CN111513395A - Novel antimicrobial environment-friendly mask and manufacturing method thereof - Google Patents
Novel antimicrobial environment-friendly mask and manufacturing method thereof Download PDFInfo
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- CN111513395A CN111513395A CN202010421310.6A CN202010421310A CN111513395A CN 111513395 A CN111513395 A CN 111513395A CN 202010421310 A CN202010421310 A CN 202010421310A CN 111513395 A CN111513395 A CN 111513395A
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- quaternary ammonium
- chitin
- mask
- spinning
- polylactic acid
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- A—HUMAN NECESSITIES
- A41—WEARING APPAREL
- A41D—OUTERWEAR; PROTECTIVE GARMENTS; ACCESSORIES
- A41D13/00—Professional, industrial or sporting protective garments, e.g. surgeons' gowns or garments protecting against blows or punches
- A41D13/05—Professional, industrial or sporting protective garments, e.g. surgeons' gowns or garments protecting against blows or punches protecting only a particular body part
- A41D13/11—Protective face masks, e.g. for surgical use, or for use in foul atmospheres
- A41D13/1192—Protective face masks, e.g. for surgical use, or for use in foul atmospheres with antimicrobial agent
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- A—HUMAN NECESSITIES
- A41—WEARING APPAREL
- A41D—OUTERWEAR; PROTECTIVE GARMENTS; ACCESSORIES
- A41D31/00—Materials specially adapted for outerwear
- A41D31/04—Materials specially adapted for outerwear characterised by special function or use
- A41D31/10—Impermeable to liquids, e.g. waterproof; Liquid-repellent
- A41D31/102—Waterproof and breathable
-
- A—HUMAN NECESSITIES
- A41—WEARING APPAREL
- A41D—OUTERWEAR; PROTECTIVE GARMENTS; ACCESSORIES
- A41D31/00—Materials specially adapted for outerwear
- A41D31/04—Materials specially adapted for outerwear characterised by special function or use
- A41D31/14—Air permeable, i.e. capable of being penetrated by gases
- A41D31/145—Air permeable, i.e. capable of being penetrated by gases using layered materials
-
- A—HUMAN NECESSITIES
- A41—WEARING APPAREL
- A41D—OUTERWEAR; PROTECTIVE GARMENTS; ACCESSORIES
- A41D31/00—Materials specially adapted for outerwear
- A41D31/04—Materials specially adapted for outerwear characterised by special function or use
- A41D31/30—Antimicrobial, e.g. antibacterial
- A41D31/305—Antimicrobial, e.g. antibacterial using layered materials
Abstract
The invention provides a novel antimicrobial environment-friendly mask and a manufacturing method thereof. The novel antimicrobial environment-friendly mask comprises a mask main body, ear bands and a nose strip, wherein the mask main body is formed by sequentially bonding an outer layer, a filter layer and an inner layer, the outer layer is made of quaternary ammonium salinized chitin non-woven fabric coated with a quaternary ammonium salinized chitin-polylactic acid composite nanofiber membrane, the filter layer is made of 1-2 layers of quaternary ammonium salinized chitin nanofiber felts, and the inner layer is made of quaternary ammonium salinized chitin non-woven fabric which is close to skin and absorbs moisture. The mask has the advantages of wide raw material sources, low cost, simple manufacturing process and natural degradation, can continuously adsorb and kill microbes such as bacteria, viruses and the like by utilizing the electrostatic action of quaternary ammonium salt ions, solves the problem that the traditional medical protective mask has no antibacterial property, can greatly prolong the service time while ensuring the air permeability, can not cause secondary pollution and white pollution of pathogenic microbes when being discarded, can relieve the situation of shortage of medical mask resources, and can effectively inhibit the diffusion of infection.
Description
Technical Field
The invention belongs to the field of medical material development, and particularly relates to a novel antimicrobial environment-friendly mask and a manufacturing method thereof.
Background
In order to prevent fine particles, harmful gases, bacteria and viruses from invading human bodies, the mask becomes a necessary product in the life of people, and particularly for clinical medical workers, the protective mask is the basis of the occupational protection. The existing medical masks are mainly divided into common medical masks, medical surgical masks and medical protective masks. The medical protective mask has effective protective effect, is made of polypropylene and has at least three-layer structure. Wherein, the outer layer is a water-resistant layer which can prevent spray and body fluid from entering the inside of the mask; the middle layer is provided with a filter layer which is composed of polypropylene melt-blown superfine fibers and has a physical interception function on larger particles, and the tiny particles are adsorbed on the fibers due to the electrostatic effect; the inner layer of the near-mouth and the near-nose is used for absorbing moisture. Medical protective facial mask has obvious filtering action to the virus, but when wearing for a long time, because gauze mask itself does not have the function of disinfecting, microorganism such as bacterium breed, and the particulate matter can block the gauze mask filter layer, and electrostatic interaction is inefficacy to lead to filtration efficiency to descend and respiratory resistance to rise. The used mask is disinfected by high temperature and ultraviolet rays to cause the polypropylene fiber structure of the filter layer to be damaged, the static electricity effect disappears, and the mask cannot be reused; the water molecules can soak the filter layer by means of steaming, scalding, washing and the like, so that the charges disappear rapidly, and the filtering effect is greatly reduced. Therefore, the medical mask needs to be replaced after being worn for 4 to 6 hours, and when medical staff touches infected patients, the medical mask also needs to be replaced immediately.
Chitin is a crystalline polysaccharide composed of beta- (1 → 4) -2-acetamido-D-glucose, widely exists in exoskeletons of aquatic animals such as shrimps and crabs, the horny layer of invertebrates, green algae, fungi and yeast cell walls, and is a natural polymer with the next accumulation amount to cellulose on the earth. The material is derived from organisms, is a reproducible natural high molecular material, and has the characteristics of good biocompatibility, biodegradability, no toxicity, no immunogenicity and the like. A large number of researches prove that the solubility of the chitin can be further improved after the chitin is modified by quaternary ammonium salt, and the chitin has durable, efficient and broad-spectrum antibacterial effect. Polylactic acid (PLA) is a high-molecular polymer prepared by using lactic acid generated by fermentation of corn starch and the like as a basic raw material and performing polycondensation reaction or ring-opening polymerization reaction of dimer lactide thereof, can be degraded in nature to generate carbon dioxide and water, and is widely applied to the fields of biomedical materials, synthetic fibers and the like because of the characteristics of no toxicity, no irritation, good mechanical properties and processability, excellent biocompatibility, super hydrophobicity and the like.
Disclosure of Invention
One of the objectives of the present invention is to provide a novel antimicrobial environment-friendly mask, which can solve the problem of no antimicrobial property of the existing mask, greatly improve the use efficiency of the mask, and reduce the secondary pollution of the waste mask.
The second purpose of the invention is to provide a manufacturing method of the novel antimicrobial environment-friendly mask, which is simple and practical and can be used for industrial production.
One of the purposes of the invention adopts the following technical scheme:
a novel antimicrobial environment-friendly mask comprises a mask main body, ear bands and nose strips, wherein the mask main body is formed by sequentially bonding an outer layer, a filter layer and an inner layer, the outer layer is arranged far away from a face, the inner layer is arranged close to the face, and the filter layer is arranged between the outer layer and the inner layer; the ear belt is connected with the inner layer and is used for tightly attaching the mask body to the face; the nose strip is arranged at the upper part of the mask main body and is used for tightly attaching the mask main body to the nose bridge; the outer layer is made of quaternary ammonium salinized chitin non-woven fabric coated with a quaternary ammonium salinized chitin-polylactic acid composite nanofiber membrane, the filter layer is made of 1-2 layers of quaternary ammonium salinized chitin nanofiber felts, and the inner layer is made of quaternary ammonium salinized chitin non-woven fabric with the skin-friendly and moisture-absorbing effects.
The second purpose of the invention is realized by adopting the following technical scheme:
a method for manufacturing a novel antimicrobial environment-friendly mask comprises the following steps:
(1) preparing a quaternary ammonium salt chitin solution, weighing quaternary ammonium salt chitin with a certain mass, dissolving the quaternary ammonium salt chitin in deionized water, and uniformly stirring until the quaternary ammonium salt chitin is completely dissolved to obtain a 6-10 wt% quaternary ammonium salt chitin solution;
(2) weighing a certain mass of cellulose, dissolving the cellulose in an alkali/urea/water solvent system, and quickly and uniformly stirring the cellulose below a freezing point until the cellulose is completely dissolved to obtain a 4-7 wt% cellulose solution, wherein the alkali/urea/water solvent system is an aqueous solution containing 5-10 wt% of KOH and 8-15 wt% of urea;
(3) mixing the quaternary ammonium salinized chitin solution obtained in the step (1) and the cellulose solution obtained in the step (2), adding a cross-linking agent for cross-linking reaction, and performing centrifugal defoaming to obtain a spinning solution A, wherein the cross-linking agent is epoxy chloropropane, the cross-linking reaction temperature is-4-0 ℃, the reaction time is 1-2 hours, and the spinning solution A contains 0.2-2 wt% of quaternary ammonium salinized chitin and 2-5 wt% of cellulose;
(4) performing electrostatic spinning on the spinning solution A obtained in the step (3) on a spinning machine, and drying and qualifying to obtain a quaternary ammonium salinization chitin nano fiber felt;
(5) spinning the spinning solution A obtained in the step (3) on a spinning machine by adopting a wet spinning technology, solidifying and regenerating in a coagulating bath, stretching, desalting and drying to obtain the quaternary ammonium salinized chitin fiber, wherein the coagulating bath is a mixed water solution containing 5-20 wt% of phytic acid and 0-10 wt% of sodium sulfate, and the temperature is 0-10 ℃;
(6) positioning and arranging the quaternary ammonium salinization chitin fibers prepared in the step (5), and preparing quaternary ammonium salinization chitin non-woven fabrics by hot pressing;
(7) weighing a certain mass of polylactic acid, dissolving the polylactic acid in a mixed solvent of dichloromethane and N, N-dimethylformamide, and magnetically stirring the mixture below a freezing point until the polylactic acid is completely dissolved to obtain a polylactic acid spinning solution, wherein the mass ratio of dichloromethane to N, N-dimethylformamide is 7:3, and the polylactic acid spinning solution contains 5-10 wt% of polylactic acid;
(8) mixing the quaternary ammonium salinization chitin solution obtained in the step (1) with the polylactic acid spinning solution obtained in the step (7), magnetically stirring for more than 1h below a freezing point, and performing ultrasonic treatment to obtain spinning solution B, wherein the mass ratio of quaternary ammonium salinization chitin to polylactic acid in the spinning solution B is 1:5-1: 20;
(9) performing electrostatic spinning on the spinning solution B prepared in the step (8) on a spinning machine to obtain a quaternary ammonium salt chitin-polylactic acid composite nanofiber membrane;
(10) tightly covering the quaternary ammonium salinized chitin-polylactic acid composite nanofiber membrane prepared in the step (9) on the quaternary ammonium salinized chitin non-woven fabric obtained in the step (6) to obtain the quaternary ammonium salinized chitin non-woven fabric coated with the quaternary ammonium salinized chitin-polylactic acid composite nanofiber membrane;
(11) and (3) sequentially bonding the quaternary ammonium salinized chitin non-woven fabric coated with the quaternary ammonium salinized chitin-polylactic acid composite nanofiber membrane obtained in the step (10), the quaternary ammonium salinized chitin nanofiber felt obtained in the step (4) and the quaternary ammonium salinized chitin non-woven fabric obtained in the step (6) and integrating the quaternary ammonium salinized chitin non-woven fabric with an ear band and a nose strip through sewing, ultrasonic fusion or hot fusion.
Further, in the step (1), the deacetylation degree of the quaternary ammonium salt chitin is 0.75-0.87, and the substitution degree of the quaternary ammonium salt is 0.35-0.47.
Further, in the step (4), an aluminum foil is adhered to a receiving plate of the spinning machine, and the spinning parameters are as follows: the spinning voltage is 20-30kV, the extrusion speed is 2-3ml/h, and the curing distance is 20-30 cm.
Further, in the step (7), the rotation speed of the magnetic stirrer is 100 rpm.
Further, in the step (8), the rotation speed of the magnetic stirrer is 300 rpm.
Further, in the step (9), an aluminum foil is adhered to a receiving plate of the spinning machine, and the spinning parameters are as follows: spinning voltage is 8-25kV, extrusion speed is 0.5-1ml/h, and curing distance is 10-20 cm.
Further, in the step (11), the number of layers of the quaternary ammonium salinization chitin nano fiber felt is 1-2, the ear belt is made of natural rubber or natural resin, and the nose strip is made of bendable plastic materials or metal wires wrapped with plastics.
Furthermore, the ear straps are arranged on two sides of the inner layer of the mask body through ear hanging type, headgear type or strap type.
When the mask provided by the invention is used, after the mask is worn, the mask can cover the mouth, the nose and the lower jaw of a wearer.
Compared with the prior art, the invention has the following beneficial technical effects:
(1) the invention provides a novel antimicrobial environment-friendly mask, which is prepared by preparing quaternary ammonium salinization chitin into antimicrobial non-woven fabric and further preparing the quaternary ammonium salinization chitin mask. The novel mask takes quaternary ammonium salinization chitin non-woven fabric coated with a quaternary ammonium salinization chitin-polylactic acid composite nanofiber membrane as an outer layer of the mask, 1-2 layers of quaternary ammonium salinization chitin nanofiber non-woven fabric as a middle filter layer of the mask, quaternary ammonium salinization chitin non-woven fabric with skin-friendly and moisture absorption effects as an inner layer of the mask, microorganisms such as bacteria, viruses and the like are continuously adsorbed and killed by utilizing the electrostatic effect of quaternary ammonium salt ions, the outer layer of the mask also utilizes the hydrophobicity of polylactic acid to block the permeation of water and body fluid, the used raw materials can be naturally degraded, the problems that the existing mask is free of antibacterial property, long in use and limited and pollutes the environment are solved, and the problem that the viruses can still be spread after the existing mask is abandoned.
(2) The quaternary ammonium salinized chitin is dissolved in water, the fiber strength is insufficient, and spinning can not be directly carried out.
(3) The quaternary ammonium salinization chitin non-woven fabric has strong hydrophilicity, and can not obstruct splashed flying foam and body fluid when being used for the outer layer of the mask. According to the invention, the quaternary ammonium salinization chitin and the polylactic acid are compounded, and the nanofiber membrane is prepared through electrostatic spinning and is tightly coated on the surface of the quaternary ammonium salinization chitin non-woven fabric, so that the mask outer layer can be endowed with excellent antibacterial property and hydrophobicity.
(4) The novel antimicrobial environment-friendly mask has the advantages of wide raw material sources, low cost and simple manufacturing process, can greatly prolong the service time while ensuring the air permeability, does not cause secondary pollution of pathogenic microorganisms due to waste masks, has environment-friendly degradation products, can relieve the situation of shortage of medical mask resources, and can effectively inhibit the diffusion of infection.
Detailed Description
The technical solution of the present invention is further illustrated by the following specific examples. The examples provided, however, are merely illustrative of the methods of the present invention and do not limit the remainder of the disclosure in any way, as the invention may be embodied in many different forms and is not limited to the examples described herein.
In the present invention, the alkali/urea/water solvent system means an aqueous solution containing alkali and urea, and the phytic acid/sodium sulfate aqueous solution means an aqueous solution containing phytic acid and sodium sulfate.
Example 1
The preparation method of the novel antimicrobial environment-friendly mask comprises the following steps:
(1) preparing a quaternary ammonium salt chitin solution, weighing 10g of quaternary ammonium salt chitin, dissolving in 90g of deionized water, uniformly stirring until the quaternary ammonium salt chitin is completely dissolved, wherein the deacetylation degree of the quaternary ammonium salt chitin is 0.87, and the substitution degree of the quaternary ammonium salt is 0.47.
(2)93g of 10 wt% KOH/15 wt% urea mixed aqueous solution is precooled to-12 ℃, 7g of cellulose is weighed and dissolved in the mixed aqueous solution, and the mixed aqueous solution is quickly and uniformly stirred until the cellulose is completely dissolved.
(3) And (3) mixing 4ml of the quaternary ammonium salinization chitin solution obtained in the step (1) with 14ml of the cellulose solution obtained in the step (2), adding 2ml of epoxy chloropropane for crosslinking reaction, and continuously stirring, wherein the reaction temperature is 0 ℃, and the reaction time is 2 hours.
(4) And (4) centrifuging the mixed solution obtained in the step (3) at the temperature of 5 ℃ and the rotating speed of 8000rpm for 15 minutes for defoaming to prepare the spinning solution A.
(5) And (4) performing electrostatic spinning on the spinning solution A obtained in the step (4), setting the spinning voltage to be 30kV, the extrusion speed to be 3ml/h and the curing distance to be 30cm, adhering an aluminum foil on a receiving plate, and drying and qualifying after spinning to obtain the quaternary ammonium salinization chitin nano fiber felt.
(6) And (3) pressurizing the spinning solution A obtained in the step (4) through a spinning machine spinneret with 0.16mm diameter by 50 holes by adopting a wet spinning technology, allowing the spinning solution A to enter a coagulating bath for coagulation and regeneration, wherein the coagulating bath is 20 wt% phytic acid/10 wt% sodium sulfate aqueous solution, and the bath temperature is 5 ℃. The quaternary ammonium salinization chitin fiber is obtained by stretching, washing, oiling, drying and winding.
(7) And (3) positioning and arranging the quaternary ammonium salinization chitin fibers prepared in the step (6), hot-pressing to form a fiber net structure, and sizing, drying, opening, desizing and drying to obtain the quaternary ammonium salinization chitin non-woven fabric.
(8) Weighing 10g of polylactic acid, dissolving the polylactic acid in 90g of mixed solvent of dichloromethane and N, N-dimethylformamide in a mass ratio of 7:3, and stirring for 4 hours at 100rpm of a magnetic stirrer below a freezing point until the polylactic acid is completely dissolved to obtain the polylactic acid spinning solution.
(9) And (3) mixing 2ml of the quaternary ammonium salinization chitin solution obtained in the step (1) with 20ml of the polylactic acid spinning solution obtained in the step (8), magnetically stirring for more than 1h at 300rpm below a freezing point, and performing ultrasonic treatment to obtain a spinning solution B.
(10) And (4) performing electrostatic spinning on the spinning solution B prepared in the step (9), setting the spinning voltage to be 25kV, the extrusion speed to be 1ml/h, the curing distance to be 20cm, adhering an aluminum foil on a receiving plate, and obtaining the quaternary ammonium salt chitin-polylactic acid composite nanofiber membrane on the aluminum foil after spinning.
(11) And (3) tightly covering the quaternary ammonium salinized chitin-polylactic acid composite nanofiber membrane prepared in the step (10) on the quaternary ammonium salinized chitin non-woven fabric obtained in the step (7) to obtain the quaternary ammonium salinized chitin non-woven fabric coated with the quaternary ammonium salinized chitin-polylactic acid composite nanofiber membrane.
(12) And (3) sequentially bonding the quaternary ammonium salinized chitin non-woven fabric coated with the quaternary ammonium salinized chitin-polylactic acid composite nanofiber membrane obtained in the step (11), the quaternary ammonium salinized chitin nanofiber felt obtained in the step (5) and the quaternary ammonium salinized chitin non-woven fabric obtained in the step (7) and integrating the quaternary ammonium salinized chitin non-woven fabric with an ear band and a nose strip through sewing, ultrasonic fusion or hot fusion.
Preferably, the ear straps are arranged on two sides of the inner layer of the mask body through ear hanging type, headgear type or strap type.
Preferably, the ear straps are made of natural rubber or natural resin, the static tension of the ear straps is measured by 10N for 5 seconds, and the breaking strength of each ear strap at the connecting point of each ear strap and the outer layer of the mask body is not less than 10N; the nose strip is made of bendable plastic materials or metal wires wrapped with plastic, and the length of the nose strip is not less than 8.0 cm.
Specifically, when the mask is used, the mouth, nose and lower jaw of a wearer can be covered after the mask is worn.
Example 2
The preparation method of the novel antimicrobial environment-friendly mask comprises the following steps:
(1) preparing a quaternary ammonium salt chitin solution, weighing 6g of quaternary ammonium salt chitin, dissolving in 94g of deionized water, uniformly stirring until the quaternary ammonium salt chitin is completely dissolved, wherein the deacetylation degree of the quaternary ammonium salt chitin is 0.75, and the substitution degree of the quaternary ammonium salt is 0.35.
(2)96g of 5 wt% KOH/8 wt% urea mixed aqueous solution is precooled to-12 ℃, 4g of cellulose is weighed and dissolved in the mixed aqueous solution, and the mixed aqueous solution is quickly and uniformly stirred until the cellulose is completely dissolved.
(3) And (3) mixing 6ml of the quaternary ammonium salinization chitin solution obtained in the step (1) with 12ml of the cellulose solution obtained in the step (2), adding 2ml of epoxy chloropropane for crosslinking reaction, and continuously stirring, wherein the reaction temperature is-4 ℃, and the reaction time is 1 h.
(4) And (4) centrifuging the mixed solution obtained in the step (3) at the temperature of 5 ℃ and the rotating speed of 8000rpm for 15 minutes for defoaming to prepare the spinning solution A.
(5) And (4) performing electrostatic spinning on the spinning solution A obtained in the step (4), setting the spinning voltage to be 20kV, the extrusion speed to be 2ml/h, the curing distance to be 20cm, adhering an aluminum foil on a receiving plate, and drying and qualifying after spinning to obtain the quaternary ammonium salinization chitin nano fiber felt.
(6) And (3) pressurizing the spinning solution A obtained in the step (4) through a spinning machine spinneret with 0.16mm diameter and 50 holes by adopting a wet spinning technology, allowing the spinning solution A to enter a coagulating bath for coagulation and regeneration, wherein the coagulating bath is a 5 wt% phytic acid aqueous solution and the bath temperature is 10 ℃. The quaternary ammonium salinization chitin fiber is obtained by stretching, washing, oiling, drying and winding.
(7) And (3) positioning and arranging the quaternary ammonium salinization chitin fibers prepared in the step (6), hot-pressing to form a fiber net structure, and sizing, drying, opening, desizing and drying to obtain the quaternary ammonium salinization chitin non-woven fabric.
(8) Weighing 5g of polylactic acid, dissolving the polylactic acid in 95g of a mixed solvent of dichloromethane and N, N-dimethylformamide in a mass ratio of 7:3, and stirring for 4 hours at 100rpm of a magnetic stirrer below a freezing point until the polylactic acid is completely dissolved to obtain the polylactic acid spinning solution.
(9) And (3) mixing 5ml of the quaternary ammonium salinization chitin solution obtained in the step (1) with 25ml of the polylactic acid spinning solution obtained in the step (8), magnetically stirring for more than 1h at 300rpm below a freezing point, and performing ultrasonic treatment to obtain a spinning solution B.
(10) And (4) performing electrostatic spinning on the spinning solution B prepared in the step (9), setting the spinning voltage to be 8kV, the extrusion speed to be 0.5ml/h, the curing distance to be 10cm, adhering an aluminum foil on a receiving plate, and obtaining the quaternary ammonium salinization chitin-polylactic acid composite nanofiber membrane on the aluminum foil after spinning.
(11) And (3) tightly covering the quaternary ammonium salinized chitin-polylactic acid composite nanofiber membrane prepared in the step (10) on the quaternary ammonium salinized chitin non-woven fabric obtained in the step (7) to obtain the quaternary ammonium salinized chitin non-woven fabric coated with the quaternary ammonium salinized chitin-polylactic acid composite nanofiber membrane.
(12) And (3) sequentially bonding the quaternary ammonium salinized chitin non-woven fabric coated with the quaternary ammonium salinized chitin-polylactic acid composite nanofiber membrane obtained in the step (11), the quaternary ammonium salinized chitin nanofiber felt obtained in the step (5) and the quaternary ammonium salinized chitin non-woven fabric obtained in the step (7) and integrating the quaternary ammonium salinized chitin non-woven fabric with an ear band and a nose strip through sewing, ultrasonic fusion or hot fusion.
Preferably, the ear straps are arranged on two sides of the inner layer of the mask body through ear hanging type, headgear type or strap type.
Preferably, the ear straps are made of natural rubber or natural resin, the static tension of the ear straps is measured by 10N for 5 seconds, and the breaking strength of each ear strap at the connecting point of each ear strap and the outer layer of the mask body is not less than 10N; the nose strip is made of bendable plastic materials or metal wires wrapped with plastic, and the length of the nose strip is not less than 8.0 cm.
Specifically, when the mask is used, the mouth, nose and lower jaw of a wearer can be covered after the mask is worn.
Example 3
The preparation method of the novel antimicrobial environment-friendly mask comprises the following steps:
(1) preparing a quaternary ammonium salt chitin solution, weighing 10g of quaternary ammonium salt chitin, dissolving in 90g of deionized water, uniformly stirring until the quaternary ammonium salt chitin is completely dissolved, wherein the deacetylation degree of the quaternary ammonium salt chitin is 0.78, and the substitution degree of the quaternary ammonium salt is 0.47.
(2)93g of 7 wt% KOH/12 wt% urea mixed aqueous solution is precooled to-12 ℃, 7g of cellulose is weighed and dissolved in the mixed aqueous solution, and the mixed aqueous solution is quickly and uniformly stirred until the cellulose is completely dissolved.
(3) And (3) mixing 4ml of the quaternary ammonium salinization chitin solution obtained in the step (1) with 14ml of the cellulose solution obtained in the step (2), adding 2ml of epoxy chloropropane for crosslinking reaction, and continuously stirring, wherein the reaction temperature is 0 ℃, and the reaction time is 2 hours.
(4) And (4) centrifuging the mixed solution obtained in the step (3) at the temperature of 5 ℃ and the rotating speed of 8000rpm for 15 minutes for defoaming to prepare the spinning solution A.
(5) And (4) performing electrostatic spinning on the spinning solution A obtained in the step (4), setting the spinning voltage to be 30kV, the extrusion speed to be 3ml/h and the curing distance to be 30cm, adhering an aluminum foil on a receiving plate, and drying and qualifying after spinning to obtain the quaternary ammonium salinization chitin nano fiber felt.
(6) And (3) pressurizing the spinning solution A obtained in the step (4) through a spinning machine spinneret with 0.16mm diameter and 50 holes by adopting a wet spinning technology, allowing the spinning solution A to enter a coagulating bath for coagulation and regeneration, wherein the coagulating bath is 15 wt% phytic acid/5 wt% sodium sulfate aqueous solution, and the bath temperature is 5 ℃. The quaternary ammonium salinization chitin fiber is obtained by stretching, washing, oiling, drying and winding.
(7) And (3) positioning and arranging the quaternary ammonium salinization chitin fibers prepared in the step (6), hot-pressing to form a fiber net structure, and sizing, drying, opening, desizing and drying to obtain the quaternary ammonium salinization chitin non-woven fabric.
(8) Weighing 8g of polylactic acid, dissolving the polylactic acid in 92g of mixed solvent of dichloromethane and N, N-dimethylformamide in a mass ratio of 7:3, and stirring for 4 hours at 100rpm of a magnetic stirrer below a freezing point until the polylactic acid is completely dissolved to obtain the polylactic acid spinning solution.
(9) And (3) mixing 2ml of the quaternary ammonium salinization chitin solution obtained in the step (1) with 25ml of the polylactic acid spinning solution obtained in the step (8), magnetically stirring for more than 1h at 300rpm below a freezing point, and performing ultrasonic treatment to obtain a spinning solution B.
(10) And (4) performing electrostatic spinning on the spinning solution B prepared in the step (9), setting a spinning voltage of 22kV, an extrusion speed of 0.5ml/h and a curing distance of 18cm, adhering an aluminum foil on a receiving plate, and spinning to obtain the quaternary ammonium salinization chitin-polylactic acid composite nanofiber membrane on the aluminum foil.
(11) And (3) tightly covering the quaternary ammonium salinized chitin-polylactic acid composite nanofiber membrane prepared in the step (10) on the quaternary ammonium salinized chitin non-woven fabric obtained in the step (7) to obtain the quaternary ammonium salinized chitin non-woven fabric coated with the quaternary ammonium salinized chitin-polylactic acid composite nanofiber membrane.
(12) And (3) sequentially bonding the quaternary ammonium salinized chitin non-woven fabric coated with the quaternary ammonium salinized chitin-polylactic acid composite nanofiber membrane obtained in the step (11), 2 layers of the quaternary ammonium salinized chitin nanofiber felt obtained in the step (5) and the quaternary ammonium salinized chitin non-woven fabric obtained in the step (7) with an ear band and a nose strip into a whole through sewing, ultrasonic fusion or thermal fusion.
Preferably, the ear straps are arranged on two sides of the inner layer of the mask body through ear hanging type, headgear type or strap type.
Preferably, the ear straps are made of natural rubber or natural resin, the static tension of the ear straps is measured by 10N for 5 seconds, and the breaking strength of each ear strap at the connecting point of each ear strap and the outer layer of the mask body is not less than 10N; the nose strip is made of bendable plastic materials or metal wires wrapped with plastic, and the length of the nose strip is not less than 8.0 cm.
Specifically, when the mask is used, the mouth, nose and lower jaw of a wearer can be covered after the mask is worn.
The quaternary ammonium salt chitin nano fiber felt prepared by the method has the fiber diameter of about 50nm and ultrathin thickness, and the non-woven fabric is used as a filter layer of the mask main body, can adsorb and kill microbes such as bacteria and viruses through the electrostatic action of quaternary ammonium salt, and can intercept the microbes and other micro particles through the physical barrier action, so that the service time of the mask can be greatly prolonged, and the replacement frequency of the mask can be reduced. When the two layers are superposed together for use, the barrier and killing effects on microorganisms such as bacteria, viruses and the like can be greatly enhanced, and the influence on the respiratory resistance is small. The quaternary ammonium salinization chitin non-woven fabric has the functions of moisture absorption and microorganism resistance, has excellent biocompatibility and large mechanical strength, can play a role in skin-friendly moisture absorption, and simultaneously plays a role in protecting a filter layer of a mask. The quaternary ammonium salinization chitin coated non-woven fabric has good waterproof effect and antibacterial effect, can obstruct splashed body fluid, can kill pathogenic microorganisms remained on the surface of the mask, and prevents secondary pollution of the abandoned mask.
The quaternary ammonium salinized chitin nanofiber felt, the quaternary ammonium salinized chitin nonwoven fabric and the quaternary ammonium salinized chitin nonwoven fabric coated with the quaternary ammonium salinized chitin-polylactic acid composite nanofiber membrane prepared in the above embodiments 1 to 3 are respectively subjected to an antibacterial experiment, an antiviral experiment, a hygroscopicity experiment and a skin irritation experiment:
(1) antibacterial experiment, each layer of nanofiber felt and nonwoven fabric prepared in examples 1-3 was cut into square pieces of 2cm × 2cm, 100. mu.L of cultured Staphylococcus aureus, Escherichia coli, and Klebsiella pneumoniae (about 10 bacteria) were collected6cfu/mL) were dropped onto different nonwoven fabric surfaces and spread evenly with a sterile spatula. Placing the small square non-woven fabric with the added bacteria liquid into a sterile bacteria culture dish, placing the small square non-woven fabric in a sterile environment at room temperature for 12h, placing the small square non-woven fabric into a sterile centrifuge tube which is preheated at 37 ℃ and contains 5mL of LB bacterial culture medium, removing the small square non-woven fabric after shaking and whirling for 1min, removing supernatant after centrifugation, and diluting the small square non-woven fabric with the LB bacterial culture medium by 0 time, 10 times and 10 times respectively210 times of310 times of4Then, 100 mul of the mixture is evenly coated on an LB solid plate culture medium respectively, and cultured for 24h at 37 ℃, and the bacteriostasis rate is checked and calculated. The experimental results show that the bacteriostatic rates of the quaternary ammonium salinized chitin non-woven fabric, the quaternary ammonium salinized chitin non-woven fabric and the quaternary ammonium salt chitin nano-fiber felt coated with the quaternary ammonium salinized chitin-polylactic acid composite nano-fiber membrane obtained in the embodiments on staphylococcus aureus, escherichia coli and klebsiella pneumoniae are all more than 99%.
(2) Antiviral experiments: the nanofiber mats and the non-woven fabrics prepared in the above examples 1 to 3 were cut into 2cm × 2cm square pieces, 100 μ L of 100TCID50 virus diluent was dropped onto the surfaces of different square pieces of non-woven fabrics, and the pieces were uniformly spread with an aseptic spatula. Placing the small square non-woven fabric dropwise added with the virus diluent into a sterile bacteria culture dish, placing the sterile bacteria culture dish in a sterile environment at room temperature for 12 hours, placing the small square non-woven fabric into a sterile centrifuge tube precooled at 4 ℃ and containing 5mL of virus transport fluid, removing the small square non-woven fabric after shaking and vortexing for 1min, removing supernatant after centrifugation at 4 ℃, performing suspension precipitation by using 1mL of culture solution, performing cryopreservation at-80 ℃, performing freeze thawing before use, adding a double antibody, and performing action at 4 ℃ for 1-2 hours to obtain the inoculum. Vero-E6 cells overgrow 80-90% within 48h of passage, inoculated with virus inoculation liquid, and treated in the same way by replacing inoculum with maintenance liquid, and used as normal cell control. The flasks were checked for cytopathic effects every day from the following day, and if no CPEs were observed after 5 days of cell culture, a portion of the medium was removed from the inoculated cells, placed in a fresh cell flask full of cells, and cultured. The experimental results show that no virus-typical CPE is found in the third blind passage of the specimen, and all the viruses remained on the non-woven fabric obtained in each example die and do not survive.
(3) Moisture absorption test: the quaternary ammonium salinized chitin nonwoven fabric prepared in the above examples 1 to 3 was cut into 5cm by 5cm size, and the dry weight (W) of the nonwoven fabric piece was weighed. Putting the non-woven fabric block into a beaker, adding 50mL of physiological saline, placing for 30 minutes, clamping one corner of the non-woven fabric block by using a pair of tweezers, hanging for 30 seconds in the air, then weighing the wet weight (W1) of the non-woven fabric block, putting the non-woven fabric block back into the physiological saline, weighing once every 30 minutes for 6 times in total, and calculating the hygroscopicity of the non-woven fabric block in unit weight at different time. The above procedure was repeated with plain gauze as a control. The experimental result shows that the moisture absorption of the quaternary ammonium salinization chitin non-woven fabric is more than 5 times of that of common gauze.
(4) Skin irritation test: 27 male white rabbits were selected and randomly divided into 9 groups. The hair on both sides of the spine of the rabbit is removed by depilatory 24h before the test, and the skin is not damaged. The dehairing range was about 3cm by 3cm on each of the left and right. The next day, each layer of nanofiber felt and nonwoven prepared in examples 1-3 above was applied directly to the left unhaired intact skin, covered with a layer of non-irritating plastic film, and fixed with a non-irritating adhesive tape. The other side had hair removed as a blank control. The application time was 4 h. After the test is completed, the residual test substance is removed with warm water or a non-irritating solvent. The skin local reactions were observed at 1h, 24h and 48h after removal of the test substance, respectively. The experimental results show that at all time points, the rabbit skin has no edema, erythema and skin irritation reaction.
The novel antimicrobial environment-friendly mask prepared in each example is subjected to a filtration efficiency experiment, an airflow resistance experiment, a synthetic blood penetration experiment and a surface moisture resistance experiment:
according to the technical requirements of GB 19083-2010 medical protective mask, an automatic filtration efficiency instrument of TSI 8130 type is adopted to test the filtration efficiency (percentage of the mask to the bacteria-containing suspended particles filtered under the specified flow) and the airflow resistance (resistance of the mask under the specified flow) of the protective mask. The experimental results showed that the mask of example 1 had a filtration efficiency of 97.834% and an airflow resistance of 23.5mmH at an airflow rate of 85L/min2O; the mask obtained in example 2 had a filter efficiency of 98.152% and an airflow resistance of 23.7mmH2O; the mask obtained in example 2 had a filtration efficiency of 99.827% and an airflow resistance of 26.3mmH2And O, all meet the national standard.
According to a YY/T0691-.
According to the GB/T4745-1997 test for measuring the moisture resistance of the surface of the textile fabric and measuring the water pick-up, 250mL of distilled water is injected into a 150mm funnel, a mask to be measured is placed 150mm below a nozzle of the funnel in an inclined way at an angle of 45 degrees, and the spraying is continuously carried out for 30 s. After spraying, the mask is horizontally hung, and after the mask is slightly knocked for two times, observation is carried out, so that the surface of the mask is not wetted, and the mask meets the national standard.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, several modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.
Claims (9)
1. A novel antimicrobial environment-friendly mask is characterized in that: the mask comprises a mask body, ear bands and nose strips, wherein the mask body is formed by sequentially bonding an outer layer, a filter layer and an inner layer, the outer layer is arranged far away from the face, the inner layer is arranged close to the face, and the filter layer is arranged between the outer layer and the inner layer; the ear belt is connected with the inner layer and is used for tightly attaching the mask body to the face; the nose strip is arranged at the upper part of the mask main body and is used for tightly attaching the mask main body to the nose bridge; the outer layer is made of quaternary ammonium salinized chitin non-woven fabric coated with a quaternary ammonium salinized chitin-polylactic acid composite nanofiber membrane, the filter layer is made of 1-2 layers of quaternary ammonium salinized chitin nanofiber felts, and the inner layer is made of quaternary ammonium salinized chitin non-woven fabric with the skin-friendly and moisture-absorbing effects.
2. The method for manufacturing the novel antimicrobial environment-friendly mask as claimed in claim 1, wherein the method comprises the following steps: the method comprises the following steps:
(1) preparing a quaternary ammonium salt chitin solution, weighing quaternary ammonium salt chitin with a certain mass, dissolving the quaternary ammonium salt chitin in deionized water, and uniformly stirring until the quaternary ammonium salt chitin is completely dissolved to obtain a 6-10 wt% quaternary ammonium salt chitin solution;
(2) weighing a certain mass of cellulose, dissolving the cellulose in an alkali/urea/water solvent system, and quickly and uniformly stirring the cellulose below a freezing point until the cellulose is completely dissolved to obtain a 4-7 wt% cellulose solution, wherein the alkali/urea/water solvent system is an aqueous solution containing 5-10 wt% of KOH and 8-15 wt% of urea;
(3) mixing the quaternary ammonium salinized chitin solution obtained in the step (1) and the cellulose solution obtained in the step (2), adding a cross-linking agent for cross-linking reaction, and performing centrifugal defoaming to obtain a spinning solution A, wherein the cross-linking agent is epoxy chloropropane, the cross-linking reaction temperature is-4-0 ℃, the reaction time is 1-2 hours, and the spinning solution A contains 0.2-2 wt% of quaternary ammonium salinized chitin and 2-5 wt% of cellulose;
(4) performing electrostatic spinning on the spinning solution A obtained in the step (3) on a spinning machine, and drying and qualifying to obtain a quaternary ammonium salinization chitin nano fiber felt;
(5) spinning the spinning solution A obtained in the step (3) on a spinning machine by adopting a wet spinning technology, solidifying and regenerating in a coagulating bath, stretching, desalting and drying to obtain the quaternary ammonium salinized chitin fiber, wherein the coagulating bath is a mixed water solution containing 5-20 wt% of phytic acid and 0-10 wt% of sodium sulfate, and the temperature is 0-10 ℃;
(6) positioning and arranging the quaternary ammonium salinization chitin fiber prepared in the step (5), and preparing a quaternary ammonium salinization chitin non-woven fabric through hot pressing;
(7) weighing a certain mass of polylactic acid, dissolving the polylactic acid in a mixed solvent of dichloromethane and N, N-dimethylformamide, and magnetically stirring the mixture below a freezing point until the polylactic acid is completely dissolved to obtain a polylactic acid spinning solution, wherein the mass ratio of the dichloromethane to the N, N-dimethylformamide is 7:3, and the polylactic acid spinning solution contains 5-10 wt% of polylactic acid;
(8) mixing the quaternary ammonium salinization chitin solution obtained in the step (1) with the polylactic acid spinning solution obtained in the step (7), magnetically stirring for more than 1h below a freezing point, and performing ultrasonic treatment to obtain spinning solution B, wherein the mass ratio of quaternary ammonium salinization chitin to polylactic acid in the spinning solution B is 1:5-1: 20;
(9) performing electrostatic spinning on the spinning solution B prepared in the step (8) on a spinning machine to obtain a quaternary ammonium salinization chitin-polylactic acid composite nanofiber membrane;
(10) tightly coating the quaternary ammonium salinization chitin-polylactic acid composite nanofiber membrane prepared in the step (9) on the quaternary ammonium salinization chitin non-woven fabric obtained in the step (6) to obtain the quaternary ammonium salinization chitin non-woven fabric coated with the quaternary ammonium salinization chitin-polylactic acid composite nanofiber membrane;
(11) and (3) sequentially bonding the quaternary ammonium salinized chitin non-woven fabric coated with the quaternary ammonium salinized chitin-polylactic acid composite nanofiber membrane obtained in the step (10), the quaternary ammonium salinized chitin nanofiber felt obtained in the step (4) and the quaternary ammonium salinized chitin non-woven fabric obtained in the step (6) and integrating the quaternary ammonium salinized chitin non-woven fabric with an ear band and a nose strip through sewing, ultrasonic fusion or hot fusion.
3. The method for manufacturing a novel antimicrobial environment-friendly mask according to claim 2, wherein the method comprises the following steps: in the step (1), the deacetylation degree of the quaternary ammonium salinization chitin is 0.75-0.87, and the substitution degree of the quaternary ammonium salt is 0.35-0.47.
4. The method for manufacturing a novel antimicrobial environment-friendly mask according to claim 2, wherein the method comprises the following steps: in the step (4), aluminum foil is adhered to a receiving plate of the spinning machine, and the spinning parameters are as follows: the spinning voltage is 20-30kV, the extrusion speed is 2-3ml/h, and the curing distance is 20-30 cm.
5. The method for manufacturing a novel antimicrobial environment-friendly mask according to claim 2, wherein the method comprises the following steps: in the step (7), the rotation speed of the magnetic stirrer is 100 rpm.
6. The method for manufacturing a novel antimicrobial environment-friendly mask according to claim 2, wherein the method comprises the following steps: in the step (8), the rotation speed of the magnetic stirrer is 300 rpm.
7. The method for manufacturing a novel antimicrobial environment-friendly mask according to claim 2, wherein the method comprises the following steps: in the step (9), aluminum foil is adhered to a receiving plate of the spinning machine, and the spinning parameters are as follows: spinning voltage is 8-25kV, extrusion speed is 0.5-1ml/h, and curing distance is 10-20 cm.
8. The method for manufacturing a novel antimicrobial environment-friendly mask according to claim 2, wherein the method comprises the following steps: in the step (11), the number of layers of the quaternary ammonium salinization chitin nano fiber felt is 1-2, the ear belt is made of natural rubber or natural resin, and the nose strip is made of bendable plastic materials or metal wires wrapped with plastics.
9. The method for manufacturing a novel antimicrobial environment-friendly mask according to claim 2, wherein the method comprises the following steps: the ear belts are arranged on two sides of the inner layer of the mask main body through ear hanging type, headgear type or lacing type.
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