KR20030069502A - Manufacturing of Colloidal Silver in Organic Solvents containing Ethanol - Google Patents
Manufacturing of Colloidal Silver in Organic Solvents containing Ethanol Download PDFInfo
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- KR20030069502A KR20030069502A KR1020020009158A KR20020009158A KR20030069502A KR 20030069502 A KR20030069502 A KR 20030069502A KR 1020020009158 A KR1020020009158 A KR 1020020009158A KR 20020009158 A KR20020009158 A KR 20020009158A KR 20030069502 A KR20030069502 A KR 20030069502A
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Abstract
Description
콜로이드 실버(은, Ag)는 잘 알려진 바와 같이 범용적인 항생재로서 세균을 비롯한 균류 및 바이러스 등에도 탁월한 효과가 있으면서도 부작용은 전혀 없는 것으로 잘 알려져 있다. 특히 은이 극미세의 입자(1-100nm)로 분산되어진 콜로이드 실버 용액의 경우, 은 미립자가 쉽게 세포내로 침투하여 바이러스, 박테리아, 곰팡이, 균류 등이 호흡할 때 필요한 효소의 기능을 정지시켜 질식시킴으로써 이들을 죽게 한다. 이는 은이 병균의 신진대사를 막아 살균함과 더불어 금속의 은이 방출하는 은의 전기적 부하가 병균의 생식 기능을 억제하기 때문이다.Colloidal silver (silver, Ag), as is well known as a general-purpose antibiotic is known to have excellent effects on bacteria, fungi and viruses, but also no side effects. Particularly in the case of colloidal silver solution in which silver is dispersed into very fine particles (1-100 nm), silver fine particles easily penetrate into cells and stop the function of enzymes necessary for viruses, bacteria, fungi, fungi, etc. to breathe and suffocate them. To die. This is because silver prevents germ metabolism and sterilizes, and the electrical load of silver released from silver suppresses germ reproductive function.
일반적으로 콜로이드 실버는 전기분해법, 액상환원법, grinding 등의 방법에 의해 물에 분산되어진 형태로 제조되어진다. 수분산의 경우 기존에는 주로 전기분해법이 많이 사용되었다. 이는 순수한 은을 전기 분해를 통해 증류수의 물에 분산시켜 건강 보조식품으로 음용하거나 화장수 등으로 주로 사용되었으나, 농도가 낮아 공업적으로 이용할 경우에는 고농도의 나노 크기의 은이 분산된 콜로이드 실버가 선호되어 지고 있는 실정이다. 출원번호 99-54938의 특허 '수용액상에서 계면활성물질을 이용한 미세 금속 입자의 제조방법'는 이러한 목적으로 개발되어진 한 예라고 볼 수 있다. 그러나 수분산의 형태로 얻어진 콜로이드 실버는 섬유나 플라스틱 등에 처리할 경우 섬유나 플라스틱의 표면이 친유성을 띠기 때문에 잘 분산이 되지 않아 응용하는데 한계가 있다. 따라서 본 발명에서는 콜로이드 실버의 응용 범위를 확장시키기 위하여 수용액 분산 대신 유기 용매에 분산된 콜로이드 실버를 제조하는 방법을 제시하고 있다. 더불어 공업적인 응용을 위해 고농도(1000 ppm이상)로 안정된 분산과 더불어 입자 크기의 분포가 좁은 콜로이드 실버의 제조에 관한 것이다.In general, colloidal silver is prepared in the form of being dispersed in water by electrolysis, liquid reduction, grinding, or the like. In the case of water dispersion, electrolysis was mainly used. Pure silver was dispersed in distilled water through electrolysis to be used as a health supplement or as a lotion. However, when the concentration is low and industrially used, colloidal silver with high concentration of nano-sized silver is preferred. There is a situation. Patent No. 99-54938 'Method for producing fine metal particles using the surface active material in the aqueous phase' can be seen as an example developed for this purpose. However, the colloidal silver obtained in the form of water dispersion is limited to the application because it is difficult to disperse because the surface of the fiber or plastic is lipophilic when treated to fiber or plastic. Therefore, the present invention proposes a method for preparing colloidal silver dispersed in an organic solvent instead of aqueous solution in order to expand the application range of colloidal silver. In addition, the present invention relates to the production of colloidal silver having a narrow particle size distribution with stable dispersion at high concentration (more than 1000 ppm) for industrial applications.
입자의 활용기술에서 입자의 크기가 미세단위 (300 nm이하)로 작게 되면 입자의 물성 및 성능이 입자 크기가 μm 이상인 경우와는 매우 다르게 된다. 이는 입자의 표면 대 질량의 비율이 증가되어 단위 질량당 표면적이 증가되어 입자의 성능이 향상되고 입자의 융점이 감소되는 등 물성이 변화되며 입자의 색상까지 크기에 따라 변화되는 등 큰 입자의 경우와는 다른 성질을 나타낸다. 특히 입자의 효용면에서 보면 사이즈가 작을수록 그 효과는 더욱 커지게 되는데 기존의 고농도로 제조된 수분산의 콜로이드 실버의 입자 크기에 비해 훨씬 작으면서도 입자 분포가 좁은 유기 용매상에 분산된 콜로이드 실버를 제조함으로써 다방면에 걸쳐 응용이 가능하도록 하는데 본 발명이 일차적으로 지향하는 목표이다.In the particle utilization technology, when the particle size is reduced to fine units (less than 300 nm), the physical properties and performance of the particle are very different from those when the particle size is larger than μm. This is due to the increase in the surface-to-mass ratio of the particles, which increases the surface area per unit mass, which improves the performance of the particles, decreases the melting point of the particles, and changes the properties of the particles. Has different properties. In particular, the smaller the size, the more effective the effect becomes.The colloidal silver dispersed in the organic solvent which is much smaller than the particle size of the colloidal silver of the aqueous dispersion prepared in high concentration but has narrow particle distribution The present invention aims primarily at making it possible to apply a wide range of applications by manufacturing.
따라서 본 발명에서는 상기한 바와 같은 선행 기술의 단점을 감안하여 나노미터 크기의 은미립자가 유기용매상에 분산된 콜로이드 실버를 제조함으로써 고대로부터 알려진 은의 항균 효과를 다방면에 걸쳐 응용 범위를 넓히고자 한다. 은의 항균 효과성은 입자의 사이즈와 밀접한 관련이 있는데 일반적으로는 입자의 사이즈가 감소함에 따라 항균성은 크게 증가하는 것으로 알려져 있다. 또한 은의 함량과 항균성과의 관계는 농도가 증가함에 따라 항균성이 비례적으로 증가하는데, 은은 귀금속 중의 하나로써 비교적 고가이므로 경제성을 갖기 위해서는 소량으로써도 큰 효과를 나타내어야 한다. 따라서 본 발명에서는 다방면에 걸친 응용성의 증가라는 측면과 더불어 5 nm 이하의 은미립자가 분산된 콜로이드 실버를 제조함으로써 그 효과를 극대화시키려는데 주 목적이 있다.Therefore, in the present invention, in consideration of the disadvantages of the prior art as described above, by preparing a colloidal silver in which nanometer-sized silver fine particles are dispersed in an organic solvent, it is intended to broaden the application range of antimicrobial effects of silver known from ancient times. The antimicrobial effectiveness of silver is closely related to the particle size. Generally, it is known that antimicrobial activity greatly increases as the particle size decreases. In addition, the relationship between the silver content and the antimicrobial activity is proportionally increased as the concentration is increased. Silver is one of the precious metals and is relatively expensive, so in order to have economic feasibility, a small amount must be produced. Therefore, in the present invention, the main purpose is to maximize the effect by producing colloidal silver in which silver fine particles of 5 nm or less are dispersed together with the aspect of increasing the applicability over various aspects.
유기 용매에 분산된 실버 콜로이드는 polyol 공정을 사용하면 얻어질 수 있다고 잘 알려져 있다. 이 경우는 질산은 중의 은이온을 안정제가 포함된 에틸렌글리콜 용매하에서 120℃에서 reflux하여 얻어진 은미립자를 원심분리 등을 통해 분리하여 얻은 다음 이를 알코올 용매에 분산시켜 평균 20∼30 nm 분포를 갖는 은미립자가 분산된 콜로이드 실버를 제조한다. 여기에 사용되는 PVP 등의 안정제는 분산의 효과와 더불어 입자 크기를 조절해 주는 역할을 하는 것으로 알려져 있다. 그러나 polyol 공정의 경우 입자의 크기는 15 nm 이하로 작아지기는 힘들며, reflux 하고나서 다시 원심분리하여 건져진 입자를 재분산 시키기 때문에 다소 복잡하다는 단점을 지니고 있다. 따라서 본 발명에서는 보다 간단한 공정으로 수 nm의 보다 작고 균일한 크기를 지닌 실버 콜로이드를 제조하는 방법을 제공하고자 한다.It is well known that silver colloids dispersed in organic solvents can be obtained using the polyol process. In this case, silver fine particles obtained by refluxing silver ions in silver nitrate at 120 ° C. in an ethylene glycol solvent containing a stabilizer were obtained by centrifugation or the like, and then dispersed in an alcohol solvent. Prepare dispersed colloidal silver. Stabilizers such as PVP used here are known to play a role in controlling the particle size as well as the effect of dispersion. However, in the case of the polyol process, it is difficult to reduce the size of the particles to less than 15 nm, and it is somewhat complicated because the particles are redispersed by refluxing and centrifugation again. Therefore, the present invention is to provide a method for producing a silver colloid having a smaller and uniform size of several nm in a simpler process.
도 1은 Ag 100 ppm으로 제조된 콜로이드 실버의 TEM Image.1 is a TEM image of colloidal silver prepared with Ag 100 ppm.
도 2는 Ag 1000 ppm으로 제조된 콜로이드 실버의 TEM Image.2 is a TEM image of colloidal silver prepared with Ag 1000 ppm.
도 3은 Ag 5000 ppm으로 제조된 콜로이드 실버의 TEM Image.3 is a TEM image of colloidal silver prepared with Ag 5000 ppm.
도 4는 Ag 1000 ppm으로 제조된 콜로이드 실버의staphylococcus aureus, Klebsiella pneumoniae에 대한 항균 test 결과Figure 4 shows the antimicrobial test results for staphylococcus aureus, Klebsiella pneumoniae of colloidal silver prepared with Ag 1000 ppm
메탄올, 에탄올, 프로판올 등의 유기 용매에 PVP(polyvinyl pyrrolidone, PVA(polyvinyl alcohol), PMVE(poly methyl vinyl ether)등의 고분자를 녹이고 여기에 분산제인 A60, HIPLUS DS-101(san nopco korea) 등을 추가하여 녹인 혼합액에 실버 아세테이트, 질산등의 은염을 유기용매에 녹인 용액을 추가하여 준 다음 이를 가해준 용매의 끓는점에서 reflux 하여 줌으로써 수 나노 크기로 분산된 실버 콜로이드를 얻을 수 있다. 은 이온은 가해준 고분자에 의해 은 미립자로 환원이 되며 이들 고분자의 입체적 장애로 인해 일정 크기 이상으로 커지지 않게 되며, 또한 가해준 분산제가 은 미립자에 흡착되어 입체 장애 및 전기 반발력을 유발하여 줌으로써 입자들의 재응집을 방지하여 주게 된다. 따라서 나노 미립자로 분산된 실버 콜로이드를 얻을 수 있게 되며, 이 콜로이드는 고분자 및 분산제와의 상호 작용에 의해 안정화되어 실온에서도 6개월 이상 안정한 상태를 유지하게 된다.Dissolve polymers such as PVP (polyvinyl pyrrolidone, PVA (polyvinyl alcohol), PMVE (poly methyl vinyl ether) in organic solvents such as methanol, ethanol and propanol, and dispersants A60, HIPLUS DS-101 (san nopco korea) The silver colloid dispersed in several nano size can be obtained by adding a solution in which silver salts such as silver acetate and nitric acid are dissolved in an organic solvent and refluxing at the boiling point of the solvent. It is reduced to silver fine particles by semi polymer, and it does not grow over a certain size due to steric hindrance of these polymers, and also prevents reaggregation of particles by adsorbing dispersant to silver fine particles, causing steric hindrance and electric repulsion. Therefore, silver colloid dispersed in nano fine particles can be obtained. It is stabilized by interaction with maintains a stable state for more than 6 months at room temperature.
일례로 12.5g의 PVP(MW=40000)와 2.5g의 A60을 에탄올 용매에 넣고 약 50℃로 열을 가하면서 녹여준다. 여기에 0.786g의 실버 아세테이트가 녹은 에탄올 용액을 가하고 이를 질소를 흘려보내면서 약 80℃에서 6시간 reflux하여 주면 2-5nm의 크기를 지닌 은 미립자가 분산된 실버 콜로이드를 얻을 수 있다. 콜로이드 내에 은이온이 존재하면 햇빛등에 의해 반응이 일어나 이미 형성된 은미립자가 커져 안정성이 감소하게 되므로 완전히 환원시켜 주기 위해서는 reflux 시간을 조절해 주거나 하이드라진등의 환원제를 극미량 첨가하여 주면 된다.For example, 12.5 g of PVP (MW = 40000) and 2.5 g of A60 are dissolved in ethanol and heated to about 50 ° C. to melt. 0.786 g of silver ethanol dissolved in ethanol solution was added to this, while flowing nitrogen and refluxing at 80 ° C. for 6 hours to obtain a silver colloid dispersed with silver particles having a size of 2-5 nm. When silver ions are present in the colloid, the reaction is caused by sunlight and the silver particles are formed, which increases the stability. Therefore, the total amount of silver ions can be controlled by adjusting the reflux time or by adding a very small amount of a reducing agent such as hydrazine.
수용액상으로 제조된 실버 콜로이드는 섬유나 플라스틱 등에 분산시킬 경우 많은 문제는 분산에 관한 것이다. 즉, 서로 잘 분산이 되지 않기 때문에 은입자들끼리 뭉치게 되므로 전체적으로 불균일하게 되며, 더불어 은의 효과가 반감하게 되는 단점이 있다. 본 발명의 효과로는 각종 균류, 바이러스, 곰팡이 등 거의 모든 병원균에 대해 항균성을 지닌 것으로 알려진 실버콜로이드를 유기 용매에 분산된 형태로 제조하여 기존의 수용액상으로 제조된 실버 콜로이드를 적용하는 데 한계가 있었던 섬유나 플라스틱 등에 적용하여 섬유나 플라스틱 등에 항균 효과를 부여하고자 한다. 또한 수용액상으로 제조되는 콜로이드 실버에 비해 입자 사이즈가 작아 보다 적은 양으로 효과를 극대화시킬 수 있으며, 안정성이 뛰어나 6개월 이상 유지되므로 수용액상의 콜로이드 실버가 가졌던 부분적인 적용한계를 보충해 줄 수 있다는 장점을 지니고 있다.Silver colloids prepared in aqueous solution have many problems when dispersed in fibers or plastics. In other words, since they are not dispersed well with each other, the silver particles are bundled together, resulting in an overall nonuniformity, and a silver effect is halved. The effect of the present invention is to produce a silver colloid known to have an antimicrobial against almost all pathogens such as various fungi, viruses, fungi in a dispersed form in an organic solvent has a limit in applying the silver colloid prepared in the conventional aqueous solution It is intended to give antimicrobial effect to fibers or plastics by applying them to fibers or plastics. In addition, the particle size is smaller than the colloidal silver prepared in the aqueous solution to maximize the effect in a smaller amount, and the stability is excellent for more than six months, so it can supplement the partial application limit of the colloidal silver in the aqueous solution It has
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| KR100479847B1 (en) * | 2002-04-16 | 2005-03-30 | 학교법인 포항공과대학교 | Stable metal colloids with uniform shape and narrow size distribution and a method for preparation thereof |
| KR100838254B1 (en) * | 2008-01-03 | 2008-06-17 | 주식회사 신일 | Silver colloid and producing method thereof |
| CN115777725A (en) * | 2022-12-02 | 2023-03-14 | 山西益鑫泰生物科技有限公司 | Nano-silver disinfectant and preparation method thereof |
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| KR101659449B1 (en) | 2014-12-03 | 2016-09-26 | 서강대학교산학협력단 | Preparation method for silver colloid |
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| US5073303A (en) * | 1988-06-20 | 1991-12-17 | Bsg, Inc. | Photochromic emulsion |
| EP0517961B1 (en) * | 1991-06-11 | 1998-03-25 | Agfa-Gevaert N.V. | Method of preparing light-sensitive silver halide emulsions |
| US5750411A (en) * | 1996-06-03 | 1998-05-12 | Bayer Corporation | Sol particle decay protection immunoassay |
| JPH10110123A (en) * | 1996-10-08 | 1998-04-28 | Sumitomo Osaka Cement Co Ltd | Coating material for forming transparent conductive membrane and its production, transparent conductive low reflective membrane and its production, and display with the transparent conductive low reflective membrane |
| KR100375525B1 (en) * | 1999-12-03 | 2003-03-10 | 오성근 | Method for Manufacturing of Metallic Nanoparticles in Surfactant Solutions and Method to use the same |
| KR20010069645A (en) * | 2001-04-24 | 2001-07-25 | 오성근 | Sterilization of water using the particles coated with silver |
| KR100425976B1 (en) * | 2001-04-30 | 2004-04-06 | 주식회사 화진 | Preparation Method of the Silver Colloids with Nanometer Size Irradiated by Radiation and Its Silver Colloid with Nanometer Size |
| KR20020008375A (en) * | 2001-10-31 | 2002-01-30 | 김우협 | Spray containing Colloidal Silver as Antiseptic |
-
2002
- 2002-02-20 KR KR10-2002-0009158A patent/KR100477912B1/en not_active IP Right Cessation
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100479847B1 (en) * | 2002-04-16 | 2005-03-30 | 학교법인 포항공과대학교 | Stable metal colloids with uniform shape and narrow size distribution and a method for preparation thereof |
| KR100838254B1 (en) * | 2008-01-03 | 2008-06-17 | 주식회사 신일 | Silver colloid and producing method thereof |
| CN115777725A (en) * | 2022-12-02 | 2023-03-14 | 山西益鑫泰生物科技有限公司 | Nano-silver disinfectant and preparation method thereof |
| CN115777725B (en) * | 2022-12-02 | 2024-01-26 | 山西益鑫泰生物科技有限公司 | Nano silver disinfectant and preparation method thereof |
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| KR100477912B1 (en) | 2005-03-17 |
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