阅读说明：本技术 一种口罩熔喷层及其制备方法 (Mask melt-blown layer and preparation method thereof ) 是由 李义涛 肖文武 云晧 张凌飞 程宗盛 邹智杰 黄连红 满金芝 于 2020-05-29 设计创作，主要内容包括：本发明提供了一种口罩熔喷层及其制备方法。所述制备方法包括：S1、配制含银抗菌剂分散液；S2、将口罩熔喷层放置在具有凸起微图案或凹坑微图案的铌酸锂晶体上,并对铌酸锂晶体进行加热处理；S3、将含银抗菌剂分散液沉积在S2中的口罩熔喷层上,得到所述口罩熔喷层。采用本发明方法得到的口罩熔喷层,抗菌剂在熔喷层上的分布可控、抗菌剂用量少,抗菌效果和透气性俱佳,有效地控制了生产成本。(The invention provides a mask melt-blown layer and a preparation method thereof. The preparation method comprises the following steps: s1, preparing silver-containing antibacterial agent dispersion liquid; s2, placing the mask melt-blown layer on the lithium niobate crystal with the convex micro-patterns or the concave micro-patterns, and heating the lithium niobate crystal; and S3, depositing the silver-containing antibacterial agent dispersion liquid on the mask melt-blown layer in the S2 to obtain the mask melt-blown layer. The mask melt-blown layer obtained by the method has controllable distribution of the antibacterial agent on the melt-blown layer, less consumption of the antibacterial agent, good antibacterial effect and air permeability, and effectively controlled production cost.)

1. The mask meltblown layer is characterized by comprising silver-containing antibacterial agent loaded areas and silver-containing antibacterial agent unloaded areas which are arranged at intervals, wherein the coverage rate of the silver-containing antibacterial agent loaded areas is more than or equal to 55% and less than 100%, and the distance between every two adjacent silver-containing antibacterial agent loaded areas is 200-400 mu m;

or the mask melt-blown layer comprises silver-containing antibacterial agent loaded areas and silver-containing antibacterial agent unloaded areas which are arranged at intervals, wherein the coverage rate of the silver-containing antibacterial agent loaded areas is more than or equal to 55% and less than 100%, and the distance between the two adjacent silver-containing antibacterial agent unloaded areas is 200-400 mu m.

2. The method of making a melt-blown layer for a mask of claim 1 comprising the steps of:

s1, preparing silver-containing antibacterial agent dispersion liquid;

s2, placing the mask melt-blown layer on the lithium niobate crystal with the convex micro-patterns or the concave micro-patterns, and heating the lithium niobate crystal;

s3, depositing the silver-containing antibacterial agent dispersion liquid on the mask melt-blown layer in the S2 to obtain a mask melt-blown layer loaded with the silver-containing antibacterial agent;

wherein when the area of the convex micro-pattern or the concave micro-pattern is larger than that of the non-micro-pattern, the silver-containing antibacterial agent is loaded in the area corresponding to the convex micro-pattern or the concave micro-pattern; when the area of the non-micropattern is larger than the area of the raised micropattern or the recessed micropattern, the silver-containing antimicrobial agent is supported in the corresponding region of the non-micropattern.

3. The method for preparing a mask meltblown layer according to claim 2, wherein the distance between two adjacent raised micro-patterns is 200-400 μm, and the height of each raised micro-pattern is 100-500 μm.

4. The method for preparing a mask meltblown layer according to claim 2, wherein the distance between two adjacent dimple micropatterns is 200-400 μm, and the depth of the dimple is 100-500 μm.

5. The method for manufacturing a mask meltblown layer according to claim 2, wherein the heating temperature in step S2 is 60 to 80 ℃.

6. The method for manufacturing a mask meltblown layer according to claim 2, wherein in step S3, the distance between the silver-containing antimicrobial dispersion and the mask meltblown layer is 0.05-1 mm.

7. The method for preparing a mask meltblown layer according to claim 2, wherein the silver-containing antimicrobial dispersion is deposited at a deposition rate of 0.5-5mL/h and a deposition time of 2-5S in step S3.

8. The method for preparing a mask meltblown layer according to claim 2, wherein said silver-containing antimicrobial dispersion of step S1 comprises: silver particles, a dispersing agent, a binder, deionized water, a wetting agent and a thickening agent.

9. The method for preparing a mask meltblown layer according to claim 8, wherein said dispersing agent is at least one of BYK LP-C2005, octadecyl trimethyl ammonium chloride, polyethylene glycol;

preferably, the thickener is at least one of sodium carboxymethylcellulose, methylcellulose, hydroxyethyl cellulose, hydroxyethyl methylcellulose, hydroxypropyl methylcellulose, polyacrylamide, polyethylene oxide, xanthan gum and sodium alginate;

preferably, the binder is at least one of styrene-butadiene rubber emulsion, polyvinyl alcohol, ethylene-ethyl acetate, sodium hydroxymethyl cellulose and polyvinylpyrrolidone;

preferably, the wetting agent is at least one of BYK LP-X20990, alkyl sulfate, Tween 80, ethanol, glycol, glycerol and ethyl acetate.

10. A mask comprising the mask meltblown layer of claim 1 or the mask meltblown layer obtained by the method of any of claims 2 to 9.

Technical Field

The invention relates to the technical field of masks, in particular to a mask melt-blown layer, a preparation method of the mask melt-blown layer and a mask comprising the mask melt-blown layer.

Background

The large-scale epidemic outbreaks in recent years are respiratory infectious diseases such as COVID-19, SARS, highly pathogenic avian influenza, influenza A H1N1, and the like. The respiratory infectious disease is transmitted by droplets and air, has the characteristics of high transmission speed, wide susceptible population, high morbidity and the like, and poses great threats to public health and social stability. The protective mask can block pathogenic microorganisms from invading human bodies when being worn, and is an effective means for preventing the epidemic of respiratory infectious diseases and protecting the health of personnel.

At present, polypropylene (PP) melt-blown non-woven fabric or electret polypropylene melt-blown non-woven fabric is mostly adopted as a filtering and blocking layer of the conventional protective mask, and the high-efficiency blocking of tiny particles and pathogenic microorganisms is realized by physical actions such as blocking and interception, inertial collision, Brownian diffusion, electrostatic adsorption and the like. The conventional protective mask serves as a physical barrier to filter contaminants, but microorganisms such as bacteria and viruses, which are retained on the filter material, can survive and propagate under appropriate conditions, which may cause secondary pollution to people and the environment. There is therefore a need in the market for protective masks that can capture viruses or bacteria and kill them on the spot.

In order to prevent secondary pollution caused by re-diffusion of pathogenic microorganisms attached to the mask, protective masks capable of inhibiting or killing pathogenic microorganisms have been developed, in which addition of an antibacterial agent to a filter material is one of simple and effective methods for imparting an antibacterial function to the mask.

The silver particles have excellent antibacterial effect, but the price is expensive, and the price of the silver-containing antibacterial mask is greatly improved.

At present, the silver-containing antibacterial agent is loaded on the mask melt-blown layer by adopting a dipping or spraying mode, and the defects are as follows: the silver-containing antibacterial agent has large usage amount, and the cost of raw materials is increased; the production time is long, and the production efficiency is reduced.

Therefore, the protective mask which not only saves the cost, but also has better antibacterial effect is the most urgent need at present.

Disclosure of Invention

The invention aims to provide a mask melt-blown layer, a preparation method thereof and a mask comprising the mask melt-blown layer, aiming at the defects in the prior art. The preparation method provided by the invention reduces the production cost of the antibacterial mask, and has the advantages of short operation time, high efficiency, and good mask air permeability and antibacterial effect.

In order to achieve the purpose, the technical scheme adopted by the invention is as follows:

in one aspect, the invention provides a mask meltblown layer, which comprises silver-containing antibacterial agent loaded areas and silver-containing antibacterial agent unloaded areas which are arranged at intervals, wherein the coverage rate of the silver-containing antibacterial agent loaded areas is greater than or equal to 55% and less than 100%, and the distance between two adjacent silver-containing antibacterial agent loaded areas is 200-400 μm;

or the mask melt-blown layer comprises silver-containing antibacterial agent loaded areas and silver-containing antibacterial agent unloaded areas which are arranged at intervals, wherein the coverage rate of the silver-containing antibacterial agent loaded areas is more than or equal to 55% and less than 100%, and the distance between the two adjacent silver-containing antibacterial agent unloaded areas is 200-400 mu m.

In some embodiments, the areas of the mask meltblown layer that carry the silver-containing antimicrobial agent are circular in shape at intervals.

In other embodiments, the areas of the mask meltblown layer not loaded with silver-containing antimicrobial agent are circular in shape and are spaced apart.

Further, the coverage of the silver-containing antibacterial agent-loaded area is 55-70%.

In the invention, the bacteriostatic rate of the mask melt-blown layer on staphylococcus aureus is more than 99%.

On the other hand, the invention provides a preparation method of the mask melt-blown layer, which comprises the following steps:

s1, preparing silver-containing antibacterial agent dispersion liquid;

s2, placing the mask melt-blown layer on the lithium niobate crystal with the convex micro-patterns or the concave micro-patterns, and heating the lithium niobate crystal;

s3, depositing the silver-containing antibacterial agent dispersion liquid on the mask melt-blown layer in the S2 to obtain a mask melt-blown layer loaded with the silver-containing antibacterial agent;

wherein when the area of the convex micro-pattern or the concave micro-pattern is larger than that of the non-micro-pattern, the silver-containing antibacterial agent is loaded in the area corresponding to the convex micro-pattern or the concave micro-pattern; when the area of the non-micropattern is larger than the area of the raised micropattern or the recessed micropattern, the silver-containing antimicrobial agent is supported in the corresponding region of the non-micropattern.

The lithium niobate crystal with the convex micro-patterns or the concave micro-patterns is obtained by processing a lithium niobate crystal block with a smooth surface, and the processing specific steps comprise: adopting CNC (computer numerical control) or photoetching technology to reserve the micro-pattern part and remove the non-micro-pattern part to obtain the lithium niobate crystal with the convex micro-pattern; or removing the micro-pattern part and reserving the non-micro-pattern part to obtain the lithium niobate crystal with the pit micro-pattern.

Lithium niobate (LiNbO)₃) The crystal is a pyroelectric crystal material, and the surface of the heated lithium niobate crystal with the convex micro-patterns or the concave micro-patterns is polarized and charged (if the surface of the lithium niobate crystal is flat, the heating cannot be polarized to generate positive and negative charges). Because the micro-pattern area and the non-micro-pattern area are not on the same plane in the lithium niobate crystal with the micro-pattern, the lithium niobate crystal is polarized and charged with different charges after being heated, and the relatively raised parts in the micro-pattern area and the non-micro-pattern area are positively charged, for example, when the lithium niobate crystal block is provided with the raised micro-pattern, the raised micro-pattern area is positively charged, and the non-micro-pattern area is negatively charged; for example, when the lithium niobate crystal block has a pit micro pattern, the non-micro pattern area is positively charged, and the pit micro pattern area is negatively charged. When the silver-containing antibacterial agent dispersion liquid with certain conductivity is close to the lithium niobate crystal, the intensity of a bipolar electric field mode formed by the lithium niobate crystal can beThe surface of the silver-containing antibacterial agent dispersion liquid is charged, and the silver-containing antibacterial agent dispersion liquid is close to the lithium niobate crystal by electrostatic attraction between charges, so that the silver-containing antibacterial agent dispersion liquid is deposited on the mask melt-spraying layer in an electrostatic spraying mode. And the surface charge of the silver-containing antibacterial agent dispersion liquid is opposite to that of the part with larger area in the micropattern area and the non-micropattern area, so that the silver-containing antibacterial agent dispersion liquid is deposited on the region corresponding to the part with larger area in the micropattern area and the non-micropattern area on the mask melt-blown layer in the form of electrostatic spraying.

The micro-pattern can be regular patterns such as circles, squares, rectangles, diamonds and the like, and can also be irregular patterns.

In some embodiments, the lithium niobate crystal has raised micro patterns, the distance between two adjacent raised micro patterns is 200-.

In other embodiments, the lithium niobate crystal has a pit micro pattern, the distance between two adjacent pit micro patterns is 200-400 μm, and the depth of the pit is 100-500 μm.

In some embodiments, the lithium oxide crystals have a raised micropattern with an area greater than an area of the non-micropattern, and the silver-containing antimicrobial agent is supported on the raised micropattern areas.

In other embodiments, the lithium oxide crystals have a raised micropattern with an area smaller than an area of the non-micropattern, and the silver-containing antimicrobial agent is supported in the non-micropatterned area.

In other embodiments, the lithium acid crystal has a pit micropattern with an area larger than an area of the non-micropattern, and the silver antimicrobial agent is supported in the pit micropattern region.

In other embodiments, the lithium acid crystal has a pit micropattern with an area smaller than an area of the non-micropattern, and the silver-containing antibacterial agent is supported on the non-micropatterned area.

In some embodiments, the mask meltblown layer is a PP meltblown layer.

In some embodiments, the heating temperature in step S2 is 60 to 80 ℃.

Specifically, the heat treatment temperature is: 60 ℃, 65 ℃, 70 ℃, 75 ℃, 80 ℃, etc.

The purpose of the heat treatment is to polarize the lithium niobate so that the relatively convex portions in the micropattern areas and the non-micropattern areas are positively charged and the non-convex portions are negatively charged. Because the melting point of the PP melt-blown layer is about 165 ℃, the PP melt-blown layer can be influenced to a certain extent when the temperature is too high, and when the temperature is 60-80 ℃, the silver-containing antibacterial agent dispersion liquid can be guaranteed to have good deposition effect, and energy waste can not be caused.

In the embodiment of the present invention, in step S3, the distance between the silver-containing antibacterial agent dispersion and the mask meltblown layer during deposition is 0.05 to 1mm, preferably 0.1 to 1 mm.

Specifically, the distance between the silver-containing antibacterial agent dispersion liquid and the mask melt-blown layer is as follows: 0.05mm, 0.1mm, 0.2mm, 0.3mm, 0.4mm, 0.5mm, 0.6mm, 0.7mm, 0.8mm, 0.9mm, 1mm, etc.

When the distance between the silver-containing antibacterial agent dispersion liquid and the mask melt-blown layer is too short, the deposition range of the dispersion liquid is too small, and the antibacterial effect of the mask melt-blown layer is poor; when the distance is too far, the degree to which the dispersion is polarized is low, and the effect of deposition is also affected.

In some embodiments, the silver-containing antibacterial agent dispersion is deposited at a deposition rate of 0.5 to 5mL/h, preferably 0.5 to 4mL/h, and for a deposition time of 2 to 5S in step S3.

Specifically, the deposition rate of the silver-containing antibacterial agent dispersion liquid is 0.5mL/h, 1mL/h, 2mL/h, 3mL/h, 4mL/h, 5mL/h, or the like.

When the deposition rate of the silver-containing antibacterial agent dispersion is too high, the coverage rate of the silver-containing antibacterial agent is too high, and raw materials are wasted.

The deposition rate of the silver-containing antibacterial agent dispersion is mainly related to the polarization degree thereof, and the polarization degree is related to the heating temperature of lithium niobate and the distance between the silver-containing antibacterial agent dispersion and the mask meltblown layer, so that when the heating temperature of lithium niobate is 60-80 ℃ and the distance between the silver-containing antibacterial agent dispersion and the mask meltblown layer is 0.05-1mm, the deposition effect is best when the deposition rate of the silver-containing antibacterial agent dispersion is controlled to be 0.5-5 mL/h.

In the present invention, the silver-containing antibacterial agent dispersion is loaded into a syringe, and the deposition rate of the silver-containing antibacterial agent dispersion is controlled by adjusting the syringe pump of the syringe.

Specifically, the deposition time is 2s, 2.5s, 3s, 3.5s, 4s, 4.5s, 5s, and the like.

When the deposition time is less than 2s, the coverage rate of the silver-containing antibacterial agent on the mask melt-blown layer is low, the antibacterial effect of the melt-blown layer is poor, and the deposition time is too long, so that the raw materials are wasted, therefore, the reasonable deposition time is 2-5s, and the temperature is controlled to be 60-80 ℃.

In the present invention, the composition of the silver-containing antimicrobial dispersion liquid in step S1 is not particularly limited, and a composition that is safe and environmentally friendly to use may be used. Since the silver particles themselves have conductivity, so that the silver-containing antimicrobial agent dispersion liquid can be polarized electrically, the remaining components may be added as needed.

In some embodiments, the silver-containing antimicrobial agent dispersion in step S1 includes: silver particles, a dispersing agent, a binder, deionized water, a wetting agent and a thickening agent.

Among them, silver particles refer to a simple substance of silver, and in the present invention, silver nanoparticles are preferably used in view of excellent antibacterial effect of nano silver.

In a specific embodiment, the silver-containing antibacterial agent dispersion in step S1 includes: silver nanoparticles, a dispersing agent, a binder, deionized water, a wetting agent and a thickening agent.

In some embodiments, the ratio of each component is, based on 100 parts by weight of the silver-containing antibacterial agent dispersion liquid: 10 parts of silver particles, 1 part of dispersing agent, 2 parts of binder, 0.5 part of thickening agent and wetting agent respectively, and 86 parts of deionized water.

Specifically, the dispersing agent is at least one of BYK LP-C2005, octadecyl trimethyl ammonium chloride and PEG (polyethylene glycol); the thickening agent is at least one of sodium carboxymethylcellulose (CMC), methylcellulose, hydroxyethyl cellulose, hydroxyethyl methylcellulose, hydroxypropyl methylcellulose, polyacrylamide, polyethylene oxide, xanthan gum and sodium alginate; the binder is at least one of styrene-butadiene rubber emulsion (SBR), polyvinyl alcohol, ethylene-ethyl acetate, sodium carboxymethylcellulose and polyvinylpyrrolidone; the wetting agent is at least one of BYK LP-X20990, alkyl sulfate, Tween 80, ethanol, glycol, glycerol and ethyl acetate.

In the invention, the distribution of the silver-containing antibacterial agent on the mask melt-blown layer can be controlled by changing the shape of the micro-pattern and the area of the micro-pattern on the surface of the lithium niobate crystal, meanwhile, the using amount of the silver-containing antibacterial agent is reduced, the deposition time is only 2-5s, the production cost can be effectively controlled, the production efficiency is improved, and the air permeability of the melt-blown layer is not influenced.

In a third aspect, the present invention provides a mask comprising the above mask meltblown layer, or the mask meltblown layer obtained by the above mask meltblown layer preparation method.

The invention has the beneficial effects that:

(1) the silver-containing antibacterial agent is loaded on the mask melt-blown layer in the form of electrostatic spraying by utilizing the polarized charged performance of the lithium niobate pyroelectric material, the distribution shape of the silver-containing antibacterial agent loaded on the melt-blown layer is controllable, the operation time is short, meanwhile, the using amount of silver particles is saved, and the cost can be effectively controlled.

(2) The mask melt-blown layer obtained by the invention has good antibacterial effect, is not inferior to modes such as dipping, spraying and the like, and has excellent air permeability.

Definition of terms

In the present invention, when the name and structure of the compound conflict, the structure of the compound is taken as the standard.

All ranges cited herein are inclusive, unless expressly stated to the contrary.

The terms "a" or "an" are used herein to describe elements and components described herein. This is done merely for convenience and to provide a general sense of the scope of the invention. Such description should be understood to include one or at least one and the singular also includes the plural unless it is obvious that it is meant otherwise. "plural" means two or more.

The numbers in this disclosure are approximate, regardless of whether the word "about" or "approximately" is used. The numerical value of the number may have differences of 1%, 2%, 5%, 7%, 8%, 10%, etc. Whenever a number with a value of N is disclosed, any number with a value of N +/-1%, N +/-2%, N +/-3%, N +/-5%, N +/-7%, N +/-8% or N +/-10% is explicitly disclosed, wherein "+/-" means plus or minus, and a range between N-10% and N + 10% is also disclosed.

The following definitions, as used herein, should be applied unless otherwise indicated. For the purposes of the present invention, the chemical elements are in accordance with the CAS version of the periodic Table of elements, and the 75 th version of the handbook of chemistry and Physics, 1994. In addition, general principles of Organic Chemistry can be found in the descriptions of "Organic Chemistry", Thomas Sorrell, University Science Books, Sausaltito: 1999, and "March's Advanced Organic Chemistry" by Michael B.Smith and JerryMarch, John Wiley & Sons, New York:2007, the entire contents of which are incorporated herein by reference.

Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although methods and materials similar or equivalent to those described herein can also be used in the practice or testing of embodiments of the present invention, suitable methods and materials are described below. All publications, patent applications, patents, and other references mentioned herein are incorporated by reference in their entirety, unless a specific section is cited. In case of conflict, the present specification, including definitions, will control. In addition, the materials, methods, and examples are illustrative only and not intended to be limiting.

Drawings

FIG. 1 is a schematic view of examples 1 to 5 of the present invention;

FIG. 2 is a schematic representation of examples 6-7 of the present invention.

Detailed Description

The following description is of the preferred embodiment of the present invention only, and is not intended to limit the present invention, and any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.

Lithium niobate crystal i: has a raised micro-pattern with a height of 200 μm, a circular shape and a circular area of 0.0314mm²The pitch of adjacent circles is 400 μm and the total area of the raised micro-pattern is smaller than the area of the non-micro-pattern (as shown in fig. 1).

Lithium niobate crystal ii: has a raised micro pattern with a height of 200 μm, a circular shape with an area of 0.785mm²The pitch of adjacent circles is 200 μm, and the total area of the raised micro-patterns is greater than the area of the non-micro-patterns (as shown in fig. 2).

When the lithium niobate crystal has a pit micropattern, the principle of deposition of the silver-containing antibacterial agent on the mask meltblown layer is the same as that of the lithium niobate crystal having a convex micropattern, and therefore, in the following specific examples, only the lithium niobate crystal having a convex micropattern is represented.

Mask melt-blown layer: PP meltblown layer, available from sikawa energy concentrating filter limited.

The preparation method of the mask melt-blown layer provided by the invention is further explained in detail.

The preparation method of the mask melt-blown layer specifically comprises the following steps:

s1, preparing silver-containing antibacterial agent dispersion liquid: uniformly mixing silver particles, a dispersing agent, a binder, deionized water, a wetting agent and a thickening agent according to a certain proportion, and filling the mixture into an injector to enable an injection pump of the injector to be in a closed state;

s2, placing the lithium niobate crystal with the convex micro-pattern or the concave micro-pattern on a heating table, laying a PP mask melt-spraying layer on the lithium niobate crystal, and keeping the heating table in a closed state; approaching the injector filled with the silver-containing antibacterial agent dispersion liquid in the step S1 to the mask melt-blown layer, and controlling the distance between the injector and the mask melt-blown layer to be 0.05-1mm, wherein the injection pump of the injector is still in a closed state; starting a power supply of a heating table, and setting the temperature to be 60-80 ℃;

and S3, after the temperature is stabilized, starting an injection pump of the injector, controlling the deposition speed of the silver-containing antibacterial agent dispersion liquid to be 0.5-5mL/h, starting deposition, and after 2-5S, closing the injection pump of the injector and a heating table power supply to obtain the mask melt-spraying layer loaded with the silver-containing antibacterial agent.