KR101167157B1 - Magnesia-graphite type refractory - Google Patents
Magnesia-graphite type refractory Download PDFInfo
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- KR101167157B1 KR101167157B1 KR1020100136527A KR20100136527A KR101167157B1 KR 101167157 B1 KR101167157 B1 KR 101167157B1 KR 1020100136527 A KR1020100136527 A KR 1020100136527A KR 20100136527 A KR20100136527 A KR 20100136527A KR 101167157 B1 KR101167157 B1 KR 101167157B1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/66—Monolithic refractories or refractory mortars, including those whether or not containing clay
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- C04B14/02—Granular materials, e.g. microballoons
- C04B14/32—Carbides; Nitrides; Borides ; Silicides
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- C04B14/326—Aluminium nitride
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- C04B20/00—Use of materials as fillers for mortars, concrete or artificial stone according to more than one of groups C04B14/00 - C04B18/00 and characterised by shape or grain distribution; Treatment of materials according to more than one of the groups C04B14/00 - C04B18/00 specially adapted to enhance their filling properties in mortars, concrete or artificial stone; Expanding or defibrillating materials
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Abstract
제철소 제강공정에서 사용하는 전로, 티밍 레이들 등에 적용될 수 있는 마그네시아-흑연질 내화물이 제공된다. 이 마그네시아-흑연질 내화물은 마그네시아-흑연질 내화조성물 100중량부에 대해 질화 알루미늄이 1~5중량부 포함하여 이루어지는 것이다. 마그네시아-흑연질 내화물에서 질화 알루미늄은 고온 분해과정을 통해 발생하는 Al 산화물과 마그네시아 입자가 반응하여 내화물의 표면에 스피넬 조성의 보호층을 형성함으로써 내산화성을 크게 개선한다. Provided is a magnesia-graphite refractory material that can be applied to converters, teaming ladles, and the like used in steel making processes. The magnesia-graphite refractory material comprises 1 to 5 parts by weight of aluminum nitride based on 100 parts by weight of the magnesia-graphite refractory composition. In the magnesia-graphite refractory, aluminum nitride significantly improves oxidation resistance by forming a protective layer of spinel composition on the surface of the refractory by reacting Al oxide and magnesia particles generated through high temperature decomposition.
Description
본 발명은 전로, 티밍 레이들 등의 제강 설비에 사용 가능한 마그네시아-흑연질 내화물에 관한 것이다. 보다 상세하게는, 질화 알루미늄 분말을 첨가하여 고온 분해과정을 통해 발생하는 Al 산화물과 마그네시아 입자가 반응하여 내화물의 표면에 스피넬 조성의 보호층을 형성함으로써 내산화성이 향상되는 마그네시아-흑연질 내화물에 관한 것이다.TECHNICAL FIELD This invention relates to the magnesia-graphite refractory body which can be used for steelmaking facilities, such as a converter and a teaming ladle. More specifically, Magnesia-graphite refractory material having improved oxidation resistance by forming a protective layer of spinel composition on the surface of the refractory material by adding aluminum nitride powder to react with Al oxide and magnesia particles generated through high-temperature decomposition process will be.
제철소 제강공정에서는 전로, 레이들 등의 설비가 사용되는데, 이들 설비에는 슬래그와 접촉하는 부위에 마그네시아-흑연질 내화물을 사용하고 있다. 마그네시아-흑연질 내화물은 마그네시아 입자와 흑연 입자를 페놀수지를 첨가하여 혼합한 후, 가압성형하여 제조한다. 상기 내화물은 고온에서 산화성 분위기에 노출되면 흑연원료가 산화되면서 공극이 생성되므로 용강이나 슬래그의 침투가 증가하여 사용수명이 감소한다.In the steelmaking process of steelworks, facilities such as converters and ladles are used, and magnesia-graphite refractory materials are used in these facilities in contact with slag. Magnesia-graphite refractory material is prepared by mixing magnesia particles and graphite particles by adding a phenol resin, followed by press molding. When the refractory material is exposed to an oxidizing atmosphere at a high temperature, the graphite raw material is oxidized to form voids, thereby increasing penetration of molten steel or slag, thereby reducing the service life.
이와 관련된 선행기술은 아래와 같다. Related prior art is as follows.
일본공개특허 2002-249371에서는 내산화성의 특성을 갖고 고강도로 손실이 적은 마그네시아-카본질 내화물이 제시되어 있다. 이 내화물은, 금속 붕소 0.1~6%，탄소 1~40%를 함유하고，금속 알루미늄，금속 실리콘，금속 마그네슘의 일종 또는 2종 이상을 합계로 1~10％함유하고，나머지 산화 마그네슘을 주체로 하는 것이다.Japanese Laid-Open Patent Publication No. 2002-249371 discloses a magnesia-carbon refractory having high oxidation resistance and low loss at high strength. This refractory contains 0.1 to 6% of metal boron, 1 to 40% of carbon, 1 to 10% of metal aluminum, metal silicon, metal magnesium, or two or more kinds in total, and the rest of magnesium oxide mainly It is.
일본공개특허 2000-001364에서는 용강표면에 대 유량의 산소를 취부한 경우에 사용해도 용손이 적은 마그네시아-카본 내화물 라이닝이 제시되어 있다. 이 내화물 라이닝은, 흑연 5~15 중량％，비정질 탄소 분 0~5 중량％를 함유하고，더욱 Al 금속，Si 금속 및 Al-Si질 금속중의 1 종 또는 2종 이상이 1~4 중량％로，모든 금속 성분중에 차지한 Si 성분의 비율이 70 중량％이하의 마그네시아-카본 내화물이다. Japanese Laid-Open Patent Publication No. 2000-001364 discloses a magnesia-carbon refractory lining having low melt loss even when used in a case where a large flow rate of oxygen is attached to a molten steel surface. The refractory lining contains 5 to 15% by weight of graphite, 0 to 5% by weight of amorphous carbon, and furthermore, 1 to 4% by weight of one or two or more of Al metal, Si metal and Al-Si-based metal. The proportion of Si component in all metal components is magnesia-carbon refractory material of 70% by weight or less.
일본공개특허 2002-316864에는 극저탄소강의 용제시에 용강의 탄소함유량의 픽업이 없고 고온의 산화분위기 조건하에서 슬래그 공격에 대해서도 안정한 내식성을 갖는 마그네시아 질화 붕소질 내화물이 제시되어 있다. 이 내화물은, MgO 70 mass％이상으로 ，질화 붕소 함유량이 1~30mass％으로 하는 마그네시아 질화 붕소질 내화물이다. Japanese Laid-Open Patent Publication No. 2002-316864 discloses a magnesia boron nitride refractory having no pick up of carbon content in molten steel at the time of solvent of ultra low carbon steel and having stable corrosion resistance against slag attack under high temperature oxidizing atmosphere conditions. This refractory material is magnesia boron nitride refractory material with MgO 70 mass% or more and boron nitride content 1-30 mass%.
이들 특허에서 제안된 마그네시아-흑연질 내화물은 내산화성을 향상하는데 한계가 있다. 일본공개특허 2002-249371과 일본공개특허 2000-001364에는 산화방지제로서 금속분말을 다량 사용하고 있어 스폴링 저항성이 감소하여 이에 의한 수명 이 저하한다. 또한, 일본공개특허 2002-316864에서 붕소계 분말은 저융점 물질을 생성하므로 내화물의 내식성이 감소되므로써 수명 저하를 초래한다.The magnesia-graphite refractory proposed in these patents is limited in improving oxidation resistance. Japanese Patent Laid-Open Publication No. 2002-249371 and Japanese Patent Laid-Open Publication No. 2000-001364 use a large amount of metal powder as an antioxidant, so that the spalling resistance is reduced, thereby reducing the service life. In addition, boron-based powder in Japanese Laid-Open Patent Publication No. 2002-316864 produces a low melting point material, thereby reducing the corrosion resistance of the refractory material, resulting in a decrease in life.
본 발명은 상기한 마그네시아-흑연질 내화물의 문제점을 해결하기 위하여 안출된 것으로서, 내산화성이 개선된 마그네시아-흑연질을 제공하고자 하는 것이다. The present invention has been made to solve the above problems of magnesia-graphite refractory, to provide a magnesia-graphite with improved oxidation resistance.
본 발명의 마그네시아-흑연질 내화물은, 마그네시아 원료와 흑연 원료에 페놀수지를 첨가하여 제조되는 마그네시아-흑연질 내화물로서, 마그네시아-흑연질 내화조성물 100중량부에 대해 질화 알루미늄이 1~5중량부 포함하여 이루어진다.The magnesia-graphite refractory material of the present invention is a magnesia-graphite refractory material prepared by adding a phenol resin to a magnesia raw material and a graphite raw material, and contains 1 to 5 parts by weight of aluminum nitride based on 100 parts by weight of the magnesia-graphite refractory composition. It is done by
바람직하게, 상기 마그네시아-흑연질 내화조성물의 표면에는 상기 마그네시아-흑연질 내화조성물의 고온 분해과정을 통해 스피넬(MgO-Al2O3) 조성 보호층이 형성된다.Preferably, the protective layer of spinel (MgO-Al 2 O 3 ) composition is formed on the surface of the magnesia-graphite refractory composition through the high temperature decomposition process of the magnesia-graphite refractory composition.
바람직하게, 상기 질화 알루미늄의 평균크기는 0.01~0.2mm이다. 이때, 보다 바람직하게, 상기 질화 알루미늄의 평균크기는 0.1~0.15mm이며, 그 함량은 3~4중량부이다.Preferably, the average size of the aluminum nitride is 0.01 ~ 0.2mm. At this time, more preferably, the average size of the aluminum nitride is 0.1 ~ 0.15mm, the content is 3 to 4 parts by weight.
바람직하게, 상기 질화 알루미늄은 금속 알루미늄(Al)을 자전연소반응법을 통해 질소 분위기에서 고온 반응하여 제조된다.Preferably, the aluminum nitride is prepared by the high temperature reaction of metal aluminum (Al) in a nitrogen atmosphere through a self-burning reaction method.
바람직하게, 상기 고온 분해과정은 산화성 분위기에서 전기로를 이용하여 1500도 고온에서 1시간 열처리한다.Preferably, the high temperature decomposition process is heat-treated for 1 hour at 1500 degrees high temperature using an electric furnace in an oxidizing atmosphere.
상기한 바와 같은 본 발명에 따른 마그네시아 흑연질 내화물은 사용 수명을 향상시킴으로써 전로 및 티밍 레이들 등 제강설비의 생산성 향상 및 자재 비용 절감을 도모할 수 있다.Magnesia graphite refractory according to the present invention as described above can improve the productivity and material cost reduction of steelmaking equipment such as converter and teaming ladle by improving the service life.
이하, 본 발명의 실시예에 따른 마그네시아-흑연질 내화물을 상세히 설명하고자 한다. 본 발명은 이하에서 설명되는 실시예에 한정되는 것이 아니라, 본 발명의 기술사상에 기초하여 다양한 형태로 구현될 수 있으며, 예시된 실시예들은 본 발명의 보다 구체적으로 설명하기가 위한 것으로 본 발명을 한정하기 위한 것은 아니다. Hereinafter, the magnesia-graphite refractory according to an embodiment of the present invention will be described in detail. The present invention is not limited to the embodiments described below, but can be implemented in various forms based on the technical idea of the present invention, the illustrated embodiments are intended to describe the present invention in more detail as It is not intended to be limiting.
본 발명은 마그네시아-흑연질 내화물에 질화 알루미늄을 포함하는 구성으로, 해당 표면에 스피넬(MgO-Al2O3) 산화물 층은 형성함으로써, 외부로부터 공기 등 산화성 물질의 침투를 억제하여 내화물 중에 함유된 흑연의 산화가 방지되도록 한다. The present invention comprises a composition containing aluminum nitride in the magnesia-graphite refractory, by forming a spinel (MgO-Al 2 O 3 ) oxide layer on the surface, thereby suppressing the penetration of oxidizing substances such as air from the outside to be contained in the refractory To prevent oxidation of graphite.
구체적으로, 본 발명에 포함되는 질화 알루미늄은 금속 알루미늄(Al)을 자전연소반응법을 통해 질소 분위기에서 고온 반응하여 제조된다. 이렇게 제조된 질화 알루미늄을 마그네시아-흑연질 내화물 중에 혼합하여 사용하게 되면, 고온에 노출되어 분해가 진행되면서 Al(g)가 생성된다. 이때, Al(g)의 생성을 위한 고온 분해과정은 산화성 분위기에서 전기로를 이용하여 1500도 고온에서 1시간 열처리된다. Specifically, aluminum nitride included in the present invention is produced by reacting metallic aluminum (Al) at high temperature in a nitrogen atmosphere through a self-burning reaction method. When the aluminum nitride thus prepared is mixed and used in the magnesia-graphite refractory, Al (g) is produced while being decomposed and exposed to high temperature. At this time, the high temperature decomposition process for the production of Al (g) is heat-treated for 1 hour at 1500 degrees high temperature using an electric furnace in an oxidizing atmosphere.
그리고 고온 분해과정을 통해 생성된 Al(g)가 내화물 표면으로 이동하여 Al2O3를 생성한다. 생성된 Al2O3는 주위에 존재하는 내화물의 주성분인 MgO와 반응함으로써 화학적으로 안정한 스피넬(MgO-Al2O3) 입자가 된다. 이 스피넬 입자들은 수 마이크론의 미세하므로 고온의 용강과 접한 계면상에서 소결되어 치밀한 산화물 층을 형성한다. 이에 따라, 스피넬 산화물 층은 외부로부터 공기 등 산화성 물질의 침투를 억제함으로써 내화물 중에 함유된 흑연의 산화를 방지할 수 있다. And Al (g) generated through the high temperature decomposition process is moved to the refractory surface to produce Al 2 O 3 . The produced Al 2 O 3 reacts with MgO, the main component of the refractory present in the surroundings, to form chemically stable spinel (MgO-Al 2 O 3 ) particles. These spinel particles are several microns fine and therefore sintered at the interface with hot molten steel to form a dense oxide layer. Accordingly, the spinel oxide layer can prevent the oxidation of graphite contained in the refractory by suppressing the penetration of oxidizing substances such as air from the outside.
본 실시예에 따른 질화 알루미늄은 마그네시아-흑연질 내화물에서 MgO와 반응하여 스피넬을 형성하는 것이기 때문에, MgO가 주체가 되는 마그네시아-흑연질 내화물이면 적용될 수 있을 것이다. 그리고 통상의 질화 알루미늄은 마그네사아-흑연질 내화물의 종류에 적용될 수 있는 것으로, 마그네시아-흑연질 내화물의 특정한 형태에 한정되는 것은 아니다. 마그네시아-흑연질 내화물로는 다양하게 제시되어 있다. 마그네시아-흑연질 내화물로는, 한국공개특허 2009-0072477, 2004-0049585 등을 예로 들 수 있다. Since the aluminum nitride according to the present embodiment is to react with MgO in the magnesia-graphite refractory to form a spinel, the aluminum nitride may be applied if the MgO is a magnesia-graphite refractory. And ordinary aluminum nitride can be applied to the kind of magnesia-graphite refractory, and is not limited to the specific form of magnesia-graphite refractory. Magnesia-graphite refractory has been suggested in various ways. Examples of magnesia-graphite refractory include Korea Patent Publication No. 2009-0072477, 2004-0049585, and the like.
본 발명에서 질화 알루미늄은, 마그네시아-흑연질 내화조성물에 추가로 포함되는 것인데, 일실시예로서, 마그네시아-흑연질 내화조성물 100중량부에 대해 질화 알루미늄이 1~5중량부 포함된다.In the present invention, the aluminum nitride, which is further included in the magnesia-graphite refractory composition, as an example, 1 to 5 parts by weight of aluminum nitride is included with respect to 100 parts by weight of magnesia-graphite refractory composition.
여기서, 질화 알루미늄이 1 중량%보다 작으면 내산화성 향상효과가 적고, 5중량% 초과의 경우에는 내산화성 향상 효과는 크지 않으면서 첨가량 증가에 의한 비용증가의 단점이 있다. 첨가량을 고려한 내산화성의 효과측면을 고려 할 때, 3~4중량%가 가장 바람직하다.Here, when the aluminum nitride is less than 1% by weight, the oxidation resistance improving effect is less, and in the case of more than 5% by weight, the oxidation resistance improving effect is not great, but there is a disadvantage of an increase in cost due to the addition amount. In consideration of the effect of oxidation resistance in consideration of the addition amount, 3 to 4% by weight is most preferred.
본 발명에서 질화 알루미늄의 평균크기는 0.01~0.2mm일 수 있다. 질화 알루미늄의 평균 크기가 0.01mm보다 작으면 마그네시아-흑연질 내화물에 균일한 분산이 어려워 내산화성 향상 효과가 적고, 또한 비용이 크게 증가한다.In the present invention, the average size of aluminum nitride may be 0.01 ~ 0.2mm. If the average size of aluminum nitride is smaller than 0.01 mm, it is difficult to uniformly disperse the magnesia-graphite refractory, so that the effect of improving oxidation resistance is small, and the cost is greatly increased.
이대, 질화 알루미늄의 평균크기가 0.2mm보다 크면 내산화성 향상을 위해 첨가량이 증가하므로 비용이 증가하고, 작은 입자와 동일한 양으로 첨가할 경우 비표면적이 적어 내산화성 향상 효과가 낮다. 본 발명의 바람직한 일실시예로서, 질화 알루미늄의 평균크기는 0.1~0.15mm이다.If the average size of aluminum nitride is larger than 0.2mm, the amount of the additive is increased to improve oxidation resistance, and the cost is increased. When the additive is added in the same amount as small particles, the specific surface area is small and the effect of improving oxidation resistance is low. As a preferred embodiment of the present invention, the average size of aluminum nitride is 0.1 ~ 0.15mm.
본 발명의 일실시예서 가장 바람직한 질화 알루미늄은 평균 크기가 0.1~0.15mm이고 그 첨가량은 마그네시아-흑연질 내화조성물 100중량부에 대해 3~4중량부 포함되는 것이다.
In one embodiment of the present invention, the most preferable aluminum nitride has an average size of 0.1 to 0.15 mm and the added amount is 3 to 4 parts by weight based on 100 parts by weight of magnesia-graphite refractory composition.
(실시예)(Example)
통상적으로 내화물 제조에 사용하는 순도 99% 이상의 마그네시아 원료와 레졸형 페놀수지를 혼합하여 마그네시아-흑연질 내화물을 제조하였다. 자전연소합성법을 이용하여 제조한 질화 알루미늄을 첨가제로 사용하였다. 마그네시아-흑연질 내화물의 성형은 CIP를 이용하였다. 제조된 제품을 전기로를 이용하여 산화성 분위기에서 1500도의 고온으로 1시간 열처리하였다. Typically, magnesia-graphite refractory material was prepared by mixing a magnesia raw material having a purity of 99% or more and a resol type phenolic resin used for the production of refractory materials. Aluminum nitride prepared by the autocombustion synthesis method was used as an additive. The molding of the magnesia-graphite refractory used CIP. The prepared product was heat-treated for 1 hour at an elevated temperature of 1500 degrees in an oxidizing atmosphere using an electric furnace.
시험 후 수거한 시편을 절단하여 흑연이 제거된 탈탄면적을 측정하였으며, 실시예 1의 탈탄면적을 100으로 하여 백분율 지수로 산화지수를 표기하였다. 표 1에 시편 제조조건과 시험결과를 정리하였다. 실시예6,7에서 내화물의 산화가 크게 감소 하였음을 알 수 있다.
After the test, the collected specimens were cut and the decarburized area from which graphite was removed was measured. The decarburized area of Example 1 was 100, and the oxidation index was expressed as a percentage index. Table 1 summarizes the specimen manufacturing conditions and test results. In Examples 6 and 7, it can be seen that the oxidation of the refractory is greatly reduced.
division
Test result
상술한 바와 같이, 본 발명은 질화 알루미늄 분말을 첨가하여 고온 분해과정을 통해 발생하는 Al 산화물과 마그네시아 입자가 반응하여 내화물의 표면에 스피넬 조성의 보호층을 형성함으로써, 내산화성을 향상시키고 전로 및 티밍 레이들 등 제강설비의 생산성 향상 및 자재 비용 절감을 도모할 수 있는 등의 우수한 장점을 갖는 것이다.As described above, according to the present invention, aluminum oxide powder is added to react with Al oxide and magnesia particles generated through high-temperature decomposition to form a protective layer of spinel composition on the surface of the refractory, thereby improving oxidation resistance and converter and teaming. It has excellent advantages such as productivity improvement and material cost reduction of steelmaking facilities such as ladle.
Claims (6)
마그네시아-흑연질 내화조성물 100중량부에 대해 질화 알루미늄이 1~5중량부 포함하여 이루어지는 마그네시아-흑연질 내화물.Magnesia-graphite refractory material prepared by adding phenol resin to magnesia raw material and graphite raw material,
A magnesia-graphite refractory comprising 1 to 5 parts by weight of aluminum nitride with respect to 100 parts by weight of magnesia-graphite refractory composition.
상기 마그네시아-흑연질 내화조성물의 표면에는 상기 마그네시아-흑연질 내화조성물의 고온 분해과정을 통해 스피넬(MgO-Al2O3) 조성 보호층이 형성되는 것을 특징으로 하는 마그네시아-흑연질 내화물.The method of claim 1,
Magnesia-graphite refractory, characterized in that the protective layer of the spinel (MgO-Al 2 O 3 ) composition is formed on the surface of the magnesia-graphite refractory composition through a high temperature decomposition process of the magnesia-graphite refractory composition.
상기 질화 알루미늄의 평균크기는 0.01~0.2mm임을 특징으로 하는 마그네시아-흑연질 내화물.The method of claim 1,
Magnesia-graphite refractory, characterized in that the average size of the aluminum nitride is 0.01 ~ 0.2mm.
상기 질화 알루미늄은 금속 알루미늄(Al)을 자전연소반응법을 통해 질소 분위기에서 고온 반응하여 제조되는 것을 특징으로 하는 마그네시아-흑연질 내화물.The method of claim 1,
The aluminum nitride is a magnesia-graphite refractory, characterized in that the metal aluminum (Al) is produced by a high temperature reaction in a nitrogen atmosphere through a self-burning reaction method.
상기 고온 분해과정은 산화성 분위기에서 전기로를 이용하여 1500도 고온에서 1시간 열처리하는 것을 특징으로 하는 마그네시아-흑연질 내화물.The method of claim 2,
The high temperature decomposition process is a magnesia-graphite refractory, characterized in that for 1 hour heat treatment at 1500 degrees high temperature using an electric furnace in an oxidizing atmosphere.
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