JP2018062435A - Method of producing alumina silica brick containing cordierite - Google Patents
Method of producing alumina silica brick containing cordierite Download PDFInfo
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- JP2018062435A JP2018062435A JP2016200167A JP2016200167A JP2018062435A JP 2018062435 A JP2018062435 A JP 2018062435A JP 2016200167 A JP2016200167 A JP 2016200167A JP 2016200167 A JP2016200167 A JP 2016200167A JP 2018062435 A JP2018062435 A JP 2018062435A
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- 229910052878 cordierite Inorganic materials 0.000 title claims abstract description 44
- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 239000011449 brick Substances 0.000 title claims abstract description 18
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 15
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title abstract description 4
- 238000000034 method Methods 0.000 title abstract description 4
- 239000002245 particle Substances 0.000 claims abstract description 27
- 239000002994 raw material Substances 0.000 claims abstract description 22
- 229910052851 sillimanite Inorganic materials 0.000 claims abstract description 13
- 229910052849 andalusite Inorganic materials 0.000 claims abstract description 12
- 239000004927 clay Substances 0.000 claims abstract description 9
- 239000011230 binding agent Substances 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 230000035939 shock Effects 0.000 abstract description 19
- 238000000465 moulding Methods 0.000 abstract description 4
- 150000001875 compounds Chemical class 0.000 abstract 2
- 230000007423 decrease Effects 0.000 description 8
- 238000010304 firing Methods 0.000 description 6
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 4
- 229910004298 SiO 2 Inorganic materials 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 239000000919 ceramic Substances 0.000 description 3
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000011819 refractory material Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 235000021167 banquet Nutrition 0.000 description 1
- 229910001570 bauxite Inorganic materials 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000011451 fired brick Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 229910052907 leucite Inorganic materials 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 229910052863 mullite Inorganic materials 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
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- Furnace Housings, Linings, Walls, And Ceilings (AREA)
Abstract
Description
本発明は、熱風炉の内張り耐火物やセラミックバーナーを構成する耐火物として好適に使用されるコージェライト含有アルミナ−シリカれんがの製造方法に関する。 The present invention relates to a method for producing a cordierite-containing alumina-silica brick that is suitably used as a refractory for a hot blast furnace lining refractory or a ceramic burner.
熱風炉の内張り耐火物には耐熱衝撃性と耐クリープ性が要求されるため、一般的にアルミナ−シリカれんがが使用されている。また、熱風炉のセラミックバーナーにおいては温度変動が苛酷なため耐熱衝撃性を最重要特性と考え、コージェライト含有アルミナ−シリカれんがが使用される場合もある。例えば、熱風炉のセラミックバーナーに使用されるコージェライト含有アルミナ−シリカれんがとしては、特許文献１に、シリマナイト、アンダリュサイト又はその双方に１０重量％以上のコージェライトを添加混合し焼成した耐火物が開示されている。 Alumina-silica brick is generally used because the refractory lining the hot-blast furnace is required to have thermal shock resistance and creep resistance. Moreover, in a ceramic burner of a hot stove, since temperature fluctuation is severe, thermal shock resistance is considered to be the most important characteristic, and cordierite-containing alumina-silica brick is sometimes used. For example, as a cordierite-containing alumina-silica brick used for a ceramic burner in a hot stove, a refractory obtained by adding and mixing 10% by weight or more of cordierite with sillimanite, andaludite or both in Patent Document 1. Is disclosed.
しかしながら近年は、熱風炉で高温熱風を発生する操業へ移りつつあり、熱風炉に使用される耐火物としてはより高い耐クリープ性と耐熱衝撃性が要求されるようになってきているところ、特許文献１のような従来のコージェライト含有アルミナ−シリカれんがでは、特に耐クリープ性に問題があり、前述のような高温での熱風炉の操業等では寿命のネックとなると考えられる。 However, in recent years, it has been shifting to an operation that generates high-temperature hot air in a hot air furnace, and as a refractory used in the hot air furnace, higher creep resistance and thermal shock resistance have been required. Conventional cordierite-containing alumina-silica bricks such as those in Literature 1 have a problem in creep resistance, and are considered to become a bottleneck in the life of hot stove operations at high temperatures as described above.
本発明が解決しようとする課題は、耐クリープ性を向上ししかも十分な耐熱衝撃性を有するコージェライト含有アルミナ−シリカれんがの製造方法を提供することにある。 The problem to be solved by the present invention is to provide a method for producing a cordierite-containing alumina-silica brick having improved creep resistance and sufficient thermal shock resistance.
本発明者らは、コージェライト含有アルミナ−シリカれんがにおいて耐クリープ性を向上するために耐火原料配合物中のコージェライトの粒度及び使用量について種々検討した結果、コージェライトの粒度が０．０７４ｍｍ未満の微粉を使用しないかあるいは５質量％以下とすることで大幅に耐クリープ性が向上することを知見した。さらに、粘土を結合組織とする場合には粒度が０．０７４ｍｍ以上のコージェライトは、３０質量％を超えると耐熱衝撃性が低下傾向となりしかも歩留りが低下することが分かった。 In order to improve the creep resistance in the cordierite-containing alumina-silica brick, the present inventors have conducted various studies on the cordierite particle size and the amount of use in the refractory raw material composition. As a result, the cordierite particle size is less than 0.074 mm. It was found that the creep resistance was greatly improved by using no fine powder of 5 or 5% by mass or less. Further, when clay is used as the connective structure, it has been found that when the cordierite having a particle size of 0.074 mm or more exceeds 30% by mass, the thermal shock resistance tends to decrease and the yield decreases.
すなわち、本発明のコージェライト含有アルミナ−シリカれんがの製造方法は、粒度が３ｍｍ未満のアンダリュサイト及び／又はシリマナイトを６０質量％以上８８質量％以下、粒度が０．０７４ｍｍ以上３ｍｍ未満のコージェライトを１０質量％以上３０質量％以下、及び粘土を２質量％以上１２質量％以下含有し、粒度が０．０７４ｍｍ未満のコージェライトの含有量が５質量％以下（０を含む。）である耐火原料配合物に、バインダーを添加して混練し、成形後、１１００℃以上１４００℃以下で焼成することを特徴とするものである。 That is, the method for producing the cordierite-containing alumina-silica brick according to the present invention is a cordierite having a particle size of less than 3 mm of andalusite and / or sillimanite of 60 to 88% by mass and a particle size of 0.074 to 3 mm. 10 mass% or more and 30 mass% or less, and clay is 2 mass% or more and 12 mass% or less, and the content of the cordierite whose particle size is less than 0.074 mm is 5 mass% or less (including 0). A binder is added to the raw material blend, kneaded, and after molding, fired at 1100 ° C. or higher and 1400 ° C. or lower.
以下、本発明を詳しく説明する。 The present invention will be described in detail below.
本発明において、粒度が３ｍｍ未満のアンダリュサイト及び／又はシリマナイトは十分な耐クリープ性を確保するために使用し、６０質量％未満では耐クリープ性が不足し、８８質量％を超えると耐熱衝撃性が低下する。 In the present invention, andalusite and / or sillimanite having a particle size of less than 3 mm is used to ensure sufficient creep resistance. If it is less than 60% by mass, the creep resistance is insufficient. Sexuality decreases.
粒度が０．０７４ｍｍ以上３ｍｍ未満のコージェライトは耐熱衝撃性を向上するために使用し、１０質量％未満では耐熱衝撃性が不十分となり、３０質量％を超えると耐熱衝撃性が逆に低下ししかも焼成後の歩留りの低下も問題となる。すなわち、コージェライトは熱膨張率が小さいため耐火原料配合物に使用することでれんがの熱膨張率が小さくなるため耐熱衝撃性は向上するが、使用量が多すぎると１１００℃程度の焼成でも粘土などと反応して組織が緻密化しガラスが生成するために耐熱衝撃性が低下する。焼成温度を下げると耐熱衝撃性の低下を抑制できるが、今度は粘土などの結合組織の発達が不十分となり耐クリープ性の低下が問題となる。 Cordierite with a particle size of 0.074 mm or more and less than 3 mm is used to improve the thermal shock resistance. If it is less than 10% by mass, the thermal shock resistance is insufficient, and if it exceeds 30% by mass, the thermal shock resistance is decreased. Moreover, a decrease in yield after firing is also a problem. That is, since cordierite has a small coefficient of thermal expansion, it can be used in a refractory raw material composition to reduce the coefficient of thermal expansion of bricks, so that the thermal shock resistance is improved. The thermal shock resistance is lowered because the structure is densified and glass is formed by reaction with the above. Lowering the firing temperature can suppress a decrease in thermal shock resistance, but this time, the development of a connective structure such as clay becomes insufficient, and a decrease in creep resistance becomes a problem.
粒度が０．０７４ｍｍ未満のコージェライトは耐クリープ性を低下させるために使用しないことが好ましいが、５質量％以下であれば大きな影響はないため使用することもできる。 Cordierite having a particle size of less than 0.074 mm is preferably not used in order to reduce creep resistance. However, if it is 5% by mass or less, it can be used because there is no significant influence.
粘土は、焼成によって結合組織を形成するために２質量％以上１２質量％以下で使用し、２質量％未満では十分な結合組織が得られないため強度及び耐クリープ性が不十分となり、１２質量％を超えると組織が緻密になりすぎ耐熱衝撃性が低下する。 Clay is used in an amount of 2% by mass or more and 12% by mass or less to form a connective structure by firing, and if it is less than 2% by mass, a sufficient connective structure cannot be obtained, resulting in insufficient strength and creep resistance. If it exceeds%, the structure becomes too dense and the thermal shock resistance decreases.
コージェライトとしては、電融コージェライトでも焼結コージェライトでも使用することができるが、焼結コージェライトを使用した方がより耐クリープ性が高くなる点で好ましい。 As cordierite, either electrofused cordierite or sintered cordierite can be used. However, the use of sintered cordierite is preferable in that the creep resistance becomes higher.
本発明のコージェライト含有アルミナ−シリカれんがは、前述の耐火原料配合物にバインダーを添加して混練し、成形後、焼成する通常の方法によって得られる。このとき焼成温度は１１００℃以上１４００℃以下の範囲とする。焼成温度が１１００℃未満では強度が不足し、１４００℃を超えると組織が緻密になりすぎ耐熱衝撃性が低下する。 The cordierite-containing alumina-silica brick of the present invention can be obtained by an ordinary method of adding a binder to the above-mentioned refractory raw material mixture, kneading, molding and firing. At this time, the firing temperature is in the range of 1100 ° C. or higher and 1400 ° C. or lower. If the firing temperature is less than 1100 ° C., the strength is insufficient, and if it exceeds 1400 ° C., the structure becomes too dense and the thermal shock resistance decreases.
なお、本発明でいう粒度とは、ＪＩＳ標準篩におけるフルイ目開き（ｍｍ）で示している。例えば、粒度が０．０７４ｍｍ未満の原料粒子とは、フルイ目開きが０．０７４ｍｍの篩で篩ったときに篩い目を通過した原料粒子のことであり、粒度が０．０７４ｍｍ以上の原料粒子とは、同篩上に残った原料粒子のことである。 In addition, the particle size as used in the field of this invention is shown with the sieve opening (mm) in a JIS standard sieve. For example, a raw material particle having a particle size of less than 0.074 mm is a raw material particle having passed through a sieve when the sieve opening is 0.074 mm, and a raw material particle having a particle size of 0.074 mm or more. Is the raw material particles remaining on the same sieve.
本発明によれば、耐クリープ性及び耐熱衝撃性に優れるコージェライト含有アルミナ−シリカれんが得られるため、これを使用した熱風炉の寿命が向上する。また、熱風炉において高温熱風を発生する操業が可能となる。 According to the present invention, cordierite-containing alumina-silica brick having excellent creep resistance and thermal shock resistance can be obtained, so that the life of a hot stove using the same is improved. Moreover, the operation | movement which generate | occur | produces a high temperature hot air in a hot air furnace is attained.
本発明で使用するアンダリュサイト及びシリマナイトは、耐火物の原料として一般的に使用されているものを使用することができる。これらの原料は、天然から採掘される鉱物であり、それらを精製して使用することができる。より耐クリープ性を確保したい場合には、不純物としての酸化鉄含有量が約２質量％以下、好ましくは１質量％以下のものを使用することもできる。 What is generally used as a raw material of a refractory can be used for the Andalusite and sillimanite used by this invention. These raw materials are minerals mined from nature and can be used by refining them. When it is desired to further ensure the creep resistance, an iron oxide content as an impurity can be about 2% by mass or less, preferably 1% by mass or less.
前述のとおり、アンダリュサイト及び／又はシリマナイトは耐火原料配合物中に６０質量％以上含有することで十分な耐クリープ性を確保することができる。このときアンダリュサイト及び／又はシリマナイトは、粒度が３ｍｍ未満のものを適切な粒度構成に調整して使用する。例えば粒度が０．０７４ｍｍ以上３ｍｍ未満のアンダリュサイト及び／又はシリマナイトを３０質量％以上７０質量％以下、粒度が０．０７４ｍｍ未満のアンダリュサイト及び／又はシリマナイトを１０質量％以上４０質量％以下とすることができる。このように粒度を適切に調整することで成形時の充填性に優れより組織が緻密で強度の高いれんがとすることができる。 As described above, sufficient creep resistance can be ensured by including 60% by mass or more of andalusite and / or sillimanite in the refractory raw material composition. At this time, andalusite and / or sillimanite having a particle size of less than 3 mm is adjusted to an appropriate particle size configuration. For example, andalusite and / or sillimanite with a particle size of 0.074 mm or more and less than 3 mm are 30% by mass or more and 70% by mass or less, and andalusite and / or sillimanite with a particle size of less than 0.074 mm is 10% by mass or more and 40% by mass or less. It can be. By appropriately adjusting the particle size in this way, it is possible to obtain a brick which is excellent in filling property at the time of molding and has a finer structure and higher strength.
本発明で使用するコージェライトは、耐火物の原料として一般的に使用されているものを使用することができ、例えば電融コージェライトや焼結コージェライトなどを使用することができるが、前述のとおり耐クリープ性をより向上する点からは焼結コージェライトを使用することが好ましい。 The cordierite used in the present invention can be one commonly used as a raw material for refractories, for example, electrofused cordierite or sintered cordierite can be used. As described above, it is preferable to use sintered cordierite from the viewpoint of further improving the creep resistance.
本発明で使用する粘土は、通常の耐火物の原料として市販されているものを使用することができ、例えばＳｉＯ２含有量が４０〜７０質量％、Ａｌ２Ｏ３含有量が２０〜３０質量％のものなどを使用することができる。 As the clay used in the present invention, those commercially available as raw materials for ordinary refractories can be used. For example, the SiO 2 content is 40 to 70% by mass and the Al 2 O 3 content is 20 to 30% by mass. % Can be used.
本発明では前述の原料以外に、アルミナ系原料やアルミナ−シリカ系原料を１０質量％以下であれば耐火原料配合物中に含有することができる。例えば、ボーキサイト、バンケツ、シャモット、ろう石、アルミナ、あるいはムライトなどである。 In the present invention, in addition to the above-mentioned raw materials, an alumina-based raw material or an alumina-silica-based raw material can be contained in the refractory raw material composition as long as it is 10 mass% or less. For example, bauxite, banquet, chamotte, wax, alumina, or mullite.
表１に示す耐火原料配合物に水系のバインダーを添加して混練し、プレス機で並形れんがを成形し、乾燥後、１２００℃で焼成した。 A water-based binder was added to the refractory raw material composition shown in Table 1 and kneaded, and an ordinary brick was formed with a press, dried, and fired at 1200 ° C.
原料として使用したコージェライトはコージェライト含有量が９０質量％の焼結コージェライトを使用し、粘土はＡｌ２Ｏ３含有量が２５質量％、ＳｉＯ２含有量が５５質量％のものを、アンダリュサイトはＡｌ２Ｏ３含有量が６０質量％、ＳｉＯ２含有量が３７質量％のものを、シリマナイトはＡｌ２Ｏ３含有量が７５質量％、ＳｉＯ２含有量が２０質量％のものを使用した。 The cordierite used as the raw material was sintered cordierite with a cordierite content of 90% by mass, and the clay had an Al 2 O 3 content of 25% by mass and an SiO 2 content of 55% by mass. Leucite has an Al 2 O 3 content of 60% by mass and SiO 2 content of 37% by mass, and sillimanite has an Al 2 O 3 content of 75% by mass and an SiO 2 content of 20% by mass. used.
そして焼成後のれんがから、サンプルを切り出し、圧縮強さ、耐熱衝撃性試験及び耐クリープ性の評価として荷重軟化試験を行った。圧縮強さはＪＩＳ−Ｒ２２０６に従い測定した。耐熱衝撃性試験はＪＩＳ−Ｒ２６５７に従い８００℃加熱後の水冷法により、２０回行い剥落の状態を観察した。荷重軟化試験はＪＩＳ−Ｒ２２０９に従い０．２ＭＰａの荷重を加えて２％軟化点であるＴ２（℃）を測定した。 And the sample was cut out from the brick after baking, and the load softening test was done as evaluation of compressive strength, a thermal shock resistance test, and creep resistance. The compressive strength was measured according to JIS-R2206. The thermal shock resistance test was performed 20 times by a water cooling method after heating at 800 ° C. according to JIS-R2657, and the state of peeling was observed. In the load softening test, a load of 0.2 MPa was applied according to JIS-R2209, and T2 (° C.) which was a 2% softening point was measured.
実施例１から実施例３は０．０７４ｍｍ以上３ｍｍ未満のコージェライトの使用量が異なる場合であるがいずれも良好であった。これに対して比較例１は０．０７４ｍｍ以上３ｍｍ未満のコージェライトの使用量が５質量％と本発明の下限値を下回っており、耐熱衝撃性試験では１７回で剥落が発生し耐熱衝撃性に問題があることがわかった。また、比較例２は０．０７４ｍｍ以上３ｍｍ未満のコージェライトの使用量が４０質量％と本発明の上限値を超えており、耐熱衝撃性試験では１５回で剥落が発生し耐熱衝撃性に問題があることがわかった。この比較例２では、２％軟化点Ｔ２も１３８５℃と低下し、さらに焼成後のれんがには、表面にガラスによる発泡とれんがの変形が生じたものがあった。 Example 1 to Example 3 were cases where the amount of cordierite used was 0.074 mm or more and less than 3 mm, but all were good. On the other hand, in Comparative Example 1, the amount of cordierite of 0.074 mm or more and less than 3 mm is 5 mass%, which is lower than the lower limit value of the present invention. I found that there was a problem. In Comparative Example 2, the use amount of cordierite of 0.074 mm or more and less than 3 mm exceeds 40% by mass and exceeds the upper limit of the present invention, and in the thermal shock resistance test, peeling occurs 15 times, and there is a problem in thermal shock resistance. I found out that In Comparative Example 2, the 2% softening point T2 also decreased to 1385 ° C., and some of the fired bricks were foamed and deformed by glass on the surface.
実施例４と実施例５は０．０７４ｍｍ未満のコージェライトの使用量が異なる場合であるがいずれも良好であった。これに対して、比較例３は０．０７４ｍｍ未満コージェライトの使用量が８質量％と本発明の上限値を上回っており、２％軟化点Ｔ２が１３８０℃と低くなり耐クリープ性に問題があることがわかった。 Example 4 and Example 5 were cases where the amount of cordierite used was less than 0.074 mm, but both were good. In contrast, in Comparative Example 3, the amount of cordierite used is less than 0.074 mm, which is 8 mass%, exceeding the upper limit of the present invention, and the 2% softening point T2 is as low as 1380 ° C. I found out.
実施例６と実施例７は０．０７４ｍｍ未満のアンダリュサイトと粘土の使用量が異なる場合であるがいずれも良好な結果となった。 Although Example 6 and Example 7 are cases where the amounts of andalusite and clay used are less than 0.074 mm, the results are good.
実施例８と実施例９はアンダリュサイトの代わりにシリマナイトを使用した場合、実施例１０はアンダリュサイトとシリマナイトを併用した場合であるがいずれも良好な結果となった。 In Examples 8 and 9, when sillimanite was used instead of andalusite, Example 10 was a case where andalusite and sillimanite were used in combination.
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| CN115745631A (en) * | 2022-11-09 | 2023-03-07 | 宜兴市丁山耐火器材有限公司 | Andalusite modified cast glazed oven door brick for coke oven and preparation method thereof |
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