KR20070069269A - Method for preparing hydrophilic gold particle - Google Patents
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- KR20070069269A KR20070069269A KR1020050131164A KR20050131164A KR20070069269A KR 20070069269 A KR20070069269 A KR 20070069269A KR 1020050131164 A KR1020050131164 A KR 1020050131164A KR 20050131164 A KR20050131164 A KR 20050131164A KR 20070069269 A KR20070069269 A KR 20070069269A
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
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Abstract
Description
도 1은 티올기로 치환된 폴리에틸렌글리콜 수용액에 금박을 첨가하여 제조된 친수성 금 입자를 나타낸 사진이다.1 is a photograph showing hydrophilic gold particles prepared by adding gold leaf to a polyethylene glycol aqueous solution substituted with a thiol group.
도 2는 아민기로 치환된 폴리에틸렌글리콜 수용액에 금박을 첨가하여 제조된 친수성 금 입자를 나타낸 사진이다.2 is a photograph showing hydrophilic gold particles prepared by adding gold leaf to an aqueous polyethylene glycol solution substituted with an amine group.
본 발명은 친수성 금 입자의 제조방법에 관한 것으로, 더욱 자세하게는, (a) 폴리에틸렌글리콜 말단을 금과 친화력을 가지는 작용기로 치환하는 단계; 및 (b) 상기 치환된 폴리에틸렌글리콜 수용액에 금입자를 첨가하여 반응시키는 단계를 포함하는 친수성 금입자의 제조방법 및 상기 방법에 의해 제조된 친수성 금 입자를 유효성분으로 함유하는 금 코팅제에 관한 것이다.The present invention relates to a method for producing hydrophilic gold particles, and more particularly, (a) replacing the polyethylene glycol terminal with a functional group having affinity with gold; And (b) relates to a method for producing hydrophilic gold particles comprising the step of reacting by adding gold particles to the aqueous solution of polyethylene glycol substituted and a gold coating agent containing the hydrophilic gold particles prepared by the method as an active ingredient.
금은 그 굳기가 2.5∼3으로, 전성(展性) 및 연성(延性)이 매우 크다. 보통, 순금 또는 금 8, 은 2의 비율의 합금을 두드려 아주 얇게 만드는 금박(金箔)의 두께는 0.00001cm이고, 1g의 금으로는 약 3,000m의 금실을 뽑을 수 있다. 순금의 빛깔은 그 상태에 따라 다르며, 괴상(塊狀)의 것은 황색이지만, 분말이나 콜로이드로 되면 보라색이 되고, 녹으면 녹색, 증착막(蒸着膜)을 형성하면 적색이 된다. 얇은 박(箔)이 되면 투과광선에 의해서 녹색에서 청색이 된다. 전기 및 열의 양도체이며, 전기전도도는 은의 67%이고, 비저항은 2.2×10-6Ω·cm(18 ℃)이다. 열전도율은 0.708cal/cm·sec·deg로 은의 70%이다. Gold has a hardness of 2.5 to 3, and is very malleable and ductile. Usually, the thickness of the gold foil or the gold foil that makes the alloy thin in the ratio of gold 8 and silver 2 is very thin. The thickness of the gold leaf is 0.00001 cm, and about 3,000 m of gold thread can be drawn with 1 g of gold. The color of pure gold varies depending on its state, and the mass is yellow, but when it becomes powder or colloid, it becomes purple, when it melts, it becomes green, and when a vapor deposition film is formed, it turns red. When it becomes thin foil, it becomes green to blue by transmitted light. It is a good conductor of electricity and heat, the electrical conductivity is 67% of silver, and the specific resistance is 2.2 x 10 < -6 > The thermal conductivity is 0.708 cal / cmsec deg, which is 70% of silver.
또한, 공기나 물에서는 변하지 않으며, 빛깔의 변화도 없고, 강한 산화제에 의해서도 변하지 않는다. 산 및 염기에도 녹지 않지만, 왕수(王水)에는 녹아서 염화금산이 된다. 산소가 존재할 때에는 시안화알칼리염의 수용액에서 시아노금산염을 만들며 녹는다. 산소 및 황과는 고온에서도 반응하지 않지만, 염소 및 브롬과는 직접 결합한다. 화합물에서 보통 산화수는 1가(價)와 3가이다.In addition, it does not change in air or water, does not change color, and does not change even by a strong oxidizing agent. It is insoluble in acids and bases, but it dissolves in aqua regia to form geum chloride. When oxygen is present, it dissolves in the aqueous solution of alkali cyanide salt, making cyanoacetate. Oxygen and sulfur do not react even at high temperatures, but bond directly with chlorine and bromine. In the compounds, the oxidation number is usually monovalent or trivalent.
일반적으로 금은 고가이고 생산량이 적어 예전에는 주로 반지, 목걸이, 귀걸이 또는 브로치 등 소정의 형상을 갖는 특정의 장식물로 사용하거나 경제적 부의 축적 수단으로 이용되는 경우가 대부분이었다. 그러나 최근에는 상기와 같은 물리화학적 성질을 때문에, 반도체 등과 같은 전기전자 분야 등 다양한 분야에서 금이직접 사용되는 것은 물론이고, 제품의 외부를 코팅하는 것으로 사용되는 경우가 증가하고 있다.In general, gold is expensive and low in production, and in the past, it was mostly used as a specific decoration having a predetermined shape such as a ring, a necklace, an earring or a brooch or as a means of accumulating economic wealth. However, in recent years, due to the above physicochemical properties, the use of gold is directly used in various fields such as electric and electronic fields, such as semiconductors, as well as increasing the use of coating the outside of the product.
그 예로, 열전도율이 높고, 화학적으로 안정된 표면을 가지는 불판 및 석쇠 에 금을 코팅함으로써 예열시간을 단축하여 가스 사용량을 줄리고, 조리중에 발생하는 기름 등과 반응이 일어나지 않도록 하며, 조리과정에서 인체에 유해한 물질이 음식물에 흡착하지 않도록 기능을 하는 "금 코팅 가열 조리기"(대한민국등록실용신안 제20-0361692호), 음식물을 섭취할 때 입속으로 유입되는 해당 부위에 인체에 유익한 금을 떨어지기 쉽게 소정 두께로 코팅시켜 아름다운 외관의 제공은 물론 음식물을 섭취할 때 혈액순환 및 노화를 방지하여 건강에 이로운 효과가 있는 "금 코팅 수저"(등록실용신안 제20-0390870호), 티타늄픽스츄어와 세라믹 어버트먼트간의 접촉 부위를 순금이나 금합금으로 코팅막을 형성하여 인서트를 사용하지 아니하고도 수려한 심미성을 가지며 티타늄픽스츄어와 세라믹 어버트먼트간의 접합부분에 대한 X-ray 접합도 검사가 가능하고 세라믹 어버트먼트로 인한 티타늄픽스츄어의 손상을 방지할 수 있는 세라믹어버트먼트인 "금 코팅막을 가진 세라믹어버트먼트"(등록실용신안 제20-0338092호), 그 외에도, 항균, 항취, 혈액순환이 우수한 비금속광물질이 코팅된 모기장(등록실용신안 제20-0372049호), 금입자로 코팅되고 불포화 탄화수소 산화에 사용되는 담지 촉매의 재생방법(공개특허 특2001-0040709) 등이 있다. For example, by coating gold on a plate and grill with a high thermal conductivity and chemically stable surface, the preheating time is shortened, reducing gas consumption, and preventing reactions such as oils generated during cooking. "Gold-coated heated cooker" that functions to prevent substances from adsorbing on food (Korean Utility Model No. 20-0361692), a certain thickness that makes it easier to drop gold that is beneficial to the human body to the area that enters the mouth when ingesting food "Gold coated cutlery" (Registration Utility Model No. 20-0390870), titanium fixtures and ceramic averts that provide a beautiful appearance as well as a beautiful appearance by preventing blood circulation and aging when ingesting food. Coated film is formed of pure gold or gold alloy on the contact area between the parts, so it has a beautiful aesthetic without using inserts. It is also possible to inspect the X-ray joint of the joint between the titanium fixture and the ceramic abutment and to prevent the damage of the titanium fixture due to the ceramic abutment. Abutment "(Registration Utility Model No. 20-0338092), as well as a mosquito net coated with a non-metallic mineral with excellent antibacterial, deodorant and blood circulation (Registration Utility Model No. 20-0372049), unsaturated hydrocarbons coated with gold particles There is a regeneration method of the supported catalyst used for oxidation (Patent No. 2001-0040709).
상기에서 살펴본 바와 같이, 금 코팅 기술이 실제로 다양한 분야에서 적용되고 있지만, 지금까지의 금 코팅에 관한 기술로는 금 코팅을 하는 장치에 관한 실용신안이 다수 존재한다. 그 예로, 등록실용신안인 "자동금박인쇄기", "수동금박인쇄기", "무늬용금박인쇄기", "호스용금박인쇄장치", "자판금박인쇄기", "금박전사기" 등이며, 금박의 형성방법에 관한 공개특허로서 금분의 도색에 의해 필요부분에 금 박을 형성키 위한 금박의 형성방법에 관한 것으로, 금분을 물, 광택제와 섞여 볼과 함께 회전용기내에 내입하여 회전시키는 금분 광택공정과 볼을 제거하고, 물과 광택제를 여과지에 의해 분리하는 분리공정, 건조된 금분을 PVC 용액과 섞여 금색잉크를 형성하는 금색 잉크 형성공정 및 금색잉크를 피장식품의 표면에 실크스크린 인쇄하는 인쇄공정의 결합하여 금박을 형성하는 "금박의 형성방법"(대한민국특허출원 제1996-0021904호)이 있다.As described above, although the gold coating technology is actually applied in various fields, there have been a number of utility models related to the gold coating device as a technology related to the gold coating. For example, the registered utility model "automatic gold foil printing machine", "manual gold foil printing machine", "pattern gold foil printing machine", "hose gold foil printing machine", "keyboard foil printing machine", "gold foil printing machine", etc. The present invention relates to a method of forming a gold foil for forming a gold foil on a necessary part by painting gold powder. The gold powder polishing process is performed by mixing gold powder with water and a polishing agent and inserting it into a rotating container with a ball. Separation process of removing the ball, separating water and polish by filter paper, gold ink forming process of mixing dried gold powder with PVC solution to form gold ink, and printing process of silk screen printing gold ink on the surface of packaged food. There is a " method of forming gold leaf " (Korean Patent Application No. 1996-0021904) that combines to form a gold leaf.
그러나, 현재까지는 상기와 같이 일반적인 성질의 금박 형성방법 또는 금박에 필요한 장치에 관한 기술 등이 개발되어 있을 뿐, 금박의 안정성, 특히 물속에서 효율적인 수용화를 통하여 안정하게 금박이 유지되는 기술에 관해서는 알려진 바가 없었다.However, until now, only gold foil forming methods or devices necessary for gold foil having general properties have been developed as described above, and gold foil stability, in particular, technology in which gold foil is stably maintained through efficient solubility in water is described. None known.
이에 본 발명자들은 상기와 같은 문제점을 해결하기 위해 예의 노력한 결과, 폴리에틸렌글리콜을 금과 친화력을 가지는 화학적 작용기로 치환시킨 다음, 금 입자와 함께 반응시켜 친수성 금 입자를 제조하고, 상기 제조된 금 입자의 수용성이 증가한다는 것을 확인하고, 본 발명을 완성하게 되었다.Accordingly, the present inventors have made diligent efforts to solve the above problems. Subsequently, the polyethylene glycol is substituted with a chemical functional group having affinity with gold, and then reacted with the gold particles to produce hydrophilic gold particles. It was confirmed that the water solubility increases, and the present invention was completed.
결국, 본 발명의 주된 목적은 폴리에틸렌글리콜 말단을 금과 친화력 있는 화학적 작용기로 치환한 다음, 금 입자와 함께 반응시키는 것을 특징으로 하는 수용성이 증가된 금 입자의 제조방법을 제공하는 데 있다. After all, the main object of the present invention is to provide a method for producing water-soluble increased gold particles, characterized in that the polyethylene glycol terminal is replaced with a gold affinity chemical functional group, and then reacted with the gold particles.
본 발명의 다른 목적은 상기 방법에 의해 제조된 금 입자를 함유한 친수성 금 코팅제를 제공하는데 있다.Another object of the present invention is to provide a hydrophilic gold coating containing gold particles produced by the above method.
상기 목적을 달성하기 위하여, 본 발명은 (a) 폴리에틸렌글리콜 말단을 금과 친화력을 가지는 화학적 작용기로 치환하는 단계; 및 (b) 상기 치환된 폴리에틸렌글리콜을 함유한 수용액에 금입자를 첨가한 다음, 반응시키는 단계를 포함하는 친수성 금입자의 제조방법을 제공한다.In order to achieve the above object, the present invention comprises the steps of (a) replacing the polyethylene glycol end with a chemical functional group having affinity with gold; And (b) adding gold particles to the aqueous solution containing substituted polyethylene glycol, and then reacting the hydrophilic gold particles.
본 발명에 있어서, 상기 금과 친화력을 가지는 화학적 작용기는 아민기 또는 티올기인 것을 특징으로 할 수 있다. 또한, 금 입자 100중량부에 대하여 상기 티올기로 치환된 폴리에틸렌글리콜 및 상기 아민기로 치환된 폴리에틸렌글리콜의 첨가량은 각각 4 ∼ 100 중량부 및 100 ∼ 300 중량부인 것을 특징으로 할 수 있다. In the present invention, the chemical functional group having affinity with gold may be an amine group or a thiol group. The amount of the polyethylene glycol substituted with the thiol group and the polyethylene glycol substituted with the amine group may be 4 to 100 parts by weight and 100 to 300 parts by weight based on 100 parts by weight of the gold particles, respectively.
본 발명은 또한, 상기 방법에 의해 제조된 친수성 금 입자를 유효성분으로 함유하는 금 코팅제를 제공한다. The present invention also provides a gold coating agent containing the hydrophilic gold particles produced by the above method as an active ingredient.
이하, 본 발명을 상세히 설명한다. Hereinafter, the present invention will be described in detail.
폴리에틸렌글리콜(polyethyleneglycol, PEG)은 carbowax, 폴리왁스라고도 하고, 화학구조는 HO-(CH2-CH2-O)n-H이며, CAS(Chemical Abstract Service) number는 25322-68-3이다. 녹는점은 65℃, 비중은 1.101이고, 인화점은 171℃이다. 그 예로는 PEG-100, PEG-200, PEG-400, PEG-500, PEG-800, PEG-1000, PEG-4000, PEG-6000, PEG-9000, PEG-20000 등이 있고, PEG 뒤의 숫자는 폴리에틸렌글리콜의 평균 분자량을 의미하여, 폴리에틸렌글리콜의 반복단위는 -OCH2CH2-이고, 숫자가 높을수록 반복단위가 커진다. PEG는 통상적으로 용해보조제나 고분자 합성시 사용되는 원료물질로, 용해시키고자 하는 물질의 종류에 따라, 또는 합성하고자 하는 고분자의 종류에 따라 적절한 PEG를 선택하여 사용하고, 희석력이 우수하며, 중합도의 차이에 따라 물성이 차이가 난다.Polyethyleneglycol (PEG) is also referred to as carbowax and polywax, its chemical structure is HO- (CH 2 -CH 2 -O) nH, and the Chemical Abstract Service (CAS) number is 25322-68-3. Melting point is 65 ℃, specific gravity is 1.101, flash point is 171 ℃. Examples include PEG-100, PEG-200, PEG-400, PEG-500, PEG-800, PEG-1000, PEG-4000, PEG-6000, PEG-9000, PEG-20000, and the number after PEG. The mean molecular weight of polyethylene glycol, the repeating unit of polyethylene glycol is -OCH 2 CH 2- , the higher the number, the larger the repeating unit. PEG is a raw material used in the synthesis of dissolution aids or polymers, and suitable PEG is selected depending on the type of material to be dissolved or the type of polymer to be synthesized. Depending on the difference in physical properties.
또한, 폴리에틸렌글리콜은 친수성이 높은 물질이며 말단에 여러 가지 물질로 치환 가능한 특징을 가지고 있다. 이에 말단에 금과 친화력이 있는 티올기 또는 아민기로 처리된 폴리에틸렌글리콜(polyethylene glycol, PEG) 수용액과 금박을 함께 섞어주면, 말단의 기능기들이 금박 표면에 강하게 결합하여 금박을 폴리에틸렌글리콜로 안정적으로 코팅할 수 있다. In addition, polyethylene glycol is a material having high hydrophilicity and has a feature that can be substituted with various substances at its ends. When the gold foil is mixed with an aqueous solution of polyethylene glycol (PEG) treated with a thiol group or an amine group having affinity with gold at the end, the functional groups at the end bind strongly to the surface of the gold foil and stably coat the gold foil with polyethylene glycol. can do.
금과 친화력이 있는 화학적 작용기에는 티올기, 아민기가 있으나, 이에 한정되는 것은 아니다.Chemical functional groups having affinity with gold include, but are not limited to, thiol groups and amine groups.
원래 금박 자체에는 친수성이 없어 일반적으로는 물 위에 떠 있지만, 본 발명에 따른 폴리에틸렌글리콜로 코팅된 금박은 물속에 안정적으로 떠 있을 수 있다. 아민기를 가진 폴리에틸렌글리콜(NH2-PEG)의 경우, 농도가 낮아질수록 금박의 친수성이 떨어지지만, 티올기를 가진 폴리에틸렌글리콜(SH-PEG)은 같은 농도의 아민-폴리에틸렌글리콜에 비해 거의 완벽하게 금박을 친수화 시켰다. Originally, the gold foil itself is not hydrophilic and generally floats on water, but the gold foil coated with polyethylene glycol according to the present invention may stably float in water. In the case of polyethylene glycol (NH 2 -PEG) having an amine group, the hydrophilicity of the gold foil is decreased at lower concentrations, but the polyethylene glycol (SH-PEG) having a thiol group is almost completely more effective than the amine-polyethylene glycol having the same concentration. Hydrophilized.
이하, 실시예를 통하여 본 발명을 더욱 상세히 설명하고자 한다. 이들 실시예는 오로지 본 발명을 예시하기 위한 것으로서, 본 발명의 범위가 이들 실시예에 의해 제한되는 것으로 해석되지는 않는 것은 당업계에서 통상의 지식을 가진 자에게 있어서 자명할 것이다.Hereinafter, the present invention will be described in more detail with reference to Examples. These examples are only for illustrating the present invention, it will be apparent to those skilled in the art that the scope of the present invention is not to be construed as being limited by these examples.
실시예Example 1: 말단이 1: terminal 티올기로Thiol group 치환된 폴리에틸렌글리콜 수용액을 이용한 금 입자의 제조 및 효과 Preparation and Effect of Gold Particles Using Substituted Polyethylene Glycol Solution
폴리에틸렌글리콜의 말단을 티올기로 치환하고, 상기 치환된 폴리에틸렌글리콜 수용액인, 0mg/ml, 0.0001mg/ml, 0.001mg/ml, 0.01mg/ml, 0.02mg/ml의 티올기를 가진 폴리에틸렌글리콜(SH-PEG) 수용액 10ml에 각각 5mg의 금박을 첨가한 후 24시간 동안 반응시킨 다음, 상태를 관찰하였다. The terminal of the polyethylene glycol is substituted with a thiol group, and the polyethylene glycol having a thiol group of 0 mg / ml, 0.0001 mg / ml, 0.001 mg / ml, 0.01 mg / ml, and 0.02 mg / ml, which is the substituted polyethylene glycol solution (SH- 5 mg of gold leaf was added to 10 ml of each aqueous solution of PEG) and reacted for 24 hours, and then the state was observed.
그 결과, 도 1에 나타난 바와 같이, SH-PEG 가 전혀 섞이지 않은 수용액(A)에 있는 금박과 비교하여 낮은 농도의 SH-PEG 수용액에서는 일부 금박이 물과 섞였으며, SH-PEG의 농도가 높을수록 친수성은 높아져 0.02mg/ml SH-PEG 수용액(E)에서는 대부분의 금박이 물에 섞여있는 것을 확인할 수 있었다. As a result, as shown in Figure 1, compared to the gold foil in the aqueous solution (A) that is not mixed with SH-PEG, some gold leaf was mixed with water in the SH-PEG aqueous solution of low concentration, the concentration of SH-PEG was high As the hydrophilicity was increased, most gold leaf was mixed with water in 0.02mg / ml SH-PEG aqueous solution (E).
실시예Example 2: 말단이 아민기로 치환된 폴리에틸렌글리콜 수용액을 이용한 금 입자의 제조 및 효과 2: Preparation and Effect of Gold Particles Using Aqueous Polyethylene Glycol Substituted with Amine Group
폴리에틸렌글리콜의 말단을 아민기로 치환하고, 상기 치환된 폴리에틸렌글리콜 수용액인, 0mg/ml, 0.025mg/ml, 0.05mg/ml, 0.25mg/ml, 0.5mg/ml의 아민기를 가 진 폴리에틸렌글리콜(NH2-PEG) 용액 10ml에 각각 5mg의 금박을 첨가한 후 24시간 동안 반응시킨 다음, 상태를 관찰하였다. A polyethylene glycol having an amine group of 0 mg / ml, 0.025 mg / ml, 0.05 mg / ml, 0.25 mg / ml, and 0.5 mg / ml, which is substituted with an amine group and terminated at an end of the polyethylene glycol. 2 -PEG) 5mg of gold leaf was added to each 10ml solution and reacted for 24 hours, and then the state was observed.
도 2에 나타난 바와 같이, 농도가 가장 높은 NH2-PEG 수용액(E)에서는 금박이 대부분 물과 섞였으나 농도가 낮을수록 금박이 물과 덜 섞이고, 전혀 섞이지 않은 수용액(A)에 비하여 농도가 높을수록 금박이 물에 잘 섞이는 것을 확인할 수 있었다(도 2).As shown in FIG. 2, in the NH 2 -PEG aqueous solution (E) having the highest concentration, the gold leaf was mostly mixed with water, but as the concentration was lower, the gold leaf was less mixed with the water, and the concentration was higher than that of the aqueous solution (A) which was not mixed at all. As the gold leaf was mixed well with water was confirmed (Fig. 2).
이상으로 본 발명 내용의 특정한 부분을 상세히 기술하였는 바, 당업계의 통상의 지식을 가진 자에게 있어서, 이러한 구체적 기술은 단지 바람직한 실시양태일 뿐이며, 이에 의해 본 발명의 범위가 제한되는 것은 아니다. 본 발명의 실질적인 범위는 첨부된 청구항들과 그것들의 등가물에 의하여 정의된다고 할 것이다.As described above in detail specific parts of the present invention, those skilled in the art, these specific descriptions are only preferred embodiments, and the scope of the present invention is not limited thereby. It is intended that the scope of the invention be defined by the claims appended hereto and their equivalents.
이상 상세히 기술한 바와 같이, 본 발명은 친수성 금 입자의 제조방법 및 상기 방법에 의해 제조된 친수성 금 입자를 유효성분으로 함유하는 금 코팅제를 제공하는 효과가 있다. 또한, 기존 금박은 친수성이 없어 물에 부유되나, 본 발명에 따른 금 입자는 친수성이 매우 높아 물 속에서도 안정성을 유지할 수 있어 금 코팅제로서 유용하다.As described in detail above, the present invention has the effect of providing a method for producing hydrophilic gold particles and a gold coating agent containing the hydrophilic gold particles produced by the method as an active ingredient. In addition, the existing gold foil is suspended in water because it is not hydrophilic, gold particles according to the present invention is very high hydrophilicity can maintain stability in water is useful as a gold coating agent.
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