KR101572613B1 - an antibacterial composition and a wet tissue having the same - Google Patents

Abstract

The present invention relates to an antibacterial composition harmless to a human body and antibacterial wet wipes comprising the same. The antibacterial composition and the antibacterial wet wipes according to the present invention comprise zinc oxide, citric acid and sodium citrate. The present invention can implement an antibacterial composition harmless to the human body, and can also implement antibacterial wet wipes which is harmless to the human body and has excellent antibacterial property using the antibacterial composition.

Description

The present invention relates to an antimicrobial composition harmless to humans and an antibacterial composition and a wet tissue having the same,

The present invention relates to an antibacterial composition harmless to humans and an antibacterial wet tissue including the same, and more particularly, to an antibacterial composition having an antibacterial property including an environmentally friendly substance without being harmful to human body, and an antibacterial wet tissue containing the same.

Currently, microorganisms such as bacteria and fungi in everyday life are not only highly abundant but also widely distributed in the natural world such as soil, air, water, and seawater, and can grow and reproduce at any time if their growth conditions are met. Disease, food spoilage, housing, clothing, and industrial products are all seriously affected by microorganisms.

As a result, it is recognized that microbial damage is serious in textile, plastic, paper, wood, metal, glass and the like for a long time. Therefore, researches on prevention measures have been actively carried out, and diapers, Chloromethylisothiazolinone (CMIT), 3-lodo-2-propylbutylcarbamate (3-iodophenylacetamide) and the like are used in order to remove or suppress the occurrence of microorganisms propagating in cosmetics, detergents, propynylbutylcarbamate (IPBC), benzalkonium chloride, polyhexamethylene guanidine (PHMG), polyhexamethylene biguanide (PHMB), and oligo (2- (2-ethoxy) ethoxyethyl guanidine chloride)

It is used as antibacterial and fungicide. However, these conventional antibacterial and fungicidal agents are currently restricted in use or restricted in use due to human toxicity and skin irritation.

In general, a wet tissue is provided with a function of cleaning the skin by adding purified water, a moisturizer, a surfactant, a vegetable preservative, a fragrance and the like to the nonwoven fabric. In recent years, along with the development of the food service industry, the consumption of wipes is also increasing. In the past, antibacterial wipes were used to prevent bacteria by disinfecting the antiseptic wipes during the wet tissue manufacturing process. This can stimulate the skin, and the second bacterium may propagate in wet wipes and resins during distribution. In addition, existing wet tissues may be contaminated with bacteria even after sterilization, after exposure to air.

A wet tissue product can be prepared by impregnating a nonwoven fabric with a composition for a wet tissue. At this time, 90 to 95% of the composition for a wet tissue is composed of water, and the rest is generally composed of a surfactant, a disinfectant, a preservative, a moisturizer, an incense, and a deodorant. The conventional wet tissue contains a large amount of a chemical sterilizing agent and a preservative, so that it can have a certain degree of hygienic effect, but it is insufficient in terms of environmental viewpoint and influence on the human body. Therefore, it is required to reduce the use of the conventional chemical antimicrobial agent and to develop a wet tissue product which is environmentally friendly and harmless to human body.

Conventionally, an organic antimicrobial agent has been used in order to secure the antimicrobial activity. Recently, development of an inorganic antimicrobial agent has been proceeding due to controversy about human health. For example, the Korean Registered Utility Model No. 20-0384399 (May 05, 2005) discloses a wet tissue produced by impregnating tributaries and fabrics with chemicals such as nano-silver-treated water, a surfactant, and antifungal agents and preservatives , And the wet tissue is prepared by impregnating the wetted tissue with 25 to 150 ppm of nanosilver-treated water. Korean Patent Registration No. 10-0752111 (Aug. 20, 2007) discloses nano silver having an average particle diameter of 5 to 50 nm and a purity of 92% or more, and a titanium dioxide or anatase type titanium dioxide having an average particle diameter of 5 to 10 nm An antimicrobial wet tissue containing nanoparticles is disclosed.

1. Korean Registered Utility Model No. 20-0384399 (May 5, 2005) 2. Korean Patent Registration No. 10-0752111 (Aug. 20, 2007)

The present invention provides an antimicrobial composition which is harmless to human body and excellent in antibacterial activity and an antimicrobial wet tissue containing the antimicrobial composition.

In order to solve the above problems,

The first aspect of the present invention may be an antimicrobial composition characterized in that it comprises zinc oxide, citric acid and sodium citrate.

The zinc oxide may have an average particle diameter of the primary particles of 10 nm to 50 nm and an average particle diameter of the secondary particles of 300 nm to 1 um.

In 100 parts by weight of the total composition, zinc oxide may be 0.1 to 5 parts by weight, citric acid may be 0.1 to 5 parts by weight, sodium citrate may be 0.1 to 5 parts by weight, and the balance may be purified water.

A second aspect of the present invention is a method for preparing a slurry comprising: (a) milling a zinc oxide slurry to adjust the zinc oxide particle size, (b) adding a citric acid to the slurry and stirring the slurry, (c) Adding and stirring, and (d) stabilizing the slurry.

A third aspect of the present invention is a method for producing a zinc oxide slurry, comprising the steps of: (a) milling zinc oxide powder to adjust the particle size of zinc oxide; (b) adding purified water to zinc oxide and stirring to prepare a zinc oxide slurry; Adding the citric acid to the slurry and stirring the slurry, (d) adding the sodium citrate to the slurry and stirring the slurry, and (e) stabilizing the slurry.

In the step (a) of the second and third aspects, the size of the milled zinc oxide is such that the average particle diameter of the primary particles is 10 nm to 50 nm, the average particle diameter of the secondary particles is 1 to 15 μm, The size of the post-zinc oxide may be an average particle size of the secondary particles of 300 nm to 1 um.

In the second and third aspects, 0.1 to 5 parts by weight of zinc oxide, 0.1 to 5 parts by weight of citric acid and 0.1 to 5 parts by weight of sodium citrate are contained in 100 parts by weight of the total composition, .

A fourth aspect of the present invention may be an antimicrobial wet tissue characterized in that it comprises zinc oxide, citric acid and sodium citrate.

The zinc oxide may have an average particle diameter of the primary particles of 10 nm to 50 nm and an average particle diameter of the secondary particles of 300 nm to 1 um.

In 100 parts by weight of the total composition, zinc oxide may be 0.1 to 5 parts by weight, citric acid may be 0.1 to 5 parts by weight, sodium citrate may be 0.1 to 5 parts by weight, and the balance may be purified water.

According to the present invention, an antimicrobial composition which is harmless to human body can be produced, and an antimicrobial wet tissue which is harmless to human body and excellent in antibacterial property can be produced by using such antimicrobial composition.

1 is a result of a test for the antibacterial activity against Staphylococcus aureus ATCC 6538 (strain 1) of an antimicrobial composition according to an embodiment of the present invention.
2 is a result of a test of the antibacterial activity against Escherichia coli ATCC 25922 (strain 2) of the antimicrobial composition according to an embodiment of the present invention.
FIG. 3 is a result of a test for the antibacterial activity against Pseudomonas aeruginosa ATCC 27853 (strain 3) of the antimicrobial composition according to an embodiment of the present invention.

Hereinafter, preferred embodiments of the present invention will be described with reference to the accompanying drawings. The embodiments of the present invention can be modified into various other forms, and the scope of the present invention is not limited to the embodiments described below. Furthermore, embodiments of the present invention are provided to more fully explain the present invention to those skilled in the art. Accordingly, the shapes and sizes of the elements in the drawings may be exaggerated for clarity of description, and the elements denoted by the same reference numerals in the drawings are the same elements.

A first aspect of the present invention may be an antimicrobial composition characterized by comprising zinc oxide, citric acid and sodium citrate. The remainder excluding the above components may be purified water.

In the case of a composition prepared by injecting only citric acid into a zinc oxide slurry, precipitation may occur. It is a feature of the present invention that precipitation does not occur by further adding sodium citrate.

The antimicrobial composition according to this aspect is a transparent solution, and is a transparent solution composition having excellent dispersion stability without causing precipitation even after a lapse of time.

Zinc oxide, which is an inorganic type, can be used as an antimicrobial agent. Since zinc oxide has excellent levels of poisons and stars against bacteria, single cell animals such as bacteria, viruses and fungi act on oxygen and special enzymes that digest metabolism and can neutralize them, .

Until recently, a method for dispersing silver nanoparticles as an inorganic antimicrobial agent has been continuously tried, but silver nanoparticles are limited to actual products due to their inherent risks and lack of economical efficiency. On the other hand, zinc oxide has been extensively used as an ultraviolet ray blocking agent due to its excellent ultraviolet shielding effect, and it has been widely applied to cosmetics, vitamin preparations and the like due to its low environmental risk and excellent human suitability. Therefore, zinc oxide can be applied as an antimicrobial agent that can replace silver nanoparticles.

The antimicrobial effect of zinc oxide is based not on the sterilization effect by the photocatalytic activity, but on the mechanism of eliminating it by inhibiting the metabolism of viruses and bacteria. Because of the large specific surface area of nano-sized zinc oxide, it can exhibit surface effects not provided by bulk materials. Especially, when it comes into contact with moisture in the air, the zinc metal component of zinc oxide ionizes and can act as an antimicrobial against harmful bacteria such as bacteria.

As the zinc oxide, a powder composed of secondary particles in which primary particles are aggregated can be used. By using zinc oxide having such a structure, the surface effect of zinc oxide can be maximized.

The dispersibility and workability can be improved by controlling the size of primary particles and secondary particles of zinc oxide through milling or the like. The average particle diameter of the zinc oxide primary particles before milling may be 10 nm to 50 nm. These primary particles aggregate with each other to form secondary particles, and the average particle diameter of the zinc oxide secondary particles may be 1 탆 to 15 탆. The surface effect of zinc oxide can be maximized when the size of the secondary particles is close to the size of the primary particles. After milling, the average particle size of the secondary particles of zinc oxide may be between 300 nm and 1 um.

The average particle diameter means a cumulative average particle diameter (D50) corresponding to 50% by volume in the cumulative distribution curve of the particle size at 100% of the total volume. The average particle diameter D50 can be measured by methods well known to those skilled in the art. For example, D50 may be measured from a particle size analyzer, TEM or SEM photograph. In addition, the data is analyzed using a dynamic light-scattering measuring device, and the number of particles is counted for each size range, and the average particle size D50 can be easily obtained through calculation from this .

The milling process can be wet milling or dry milling. For example, when a zinc oxide slurry is used, wet milling such as a beads mill, a planetary mill, a stirred ball mill, or a vibration mill may be used. When zinc oxide powder is used, particle size can be controlled by milling the aggregated zinc oxide particles using dry milling, especially a jet mill. If the machining energy is excessively applied in the milling process, the bonding force between the particles becomes too strong, which makes it difficult to disperse the particles. Care should be taken not to cause such problems.

Citric acid refers to tricarboxylic acid (C ₃ H ₄ (OH) (COOH) ₃ ) with one OH group. It is also called citric acid. The chemical structure is shown below. Particularly, in the present invention, an antimicrobial composition harmless to the human body can be produced by using the edible citric acid.

≪ Formula 1 >

Sodium citrate is widely used as a food additive, including the following three types: monosodium citrate, disodium citrate, and trisodium citrate.

When only the citric acid solution was added to the zinc oxide slurry, precipitation occurred and it was difficult to apply it to the wet tissue. The addition of sodium citrate further prevented the occurrence of precipitation, and precipitation occurred over time A transparent zinc oxide dispersion excellent in stability can be obtained.

(2)

(3)

≪ Formula 4 >

In 100 parts by weight of the total composition, zinc oxide may be 0.1 to 5 parts by weight, citric acid may be 0.1 to 5 parts by weight, sodium citrate may be 0.1 to 5 parts by weight, and the balance may be purified water. When the content of each component is within the above range, the dispersion stability is excellent and no precipitation occurs.

The antimicrobial composition of this aspect does not contain any organic compounds and is harmless to the human body. In particular, the above-mentioned ingredients can support the harmlessness of humans in that the substances are proved to be harmless to humans which are widely used for edible or cosmetics.

(B) adding a citric acid to the slurry and stirring the slurry; (c) mixing the slurry with the slurry; and Adding sodium citrate and stirring, and (d) stabilizing the slurry.

First, the particle size of the zinc oxide can be controlled by wet milling a zinc oxide slurry having a solid content of 20%. As the wet milling, a bead mill or a Rotate mill may be used. The particle size of the wet milled zinc oxide may be such that the average particle size of the primary particles is 10 nm to 50 nm and the average particle size of the secondary particles is 1 μm to 15 μm. The average particle size of the secondary particles of zinc oxide after wet milling may be 300 nm to 1 um.

Next, after adding the citric acid and stirring, sodium citrate can be added and stirred. When only citric acid is injected, precipitation may occur. By injecting sodium citrate, a transparent solution in which zinc oxide is completely dispersed can be produced.

Next, the thus prepared transparent solution is subjected to a stabilization process. The stabilization step is preferably carried out at room temperature for 1 hour or more. If it is shorter than 1 hour, stabilization of the solution may be insufficient and subsequent precipitation may occur. However, productivity may be a problem if it is too long. Therefore, the upper limit can be determined considering this point. Through this process, the solution is stabilized, and precipitation does not occur even after a lapse of time.

In 100 parts by weight of the finally obtained transparent solution composition, zinc oxide may be 0.1 to 5 parts by weight, citric acid may be 0.1 to 5 parts by weight, sodium citrate may be 0.1 to 5 parts by weight, and the balance may be purified water. Within this range, the composition does not undergo precipitation and can exhibit excellent antibacterial activity.

A third aspect of the present invention is a method for preparing a zinc oxide slurry, comprising the steps of: (a) adjusting the particle size of zinc oxide through a milling process of zinc oxide powder; (b) (c) adding the citric acid to the slurry and stirring the slurry, (d) adding and stirring the slurry to the sodium citrate, and (e) stabilizing the slurry. have.

This aspect is a case where zinc oxide powder is used as a starting material, and the steps (a) and (b) are different from each other in the second side name, and the remaining steps are the same.

In step (a) of this aspect, the particle size of the zinc oxide can be adjusted by dry milling the zinc oxide powder. Specifically, aggregated zinc oxide particles can be crushed and adjusted in size using a jet mill.

In step (b) of this aspect, purified water is added to the zinc oxide powder having a controlled particle size, and then stirred for about 30 minutes to prepare a zinc oxide slurry.

Subsequently, the matters relating to the introduction of the citric acid and sodium citrate, the stabilization process, and the like are the same as in the second aspect.

A fourth aspect of the present invention may be an antimicrobial wet tissue including zinc oxide, citric acid, and sodium citrate.

The wet tissue may be packed in a sealed state, for example, in a wrapping paper of a synthetic resin material in a state of containing a raw liquid after cutting a tentaceous material or fibers having no skin irritation in a usual manner to a predetermined size.

In this aspect, nonwoven fabric can be used as a tissue fabric. The nonwoven fabric may be produced in the form of a felt by arranging and bonding the fibers in parallel or in a negative direction (indefinite direction). As the raw material fiber of the nonwoven fabric, synthetic fibers such as viscos Rayon, polyester (PE), polypropylene (PP), cotton, or natural pulp can be used.

The nonwoven fabric cut to a predetermined size is impregnated with the antimicrobial transparent solution composition, taken out of the nonwoven fabric, and stored in a closed case to prepare an antimicrobial wet tissue.

The antimicrobial wet tissue according to this aspect is prepared by impregnating an antimicrobial composition containing only zinc oxide, citric acid, sodium citrate, and purified water into a nonwoven fabric, which is harmless to the human body since it contains no organic compound at all. In particular, the above-mentioned ingredients are more preferable in that they are proved to be harmless substances widely used for edible and cosmetics.

The antimicrobial wet tissue according to this aspect contains a composition having excellent antimicrobial properties, and thus has excellent antibacterial properties.

As the zinc oxide, an average particle diameter of primary particles of 10 nm to 50 nm and an average particle diameter of secondary particles of 300 nm to 1 um can be used.

In 100 parts by weight of the total composition, zinc oxide may be 0.1 to 5 parts by weight, citric acid may be 0.1 to 5 parts by weight, sodium citrate may be 0.1 to 5 parts by weight, and the balance may be purified water.

In this aspect, the matters relating to zinc oxide, the sheet rack acid, the sodium citrate, the composition ratio and the like are the same as described above.

Hereinafter, the present invention will be described in detail with reference to examples. However, the scope of the present invention is not limited thereto.

<Examples>

1. Preparation of zinc oxide dispersion (slurry)

The zinc oxide slurry with a solid content of 20% was processed for 4 hours using a rotary mill. The zinc oxide before processing had an average particle size of primary particles of 30 nm and an average particle size of secondary particles of 7 μm. After processing, the size of zinc oxide (average particle diameter of secondary particles) was 500 nm.

2. Preparation of antimicrobial solution

Citric acid and sodium citrate are added to the processed zinc oxide slurry so that the weight ratio of zinc oxide, citric acid, sodium citrate and purified water is 1: 1.5: 1: 96.5. To prepare an antibacterial solution. Specifically, purified water was first added to the zinc oxide slurry and stirred for 10 minutes to uniformly mix. The citric acid was then added and stirred for 10 minutes. Then sodium citrate was added and stirred for 30 minutes. Then, the solution was stabilized at room temperature for 2 hours to prepare an antimicrobial solution.

3. Manufacture of antibacterial wipes

The nonwoven fabric (polyester, rayon) was cut into a size of 200 mm x 150 mm and impregnated with the composition for an antimicrobial wet tissue to prepare an antimicrobial wet tissue.

&Lt; Evaluation of antibacterial activity &

The antibacterial activity of the antimicrobial solution prepared according to the examples was evaluated according to KS J 4206.

Staphylococcus aureus ATCC 6538 (strain 1), Escherichia coli ATCC 25922 (strain 2), and Pseudomonas aeruginosa ATCC 27853 (strain 3) were used as the strains.

The test strain was incubated at 37 ± 1 ° C for 24 hours with shaking culture (120 times / min) and the number of bacteria was measured.

For the test sample, a stock solution was used, and a phosphate buffer solution (pH 7.0 ± 0.2) was used as a neutral solution.

The rate of decrease and the rate of increase were calculated according to the following equations (1) and (2).

Reduction rate (%) = [(Mb - Mc) / Mb] x 100 ------ (1)

Growth rate (F) = Mb / Ma (31.6 times or more) ------- (2)

here,

- Ma: initial number of bacteria (average value) of the control sample,

- Mb: number of bacteria (average value) of the control sample after 24 hours of culture,

- Mc: Bacterium number (average value) of the test sample after 24 hours of incubation.

The antibacterial test results are shown in Tables 1 to 3 below.

Strain 1: Staphylococcus aureus ATCC 6538 Inoculum concentration (CFU / ml) 1.3 x 10 ⁵ Growth rate (F) 45 times Ma 1.3 x 10 ⁵ Mb 5.9 x 10 ⁶ Mc <10 Decrease (%) 99.9

(CFU: Colony Forming Unit, <: less than)

Strain 2: Escherichia coli ATCC 25922 Inoculum concentration (CFU / ml) 1.6 x 10 ⁵ Growth rate (F) 52 times Ma 1.6 x 10 ⁵ Mb 8.3x10 ⁶ Mc <10 Decrease (%) 99.9

(CFU: Colony Forming Unit, <: less than)

Strain 3: Pseudomonas aeruginosa ATCC 27853 Inoculum concentration (CFU / ml) 1.5 x 10 ⁵ Growth rate (F) 51 times Ma 1.5 x 10 ⁵ Mb 7.7 x 10 ⁶ Mc <10 Decrease (%) 99.9

(CFU: Colony Forming Unit, <: less than)

Referring to Tables 1 to 3 and FIGS. 1 to 3, it can be confirmed that the antibacterial solution composition according to the present invention has excellent antimicrobial activity. The antimicrobial composition of the present invention can be applied to an antibacterial wet tissue or the like to realize an antibacterial wet tissue which is harmless to the human body and has excellent antibacterial activity.

The terms used in the present invention are intended to illustrate specific embodiments and are not intended to limit the present invention. The singular presentation should be understood to include plural meanings, unless the context clearly indicates otherwise. The word &quot; comprises &quot; or &quot; having &quot; means that there is a feature, a number, a step, an operation, an element, or a combination thereof described in the specification. The present invention is not limited by the above-described embodiments and the accompanying drawings, but is intended to be limited only by the appended claims. It will be apparent to those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims. something to do.

Claims (10)

Wherein the antimicrobial composition comprises zinc oxide, citric acid, and sodium citrate.
The method according to claim 1,
Wherein the zinc oxide has an average particle diameter of primary particles of 10 nm to 50 nm and an average particle diameter of secondary particles of 300 nm to 1 μm.
The method according to claim 1,
Wherein the zinc oxide is 0.1 to 5 parts by weight, the citric acid is 0.1 to 5 parts by weight, the sodium citrate is 0.1 to 5 parts by weight and the balance is purified water in 100 parts by weight of the total composition .
(a) milling a zinc oxide slurry to adjust the particle size of the zinc oxide;
(b) adding a citric acid to the slurry and stirring the slurry;
(c) adding sodium citrate to the slurry and stirring; And
(d) stabilizing the slurry.
(a) milling a zinc oxide powder to adjust the particle size of the zinc oxide;
(b) adding purified water to the zinc oxide and stirring to produce a zinc oxide slurry;
(c) adding a citric acid to the slurry and stirring the slurry;
(d) adding sodium citrate to the slurry and stirring; And
(e) stabilizing the slurry.
The method according to claim 4 or 5,
(a), the size of the zinc oxide before the milling is such that the average particle size of the primary particles is 10 nm to 50 nm, the average particle size of the secondary particles is 1 μm to 15 μm, Wherein the average particle size of the secondary particles is 300 nm to 1 μm.
The method according to claim 4 or 5,
Wherein the zinc oxide is 0.1 to 5 parts by weight, the citric acid is 0.1 to 5 parts by weight, the sodium citrate is 0.1 to 5 parts by weight and the balance is purified water in 100 parts by weight of the total composition &Lt; / RTI &gt;
An antimicrobial antimicrobial wet tissue characterized by comprising zinc oxide, citric acid and sodium citrate.
9. The method of claim 8,
Wherein the zinc oxide has an average particle diameter of primary particles of 10 nm to 50 nm and an average particle diameter of secondary particles of 300 nm to 1 μm.
9. The method of claim 8,
Wherein the zinc oxide is 0.1 to 5 parts by weight, the citric acid is 0.1 to 5 parts by weight, the sodium citrate is 0.1 to 5 parts by weight and the balance is purified water in 100 parts by weight of the whole composition. .

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