KR20230051863A - a functional antibiotic powder and the functional antibiotic powder production method - Google Patents

Abstract

The present invention relates to an antibacterial powder, in particular, a silver-glass system formed by pulverizing an ingot produced by heating raw materials including silver nitrate (AgNO ₃ ) reacted with sodium hydroxide as a raw material to synthesize Ag ₂ O The invention relates to an antibacterial inorganic powder.
The present invention is phosphorus oxide (P2O5), sodium oxide (Na2O), magnesium oxide (MgO), aluminum oxide (Al2O3), silicon oxide (SiO2), sulfur oxide (SO3), calcium oxide (CaO), titanium oxide (TiO2) , iron oxide (Fe2O3), cobalt oxide (Co3O4), nickel oxide (NiO), copper oxide (CuO), silver oxide (Ag2O), tungsten oxide (WO3), and chlorine (Cl).
It also provides an antibacterial powder configured to further include potassium oxide (K O) in the above configuration.
In addition, the present invention is a process of preparing a glass ingot by mixing the raw materials included in the antibacterial powder and heating to about 1000 to 1100 degrees Celsius (step 1),
It provides a method for producing an antibacterial powder comprising a process (step 2) of preparing an antibacterial powder by pulverizing the manufactured glass ingot.

Description

Functional antibiotic powder and method for producing the same {a functional antibiotic powder and the functional antibiotic powder production method}

The present invention relates to an antibacterial powder, in particular, a silver-glass system formed by pulverizing an ingot produced by heating raw materials including silver nitrate (AgNO ₃ ) reacted with sodium hydroxide as a raw material to synthesize Ag ₂ O The invention relates to an antibacterial inorganic powder.

Antibacterial means inhibiting or preventing the propagation of microorganisms, and a substance having such an effect is called an antibacterial substance or an antibacterial agent. In addition, sterilization (sterilization) means to fundamentally kill microorganisms. Bactericides show excellent activity in removing all propagated microorganisms, but the effect is not sustained, whereas antibacterial substances are known to exhibit relatively persistent effects. Therefore, products containing antibacterial agents as additives can be expected to have an effect of preventing diseases caused by microbial infection by preventing the propagation of microorganisms.

Antibacterial agents added to prevent bacterial growth can be largely classified into organic (including organometallic) and inorganic.

The organic antibacterial agent mainly uses the effect of the dissolution of the drug, and acts close to antibacterial to prevent the formation of bacterial colonies rather than sterilization. The biggest advantage of using an organic antibacterial agent is that it is rapidly exposed to the surface of an object to be sterilized, thereby immediately preventing the propagation of bacteria, and has the advantage of being relatively inexpensive. On the other hand, the durability of the product is weak due to the rapid elution caused by the rapid migration of the organic antimicrobial agent, and when high temperature work is required during the manufacturing process, it is impossible to apply due to the thermal decomposition of the organic antimicrobial agent, and it is harmful to the human body and the environment. etc., and in particular, there is a disadvantage that it cannot be used where toxicity problems are raised due to the fluidity and solubility of organic matter.

Inorganic antimicrobials are products made by substituting silver, zinc, copper, etc., which are metal ions that have an antibacterial effect on inorganic substances such as zeolite, calcium phosphate, zirconium phosphate, and silica gel, and are currently used in various fields such as most plastic products, paper, and textiles. It is becoming. Inorganic antibacterial agents have lower temporary antibacterial activity than organic antimicrobial agents, but have high human safety, do not show resistant bacteria, and have almost semi-permanent antibacterial duration, so the use area is expanding. Currently, these inorganic antimicrobial agents are mainly commercially available in the form of zeolite-based, calcium phosphate-based, and zirconium phosphate-based, among which zeolite-based inorganic antimicrobial agents have the highest market share. Compared to zeolite-based inorganic antimicrobial agents, calcium phosphate-based inorganic antimicrobial agents have the disadvantage of having lower antibacterial activity than zeolite-based inorganic antimicrobial agents because the concentration of metal ions to be substituted is lower than that of zeolite-based inorganic antimicrobial agents. has a high disadvantage.

In this way, zeolite-based inorganic antimicrobial agents have several advantages, such as no discoloration problem, high antibacterial activity, and low particle hardness, compared to other antimicrobial agents. It is difficult to evaluate that it provides superior antibacterial power because it has a very high probability of contaminating the water quality environment by metal ions that provide antibacterial activity as it is eluted by The situation is.

In this way, in order to overcome the disadvantages of the conventional inorganic antibacterial agent, an inorganic antimicrobial agent having a high substitution rate with metal ions and not eluted in water under water conditions can provide high antibacterial activity while minimizing economic feasibility and environmental pollution. A lot of research is going on to develop it.

In general, it is known that metal ions such as silver ions, copper ions, and zinc ions have strong antibacterial properties. Based on this, in recent years, these antibacterial metal ions have been developed using ion exchange inorganic materials such as zeolite, which is an aluminum silicate crystal, and zirconium phosphate (US Patent 4911898, 5900258, Japanese Patent Laid-open Publication No. 60-181002, Japanese Patent Laid-open Publication No. 3-83905 ), porous silica gel (Japanese Patent Laid-Open No. 8-183113), etc., it is safe and has been developed as an antibacterial inorganic material that can be used for a wide range of applications such as paints, synthetic fibers, and wallpaper.

In the case of antibacterial inorganic materials carrying silver ions, they are affected by sunlight, heat, pressure, chemicals, etc. during various processing or final use, and when they are affected, they have antibacterial action, discoloration in appearance, or mechanical Strength and the like may be reduced.

For example, when mixed with an antimicrobial inorganic resin containing silver ions and used as an antimicrobial resin composition, it is known that the antimicrobial resin composition is discolored over time due to ultraviolet rays such as sunlight, thereby reducing product value. This is caused by discoloration in the process of converting antimicrobial metal ions slowly released from the antimicrobial resin composition into metal particles by receiving ultraviolet rays.

In order to solve this problem, Japanese Patent Application Publication No. 63-265809 proposes an antibacterial zeolite in which antibacterial silver ions and ammonium ions are supported at the same time. It is claimed that the ammonium ion has the effect of preventing discoloration by suppressing the elution of antibacterial silver (Ag) ion.

In addition, as a prior art, a Japanese patent (No. 6009404, antibacterial glass and antibacterial glass manufacturing method) is provided.

In addition, Korean Patent Publication No. 1996-0029493 discloses an insoluble silver phosphate inorganic in which a support is prepared and silver ions are supported at the same time by sequentially adding and mixing phosphoric acid, silver nitrate aqueous solution, titanium dioxide, and colloidal silica solution. A method for preparing an antibacterial agent is proposed. This makes it easy to control the content of silver ions and stably and continuously provides bactericidal and antibacterial properties by simultaneously preparing the carrier and supporting silver ions, but since silver (Ag) included as an inorganic antibacterial agent is very expensive There is a disadvantage that it is difficult to apply to various fields for providing antibacterial activity according to the method.

In addition, Korean Patent Registration No. 10-1336822 (Method for Producing Inorganic Antimicrobial Agent) describes "dissolving aluminum sulfate in water to prepare an aluminum sulfate solution; preparing a slurry by mixing a calcium salt with water; the aluminum sulfate preparing a mixed solution by mixing the solution and the slurry so that the molar ratio of aluminum sulfate and calcium salt is 1:4 to 8; and adsorbing or substituting one or more antimicrobial metal ions selected from among nickel, cobalt, zinc, chromium, cadmium, lead, mercury, arsenic and copper to the calcium aluminum sulfate. there is.

In the case of the inorganic antibacterial agent of the prior art and the prior art, there was a problem that the elution efficiency of silver was lowered and the antibacterial ability was lowered,

An object of the present invention is to provide a functional antibacterial powder having remarkably high antibacterial efficiency and a method for manufacturing the same, since the elution efficiency of the silver component is significantly increased, and the elution effect of CaO, P2O5, SiO2 or/and K2O is high.

In order to solve the above problems and needs, the present invention

Phosphorus oxide (P2O5), sodium oxide (Na2O), magnesium oxide (MgO), aluminum oxide (Al2O3), silicon oxide (SiO2), sulfur oxide (SO3), calcium oxide (CaO), titanium oxide (TiO2), iron oxide ( Fe2O3), cobalt oxide (Co3O4), nickel oxide (NiO), copper oxide (CuO), silver oxide (Ag2O), tungsten oxide (WO3), and chlorine (Cl).

It also provides an antibacterial powder configured to further include potassium oxide (K O) in the above configuration.

In addition, the present invention is a process of preparing a glass ingot by mixing the raw materials included in the antibacterial powder and heating to about 1000 to 1100 degrees Celsius (step 1),

It provides a method for producing an antibacterial powder comprising a process (step 2) of preparing an antibacterial powder by pulverizing the manufactured glass ingot.

The functional antibacterial powder according to the present invention has a remarkably high elution of the silver component, resulting in a remarkably high antibacterial efficiency.

In addition, the functional antibacterial powder according to the present invention has the effect of eluting CaO, P2O5, SiO2 or / and K2O components, so that these components significantly increase the antibacterial efficiency.

1 is a photograph of a functional antibacterial powder according to the present invention.
Figure 2 is a photograph of a functional antibacterial powder according to another embodiment of the present invention.
Figure 3 is an antibacterial test result of the functional antibacterial powder according to the present invention.
Figure 4 is a sample picture for the antibacterial test of the functional antibacterial powder according to the present invention.
Figure 5 is a particle size distribution of the functional antibacterial powder according to the present invention.
Figure 6 is a masterbatch implementation containing the antibacterial powder of the present invention.
Figure 7 is a manufacturing process diagram of a functional antibacterial powder according to the present invention.

Hereinafter, the present invention will be described in detail with reference to the drawings.

The present invention is phosphorus oxide (P2O5), sodium oxide (Na2O), magnesium oxide (MgO), aluminum oxide (Al2O3), silicon oxide (SiO2), sulfur oxide (SO3), calcium oxide (CaO), titanium oxide (TiO2) , iron oxide (Fe2O3), cobalt oxide (Co3O4), nickel oxide (NiO), copper oxide (CuO), silver oxide (Ag2O), tungsten oxide (WO3), and chlorine (Cl).

The present invention preferably contains 100 parts by weight of phosphorus oxide (P2O5), 0.03 to 0.1 parts by weight of sodium oxide (Na2O), 30 to 60 parts by weight of magnesium oxide (MgO), 10 to 20 parts by weight of aluminum oxide (Al2O3), and silicon oxide. (SiO2) 0.1 to 0.5 parts by weight, sulfur oxide (SO3) 0.01 to 0.05 parts by weight, calcium oxide (CaO) 0.1 to 0.5 parts by weight, titanium oxide (TiO2) 0.005 to 0.02 parts by weight, iron oxide (Fe2O3) 0.01 to 0.05 parts by weight part, cobalt oxide (Co3O4) 0.005 to 0.02 parts by weight, nickel oxide (NiO) 0.0001 to 0.003 parts by weight, copper oxide (CuO) 0.005 to 0.02 parts by weight, silver oxide (Ag2O) 5 to 10 parts by weight, tungsten oxide (WO3) Provides an antibacterial powder comprising 0.03 to 0.09 parts by weight and 0.02 to 0.09 parts by weight of chlorine (Cl).

The present invention provides an antibacterial powder configured to further include potassium oxide (K O) to the above configuration.

It is effective to include 5 to 10 parts by weight of potassium oxide (K2O) based on 100 parts by weight of phosphorus oxide (P2O5).

In addition, the present invention provides a method for producing an antibacterial powder consisting of the above configuration.

The present invention performs a process of manufacturing a glass ingot by mixing the raw materials composed of the above weight parts and heating them at about 1000 to 1100 degrees Celsius. (Step 1)

The present invention is formulated by mixing raw materials composed of parts by weight as described above.

The present invention is characterized in that phosphorus oxide (P2O5) is introduced using phosphoric acid (H3PO4) as a raw material, and the inclusion of the phosphorus oxide (P2O5) has the characteristic of making the elution of the silver component more effective.

In addition, the silver oxide (Ag2O) of the present invention is characterized in that a synthesized product by reacting silver nitrate (AgNO ₃ ) with sodium hydroxide (NaOH) is added as follows, and silver oxide is mixed with other components to form a glass ingot. Since the (Ag) component is appropriately combined with other components, it performs a function of allowing the silver component to be eluted at a constant rate, thereby performing a function of performing a continuous antibacterial action.

[2AgNO ₃ + 2NaOH = Ag ₂ O + 2Na ₂ NO ₃ + H ₂ O]

Calcium carbonate (CaCO3) is used as a raw material for the calcium oxide (CaO).

It is effective to use Al(OH)3 as a raw material for the aluminum oxide (Al2O3).

It is preferable to use potassium carbonate (K2CO3) as the potassium oxide (K2O).

For other components, it is preferable to use the component itself or a material containing the component.

In the present invention, a process of preparing an antibacterial powder is performed by pulverizing the glass ingot prepared above. (Step 2)

As shown in FIG. 1, the antibacterial powder prepared by grinding the glass ingot prepared at the above composition ratio of the present invention corresponds to Silver-Glass antibacterial inorganic powder (powder).

It is effective to grind the antibacterial powder of the present invention to a size of 0.1 to 100 μm in diameter.

Preferably, it is more effective to grind to a size of 1 to 40 μm.

In the present invention, the antibacterial powder composed of the above manufacturing method and configuration exhibits a remarkably high antibacterial efficiency due to the high effect of elution of Ag2O, CaO, P2O5, and SiO2.

In the present invention, a process for preparing a masterbatch including the above antibacterial powder may be performed.

As shown in Figure 6, the present invention can provide a masterbatch containing the antibacterial powder of the present invention.

The present invention shows the results of silver elution and antibacterial experiments through the following examples.

<Example>

1. Manufacturing of functional antibacterial powder 1 (Mg-Al-P-Ag composition)

(1) Phosphorus oxide (P2O5) 1000g, sodium oxide (Na2O) 0.5g, magnesium oxide (MgO) 500g, aluminum oxide (Al2O3) 150g, silicon oxide (SiO2) 4g, sulfur oxide (SO3) 0.2g, calcium oxide ( CaO) 3g, titanium oxide (TiO2) 0.1g, iron oxide (Fe2O3) 0.4g, cobalt oxide (Co3O4) 0.1g, nickel oxide (NiO) 0.01g, copper oxide (CuO) 0.1g, silver oxide (Ag2O) 75g, oxide 0.7 g of tungsten (WO3) and 0.7 g of chlorine (Cl) are mixed and heated at 1000 degrees Celsius to prepare a glass ingot.

Phosphoric acid (H3PO4) is used as a raw material for the phosphorus oxide (P2O5),

Calcium carbonate (CaCO3) is used as a raw material for the calcium oxide (CaO),

Al(OH)3 is used as a raw material for the aluminum oxide (Al2O3),

It is added in an equivalent ratio so that the mass of the above-mentioned raw materials comes out.

(That is, 1000 g of phosphorus oxide (P2O5) is required, phosphorus oxide mass is 142, phosphoric acid mass is 98,

Since phosphorus oxide (P2O5) : phosphoric acid (2(H3PO4)) = 142 : 98 × 2,

[(98 × 2 × 1000)/142] = 1380 g of phosphoric acid (H3PO4) is added to 1000 g of phosphorus oxide (P2O5).

For 3 g of calcium oxide (CaO),

Since calcium oxide (CaO) : calcium carbonate (CaCO3) = 56 : 100,

[(3×100)/56] = 5.36 g of calcium carbonate (CaCO3) was added,

For 150 g of aluminum oxide (Al2O3),

Since aluminum oxide (Al2O3) : 2(Al(OH)3) = 102 : 2 × 78,

(For Al(OH)3, add [(150 × 2 × 78)/102] = 230g.

(2) As shown in Figure 1, the prepared glass ingot is pulverized to 15 ~ 25μm to prepare a functional antibacterial powder. (First functional antibacterial powder, PW 1)

2. Manufacturing of functional antibacterial powder 2 (composition containing K2O)

(1) Phosphorus oxide (P2O5) 1000g, sodium oxide (Na2O) 0.5g, magnesium oxide (MgO) 500g, aluminum oxide (Al2O3) 150g, silicon oxide (SiO2) 4g, sulfur oxide (SO3) 0.2g, calcium oxide ( CaO) 3g, titanium oxide (TiO2) 0.1g, iron oxide (Fe2O3) 0.4g, cobalt oxide (Co3O4) 0.1g, nickel oxide (NiO) 0.01g, copper oxide (CuO) 0.1g, silver oxide (Ag2O) 75g, oxide 0.7 g of tungsten (WO3), 0.7 g of chlorine (Cl), and 50 g of K2O are mixed and heated to 1000 degrees Celsius to prepare a glass ingot.

The above-mentioned potassium oxide (K2O) is added using potassium carbonate (K2CO3), but as described above, it is added in a sugar ratio so that the mass of the above-mentioned raw material comes out.

(That is, 50 g of potassium oxide (K O) is required, potassium oxide mass 94, potassium carbonate mass 138,

Since K2O : K2CO3 = 94 : 138,

For 50 g of potassium oxide (K2O), potassium carbonate (K2CO3) is added [(50×138)/94] = 73.4 g)

(2) The prepared glass ingot is pulverized to 15 ~ 25 μm to prepare a functional antibacterial powder. (First functional antibacterial powder, PW 2)

3. Experimental results

(1) To analyze the characteristics of the manufactured powder, particle size analysis and Ag elution test analysis were performed, and after making a 5% PP master batch of antibacterial glass powder, a plastic specimen for antibacterial test of 0.5% was prepared and tested for antibacterial activity according to the JIS2801 test method. (See Figure 6)

(2) Silver dissolution test

After mixing 5 g of the prepared powder in 100 ml of ultrapure water, stirring for 10 minutes, and leaving it for 24 hours, 48 hours, and 72 hours, the supernatant was collected and the Ag content was analyzed by ICP.

As shown in [Table 1], it can be seen that a certain amount of Ag is increased and eluted with time, and that it is continuously eluted, and the antibacterial effect is remarkably high.

sample PW 1 PW2 24hrs 0.59 ppm 0.56 ppm 48hrs 1.69 ppm 1.59 ppm 72hrs 2.86 ppm 2.53 ppm

(3) Antibacterial activity test

As a result of testing the antibacterial power against Escherichia coli and Staphylococcus aureus with the above-mentioned Example PW1, Escherichia coli showed sterilization power of 99.9% or more, and Staphylococcus aureus showed sterilization power of 99.5% or more, the antibacterial powder of the present invention. It can be seen that the antibacterial activity is remarkably high. (See FIGS. 3 and 4)

(4) Particle size analysis

As a result of particle size analysis with the above example PW1, it can be seen that the average particle diameter (D50) is 15 μm and has significantly higher antibacterial activity compared to the specific surface area. (See FIG. 5)

The present invention provides a functional antibacterial powder consisting of the above configuration and function and a method for producing the same.

The present invention is useful for industries producing, manufacturing, selling, distributing, and researching inorganic antibacterial agents.

In particular, the present invention is very useful for industries producing, manufacturing, selling, distributing, and researching functional antibacterial powders.

Claims (3)

Phosphorus oxide (P2O5), sodium oxide (Na2O), magnesium oxide (MgO), aluminum oxide (Al2O3), silicon oxide (SiO2), sulfur oxide (SO3), calcium oxide (CaO), titanium oxide (TiO2), iron oxide ( Fe2O3), cobalt oxide (Co3O4), nickel oxide (NiO), copper oxide (CuO), silver oxide (Ag2O), tungsten oxide (WO3), and chlorine (Cl).
According to claim 1,
An antibacterial powder that further contains potassium oxide (K2O).
The process of manufacturing a glass ingot by mixing the raw materials of claim 1 or 2 and heating them to about 1000 to 1100 degrees Celsius (Step 1);
A method for producing an antibacterial powder comprising a process (step 2) of preparing an antibacterial powder by pulverizing the manufactured glass ingot.

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