KR20160124712A - The manufacturing method of magnesium hydroxide and calcium chloride using dolomite for raw material - Google Patents

The manufacturing method of magnesium hydroxide and calcium chloride using dolomite for raw material Download PDF

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KR20160124712A
KR20160124712A KR1020160130677A KR20160130677A KR20160124712A KR 20160124712 A KR20160124712 A KR 20160124712A KR 1020160130677 A KR1020160130677 A KR 1020160130677A KR 20160130677 A KR20160130677 A KR 20160130677A KR 20160124712 A KR20160124712 A KR 20160124712A
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calcium chloride
magnesium hydroxide
magnesium
hydroxide
dolomite
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규 재 유
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규 재 유
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F5/00Compounds of magnesium
    • C01F5/14Magnesium hydroxide
    • C01F5/16Magnesium hydroxide by treating magnesia, e.g. calcined dolomite, with water or solutions of salts not containing magnesium
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F11/00Compounds of calcium, strontium, or barium
    • C01F11/20Halides
    • C01F11/24Chlorides
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F5/00Compounds of magnesium
    • C01F5/02Magnesia
    • C01F5/06Magnesia by thermal decomposition of magnesium compounds
    • C01F5/08Magnesia by thermal decomposition of magnesium compounds by calcining magnesium hydroxide
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F5/00Compounds of magnesium
    • C01F5/14Magnesium hydroxide
    • C01F5/145Purification
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/80Particles consisting of a mixture of two or more inorganic phases
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/80Compositional purity

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  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)

Abstract

The present invention relates to a manufacturing method of magnesium hydroxide and calcium chloride using dolomite, which can be used as a base material of 25 types of magnesium compounds by manufacturing magnesium hydroxide with dolomite. The manufacturing method comprises the steps of: manufacturing a mixed chloride solution of calcium chloride and magnesium chloride; lowing a PH; and filtering, separating, and purifying the same, by regulating the PH above 2.0.

Description

백운석을 이용하는 수산화마그네슘과 염화칼슘 제조방법{The manufacturing method of magnesium hydroxide and calcium chloride using dolomite for raw material}[0001] The present invention relates to a process for preparing magnesium hydroxide and calcium chloride using dolomite,

염화칼슘은 제설, 방진, 흡습, Polymer 응고제, 식품첨가물로 사용되며 수산화마그 네슘은 탄산마그네슘, 황산마그네슘, 고무, 난연재, 보온재, 비료, 환경처리제, 식품, 인체와 동물의 무기 영양소, 의약 원료용등 광범위한 용도로 사용되는 정밀화학 무기 소재 분야이다.       Magnesium chloride is used as magnesium carbonate, magnesium sulfate, rubber, flame retardant, thermal insulation material, fertilizer, environmental treatment agent, food, inorganic nutrient of human and animal, raw material for medicine, etc. It is a field of fine chemical inorganic materials used for a wide range of applications.

종래의 염화칼슘 제조는 석회석(CaCO3)을 염산에 용해하여 정제하고 농도 조정하여 액상의 염화칼슘을 제조하며 분무식으로 건조하여 분말 염화칼슘을 제조한다.   Conventional production of calcium chloride is performed by dissolving limestone (CaCO3) in hydrochloric acid, refining it, adjusting the concentration thereof to prepare liquid calcium chloride, and drying it by spraying to produce powdered calcium chloride.

수산화마그네슘의 종래 제조방법은 Magnesite를 소성하여 MgO를 만들고 이를 열수 수화하여 제조하며 Dolomite를 경소성 탈탄산하여 경소백운회(CaO.MgO)를 만들어 제강공정의 Slag 제거용으로 이용되며    The conventional method of producing magnesium hydroxide is to produce MgO by firing Magnesite, and hydrothermalizing it to produce Dolomite, which is used to remove slag from the steelmaking process by making light caustic soda (CaO.MgO)

이를 수화하여 수산화마그네슘[Mg(OH)2]과 수산화칼슘[Ca(OH)2]혼합 백운회유를 제조하여 배연탈황제 및 산성폐수 정화용으로 이용되고 있다.It is hydrated and used as a flue gas desulfurizing agent and an acidic wastewater purification by producing a mixture of magnesium hydroxide [Mg (OH) 2 ] and calcium hydroxide [Ca (OH) 2 ]

백운회유의 Ca(OH)2와 Mg(OH)2 분리는 MgCl2 .를 기질로 하여 고형물 Ca(OH)2을 용액 CaCl2로 치환 반응하여 고액 분리되는 방법이 문헌등에 개시되어 공지되고 있으나 MgCl2는 고가의 화학제품으로 과중한 원가문제로 활용성이 제약되고 있다.Ca (OH) 2 and Mg (OH) 2 Separation is MgCl 2. (Solid solution) of Ca (OH) 2 with a solution of CaCl 2 is solubilized by solid-liquid separation, and MgCl 2 is expensive chemical product because of a heavy cost problem.

종래기술의 문제점은 다음과 같다.    The problems of the prior art are as follows.

1. Magnesite 및 Dolomite를 경소성하고 열수로 수화하는 고에너지 소비이다.    1. Magnesite and Dolomite are high energy consumption which lightly burns and hydrothermally hydrates.

2. 소성로에서 배출되는 이산화탄소 및 Sox, Nox등 환경오염 물질이 배출된다.    2. Environmental pollutants such as carbon dioxide and Sox and Nox emitted from the firing furnace are discharged.

3. Dolomite 경소백운회유는 Ca(OH)2와 Mg(OH)2 혼합물로 배연탈황용으로 이용시 고형물인 석고의 2차 폐기물이 발생되고 있다.3. Dolomite light Caucasian milks were Ca (OH) 2 and Mg (OH) 2 When used as a flue gas desulfurization mixture, secondary wastes of solid gypsum are generated.

1. 化合物生産應用 中國 化學工業出版社 胡慶福 主編     1. Compound production 應用 中國學學 工業 publisher 胡慶福 2. 鹽基性炭酸マグネシウムに就て(講演會硏究報告書) 日本コム協會關西支部     2. On the basic magnesium carbonate (Lecture Report) Nippon Com Association (NIS) 3. Lime and Limestone Chemistry and Technology Production and Uses by J.A.H. Oates     3. Lime and Limestone Chemistry and Technology Production and Uses by J.A.H. Oates 4. LANGE’S HANDBOOK OF CHEMISTRY-McGraw-Hill Book Company     4. LANGE'S HANDBOOK OF CHEMISTRY-McGraw-Hill Book Company 5. 鑛産物の智識と取引-工業用鑛物編-吉田國夫 著     5. Knowledge and Transaction of Products - Industrial Products - Yoshida Kunioo

원료의 안정조달과 경제성 확보 및 종래기술의 문제점등을 개선 하기 위해 백운석등 마그네슘 및 칼슘성분 혼합광물을 염산에 용해하여 CaCl2와 MgCl2 혼합용액을 제조 하고 이 혼합용액을 물리적 특성을 상이하게 변환하여 성분을 분리하는 방안을 고안 하고 저 한다. In order to improve the stability of raw materials, to secure economical efficiency, and to solve the problems of the prior art, dolomite and other magnesium and calcium mixed minerals were dissolved in hydrochloric acid and CaCl 2 and MgCl 2 A method of preparing a mixed solution and separating the components by converting the mixed solution into different physical properties is devised and reduced.

백운석등 마그네슘 및 칼슘성분 혼합광물을 파쇄 및 분쇄한 원광석 소괴 또는 경 소성용으로 체별하는 30mmØ 원석 또는 경소백운회의 미수화 잔유물등을 염산에 용해하면 CaCl2, MgCl2 및 물이 생성되는 반응으로 염산용해액(MgCl2+CaCl2 혼성 용액)을 만들고 용액상태에서 불순물을 정제하고 소석회 Ca(OH)2 를 기질로 하여 Mg(OH)2 와 염화칼슘(CaCl2)으로 분리하는 방법을 고안하였다. 백운석 염산용해와 소석회 기질반응식은 다음과 같다.Dolomite and other magnesium and calcium mixed minerals are crushed and pulverized. When 30mm Ø gemstones or unirradiated remnants are separated into hydrochloric acid, CaCl 2 , MgCl 2 and water are produced, hydrochloric acid The solution (MgCl 2 + CaCl 2 (OH) 2 and calcium chloride (CaCl 2 ) were prepared from the calcium hydroxide (Ca (OH) 2 ) as a substrate. The decomposition of dolomite hydrochloric acid and slaked lime matrix is as follows.

백운석 염산용해반응식 : Ca.Mg(CO3)2+4HCl → MgCl 2 + CaCl 2 +2CO2↑+2H2ODolomite hydrochloric acid dissolution reaction formula: Ca.Mg (CO 3 ) 2 + 4HCl → MgCl 2 + CaCl 2 + 2CO 2 ↑ + 2H 2 O

반응성 G에너지 △Gf = -517.14x31.37→-171.4178.82x94.262x56.69     Reactive G energy? Gf = -517.14x31.37? -171.4178.82x94.262x56.69

= -642.58 → -652.10 = -9.52 < 0 정반응                          = -642.58 - &gt; -652.10 = -9.52 &lt;

소석회 염산용해액반응 : MgCl 2 + CaCl 2 + Ca(OH)2 Mg(OH) 2 + 2CaCl 2 Calcium hydroxide hydrochloric acid solution Reaction: MgCl 2 + CaCl 2 + Ca (OH) 2 Mg (OH) 2 + 2CaCl 2

반응성 G에너지 △Gf = -141.52-178.80-214.75 → -199.30-2x178.80      Reactive G energy? Gf = -141.52-178.80-214.75? -199.30-2x178.80

= -535.07 → -556.90 = -21.83 < 0 정반응                           = -535.07 → -556.90 = -21.83 <0

염산용해액에 함유되어 있는 Fe2 +~3+, Mn2 +, Al2 +등의 불순물을 제거하기 위해 산화제 로 H2O2,를 적가교반하고 Ca(OH)2를 PH2.7~6.5(7.5) 까지 적가중화여 아래의 침전 생성 PH범위로 조정하여 정치 후 Fe, Mn, Al등 이 금속수산화물로 침전되면 이를 여과 정제한다.Fe 2 contained in the hydrochloric acid solution was + ~ 3 +, Mn 2 + , Al 2 + in order to remove impurities such as stirring is added dropwise a H 2 O 2, with an oxidizing agent and the PH2.7 Ca (OH) 2 ~ 6.5 (7.5). Adjust the pH to the range of precipitate formation PH below, and after the precipitation of Fe, Mn, Al, etc. as metal hydroxide, filter and purify it.

반응식 = Fe(OH)2 + MnO2 + O2 + xH2O → Fe(OH)3↓+MnO4Scheme = Fe (OH) 2 + MnO 2 + O 2 + xH 2 O? Fe (OH) 3 ↓ + MnO 4

금속원소별 수산화물의 침전생성 Precipitation of hydroxides by metal elements PHPH 범위(이론치) Range (theoretical) 원소 element PHPH 원소 element PHPH 원소 element PH PH 원소 element PH PH FeFe 22 ++ 7.5~7.5 ~ MnMn 22 ++ 8.0~8.0 ~ PbPb 22 ++ 7.5~13.0 7.5 to 13.0 CuCu 22 ++ 6.0~ 6.0 ~ FeFe 33 ++ 2.7~2.7 ~ MnMn 44 + + 2.7~2.7 ~ AlAl 33 ++ 3.7~103.7 to 10 CrCr 33 ++ 4.7~4.7 ~

단 : Cu,               However, Cr은Cr KOH, NaOH에 반응되며 기타금속은  KOH, NaOH, and other metals Ca(OH)2Ca (OH) 2

상기 2Mg(OH)2↓를 Filter Press로 탈수분리하면 Cake는 Mg(OH)2↓이며 여과액은 CaCl2용액이다. Cake에 약40% 잔류되어 Cake를 충분한 물로 분산희석 하여 잔류 CaCl2 용액을 재 탈수하면 Mg(OH)2 순도 약96%로 분리된다.When 2Mg (OH) 2 ↓ is dehydrated by filter press, Cake is Mg (OH) 2 ↓ and the filtrate is CaCl 2 solution. Cake is about 40% and the cake is dispersed with sufficient water to rehydrate the residual CaCl 2 solution, and the purity of Mg (OH) 2 is about 96%.

Cake를 분산희석 할 때 분산제로 메타인산소다등을 약0.1~10 중량부 첨가하여 신속 한 분산과 탈수효율을 증대시킨다. 탈수용액은 CaCl2로 농도 22~38%로 조정하여 제설제 및 Polymer 응고제, 방진제 용도의 액상염화칼슘으로 제조하며 분무식등 건조하여 식품용, 방습제용의 분말염화칼슘을 제조한다. When dispersing cakes, 0.1 to 10 parts by weight of sodium metaphosphate is added as a dispersant to increase the rapid dispersion and dehydration efficiency. The dehydrated solution is adjusted to a concentration of 22 ~ 38% with CaCl 2 , and is made into liquid calcium chloride for use as a snow remover, a polymer coagulant, and a dustproofing agent, and dried by spraying to produce powdered calcium chloride for food and desiccant.

염화칼슘은 흡습성과 부식성이 강함으로 상기 분말염화칼슘에 방습기능을 부여하기 위해 Agar, 지방산, 수지산, Steralic 산 중에서 하나이상을 선택하여 열수에 용해 하여 표면을 코팅하며     Since calcium chloride is highly hygroscopic and highly corrosive, at least one of agar, fatty acid, resin acid, and Steralic acid is selected and dissolved in hot water to coat the surface to impart the moisture proof function to the powdered calcium chloride

부식방지제로 Alcohol, Urea[CO(NH2)2), Sodium Nitrite(NaNO2)등에서 하나 이상을 선택하여 1~5부 첨가하면 부식성이 현저히 개선된다.Corrosion resistance is significantly improved by adding 1 to 5 parts of at least one selected from Alcohols, Urea [CO (NH 2 ) 2 ) and Sodium Nitrite (NaNO 2 ) as corrosion inhibitors.

본 발명으로 마그네슘 화합물의 주원료 광물인 Magensite 부존이 없어도 백운석으로 수산화마그네슘을 제조하여 마그네슘화합물 25여종의 기초소재로 활용할 수 있다.     According to the present invention, magnesium hydroxide can be prepared from dolomite and used as a base material for 25 kinds of magnesium compounds even if there is no magensite present as a main mineral of the magnesium compound.

또한 완제품화 되는 공정부산물 액상염화칼슘을 건조하고 표면코팅 제품화하여 경제성을 배가하게 된다.    In addition, the process by-product liquid calcium chloride, which is a finished product, is dried and surface-coated, thereby doubling the economic efficiency.

본 발명의 주요공정을 다음의 실험예와 같이 시험하였으며 본 실험예는 공정 설명과 공정 확인을 위한 실험이며 발명의 범위를 제한하는 것은 아니다.    The main process of the present invention was tested as in the following Experimental Example. This Experimental Example is an experiment for process description and process confirmation, and does not limit the scope of the invention.

본 발명을 다음의 실험예를 참조하여 상세히 설명하면 다음과 같다.     The present invention will be described in detail with reference to the following experimental examples.

([실험예 1]) 백운석원석 염산용해 시험   ([Experimental Example 1]) Dolomite gemstone hydrochloric acid dissolution test

백운석을 염산에 용해하는 실험을 다음과 같이 실시하고 본 발명의 제1기질로 활용하는데 적합한 소재임이 확인되었다.    The experiment for dissolving dolomite in hydrochloric acid was carried out as follows and it was confirmed that it is a suitable material for utilization as the first substrate of the present invention.

용해시험 종합표 및 용해비율Comprehensive table of dissolution test and dissolution ratio 염산용해         Hydrochloric acid dissolution 용해액/용해율        Solution / dissolution rate 비고 Remarks 백운석dolomite 염산량 Amount of hydrochloric acid 합계 Sum 용액 solution 잔석 Zeolite 합계 Sum 용해%Dissolution% 2.000gr2.000 gr 1,000gr1,000gr 3,000gr3,000 gr 1,114gr1,114 gr 1,688gr1,688gr 2,802gr2,802 gr 15.60%15.60% 1,688gr1,688gr 1,000gr1,000gr 2,688gr2,688gr 1,298gr1,298gr 1,212gr1,212gr 2,510gr2,510 gr 28.20%28.20% 1,212gr1,212gr 1,000gr1,000gr 2,212gr2,212gr 1,266gr1,266gr 754gr 754gr 2,020gr2,020gr 37.79%37.79% 754gr754gr 1,000gr1,000gr 1,754gr1,754 gr 1,268gr1,268 gr 312gr312gr 1,580gr1,580gr 58.62%58.62% 2,000gr2,000 gr 4,000gr4,000 gr 6,000gr6,000 gr 4,946gr4,946gr 312gr312gr 5,258gr5,258 gr 84.40%84.40% PH4.15PH4.15

용해고찰 : 입자가 미세할수록 용해속도 빠르며 PH 1.7정도에서 완속 용해됨 장시간 염산에 답가 두면 PH4.15에서 용해 종료됨 Dissolution considerations: As the particles become finer, the dissolution rate is faster and the dissolution rate is slower at about pH 1.7.

여과액농도 : 42.43%             Filtrate concentration: 42.43%

([실험예 2]) 여과용액 정제시험  ([Experimental Example 2]) Filtration solution purification test

1) 원석을 용액에 소량넣고 1야 정치 후 Fe2 ~3+ Layer 생성되었으며 투명성이 개선된 용액이 되었음. 1) A small amount of ore was put into the solution, and Fe 2 ~ 3 + Layer was formed after 1 night, and the solution was improved in transparency.

2) 여과액에 35% H2O2를 적가 교반하고 소석회를 첨가하며 PH를 3.0으로 조정하여 1시간 정치 후 적갈색 침전물(Fe2 ~3+ 산화침전물) 침전되며 상등액 투명화되었음.2) 35% H 2 O 2 was added dropwise to the filtrate, and slaked lime was added to adjust pH to 3.0. After standing for 1 hour, a reddish brown precipitate (Fe 2 ~ 3 + oxidized precipitate) was precipitated and the supernatant liquidified.

Fe2 ~3+, Fe(OH)2, MnO2, + O2 + H2O → Fe(OH)3↓, MnO4↓Fe 2 + 3 + , Fe (OH) 2, MnO 2, + O 2 + H 2 O -> Fe

3) 여과액에 35% H2O2 대신 KOH/NaOH PH3.0 으로 적가하여도 Fe2 ~ 3+ → Fe(OH)3↓적갈색 산화침전물 전되며 상등액 투명화 되었음. 3) To the filtrate was added 35% H 2 O 2 Instead, Fe 2 ~ 3+ → Fe (OH) 3 ↓ reddish brown oxidized precipitate was transferred even when added dropwise with KOH / NaOH PH 3.0, and the supernatant became transparent.

4) 여과액에 NH4OH + NH4Cl 적가하며 PH를 3.0으로 조정하여 Al(OH)3↓, MnO4↓적갈색 산화침전물 침전되며 상등액 투명화 되었음.4) NH4OH + NH4Cl was added dropwise to the filtrate, and the pH was adjusted to 3.0 to precipitate Al (OH) 3 and MnO 4 ↓ reddish brown oxidized precipitates. The supernatant was clarified.

([실험예 3]) 경소성백운회 염산용해 시험([Experimental Example 3]) Hardened white lye hydrochloric acid dissolution test

경소성백운회를 염산에 용해시험결과 유기유색물등이 소성시 소각되어 염산용해액은 여과없이 백운석 용해액 2회 여과액과 동등한 Clear 용액임이 확인되었 으며 용해 종말점은 PH2.45로 백운석 PH4.15에 비해 강산성에서 종료되었으나 여과 공정없이 사용 가능함이 확인되었음. 약간의 카본 부유물이 있으나 소석회 반응 물로 여과공정 없이 사용가능하다고 판단되었음.    It was confirmed that the solution of hydrochloric acid dissolved in hydrochloric acid was the clear solution equivalent to the filtrate of dolomite solution twice without filtration. The end point of dissolution was PH2.45 and dolomite PH4.15 , It was confirmed that it can be used without filtration process. It is judged that it can be used without filtration process in the slaked lime reactant although there is some carbon suspended matter.

용해액의 농도 : 56.03% = CaCl2 30.16% + MgCl2 25.87% Concentration of solution: 56.03% = CaCl 2 30.16% + MgCl 2 25.87%

([실험예 4]) 여과여액 건조시험([Experimental Example 4]) Filtration filtrate Drying test

실험예 2에서 1차탈수 여액1kg을 분취하여 전기건조기에서 130℃로 건조하여 분말염화칼슘 424g이 석 출되어 고백색의 염화칼슘을 생성되었음.      In Experimental Example 2, 1 kg of the primary dehydrated filtrate was collected and dried in an electric drier at 130 ° C. to produce 424 g of powdered calcium chloride, which produced a clear white calcium chloride.

제작된 염화칼슘은 신속하게 유발로 분쇄하고 한천(Agar)15g을 10배의 열수에 용해 하여 분무식으로 분사하여 표면 처리를 하고 다시 건조하여 1시간 동안 방치하여도 흡습하여 Gel 상으로 변하지 않고 분말 상으로 유지되었다.     The prepared calcium chloride was pulverized rapidly and agar (15 g) was dissolved in 10 times of hot water, sprayed in a spraying manner, treated with surface, dried again after being left for 1 hour to absorb moisture, Respectively.

([실험예 5]) 여과수산화마그네슘 Cake분산시험([Experimental Example 5]) Filtration Magnesium hydroxide Cake dispersion test

제2항의 수산화마그네슘을 Filter Press로 여과 고형물 Cake는 수분이 48.50%인 단단한 Cake 12kg을 고형분 농도를 10%로 분산하기 위하여 물 49.8kg에 메타인산소다 약 4부량 250g을 용해하여 Cake에 적가하며 분산기로 분산하여 고형분 농도 10%의 수산화마그네슘 Slurry로 30분에 분산하였다.      The magnesium hydroxide of claim 2 is filtered with a filter press. Cake is a solid cake having 48.50% water content. To disperse the solid content to 10%, 250 g of sodium methaphosphate is added to 49.8 kg of water and added dropwise to the cake. And dispersed in a magnesium hydroxide slurry having a solid content concentration of 10% for 30 minutes.

([실험예 6]) 재탈수시험([Experimental Example 6]) Rehydration test

실험예 4의 분산 Slurry를 Filter Press에서 8kg/cm2 공기압으로 재탈수하고 Cake와 여액을 분석하 고 그결과는 다음과 같다.      The dispersed slurry of Experimental Example 4 was re-dewatered to 8 kg / cm2 air pressure by a filter press, and the cake and filtrate were analyzed. The results are as follows.

Cake 수분 : 48.70%(고형분 51.30%)                Cake moisture: 48.70% (solid content 51.30%)

Mg(OH)2함량 : 94.22%(Ca화합물 성분 5.62%)Mg (OH) 2 content: 94.22% (Ca compound component: 5.62%)

여액증발시험 : 고형 염화칼슘 0.55%                Filtrate Evaporation test: solid calcium chloride 0.55%

Claims (1)

백운석등 마그네슘과 칼슘성분이 혼합되는 광물을 염산에 용해하여 염화칼슘과 염화마그네슘 혼성
염화물용액 을 만드는 단계;
상기 염화물용액 에 백운석을 용액에 넣고 정치하여 더 용해하고 숙성하여 PH를 낯추는 단계;

상기 염화물용액 에 산화제로 과산화수소(H2O2)를 첨가하고 수산화물을 첨가하여 PH를 2.0이상 조정하 여 Fe2~3+, Mn2+, Mn2+, Al2+등 불순물을 수산화물로 만들어 침전 시키고 여과 분리하여 정제하는 단계;
상기 마그네슘성분을 함유하는 광물은 백운석, Magnesite, Brucite, Huntite, 경소 백운회, 경소백 운회 미수화잔유물등에서 하나이상을 선택하는 것;
상기 수산화물은 Ca(OH)2, NaOH, KOH중에서 하나이상을 선택하는 것;
[청구항 2]
제1항의 염화물용액에 소석회[Ca(OH)2]를 기질로 첨가 반응하여 고형물 수산화 마그네슘[Mg(OH)2]과 수용물 염화칼슘(CaCl2)으로 물리적 특성을 다르게하여 여과 탈수하여 수산화마그네슘과 염화칼슘을 고액으로 성분을 분리하는 단계;
상기 분리된 고형수산화마그네슘에 분산제 를 0.1부~10부 첨가하여 분산을 용이 하게 하고 물로 희석 분산하고 재 탈수방법으로 수세를 반복하여 분리 수산화 마그네슘의 순도를 높이는 단계;
상기 수산화마그네슘을 습식마쇄하고 체 별하여 입자응집을 해쇄하여 고반응성 액상 수산화마그네슘 을 제조하는 단계;
상기 고반응성 액상수산화마그네슘을 탈수, 건조, 해쇄하여 고반응성 분말상 수산화 마그네슘을 제 조하는 단계;
상기 수산화마그네슘을 지방산, 수지산, Silane Coupling Agent, Stearic산으로 습식 또는 건식으로 표면을 코팅하여 표면처리 수산화마그네슘을 제조하는 단계;
상기 분산제는 메타인산소다, 아라비아검등의 천연검류, 대두다당류, PGA, 레시친, Vitamin-D등에서 하나 이상으로 선택하는 분산제인 것을 특징으로 하는 것.
[청구항 3]
상기 제2항의 수산화마그네슘을 700℃ 이상 가열하여 물과 가스를 기화시켜 분말의 산화마그네슘 MgO 를 제조하는 단계;
[청구항 4]
제2항의 여과용액인 염화칼슘용액을 농도 조정하여 액상염화칼슘을 제조하는 단계;
상기 염화칼슘용액에 부식방지제를 첨가하여 부식성 저감 염화칼슘 제조단계;
상기 액상염화칼슘을 분무식 건조하여 분말 염화칼슘을 제조하는 단계;
상기 분말염화칼슘에 방습기능을 부여하기 위해 Agar, 지방산, 수지산, Steralic 산 중에서 하나이상 을 선택하여 열수에 용해하여 표면을 코팅하는 단계;
상기 부식방지제는 Alcohol, Urea[CO(NH2)2), Sodium Nitrite(NaNO2)등에서 하나 이상을 선택하는 것
Dolomite and other minerals in which magnesium and calcium components are mixed is dissolved in hydrochloric acid to prepare a mixture of calcium chloride and magnesium chloride
Making a chloride solution ;
Adding dolomite to the chloride solution , allowing the solution to stand, dissolving it, and aging to dissolve the PH;

Hydrogen peroxide (H 2 O 2 ) is added as an oxidizing agent to the chloride solution , and hydroxide is added to adjust pH to 2.0 or more to make impurities such as Fe 2 to 3+ , Mn 2+ , Mn 2+ and Al 2+ into hydroxide Precipitating and purifying by filtration;
The mineral containing the magnesium component may be at least one selected from dolomite, magnesite, brucite, huntite, light whitewash, light unbleached unfinished remnants, and the like;
The hydroxide is selected from the group consisting of Ca (OH) 2 , NaOH, and KOH;
[Claim 2]
The calcium chloride solution of claim 1 is added and reacted with calcium hydroxide [Ca (OH) 2 ] as a substrate to separate the magnesium hydroxide [Mg (OH) 2 ] and the aqueous calcium chloride (CaCl 2 ) Separating the components of calcium chloride into a high liquid;
Adding 0.1 to 10 parts of a dispersing agent to the separated solid magnesium hydroxide so as to facilitate dispersion, diluting and dispersing the mixture with water, and repeating water washing by a rehydration method to increase the purity of the separated magnesium hydroxide;
Subjecting the magnesium hydroxide to wet grinding and crushing the particle agglomeration to prepare a highly reactive liquid magnesium hydroxide;
Drying the magnesium hydroxide to prepare a highly reactive powdery magnesium hydroxide;
Preparing surface-treated magnesium hydroxide by coating the surface of the magnesium hydroxide with a fatty acid, a resinous acid, a silane coupling agent, or a stearic acid in a wet or dry manner;
Characterized in that the dispersant is at least one dispersant selected from natural gums such as sodium metaphosphate, gum arabic, soybean polysaccharide, PGA, lecithin and Vitamin-D.
[Claim 3]
Heating the magnesium hydroxide of claim 2 above 700 ° C to vaporize water and gas to produce magnesium oxide MgO powder;
[Claim 4]
Adjusting the concentration of the calcium chloride solution as the filtration solution of claim 2 to produce liquid calcium chloride;
Adding a corrosion inhibitor to the calcium chloride solution to prepare a corrosive reducing calcium chloride;
Drying the liquid calcium chloride by spray drying to prepare powdered calcium chloride;
Selecting at least one of agar, fatty acid, resin acid, and Steralic acid so as to impart a moisture-proof function to the powdery calcium chloride, and dissolving it in hot water to coat the surface;
The corrosion inhibitor may be at least one selected from Alcohols, Urea [CO (NH 2 ) 2 ), Sodium Nitrite (NaNO 2 )
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CN108314334A (en) * 2017-01-17 2018-07-24 中国科学院过程工程研究所 A method of producing high-purity magnesium oxide by raw material of magnesite
CN109535482A (en) * 2018-11-12 2019-03-29 大连亚泰科技新材料股份有限公司 A kind of no resin, nano flame retardant masterbatch of binder free and preparation method thereof
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