KR100349165B1 - A Method of Manufacturing Dolomite Refractory Materials Having Superior Anti-Hydration - Google Patents

A Method of Manufacturing Dolomite Refractory Materials Having Superior Anti-Hydration Download PDF

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KR100349165B1
KR100349165B1 KR1019970042162A KR19970042162A KR100349165B1 KR 100349165 B1 KR100349165 B1 KR 100349165B1 KR 1019970042162 A KR1019970042162 A KR 1019970042162A KR 19970042162 A KR19970042162 A KR 19970042162A KR 100349165 B1 KR100349165 B1 KR 100349165B1
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dolomite
barium titanate
hydration
waste
clinker
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KR19990018882A (en
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박재원
홍기곤
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주식회사 포스코
재단법인 포항산업과학연구원
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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • 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
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/03—Shaped 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
    • C04B35/06—Shaped 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 oxide mixtures derived from dolomite
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/46—Shaped 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 titanium oxides or titanates
    • C04B35/462—Shaped 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 titanium oxides or titanates based on titanates
    • C04B35/465—Shaped 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 titanium oxides or titanates based on titanates based on alkaline earth metal titanates
    • C04B35/468—Shaped 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 titanium oxides or titanates based on titanates based on alkaline earth metal titanates based on barium titanates
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/62204—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products using waste materials or refuse
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
    • C04B2235/9669—Resistance against chemicals, e.g. against molten glass or molten salts

Abstract

PURPOSE: A method for preparing a dolomite refractory is provided, to obtain a dolomite refractory with the improved the hydration resistance by recycling the barium titanate waste with low cost. CONSTITUTION: The method comprises the steps of adding the barium titanate waste to a dolomite clinker in the content of 1-10 wt% based on the amount of the dolomite clinker and mixing them; molding the mixture; and calcining the molded one. The barium titanate waste has a particle size of 1 mm or less, and its barium titanate content is 90% or more.

Description

내수화성이 우수한 돌로마이트 내화재료의 제조방법{A Method of Manufacturing Dolomite Refractory Materials Having Superior Anti-Hydration}A Method of Manufacturing Dolomite Refractory Materials Having Superior Anti-Hydration}

본 발명은 전기로의 내장내화물 등으로 사용되고 있는 돌로마이트 클링커 내화재료의 제조방법에 관한 것으로, 보다 상세하게는 돌로마이트에 바륨티타네이트 폐기물을 첨가한 내수화성이 우수한 돌로마이트 내화재료를 제조하는 방법에 관한 것이다.The present invention relates to a method for producing a dolomite clinker refractory material used in interior refractories of an electric furnace, and more particularly, to a method for producing a dolomite refractory material having excellent water resistance in which barium titanate waste is added to dolomite.

돌로마이트질의 부정형 내화물은 전기로 바닥재 등으로 사용되고 있으며, 마그네시아에 비해 상대적으로 슬래그에 대한 내침윤성과 열충격저항성이 높고 증기압이 낮아 강의 오염을 저감시키는 장점을 지니고 있다. 그러나 돌로마이트 중에 함유되어 있는 칼시아가 수화되기 쉽게 때문에 사용에 제한을 받고 있다. 현재, 클링커 형태의 돌로마이트의 내수화성을 향상시키기 위한 방법으로는 클링커 생산시, 첨가물(산화물)을 첨가하는 방법이 가장 널리 사용되고 있다.Dolomite amorphous refractory materials are used as flooring materials for electric furnaces, and have the advantage of reducing the pollution of steel due to relatively high invasion resistance and thermal shock resistance to slag and low vapor pressure, compared with magnesia. However, since the calcia contained in dolomite is easily hydrated, its use is limited. Currently, as a method for improving the water resistance of clinker-type dolomite, a method of adding an additive (oxide) in the production of clinker is most widely used.

종래의 공지기술로는 일본특허 공개공보 소55-35354 호에서는 Fe2O3, MgO, Al2O3, SiO2또는 Cr2O3를 단독으로 사용하고 있으며, 소 57-205367 호에서는 CaO에 대하여1-20mol%의 SrO 또는 BaO의 고용체에 1-10%의 산화철을 함유하는 칼시아 클링커로 내수화성을 향상시키고 있다. 또한, 소 59-35060 호에서는 TiO2를 첨가하여 내수화성을 향상시키고 있다. 그러나, 상기와 같은 제안들에서는 내수화성을 향상시키기 위해 시약형태의 첨가물을 사용하기 때문에, 비용측면에서 고가라는 문제점이 있다.In the prior art, Japanese Patent Laid-Open Publication No. 55-35354 uses Fe 2 O 3 , MgO, Al 2 O 3 , SiO 2, or Cr 2 O 3 alone, and in Small 57-205367 to CaO. Hydration resistance is improved by calcia clinker containing 1-10% of iron oxide in solid solution of 1-20 mol% of SrO or BaO. In addition, in No. 59-35060, TiO 2 is added to improve the water resistance. However, the above proposals have a problem in that they are expensive in terms of cost because they use additives in the form of reagents to improve the water resistance.

본 발명은 돌로마이트에 바륨티타네이트 폐기물을 첨가하여, 돌로마이트 내화재료를 제조함으로써, 폐기되는 자원의 재활용 및 공해방지 측면에서 유용하면서, 저렴한 비용으로 우수한 내수화성을 얻을 수 있는 돌로아미트 내화재료의 제조방법을 제공하고자 하는데, 그 목적이 있다.The present invention provides a dolomite refractory material by adding barium titanate waste to dolomite to produce a dolomite refractory material, which is useful in terms of recycling waste and preventing pollution, and can obtain excellent water resistance at low cost. The purpose is to provide a method.

일반적으로 바륨티타네이트는 콘덴서의 재료등으로 사용되며 융점은 1618℃로 낮다. 그리고, 전자재료 제조시 첨가되는 각종 산화물로 인하여 융점이 약 100℃정도 낮아진다. 그러므로, 1600℃이상에서는 용융되어 액상으로 존재한다. 이와같이 용융상태로 되면 BaO는 돌로마이트 중의 CaO에 고용되어 내수화성을 향상시킴과 동시에 TiO2는 바륨티타네이트보다 융점이 높은 CaTiO3를 형성하여 내수화성을 향상시킨다. 본 발명자들은 상기한 바와같은 효과를 바륨티타네이트 폐기물을 이용하면 저렴한 비용으로도 충분히 얻을 수 있고, 또한, 소결성 측면에서도 바륨티타네이트 폐기물을 첨가하여 향상을 도모할 수 있는 것을 알아내었다.In general, barium titanate is used as a condenser material and the melting point is as low as 1618 ℃. In addition, the melting point is lowered by about 100 ° C. due to various oxides added during the manufacture of electronic materials. Therefore, above 1600 ° C., they melt and exist in the liquid phase. In this manner, BaO is dissolved in CaO in the dolomite to improve water resistance, while TiO 2 forms CaTiO 3 having a higher melting point than barium titanate to improve water resistance. The present inventors have found that the barium titanate waste can be sufficiently obtained at low cost by using the barium titanate waste, and the barium titanate waste can be added to improve the sinterability.

이러한 관점으로 부터 출발한 본 발명은 돌로마이트 내화재료를 제조하는 방법에 있어서, 돌로마이트 클링커에, 1mm 이하의 입경을 갖는 바륨티타네이트 폐기물을 상기 돌로마이트 대비 1-10중량% 첨가하여 혼합한 후, 성형 및 소성하는 내수화성이 우수한 돌로마이트 내화재료의 제조방법에 관한 것이다.Starting from this point of view, the present invention provides a method for producing a dolomite refractory material, wherein after mixing 1-10% by weight of barium titanate waste having a particle size of 1 mm or less with respect to the dolomite clinker, and then molding and The present invention relates to a method for producing a dolomite refractory material having excellent fire resistance.

이하, 본 발명을 보다 상세히 설명한다.Hereinafter, the present invention will be described in more detail.

일반적으로 돌로마이트 클링커는 마그네시아의 주변에 칼시아가 균일하게 분포되어 있으며, 돌로마이트 클링커중에 CaO가 일반적으로 5-40중량% 함유되어 있다. 본 발명에서는 이러한 돌로마이트 클링커를 사용하는데, 저융점 물질의 생성을 최소화하기 위하여 MgO와 CaO를 제외한 나머지 성분이 1중량% 이하인 것을 사용하는 편이 보다 바람직하다.In general, dolomite clinker has a uniform distribution of calcia around the magnesia, and generally contains 5-40% by weight of CaO in the dolomite clinker. In the present invention, such a dolomite clinker is used, and in order to minimize the generation of low melting point materials, it is more preferable to use 1 wt% or less of the remaining components except for MgO and CaO.

또한, 본 발명에서는 바륨티타네이트 폐기물을 이용한다. 상기 바륨티타네이트 폐기물은 콘덴서 제조 및 여러산업 분야에서 발생하는 폐기물을 이용할 수 있는데, 내화물의 수화성 방지의 효과측면에서 바륨티타네이트가 90%이상인 것을 사용하는 것이 바람직하다.In the present invention, barium titanate waste is used. The barium titanate waste may be a waste produced in capacitor manufacturing and various industrial fields, and it is preferable to use a barium titanate of 90% or more in view of the effect of preventing hydration of the refractory material.

상기 바륨티타네이트 폐기물은 분쇄후 입도가 1mm 이하이어야 한다. 바륨티타네이트의 입자크기가 1mm 이상이 되면 돌로마이트 클링커중에 극단적인 액상과잉영역을 생성시켜 돌로마이트 클링커의 국부적 손상을 가속화시키기 때문이다.The barium titanate waste should have a particle size of 1 mm or less after grinding. This is because when the particle size of barium titanate is 1 mm or more, an extreme liquid excess region is generated in the dolomite clinker to accelerate the local damage of the dolomite clinker.

상기 바륨티타네이트의 첨가량은 돌로마이트에 대하여 외삽으로 1-10중량% 이어야 한다. 바륨티타네이트의 첨가량이 1중량% 미만이 되면 첨가량이 부족하여 돌로마이트 클링커의 내수화성 향상이 미약하며, 첨가량이 10중량%를 초과하면 입계에 존재하는 액상의 증가로 오히려 돌로마이트 클링커의 물성을 저하시키게 되기 때문이다.The amount of barium titanate added should be 1-10% by weight extrapolated to dolomite. When the addition amount of barium titanate is less than 1% by weight, the addition amount is insufficient to improve the water resistance of the dolomite clinker, and when the addition amount is more than 10% by weight, the increase of the liquid phase present at the grain boundary lowers the physical properties of the dolomite clinker. Because it becomes.

또한, 본 발명에서는 돌로마이트에 바륨티타네이트 폐기물을 혼합후, 성형 및 소성한다. 상기 성형 및 소성은 통상의 방법에 의해 행할 수 있다.In addition, in the present invention, barium titanate waste is mixed with dolomite, and then molded and fired. The said molding and baking can be performed by a conventional method.

이하, 실시예를 통하여 본 발명을 보다 상세히 설명한다.Hereinafter, the present invention will be described in more detail with reference to Examples.

실시예Example

마그네시아와 칼시아가 중량비로 7:3으로 이루어진 돌로마이트 클링커에 분쇄한 바륨티타네이트 폐기물을 외삽으로 하기 표1과 같은 함량으로 첨가하여 혼합하고, 500kg/㎠의 압력으로 성형한 후 1650℃에서 3시간 소성하였다. 얻어진 소성품의 기공율 및 밀도를 구하여 그 결과를 하기 표1에 나타내었다. 또한, 염기도 비가 2.1인 전기로 슬래그(Slag)를 침식제로 사용하여 1700℃x1시간x침식제배제x3회반복의 시험조건으로 침식시험을 행한 후 침식전후의 침식면적을 측정하고, 그 측정값을 비교예(3)을 기준으로 하였을 때의 상대비교값인 침식지수를 구하여 하기 표1에 나타내었다.Barium titanate waste, which was ground to a dolomite clinker composed of magnesia and calcia at 7: 3 by weight, was extrapolated and added in the contents as shown in Table 1 below, mixed at a pressure of 500 kg / cm 2, and then 3 hours at 1650 ° C. Fired. The porosity and density of the resulting fired article were obtained and the results are shown in Table 1 below. In addition, using an electric furnace slag having a basicity ratio of 2.1 as an erosion agent, the erosion test was carried out under test conditions of 1700 ° C x 1 hour x erosion exclusion x 3 repetitions, and the erosion area before and after erosion was measured. The erosion index, which is a relative comparison value based on Comparative Example (3), was obtained and shown in Table 1 below.

또한, 오토클래이브를 이용하여 120℃x24시간 동안 수화시험을 행한 후의 중량증가율을 측정하여 하기 표1에 나타내었다.In addition, the weight increase rate after performing a hydration test for 120 ℃ x 24 hours using an autoclave was measured and shown in Table 1 below.

또한, 국부침식발생 면적율을 구하여 하기 표1에 나타내었다.In addition, the local erosion area ratio was calculated and shown in Table 1 below.

발 명 예Foot honor 비 교 예Comparative Example 1One 22 33 1One 22 33 바륨티타네이트의 입도(㎛)Particle Size of Barium Titanate (㎛) 1이하1 or less 1이하1 or less 1이하1 or less 1이상1 or more 1이하1 or less 1이하1 or less 바륨티타네이트의 첨가량(외삽, 중량%)Addition amount of barium titanate (extrapolation, weight%) 1One 66 1010 44 1414 00 기공율(%)Porosity (%) 3.53.5 2.12.1 1.31.3 4.24.2 0.70.7 16.216.2 밀도(g/㎤)Density (g / cm 3) 3.283.28 3.303.30 3.353.35 3.243.24 3.363.36 3.183.18 침식지수Erosion Index 0.400.40 0.150.15 0.450.45 1.041.04 1.401.40 1.001.00 수화에 의한 중량 증가율(%)Weight increase rate by hydration (%) 0.010.01 00 00 1.201.20 00 2.002.00 국부침식발생 면적율(%)Local erosion area rate (%) 00 00 00 5050 1717 00

상기 표1에서 알 수 있는 바와같이, 본 발명의 조건을 만족하는 발명예(1-3)은 침식지수가 낮았으며, 수화현상도 미약하게 나타나거나 거의 발생하지 않았다. 또한, 국부침식 발생도 없었다.As can be seen in Table 1, Inventive Example (1-3) that satisfies the conditions of the present invention had a low erosion index, the hydration phenomenon is weak or rarely occurred. There was also no local erosion.

이에 반하여, 바륨티타네이트의 입도가 1㎛이상인 것을 사용한 비교예(1)은 침식이 많이 발생하였고, 수화도 상당히 발생하였다. 또한, 바륨티타네이트의 첨가량이 본 발명의 범위보다 많은 14중량%를 첨가한 비교예(2)는 수화는 방지되었으나, 많은 침식이 발생하였다. 또한, 바륨티타네이트를 첨가하지 않은 비교예(3)은 높은 수화율을 나타내었다.On the contrary, in Comparative Example (1) using a particle size of barium titanate of 1 µm or more, erosion occurred a lot, and hydration also occurred considerably. In addition, in Comparative Example (2) in which 14 wt% of the barium titanate was added in an amount greater than the range of the present invention, hydration was prevented, but a lot of erosion occurred. In addition, Comparative Example (3) without addition of barium titanate showed high hydration rate.

상술한 바와같은 본 발명에 의하면, 돌로마이트 클링커에 바륨티타네이트 폐기물을 첨가하여 내화재료를 제조함으로써, 제조되는 내화재료의 내수화성을 향상시킬 뿐만 아니라, 환경오염방지 측면에서도 폐기물을 재이용하는 효과가 제공된다.According to the present invention as described above, by adding barium titanate waste to the dolomite clinker to produce a refractory material, not only improves the water resistance of the refractory material to be produced, but also provides the effect of recycling the waste in terms of environmental pollution prevention do.

Claims (1)

돌로마이트 내화재료를 제조하는 방법에 있어서,In the method for producing the dolomite refractory material, 돌로마이트 클링커에, 1mm이하의 입경을 가지며 바륨티타네이트가 90%이상인 바륨타타네이트 폐기물을 상기 돌로마이트 대비 1-10중량% 첨가하여 혼합한 후, 성형 및 소성하는 것을 특징으로 하는 내수화성이 우수한 돌로마이트 내화재료의 제조방법.Dolomite refractory, characterized in that the dolomite clinker, 1-10% by weight of barium titanate waste having a particle diameter of 1 mm or less and 90% or more of barium titanate is added to the dolomite, and then molded and calcined. Method of manufacturing the material.
KR1019970042162A 1997-08-28 1997-08-28 A Method of Manufacturing Dolomite Refractory Materials Having Superior Anti-Hydration KR100349165B1 (en)

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