WO2023113101A1 - Manufacturing method of antibacterial nonwoven fabric, and antibacterial nonwoven fabric manufactured using manufacturing method - Google Patents

Abstract

Provided are a manufacturing method of an antibacterial nonwoven fabric, and an antibacterial nonwoven fabric manufactured using the manufacturing method, the method allowing copper to be deposited on a calcium carbonate powder so that a copper antibacterial agent, which is relatively resistant to oxidation, is prepared and used as a material for a nonwoven fabric, and thus the present invention is advantageous for color setting of a nonwoven fabric and has excellent antibacterial properties. To this end, the manufacturing method of an antibacterial nonwoven fabric, according to the present invention, comprises the steps of: (S1) depositing copper on a calcium carbonate powder so as to prepare a copper antibacterial agent; (S2) mixing the copper antibacterial agent with a polypropylene so as to prepare master batch chips; (S3) melt spinning the master batch chips so as to manufacture a single-layer nonwoven fabric; (S4) melt spinning the master batch chips on at least one surface of the single-layer nonwoven fabric so as to manufacture a multilayer nonwoven fabric; and (S5) embossing the multilayer nonwoven fabric by means of compression rollers.

Description

Manufacturing method of antibacterial nonwoven fabric and antibacterial nonwoven fabric manufactured by the manufacturing method

The present invention relates to a method for producing an antibacterial nonwoven fabric and an antibacterial nonwoven fabric manufactured by the method (A MANUFACTURING METHOD OF ANTIBACTERIAL NON WOVEN FABRIC, AND A ANTIBACTERIAL NON WOVEN FABRIC MANUFACTURED USING THE MANUFACTURING METHOD), and more specifically polypropylene It relates to a method for manufacturing an antibacterial nonwoven fabric containing copper deposition powder having antibacterial properties in fibers and an antibacterial nonwoven fabric manufactured by the manufacturing method.

In general, air filters and masks are manufactured using meltblown nonwoven fabric as a filter material. Various microorganisms can propagate on the surface of the nonwoven fabric from which various contaminants are filtered out. An antibacterial nonwoven fabric with this is being developed.

Meanwhile, silver, titanium dioxide, zinc oxide, copper, and the like are known as antibacterial agents harmless to the human body.

The silver is melted with nitric acid to make a metal salt with silver nitrate, and a dispersant is added, and the dispersant is added to the zeolite while being reduced again to prepare a fine silver nano-zeolite of 2 to 100 nm, which is used as an antibacterial agent.

The titanium dioxide is used as an antibacterial agent by making a fine powder by a mechanical milling method, but has the disadvantage of having to be irradiated with ultraviolet rays to exhibit antibacterial activity.

In addition, the zinc oxide is used as an antibacterial agent by a mechanical milling method or a method of reducing metal zinc as a metal salt by dissolving it in strong acid like the silver.

On the other hand, since the copper has excellent antibacterial activity and is inexpensive compared to the silver, a technique for manufacturing an antibacterial nonwoven fabric using it as a raw material for the nonwoven fabric is being developed.

As an example of an antibacterial nonwoven fabric technology manufactured using copper as a raw material, Korean Patent Registration No. 10-2239866 (2021.04.14.) (hereinafter referred to as 'prior art') discloses 'a copper-coated nonwoven fabric with excellent antibacterial and durable properties' A manufacturing method' is disclosed.

The prior art, (S1) depositing copper on PE raw material by physical vapor deposition to prepare a copper-deposited PE raw material, (S2) compounding the copper-deposited PE raw material to prepare a master batch, and then pelletizing ( pelletizing) and (S3) the pelletized copper-coated PE raw material as a sheath part, and the PP raw material as a core part by sheath core composite spinning to produce copper-coated PE sheath-PP core composite spun fibers and (S4) manufacturing the copper-coated PE sheath-PP core composite spun fiber into a thermal bond nonwoven fabric.

However, the copper has a stronger oxidizing power than the silver, so when copper is oxidized, there is a disadvantage of discoloration and a decrease in antibacterial activity. In the prior art, the copper-coated PE raw material obtained in step (S1) is Due to discoloration, there is a problem that not only has an adverse effect on the color setting of the nonwoven fabric, but also lowers the antimicrobial activity of the nonwoven fabric.

In addition, in the prior art, in manufacturing the copper-coated PE sheath-PP core composite spun fibers into a thermal bond nonwoven fabric in step (S4), a plurality of the copper-coated PE sheath-PP core composite spun fibers are laminated and then thermally bonded. Since the copper-coated PE sheath-PP core composite spun fiber is laminated on the base material PET fiber and then thermally bonded to produce the non-woven fabric, the copper-coated PE sheath-PP core composite spun fiber is not produced by manufacturing a nonwoven fabric. Compared to the case of manufacturing a nonwoven fabric by laminating and thermal bonding, there is also a problem in that antibacterial activity is relatively lowered.

The technical problem of the present invention is to deposit copper on calcium carbonate powder to prepare a copper antimicrobial agent that is relatively resistant to oxidation and use it as a raw material for nonwoven fabric, so that it is not only advantageous in setting the color of the nonwoven fabric but also has excellent antibacterial activity. To provide an antibacterial nonwoven fabric produced by the manufacturing method.

Another technical problem of the present invention is to manufacture a nonwoven fabric by laminating only the spun fibers prepared using the copper antimicrobial agent as a raw material without laminating the spun fibers prepared using the copper antimicrobial agent as a raw material on the base fiber, thereby providing excellent antibacterial activity. To provide an antibacterial nonwoven fabric manufacturing method and an antibacterial nonwoven fabric manufactured by the manufacturing method.

The technical problem of the present invention is not limited to the above-mentioned problems, and other problems not mentioned will be clearly understood by those skilled in the art from the following description.

In order to achieve the above object, the method for manufacturing an antimicrobial nonwoven fabric according to the present invention includes (S1) depositing copper on calcium carbonate powder to prepare a copper antimicrobial agent, (S2) mixing the copper antimicrobial agent with polypropylene to master the master Preparing a batch chip, (S3) preparing a single-layer nonwoven fabric by melt-spinning the master batch chip, and (S4) melt-spinning the master batch chip on at least one surface of the single-layer non-woven fabric to produce a multi-layer nonwoven fabric and (S5) embossing the multilayer nonwoven fabric with a pressure roller.

In the step (S1), the weight ratio of the calcium carbonate powder and the copper may be 99.7:0.3 to 98.0:2.0.

In the step (S1), the particle size of the calcium carbonate powder may be 1 to 3 μm.

In the step (S2), the weight ratio of the copper antimicrobial agent and the polypropylene may be 10.0:90.0 to 30.0:70.0.

In the step (S3) and the step (S4), the diameter of the fiber filament melt-spun from the master batch chip may be 10 to 30 μm.

In the (S3) step and the (S4) step, the masterbatch chip may have a density of 0.90 to 0.93g/cm 3 and a melt index of 20 to 60g/10min.

In the step (S5), the multilayer nonwoven fabric may have an embossing rate of 10 to 30% and a unit weight of 10 to 100 g/m 2 .

The antibacterial nonwoven fabric according to the present invention is prepared by the method for manufacturing the antibacterial nonwoven fabric according to the present invention.

Other embodiment specifics are included in the detailed description and drawings.

The antibacterial nonwoven fabric manufacturing method according to the present invention and the antibacterial nonwoven fabric produced by the manufacturing method are prepared by depositing copper on calcium carbonate powder to prepare a copper antimicrobial agent that is relatively resistant to oxidation and used as a raw material for the nonwoven fabric, thereby setting the color of the nonwoven fabric. Not only is it advantageous, but it also has the effect of improving antibacterial activity.

In addition, the method for manufacturing an antimicrobial nonwoven fabric according to the present invention and the antibacterial nonwoven fabric produced by the method are prepared by using the copper antimicrobial agent as a raw material without laminating the spun fibers produced using the copper antimicrobial agent as a raw material on the base fiber. Since the nonwoven fabric is manufactured by laminating only the spun fibers, the antimicrobial activity of the nonwoven fabric is excellent.

The effects of the present invention are not limited to the effects mentioned above, and other effects not mentioned will be clearly understood by those skilled in the art from the description of the claims.

1 is a view showing an apparatus for manufacturing a copper antimicrobial agent used as an antimicrobial raw material for an antibacterial nonwoven fabric according to embodiments of the present invention;

2 is a view showing observations over time after depositing copper on glucose, which is a white powder;

3 is a view showing observations over time after depositing copper on a polyethylene (PE) chip;

4 is a view showing observations over time after depositing copper on calcium carbonate powder;

5 is a block diagram showing a process according to a method for manufacturing an antibacterial nonwoven fabric according to embodiments of the present invention;

6 is a longitudinal cross-sectional view showing an antibacterial nonwoven fabric manufactured by the method for manufacturing an antibacterial nonwoven fabric according to a first embodiment of the present invention;

7 is a view showing an apparatus for manufacturing an antibacterial nonwoven fabric produced by a method for manufacturing an antibacterial nonwoven fabric according to a first embodiment of the present invention;

8 is a longitudinal cross-sectional view showing an antibacterial nonwoven fabric manufactured by a method for manufacturing an antibacterial nonwoven fabric according to a second embodiment of the present invention;

9 is a view showing an apparatus for manufacturing an antibacterial nonwoven fabric produced by a method for manufacturing an antibacterial nonwoven fabric according to a second embodiment of the present invention.

<Description of codes>

1: polypropylene resin 2a: first hopper

2b: second hopper 3a: first extruder

3b: second extruder 4a: first filter

4b: second filter 5a: first metering pump

5b: second metering pump 6a: first spin pack

6b: second spin pack 7a: first cooling and stretching device

7b: second cooling and stretching device 8: forming belt

9a: first suction device 9b: second suction device

10: cooling device 11: coupling device

12, 13: compression roller 14: winder

15: winder shaft 16: unwinder

17: unwinder shaft 18: preheating device

19, 20: heating plate 100, 200: antibacterial non-woven fabric

Hereinafter, a method for manufacturing an antibacterial nonwoven fabric according to embodiments of the present invention and an antibacterial nonwoven fabric manufactured by the manufacturing method will be described with reference to the drawings.

1 is a view showing an apparatus for manufacturing a copper antimicrobial agent used as an antimicrobial raw material for an antimicrobial nonwoven fabric according to embodiments of the present invention.

Referring to Figure 1, the copper antimicrobial agent used as an antibacterial raw material of the antibacterial nonwoven fabric according to embodiments of the present invention is prepared by depositing nano-sized copper on the surface of calcium carbonate powder. In order to nanonize copper, a mechanical milling method, a physical vapor deposition (PVD) method, a chemical method, etc. may be considered, but in this embodiment, metal copper is nanonized using the physical vapor deposition method and deposited on a carrier. method was used.

In addition, by conducting experiments with various materials to select a carrier on which copper will be deposited, and using a carrier that does not oxidize copper the most after copper is deposited, the copper antimicrobial agent is not easily oxidized and can be used as a raw material for nonwoven fabrics. When used, the color setting of the nonwoven fabric should not be adversely affected by discoloration due to oxidation, and when the copper was deposited on the calcium carbonate powder, it was concluded that the copper was not easily oxidized. It will be examined in detail later through examples.

An apparatus for manufacturing a copper antimicrobial agent according to embodiments of the present invention may include a vacuum deposition bath 30, a stirring bath 31, and stirring blades 32.

The vacuum deposition bath 30 may form a vacuum chamber therein. A vacuum generating means for forming a vacuum chamber may be provided in the vacuum deposition bath 30 , and the vacuum generating means may set the vacuum pressure in the vacuum deposition bath 30 to 10 ⁻³ to 10 ⁻⁵ torr.

The stirring tank 31 may be formed in a cylindrical shape with an open top. The calcium carbonate powder 40 as a carrier may be supported in the stirring tank 31 .

The stirring blades 32 may be rotatably provided on the bottom surface of the stirring tank 31 . The stirring blades 32 may be shaped like an axial flow fan having a plurality of blades. The rotating shaft of the stirring blades 32 may be arranged vertically. When the stirring blades 32 are rotated, the calcium carbonate powder supported in the stirring tank 31 may be stirred.

Copper 50 may be provided above the stirring bath 31 in the vacuum deposition bath 30 . By putting an inert gas into the vacuum chamber and applying a predetermined voltage to the copper 50 to generate copper plasma, the generated copper plasma is deposited on the surface of the calcium carbonate powder 40. Copper antimicrobial agents can be prepared by Here, the inert gas is a gas for generating the copper plasma, and it is preferable to put a small amount of the inert gas into the vacuum deposition tank 30 without filling it up.

As the copper plasma generating method, methods such as DC sputtering, RF sputtering, laser sputtering, electron beam evaporation, and thermal evaporation using a heating method may be used.

The inert gas introduced into the vacuum deposition bath 30 may be argon (Ar), neon (Ne), N2, O2, CH4, etc., preferably argon (Ar), but is not limited thereto.

The copper antimicrobial agent according to an embodiment of the present invention may be composed of calcium carbonate powder and copper. Here, the copper may be deposited on the surface of the calcium carbonate powder by physical vapor deposition. The weight ratio of the calcium carbonate powder and the copper may be 99.7:0.3 to 98.0:2.0. When the weight ratio of copper is lower than 0.3, the amount of copper deposited on the surface of the calcium carbonate powder is small, so antibacterial activity and deodorizing power may not be good. And, when the weight ratio of copper is greater than 2, the copper is deposited overlapping the surface of the calcium carbonate powder, and the specific surface area per weight of the copper is lowered, so antibacterial efficiency and deodorization efficiency may not be good.

The method of manufacturing a copper antimicrobial agent according to an embodiment of the present invention includes (a) supporting calcium carbonate powder 40 in a stirring tank 31, (b) putting an inert gas into a vacuum deposition tank 30 and vacuum Copper plasma is generated by targeting the copper 50 provided in the deposition bath 30, and the stirring blades 32 are rotated to deposit the copper 50 on the surface of the calcium carbonate powder 40 to obtain a copper antimicrobial agent It may include the step of preparing. In the copper antimicrobial agent prepared in step (b), the weight ratio of the calcium carbonate powder 40 and the copper 50 may be 99.7:0.3 to 98.0:2.0.

In the step (a) of the embodiment of the present invention, the particle size of the calcium carbonate powder 40 supported in the stirring tank 31 may be 1 to 3 μm. When the particle size of the calcium carbonate powder 40 is smaller than 1 μm, the copper 50 is deposited to overlap on the surface of the calcium carbonate powder 40, so that the specific surface area per weight of the copper 50 is lowered, resulting in antibacterial efficiency and deodorization efficiency. This may not be good, and the particles of the calcium carbonate powder 40 are too small, and the calcium carbonate powder 40 may scatter in the vacuum chamber when the stirring blades 32 rotate. Also, when the particle size of the calcium carbonate powder 40 is larger than 3 μm, the copper 50 may not be evenly deposited on the surface of the calcium carbonate powder 40 .

In the step (b) of the embodiment of the present invention, the vacuum pressure in the vacuum deposition bath 30 is 10 ^-3 to 10 ^-5 torr. When the vacuum pressure in the vacuum deposition tank 30 is higher than 10 ^-3 torr, the copper plasma generation rate is not good, so the amount of copper deposited on the surface of the calcium carbonate powder 40 may be small, and the vacuum deposition tank 30 ) When the vacuum pressure in the inside is lower than 10 ^-5 torr, the generation rate of the copper plasma is too high, and the amount of copper deposited on the surface of the calcium carbonate powder 40 may be too large.

Hereinafter, in depositing the copper 50 on the carrier, an experiment that led to the conclusion that the copper 50 is not easily oxidized when the calcium carbonate powder 40 is selected as the carrier will be described. do.

[Experiment 1] - Using glucose powder as a carrier

Using white powdered glucose powder as a carrier, 99.9% pure copper was deposited at 0.3% of the weight of the glucose powder by physical vapor deposition.

Glucose is a monosaccharide with a molecular formula of C ₆ H ₁₂ O ₆ , and anhydrous glucose crystals were used in the test.

The nano-copper deposition used the DC sputtering method, and the operation of the copper antimicrobial agent manufacturing device was carried out for 23 hours with 16KW of power to obtain a deposition amount of 3000ppm (0.3% by weight) of copper concentration.

Several conditions were implemented to reduce the time, but when the power of the copper antibacterial agent manufacturing device is over 16KW, the anhydrous glucose crystals melt at high temperature and stick to each other. It worked with 16KW of phosphorus.

2 is a view showing observations over time after depositing copper on glucose, which is a white powder.

Referring to FIG. 2 , the anhydrous glucose crystals, which were initially white powder, changed color to black red after copper deposition, as shown in (a) of FIG. 2 . After depositing copper, it was observed that the black-red color gradually changed to blue due to oxidation of copper over time when left under the condition of 80% RH relative humidity. That is, FIG. 2 (b) shows two months after depositing copper on anhydrous glucose crystals, and FIG. 2 (c) shows five months after depositing copper on anhydrous glucose crystals.

In this way, the copper antimicrobial agent prepared by depositing 0.3% by weight of copper relative to the weight of glucose powder is mixed with 1%, 3%, 5%, 10% and 20% of the weight of polypropylene, respectively, and injected. After making a plastic substrate having a width of 50 mm, a length of 50 mm, and a thickness of 1 mm, an antibacterial test was performed on the surface of the substrate.

The test method was JIS Z 2801: 2010 (film adhesion method), and the number of bacteria after 24 hours was compared with the control group for Staphylococcus aureus and Escherichia coli, and the test results are shown in Table 1 below.

division	Staphylococcus aureus	Escherichia coli
Initial bacterial count (CFL/mL)	2.7 x 10 5	2.2 x 10 5
control group	6.5 x 10 6	4.9 x 10 7
PP+CU/glucose 1%	0	0
PP+CU/glucose 3%	0	0
PP+CU/Glucose 5%	82.0%	0
PP+CU/glucose 10%	99.9%	0
PP+CU/glucose 20%	99.9%	99.9%

The test was conducted before the oxidation of the copper antimicrobial agent prepared by depositing 0.3% by weight of copper relative to the weight of the glucose powder, and after the oxidation progressed, even when 20% of the copper antimicrobial agent was mixed with respect to the weight of polypropylene (PP), E. coli The result was less than 99.9% of antibacterial activity. This can be seen as a result that antibacterial activity is exhibited even when oxidation proceeds, but the effect does not reach the non-oxidized state.

[Experiment 2] - Using a polyethylene (PE) chip as a carrier

Using a polyethylene chip (PE) as a carrier, copper of 99.9% purity was deposited by 0.3% of the weight of the polyethylene (PE) chip by physical vapor deposition.

Nano copper deposition used the DC sputtering method, and the operation of the inorganic antimicrobial agent manufacturing device was carried out for 13 hours with a power of 16KW to obtain a deposition amount of 3000ppm (0.3% by weight) of copper concentration.

In order to shorten the time, various conditions were implemented. In the power of 16KW or more of the inorganic antimicrobial agent manufacturing device, polyethylene (PE) chips melted at high temperature and entangled with each other, and the power of the copper antimicrobial agent manufacturing device I worked with 16KW, the limit of not sticking.

3 is a view showing observations over time after depositing copper on a polyethylene (PE) chip.

Referring to FIG. 3 , the initially transparent polyethylene (PE) chip had a color change to black after copper deposition, as shown in (a) of FIG. 3 . After depositing copper, it was observed that the black color gradually turned blue as time passed when left under the condition of 80% RH as the copper was oxidized. Figure 3 (b) shows four months after depositing copper on a polyethylene (PE) chip.

In this way, the copper antimicrobial agent prepared by depositing 0.3% by weight of copper relative to the weight of the polypropylene (PE) chip is mixed with 10%, 15%, and 20% of the weight of polypropylene, respectively, and injected to a width of 50 mm. , After making a plastic substrate having a length of 50 mm and a thickness of 1 mm, an antibacterial test was performed on the surface of the substrate.

The test method was JIS Z 2801: 2010 (film adhesion method), and the number of bacteria after 24 hours was compared with the control group for Staphylococcus aureus and Escherichia coli, and the test results are shown in Table 2 below.

division	Staphylococcus aureus	Escherichia coli
Initial bacterial count (CFL/mL)	1.4 x 10 4	1.4 x 10 4
control group	2.6 x 10 4	1.1 x 10 6
PP+Cu/PE 10%	0	71.8%
PP+Cu/PE 15%	0	82.4%
PP+Cu/PE 20%	99.9%	99.9%

The test was conducted before the oxidation of the copper antimicrobial agent prepared by depositing 0.3% by weight of copper relative to the weight of the polyethylene (PE) chip. Even when tested, the results were less than 99.9% of the antibacterial activity against E. coli. This can be seen as a result that antibacterial activity is exhibited even when oxidation proceeds, but the effect does not reach the non-oxidized state.

[Experiment 3] - Using calcium carbonate powder as a carrier

Using the white powdery calcium carbonate powder as a carrier, 99.9% pure copper was deposited by physical vapor deposition in an amount of 0.8% based on the weight of the calcium carbonate powder.

The calcium carbonate powder had a particle size of 1 to 3 μm, and calcium bicarbonate powder having a purity of 99.9% or more was used. Calcium carbonate powder has a larger particle size distribution than industrially manufactured glucose powder or polypropylene chips, so if you do not use powder that has been filtered to a uniform size, fine powders of 1 μm or less will scatter in the vacuum chamber, greatly impairing workability. showed

The nano-copper deposition used the DC sputtering method, and the operation of the inorganic antimicrobial agent manufacturing device was carried out for 8 hours with a power of 30KW to obtain a deposition amount of 9000ppm (0.8% by weight) of copper concentration.

Calcium carbonate powder does not melt even when the internal temperature rises to 300 ° C, so it is possible to work, and at high temperatures, the amount of deposition per hour is large, resulting in greatly improved productivity.

That is, calcium carbonate powder does not melt even at high temperatures, so it has higher productivity of inorganic antimicrobial agents when used as a carrier than other materials, and it is easy to store because it is difficult to oxidize even after time elapses after copper is deposited on calcium carbonate powder. and showed high antibacterial activity when used as an antibacterial agent.

The reason why calcium carbonate powder prevents oxidation of copper over time is that calcium carbonate has a calcite structure, so the calcium (Ca) cation (+2 valency) and carbonate (CO ₃ ) anion (-2 valency) This is because in the ionic bond, three oxygens (O) and copper, which are coordinated around carbon (C), are stabilized by exchanging electrons.

4 is a view showing observations over time after depositing copper on calcium carbonate powder.

Referring to FIG. 4 , the calcium carbonate powder, which was initially a white powder, had a color change to grayish red after copper deposition, as shown in FIG. 4 (a). After depositing copper, it was observed that the grayish-red calcium carbonate powder did not oxidize and maintained its color over time when left under the condition of a relative humidity of 80% RH. Figure 4 (b) shows two months after depositing copper on calcium carbonate powder, and Figure 4 (c) shows five months after depositing copper on calcium carbonate powder.

In this way, the copper antimicrobial agent prepared by depositing 0.8% by weight of copper relative to the weight of calcium carbonate powder is mixed with 0.5%, 1%, 3%, and 5% of the weight of polypropylene in polypropylene, respectively, and injected to a width of 50 mm. , After making a plastic substrate having a length of 50 mm and a thickness of 1 mm, an antibacterial test was performed on the surface of the substrate.

The test method was JIS Z 2801: 2010 (film adhesion method), and the number of bacteria after 24 hours was compared with the control group for Staphylococcus aureus and Escherichia coli, and the test results are shown in Table 3 below.

division	Staphylococcus aureus	Escherichia coli
Initial bacterial count (CFL/mL)	1.5 x 10 4	1.4 x 10 4
control group	3.0 x 10 4	3.3 x 10 5
PP+Cu/calcium carbonate 0.5%	99.9%	0
PP+Cu/calcium carbonate 1%	99.9%	92.7%
PP+Cu/calcium carbonate 3%	99.9%	99.9%
PP+Cu/calcium carbonate 5%	99.9%	99.9%

In the test, 0.8% by weight of copper was deposited relative to the weight of the calcium carbonate powder, and the copper antimicrobial agent was tested with two months after the preparation.

As such, it can be seen that the copper antimicrobial agent prepared by depositing copper on the surface of the calcium carbonate powder has little discoloration and excellent antibacterial activity over time. Therefore, when the copper antimicrobial agent prepared by depositing copper on the surface of calcium carbonate powder is used as a raw material for nonwoven fabric, not only can the freedom of color setting of the nonwoven fabric be increased, but also antibacterial activity can be maintained for a long time.

5 is a block diagram showing a process according to a method for manufacturing an antibacterial nonwoven fabric according to embodiments of the present invention.

Referring to Figure 5, the method of manufacturing an antibacterial nonwoven fabric according to embodiments of the present invention, (S1) depositing copper on calcium carbonate powder to prepare a copper antimicrobial agent, (S2) the copper antimicrobial agent with polypropylene Mixing to prepare a masterbatch chip, (S3) melt-spinning the masterbatch chip to prepare a single-layer nonwoven fabric, (S4) melt-spinning the masterbatch chip on at least one surface of the single-layer nonwoven fabric to produce a multi-layer nonwoven fabric and (S5) embossing the multilayer nonwoven fabric with a compression roller.

In the step (S1), the weight ratio of the calcium carbonate powder and the copper may be 99.7:0.3 to 98.0:2.0. When the weight ratio of copper is lower than 0.3, the amount of copper deposited on the surface of the calcium carbonate powder is small, so antibacterial activity and deodorizing power may not be good. And, when the weight ratio of copper is greater than 2, the copper is deposited overlapping the surface of the calcium carbonate powder, and the specific surface area per weight of the copper is lowered, so antibacterial efficiency and deodorization efficiency may not be good.

In addition, in the step (S1), the particle size of the calcium carbonate powder may be 1 to 3 μm. When the particle size of the calcium carbonate powder 40 is smaller than 1 μm, the copper 50 is deposited to overlap on the surface of the calcium carbonate powder 40, so that the specific surface area per weight of the copper 50 is lowered, resulting in antibacterial efficiency and deodorization efficiency. This may not be good, and the particles of the calcium carbonate powder 40 are too small, and the calcium carbonate powder 40 may scatter in the vacuum chamber when the stirring blades 32 rotate. Also, when the particle size of the calcium carbonate powder 40 is larger than 3 μm, the copper 50 may not be evenly deposited on the surface of the calcium carbonate powder 40 .

In the step (S2), the weight ratio of the copper antimicrobial agent and the polypropylene may be 10.0:90.0 to 30.0:70.0. The copper antimicrobial agent is mixed with the polypropylene at a ratio of 10 to 30% by weight. If mixed at a ratio lower than 10% by weight, the effect of eradicating bacteria and viruses is insufficient, which is undesirable. It is undesirable because spinnability is lowered and productivity is deteriorated.

In the step (S3), the single-layer nonwoven fabric may be a one-ply nonwoven fabric constituting the multi-layer nonwoven fabric, and in the step (S4), the single-layer nonwoven fabric is at least two plies Alternatively, it may be a structure composed of at least two layers. The single-layer nonwoven fabric constituting one multi-layer non-woven fabric may have the same physical properties and size, but, if necessary, single-layer non-woven fabrics having different requirements such as thickness may be laminated and combined to form one multi-layer non-woven fabric. The thickness of the single-layer nonwoven fabric is not particularly limited, and a nonwoven fabric having a thickness commonly used in the art may be used in consideration of the purpose of the final product and the number of layers. Hereinafter, in the description, 'two layers' may be used as the same meaning as 'two layers', and 'three layers' may be used as the same meaning as 'three layers'.

In the step (S3) and the step (S4), the diameter of the fiber filament melt-spun from the master batch chip may be 10 to 30 μm. If the diameter of the fiber filament is less than 10㎛, the filament is too thin and sufficient breaking strength is not exhibited. If the diameter of the fiber filament exceeds 30㎛, the filament is too thick and orientation is not sufficiently achieved, so the breaking strength is reduced. It becomes inflexible and difficult to use as a product.

In the (S3) step and the (S4) step, the masterbatch chip may have a density of 0.90 to 0.93g/cm 3 and a melt index of 20 to 60g/10min. When the density of the masterbatch chip is less than 0.90 g / cm 3, the strength of the nonwoven fabric may be lowered, and when the density of the masterbatch chip exceeds 0.93 g / cm 3, the melting temperature increases and the adhesion temperature of the nonwoven fabric increases. A problem may occur. . When the melt index of the masterbatch chip is less than 20g/10min, the flowability of the melt is too low, making it difficult to form fibers, making it difficult to manufacture a nonwoven fabric, and when the melt index of the masterbatch chip exceeds 60g/10min, the strength of the nonwoven fabric A problem of lowering may occur.

In the step (S5), the multilayer nonwoven fabric may have an embossing rate of 10 to 30% and a unit weight of 10 to 100 g/m 2 . When the embossing rate is less than 5%, the adhesive strength between single-layer nonwoven fabrics is lowered and the unit nonwoven fabrics may be separated from each other, and when the embossing rate exceeds 30%, product flexibility is lowered. If the unit weight of the multi-layer nonwoven fabric is less than 10 g / m 2, the breaking strength is weak and cannot be used as a product.

The cooling, which may be performed between the steps (S4) and (S5), may be performed at a temperature of 25° C. or less, and may be performed using a conventional cooling device. When the cooling temperature exceeds 25 ° C., the surface of the single-layer nonwoven fabric becomes smooth, and even if a compression roller is used, physical bonding between the single-layer nonwoven fabrics may not occur well. In the present invention, the compression roller compresses the multilayer nonwoven fabric under certain conditions so that embossing is expressed.

In the step (S5), at least one of heat and adhesive (binder) may be used together with the compression roller. In the case of using heat, the temperature of the compression roller may be in the range of 130 to 170 ° C. in order to appropriately suppress the increase in elongation. When the temperature of the compression roller is less than 130° C., the multi-layered nonwoven fabric does not receive enough heat, and thus the adhesive strength between the single-layer nonwoven fabrics is lowered. When the temperature of the compression roller exceeds 170 ° C., the surface of the multilayer nonwoven fabric is melted and adhered to the compression roller so that the operation does not proceed or the multilayer nonwoven fabric is damaged by heat and the strength is lowered.

6 is a longitudinal cross-sectional view showing an antibacterial nonwoven fabric manufactured by the method for manufacturing an antibacterial nonwoven fabric according to a first embodiment of the present invention. Here, the embossing treatment of the antibacterial nonwoven fabric 100 is not expressed.

Referring to FIG. 6, the antibacterial nonwoven fabric 100 according to the first embodiment of the present invention has two layers of single layer nonwoven fabrics 101 and 102 in which a second single layer nonwoven fabric 102 is overlapped on the first single layer nonwoven fabric 101. ) can be formed. Here, both the first single-layer nonwoven fabric 101 and the second single-layer nonwoven fabric 102 may be formed of a nonwoven fabric containing the copper antimicrobial agent.

7 is a view showing an apparatus for manufacturing an antibacterial nonwoven fabric produced by a method for manufacturing an antibacterial nonwoven fabric according to a first embodiment of the present invention.

6 and 7, the manufacturing apparatus of the antibacterial nonwoven fabric 100 manufactured by the manufacturing method of the antibacterial nonwoven fabric 100 according to the first embodiment of the present invention, a forming belt (forming belt, 8), A first melt spinning machine 21 and a second melt spinning machine 22 disposed apart from each other in the conveying direction of the forming belt 8 on the upper side of the forming belt 8, a cooling device 10, and a coupling device 11 ) and a winder 14.

Here, the first melt spinning machine 21 and the second melt spinning machine 22 may be devices for forming web-type fiber filaments by melt spinning the master batch chip 1. The first melt spinning machine 21 may be for forming the first single layer nonwoven fabric 101 of the antibacterial nonwoven fabric 100, and the second melt spinning machine 22 is the second single layer nonwoven fabric 102 of the antibacterial nonwoven fabric 100 It may be for forming.

The first melt spinning machine 21 and the second melt spinning machine 22 may be formed in the same structure. Specifically, the first melt spinning machine 21 includes a first hopper 2a, a first extruder 3a, a first filter 4a, a first metering pump 5a, a first spin pack 6a, a first 1 cooling and stretching device 7a and a first suction device 9a. And, the second melt spinning machine 22, the second hopper (2b), the second extruder (3b), the second filter (4b), the second metering pump (5b), the second spin pack (6b), the second A cooling and stretching device 7b and a second suction device 9b may be included.

The manufacturing of the first single-layer nonwoven fabric 101 is described with reference to FIGS. 6 and 7 as follows.

The masterbatch chips 1 are supplied to the first extruder 3a through the first hopper 2a and melted. The molten masterbatch chips are supplied to the first spin pack 6a in a constant amount through the first metering pump 5a after impurities are removed through the first filter 4a. In the first spin pack 6a, fiber filaments are formed through a spinneret having a diameter of 0.3 to 1.0 mm. At this time, the fiber filaments may have a diameter of 10 to 30 μm. The formed fiber filaments are cooled and stretched by air in the first cooling and stretching device 7a, and then seated on the forming belt 8 by the first suction device 9a to form a web, thereby forming a first single-layer nonwoven fabric ( 101) is formed and transferred to the side of the second melt spinning machine 22.

The manufacturing of the two-ply multilayer nonwoven fabric 101 and 102 by laminating the second single layer nonwoven fabric 102 on the first single layer nonwoven fabric 101 will be described with reference to FIGS. 6 and 7 as follows.

The second single layer nonwoven fabric 102 may be formed by the second melt spinning machine 22 on the first single layer nonwoven fabric 101 transferred to the side of the second melt spinning machine 22 through the forming belt 8. That is, the masterbatch chips 1 are supplied to the second extruder 4b through the second hopper 2b and melted. The molten masterbatch chips 1 are supplied to the second spin pack 6b in a constant amount through the second metering pump 5b after impurities are removed through the second filter 4b. In the second spin pack 6b, fiber filaments are formed through a spinneret having a diameter of 0.3 to 1.0 mm. The formed fiber filaments are cooled and stretched through the second cooling and stretching device 7b, and then seated on the first single-layer nonwoven fabric 101 by the second suction device 9b to form a web, thereby forming a two-layer multilayer nonwoven fabric. (101, 102) are formed.

The two layers of multilayer nonwoven fabrics 101 and 102 formed on the forming belt 8 may be cooled to 25° C. or less by the cooling device 10.

The cooled two-ply multilayer nonwoven fabrics 101 and 102 may be coupled while being embossed by the compression rollers 12 and 13 of the coupling device 11. The compression roller 12 is embossed with a pattern such as a diamond shape or a circular or oval shape, so that the multilayer nonwoven fabrics 101 and 102 stacked in two layers are embossed at the same time, and as a result, the finally obtained multilayer nonwoven fabric 101 , 102) on which embossing is formed. The embossing rate, which is the area occupied by the embossed pattern among the total surface areas of the multilayer nonwoven fabrics 101 and 102, may be in the range of 5 to 30%. When the embossing rate is less than 5%, the first single-layer nonwoven fabric 101 and the second single-layer nonwoven fabric 102 may be separated from each other because of weak adhesive or bonding strength, and when the embossing rate exceeds 30%, the product Flexibility may be reduced.

The antibacterial nonwoven fabric 100 formed of the two layers of embossed multilayer nonwoven fabrics 101 and 102 may be wound around the winder shaft 15 of the winder 14 .

8 is a longitudinal cross-sectional view showing an antibacterial nonwoven fabric manufactured by a method for manufacturing an antibacterial nonwoven fabric according to a second embodiment of the present invention. Here, the embossing treatment of the antibacterial nonwoven fabric 200 is not expressed.

Referring to FIG. 8, the antibacterial nonwoven fabric 200 according to the second embodiment of the present invention is a three-layered single-layer nonwoven fabric in which the second single-layer nonwoven fabric 102 is overlapped on the upper and lower surfaces of the first single-layer nonwoven fabric 101, respectively ( 101, 102). Here, both the first single-layer nonwoven fabric 101 and the second single-layer nonwoven fabric 102 may be formed of a nonwoven fabric containing the copper antimicrobial agent.

9 is a view showing an apparatus for manufacturing an antibacterial nonwoven fabric produced by a method for manufacturing an antibacterial nonwoven fabric according to a second embodiment of the present invention.

8 and 9, the manufacturing apparatus of the antibacterial nonwoven fabric 200 manufactured by the manufacturing method of the antibacterial nonwoven fabric 200 according to the second embodiment of the present invention, in the first embodiment of the present invention described above Compared to the manufacturing apparatus of the antibacterial nonwoven fabric 100 manufactured by the manufacturing method of the antibacterial nonwoven fabric 100 by the method, the unwinder 16 and the preheating device 18 may be further included.

Here, the unwinder 16 may include an unwinder shaft 17 . Unwinder 16 may be disposed opposite to winder 14 . Here, the unwinder shaft 17 may have substantially the same configuration as the winder shaft 15 . That is, the winder shaft 15 on which the two layers of multilayer nonwoven fabrics 101 and 102 manufactured in the first embodiment are wound may be mounted on the unwinder 16 to become the unwinder shaft 17.

That is, the antibacterial nonwoven fabric 200 according to the second embodiment of the present invention is preheated while the antibacterial nonwoven fabric 100 manufactured in the first embodiment is unwound from the unwinder shaft 17 of the unwinder 16. After being preheated while passing through the heating plates 19 and 20 of the device 18, the antibacterial nonwoven fabric 100 is supplied to the forming belt 8 so that the lower surface faces upward, and then the process of the first embodiment described above By repeating the same, an antibacterial nonwoven fabric 200 formed of three layers of multilayer nonwoven fabrics 101 and 102 can be manufactured.

Hereinafter, examples will be described in detail to explain the present invention in detail.

<Example 1: Preparation of nonwoven fabric>

The masterbatch chip (1) prepared by mixing 15% by weight of copper antimicrobial agent with 85% by weight of polypropylene is introduced into the first extruder (3a) having a temperature of 230 ° C through the first hopper (2a) and melted. After removing impurities by passing them through the filter 4a, they were supplied to the first spin pack 6a using the first metering pump 5a, and then spun through a spinneret having a temperature of 220°C in the first spin pack 6a. . The spun fiber filaments are cooled and drawn by the first cooling and stretching device 7a, and then seated on the forming belt 8 by the first suction device 9a to form a web, thereby forming a first single layer nonwoven fabric 101. ) was formed.

In order to laminate the second single-layer nonwoven fabric 102 on the first single-layer nonwoven fabric 101, the masterbatch chip 1 prepared by mixing 15% by weight of a copper antimicrobial agent with 85% by weight of polypropylene is mixed with the second hopper 2b through the second extruder (3b) at a temperature of 230 ° C., melted, passed through the second filter (4b) to remove impurities, and then supplied to the second spin pack (6b) using the second metering pump (5b) Thus, the second spin pack 6b was spun through a spinneret having a temperature of 220°C. The spun fiber filaments are cooled and drawn by the second cooling and stretching device 7b, and then seated on the first single-layer nonwoven fabric 101 by the second suction device 9b to form a web, thereby forming two layers of multilayer Nonwoven fabrics 101 and 102 were formed.

The two layers of multilayer nonwoven fabrics 101 and 102 on the forming belt 8 passed through the cooling device 10 maintained at 20°C. Subsequently, the compression rollers 12 and 13 having an embossing rate of 14% are pressed and embossed on the two layers of multilayer nonwoven fabrics 101 and 102 at a pressure of 5 kgf / cm 2 and a temperature of 165 ° C. 102) to prepare an antibacterial nonwoven fabric (100). The prepared antibacterial nonwoven fabric 100 was wound around the winder shaft 15 of the winder 14 to a certain length.

<Example 2: Preparation of nonwoven fabric>

A multilayer nonwoven fabric was prepared in the same manner as in Example 1, except that 12% by weight of the copper antimicrobial agent was changed to a masterbatch chip prepared by mixing 88% by weight of polypropylene.

<Example 3: Preparation of nonwoven fabric>

A multilayer nonwoven fabric was prepared in the same manner as in Example 1, except that 27% by weight of the copper antimicrobial agent was changed to a masterbatch chip prepared by mixing 73% by weight of polypropylene.

<Example 4: Preparation of nonwoven fabric>

A multilayer nonwoven fabric was prepared in the same manner as in Example 1, except that the fiber filament diameter was changed to 12 μm.

<Example 5: Preparation of nonwoven fabric>

A multilayer nonwoven fabric was prepared in the same manner as in Example 1, except that the fiber filament diameter was changed to 27 μm.

<Comparative Example 1: Manufacture of nonwoven fabric>

A multilayer nonwoven fabric was prepared in the same manner as in Example 1, except that 8% by weight of the copper antimicrobial agent was mixed with 92% by weight of polypropylene to change to a masterbatch chip.

<Comparative Example 2: Manufacture of nonwoven fabric>

A multilayer nonwoven fabric was prepared in the same manner as in Example 1, except that 35% by weight of the copper antimicrobial agent was mixed with 65% by weight of polypropylene to change to a masterbatch chip.

<Comparative Example 3: Manufacture of nonwoven fabric>

A multilayer nonwoven fabric was prepared in the same manner as in Example 1, except that the fiber filament diameter was changed to 7 μm.

<Comparative Example 4: Manufacture of nonwoven fabric>

A multilayer nonwoven fabric was prepared in the same manner as in Example 1, except that the fiber filament diameter was changed to 40 μm.

Evaluation Example 1: Measurement of strength and elongation KS K ISO 9073-3

For this evaluation, the breaking strength and elongation values were measured from the load-elongation curve recorded after constant rate elongation so that force was applied in the longitudinal direction for the test piece of the specified length and width. The nonwoven fabric cut to a width of 50 mm was gripped by a strength measuring machine to a length of 75 mm, and then measured at a speed of 300 mm/min.

item			Example 1	Example 2	Example 3	Example 4	Example 5
polypropylene non-woven fabric	Composition ratio (% by weight)	polypropylene	85	88	73	85	85
		copper antimicrobial	15	12	27	15	15
	Fiber filament diameter (μm)		20	20	20	12	27
	radiation fairness		Good	Good	Good	Good	Good
Combination condition	Preheating temperature (℃)		130	130	130	130	130
	Cooling temperature (℃)		20	20	20	20	20
	Compression roller pressure (kgf/㎠)		5	5	5	5	5
	Pressure roller temperature (℃)		165	165	165	165	165
	Embossing rate (%)		14	14	14	14	14
Multi-layer polypropylene non-woven fabric	Unit weight (g/㎡)		70	70	70	70	70
	Strength (kg/5cm)	longitudinal direction	21.2	21.3	20.9	21.2	21.1
		width direction	13.6	13.6	12.8	12.6	12.8
	Elongation (%/5cm)	longitudinal direction	74	76	70	70	72
		width direction	94	94	88	96	90
	antibacterial performance		Good	Good	Good	Good	Good

item			Comparative Example 1	Comparative Example 2	Comparative Example 3	Comparative Example 4
polypropylene non-woven fabric	Composition ratio (% by weight)	polypropylene	92	65	85	85
		copper antimicrobial	8	35	15	15
	Fiber filament diameter (μm)		20	20	7	40
	radiation fairness		Good	error	error	Good
Combination condition	Preheating temperature (℃)		130	130	130	130
	Cooling temperature (℃)		20	20	20	20
	Compression roller pressure (kgf/㎠)		5	5	5	5
	Pressure roller temperature (℃)		165	165	165	165
	Embossing rate (%)		14	14	14	14
Multi-layer polypropylene non-woven fabric	Unit weight (g/㎡)		70	70	70	70
	Strength (kg/5cm)	longitudinal direction	21.7	19.1	18.4	17.6
		width direction	14.4	11.4	9.0	8.2
	Elongation (%/5cm)	longitudinal direction	78	62	48	50
		width direction	100	86	71	74
	antibacterial performance		fall short	Good	Good	fall short

Referring to Tables 4 and 5, in Examples 1 to 3 and Comparative Examples 1 and 2 according to the addition ratio of the copper antimicrobial agent, in the case of Comparative Example 1 in which the addition ratio of the copper antimicrobial agent was 8% by weight In the case of Comparative Example 2 in which the antimicrobial performance is insufficient and the addition ratio of the copper antimicrobial agent is 35% by weight, the product cannot be mass-produced due to poor spinning processability.

Looking at Examples 4 and 5 and Comparative Examples 3 and 4 for comparison of effects according to the fiber filament diameter, in the case of Comparative Example 3 having a fiber filament diameter of 7 μm, the spinning fairness was poor and the fiber was too thin In the case of Comparative Example 4 in which the fiber filament diameter is 40 μm, the fiber is too thick, so the temperature is not sufficiently transmitted during bonding, so that the bonding is not properly performed, resulting in layer separation, resulting in low strength and poor antibacterial performance. Because of this, it is difficult to use as a product.

As described above, the manufacturing method of the antibacterial nonwoven fabric (100, 200) according to the embodiments of the present invention and the antibacterial nonwoven fabric (100, 200) manufactured by the manufacturing method are relatively oxidized by depositing copper on calcium carbonate powder. By manufacturing a copper antimicrobial agent resistant to and using it as a raw material for nonwoven fabric, it is not only advantageous to set the color of the nonwoven fabric, but also has excellent antibacterial power.

In addition, the manufacturing method of the antibacterial nonwoven fabric (100, 200) according to the embodiments of the present invention and the antibacterial nonwoven fabric (100, 200) manufactured by the manufacturing method are based on spun fibers manufactured using copper antimicrobial agent as a raw material Since the nonwoven fabric is manufactured by laminating only the spun fibers produced using the copper antimicrobial agent as a raw material without laminating the fiber, the antimicrobial activity of the nonwoven fabric can be improved.

Those skilled in the art to which the present invention pertains will understand that the present invention can be embodied in other specific forms without changing its technical spirit or essential features. Therefore, it should be understood that the embodiments described above are illustrative in all respects and not restrictive. The scope of the present invention is indicated by the following claims rather than the above detailed description, and all changes or modifications derived from the meaning and scope of the claims and equivalent concepts thereof should be construed as being included in the scope of the present invention.

The present invention is to deposit copper on calcium carbonate powder to prepare a copper antimicrobial agent that is relatively resistant to oxidation and use it as a raw material for nonwoven fabric, thereby providing a method for manufacturing an antibacterial nonwoven fabric that is not only advantageous in setting the color of the nonwoven fabric but also has excellent antimicrobial activity, and a manufacturing method thereof. Provided is an antibacterial nonwoven fabric manufactured.

Claims (8)

1. (S1) preparing a copper antimicrobial agent by depositing copper on calcium carbonate powder;

   (S2) preparing a masterbatch chip by mixing the copper antimicrobial agent with polypropylene;

   (S3) preparing a single-layer nonwoven fabric by melt-spinning the master batch chips;

   (S4) preparing a multi-layer non-woven fabric by melt-spinning the master batch chips on at least one surface of the single-layer non-woven fabric; and

   (S5) step of embossing the multi-layer non-woven fabric with a compression roller; manufacturing method of the antibacterial non-woven fabric containing.
2. The method of claim 1,

   In the step (S1),

   The weight ratio of the calcium carbonate powder and the copper is 99.7: 0.3 to 98.0: 2.0 method of producing an antibacterial nonwoven fabric.
3. The method of claim 2,

   In the step (S1),

   The particle size of the calcium carbonate powder is a method for producing an antibacterial nonwoven fabric of 1 to 3㎛.
4. The method of claim 3,

   In the step (S2),

   The weight ratio of the copper antimicrobial agent and the polypropylene is 10.0: 90.0 to 30.0: 70.0 method of producing an antibacterial nonwoven fabric.
5. The method of claim 4,

   In the step (S3) and the step (S4),

   Method for producing an antibacterial nonwoven fabric having a diameter of 10 to 30 μm of the fiber filament obtained by melt-spinning the masterbatch chip.
6. The method of claim 5,

   In the step (S3) and the step (S4),

   The masterbatch chip has a density of 0.90 to 0.93 g / cm 3 and a melt index of 20 to 60 g / 10 min. Method for producing an antibacterial nonwoven fabric.
7. The method of claim 6,

   In the step (S5),

   The multi-layer nonwoven fabric has an embossing rate of 10 to 30% and a unit weight of 10 to 100 g / m 2 Method for producing an antibacterial nonwoven fabric.
8. An antibacterial nonwoven fabric manufactured by the method for manufacturing an antibacterial nonwoven fabric according to any one of claims 1 to 7.

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