KR20060026377A - Method for preparing germanium-containing water using loess - Google Patents
Method for preparing germanium-containing water using loess Download PDFInfo
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- KR20060026377A KR20060026377A KR1020040075268A KR20040075268A KR20060026377A KR 20060026377 A KR20060026377 A KR 20060026377A KR 1020040075268 A KR1020040075268 A KR 1020040075268A KR 20040075268 A KR20040075268 A KR 20040075268A KR 20060026377 A KR20060026377 A KR 20060026377A
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- C22B41/00—Obtaining germanium
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Abstract
본 발명은 자연계 지표면에 분포하고 있는 황토, 복용간(반복적인 고열을 가했다가 식힘을 반복한 황토)으로부터 게르마늄 함유수 및 게르마늄함유 부산물(이하 미세분말의 황토액)제조 방법에 관한 것으로 더욱 상세하게는 황토나 복용간에 분포하고 있는 게르마늄 (70(20.55%), 72(27.37%), 73(7.67%), 74(36.74%), 76(7.67%))을 경단(이하 황토나 복용간으로 만든 닭알 크기 및 무게를 같은 형태의 것을 칭함)을 만들어 적열(赤熱:빨갛게 달군 현상)을 가한후 적열 상태에서 지하수(샘물)에 침수시켜 산화된 수용성 유기 게르마늄(이하 게르마늄 함유수로 칭함)함유수를 제조하는 방법으로 유기 게르마늄은 인체 산소 활성 농도를 향상시켜 면역력을 높여주는 작용을 함으로서 면역 체게 개선및 피부 미용 부분 보조 원료로 사용되고 있다.The present invention relates to a process for producing germanium-containing water and germanium-containing by-products (hereinafter referred to as fine powder ocher solution) from loess distributed between natural lands and between doses (ocher after repeated high temperature and cooling). Germanium (70 (20.55%), 72 (27.37%), 73 (7.67%), 74 (36.74%), 76 (7.67%)) distributed between ocher or doses Make water of same size and weight), apply redness (赤 熱: red moon phenomenon), and immerse in groundwater (spring water) in red state to produce oxidized water-soluble organic germanium (hereinafter referred to as germanium-containing water). In this way, organic germanium is used as an auxiliary material to improve immune system and skin beauty by acting to increase the oxygen concentration of the human body to enhance immunity.
이를 위하여 본 발명은 황토나 복용간으로 경단을 만드는 단계, 경단을 실온에서 24시간 이상 건조 시키거나, 열을 가하여 건조 시키는 단계, 경단을 적열시 열을 가하는 매개체를 숯,석탄,전기,가스로 하는 단계, 경단을 750도C-930도C로 30분-60분 동안 적열 시키는 단계, 적열 상태인 경단을 지하수(샘물)에 완전 침수시켜서 산화 게르마늄을 추출 유기 시키는 단계, 추출된 게르마늄 함유수를 여과 시키는 단계, 게르마늄 함유수 제조후 남는 부산물을 분리하여 교반 과정을 거쳐 미립자 상태의 액으로 침전 시켜 따로 분리하는 단계, 적열 상태의 경단량을 가 감 조절하며 지하수에 침수하여 게르마늄 함유수의 게르마늄 함유 농도 비율을 조절하 는 방법, 이와 같은 게르마늄 함유수 및 부산물에서 분리한 미립자 상태인 액의 성질이 게르마늄 70,72,73,74,76이 포함하는 내용의 성질을 가지는 것으로 이루어 진것이 특징이다.To this end, the present invention is a step of making dumplings between loess or dose, drying the dumplings at room temperature for more than 24 hours, or drying them by applying heat, and applying the heat when glowing dumplings to charcoal, coal, electricity, and gas Step, the dandelion is glowing at 750 ° C-930 ° C for 30-60 minutes, the dumped water is completely submerged in groundwater (spring water) to extract and organically extract germanium oxide, and the extracted germanium-containing water The step of filtering, separating the by-products left after the production of germanium-containing water, and stirring them into a liquid in the form of fine particles after stirring, separating them separately. The method of controlling the concentration ratio, and the properties of the liquid in the form of particulates separated from such germanium-containing water and by-products are 70,72,73,74,76. Jingeot is characterized as having achieved the properties of the box contents.
수용성 게르마늄. 적열. 면역체계. 복용간. 황토. 경단.Water soluble germanium. Glowing. Immune system. Taking liver. ocher. Dumpling.
Description
본 발명은 자연계 지표면에 분포 하고 있는 황토 복용간으로부터 게르마늄 함유수 및 게르마늄 함유 부산물을 제조하는 방법에 관한 것으로 상세하게는 게르마늄은 주기율 표 제4B족에 속하는 탄소족 원소로서 원소기호(Ge), 원자번호:32, 녹는점(융점):958.5도C, 끓는점(비점):2700도C의 성질을 지니고 있는 금속이 아닌 아금속 원소로서 지각속 자연계에 넓고 얇게 분호 되어 있으며 또한 특정한 식물에도 함유되어 있으며 공기중에서는 안정하지만 적열 이상으로 가열하면 산화하는 성질을 지니고 있는 물질이다. 고로 이를 추출하는 종래의 방법은 황화광물 제련시 부산물로 얻어지는 방법으로 게르마늄 함유석을 태워 산화 물을 만들고 석탄과 식염을 가하여 소결하면 게르마늄과 카드뮴이 휘발분으로 나온다.The present invention relates to a method for producing germanium-containing water and germanium-containing by-products from the ocher doses distributed on the natural surface of the earth. Specifically, germanium is a carbon group element belonging to group 4B of the periodic table and has an element symbol (Ge), an atom. No. 32, melting point (melting point): 958.5 degrees C, boiling point (boiling point): 2700 degrees C. A non-metallic submetallic element, broadly and thinly divided in the earth's crust, and also contained in certain plants. It is stable in air, but oxidizes when heated above red heat. The conventional method of extracting the blast furnace is a method obtained as a by-product during the smelting of sulfide minerals, burning germanium-containing stones to form oxides, and sintering by adding coal and salt to sinter germanium and cadmium.
이것을 황산에 흡수 시켜 아연말을 사용 카드뮴을 제거하고 건조.배소 시킨다음 염산과 증류하여 염화 게르마늄을 석출시켜 얻는 방법과, 석탄 연소시 연탄을 모으는 방법으로 탄산 나트륨과 석회를 가하고 산화 구리를 혼합 가열하면 그광재 에 게르마늄이 모인다. 이광재를 가루로 만들어 염소를 통과 시키면서 염화철의 수용액 속에서 염산과 황산을 가하여 증류하면 염화 게르마늄을 얻을수 있는 통상적인 방법등이 있으며 국내에 발표된 출원번호 10-1999-0031010은 천연 게르마늄 광석으로부터 게르마늄 함유수를 제조하는 방법으로 천연 게르마늄 광석을 200-250메쉬로 분쇄하여 100-110도C에서 1-2시간 건조 시킨후 공기중에서 냉각시켜 이를 1050-1100도C에서 4-5시간 소성 처리하여 소성된 시료를 공기중에 냉각시킨후 상기 시료가 0.5-1kg/L가 되도록 증류수를 가하여 30-40분간 교반하여 이를 여과하는 단계로 이루어 져 있다.This is absorbed by sulfuric acid, zinc powder is used, cadmium is removed, dried and roasted, and then distilled with hydrochloric acid to obtain germanium chloride, and the method of collecting coal briquettes during coal combustion adds sodium carbonate and lime and mixes copper oxide. Germanium collects in the slag. There is a conventional method for obtaining germanium chloride by distilling hydrochloric acid and sulfuric acid in an aqueous solution of iron chloride while chlorine is passed through the powder of this slag. Application number 10-1999-0031010 published in Korea contains germanium from natural germanium ore. Natural germanium ore is pulverized with 200-250 mesh, dried at 100-110 ° C for 1-2 hours, cooled in air and calcined at 1050-1100 ° C for 4-5 hours. After the sample is cooled in air, distilled water is added so that the sample becomes 0.5-1 kg / L, followed by stirring for 30-40 minutes, followed by filtration.
이와 같은 종래의 기술은 제련 과정의 막대한 시설에 대한 투자 비용과 제련과정에서 발생되는 부산물들의 환경 정화 비용이 과다하게 들어가는 결함사항을 가지고 있으며 앞에서 언급한 2가지 방법은 분말 게르마늄을 얻을수 있는 방법이고, 출원번호 10-1999-0031010은 게르마늄 함유수를 천연 게르마늄 원석로부터 얻는 방법으로 본 발명과 다른 제조 방법으로 구성되어 있음을 발견할수 있으며 제조 비용이 과다하게 들어 가는 단점이 있다.This conventional technology has the disadvantage of excessive investment in the enormous facility of the smelting process and the environmental cleanup cost of the by-products generated in the smelting process, and the two methods mentioned above are methods to obtain powder germanium, Application No. 10-1999-0031010 is a method of obtaining a germanium-containing water from natural germanium ore can be found to be composed of the present invention and other manufacturing methods, there is a disadvantage in that excessive manufacturing costs.
본 발명은 상기와 같은 문제점을 해소하기 위해 자연계 지표면에 게르마늄을 함유하고 있는 황토와 복용간을 이용하여 게르마늄의 본래의 성질인 적열을 가하면 산화할여는 특징을 이용하여 환경에 영향을 주지 않으면서 저렴한 제조 비용으로 게르마늄 함유수를 제조 하는 방법을 제공하는데 목적이 있는 것이다.The present invention is inexpensive without affecting the environment by using a feature that can be oxidized by applying red heat, which is an inherent property of germanium, using the ocher containing germanium and the dose between the natural surface to solve the above problems It is an object of the present invention to provide a method for producing germanium-containing water at production cost.
이와 같은 목적을 달성하기 위해 본 발명은 게르마늄 함유수 제조 방법에 있 어 황토나 복용간으로 경단을 만드는 단계, 경단을 실온에서 24시간 이상 자연 건조시키거나, 열을 가하여 건조시키는 단계, 경단을 적열시 열을 가하는 매개체를 숯,석탄,전기,가스로 하는 단계, 경단을 750도C-930도C로 30분-60분동안 적열시키는 단계, 적열 상태인 경단을 지하수(샘물)에 완전 침수 시켜서 산화 게르마늄을 추출 유기 시키는 단계, 추출된 게르마늄 함유수를 여과 시키는 단계 게르마늄 함유수 제조후 남은 부산물을 분리하여 교반 과정을 거쳐 미립자 상태의 액으로 침전 시켜 따로 분리하는 단계 적열 상태의 경단의 량을 가, 감 조절하며 지하수에 침수하여 게르마늄 함유수의 게르마늄 함유 농도 비율을 조절하는 방법, 이와 같은 게르마늄 함유수 및 부산물에서 분리한 미립자 상태인 액의 성질이 게르마늄 70,72,73,74,76이 포함하는 내용의 성질을 가지는 것으로 이루어 진것이 특징이다.In order to achieve the above object, the present invention provides a method for producing germanium-containing water, which comprises steps of making dumplings between loess or dosing, drying the dumplings at room temperature for at least 24 hours, or drying them by applying heat, and dumping the dumplings. Charging medium to charcoal, coal, electricity, and gas, glowing dumplings at 750 ° C-930 ° C for 30 minutes-60 minutes, and flooding the dumplings in the ground with water (spring water) Extracting and extracting germanium oxide, filtering the extracted germanium-containing water, separating the by-products after the production of the germanium-containing water, stirring the precipitates, and separating them into a liquid in a particulate state. To control the germanium-containing concentration ratio of the germanium-containing water by submerging it into groundwater, The properties of the fine particle state of the solid-liquid separation is characterized jingeot made to have the characteristics of information, comprising a germanium 70,72,73,74,76.
지표면에 오염되지 않은 황토 복용간을 경단으로 만들어 열을 가할수 있는 매개체(숯,석탄,전기,가스)로 적열(빨갛게 되도록 달군 상태)을 가하면 경단에 분포하고 있던 게르마늄 원소가 산화 할여는 불안정 상태에 이르게 된다.Unstable state in which the germanium elements distributed in the dump are oxidized when applied with red heat (coal, coal, electricity, gas) that can make heat from the uncontaminated loess to the ground. Leads to
이때(적열상태) 물에 수장(침수)하게 되면 경단 내부에 급속히 수분이 침투 하면서 적열된 경단이 고열에 수분이 팽창 증발 하면서 경단 외부로 증기가 유출 된다.At this time, when the water (water immersion) in water (immersion) is rapidly infiltrated inside the dumplings, the steamed water is leaked out of the dumplings while the swollen dumplings expand and evaporate at high temperatures.
이때 산화된 불안정한 게르마늄 원소도 팽창된 수증기와 함께 유출되어 경단이 수장된 물속에 다량 유출 분포하여 녹아 있게 된다.At this time, the oxidized unstable germanium element also flows out with the expanded water vapor so that the dump dump is dissolved in a large amount in the stored water.
이를 여과하여 게르마늄 함유수를 만들고 여과후 발생되는 부산물(침전물)중 미립자 상태의 부산물은 침전후 교반 과정을 거처 달리 제조되는 제조물의 촉진원료로 재사용이 가능하며 게르마늄 함유수는 분야별 사용 적합 유무에 따라 기능활성 촉진 보조재료 및 음용수로 사용 할 수 있다.This is filtered to make germanium-containing water, and the by-products in the form of particulates from the by-products (precipitates) generated after filtration can be reused as an accelerating raw material of the manufactured product through the stirring process after precipitation. It can be used as auxiliary material for promoting functional activity and drinking water.
본 발명의 기술적 구성 요소들을 포함하기 위해 다음과 같은 기구 및 재료들을 알파벳 순으로 표시하여 열거 하였다.In order to include the technical components of the present invention, the following instruments and materials are listed in alphabetical order.
A. 지표면의 오염이 안된 황토 및 복용간을 계란(닭알) 크기 무게로 만든 경단.A dumplings made of egg-sized weight of uncontaminated ocher and liver.
B. 적열을 가 할수 있는 로 (전기로,가스로,숯(백탄)로)B. Furnace that can apply heat (electric furnace, gas furnace, charcoal)
C. 오염이 안된 지하수 (샘물)C. Uncontaminated Groundwater (Spring Water)
D. "C"를 담을수 있는 용기D. Container for holding "C"
E. 여과 장치E. Filtration Device
경단(A)를 만들어 공기가 잘 통하는 실온에서 24시간 이상 자연 건조 또는 열을 가하여 건조한후 적열을 가할수 있는 로(B)에 적당량의 경단(A)을 투입하여 적열 상태에 도달 되게 열을 가한다.Make a dump (A) and apply it to the red (B) by putting an appropriate amount of dump dump (A) into the furnace (B) where it can be heated and dried after being naturally dried or heated at room temperature which is well ventilated for more than 24 hours. do.
이때 경단(A)의 적열 시간은 30분-60분간 적열 상태를 유지하며 적열 온도는 750도C에서 930도C까지 유지 한후 적열 상태의 경단(A)을 지하수(C)가 담긴 용기(D)속에 적열 상태로 적당한 량을 투입한다.At this time, the glowing time of the dumpling (A) is kept in the glowing state for 30 minutes to 60 minutes and the glowing temperature is maintained from 750 ° C to 930 ° C, and then the dumpling (A) in the glowing state contains the groundwater (C) Inject the appropriate amount in the red state inside.
이때 경단(A)은 완전 물속에 깊이 침수되게 작업을 행한다.At this time, the dump end A performs work to be submerged deeply in complete water.
적열상태의 경단(A)을 물에 침수 시키면 물이 끓으면서 적열된 경단(A) 속에 수분이 침투하여 팽창함과 동시에 적열시 산화 상태의 경단(A)속에 포함된 산화 게 르마늄이 팽창된 수분과 함께 경단(A)외부로 유출되어 침수된 물속에 산화된 상태로 물속에 유기 분포하게 된다.Submerged in the red dumplings (A) in water, the water boils, the water penetrates into the glowing dumplings (A), expands, and expands the germanium oxide contained in the oxidized dumplings (A). It flows out of the dump end (A) with water and is organically distributed in the water in an oxidized state in the submerged water.
이때 게르마늄 함수율을 높이려면 경단(A)와 물(C)의 양을 가감 조절함으로서 게르마늄 함수율 농도를 조절 할 수 있으며 이때 만들어진 게르마늄 함유수를 여과기(E)를 통과 시켜 여과하여 게르마늄 함유수를 얻는다.In this case, to increase the germanium moisture content, the germanium moisture content concentration can be adjusted by adjusting the amount of the dump end (A) and the water (C).
게르마늄 함유수를 생산후 남는 부산물은 교반 과정을 거쳐 침전후 미립자 형태의 것을 분리하여 수분이 포함된 상태에서 달리 제조되는 제품의 기능촉진 원료로 사용 될수 있다.The by-products left after producing the germanium-containing water can be used as a function-promoting raw material for products produced differently in the state of containing water by separating the particulate form after precipitation through the stirring process.
위에서 언급된 바와 같이 경단의 적열 온도를 750도씨-930도씨 범위를 유지하는 이유는 경단이 적열되는 최저온도가 750도씨부터이며 게르마늄의 산화 온도 시점도 750도씨부터 산화가 시작되어 958.5도씨(융점:녹는점)가 넘으면 게르마늄이 녹아 잉곳 형태로 변하여 산화 할수 없게 됨을 발견 할 수 있었다.As mentioned above, the reason why the dandelion temperature is kept in the range of 750 degrees C to 930 degrees C is because the lowest temperature at which the dandelion is glowing starts at 750 degrees C and the oxidation temperature of germanium starts at 750 degrees C. It was found that when it was above the melting point (melting point: melting point), the germanium melted and changed into an ingot, which prevented oxidation.
위와 같은 제조 방법으로 얻어진 게르마늄 함유수 농도는 아래 보기와 같은 결과를 얻을수 있으며 다음 보기의 분석 결과는 발명자가 게르마늄 함유수를 제3자인 인하대학교 초정밀 생물분리 기술연구센터에 의뢰하여 분석결과에 대한 공정성을 가미하였음.The concentration of germanium-containing water obtained by the above manufacturing method can be obtained as shown below, and the analysis results in the following example are requested by the inventor to the third-party Inha University ultra-precision bioseparation technology research center. Added.
보기 1View 1
게르마늄 함유수 추출 조건Germanium-Containing Water Extraction Conditions
1. 표준 시료 조건1. Standard Sample Conditions
1) 게르마늄 원석 : 1.70kg1) Germanium Gemstone: 1.70kg
2) 황토경단 : 1.60kg2) Yellow soil dump: 1.60kg
3) 표준수(샘물) : 각각8리터3) Standard water (spring water): 8 liters each
4) 적열온도 : 750도씨-930도씨4) Glowing temperature: 750 ° C-930 ° C
5) 적열시간 : 30분-60분5) Glowing time: 30 minutes-60 minutes
위 보기1과 같은 조건으로 게르마늄 함유수를 제조하여 원수(표준수)2리터, 게르마늄원석추출물2리터, 황토추출물2리터로 구성된 3가지 시료를 제공하여 다음보기2와 같은 결과를 얻을수 있었음.Germanium-containing water was prepared under the same conditions as in Example 1, and three samples of raw water (standard water), 2 liters of germanium gemstone extract, and 2 liters of ocher extract were obtained.
보기 2View 2
(게르마늄 함량 분석 보고서)(Germanium Content Analysis Report)
분석기관 : 인하대학교 (초정밀 생물 분리기술 연구센터)Analytical Institution: Inha University (Super Precision Bioseparation Technology Research Center)
분석장비 : ICP-M,SAnalysis equipment: ICP-M, S
분석일자 : 2004년 8월 12일Date of Analysis: August 12, 2004
원수 및 추출 시료 분석결과Raw water and extracted sample analysis results
자연계에 분포하고 있는 5종류Five kinds distributed in nature
(70(20.55%),72(27.37%),73(7.67%),74(36.74%),76(7.67%))중 가장 분포량이 많은 72와 74만 분석 하였음.Only 72 and 74 (70 (20.55%), 72 (27.37%), 73 (7.67%), 74 (36.74%) and 76 (7.67%)) were analyzed.
위의 분석 결과를 보면 2종류(Ge72,Ge74) 분석결과 원수에 비해 황토 추출의 경우 160배정도의 게르마늄이 추출되어 있음을 알수 있으며 자연계에 존재하는 5가지가 전부 추출된다고 볼수 있으므로 그 비율은 원수의 200배 이상이 될 것으로 추정할 수 있음.According to the analysis results above, two types of Ge72 and Ge74 analysis results show that the extraction of loess is about 160 times that of germanium in comparison with raw water, and it can be seen that all five kinds in nature are extracted. It can be estimated to be more than 200 times.
본 발명에서는 과대한 시설투자와 화학적 재료를 사용치 않으면서 친 환경적인 방법으로 게르마늄 함유수를 제조하는 방법으로 대량의 게르마늄 함유수를 제조할수 없는 단점을 가지고 있으나, 저렴한 비용과 친 환경적으로 매우좋은 양질의 게르마늄 함유수를 추출할 수 있으며 여기서 발생 되는 부산물은 완전 연소화 및 황토류는 다시 자연으로 돌려 보내는 환경 친화적인 방법인 것이다.In the present invention, there is a disadvantage in that a large amount of germanium-containing water can not be manufactured by a method of producing germanium-containing water in an environmentally friendly way without excessive facility investment and chemical materials, but at a low cost and very environmentally friendly. Good quality germanium-containing water can be extracted, and the by-product of this is an environmentally friendly way of complete combustion and returning the yellow earth back to nature.
Claims (2)
Priority Applications (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR1020040075268A KR100750351B1 (en) | 2004-09-20 | 2004-09-20 | Method for preparing germanium-containing water using loess |
| PCT/KR2005/003056 WO2006033535A1 (en) | 2004-09-20 | 2005-09-15 | Method of manufacturing germanium-containing solution from yellow soil |
| US10/560,668 US20070095170A1 (en) | 2004-09-20 | 2005-09-15 | Method of manufacturing germanium-containing solution from yellow soil |
| CNB2005101031845A CN100381361C (en) | 2004-09-20 | 2005-09-20 | Method of manufacturing germanium-containing solution from yellow soil |
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| Application Number | Priority Date | Filing Date | Title |
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| KR1020040075268A KR100750351B1 (en) | 2004-09-20 | 2004-09-20 | Method for preparing germanium-containing water using loess |
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| KR100750351B1 KR100750351B1 (en) | 2007-08-17 |
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| Country | Link |
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| US (1) | US20070095170A1 (en) |
| KR (1) | KR100750351B1 (en) |
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| WO (1) | WO2006033535A1 (en) |
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| ES2293831B2 (en) * | 2006-07-03 | 2008-12-16 | Universidad De Sevilla | PROCEDURE FOR THE RECOVERY OF GERMAN PRESENT IN CARBON ASHES. |
| US10909624B2 (en) * | 2012-05-02 | 2021-02-02 | Aqua-Index Ltd. | Fresh water price index based on water quality |
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| US1918178A (en) * | 1932-01-14 | 1933-07-11 | Enterprise Mfg Co | Process of treating sulphur-bearing ores |
| ES207331A1 (en) * | 1952-01-21 | 1953-03-01 | Sogo Kenkyujo Zh Sekitan | Process of recovering germanium-containing material from coal |
| DE3419120C1 (en) * | 1984-05-23 | 1985-10-10 | Preussag Ag Metall, 3380 Goslar | Process for obtaining a germanium concentrate that can be processed |
| US4678647A (en) * | 1986-05-12 | 1987-07-07 | Enron Corp. | Process for the recovery of gallium and germanium from coal fly ash |
| US4643110A (en) * | 1986-07-07 | 1987-02-17 | Enron, Inc. | Direct fuel-fired furnace arrangement for the recovery of gallium and germanium from coal fly ash |
| KR100302277B1 (en) * | 1999-07-29 | 2001-09-13 | 호 근 김 | Method for producing germanium containing water from natural germanium ores |
| KR20020086810A (en) * | 2001-05-12 | 2002-11-20 | (주)코스타 월드 | Functional aquarium water and preparation method thereof |
| KR100411293B1 (en) * | 2002-11-30 | 2003-12-24 | Yi Nam Jeon | Purified water by using yellow earth and method for preparing thereof |
| KR20040107453A (en) * | 2004-08-04 | 2004-12-20 | 제일수산영어조합법인 | Method for forming active water for aging of marine products, fruits and vegetables using far-infrared radiation gemstones |
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| CN1762826A (en) | 2006-04-26 |
| US20070095170A1 (en) | 2007-05-03 |
| WO2006033535A1 (en) | 2006-03-30 |
| KR100750351B1 (en) | 2007-08-17 |
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