KR100383454B1 - The method for manufacturing of ion exchange illite - Google Patents

The method for manufacturing of ion exchange illite Download PDF

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KR100383454B1
KR100383454B1 KR10-2000-0057790A KR20000057790A KR100383454B1 KR 100383454 B1 KR100383454 B1 KR 100383454B1 KR 20000057790 A KR20000057790 A KR 20000057790A KR 100383454 B1 KR100383454 B1 KR 100383454B1
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illite
ion exchange
solid
stirring
hours
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KR20010000465A (en
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황재효
임경천
구경완
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(주) 실버라이트
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J39/00Cation exchange; Use of material as cation exchangers; Treatment of material for improving the cation exchange properties
    • B01J39/08Use of material as cation exchangers; Treatment of material for improving the cation exchange properties
    • B01J39/10Oxides or hydroxides
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/12Naturally occurring clays or bleaching earth
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/30Ion-exchange
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/20Silicates
    • C01B33/36Silicates having base-exchange properties but not having molecular sieve properties
    • C01B33/38Layered base-exchange silicates, e.g. clays, micas or alkali metal silicates of kenyaite or magadiite type
    • C01B33/42Micas ; Interstratified clay-mica products
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B14/00Use of inorganic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of inorganic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
    • C04B14/02Granular materials, e.g. microballoons
    • C04B14/04Silica-rich materials; Silicates
    • C04B14/20Mica; Vermiculite

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  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
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  • Inorganic Chemistry (AREA)
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  • Life Sciences & Earth Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Materials Engineering (AREA)
  • Ceramic Engineering (AREA)
  • Civil Engineering (AREA)
  • Structural Engineering (AREA)
  • Silicates, Zeolites, And Molecular Sieves (AREA)
  • Disinfection, Sterilisation Or Deodorisation Of Air (AREA)
  • Catalysts (AREA)

Abstract

본 발명은 천연 일라이트 1g당 10~50ml의 증류수에 교반하여 충분히 분산시킨 다음, 0.1N~3.0 N 가성소다를 이용하여 pH 7.0까지 중화시킨 후 , 0.0195~ 0.02 g의 0.1N~3.0 N 질산은수용액을 첨가하여 6~24시간 실온에서 교반하여 제조 된 일라이트 수용액을 고액분리 시킨 다음, 고액분리된 고체를 25~120℃로 2시간 공기중에서 건조시켜 제조하며, 광물학적 구조가 인편상(운모) 삼층구조이며, 입도는 0.5~2㎛, 비표면적은 9493㎠/㎖ 이며, 물, 유기용매, 산, 알카리에 불용성으로서, 다음 구조식을 갖는 이온교환일라이트에 관한 것이다.The present invention is sufficiently dispersed by stirring in 10 ~ 50ml of distilled water per 1g of natural illite, and then neutralized to pH 7.0 using 0.1N ~ 3.0N caustic soda, 0.0195 ~ 0.02g 0.1N ~ 3.0 N silver nitrate aqueous solution The solution was prepared by solid-liquid separation of the aqueous solution of illite prepared by stirring at room temperature for 6-24 hours and then drying the solid-liquid separated solid at 25-120 ° C. for 2 hours, and the mineral structure was flaky (mica). It has a three-layer structure, has a particle size of 0.5 to 2 µm, a specific surface area of 9493 cm 2 / ml, and relates to an ion exchange illite having the following structural formula as insoluble in water, an organic solvent, an acid, and an alkali.

Description

이온교환 일라이트 및 그의 제조방법 {The method for manufacturing of ion exchange illite}Ion exchange illite and its manufacturing method {The method for manufacturing of ion exchange illite}

본 발명은 이온교환 일라이트 및 그의 제조방법에 관한 것으로서, 점토질 광물인 일라이트를 원료로 하여 여기에 금속이온을 교환시켜 제조된 이온교환 일라이트의 조성물 및 그의 제조방법에 관한 것이다.BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an ion exchange illite and a method for producing the same, and relates to a composition of an ion exchange illite prepared by exchanging metal ions therein with an illite, which is a clay mineral, and a method for producing the same.

일라이트는 자연산광물로 운모형 점토질 광물에 관한 것으로 일라이트로 명명되었다. 최근에 흡착제인 지올라이트의 개발로 합성응용분야에 흡착제 뿐만아니라 유기합성 촉매제 및 고분자합성촉매제등에 사용되는 기술개발이 활발하여 흡착제 보다는 촉매로 더 많이 개발되어 왔다. 이와 같이 일라이트 또한 처음에는 흡착제, 탈취제등으로 개발되다가 유기합성 및 고분자합성 촉매제로 개발될 것이 예상되나 본 발명에서는 항균제, 탈취제 및 흡착제등에 유용한 이온교환 일라이트를 발명한 것을 공개하고자 한다.The illite is a natural mineral and refers to the mica type clay mineral. Recently, due to the development of zeolite, which is an adsorbent, the development of technology used in organic synthesis catalysts and polymer synthesis catalysts, as well as adsorbents, has been developed more as a catalyst than an adsorbent. As described above, the illite is initially developed as an adsorbent, a deodorant, etc., but is expected to be developed as an organic synthesis and a polymer synthesis catalyst.

국내공개특허공보 공개번호 제2000-2850호에는 일라이트원료를 분쇄기에 투입하여 320~2000매쉬로 분쇄한 후 하이드로설파이드를 15:1의 체적비로 혼합한 다음 물을 투입하여 마찰분쇄기로 분쇄하여 수황화된 물질에 중화제를 투입하여 여과한 다음 건조시켜 제조하는 극세분말의 일라이트제조방법에 관한 기술이 기재되어 있으며,In Korean Laid-Open Patent Publication No. 2000-2850, elite raw materials are added to a pulverizer and pulverized in a 320 to 2000 mesh, hydrosulfide is mixed at a volume ratio of 15: 1, water is added, and crushed by a friction crusher. Described is a technique for producing an ultrafine powder produced by adding a neutralizing agent to a sulfided material, followed by filtration and drying.

국내공개특허공보 공개번호 제99-43936호 및 제93-413호에는 일라이트를 모르타르에 함유시켜 시멘트의 독성 및 냄새를 중화시켜 혈액순환, 피로회복, 공기정화기능과 각종성인병을 예방할 수 있는 일라이트모르타르의 제조방법이 기재되어 있고,Korean Laid-Open Patent Publication Nos. 99-43936 and 93-413 include illite in mortar to neutralize the toxicity and odor of cement to prevent blood circulation, fatigue recovery, air purification, and various adult diseases. A method for producing light mortar is described,

Journal of the Korean Institute of Mineral And Energy Resources Engineers,Journal of the Korean Institute of Mineral And Energy Resources Engineers,

( Vol.28, No.3, June 1991, 제목 : 영동산 illite에 의한 산업폐수처리)와,(Vol.28, No.3, June 1991, Title: Industrial Wastewater Treatment by illite in Yeongdongsan)

국내공개특허공보 공개번호 제91-14148호에는 일라이트광석을 분쇄한 다음 황산알루미늄 및 수산화 칼슘을 혼합하여 정수제를 제조한 다음, 상기 정수제에 의해 수중에 녹아 있는 중금속이온, 방사능 폐기물 이온과 유기물이온을 흡착하는 응집제의 응집작용으로 폐수를 정수시키는 흡착 침강형 정수제의 제조방법이 기재되어 있으나,Korean Unexamined Patent Publication No. 91-14148 discloses a water purifier prepared by crushing an illite ore and mixing aluminum sulfate and calcium hydroxide, and the heavy metal ions and radioactive waste ions dissolved in water by the water purifier. Although a method for preparing an adsorption sedimentation type purifying agent for purifying wastewater by flocculation of a flocculant which adsorbs organic ions is described,

상기 종래의 기술들은 천연 일라이트를 물리적인 처리를 하여 사용하거나, 단순히 일라이트에 중금속용액을 넣고 교반하여 중금속을 흡착하는 폐기물처리에 이용되는 기술로서 일라이트의 고유성질을 향상시키지 못한 문제점이 있어 왔다.The conventional techniques have a problem that the natural illite is used by physical treatment, or a waste metal adsorbing heavy metal by simply adding a heavy metal solution into the illite and stirring it. come.

상기와 같은 문제점을 해소하기 위하여, 본 발명은 일라이트의 물리적성질을 향상시키기 위하여 연구한 결과 항균 및 흡착효과가 종래의 일라이트보다 우수한새로운 일라이트의 조성물을 제조하였으며, 그 조성물의 구조를 밝혀 환경문제를 해결할 수 있는 이온교환 일라이트 및 그의 제조방법을 제공하는데 그 목적이 있는 것이다.In order to solve the above problems, the present invention has been studied to improve the physical properties of the illite produced a new illite composition excellent in antibacterial and adsorption effect than the conventional illite, revealing the structure of the composition It is an object of the present invention to provide an ion exchange illite and a method for manufacturing the same that can solve environmental problems.

상기와 같은 목적을 달성하기 위하여, 본 발명은 일라이트에 금속이온을 교환시켜 아래와 같은 구조식을 갖는 이온교환 일라이트 및 그의 제조방법에 관한 것이다.In order to achieve the above object, the present invention relates to an ion exchange illite having the following structural formula by exchanging metal ions in the illite and a method for producing the same.

본 발명에서 사용되는 일라이트(Illite)는 접촉열수변성 점토질광물로서 분자식은 (Al1.875Fe0.055Mg0.018)(Al0.55Si3.45)O10(OH)2(Na0.0446K0.61)nH2O 이다.Illite used in the present invention is a contact hydrothermally modified clay mineral whose molecular formula is (Al 1.875 Fe 0.055 Mg 0.018 ) (Al 0.55 Si 3.45 ) O 10 (OH) 2 (Na 0.0446 K 0.61 ) n H 2 O .

광물의 분포상태는 세계적으로 희귀하여 미국 일리노이주, 미시시피주, 캐나다 퀴백주 유럽 헝가리, 한국 영동 등에 분포되어 있으나 대부분 퇴적광물로서 불순물이 많아 품위가 낮으나 한국, 영동, 캐나다 퀴백주의 것은 맥상광체로서 불순물이 적어 품위가 높은 것으로서, 광물학적인 구조가 삼층인편상 구조를 갖으며 주성분은 SiO2, Al2O3, K2O로서 황백색(백색, 적색)의 합성광물이며, 상온에서 3~25마이크론 파장의 원적외선을 89~92%방사하고, 탈취력(98%)이 매우 강하며, 강력한 기(氣)를 발산하며, 수중에서 물분자를 활성화시켜 용존산소를 3배이상 확보하고 산소응집력이 강하고, 수중에서 (-)2가 전하를 갖으며, 용수중의 양이온 유기질이온을 흡착하며, 자체함수 기능으로 보습효과가 크고 직사자외선을 방지하며 활도가 높고, 토양의 지력을 향상시키며(산소, 원적외선, 음이온, 기 등에 의함), 강력한 음이온을 발산(건식 분말상태 : 141ion/cc)한다.Minerals are rare in the world and are distributed in Illinois, Mississippi, Canada, Quiback, Europe, Hungary, and Yeongdong, but most of them are sedimentary minerals. It is high in grade with few impurities. It has a three-layered mineral structure. Its main components are SiO 2 , Al 2 O 3 , and K 2 O. It is a yellow-white (white, red) synthetic mineral, and is 3-25 microns at room temperature. It emits 89 ~ 92% of far-infrared rays of the wavelength, it has very strong deodorizing power (98%), emits strong groups, activates water molecules in water, secures dissolved oxygen more than three times, and has strong oxygen coagulation power. (-) 2 has charge in water, adsorbs cationic organic ions in water, its own function makes moisturizing effect large, prevents direct ultraviolet rays, high activity, and improves soil soil Sikimyeo (by oxygen or the like, far infrared rays, anions, group), emits a strong anion (dry powder form: 141ion / cc) will be.

이하, 본 발명의 바람직한 실시예를 통하여 구체적으로 설명하면 다음과 같다.Hereinafter, described in detail through the preferred embodiment of the present invention.

실시예Example

일라이트 1g당 10~50ml의 증류수에 교반하여 충분히 분산시킨 다음 0.1N~3.0 N 가성소다를 이용하여 pH 7.0까지 중화시킨 후 ,After stirring in 10-50 ml of distilled water per 1 g of illite, the mixture was sufficiently dispersed and neutralized to pH 7.0 using 0.1 N to 3.0 N caustic soda.

상기 중화된 시액 100ml 당 0.025 g의 0.1N~3.0 N 질산은수용액을 첨가하여 6~24시간 실온에서 교반하여 제조된 일라이트 수용액을 고액분리시킨 다음,The aqueous solution of illite prepared by adding 0.025 g of 0.1 N to 3.0 N silver nitrate solution per 100 ml of the neutralized solution and stirring at room temperature for 6 to 24 hours,

여액을 이용하여 이온교환의 완료여부를 확인 한 후,After checking the completion of ion exchange using the filtrate,

확인이 되지 않았을 경우에는 0.1N~3.0 N 질산은수용액을 첨가하여 6~24시간 실온에서 교반을 반복한 다음,If not confirmed, add 0.1 N to 3.0 N silver nitrate solution and repeat the stirring at room temperature for 6 to 24 hours.

이온교환이 확인 되었을 경우에 고액분리된 고체를 25~120℃로 2시간 공기중에서 건조시켜 이온교환 일라이트를 제조하였다.When ion exchange was confirmed, the solid-liquid separated solid was dried at 25-120 ° C. for 2 hours in air to prepare an ion exchange illite.

상기와 같이 제조된 일라이트의 구조는,The structure of the illite manufactured as described above,

이고,ego,

광물학적 구조가 인편상(운모) 삼층구조이며, 입도는 0.5~2㎛, 비표면적은 9493㎠/㎖ 이며, 물, 유기용매, 산, 알카리에 불용성이다.The mineralogy structure is flaky (mica) three-layer structure, with a particle size of 0.5 ~ 2㎛, specific surface area of 9493cm2 / ml, insoluble in water, organic solvent, acid, and alkali.

상기와 같이 제조된 이온교환 일라이트는 살균제, 정수제, 악취 및 유독가스 흡착, 탈취, 분해제, 활성산소발생제로 사용되는 것이다.The ion exchange illite prepared as described above is used as a disinfectant, water purifier, odor and toxic gas adsorption, deodorization, decomposition agent, active oxygen generator.

실험예1Experimental Example 1

금속이온교환된 일라이트의성능을 확인하기 위하여 은이온교환시킨 일라이트로 대장균에 대한 항균실험을 수행하였다.In order to confirm the performance of the metal ion-exchanged illite, an antibacterial experiment was performed on E. coli with silver-ion exchanged illite.

실험방법은 ㎖ 당 106개의 대장균이 존재하는 200㎖ 에 3mg의 은이온교환 일라이트(Ag-illite yellow)를 첨가함으로써 은이온교환 일라이트를 첨가한 후 80분이 경과되지 않아 대장균은 표1과 같이 모두 사멸된 것으로 나타났다.The test method was performed by adding 3 mg of Ag-illite yellow to 200 ml where 10 6 E. coli was present per ml. All seemed dead.

본 실험결과 은이온교환된 일라이트는 항균성능을 가지며 이러한 항균성질을 응용하여 정수제로 사용할 수 있는 것이 확인되었다.As a result of the experiment, it was confirmed that silver ion-exchanged illite had antibacterial activity and could be used as a water purifier by applying such antimicrobial properties.

표1Table 1

실험예 2Experimental Example 2

금속이온교환된 일라이트의성능을 확인하기 위하여 은이온교환시킨 일라이트로 대장균에 대한 항균실험을 수행하였다.In order to confirm the performance of the metal ion-exchanged illite, an antibacterial experiment was performed on E. coli with silver-ion exchanged illite.

실험방법은 시험균주 Escherichia Coli ATCC 25922를 사용하였고 시료농도로 ㎖ 당 108개의 대장균이 존재하는 100㎖ 에 5mg의 은이온교환 일라이트를 첨가함으로써 은이온교환 일라이트를 첨가한 후 20분이 경과되지 않아 대장균은 표1과 같이 모두 사멸된 것으로 나타났다.The test method was Escherichia Coli ATCC 25922, and 5 mg of silver ion exchange illite was added to 100 ml containing 10 8 Escherichia coli per ml at the sample concentration. As a result, E. coli was all killed as shown in Table 1.

본 실험결과 은이온교환된 일라이트는 항균성능을 가지며 이러한 항균성질을 응용하여 다양한 환경친화제품과 정수제로 사용할 수 있는 것이 확인되었다.As a result of this experiment, it was confirmed that silver ion-exchanged illite has antimicrobial activity and can be used as various environmentally friendly products and water purifiers by applying such antimicrobial properties.

표2Table 2

실험예3Experimental Example 3

이온교환된 일라이트의 성능을 확인하기 위하여 은이온교환시킨 일라이트로 암모니아에 대한 탈취, 분해실험을 수행하였다.In order to confirm the performance of the ion exchanged illite, deodorization and decomposition experiments were carried out with silver ion exchanged illite.

실험방법은 6,143ml 용량의 데시케이터에 농도가 800ppm 이 되도록 암모니아가스를 주입하였다. 또한 데시케이터에 은이온교환 일라이트 3g을 넣어 시간에 따른 암모니아의 농도 변화를 측정하였다.In the experimental method, ammonia gas was injected into a desiccator having a capacity of 6,143 ml so that the concentration was 800 ppm. In addition, 3g of silver ion exchange illite was added to the desiccator and the change in concentration of ammonia over time was measured.

실험결과 표3와 같이 은이온교환일라이트를 넣은후 30분이 경과한 후 데시케이터속의 암모니아농도는 25ppm 으로 줄어든 것을 알 수 있었다.As a result, as shown in Table 3, after 30 minutes after adding silver ion exchange illite, the ammonia concentration in the desiccator was reduced to 25 ppm.

본 실험결과 은이온교환된 일라이트는 탈취, 분해 성질이 천연일라이트보다 우수한 것이 발견되었다.As a result of the experiment, it was found that silver ion-exchanged illite had better deodorization and decomposition properties than natural illite.

표 3TABLE 3

상기와 같은 본 발명은 경제적으로 천연의 일라이트를 이용하여 살균제, 정수제, 악취 및 유독가스 흡착, 탈취, 분해제, 활성산소발생제로 사용되는 인조일라이트를 대량으로 저렴하고 용이하게 제조할 수 있는 장점이 있는 것이다.As described above, the present invention can economically produce inexpensively and easily a large amount of artificial light used as a disinfectant, water purifier, odor and toxic gas adsorption, deodorant, decomposition agent, and active oxygen generator using natural illite. There is an advantage.

Claims (2)

이온교환 일라이트에 있어서, 광물학적 구조가 인편상(운모) 삼층구조이며, 입도는 0.5~2㎛, 비표면적은 9493㎠/㎖ 이며, 물, 유기용매, 산, 알카리에 불용성으로서, 다음 구조식을 갖는 이온교환 일라이트.In ion-exchange illite, the mineralogy structure is flaky (mica) three-layer structure, with a particle size of 0.5 to 2 µm, specific surface area of 9493 cm 2 / ml, and insoluble in water, organic solvent, acid, and alkali. Ion exchange illite having. 이온교환 일라이트의 제조방법에 있어서, 천연 일라이트 1g당 10~50ml의 증류수에 교반하여 충분히 분산시킨 다음 0.1N~3.0 N 가성소다를 이용하여 pH 7.0까지 중화시킨 후, 0.025 g의 0.1N~3.0N 질산은수용액을 첨가하여 6~24시간 실온에서 교반하여 제조 된 일라이트 수용액을 고액분리 시킨 다음, 고액분리된 고체를 25~120℃로 2시간 공기중에서 건조시켜 제조함을 특징으로 하는 이온교환 일라이트의 제조방법.In the production method of ion exchange illite, it is sufficiently dispersed by stirring in 10 ~ 50ml distilled water per 1g of natural illite, and neutralized to pH 7.0 using 0.1N ~ 3.0N caustic soda, 0.025g 0.1N ~ Ion exchange characterized in that the solid solution separated by the aqueous solution of illite prepared by adding 3.0 N silver nitrate aqueous solution and stirring at room temperature for 6 to 24 hours, and then drying the solid-liquid separated solid at 25 to 120 ℃ in air for 2 hours. Production method of illite.
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KR101102429B1 (en) * 2009-05-04 2012-01-05 원남메디칼 (주) Sericite exchanged metal ion having anti-bacteria and preparing methods for thereof
CN112875715A (en) * 2021-03-03 2021-06-01 滁州格锐矿业有限责任公司 Method for processing illite for facial mask
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