and the reaction was kept for another 2 h. After the reaction was completed, acetone was added to adjust the viscosity to 1000 centipoise. After being cooled to room temperature, triethylamine was added to adjust the pH value of the system to 7. Finally, deionized water and the composite filler in Example 1 were added, and high-speed dispersion was carried out at 1500 r / min for 30 min to obtain the impregnating solution.

[0070] Example 5

[0071] A waterproof and elastic non-woven fabric mask was prepared by the following steps:

[0072] In the first step, the polyester non-woven fabric was soaked in the impregnating solution for 15 seconds. The excess impregnating solution was rolled off by using a vertical small roller, and the rolling rate was 50%. Then, the non-woven fabric was soaked and rolled twice, and then was placed in a blowing drying oven for pre-drying at 80°C for 5 min, and then was baked at 150°C for 20 min. After that, the non-woven fabric was taken out, washed with water, and dried at 60°C to a constant weight to obtain the outer non-woven fabric layer.

[0073] In the second step, the inner non-woven fabric layer, the activated carbon non-woven fabric layer, and the outer non-woven fabric layer were stacked in sequence, and then were once compounded and formed to obtain the waterproof and elastic non-woven fabric mask.

[0074] The impregnating solution was prepared by the following steps:

[0075] Polyethylene glycol and polydimethylsiloxane were added into a reaction kettle, and the temperature was raised to 85°C. After stirring at 200 r / min for 20 min under nitrogen protection, isophorone diisocyanate was added dropwise into the reaction kettle. After the dropwise addition was completed, dibutyltin dilaurate was added, and the reaction was kept for 30 min. Then dimethylol acrylamide was added, and the reaction was kept for another 2 h. After the reaction was completed, acetone was added to adjust the viscosity to 1000 centipoise. After being cooled to room temperature, triethylamine was added to adjust the pH value of the system to 7. Finally, deionized water and the composite filler in Example 1 were added, and high-speed dispersion was carried out at 1500 r / min for 30 min to obtain the impregnating solution.

[0076] Example 6

[0077] A waterproof and elastic non-woven fabric mask was prepared by the following steps:

[0078] In the first step, the polyester non-woven fabric was soaked in the impregnating solution for 15 seconds. The excess impregnating solution was rolled off by using a vertical small roller, and the rolling rate was 50%. Then, the non-woven fabric was soaked and rolled twice, and then was placed in a blowing drying oven for pre-drying at 80°C for 5 min, and then was baked at 150°C for 20 min. After that, the non-woven fabric was taken out, washed with water, and dried at 60°C to a constant weight to obtain the outer non-woven fabric layer.

[0079] Secondly, the inner non-woven fabric layer, the activated carbon non-woven fabric layer and the outer non-woven fabric layer are stacked in sequence and then once compounded to form a waterproof and elastic non-woven fabric mask.

[0080] The impregnation liquid is prepared by the following steps:

[0081] Polyethylene glycol and polydimethylsiloxane are added into a reaction kettle, and the temperature is raised to 85 DEG C. After stirring at a speed of 200 r / min for 20 min under nitrogen protection, isophorone diisocyanate is added dropwise into the reaction kettle. After the dropwise addition is completed, dibutyl tin dilaurate is added, and the reaction is kept for 30 min. Then dimethylol acrylate is added, and the reaction is kept for another 2 h. After the reaction is completed, acetone is added to adjust the viscosity to 1500 centipoises. After cooling to room temperature, triethylamine is added to adjust the pH value of the system to 8. Finally, deionized water and the composite filler of Example 3 are added, and high-speed dispersion is carried out at a speed of 1500 r / min for 50 min to obtain the impregnation liquid.

[0082] Comparative Example

[0083] The non-woven fabric mask in the present comparative example is commonly seen in the market.

[0084] Examples 4-6 and the comparative example are subjected to performance testing. According to GB / T20944.3-2008 "Evaluation Method for Antibacterial Performance of Textiles Part 3: Oscillation Method", the antibacterial inhibition rate of the fabric to Escherichia coli and Staphylococcus aureus is tested. According to GB / T5453-1997 "Determination of Air Permeability of Textile Fabrics", the air permeability is determined. According to GB / T1270-1991 standard, the moisture permeability is tested. 12 people are randomly selected and divided into three groups. The masks of Examples 1-3 and the comparative example are worn for 12 h, and sensory evaluation is carried out. The evaluation results are shown in the following table:

[0085]

[0086] As shown in the above table, the masks of Examples 4-6 are superior to the comparative example in the antibacterial inhibition rate, air permeability, moisture permeability and sensory evaluation test, which indicates that the masks prepared in the present application have high antibacterial, air permeability, moisture permeability and practical use performance.

[0087] The above content is only an example and description of the concept of the present application. Those skilled in the art can make various modifications or supplements or use similar ways to replace the described specific examples, as long as the modifications or supplements or replacements do not deviate from the concept of the present application or exceed the scope defined by the present claims, which shall belong to the protection scope of the present application.

Claims

1. A waterproof elastic nonwoven cloth mask, characterized by, From top to bottom, it comprises an outer non-woven fabric layer, an activated carbon non-woven fabric layer and an inner non-woven fabric layer; the outer non-woven fabric layer is obtained by twice-dipping and twice-rolling treatment of polyester non-woven fabric soaked in an impregnating solution; The impregnating solution is prepared by the following steps: Polyethylene glycol and polydimethylsiloxane are added into a reaction kettle, and the temperature is raised to 85℃ under nitrogen protection; after stirring for 20 min, isophorone diisocyanate is added dropwise into the reaction kettle; after the dropwise addition is completed, dibutyltin dilaurate is added, and the reaction is kept for 30 min; then dimethylol acrylate is added, and the reaction is kept for 2 h; after the reaction is completed, acetone is added to adjust the viscosity to 1000-1500 centipoise; after cooling to room temperature, triethylamine is added to adjust the pH value of the system to 7-8; finally, deionized water and a composite filler are added, and high-speed dispersion is carried out for 30-50 min to obtain the impregnating solution; The composite filler is prepared by the following steps: In step A1, peppermint essential oil is added into a three-necked flask, and an emulsifier is added; after stirring for 5-10 min, a core solution is obtained; gelatin, gum arabic and deionized water are added into a reaction kettle, and the temperature is raised to 90℃; after stirring for 20 min, the core solution is added; after stirring for 20 min in a 50℃ constant-temperature water bath, the pH value of the system is controlled to be 4.4-4.5; the temperature is lowered to below 10℃; glutaraldehyde solution is added dropwise into the reaction kettle; after continuing to stir for 30 min, the temperature is raised to 50℃; the pH value of the system is adjusted to 9-10; and the stirring is continued for 30 min to obtain a microcapsule solution; In step A2, cetyltrimethylammonium bromide, a 1 mol / L hydrochloric acid solution, anhydrous ethanol, distilled water, tetraethyl orthosilicate and ammonium chloride are added into a reaction kettle; after stirring for 2-4 h, a mixed material is obtained; filtration is performed; the filter cake is washed and calcined to obtain carrier particles; In step A3, the microcapsule solution obtained in step A1 is diluted 5-10 times, and is transferred into a centrifuge tube; the carrier particles obtained in step A2 are added; after ultrasonic dispersion at a temperature of 60℃ for 30 min, the temperature is lowered to 4℃; ultrasonic dispersion is continued for 30 min; centrifugal treatment is performed at room temperature for 10-15 min; the precipitate is washed and dried to obtain an intermediate; In step A4, epichlorohydrin is added into a reactor; after keeping the temperature at 80℃ for 2 h, a mixed solution a composed of 5,5-dimethylhydantoin and a sodium hydroxide solution is added dropwise into the reactor; after the dropwise addition is completed, stirring is performed for 20 min; after standing for 1 h, a solution a is obtained; In step A5, N,N'-dimethyldodecylamine and tetramethyldichloropropyl disiloxane are added into a three-necked flask; methanol and potassium iodide are further added into the three-necked flask; after stirring for 3-5 min, the reaction temperature is controlled at 70℃ under nitrogen protection; magnetic stirring is performed for 24 h; after the reaction is completed, rotary evaporation is performed under reduced pressure; recrystallization is performed; filtration is performed; and washing and drying are performed to obtain a solid b; In step A6, the solid b and tetrahydrofuran are added into a reaction kettle; 2-aminobutanol and triethylamine are mixed uniformly according to a volume ratio of 1:3, and are added dropwise into the reaction kettle; after the dropwise addition is completed, the reaction temperature is controlled at 0℃; the reaction is performed for 2.5 h; then the reaction is performed for 2.5 h at 30℃; finally, the reaction is performed for 18 h at 50℃; after the reaction is completed, filtration is performed; the filter cake is washed and dried to obtain a solid c; Step A7, solid c and toluene were added into a three-necked flask, after ultrasonic dispersion for 10 min, solution a was added dropwise into the three-necked flask, after the dropwise addition was completed, the reaction temperature was controlled at 40 DEG C, and the reaction was carried out for 24 h to obtain a solution of d, then the intermediate was added into a three-necked flask, and the reaction was carried out at 100 DEG C under reflux for 4 h, after the reaction was completed, centrifugal treatment was carried out for 10 min, the filter cake was washed with toluene for 3 times, and finally drying was carried out in a vacuum drying box at 60 DEG C for 24 h to obtain a composite filler.

2. The method of claim 1, wherein the waterproof elastic nonwoven fabric mask is prepared by the steps of: The method comprises the following steps: The polyester non-woven fabric is soaked in the impregnating solution for 10-20 seconds, the excess impregnating solution is rolled off by using a vertical small rolling machine, the rolling rate is 50%, two-impregnation and two-rolling are adopted, then the non-woven fabric is placed into a blowing drying box and pre-dried at 80 DEG C for 5 min, then baked at 150 DEG C for 20 min, then taken out, washed, and dried at 60 DEG C to constant weight to obtain the outer non-woven fabric layer; The inner non-woven fabric layer, the activated carbon non-woven fabric layer and the outer non-woven fabric layer are stacked in sequence, and then one-time composite molding is carried out to obtain a waterproof and elastic non-woven fabric mask.

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