JP2012072051A - Powder composition for fireproof castable, and fireproof castable using the same - Google Patents
Powder composition for fireproof castable, and fireproof castable using the same Download PDFInfo
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本発明は、耐火キャスタブル用粉体組成物及びそれを用いた耐火キャスタブルに係り、特に、加熱炉等の工業炉の内張層を形成するのに好適な耐火キャスタブル用粉体組成物及びそれを用いた耐火キャスタブルに関する。 The present invention relates to a refractory castable powder composition and a refractory castable using the same, and more particularly to a refractory castable powder composition suitable for forming an inner layer of an industrial furnace such as a heating furnace and the like. It relates to the fireproof castable used.
一般に加熱炉等の工業炉は、最も外側のケーシング（鉄皮とも称す）の内側に、不定形耐火物をライニングする。この不定形耐火物のライニングは、ケーシングに近いほうから、断熱ボード、断熱キャスタブル、耐火キャスタブルの順に３層構造とするのが、一般的である。 In general, industrial furnaces such as heating furnaces line an amorphous refractory inside the outermost casing (also referred to as an iron shell). The lining of this irregular refractory generally has a three-layer structure in the order of a heat insulation board, a heat insulation castable, and a fireproof castable from the side closer to the casing.
ところで、近年、地球温暖化による環境悪化が指摘され、ＣＯ２の排出量の低減の必要性から、省エネルギー化、省資源化のためにその性能向上が望まれており、耐火キャスタブルにおいても例外ではない。従来の性能を維持しながら、軽量で低熱伝導性の耐火キャスタブルは、熱損失が低減され、省エネルギー化、省資源化に寄与できる。更には、それ自体を軽量化することで、設置作業等を容易に行えるため省エネルギー化に寄与できる。また軽量化した分、資源の使用量も低減可能となり、省資源化に寄与できる。 By the way, in recent years, environmental deterioration due to global warming has been pointed out, and due to the necessity of reducing CO 2 emissions, it is desired to improve its performance in order to save energy and resources. Absent. A fireproof castable that is lightweight and has low thermal conductivity while maintaining the conventional performance can reduce heat loss and contribute to energy saving and resource saving. Furthermore, by reducing the weight itself, installation work and the like can be easily performed, which contributes to energy saving. In addition, the amount of resources used can be reduced and the amount of resources used can be reduced, contributing to resource saving.
したがって、高い破壊強度を有しながら、軽量で低熱伝導性を有する耐火キャスタブルが求められている。ところが、従来の耐火キャスタブルは、高い破壊強度が求められているため、緻密な組織から構成されており、質量が大きいものばかりであった。 Accordingly, there is a need for a fireproof castable that is lightweight and has low thermal conductivity while having high breaking strength. However, since conventional fire-resistant castables are required to have high breaking strength, they are composed of a dense structure and have only a large mass.
一方、従来のキャスタブルには、軽量化が図られているものがいくつか知られており、例えば、軽量骨材を用いたキャスタブルとして、セラミックファイバーを使用する断熱キャスタブル（特許文献１参照）、アルミナ中空粒子などの軽量骨材を使用した断熱キャスタブル（特許文献２〜４参照）、また、アルミニウム溶湯取鍋の内張材としてアルミナ中空粒子を使用したキャスタブル（特許文献５参照）が知られている。 On the other hand, some of the conventional castables are known to be reduced in weight. For example, as castables using lightweight aggregates, heat insulating castables using ceramic fibers (see Patent Document 1), alumina Heat-insulating castables using lightweight aggregates such as hollow particles (see Patent Documents 2 to 4), and castables using alumina hollow particles as a lining material for molten aluminum ladle (see Patent Document 5) are known. .
しかしながら、特許文献１に記載されたセラミックファイバーを使用した断熱キャスタブルは、１４００℃乾燥品の嵩比重が１．４以下であり、曲げ強さが５ＭＰａと低い。特許文献２に記載された中空粒子などの軽量骨材を使用した断熱キャスタブルは、１４００℃乾燥品の嵩比重が１．５以下であり、曲げ強さが１０ＭＰａ以下と低い。特許文献３に記載された中空粒子などの軽量骨材を使用した断熱キャスタブルは、１５００℃乾燥品の嵩比重が１．０以下であり、圧縮強さが２５ＭＰａ以下と低い。特許文献４に記載された中空粒子などの軽量骨材を使用した断熱キャスタブルは、１０００℃乾燥品の嵩比重が０．６以下であり、圧縮強さが１ＭＰａ以下と低い。特許文献５に記載されたアルミナ中空粒子を使用したキャスタブルは、１２００℃乾燥品の嵩比重が１．８以下であり、圧縮強さが２５ＭＰａ以下と低い。 However, the heat insulation castable using the ceramic fiber described in Patent Document 1 has a bulk specific gravity of 1.4 or less and a bending strength of 5 MPa as low as 1400 ° C. dry product. The heat insulating castable using a lightweight aggregate such as hollow particles described in Patent Document 2 has a bulk specific gravity of 1400 ° C. dry product of 1.5 or less and a low bending strength of 10 MPa or less. Insulated castables using lightweight aggregates such as hollow particles described in Patent Document 3 have a bulk specific gravity of a dried product of 1500 ° C. of 1.0 or less and a low compressive strength of 25 MPa or less. The heat insulating castable using a lightweight aggregate such as hollow particles described in Patent Document 4 has a bulk specific gravity of 0.6 ° C. or less and a compressive strength as low as 1 MPa or less. The castable using the alumina hollow particles described in Patent Document 5 has a bulk specific gravity of 1.8 ° C. or less and a compressive strength as low as 25 MPa or less.
以上のとおり、上記した従来の軽量のキャスタブルはいずれも破壊強度が低く、耐火キャスタブルとして用いるには性能が十分でなかった。 As described above, any of the conventional lightweight castables described above has a low breaking strength, and the performance is not sufficient for use as a fireproof castable.
そこで、本発明は、従来の耐火キャスタブルの特徴である、高い破壊強度を有しながら、軽量で低熱伝導性の耐火キャスタブルを形成可能な粉体組成物及びそれを用いた耐火キャスタブルの提供を目的とする。 Therefore, the present invention aims to provide a powder composition capable of forming a light-weight and low-heat-conductivity fire-resistant castable while having high breaking strength, which is a characteristic of conventional fire-resistant castable, and a fire-resistant castable using the same. And
本発明者らは、鋭意検討した結果、特定の中空粒子を耐火骨材として用いることで、上記課題を解決できることを見出し、本発明を完成した。すなわち、本発明の耐火キャスタブル用粉体組成物は、アルミナ−ジルコニア質中空粒子、を必須成分として含有する耐火キャスタブル用粉体組成物であって、前記アルミナ−ジルコニア質中空粒子が、Ａｌ２Ｏ３を６７〜９９質量％、ＺｒＯ２を１〜３３質量％、かつ、Ａｌ２Ｏ３とＺｒＯ２の合量が９６質量％以上であるアルミナ−ジルコニア質中空粒子を含有することを特徴とする。 As a result of intensive studies, the present inventors have found that the above-mentioned problems can be solved by using specific hollow particles as a refractory aggregate, and have completed the present invention. That is, the refractory castable powder composition of the present invention is a refractory castable powder composition containing alumina-zirconia hollow particles as an essential component, and the alumina-zirconia hollow particles are Al 2 O. 3 to 67% by mass, ZrO 2 is 1% to 33% by mass, and the total content of Al 2 O 3 and ZrO 2 is 96% by mass or more, containing alumina-zirconia hollow particles. .
また、本発明の耐火キャスタブルは、上記本発明の耐火キャスタブル用粉体組成物に、水分を添加し混練して施工することで得られる。 The fire-resistant castable of the present invention can be obtained by adding water to the above-mentioned powder composition for fire-resistant castable of the present invention and kneading it.
本発明の耐火キャスタブル用粉体組成物によれば、アルミナ−ジルコニア質中空粒子という軽量の新規の骨材を使用することで、従来の軽量骨材を使用した断熱キャスタブルでは得られなかった高い破壊強度を有し、軽量で低熱伝導性の耐火キャスタブルが得られる。 According to the powder composition for refractory castables of the present invention, by using a lightweight new aggregate called alumina-zirconia hollow particles, high fracture that cannot be obtained by conventional heat-insulated castable using lightweight aggregate. A fireproof castable having strength, light weight and low thermal conductivity is obtained.
また、本発明の耐火キャスタブルによれば、従来軽量化が困難であった耐火キャスタブルの軽量化を可能とし、省エネルギー化、省資源化に寄与できる。 In addition, according to the fireproof castable of the present invention, it is possible to reduce the weight of the fireproof castable, which has been difficult to reduce in the prior art, and contribute to energy saving and resource saving.
本発明の耐火キャスタブル用粉体組成物は、高い破壊強度を有し、軽量で低熱伝導性の耐火キャスタブルを形成可能な耐火キャスタブル用粉体組成物であり、所定の骨材を必須成分として含む。なお、本明細書において、粉体組成物に含まれる成分量について使用されている、「内掛け」とは、粉体組成物全体（外掛け表示成分を含まない）を１００質量％としたとき、１００質量％の中でのそれぞれの成分割合をいう。例えば、耐火骨材を内掛けで９０質量％含むとは、該耐火骨材の含有量を含めた粉体組成物全体（外掛け表示成分を含まない）を１００質量％とし、かかる１００質量％中、耐火骨材を９０質量％含むことをいう。一方、「外掛け」とは、粉体組成物全体（外掛け表示成分を含まない）を１００質量％としたとき、かかる１００質量％に含まれていない成分の耐火物全体（外掛け表示成分を含まない）を基準にした割合をいう。例えば、添加剤を外掛けで０．１質量％とは、該添加剤を含まない粉体組成物全体（外掛け表示成分を含まない）を１００質量％として、添加剤を付加的に０．１質量％含むことをいう。 The powder composition for a fire-resistant castable according to the present invention is a powder composition for a fire-resistant castable that has a high breaking strength and can form a light-weight and low thermal conductive fire-resistant castable, and includes a predetermined aggregate as an essential component. . In this specification, “inner coating” used for the amount of components contained in the powder composition is when the entire powder composition (excluding outer display components) is 100% by mass. , Each component ratio in 100% by mass. For example, the inclusion of 90% by mass of refractory aggregate in the interior means that the entire powder composition including the content of the refractory aggregate (excluding the outer display component) is 100% by mass, and 100% by mass In the middle, it means containing 90% by mass of refractory aggregate. On the other hand, “outer covering” means that the entire powder composition (excluding the outer display component) is 100% by mass, and the entire refractory component not included in the 100% by mass (outer display component) (Not including)). For example, 0.1% by mass of the additive as an outer coating is 100% by mass of the entire powder composition not including the additive (excluding the outer display component), and the additive is further added to an amount of 0.1% by mass. 1% by mass is included.
本発明の耐火キャスタブル用粉体組成物は、耐火骨材と、水硬性結合剤とからなり、耐火骨材としては、アルミナ−ジルコニア質中空粒子からなる軽量耐火骨材を必須成分として挙げられる。なお、本明細書において、骨材とは平均粒径が２０μｍ超の粒子をいう。 The powder composition for fireproof castables of the present invention comprises a fireproof aggregate and a hydraulic binder, and the fireproof aggregate includes a lightweight fireproof aggregate composed of alumina-zirconia hollow particles as an essential component. In the present specification, aggregate means particles having an average particle diameter of more than 20 μm.
本発明で用いる軽量耐火骨材は、その化学成分としてＡｌ２Ｏ３成分及びＺｒＯ２成分を必須成分とし、そのＡｌ２Ｏ３成分の含有量を６７〜９９質量％、ＺｒＯ２成分の含有量を１〜３３質量％、かつ、それらの合量（Ａｌ２Ｏ３＋ＺｒＯ２）が９６質量％以上としたアルミナ−ジルコニア質中空粒子である。 Lightweight refractory aggregate used in the present invention, the Al 2 O 3 component and ZrO 2 component as essential components as its chemical composition, the content of Al 2 O 3 component 67-99% by weight, the content of the ZrO 2 component 1 to 33% by mass, and the total amount thereof (Al 2 O 3 + ZrO 2 ) is 96% by mass or more of alumina-zirconia hollow particles.
Ａｌ２Ｏ３成分の含有量が６７質量％未満、ＺｒＯ２成分の含有量が３３質量％を超えると、ジルコニア比率が高くなるためジルコニアの相転移に伴う体積変化を吸収しきれず、粒子に亀裂が生じやすくなり、粒子強度の低下のおそれがある。また、アルミナに比べて比重の大きいジルコニアの比率が高くなるため質量が重くなり、目的の一つである軽量化の点で問題となる。さらに、ジルコニアは原料単価が高いため、製造原価の点でも問題となるおそれがある。一方、Ａｌ２Ｏ３成分の含有量が９９質量％を超え、ＺｒＯ２成分の含有量が１質量％未満であると、破壊強度が十分に確保できなくなる。また、アルミナよりも熱伝導率の低いジルコニアが少量となり、熱伝導の低下効果が減少する。さらに、アルミニウム、ガラス、アルカリなどに対する耐食性に優れるジルコニアが少量となると、耐食性が十分に確保できなくなる。そして、ジルコニアが少量となることで中空粒子の質量が軽くなるため、耐火キャスタブルの施工中に中空粒子が浮き上がり、材料分離が発生するおそれがある。
本発明で用いる軽量耐火骨材は、Ａｌ２Ｏ３成分の含有量が６８質量％以上で、かつ、ＺｒＯ２成分の含有量が３２質量％以下であると同様の理由で好ましい。
When the content of the Al 2 O 3 component is less than 67% by mass and the content of the ZrO 2 component is more than 33% by mass, the zirconia ratio increases, so the volume change associated with the phase transition of zirconia cannot be absorbed and the particles crack. May occur, and the particle strength may be reduced. Further, since the ratio of zirconia having a larger specific gravity than alumina is increased, the mass is increased, which is a problem in terms of weight reduction, which is one of the purposes. Furthermore, since zirconia has a high raw material unit price, there is a possibility that it may become a problem also in terms of manufacturing cost. On the other hand, if the content of the Al 2 O 3 component exceeds 99% by mass and the content of the ZrO 2 component is less than 1% by mass, sufficient fracture strength cannot be ensured. Further, the amount of zirconia having a lower thermal conductivity than that of alumina is reduced, and the effect of lowering thermal conductivity is reduced. Furthermore, if the amount of zirconia excellent in corrosion resistance against aluminum, glass, alkali, or the like is small, corrosion resistance cannot be sufficiently secured. And since the mass of a hollow particle will become light because a zirconia becomes small quantity, there exists a possibility that a hollow particle may float during construction of a fireproof castable, and material separation may generate | occur | produce.
The lightweight refractory aggregate used in the present invention is preferable for the same reason that the content of the Al 2 O 3 component is 68% by mass or more and the content of the ZrO 2 component is 32% by mass or less.
また、それらの合量（Ａｌ２Ｏ３＋ＺｒＯ２）が９６質量％未満であると、その他の成分が不純物となって存在するため、上記効果のバランスがとれず、本発明の目的とする特性を有する耐火骨材が得られない。また、軽量耐火物粒子を電融法により製造する場合には、前記合量が９６質量％未満であると、溶解温度が低下し過ぎて中空の軽量耐火骨材粒子が製造できないおそれもある。前記合量が９８質量％以上であると同様の理由で好ましい。 Further, when the total amount (Al 2 O 3 + ZrO 2 ) is less than 96% by mass, other components are present as impurities, so that the above effects cannot be balanced, and the target characteristics of the present invention. A refractory aggregate having the above cannot be obtained. Moreover, when manufacturing a lightweight refractory particle by an electromelting method, when the said total amount is less than 96 mass%, there exists a possibility that a melting temperature may fall too much and a hollow lightweight refractory aggregate particle cannot be manufactured. It is preferable for the same reason that the total amount is 98% by mass or more.
通常、ＺｒＯ２の常温で安定な結晶構造は単斜晶相であり、１１００℃前後で相転移して大きな体積変化を示すため、そのままでは焼結体の製造は難しい。一般的には、ＺｒＯ２成分を主成分とする耐火物原料ではＣａＯ等を添加して立方晶に安定化して使用される。 Usually, a stable crystal structure of ZrO 2 at room temperature is a monoclinic phase, and phase transition occurs at around 1100 ° C. and shows a large volume change. Therefore, it is difficult to produce a sintered body as it is. In general, a refractory raw material containing a ZrO 2 component as a main component is used by stabilizing it into cubic crystals by adding CaO or the like.
これに対し、上記のようにＡｌ２Ｏ３成分及びＺｒＯ２成分を所定割合で配合し、コランダム鉱物とバデライト鉱物が複雑に絡んだ構造とすることで、高温で安定化されていない単斜晶相からなるＺｒＯ２を含有していても、熱的に安定な耐火骨材とできる。具体的には、ＺｒＯ２成分の転移する温度をまたいで熱サイクルを与えても粒子に亀裂が入ることを効果的に抑制し、耐火物原料として使用することを可能とした。 In contrast, a monoclinic crystal that is not stabilized at high temperature by blending Al 2 O 3 component and ZrO 2 component in a predetermined ratio as described above, and having a structure in which a corundum mineral and a badelite mineral are entangled in a complicated manner. Even if it contains ZrO 2 composed of a phase, a thermally stable refractory aggregate can be obtained. Specifically, even if a thermal cycle is applied across the temperature at which the ZrO 2 component transitions, cracking of the particles is effectively suppressed, and it can be used as a refractory material.
なお、ＺｒＯ２成分の含有量は、粒子が破砕しにくい充分な強度を有し、低熱伝導性、耐食性を付与する観点から３質量％以上が好ましく、また、ジルコニアの転移温度をまたぐ、８５０℃〜１２５０℃の熱履歴を与えても粒子に亀裂が発生するのを効果的に抑制できる点から、３１．５質量％以下が好ましい。ＺｒＯ２成分の含有量が３１質量％以下であるとさらに好ましい。 Note that the content of the ZrO 2 component is preferably 3% by mass or more from the viewpoint of giving sufficient strength that the particles are not easily crushed, imparting low thermal conductivity and corrosion resistance, and straddling the transition temperature of zirconia, 850 ° C. From the point which can suppress effectively that a crack generate | occur | produces in particle | grains, even if it gives a heat history of -1250 degreeC, 31.5 mass% or less is preferable. More preferably, the content of the ZrO 2 component is 31% by mass or less.
この軽量耐火骨材は、その最大粒径が４．０ｍｍを超えると、耐火キャスタブルの破壊強度が低下するおそれがあるので、本発明の耐火キャスタブル用粉体組成物において、軽量耐火骨材の最大粒径は４．０ｍｍ以下が好ましい。さらに、この軽量耐火骨材の粒径が２．５ｍｍ以下であると、破壊強度が高まるためさらに好ましい。 If the maximum particle size of the lightweight refractory aggregate exceeds 4.0 mm, the fracture strength of the refractory castable may be reduced. Therefore, in the refractory castable powder composition of the present invention, The particle size is preferably 4.0 mm or less. Furthermore, it is more preferable that the particle size of the lightweight refractory aggregate is 2.5 mm or less because the fracture strength increases.
本発明に用いる軽量耐火骨材は、耐火骨材として、それを適用した耐火物の耐火性を高められ、その溶解温度（融点）は１７００℃以上が軽量、良好な断熱性、かつ良好な耐熱性をバランスさせる点で好ましい。溶解温度は１７５０℃以上がさらに好ましく、１８００℃以上が特に好ましい。なお、耐火物の耐熱性は、耐火度で表現することもあるが、上記溶解温度は、耐火度としては、ＳＫ番号表示で３９〜４２に相当する。 The light-weight refractory aggregate used in the present invention can enhance the fire resistance of a refractory to which the light-weight refractory aggregate is applied, and its melting temperature (melting point) is 1700 ° C. or higher in light weight, good heat insulation, and good heat resistance. It is preferable in terms of balancing the properties. The melting temperature is more preferably 1750 ° C. or higher, and particularly preferably 1800 ° C. or higher. In addition, although the heat resistance of a refractory may be expressed by a fire resistance, the said melting temperature is equivalent to 39-42 by a SK number display as a fire resistance.
さらに、この軽量耐火骨材は、耐火物の品質を向上させるなどの観点から実用的な強度を有することが求められる。本発明に用いる軽量耐火骨材は、Ａｌ２Ｏ３成分及びＺｒＯ２成分を併用したことにより、Ａｌ２Ｏ３成分単独で構成された耐火骨材よりも強度が高い。そのため、この軽量耐火骨材で耐火物を構成した際に骨材が破損したりする等により、耐火物の形状や性能が変動することを抑制し、安定した耐火物とできる。 Furthermore, this lightweight refractory aggregate is required to have practical strength from the viewpoint of improving the quality of the refractory. The lightweight refractory aggregate used in the present invention has higher strength than the refractory aggregate composed of the Al 2 O 3 component alone by using the Al 2 O 3 component and the ZrO 2 component together. For this reason, when the refractory is composed of this lightweight refractory aggregate, the aggregate is damaged or the like, so that the shape and performance of the refractory are prevented from fluctuating and a stable refractory can be obtained.
上記に説明した本発明の軽量耐火骨材は、その原料としてＡｌ２Ｏ３及びＺｒＯ２原料を所定の配合比率に混合し、Ａｌ２Ｏ３成分及びＺｒＯ２成分を、それぞれ得られるＡｌ２Ｏ３成分及びＺｒＯ２成分の比で含有するようにして、軽量耐火骨材の出発原料とする。 Lightweight refractory aggregate of the present invention described above, the Al 2 O 3 and ZrO 2 raw material mixed in a predetermined mixing ratio as a starting material, the Al 2 O 3 component and ZrO 2 component, Al 2 O respectively obtained It is used as a starting material for a lightweight refractory aggregate so as to be contained in a ratio of 3 components and 2 components of ZrO.
軽量耐火骨材の製造方法としては、焼結法又は電融−風砕法が一般的に用いられる。前者では有機物などの球状粒子を芯材としてその周囲に原料を絡め、焼成することにより、有機物などの芯材を揮発させ中空耐火物原料を製造する。また後者では国際公開第２００９／０７２６２７号公報に記載されているように、所定の組成の原料をアーク式の電気炉などで溶解し、その溶解原料に高圧の空気などを吹き付けて中空粒子化する方法がある。本発明の軽量耐火骨材を得るには、いずれの方法を用いることも可能であるが、製造コストの面から電融法が有利である。 As a method for producing a lightweight refractory aggregate, a sintering method or an electromelting-blasting method is generally used. In the former, a spherical refractory material is produced by volatilizing a core material such as an organic material by entangling and firing the raw material around the spherical particles such as an organic material and firing it. In the latter case, as described in International Publication No. 2009/072627, a raw material having a predetermined composition is melted in an arc-type electric furnace or the like, and high-pressure air or the like is sprayed on the molten raw material to form hollow particles. There is a way. Any method can be used to obtain the lightweight refractory aggregate of the present invention, but the electrofusion method is advantageous from the viewpoint of manufacturing cost.
また、焼結法では組成を自由に選ぶことが可能であるが、電融法では、Ａｌ２Ｏ３成分及びＺｒＯ２成分の合量が、９６質量％以上が好ましく、９８質量％以上がより好ましく、９９．３質量％以上が特に好ましい。電融法においては、不純物成分値が高くなると一般的に原料の溶融温度の低下を招き、結果として中空粒子が製造できないか、もしくは嵩比重が低下せず、軽量を実現する中空の耐火骨材を得られない場合がある。 Further, the composition can be freely selected in the sintering method, but in the electromelting method, the total amount of the Al 2 O 3 component and the ZrO 2 component is preferably 96% by mass or more, more preferably 98% by mass or more. Preferably, 99.3% by mass or more is particularly preferable. In the electromelting method, when the impurity component value increases, the melting temperature of the raw material is generally lowered, and as a result, hollow particles cannot be produced, or the bulk specific gravity does not decrease, and a hollow refractory aggregate that realizes light weight You may not get.
また、その製造方法による製造過程で、不純物成分がなくなる場合には、原料としてそのような成分が含まれていても問題ない。例えば、国際公開第２００９／０７２６２７号公報に記載されているように、使用済みの耐火物をリサイクルして、Ａｌ２Ｏ３成分及びＺｒＯ２成分の含有量を高純度化し、高酸化性の耐火物粒子を簡便かつ、生産性良く製造する電融法による耐火物粒子の製造方法を用いてもよい。 Further, when the impurity component is eliminated during the manufacturing process by the manufacturing method, there is no problem even if such a component is included as a raw material. For example, as described in International Publication No. 2009/072627, the used refractory is recycled to increase the content of the Al 2 O 3 component and the ZrO 2 component, thereby increasing the oxidation resistance of the fire. You may use the manufacturing method of the refractory particle by the electromelting method which manufactures a product particle simply and with sufficient productivity.
本発明の耐火骨材としては、上記した軽量耐火骨材の他に、一般的に耐火物の原料として使用されている、例えば、アルミナ、ボーキサイト、ムライト、アンダルサイト、シャモット、シリカ、炭化ケイ素、ジルコン、ジルコニア、マグネシア、スピネルなどの公知の耐火骨材が使用できる。 As the refractory aggregate of the present invention, in addition to the above-mentioned lightweight refractory aggregate, it is generally used as a raw material for refractories, such as alumina, bauxite, mullite, andalusite, chamotte, silica, silicon carbide, Known fireproof aggregates such as zircon, zirconia, magnesia and spinel can be used.
本発明の耐火キャスタブル用粉体組成物は、上記した軽量耐火骨材と従来公知の耐火骨材から選ばれる少なくとも１種の耐火骨材と、を併用することが好ましい。このように併用した場合には、形式的には、従来の耐火キャスタブル用粉体組成物の耐火骨材の一部を、アルミナ−ジルコニア質中空粒子で置換したものとなる。このような構成とすることで、従来の耐火キャスタブルの特徴である高い破壊強度、を維持しながら、軽量で低熱伝導性という特性をも得られる。 In the fire-resistant castable powder composition of the present invention, it is preferable to use the light-weight fire-resistant aggregate described above and at least one fire-resistant aggregate selected from conventionally known fire-resistant aggregates in combination. When used in this manner, formally, a part of the refractory aggregate of the conventional powder composition for refractory castable is replaced with alumina-zirconia hollow particles. By adopting such a configuration, it is possible to obtain the characteristics of light weight and low thermal conductivity while maintaining the high breaking strength characteristic of the conventional fireproof castable.
また、本発明の耐火キャスタブル用粉体組成物中における、アルミナ−ジルコニア質中空粒子の含有量を内掛けで５〜６５質量％、残りを従来公知の耐火骨材として、耐火骨材を構成すると、本発明の耐火キャスタブル用粉体組成物の施工体の嵩比重および破壊強度がよりバランスよく確保されるため好ましい。本発明の耐火キャスタブル用粉体組成物において、アルミナ−ジルコニア質中空粒子の含有量が内掛けで１０〜６０質量％であるとより好ましく、アルミナ−ジルコニア質中空粒子の含有量が内掛けで４０〜５５質量％であると特に好ましい。 Further, in the powder composition for fireproof castable of the present invention, when the content of the alumina-zirconia hollow particles is 5 to 65% by mass in the inner portion, and the rest is a conventionally known fireproof aggregate, the fireproof aggregate is constituted. Since the bulk specific gravity and the breaking strength of the construction body of the powder composition for fireproof castable of the present invention are ensured in a better balance, it is preferable. In the refractory castable powder composition of the present invention, the content of the alumina-zirconia hollow particles is more preferably 10 to 60% by mass, and the content of the alumina-zirconia hollow particles is 40 It is especially preferable that it is -55 mass%.
本発明の耐火キャスタブル用粉体組成物においては、アルミナ−ジルコニア質中空粒子以外の軽量骨材を含んでいてもよい。ここでいう軽量骨材は、アルミナ中空粒、ジルコニア中空粒、ＣＡ６質軽量骨材などが挙げられる。 The refractory castable powder composition of the present invention may contain lightweight aggregates other than the alumina-zirconia hollow particles. Examples of the lightweight aggregate include alumina hollow particles, zirconia hollow particles, and CA6 lightweight lightweight aggregate.
次に、本発明に用いる水硬性結合剤は、アルミナセメントを必須成分とし、必要に応じてシリカ超微粉やアルミナ超微粉、分散剤、硬化調整剤を含有する。また、フッ化アルミニウムやフッ化カルシウムなどの浸透抑制剤を含有させ、アルミニウム溶湯の浸透を抑制することもできる。このほか、添加剤を含ませることによって、さまざまな機能が付与できる。 Next, the hydraulic binder used in the present invention contains alumina cement as an essential component, and contains ultrafine silica powder, ultrafine alumina powder, a dispersant, and a curing modifier as necessary. In addition, a penetration inhibitor such as aluminum fluoride or calcium fluoride can be contained to inhibit the penetration of molten aluminum. In addition, various functions can be imparted by adding additives.
ここで、本発明で用いられるアルミナセメントは、上記骨材のバインダーとして機能し、主鉱物がアルミン酸カルシウムからなる。耐熱性の問題から、１９９５年のＪＩＳ規格（Ｒ−２５１１）によるところの１種〜５種のアルミナセメントが用いられる。 Here, the alumina cement used in the present invention functions as a binder for the aggregate, and the main mineral is calcium aluminate. From the problem of heat resistance, 1 to 5 types of alumina cement according to the JIS standard (R-2511) of 1995 is used.
シリカ超微粉は、従来、耐火キャスタブル用粉体組成物に用いられているシリカ微粉であればよく、平均粒径が２０μｍ以下のシリカ粉末であり、ＳｉＯ２含有量が９０％以上であるシリカ微粒子が好ましく、１μｍ未満がより好ましい。シリカ微粒子としては、具体的にはシリカヒュームなどが挙げられる。 Ultrafine silica fine powder, conventionally, may be a silica fine powder used in the refractory castable powder composition for an average particle size of less silica powder 20 [mu] m, the silica fine particles SiO 2 content of 90% or more Is preferable, and less than 1 μm is more preferable. Specific examples of the silica fine particles include silica fume.
また、アルミナ超微粉は、従来、耐火キャスタブル用粉体組成物に用いられているアルミナ微粉であればよく、それ自体の凝集力が強く、耐火物用粉体組成物を耐火物とする際に硬化を促進する作用を有する。このアルミナ微粉は、平均粒径が２０μｍ以下のアルミナ粉末であり、仮焼アルミナが好ましい。このとき、アルミナ微粉は、その凝集により耐火物の硬化を促進する観点から、平均粒径が１０μｍ未満の粒子を用いられ、５μｍ未満が好ましい。 The alumina ultrafine powder may be any alumina fine powder conventionally used in powder compositions for refractory castables, and its own cohesive strength is strong. When the refractory powder composition is used as a refractory, Has the effect of promoting curing. The alumina fine powder is an alumina powder having an average particle diameter of 20 μm or less, and calcined alumina is preferable. At this time, from the viewpoint of accelerating the hardening of the refractory due to the aggregation, the fine alumina particles are particles having an average particle diameter of less than 10 μm, and preferably less than 5 μm.
本発明の耐火キャスタブル用粉体組成物は、所要の水分を添加後、ミキサーを用いて混練して坏土とし、それを所定の型枠の中に流し込んだ後、乾燥させて耐火キャスタブル（施工体）とする。 The powder composition for refractory castables of the present invention, after adding the required moisture, kneaded using a mixer to form a clay, poured it into a predetermined formwork, dried and fire-resistant castable (construction) Body).
本発明の耐火キャスタブル用粉体組成物を使用した流し込み施工方法では、上記所要の水分量としては、本発明の耐火キャスタブル用粉体組成物１００質量部に対して、３〜１５質量部とし、それを前記粉体組成物に添加することが好ましい。言い換えれば、外掛けで３〜１５質量％の水分を添加するのが好ましい。水分量が外掛けで３質量％未満であると、施工ができないおそれがあり、一方、水分量が外掛けで１５質量％を超えると骨材と添加水分との分離のおそれがある。 In the casting construction method using the powder composition for refractory castables of the present invention, the required water content is 3 to 15 parts by mass with respect to 100 parts by mass of the powder composition for refractory castables of the present invention, It is preferable to add it to the powder composition. In other words, it is preferable to add 3 to 15% by mass of water as an outer shell. If the moisture content is less than 3% by mass, the construction may not be possible. On the other hand, if the moisture content exceeds 15% by mass, the aggregate and the added moisture may be separated.
本施工方法の混練用ミキサーとしては、粉体組成物及び添加水を均一に混合できるものであれば特段制限されず、汎用のミキサーが使用される。 The mixer for kneading in this construction method is not particularly limited as long as the powder composition and the added water can be mixed uniformly, and a general-purpose mixer is used.
本発明の耐火キャスタブルは、上記したように軽量で低熱伝導性であり、破壊強度の大きいキャスタブルである。耐火キャスタブルの特性として、具体的には、その嵩比重は１．５以上が好ましく、１．５〜２．６がより好ましい。また、この耐火キャスタブルの熱伝導率は２．８（Ｗ／（ｍ・Ｋ））以下が好ましく、２．０（Ｗ／（ｍ・Ｋ））以下がより好ましい。圧縮強さは２５ＭＰａ以上が好ましく、５０ＭＰａ以上がより好ましい。 As described above, the fireproof castable of the present invention is a castable that is lightweight, has low thermal conductivity, and has a high breaking strength. Specifically, as a fireproof castable property, the bulk specific gravity is preferably 1.5 or more, and more preferably 1.5 to 2.6. The heat conductivity of the refractory castable is preferably 2.8 (W / (m · K)) or less, more preferably 2.0 (W / (m · K)) or less. The compressive strength is preferably 25 MPa or more, and more preferably 50 MPa or more.
以下、本発明の耐火キャスタブルの例を実施例（例１〜例３、例５〜例７）及び従来の耐火キャスタブルの例を比較例（例４、例８）で説明する。なお、本願発明は、これら実施例に限定されない。 Examples of fireproof castables according to the present invention will be described below in Examples (Examples 1 to 3, Examples 5 to 7) and conventional fireproof castables in Comparative Examples (Examples 4 and 8). The present invention is not limited to these examples.
［耐火軽量骨材の調製］
炉内径直径８００ｍｍ、高さ６００ｍｍ、炉内容積０．６ｍ３のアーク式溶融炉を試験炉として使用し、トランスとしては５００ｋＶＡを使用した。なお、溶融炉の内張耐火物は、Ａｌ２Ｏ３含有量９７％以上の電鋳耐火物を使用した。
[Preparation of fireproof lightweight aggregate]
An arc melting furnace having a furnace inner diameter of 800 mm, a height of 600 mm, and a furnace volume of 0.6 m3 was used as a test furnace, and a transformer of 500 kVA was used. As the lining refractory for the melting furnace, an electroformed refractory having an Al 2 O 3 content of 97% or more was used.
Ａｌ２Ｏ３原料としては９９．３％以上の純度のバイヤーアルミナ、ＺｒＯ２原料としては９９．５％以上の純度の電融ジルコニアカレットを用い、これら原料を所定の組成に混合して、最終的にＡｌ２Ｏ３成分及びＺｒＯ２成分が表１の割合（質量％）となるように溶融原料とした。 As the Al 2 O 3 raw material, buyer alumina having a purity of 99.3% or higher is used, and as the ZrO 2 raw material, a fused zirconia cullet having a purity of 99.5% or higher is used. In particular, the molten raw material was used so that the Al 2 O 3 component and the ZrO 2 component had the ratio (mass%) shown in Table 1.
これらの溶融原料を電気炉で溶融した。溶融条件は電圧１００−３００Ｖ、電力１００〜４００ｋＷで、溶融用混合原料の全体投入時間は２０〜３０分であった。溶解に必要とした電力は１トン当たり約２０００ｋＷｈであった。 These molten raw materials were melted in an electric furnace. The melting conditions were a voltage of 100 to 300 V, an electric power of 100 to 400 kW, and the total charging time of the mixing raw material for melting was 20 to 30 minutes. The electric power required for melting was about 2000 kWh per ton.
次に、圧力４ＭＰａの圧縮空気に０．４Ｌ／秒の水を加え、圧縮空気を水と共に溶融物の下方から前方に向けて出湯された溶融物に吹付けて、溶融物を粒子化した。粒子は耐火物で保護された金属製の捕集容器にて回収し、耐火物粒子とした。このときの圧縮空気の流速は１００ｍ／秒であった。 Next, 0.4 L / sec of water was added to the compressed air having a pressure of 4 MPa, and the compressed air was sprayed together with water onto the melt that was discharged from the bottom of the melt toward the front, thereby granulating the melt. The particles were collected in a metal collection container protected with a refractory material to form refractory particles. The flow rate of the compressed air at this time was 100 m / second.
この溶融法により得られた粒子の粒度は９５％以上が、０．１〜４ｍｍの範囲であり、９８％以上が０．０５〜１５ｍｍの範囲であった。このとき粒度のピークは１．２ｍｍであった。 The particle size of the particles obtained by this melting method was 95% or more in the range of 0.1 to 4 mm, and 98% or more was in the range of 0.05 to 15 mm. At this time, the particle size peak was 1.2 mm.
ここで得られたアルミナ・ジルコニア中空粒子１（表中、ＡＺ中空粒子１と略記）の化学成分は、Ａｌ２Ｏ３量；６８．２質量％、ＺｒＯ２量；３１．４質量％、その他；０．４質量％であり、アルミナ・ジルコニア中空粒子２（表中、ＡＺ中空粒子２と略記）の化学成分は、Ａｌ２Ｏ３量；９３．１質量％、ＺｒＯ２量；６．４質量％、その他；０．５質量％である。 The chemical components of the obtained alumina / zirconia hollow particles 1 (abbreviated as AZ hollow particles 1 in the table) are Al 2 O 3 amount; 68.2% by mass, ZrO 2 amount; 31.4% by mass, and others. The chemical component of the alumina / zirconia hollow particles 2 (abbreviated as AZ hollow particles 2 in the table) is Al 2 O 3 amount; 93.1% by mass, ZrO 2 amount; 6.4; % By mass, other: 0.5% by mass.
本実施例で用いるＡＺ中空粒子の化学成分を蛍光Ｘ線回折装置（リガク社製）により分析した結果及びその他特性を調べた結果を表１に示す。 Table 1 shows the results of analyzing the chemical components of the AZ hollow particles used in this example with a fluorescent X-ray diffractometer (manufactured by Rigaku Corporation) and other characteristics.
〔嵩比重〕
嵩比重は、体積既知の容器に０．１〜１．０ｍｍの中空粒子を軽く三回タップし充填し、擦りきり後の質量を測定して算出した。粒子の粒径を揃えた理由は、変動要素を軽減するためである。
[Bulk specific gravity]
The bulk specific gravity was calculated by lightly tapping 0.1 to 1.0 mm of hollow particles in a container with a known volume, filling it three times, and measuring the mass after rubbing. The reason why the particle diameters are made uniform is to reduce the variation factor.
〔熱伝導率〕
中空粒子のサンプルについて常温（２０℃）、５００℃、１０００℃の熱伝導率（Ｗ／（ｍ・Ｋ））を測定した。熱伝導率の測定に用いた粒子は、０．１ｍｍ〜１．０ｍｍの粒径を有するもので篩により分級した粒子を使用した。熱伝導率の測定には高温熱伝導率自動測定装置（スペインラボ社製、商品名：ＨＭＷ−１５）を用いた。
〔Thermal conductivity〕
The samples of the hollow particles were measured for thermal conductivity (W / (m · K)) at room temperature (20 ° C.), 500 ° C., and 1000 ° C. The particles used for the measurement of the thermal conductivity were particles having a particle size of 0.1 mm to 1.0 mm and classified by a sieve. A high-temperature thermal conductivity automatic measurement device (manufactured by Spain Laboratories, trade name: HMW-15) was used for measurement of thermal conductivity.
［耐火キャスタブル用粉体組成物及び耐火キャスタブルの製造］
上記得られたＡＺ中空粒子１をその粒度が２．５ｍｍ〜０．１ｍｍとなるように篩により選別し、用いるＡＺ中空粒子１とした。
表２及び表３のＡＺ中空粒子配合量が０％である例４と例８は、従来の耐火キャスタブル用粉体組成物であり、例４と例８は市販の低セメントキャスタブル製品である。それ以外の例１〜例３は例４の、例５〜例７は例８のそれぞれの耐火キャスタブル用粉体組成物を目開きが０．１ｍｍの篩網で篩上と篩下に分け、篩上の耐火骨材の一部をＡＺ中空粒子１で置換し、篩下と再混合して粉体組成物とした例である。すなわち、篩上の耐火骨材をＡＺ中空粒子で所定量を置換した耐火キャスタブル用粉体組成物である。
[Production of refractory castable powder composition and refractory castable]
The obtained AZ hollow particles 1 were selected with a sieve so that the particle size was 2.5 mm to 0.1 mm, and used as AZ hollow particles 1 to be used.
Examples 4 and 8 in which the amount of AZ hollow particles in Tables 2 and 3 is 0% are conventional powder compositions for fire-resistant castable, and Examples 4 and 8 are commercially available low cement castable products. The other Examples 1 to 3 were divided into the refractory castable powder compositions of Example 4 and Example 5 to Example 8 in Example 8 with a sieve mesh having a mesh opening of 0.1 mm, above and below the sieve. This is an example in which a part of the refractory aggregate on the sieve is replaced with AZ hollow particles 1 and remixed with the sieve below to obtain a powder composition. That is, it is a powder composition for fireproof castable in which a predetermined amount of fireproof aggregate on the sieve is replaced with AZ hollow particles.
それぞれ表２及び表３に示した所定水分量を添加して、市販のミキサーで約３分混練して、坏土とし、それを型に流し込んでＪＩＳ Ｒ２５５３にしたがってサンプル（寸法：１６０ｍｍ×４０ｍｍ×４０ｍｍ）とした。得られた各サンプルについて、嵩比重はアルキメデス法により、曲げ・圧縮強さはＪＩＳ Ｒ２５５３に、熱伝導率はＪＩＳ Ｒ２６１６に、それぞれ準じて測定した。ここで、ＡＺ中空粒子の配合量は内掛の質量％である。 Predetermined amounts of water shown in Table 2 and Table 3 were added, kneaded for about 3 minutes with a commercially available mixer to form clay, poured into a mold, and a sample (size: 160 mm × 40 mm ×) according to JIS R2553 40 mm). About each obtained sample, bulk specific gravity was measured according to Archimedes method, bending and compressive strength according to JIS R2553, and thermal conductivity according to JIS R2616, respectively. Here, the blending amount of the AZ hollow particles is an inner mass%.
得られた結果を表２及び表３に示す。なお、表２の嵩比重、曲げ強さ、圧縮強さは、１４００℃で３時間乾燥後のサンプルについての値を、それぞれ示す。また、表３の嵩比重、曲げ強さ、圧縮強さは、１２００℃で３時間乾燥後のサンプルについての値を、それぞれ示す。熱伝導率は、いずれも４００℃で５時間乾燥したサンプルを１０００℃で測定した値を示す。 The obtained results are shown in Tables 2 and 3. In addition, the bulk specific gravity, the bending strength, and the compressive strength in Table 2 indicate values for the sample after drying at 1400 ° C. for 3 hours, respectively. Moreover, the bulk specific gravity, the bending strength, and the compressive strength in Table 3 indicate values for the sample after drying at 1200 ° C. for 3 hours, respectively. Thermal conductivity shows the value which measured the sample dried at 400 degreeC for 5 hours at 1000 degreeC.
以上に示したように、本発明の耐火キャスタブル用粉体組成物は、特定のアルミナ−ジルコニア中空粒子を従来の耐火骨材の一部に用いることで、得られる耐火キャスタブルの嵩比重を小さく、熱伝導性を低くできる。それでいて、破壊強度は耐火キャスタブルとして求められる強度を確保できる。 As shown above, the powder composition for fireproof castables of the present invention uses a specific alumina-zirconia hollow particle as a part of a conventional fireproof aggregate, thereby reducing the bulk specific gravity of the fireproof castable obtained, Thermal conductivity can be lowered. Nevertheless, the fracture strength can ensure the strength required as a fireproof castable.
本発明の耐火キャスタブル用粉体組成物は、従来の耐火キャスタブルの特徴である、高い破壊強度を有し、中空粒子を骨材としているため軽量で、かつ、熱伝導率が低いため断熱性が高く、高温環境下において用いる耐火物として広く使用できる。 The powder composition for refractory castables of the present invention has a high fracture strength, which is a characteristic of conventional refractory castables, is lightweight because it uses aggregates of hollow particles, and has low heat conductivity because of its low thermal conductivity. It is high and can be widely used as a refractory used in a high temperature environment.
Claims (5)
前記アルミナ−ジルコニア質中空粒子が、Ａｌ２Ｏ３を６７〜９９質量％、ＺｒＯ２を１〜３３質量％、かつ、Ａｌ２Ｏ３とＺｒＯ２の合量が９６質量％以上であるアルミナ−ジルコニア質中空粒子を含有することを特徴とする耐火キャスタブル用粉体組成物。 A fireproof castable powder composition containing alumina-zirconia hollow particles as an essential component,
The alumina-zirconia hollow particles have an Al 2 O 3 content of 67 to 99% by mass, a ZrO 2 content of 1 to 33% by mass, and a total content of Al 2 O 3 and ZrO 2 of 96% by mass or more. A powder composition for refractory castables, comprising zirconia hollow particles.
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| JP2011184316A JP2012072051A (en) | 2010-08-31 | 2011-08-26 | Powder composition for fireproof castable, and fireproof castable using the same |
| CN2011102587789A CN102432307A (en) | 2010-08-31 | 2011-08-31 | Powder composition for refractory castable and refractory castable using same |
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| CN107740031A (en) * | 2017-12-12 | 2018-02-27 | 苏州炻原新材料科技有限公司 | A kind of shell structure Zirconium oxide powder used for hot spraying |
| CN115108843A (en) * | 2022-06-27 | 2022-09-27 | 山西禄纬堡太钢耐火材料有限公司 | Long-life anti-stripping 90t electric arc furnace top mullite prefabricated member and preparation method thereof |
| CN115650749A (en) * | 2022-11-30 | 2023-01-31 | 长兴兴鹰新型耐火建材有限公司 | Anti-skinning high-strength castable |
| CN116462521A (en) * | 2023-05-04 | 2023-07-21 | 武汉科技大学 | Method for preparing lightweight heat-insulating refractory castable from residues generated in production of magnesium hydroxide by bischofite |
| CN117209283A (en) * | 2023-09-14 | 2023-12-12 | 东台市圣德尔耐热材料有限公司 | Light heat-insulating refractory material for tunnel kiln wall and preparation process thereof |
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2011
- 2011-08-26 JP JP2011184316A patent/JP2012072051A/en not_active Withdrawn
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107740031A (en) * | 2017-12-12 | 2018-02-27 | 苏州炻原新材料科技有限公司 | A kind of shell structure Zirconium oxide powder used for hot spraying |
| CN115108843A (en) * | 2022-06-27 | 2022-09-27 | 山西禄纬堡太钢耐火材料有限公司 | Long-life anti-stripping 90t electric arc furnace top mullite prefabricated member and preparation method thereof |
| CN115108843B (en) * | 2022-06-27 | 2023-09-26 | 山西禄纬堡太钢耐火材料有限公司 | Long-life spalling-resistant 90t arc furnace roof mullite prefabricated part and preparation method thereof |
| CN115650749A (en) * | 2022-11-30 | 2023-01-31 | 长兴兴鹰新型耐火建材有限公司 | Anti-skinning high-strength castable |
| CN115650749B (en) * | 2022-11-30 | 2023-12-15 | 长兴兴鹰新型耐火建材有限公司 | Anti-skinning high-strength castable |
| CN116462521A (en) * | 2023-05-04 | 2023-07-21 | 武汉科技大学 | Method for preparing lightweight heat-insulating refractory castable from residues generated in production of magnesium hydroxide by bischofite |
| CN116462521B (en) * | 2023-05-04 | 2024-02-27 | 武汉科技大学 | Method for preparing lightweight heat-insulating refractory castable from residues generated in production of magnesium hydroxide by bischofite |
| CN117209283A (en) * | 2023-09-14 | 2023-12-12 | 东台市圣德尔耐热材料有限公司 | Light heat-insulating refractory material for tunnel kiln wall and preparation process thereof |
| CN117209283B (en) * | 2023-09-14 | 2024-02-13 | 东台市圣德尔耐热材料有限公司 | Light heat-insulating refractory material for tunnel kiln wall and preparation process thereof |
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