KR100373561B1 - Magnesia powder and its manufacturing method - Google Patents

Magnesia powder and its manufacturing method Download PDF

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KR100373561B1
KR100373561B1 KR1019950016956A KR19950016956A KR100373561B1 KR 100373561 B1 KR100373561 B1 KR 100373561B1 KR 1019950016956 A KR1019950016956 A KR 1019950016956A KR 19950016956 A KR19950016956 A KR 19950016956A KR 100373561 B1 KR100373561 B1 KR 100373561B1
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magnesia
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가네야스아끼라
야마모또신이찌
다까사끼가오루
다께우찌가쯔미
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우베 마테리알즈 가부시키가이샤
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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
    • C01F5/02Magnesia
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    • 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
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/03Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on magnesium oxide, calcium oxide or oxide mixtures derived from dolomite
    • C04B35/04Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on magnesium oxide, calcium oxide or oxide mixtures derived from dolomite based on magnesium oxide
    • C04B35/043Refractories from grain sized mixtures
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    • 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
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/62605Treating the starting powders individually or as mixtures
    • C04B35/6261Milling
    • C04B35/62615High energy or reactive ball milling
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    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
    • C04B35/632Organic additives
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    • 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
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/66Monolithic refractories or refractory mortars, including those whether or not containing clay
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    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/61Micrometer sized, i.e. from 1-100 micrometer
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    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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    • C01P2006/12Surface area
    • 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
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/34Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3418Silicon oxide, silicic acids, or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint

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  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
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Abstract

MgO 함유량이 90 중량 % 이상, 비표면적이 5 m2/g 이하, 평균 입경이 50 ㎛ 이하이고 학진법 4 (마그네시아 클링커의 소화성 시험방법) 에 의한 중량 증가율이 2.0 중량 % 이하인 마그네시아 분말.Magnesia powder with MgO content of 90 weight% or more, specific surface area of 5 m <2> / g or less, average particle diameter of 50 micrometers or less, and the weight increase rate by the Hakjin method 4 (method of digestibility test of magnesia clinker) of 2.0 weight% or less.

이 마그네시아 분말은 MgO 함유량이 98 중량 % 이상, 비표면적이 5 m2/g 이하, 그리고 평균 입경이 50 ㎛ 이하인 마그네시아 원료 분말과 유기 규소 화합물의 혼합물을 준비하고, 이 혼합물을 350 ∼ 600℃ 의 범위의 온도에서 가열함으로써 제조된다.This magnesia powder was prepared with a mixture of magnesia raw material powder and organosilicon compound having a MgO content of 98% by weight or more, a specific surface area of 5 m 2 / g or less, and an average particle diameter of 50 μm or less, and the mixture was prepared at 350 to 600 ° C. It is prepared by heating at a temperature in the range.

Description

마그네시아 분말 및 그의 제조방법Magnesia powder and preparation method thereof

본 발명은 마그네시아 분말 및 그의 제조방법에 관한 것이다. 더 상세하게는 내소화성(耐消化性) 을 필요로하는 염기성 정형노재 및 부정형 내화물의 원료로서 적합하게 사용할 수 있는 마그네시아 분말 및 그의 제조방법에 관한 것이다.The present invention relates to a magnesia powder and a preparation method thereof. More specifically, the present invention relates to a magnesia powder which can be suitably used as a raw material for basic form-furnished materials and amorphous form refractory materials requiring fire resistance and a method for producing the same.

제강용 부정형 내화물 재료인 염기성 분무재 및 유입재는 근래 첨가수분을 저감하고 재료밀도의 향상, 고온물성의 향상을 도모하는 것이 검토되고 있다.Basic spray materials and inflow materials, which are amorphous refractory materials for steel making, have recently been studied to reduce added moisture, improve material density, and improve high temperature properties.

수분 저감에 수반하여 재료의 유동성도 저하하기 때문에 기재의 마그네시아 원료에 관해서도 입도 배합을 변경하고 미세분말의 비율을 증가시킬 필요가 생겼다.Since the fluidity of the material decreases with the decrease of moisture, it is necessary to change the particle size formulation and increase the proportion of the fine powder also for the magnesia raw material of the substrate.

그러나 마그네시아 원료의 주요 구성광물인 페리클레이스가 공기중의 수증기와 반응하여 소화하는 결점을 갖고 있으며 특히 비표면적이 큰 미세분말에서는 이 경향이 보다 현저하게 나타난다. 이때문에 기존의 마그네시아 클링커를 분쇄한 마그네시아 미분말은 내소화성이 극단적으로 나쁘고 사용할 수 있는 수준은 아니었다.However, Pericles, a major component mineral of magnesia, has the disadvantage of reacting and extinguishing with water vapor in the air, especially in fine powders with large specific surface area. For this reason, the magnesia fine powder obtained by crushing the existing magnesia clinker was extremely poor in fire resistance and was not usable.

그래서 마그네시아 분말의 내소화성을 개선하기 위하여 마그네시아 분말에실란 등의 무기계 커플링제에 의한 표면처리를 실시하는 방법이 이미 제안되어 있다. 그러나 이 방법으로도 내소화성은 실용적인 수준으로는 이르지 않았다. 또 표면 처리후의 마그네시아 분말은 현저한 발수성이 인정되고 수계의 부정형 내화물 원료로서는 친밀성이 나쁘고 사용하기가 어려운 결점이 있었다.Therefore, in order to improve the fire resistance of magnesia powder, the method of surface-treating with inorganic coupling agents, such as silane, to magnesia powder is already proposed. However, even with this method, fire resistance did not reach a practical level. Moreover, the magnesia powder after surface treatment recognized the remarkable water repellency, and had the fault that it was bad in intimacy and difficult to use as an aqueous amorphous refractory raw material.

일본국 특공소 62-288114 호 공보에는 마그네시아 입자 표면상에서 유기 실리케이트화합물을 열분해 및/또는 가수분해시켜서 분말 입자표면이 연속적으로 균일한 실리카 피막으로 피복된 내수화성 마그네시아 분말이 얻어지는 것이 개시되어 있다.Japanese Patent Application Laid-Open No. 62-288114 discloses pyrolysis and / or hydrolysis of an organic silicate compound on a surface of magnesia particles to obtain a water-resistant magnesia powder whose surface surface is continuously coated with a uniform silica coating.

일본국 특개소 63-45117 호 공보에는 금속 마그네시아 분말의 가열 증기를 기상산화하여 얻어진 마그네시아 분말의 입자표면에 알콕시 실란을 열분해 하여 실리카 피막을 형성하고 내수화성 마그네시아 분말이 얻어진다는 것이 개시되어 있다.Japanese Laid-Open Patent Publication No. 63-45117 discloses that alkoxy silane is thermally decomposed on the particle surface of magnesia powder obtained by gas phase oxidation of heated vapor of metal magnesia powder to form a silica film to obtain a water-resistant magnesia powder.

상기 2 건의 공개공보에는 내소화성이 고도로 뛰어난 마그네시아 분말 및 그의 제조방법에 관해서는 하등 기재되어 있지 않다.The two publications do not describe any magnesia powder having excellent fire resistance and a method for producing the same.

또 일본국 특개평 4-42808 호 공보에는 마그네시아 분말을 1100℃ 이상으로 가열함으로써 내소화성을 개선하는 방법이 제안되어 있다. 그러나 이 방법으로도 내소화성은 실용적인 수준에 이르러있지 않다.In addition, Japanese Patent Laid-Open No. 4-42808 proposes a method for improving fire resistance by heating magnesia powder to 1100 ° C or more. But even with this method, fire resistance is not at a practical level.

이때문에 부정형 내화물의 고품위화를 위해서는 부정형 내화물의 원료인 마그네시아 분말의 소화 반응을 더욱 억제하여 내소화성을 학진법 4 (마그네시아 클링커의 소화성 시험방법) 에 의한 중량 증가율이 2.0 % 이하로 까지 대폭 향상시키고, 아울러 발수성이 적고 또한 유동성이 뛰어난 원료의 개발이 과제였다.For this reason, in order to improve the quality of amorphous refractory materials, the digestion reaction of magnesia powder, which is a raw material of amorphous refractory materials, is further suppressed, and the fire resistance is greatly improved to 2.0% or less by weight of Hakjin method 4 (test method for digestibility of magnesia clinker). In addition, the development of a raw material having low water repellency and excellent fluidity was a problem.

그때문에 본 발명의 목적은 내소화성이 고도로 뛰어난 마그네시아 분말을 제공하는데 있다.Therefore, an object of the present invention is to provide a magnesia powder having high fire resistance.

본 발명의 다른 목적은 발수성이 적고 물과 친밀하기 쉽고 또한 유동성이 뛰어나고 유입재료로서 사용하기 쉬운 마그네시아 분말을 제공하는데 있다.Another object of the present invention is to provide a magnesia powder having low water repellency, easy intimacy with water, excellent flowability and easy use as an inflow material.

본 발명의 또다른 목적은 본 발명의 상기 마그네시아 분말을 공업적으로 유리하게 또한 값싸게 제조하는 방법을 제공하는데 있다.It is a further object of the present invention to provide a process for industrially advantageously and inexpensively producing the magnesia powder of the present invention.

본 발명의 또다른 목적 및 이점은 이하의 설명에서 명백해질 것이다.Still other objects and advantages of the present invention will become apparent from the following description.

본 발명에 의하면 본 발명의 상기 목적 및 이점은 첫째로 MgO 함유량이 90 중량 % 이상, 비표면적이 5 m2/g 이하, 평균 입경이 50 ㎛ 이하, 그리고 학진법 4 (마그네시아클링커의 소화성 시험방법)에 의한 중량 증가율이 2.0 중량 % 이하인 것을 특징으로 하는 마그네시아 분말에 의해서 달성된다.According to the present invention, the above objects and advantages of the present invention are firstly MgO content of 90% by weight or more, specific surface area of 5 m 2 / g or less, average particle size of 50 μm or less, and Hakjin Method 4 (Method of Digestibility of Magnesia Clinker) It is achieved by the magnesia powder, characterized in that the weight increase rate by) is 2.0% by weight or less.

본 발명에 의하면 본 발명의 상기 마그네시아분말은 바람직하기는 MgO 함유량이 98 중량 % 이상, 비표면적이 5 m2/g 이하 그리고 평균 입경이 50 ㎛ 이하인 마그네시아 원료 분말과 유기 규소 화합물의 혼합물을 준비하고, 이 혼합물을 350 ∼ 600℃ 의 범위의 온도에서 가열함으로써 달성된다.According to the present invention, the magnesia powder of the present invention preferably has a mixture of magnesia raw material powder and organosilicon compound having a MgO content of 98% by weight or more, a specific surface area of 5 m 2 / g or less and an average particle diameter of 50 μm or less. And this mixture is achieved by heating at the temperature of 350-600 degreeC.

출발 원료인 MgO 함유량 98 중량 % 이상, 비표면적 5 m2/g 이하, 평균 입경 50 ㎛ 이하의 마그네시아 분말로서는 1800℃ 이상의 온도로 소성하여 수득되는 이른바 고온 소성 마그네시아 클링커 분말을 분쇄하여 정립한 것이 바람직하게 사용된다.Magnesium powder having a MgO content of 98% by weight or more, a specific surface area of 5 m 2 / g or less, and an average particle diameter of 50 μm or less is preferably a powder obtained by pulverizing the so-called high-temperature calcined magnesia clinker powder obtained by firing at a temperature of 1800 ° C or more. Is used.

유기 규소 화합물로서는 실란커플링제, 알콕시실란, 실리콘, 실릴화제 등이 바람직하게 사용된다. 실란커플링제로서는 예킨대 비닐트리클로로실란, 비닐트리에톡시실란, 비닐트리메톡시실란, 비닐트리스 (β- 메톡시에톡시) 실란,- (메타크릴록시프로필) 트리메톡시실란,- 아미노프로필트리에톡시실란,- 메르캅토프로필트리메톡시실란 등을 들 수 있다. 알콕시실란으로서는 예컨대 테트라에톡시실란, 테트라메톡시실란, 메틸트리에톡시실란 등을 들수 있다. 실리콘으로서는 예컨대 메틸수소실리콘오일, 디메틸실리콘 오일 등을 들 수 있다. 또 실릴화제로서는 예컨대 트리메틸클로로실란, 헥사메틸디실라잔 등을 들 수 있다.As an organosilicon compound, a silane coupling agent, an alkoxysilane, silicone, a silylating agent, etc. are used preferably. Examples of the silane coupling agent include Yekindae vinyltrichlorosilane, vinyltriethoxysilane, vinyltrimethoxysilane, vinyltris (β-methoxyethoxy) silane, -(Methacryloxypropyl) trimethoxysilane, Aminopropyltriethoxysilane, Mercaptopropyl trimethoxysilane, and the like. As an alkoxysilane, tetraethoxysilane, tetramethoxysilane, methyl triethoxysilane, etc. are mentioned, for example. As silicone, methyl hydrogen silicone oil, dimethyl silicone oil, etc. are mentioned, for example. Examples of the silylating agent include trimethylchlorosilane and hexamethyldisilazane.

마그네시아 원료 분말에 대한 유기 규소 화합물의 첨가량은 통상 0.2 ∼ 10.0 중량 %, 바람직하기는 0.5 ∼ 3.0 중량 % 이다. 첨가량이 0.2 중량 % 보다도 적으면 내소화성의 향상효과를 인정할 수 없고, 또 10.0 중량 % 보다 많이 하여도 많이한 것에 의한 효과는 없고 경제적이 아니다.The amount of the organosilicon compound added to the magnesia raw material powder is usually 0.2 to 10.0% by weight, preferably 0.5 to 3.0% by weight. When the addition amount is less than 0.2% by weight, the effect of improving fire resistance cannot be recognized, and even when it is more than 10.0% by weight, the effect is not large and is not economical.

본 발명에 있어서는 마그네시아 원료 분말에 유기규소 화합물을 첨가한 후, 350 ∼ 600℃, 바람직하기는 400 ∼ 550℃ 에서 가열처리한다. 가열처리의 온도가 350℃ 미만에서는 내소화성의 향상이 충분치 않고, 또 수득된 생성물에 유기 규소 화합물의 첨가에 의한 발수성이 강해져서 바람직하지 않다. 또 600℃ 보다도 높으면 수득된 생성물의 내소화성이 크게 저하하므로 바람직하지 않다.In this invention, after adding an organosilicon compound to magnesia raw material powder, it heat-processes at 350-600 degreeC, Preferably it is 400-550 degreeC. When the temperature of heat processing is less than 350 degreeC, the improvement of fire resistance is not enough, and since the water repellency by addition of the organosilicon compound to the obtained product becomes strong, it is unpreferable. Moreover, when it is higher than 600 degreeC, since the fire resistance of the obtained product falls large, it is unpreferable.

가열용의 장치는 전기로 가스로 등의 각종의 공업로가 사용 가능하다.As for the apparatus for heating, various industrial furnaces, such as an electric furnace gas furnace, can be used.

본 발명에서는 유동층 반응기 등의 매우 특수한 가열 장치를 사용할 필요는없고 또한 헨셀믹서 등의 특수한 혼합 분산 장치를 사용할 필요도 없기 때문에 공정이 간단하며 용이하게 운전할 수 있고, 저비용으로 내소화성이 뛰어난 마그네시아 분말을 제조할 수가 있다.In the present invention, there is no need to use a very special heating device such as a fluidized bed reactor, and there is no need to use a special mixing and dispersing device such as Henschel mixer, so that the process is simple and easy to operate, and magnesia powder having excellent fire resistance at low cost is produced. It can manufacture.

본 발명의 마그네시아 분말은 MgO 함유량 90 중량 % 이상, 비표면적 5 m2/g 이하, 평균 입경 50 ㎛ 이하이다. 특히 내소화성의 면에서 1800℃ 이상의 온도에서 소성하여 수득되는 이른바 고온소성 마그네시아 클링커를 분쇄하여 수득되는 마그네시아 분말인 것이 바람직하다.The magnesia powder of this invention is 90 weight% or more of MgO content, 5 m <2> / g or less of specific surface area, and 50 micrometers or less of average particle diameters. In particular, the magnesia powder obtained by pulverizing the so-called high-temperature fired magnesia clinker obtained by firing at a temperature of 1800 ° C. or higher in terms of fire resistance is preferable.

또 내화물로한 경우의 특성면에서 불순물중의 CaO / SiO2의 중량비가 2 이상인 것이 바람직하다.Further it is preferred in terms of properties in the case where a refractory has a weight ratio of CaO / SiO 2 of not less than 2 of an impurity.

본 발명의 마그네시아 분말은 학진법 4 (마그네시아클링커의 소화성시험방법)에 의한 중량 중가율이 2.0 중량 % 이하, 특히 바람직하기는 1.0 중량 % 이하로 내소화성이 현저하게 향상되고 있다.The magnesia powder of the present invention has a markedly improved fire resistance of 2.0 weight% or less, particularly preferably 1.0 weight% or less, according to Hakjin Method 4 (Method of Digestibility Testing of Magnesia Clinker).

또 본 발명의 마그네시아 분말은 유동성이 뛰어나고 호소까와미크론제 파우더 시험기에 의한 유동성 지수가 60 이상, 바람직하기는 70 이상이다.Moreover, the magnesia powder of this invention is excellent in fluidity | liquidity, and the fluidity | liquidity index by the powder tester made from Hosokawa Micron is 60 or more, Preferably it is 70 or more.

본 발명의 마그네시아 분말은 내소화성이 뛰어난 성질을 가졌으며, 수계의 유입기재와의 친밀성도 양호하고, 분말의 유동성이 뛰어나기 때문에 정형, 부정형 내화물의 원료로서, 특히 염기성 유입 재료의 분말원료로서 극히 유용하다.The magnesia powder of the present invention has a property of excellent fire resistance, good intimacy with an aqueous inflow base and excellent flowability of the powder, making it a raw material for form and amorphous refractory materials, especially as a powder raw material for basic inflow materials. useful.

이하, 실시예 및 비교예로서 본 발명을 더 상세히 설명한다. 또한 내소화성의 평가는 학진법 4 (마그네시아클링커의 소화성 시험방법)에 따라서 실시하였다.또 분말의 유동성의 평가는 호소까와미크론제 파우더 시험기의 취급설명서의 『분체의 유동성 및 분류성의 수적 평가에 관하여』 에 따라서 실시하였다.Hereinafter, the present invention will be described in more detail as examples and comparative examples. The fire resistance was evaluated in accordance with Hakjin Method 4 (Method of Digestibility Test of Magnesia Clinker) .In addition, the fluidity test of the powder was carried out in the water dropping and fluidity evaluation of the powder tester of Hosokawa Micron Powder Tester. Pertaining to the present invention.

[실시예]EXAMPLE

[실시예 1]Example 1

광화제 (mineralizer)로서 SiO2를 1 중량 % 첨가하여 로터리 킬른으로 소성하는 MgO 함유량 98 중량 % 의 마그네시아 클링커를 볼밀로 분쇄하여 수득된 평균 입경 23 ㎛, 비표면적 1 m2/g 의 마그네시아 분말을 원료로 하고, 이것에 메틸수소실리콘 오일 1 중량 % 를 첨가한 후 실리코니토 전기로 내에서 400℃ 로 2 시간 유지하였다.Magnesium powder having an average particle size of 23 µm and a specific surface area of 1 m 2 / g obtained by grinding a MgO content 98% by weight magnesia clinker calcined into a rotary kiln by adding 1% by weight of SiO 2 as a mineralizer was fired in a rotary kiln. It was made into a raw material, and 1 weight% of methyl hydrogen silicone oils were added to this, and it hold | maintained at 400 degreeC in a silicon | silicone furnace for 2 hours.

수득된 마그네시아 분말의 내소화성은 중량 중가율 0.6 % 로 대폭적으로 향상되고, 아울러 발수성도 볼 수 없었다. 또 파우더 시험기에 의한 유동성 지수는 73 으로 상당히 양호하였다.The fire resistance of the obtained magnesia powder was greatly improved to 0.6% by weight weight ratio, and no water repellency was seen. The fluidity index by the powder tester was 73, which was quite good.

[실시예 2]Example 2

MgO 함유량 99.5 중량 % 의 마그네시아 클링커를 볼밀로 분쇄하여 수득된 평균 입경 26 ㎛, 비표면적 1 m2/g 의 마그네시아 분말을 원료로 하고, 이것에 메틸수소실리콘 오일 1 중량 % 를 첨가한 후, 실리코니토전기로 내에서 500℃ 에서 2 시간 유지하였다.Magnesium clinker with a MgO content of 99.5% by weight was obtained by grinding a ball mill with an average particle diameter of 26 µm and a magnesia powder with a specific surface area of 1 m 2 / g as raw materials, and after adding 1% by weight of methylhydrogen silicone oil thereto, silica It was maintained at 500 ° C. for 2 hours in a Nito electric furnace.

수득된 마그네시아 분말의 내소화성은 중량 증가율 0.5 % 로 대폭적으로 향상되고 아울러 발수성도 볼 수 없었다. 또 파우더 시험기에 의한 유동성 지수는 70으로 상당히 양호하였다.The fire resistance of the obtained magnesia powder was greatly improved at a weight increase rate of 0.5%, and no water repellency was seen. In addition, the fluidity index by the powder tester was quite good, 70.

[실시예 3]Example 3

광화제로서 SiO2를 1 중량 % 첨가하여 로터리킬른으로 소성한 MgO 함유량 98 중량 % 의 마그네시아클링커를 볼밀로 분쇄하여 수득된 평균입경 23 ㎛, 비표 면적 1 m2/g 의 마그네시아 분말을 원료로하고, 이것에 메틸수소 실리콘 오일 1 중량 % 를 첨가한 후, 레토르트가 200φ×10001 인 SUS 제의 외열 킬른으로 최고온도 550℃ 로 가열하였다.Magnesium clinker with 98% by weight of MgO content calcined in a rotary kiln with 1% by weight of SiO 2 as a mineralizer was milled with a ball mill, and magnesia powder having a specific particle size of 23 µm and a specific surface area of 1 m 2 / g was used as a raw material. After 1 weight% of methylhydrogen silicone oils were added to this, it heated with the maximum temperature of 550 degreeC by the external heat kiln made from SUS whose retort is 200 (phi) 1000000.

수득된 마그네시아 분말의 내소화성은 중량 증가율 0.7 % 로 대폭적으로 향상되고, 아울러 발수성도 볼 수 없었다. 또 파우더 시험기에 의한 유동성 지수는 72 로 상당히 양호 하였다.The fire resistance of the obtained magnesia powder was greatly improved at a weight increase rate of 0.7%, and no water repellency was seen. The fluidity index by the powder tester was 72, which was quite good.

[실시예 4]Example 4

광화제로서 SiO2를 1 중량 % 첨가하여 로터리 킬른으로 소성한 MgO 함유량 98 중량 % 의 마그네시아클링커를 볼밀로 분쇄하여 수득된 평균입경 23 ㎛, 비표면적 1 m2/g 의 마그네시아 분말을 원료로하고, 이것에 메틸수소실리콘 오일 1 중량 % 를 첨가한 후 실리코니토 전기로내에서 570℃ 에서 2 시간 유지하였다.Magnesium clinker with 98% by weight of MgO content calcined into a rotary kiln by adding 1% by weight of SiO 2 as a mineralizer was obtained by milling with a ball mill a magnesia powder with an average particle diameter of 23 µm and a specific surface area of 1 m 2 / g. After 1 weight% of methylhydrogen silicone oil was added to this, it was hold | maintained at 570 degreeC for 2 hours in the siliconito electric furnace.

수득된 마그네시아 분말의 내소화성은 중량 증가율 1.5 % 로 대폭적으로 향상되고 아울러 발수성도 볼 수 없었다. 또 파우더 시험기에 의한 유동성 지수는 63 으로 양호하였다.The fire resistance of the obtained magnesia powder was greatly improved at a weight increase rate of 1.5%, and no water repellency was seen. The fluidity index by the powder tester was 63, which was good.

[비교예 1]Comparative Example 1

광화제로서 SiO2를 1 중량 % 첨가하여 로터리 킬른으로 소성한 MgO 함유량 98 중량 % 의 마그네시아 클링커를 볼밀로 분쇄하여 수득된 평균 입경 23 ㎛, 비표면적 1 m2/g 의 마그네시아 분말에 관하여 내소화성을 평가한 바, 중량 증가율은 25.3 % 이었다. 또 파우더 시험기에 의한 유동성 지수는 55 이었다. 발수성이 현저하였다.Fire resistance to magnesia powder with an average particle size of 23 µm and a specific surface area of 1 m 2 / g obtained by milling a MgO content 98% by weight magnesia clinker calcined with a rotary kiln by adding 1% by weight of SiO 2 as a mineralizer. As a result, the weight increase rate was 25.3%. Moreover, the fluidity index by the powder tester was 55. The water repellency was remarkable.

[비교예 2]Comparative Example 2

MgO 함유량 99.5 중량 % 의 마그네시아 클링커를 볼밀로 분쇄하여 수득된 평균 입경 26 ㎛, 비표면적 1 m2/g 의 마그네시아 분말을 원료로 하고, 이것을 실리코니토 전기로내에서 1200℃ 에서 2 시간 유지하였다.Magnesia clinker having a MgO content of 99.5% by weight was obtained by milling with a ball mill a magnesia powder having an average particle diameter of 26 µm and a specific surface area of 1 m 2 / g, which was kept at 1200 ° C. for 2 hours in a siliconito electric furnace.

수득된 마그네시아 분말의 내소화성은 중량 증가율 5.2 % 이었다. 또 파우더 시험기에 의한 유동성 지수는 54 이었다.The fire resistance of the magnesia powder obtained was 5.2% by weight increase. Moreover, the fluidity index by the powder tester was 54.

[비교예 3]Comparative Example 3

MgO 함유량 99.5 중량 % 의 마그네시아 클링커를 볼밀로 분쇄하여 수득된 평균 입경 26 ㎛, 비표면적 1 m2/g 의 마그네시아 분말을 원료로 하고, 이것에 메틸수소실리콘 오일 1 중량 % 를 첨가한 후, 실리코니토 전기로내에서 700℃ 에서 2 시간 유지하였다.Magnesium clinker with a MgO content of 99.5% by weight was obtained by grinding a ball mill with an average particle diameter of 26 µm and a magnesia powder with a specific surface area of 1 m 2 / g as raw materials, and after adding 1% by weight of methylhydrogen silicone oil thereto, silica It was maintained at 700 ° C. for 2 hours in a Nito electric furnace.

수득된 마그네시아 분말의 내소화성은 중량 증가율 15 % 이었다. 또 파우더시험기에 의한 유동성 지수는 61 이었다.The fire resistance of the magnesia powder obtained was 15% in weight increase. In addition, the fluidity index by the powder tester was 61.

[비교예 4][Comparative Example 4]

금속마그네슘의 가열증기를 기상산화함으로써 제조된 MgO 함유량 98 중량 %, 평균 입경 0.2 ㎛, 비표면적 8 m2/g 의 마그네시아 분말을 원료로 하고, 이것에 메틸수소실리콘 오일 2 중량 % 를 첨가한 후, 실리코니토 전기로내에서 500℃ 에서 2 시간 유지하였다.Magnesium powder containing 98% by weight of MgO content, 0.2 μm in average particle diameter, and 8 m 2 / g specific surface area, prepared by gas phase oxidation of heated steam of metal magnesium, was used as a raw material, and 2% by weight of methyl hydrogen silicone oil was added thereto. It was maintained at 500 ° C. for 2 hours in a siliconcone electric furnace.

수득된 마그네시아 분말의 내소화성은 중량 증가율 6.2 % 이었다. 또 파우더 시험기에 의한 유동성 지수는 56 이었다.The fire resistance of the magnesia powder obtained was 6.2% by weight increase. Moreover, the fluidity index by the powder tester was 56.

Claims (7)

MgO 함유량이 90 중량 % 이상 99.8 중량 % 미만, 비표면적이 5 m2/g 이하, 평균 입경이 50 ㎛ 이하 그리고 학진법(學振法) 4 (마그네시아 클링커의 소화성 시험방법) 에 의한 중량증가율이 2.0 중량 % 이하인 것을 특징으로 하는 마그네시아 분말.MgO content is more than 90% and less than 99.8% by weight, specific surface area is 5 m 2 / g or less, average particle diameter is 50 µm or less, and weight increase rate by Hakjin method 4 (Method of digestibility test of magnesia clinker) Magnesia powder, characterized in that less than 2.0% by weight. 제 1 항에 있어서, 학진법 4 에 의한 중량 증가율이 1.0 중량 % 이하인 마그네시아 분말.The magnesia powder according to claim 1, wherein the weight increase rate according to the method 4 is 1.0 wt% or less. MgO 함유량이 98 중량 % 이상, 비표면적이 5 m2/g 이하, 그리고 평균 입경이 50 ㎛ 이하인 마그네시아 원료 분말과 유기규소화합물의 혼합물을 준비하고, 이 혼합물을 350 ∼ 600℃ 의 범위의 온도에서 가열하는 것을 특징으로 하는 제 1 항에 기재한 마그네시아 분말의 제조방법.A mixture of magnesia raw material powder and organosilicon compound having a MgO content of 98% by weight or more, a specific surface area of 5 m 2 / g or less, and an average particle diameter of 50 μm or less is prepared, and the mixture is prepared at a temperature in the range of 350 to 600 ° C. The manufacturing method of the magnesia powder of Claim 1 characterized by heating. 제 3 항에 있어서, 마그네시아 원료 분말이 고온소성 마그네시아 클링커의 분쇄체인 방법.The method according to claim 3, wherein the magnesia raw material powder is a pulverized body of a high temperature fired magnesia clinker. 제 3 항에 있어서, 유기 규소화합물이 실란 커플링제, 알콕시실란, 실리콘또는 실릴화제인 방법.4. The process of claim 3 wherein the organosilicon compound is a silane coupling agent, an alkoxysilane, a silicone or a silylating agent. 제 3 항에 있어서, 유기 규소 화합물을 마그네시아 원료분말에 대하여 0.2 ∼ 10.0 중량 % 의 비율로 함유하는 방법.The method according to claim 3, wherein the organosilicon compound is contained in a proportion of 0.2 to 10.0% by weight based on the magnesia raw material powder. 제 3 항에 있어서, 가열 온도가 400 ∼ 550℃ 의 범위에 있는 방법.The method according to claim 3, wherein the heating temperature is in the range of 400 to 550 ° C.
KR1019950016956A 1994-06-23 1995-06-22 Magnesia powder and its manufacturing method KR100373561B1 (en)

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WO2023157683A1 (en) * 2022-02-17 2023-08-24 デンカ株式会社 Coated magnesia particle, filler for heat dissipation material, resin composition, and method for producing coated magnesia particle

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