An antibacterial and flame-retardant mask and its preparation method

Abstract

The present disclosure provides a method for preparing an antibacterial and flame-retardant mask, which relates to the field of masks. The method includes the following steps: (1) preparing a cotton spunlace non-woven fabric layer; (2) preparing a polypropylene melt-blown non-woven fabric protective layer; (3) preparing an antibacterial and flame-retardant layer; (4) a polypropylene melt-blown non-woven fabric protective layer; (5) stacking the fabrics in steps (1)-(4) from the inside to the outside in sequence, cutting to the required size; and inserting a nose clip above, performing embossing edge sealing on the outer side, and fixing and bonding the ear straps to the four corners of the mask body through hot melt adhesive and embossing; the antibacterial and flame-retardant layer is prepared by melt-blending a flame-retardant antibacterial nano modifier and polypropylene, spinning into a web, strengthening and finishing, and drying; the flame-retardant antibacterial nano modifier is an in-situ generated silver SiO2 / Al2O3 nanoporous hollow microsphere. The mask prepared by the present invention has good mechanical properties, good high-temperature resistance and flame-retardant effect, is not easy to cause allergic symptoms, has extremely high bactericidal effect and filtration effect, and has good inhalation and exhalation effects, and has broad application prospects.

Description

Technical Field

[0001] The present disclosure relates to the technical field of masks, and specifically discloses an antibacterial and flame-retardant mask and a preparation method thereof. Background Art

[0002] A mask is a protective article that is worn over the mouth and nose of a person to filter the air entering the mouth and nose, so as to block the entry of harmful gases, odors, dust, droplets, etc. into and out of the mouth and nose of the wearer. There are various forms of masks, and their main function is to form an air filtration layer between a person's nose and mouth and the outside world to prevent germs or soot and dust from directly entering the mouth and nose. Medical masks are generally divided into medical protective masks, medical surgical masks and disposable medical masks. The requirement for wearing a medical mask is that the mask must fit tightly with the face to a certain extent. If the face shape does not match the inherent shape of the mask and a tight fit cannot be achieved, the respiratory protection may fail, resulting in an increased risk of virus infection during the epidemic.

[0003] Traditional masks mostly adopt a simple rectangular planar structure formed by stacking multiple layers of disinfected gauze, generally a three-layer filter element (SMS structure), namely a spunbond layer (S), a meltblown layer (M), and a spunbond layer (S). The spunbond layer is close to the face, covering the oral and nasal cavity parts, and is fastened to the auricle by a mask strap.

[0004] Chinese Invention Application CN106307711A discloses a warm mask with a detachable self-heating patch, which includes a mask body, a self-heating patch, and ear straps arranged on both sides of the mask body. The mask body includes an outer layer and a cotton bag. The lower edges of the outer layer and the cotton bag are stitched and connected. The self-heating patch is inserted between the outer layer and the cotton bag. The cotton bag is filled with a cotton floc layer. An opening is provided on the cotton bag, and a zipper is provided in the opening. With this kind of mask, a detachable self-heating patch is provided inside the mask. The self-heating patch can be a mature disposable self-heating patch on the market. When in use, tear off the release paper on the back of the self-heating patch and stick it inside the mask. A cotton bag with an adjustable thickness of the cotton floc layer can be used to open the upper opening through the zipper, take out the cotton floc layer, or add a cotton floc layer, so as to automatically adjust the distance between the self-heating patch and the face, preventing chronic burns due to excessive temperature or ineffective warmth due to low temperature. A filter sheet, a sterilization sheet, an odor removal sheet, a pollen removal sheet, etc. can also be provided between the outer layer and the cotton bag. This invention realizes its functions of warmth, filtration, sterilization, odor removal, and pollen removal by adding different functional sheets. Through the combination of different functional sheets, more combinations of various different functions can be achieved to create a more suitable facial air environment. However, the combination of multiple functional sheets will inevitably lead to an increase in the volume of facial protection products, making them inconvenient to use. Moreover, disposable self-heating patches generally generate heat by the oxidation of a variety of compound powders in contact with air. When the sealing of the self-heating patch is not good, it is extremely easy to leak into the respiratory tract or harm the facial skin. When the sealing of the self-heating patch is good, it may cause a large air resistance, making it difficult for the user to breathe. Summary of the Invention

[0005] To solve the above problems, the present disclosure provides an antibacterial and flame-retardant mask and its preparation method, which has good mechanical properties, good high-temperature resistance and flame-retardant effects, is not easy to cause allergic symptoms, has extremely high sterilization and filtration effects, and has good inhalation and exhalation effects, and has broad application prospects.

[0006] The present invention provides a preparation method of an antibacterial and flame-retardant mask, including the following steps:

[0007] (1) Prepare a cotton spunlace non-woven fabric layer;

[0008] (2) Prepare a polypropylene meltblown non-woven fabric protective layer;

[0009] (3) Prepare an antibacterial and flame-retardant layer;

[0010] (4) A polypropylene meltblown non-woven fabric protective layer;

[0011] (5) Stack the fabrics in steps (1)-(4) from the inside to the outside in sequence, cut to the required size; and install a nose clip on the upper part, and perform embossing and sealing on the outer side. Fix and bond the ear straps to the four corners of the mask body through hot melt adhesive and embossing.

[0012] The antibacterial and flame-retardant layer is prepared by melt blending a flame-retardant antibacterial nano-modifier and polypropylene, spinning into a web, strengthening and finishing, and drying.

[0013] The flame-retardant antibacterial nano-modifier is SiO2 / Al2O3 nano-porous hollow microspheres with in-situ generated silver.

[0014] As a further improvement, the preparation method of the flame-retardant antibacterial nano-modifier is as follows:

[0015] S1. Dissolve tetraethyl orthosilicate and aluminum isopropoxide in an organic solvent to obtain an oil phase.

[0016] S2. Dissolve a pore-forming agent and an emulsifier in water to obtain an aqueous phase.

[0017] S3. Drop the aqueous phase prepared in step S2 into the oil phase prepared in step S1, adjust the pH of the solution, emulsify, stir and react, centrifuge, wash, and dry to obtain SiO2 / Al2O3 nano-porous hollow microspheres.

[0018] S4. Drop ammonia water into silver nitrate until the precipitate just completely disappears to obtain a silver ammonia complex ion solution.

[0019] S5. Disperse the SiO2 / Al2O3 nano-porous hollow microspheres prepared in step S3 in water, add glucose, stir and mix evenly, centrifuge, wash, and dry. Disperse the obtained microspheres in water, add the silver ammonia complex ion solution prepared in step S4, heat and stir to react, centrifuge, wash, and dry to obtain SiO2 / Al2O3 nano-porous hollow microspheres with in-situ generated silver, that is, the flame-retardant antibacterial nano-modifier.

[0020] As a further improvement, the mass ratio of tetraethyl orthosilicate to aluminum isopropoxide in step S1 is 3 - 5:1.

[0021] As a further improvement, the pore-forming agent in step S2 is polyoxyethylene sorbitan fatty acid ester or polyoxyethylene octylphenyl ether; the emulsifier is the hydrolyzate of the sodium salt of styrene-maleic anhydride alternating copolymer, and its number average molecular weight is 30000 - 75000; the mass ratio of the pore-forming agent to the emulsifier is 3 - 5:2.

[0022] As a further improvement, the mass ratio of the aqueous phase to the oil phase in step S3 is 3 - 5:7 - 10; the adjusted solution pH value is 8 - 9, the rotation speed of emulsification is 12000 - 15000 r / min, the time is 3 - 5 min, and the reaction time is 1 - 2 h.

[0023] As a further improvement, the concentration of silver nitrate in step S4 is 2 - 3 mol / L.

[0024] As a further improvement, in step S5, the mass ratio of SiO2 / Al2O3 nanoporous hollow microspheres, glucose, and silver ammine complex ion solution is 10:1-3:2-5; the heating temperature is 70-90°C, and the stirring reaction time is 30-50min.

[0025] As a further improvement, the preparation method of the antibacterial flame retardant layer is as follows: the flame retardant and antibacterial nano-modifier and polypropylene are mixed and extrude and melt through a screw extruder to obtain a melt, which is sprayed out through a spinneret of a spinning machine, cooled and solidified into filaments, which are pulled by a drawing air flow, blown to a drum, and collected on the drum to obtain a fiber web, the fiber webs are overlapped and entered into a solution jet spinning area for reinforcement, and sent into an oven for drying to obtain an antibacterial flame retardant layer.

[0026] As a further improvement, the mass ratio of the flame retardant and antibacterial nano-modifier to polypropylene is 1-2:7-10; and the melting temperature is 180-220°C.

[0027] The present invention further protects an antibacterial flame-retardant mask prepared by the above-mentioned preparation method.

[0028] Beneficial effects: The flame retardant and antibacterial nano-modifier is prepared by sol-gel reaction, which is a SiO2 / Al2O3 nano-porous hollow microsphere with in-situ silver generation, and its shell material is a mixture of SiO2 and Al2O3, which not only has excellent mechanical strength, but also can significantly improve the high temperature resistance and flame retardant effects of the material after adding polypropylene. At the same time, glucose is used to reduce the silver in the silver ammonia complex ion to form a silver element, and in-situ generation is performed. The prepared SiO2 / Al2O3 nano-porous hollow microsphere with in-situ silver generation promotes the output of silver ions when used, thereby having excellent antibacterial and antibacterial effects. At the same time, the structure of the nano-hollow porous sphere can promote polypropylene to enter the microsphere during the melting process, and will not affect the extension of the polypropylene molecular chain, thereby playing a good role in promoting the compatibility and dispersibility of the SiO2 / Al2O3 nano-porous hollow microsphere with in-situ silver generation in polypropylene, so that the material still has good mechanical properties after modification by the nano-modifier.

[0029] The mask prepared by the invention has good mechanical properties, high temperature resistance and flame retardant effects, is not easy to cause allergic symptoms, has extremely high sterilization effect and filtering effect, and has good inhalation and exhalation effects, and has broad application prospects. DETAILED DESCRIPTION

[0030] Example 1

[0031] This embodiment provides a method for preparing an antibacterial flame retardant mask:

[0032] (1) preparing a cotton spunlace nonwoven fabric layer;

[0033] (2) Prepare a polypropylene meltblown non-woven fabric protective layer;

[0034] (3) Prepare an antibacterial and flame-retardant layer;

[0035] (4) Polypropylene meltblown non-woven fabric protective layer;

[0036] (5) Stack the steps (1)-(4) from the inside to the outside in sequence, cut to the required size; and install a nose clip through insertion on the upper part, perform embossing and edge sealing on the outer side, and fix and bond the ear straps to the four corners of the mask body through hot melt adhesive and embossing;

[0037] The preparation method of the antibacterial and flame-retardant layer is as follows: Mix 10 parts by weight of a flame-retardant antibacterial nano-modifier and 70 parts by weight of polypropylene, then extrude through a screw extruder, heat to 180 °C to obtain a melt, extrude it through the spinneret of a spinning machine, cool and solidify into filaments, draw and air-draw the filaments, blow them onto a roller, and collect them on the roller to obtain a fiber web. Overlap the fiber web and enter the solution spray spinning area for reinforcement, then send it into an oven for drying to obtain the antibacterial and flame-retardant layer;

[0038] The preparation method of the flame-retardant antibacterial nano-modifier is as follows:

[0039] S1. Dissolve 3 parts by weight of tetraethyl orthosilicate and 1 part by weight of aluminum isopropoxide in 10 parts by weight of an organic solvent to obtain an oil phase;

[0040] S2. Dissolve 3 parts by weight of polyethylene glycol octyl phenyl ether and 2 parts by weight of an emulsifier in 100 parts by weight of water to obtain an aqueous phase; the emulsifier is the hydrolyzate of the sodium salt of a styrene-maleic anhydride alternating copolymer, and its number average molecular weight is 30000;

[0041] S3. Drop 30 parts by weight of the aqueous phase prepared in step S2 into 70 parts by weight of the oil phase prepared in step S1, adjust the pH of the solution to 8, emulsify at 12000 r / min for 3 min, stir and react for 1 h, centrifuge, wash, and dry to obtain SiO2 / Al2O3 nanoporous hollow microspheres;

[0042] S4. Drop 28 wt% ammonia water into 2 mol / L silver nitrate until the precipitate just completely disappears to obtain a silver ammonia complex ion solution;

[0043] S5. Disperse 10 parts by weight of the SiO2 / Al2O3 nanoporous hollow microspheres prepared in step S3 in water, add 1 part by weight of glucose, stir and mix evenly, then centrifuge, wash, and dry. Disperse the obtained microspheres in water, add 2 parts by weight of the silver ammonia complex ion solution prepared in step S4, heat and stir to react, centrifuge, wash, and dry to obtain SiO2 / Al2O3 nanoporous hollow microspheres with in-situ generated silver, that is, the flame-retardant antibacterial nano-modifier.

[0044] Example 2

[0045] This example provides a method for preparing an antibacterial and flame-retardant mask:

[0046] (1) Prepare a cotton spunlace non-woven fabric layer;

[0047] (2) Prepare a polypropylene meltblown non-woven fabric protective layer;

[0048] (3) Prepare an antibacterial and flame-retardant layer;

[0049] (4) Polypropylene meltblown non-woven fabric protective layer;

[0050] (5) Stack the fabrics in steps (1)-(4) from the inside to the outside in sequence, cut to the required size; and install a nose clip inserted above, perform embossing sealing on the outer side, and fix and bond the ear straps to the four corners of the mask body through hot melt adhesive and embossing;

[0051] The preparation method of the antibacterial and flame-retardant layer is as follows: Mix 20 parts by weight of a flame-retardant antibacterial nano-modifier and 100 parts by weight of polypropylene, and then extrude through a screw extruder, heat to 220 °C to obtain a melt, extrude it through the spinneret of a spinning machine, cool and solidify into filaments, draw and air-draw the filaments, blow them towards a roller, and collect them on the roller to obtain a fiber web. Overlap the fiber web and enter the solution jet spinning area for reinforcement, and send it into an oven for drying to obtain the antibacterial and flame-retardant layer;

[0052] The preparation method of the flame-retardant antibacterial nano-modifier is as follows:

[0053] S1. Dissolve 5 parts by weight of tetraethyl orthosilicate and 1 part by weight of aluminum isopropoxide in 10 parts by weight of an organic solvent to obtain an oil phase;

[0054] S2. Dissolve 5 parts by weight of polyoxyethylene sorbitan fatty acid ester and 2 parts by weight of an emulsifier in 100 parts by weight of water to obtain an aqueous phase; the emulsifier is the hydrolyzate of the sodium salt of a styrene-maleic anhydride alternating copolymer, and its number average molecular weight is 75000;

[0055] S3. Drop 50 parts by weight of the aqueous phase prepared in step S2 into 100 parts by weight of the oil phase prepared in step S1, adjust the pH of the solution to 9, emulsify at 15000 r / min for 5 min, stir and react for 2 h, centrifuge, wash, and dry to obtain SiO2 / Al2O3 nanoporous hollow microspheres;

[0056] S4. Drop 28 wt% ammonia water into 3 mol / L silver nitrate until the precipitate just completely disappears to obtain a silver ammonia complex ion solution;

[0057] S5. Disperse 10 parts by weight of the SiO2 / Al2O3 nanoporous hollow microspheres prepared in step S3 in water, add 3 parts by weight of glucose, stir and mix evenly, then centrifuge, wash, and dry. The obtained microspheres are dispersed in water, add 5 parts by weight of the silver ammonia complex ion solution prepared in step S4, heat and stir to react, centrifuge, wash, and dry to obtain SiO2 / Al2O3 nanoporous hollow microspheres with in-situ generated silver, namely the flame-retardant and antibacterial nano modifier.

[0058] Example 3

[0059] This example provides a preparation method of an antibacterial and flame-retardant mask:

[0060] (1) Prepare a cotton spunlace non-woven fabric layer;

[0061] (2) Prepare a polypropylene melt-blown non-woven fabric protective layer;

[0062] (3) Prepare an antibacterial and flame-retardant layer;

[0063] (4) Polypropylene melt-blown non-woven fabric protective layer;

[0064] (5) Stack the fabrics in steps (1)-(4) from the inside to the outside in sequence, cut to the required size; and install a nose clip on the upper part, perform embossing and edge sealing on the outer side, and fix and bond the ear straps to the four corners of the mask body through hot melt adhesive and embossing;

[0065] The preparation method of the antibacterial and flame-retardant layer is as follows: Mix 15 parts by weight of the flame-retardant and antibacterial nano modifier and 85 parts by weight of polypropylene, then extrude through a screw extruder, heat to 200 °C to obtain a melt, extrude through the spinneret of a spinning machine, cool and solidify into filaments, stretch and draw the filaments by air flow, blow them onto a drum, and collect them on the drum to obtain a fiber web. Overlap the fiber web and enter the solution jet spinning area for reinforcement, and then send it into an oven for drying to obtain the antibacterial and flame-retardant layer;

[0066] The preparation method of the flame-retardant and antibacterial nano modifier is as follows:

[0067] S1. Dissolve 4 parts by weight of tetraethyl orthosilicate and 1 part by weight of aluminum isopropoxide in 10 parts by weight of an organic solvent to obtain an oil phase;

[0068] S2. Dissolve 4 parts by weight of polyoxyethylene sorbitan fatty acid ester and 2 parts by weight of an emulsifier in 100 parts by weight of water to obtain an aqueous phase; the emulsifier is the hydrolyzate of the sodium salt of a styrene-maleic anhydride alternating copolymer, and its number average molecular weight is 50000;

[0069] S3. Add 40 parts by weight of the aqueous phase prepared in step S2 dropwise to 85 parts by weight of the oil phase prepared in step S1, adjust the pH of the solution to 8.5, emulsify at 13,500 r / min for 4 min, stir and react for 1.5 h, centrifuge, wash, and dry to obtain SiO2 / Al2O3 nanoporous hollow microspheres;

[0070] S4. Dropwise add 28 wt% ammonia water to 2.5 mol / L silver nitrate until the precipitate just completely disappears to obtain a silver ammonia complex ion solution;

[0071] S5. Disperse 10 parts by weight of the SiO2 / Al2O3 nanoporous hollow microspheres prepared in step S3 in water, add 2 parts by weight of glucose, stir and mix evenly, centrifuge, wash, and dry. Disperse the obtained microspheres in water, add 3.5 parts by weight of the silver ammonia complex ion solution prepared in step S4, heat and stir to react, centrifuge, wash, and dry to obtain SiO2 / Al2O3 nanoporous hollow microspheres with in-situ generated silver, namely the flame retardant and antibacterial nano modifier.

[0072] Comparative Example 1

[0073] Compared with Example 3, the difference lies in that in the preparation of the flame retardant and antibacterial nano modifier, tetraethyl orthosilicate was not added in step S1.

[0074] Comparative Example 2

[0075] Compared with Example 3, the difference lies in that in the preparation of the flame retardant and antibacterial nano modifier, aluminum isopropoxide was not added in step S1.

[0076] Comparative Example 3

[0077] Compared with Example 3, the difference lies in that in the preparation of the flame retardant and antibacterial nano modifier, the pore-forming agent was not added in step S1.

[0078] Comparative Example 4

[0079] Compared with Example 3, the difference lies in that in the preparation of the flame retardant and antibacterial nano modifier, steps S4 - S5 were not carried out.

[0080] Test Example 1

[0081] Perform mechanical property tests on the antibacterial and flame retardant masks prepared in Examples 1 - 3 and Comparative Examples 1 - 4 of the present invention, and the results are shown in Table 1.

[0082] Table 1

[0083]

[0084]

[0085] As can be seen from the above table, the antibacterial and flame-retardant mask prepared by the present invention has good mechanical properties.

[0086] Test Example 2

[0087] The antibacterial and flame-retardant masks prepared in Examples 1-3 and Comparative Examples 1-4 of the present invention were tested for flame retardancy, and the results are shown in Table 2.

[0088] Table 2

[0089] Group Limiting oxygen index (%) Example 1 26 Example 2 27 Example 3 29 Comparative Example 1 22 Comparative Example 2 16 Comparative Example 3 20 Comparative Example 4 23

[0090] As can be seen from the above table, the antibacterial and flame-retardant mask prepared by the present invention has good flame retardancy.

[0091] Test Example 3

[0092] The antibacterial and flame-retardant masks prepared in Examples 1-3 and Comparative Examples 1-4 were tested by the oscillating method (GB / T20944.3-2008). The results are shown in Table 3.

[0093] Table 3

[0094]

[0095]

[0096] As can be seen from the above table, the antibacterial and flame-retardant mask prepared by the present invention has good antibacterial properties.

[0097] The above are only the embodiments of the present disclosure and are not intended to limit the present disclosure. Any modifications, equivalent replacements, improvements, etc. made within the principles of the present disclosure shall be included within the protection scope of the present disclosure.

Claims

1. A preparation method of an antibacterial and flame-retardant mask, characterized in that, It includes the following steps: (1) Prepare a cotton spunlace non-woven fabric layer; (2) Prepare a polypropylene meltblown non-woven fabric protective layer; (3) Prepare an antibacterial and flame-retardant layer; (4) Polypropylene meltblown non-woven fabric protective layer; (5) Stack the fabrics in steps (1)-(4) from the inside to the outside in sequence, cut to the required size; and install a nose clip inserted from above, perform embossing and edge sealing on the outer side, and fix and bond the ear straps to the four corners of the mask body through hot melt adhesive and embossing; The antibacterial and flame-retardant layer is prepared by melt blending a flame-retardant antibacterial nano modifier and polypropylene, spinning into a web, strengthening and finishing, and drying; The flame-retardant antibacterial nano modifier is a SiO2 / Al2O3 nano-porous hollow microsphere with in-situ generated silver; The preparation method of the flame-retardant antibacterial nano modifier is as follows: S1. Dissolve tetraethyl orthosilicate and aluminum isopropoxide in an organic solvent to obtain an oil phase; S2. Dissolve a pore-forming agent and an emulsifier in water to obtain an aqueous phase; S3. Drop the aqueous phase prepared in step S2 into the oil phase prepared in step S1, adjust the pH of the solution, emulsify, stir and react, centrifuge, wash, and dry to obtain SiO2 / Al2O3 nano-porous hollow microspheres; S4. Drop ammonia water into silver nitrate until the precipitate just completely disappears to obtain a silver ammonia complex ion solution; S5. Disperse the SiO2 / Al2O3 nano-porous hollow microspheres prepared in step S3 in water, add glucose, stir and mix evenly, then centrifuge, wash, and dry. The obtained microspheres are dispersed in water, add the silver ammonia complex ion solution prepared in step S4, heat and stir to react, centrifuge, wash, and dry to obtain a SiO2 / Al2O3 nano-porous hollow microsphere with in-situ generated silver, that is, the flame-retardant antibacterial nano modifier.

2. The preparation method according to claim 1, wherein, In step S1, the mass ratio of tetraethyl orthosilicate to aluminum isopropoxide is 3-5:

1.

3. The preparation method according to claim 1, characterized in that, In step S2, the pore-forming agent is polyoxyethylene sorbitan fatty acid ester or polyethyleneglycol octylphenyl ether; the emulsifier is the hydrolyzate of the sodium salt of styrene-maleic anhydride alternating copolymer, and its number average molecular weight is 30000-75000; the mass ratio of the pore-forming agent to the emulsifier is 3-5:

2.

4. The preparation method according to claim 1, characterized in that, In step S3, the mass ratio of the aqueous phase to the oil phase is 3-5:7-10; the pH value of the adjusted solution is 8-9, the rotation speed of the emulsification is 12000-15000 r / min, the time is 3-5 min, and the reaction time is 1-2 h.

5. The preparation method according to claim 1, characterized in that, In step S4, the concentration of silver nitrate is 2-3 mol / L.

6. The preparation method according to claim 1, characterized in that In step S5, the mass ratio of the SiO2 / Al2O3 nano-porous hollow microspheres, glucose, and silver ammonia complex ion solution is 10:1-3:2-5; the heating temperature is 70-90 °C, and the stirring reaction time is 30-50 min.

7. The preparation method according to claim 1, wherein The preparation method of the antibacterial and flame-retardant layer is as follows: Mix the flame-retardant antibacterial nano modifier and polypropylene, then extrude and melt them through a screw extruder to obtain a melt. After being ejected from the spinneret of the spinning machine, it is cooled and solidified into filaments, pulled by a draft air flow, blown onto a roller, and collected on the roller to obtain a fiber web. The fiber web is overlapped and enters the solution jet spinning area for strengthening, and then sent into an oven for drying to obtain the antibacterial and flame-retardant layer.

8. The preparation method according to claim 7, characterized in that, The mass ratio of the flame retardant and antibacterial nano modifier to polypropylene is 1-2:7-10; the melting temperature is 180-220 °C.

9. An antibacterial and flame retardant mask prepared by the preparation method according to any one of claims 1-8.

Images