JP5978089B2 - Refractory manufacturing method and refractory - Google Patents

Refractory manufacturing method and refractory Download PDF

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JP5978089B2
JP5978089B2 JP2012221148A JP2012221148A JP5978089B2 JP 5978089 B2 JP5978089 B2 JP 5978089B2 JP 2012221148 A JP2012221148 A JP 2012221148A JP 2012221148 A JP2012221148 A JP 2012221148A JP 5978089 B2 JP5978089 B2 JP 5978089B2
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refractory
water
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矢野 淳
淳 矢野
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Hitachi Zosen Corp
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Description

本発明は、高温で焼成または熱処理を行う際に用いられる治具等に用いられる耐火物の製造方法およびそのような方法により製造される耐火物に関する。   The present invention relates to a method for producing a refractory used for a jig or the like used for firing or heat treatment at a high temperature, and a refractory produced by such a method.

従来、高温で焼成または熱処理を行うための治具、製鋼炉や焼却炉、溶融炉などの炉底などには、これらが通常1000℃を超える高温の環境に置かれるため、これらを構成する材料として耐火物が用いられている。   Conventionally, jigs for performing firing or heat treatment at high temperatures, furnace bottoms such as steel making furnaces, incinerators, melting furnaces, etc., are usually placed in a high temperature environment exceeding 1000 ° C., and therefore the materials constituting them As refractories are used.

耐火物は、通常、粒径1mmを超える粗大粒子(骨材)から100μm以下の微細な粒子が混合された不均質な組織を有している。このような耐火物を製造するには、金型による成形、あるいは原料に水を加えた後に型へ流し込む成形の後に、焼成および機械加工等を施す方法が知られている。   The refractory usually has a heterogeneous structure in which coarse particles (aggregate) having a particle size of more than 1 mm to fine particles of 100 μm or less are mixed. In order to manufacture such a refractory, there is known a method in which baking, machining, or the like is performed after molding with a mold or molding in which water is added to a raw material and then poured into the mold.

得られた耐火物の表面には、骨材を含め種々の粒径の原料由来の粒状物が現れるが、使用過程で骨材の割れや組織の「緩み」により脱落が生じる。その後、骨材の脱落が進行すると、表面の骨材痕が多く現れる。耐火物を治具に使用した場合には、治具上に設置した製品の表面が非常に「荒れた」状態になったり、熱処理中に脱落した骨材が製品に付着したり焼き付いたりするため熱処理後に機械加工が必要な状況が生じる。また耐火物を各種の炉の炉底に用いた場合には、骨材の脱落が進行していくことにより耐火物の強度が徐々に低下し、短期間で破壊に至ることもある。   On the surface of the obtained refractory material, granular materials derived from raw materials having various particle sizes including aggregates appear, but dropout occurs due to cracking of the aggregate and “loosening” of the structure in the course of use. After that, when the aggregates fall off, many aggregate marks on the surface appear. If a refractory material is used for the jig, the surface of the product placed on the jig will be in a very "rough" state, and aggregates that have fallen off during heat treatment will adhere to or stick to the product. A situation arises that requires machining after heat treatment. Moreover, when a refractory is used for the bottom of various furnaces, the strength of the refractory gradually decreases due to the progress of the dropping of the aggregate, which may lead to destruction in a short period of time.

本発明は、上記のような弊害を防止するために、平滑な表面状態を有した耐火物を製造する方法およびそのような耐火物を提供することを目的とする。   An object of the present invention is to provide a method for producing a refractory having a smooth surface state and such a refractory in order to prevent the above-described adverse effects.

上記課題を解決するため、本発明は、耐火物原料粒子粉末に水を添加して混合した後に生じた混合物を型枠に流し込み、乾燥および焼成を行うことによる、耐火物の製造方法であって、添加される水の量が、JIS R 2553に記載の水量の決定方法により求められる水量の1.2〜1.7倍であり、該混合物を型枠に流し込む際に振動を加えないことを特徴とするものである。   In order to solve the above problems, the present invention is a method for producing a refractory by pouring a mixture formed after adding and mixing water to a refractory raw material particle powder into a mold, drying and firing. The amount of water added is 1.2 to 1.7 times the amount of water determined by the method for determining the amount of water described in JIS R 2553, and no vibration is applied when the mixture is poured into a mold. It is a feature.

このような方法により耐火物を製造することによって、得られる耐火物の表面状態は良好なものとなり、このため、多数回にわたって使用しても骨材の脱落等が生じず耐久性を向上させることができる。   By producing the refractory by such a method, the surface state of the obtained refractory becomes good, and therefore, even if it is used many times, the aggregate does not fall off and the durability is improved. Can do.

上記本発明の耐火物製造方法において、前記耐火物原料粒子粉末として、比重の異なる複数の材質を用いてもよい。   In the refractory manufacturing method of the present invention, a plurality of materials having different specific gravities may be used as the refractory raw material particle powder.

このように比重の異なる複数の材質を用いることにより、表層部と中心部とで異なる材質を有する複数構造を有する耐火物を製造することが可能である。   Thus, by using a plurality of materials having different specific gravities, it is possible to manufacture a refractory having a plurality of structures having different materials in the surface layer portion and the central portion.

また、本発明は、上記の製造方法により製造される耐火物に関するものである。本発明の耐火物は、上記のように、表面状態が良好であり、かつ、耐久性に優れている。   Moreover, this invention relates to the refractory manufactured by said manufacturing method. As described above, the refractory of the present invention has a good surface state and excellent durability.

本発明による耐火物の製造方法では、添加される水の量が、JIS R 2553に記載の水量の決定方法により求められる水量の1.2〜1.7倍であり、混合物を型枠に流し込む際に振動を加えないことにより、耐火物の表面状態を良好にすることができ、このために多数回にわたって使用しても骨材の脱落等が生じず耐久性を向上させることができる。   In the method for producing a refractory according to the present invention, the amount of water added is 1.2 to 1.7 times the amount of water determined by the method for determining the amount of water described in JIS R 2553, and the mixture is poured into a mold. When vibration is not applied, the surface state of the refractory can be made good. For this reason, even if the refractory is used many times, the aggregate does not fall off and the durability can be improved.

焼成後の耐火物の断面状態を示す写真であり、(a)は実施例2により得られた耐火物を示し、(b)は比較例1により得られた耐火物を示す。It is a photograph which shows the cross-sectional state of the refractory after baking, (a) shows the refractory obtained by Example 2, (b) shows the refractory obtained by the comparative example 1. FIG. 焼成後の耐火物の表面状態を示す写真であり、(a)は実施例2により得られた耐火物を示し、(b)は比較例1により得られた耐火物を示す。It is a photograph which shows the surface state of the refractory after baking, (a) shows the refractory obtained by Example 2, (b) shows the refractory obtained by the comparative example 1. FIG.

以下、本発明による耐火物の製造方法を詳細に説明する。   Hereinafter, the manufacturing method of the refractory material by this invention is demonstrated in detail.

本発明による耐火物の製造方法は、耐火物原料粒子粉末に水を添加して混合した後に生じた混合物を型枠に流し込み、乾燥および焼成を行うことによるものであり、(1)耐火物原料粒子粉末に水を添加するに際して、その水の量が、JIS R 2553に記載の水量の決定方法により求められる水量の1.2〜1.7倍となる量とされ、さらに、(2)水と耐火物原料粒子粉末とから生じた混合物を型枠に流し込む際に振動を加えないことを特徴とする。   The method for producing a refractory according to the present invention is by pouring a mixture formed after adding and mixing water to refractory raw material particle powder into a mold, drying and firing, and (1) refractory raw material When water is added to the particle powder, the amount of water is 1.2 to 1.7 times the amount of water determined by the method for determining the amount of water described in JIS R 2553, and (2) water When the mixture produced from the refractory raw material powder is poured into the mold, no vibration is applied.

本発明方法に従って耐火物を製造するに際して用いられる耐火物原料粒子粉末は従来から知られている粒径1mmを超える粗大粒子(骨材)から100μm以下の微細な粒子が混合されたものを用いてよい。   The refractory raw material powder used in the production of the refractory according to the method of the present invention is obtained by mixing conventionally known coarse particles (aggregate) having a particle diameter exceeding 1 mm and fine particles of 100 μm or less. Good.

また、上記粗大粒子と微細粒子との比率は、最終製品である耐火物の求められる性能、粗大粒子および微細粒子の性状に応じて種々変更してよいが、例えば、重量比率で、粗大粒子/微細粒子の比は、0.4〜0.8である。   Further, the ratio of the coarse particles to the fine particles may be variously changed according to the required performance of the refractory as the final product and the properties of the coarse particles and the fine particles. The ratio of fine particles is 0.4 to 0.8.

耐火物原料粒子粉末に添加される水の量は、JIS R 2553に記載の水量の決定方法により求められる水量の1.2〜1.7倍とされる。   The amount of water added to the refractory material particle powder is 1.2 to 1.7 times the amount of water determined by the method for determining the amount of water described in JIS R2553.

ここで、JIS R 2553に記載の水量の決定方法に従って、基準となる水量を決定する手順について、上記から必要な記載を抜粋し簡単に説明すると、下記(a)〜(d)を順次行うことにより決定されることになる。   Here, according to the method for determining the amount of water described in JIS R 2553, the procedure for determining the amount of water used as a reference will be briefly described by extracting the necessary descriptions from the above and sequentially performing the following (a) to (d). Will be determined.

(a)試料約1kgを上皿はかりで計り採り、鉢に入れる。ただし、軽量キャスタブル耐火物の試料は、品種に応じて0.5〜1kgを採る。   (A) About 1 kg of a sample is weighed with an upper scale and placed in a bowl. However, the light castable refractory sample takes 0.5 to 1 kg depending on the type.

(b)温度20±3℃の水を約100mL加え、混練器具を用いて混練する。   (B) Add about 100 mL of water at a temperature of 20 ± 3 ° C. and knead using a kneading instrument.

(c)混合物を手でボール状に固め、約30cm上方に投げてこれを片手で受ける。   (C) The mixture is solidified in a ball shape by hand, thrown upward about 30 cm and received with one hand.

(d)この状態が所定の状態(標準軟度状態;具体的にはJIS R 2553参照)に示すようになるまで、(a)(b)(c)の操作を水量を変えて繰り返し、標準軟度状態に達したときに使用した水量を供試キャスタブル耐火物の乾燥質量に対する百分率(%)として算出する。   (D) Until this state becomes a predetermined state (standard softness state; specifically, refer to JIS R 2553), the operations of (a), (b), and (c) are repeated while changing the amount of water. The amount of water used when the soft state is reached is calculated as a percentage (%) of the dry weight of the test castable refractory.

耐火物原料粒子粉末に水が添加されることにより得られた混合物が流し込まれる型枠は、従来公知である種々の態様のものが用いられてよい。   As the mold into which the mixture obtained by adding water to the refractory raw material particle powder is poured, various forms known in the art may be used.

ここで、本発明では、混合物を型枠に流し込むに際して、振動は加えられずに行われることになる。   Here, in the present invention, when the mixture is poured into the mold, vibration is not applied.

型枠に混合物を流し込んだ後に行われる、乾燥および焼成は、耐火物製造のために通常用いられている条件下に行われる。例えば、乾燥は、大気雰囲気中、室温で一昼夜自然乾燥後5〜10℃/時間の昇温速度で600℃まで加熱することにより行われ、焼成は、酸化物の場合大気雰囲気中(非酸化物の場合窒素雰囲気中)、耐火物の常用温度よりも50〜100℃高い温度まで50〜100時間かけて加熱することにより行われる。   Drying and firing, which are performed after pouring the mixture into the mold, are performed under conditions normally used for refractory production. For example, drying is performed by air-drying at room temperature all day and night in an air atmosphere and then heating to 600 ° C. at a temperature increase rate of 5 to 10 ° C./hour. In the case of a nitrogen atmosphere), heating is performed over 50 to 100 hours to a temperature 50 to 100 ° C. higher than the normal temperature of the refractory.

また、記耐火物原料粒子粉末として、比重の異なる複数の材質を用いた場合、本発明では、型枠に流し込む際に振動が加えられないことにより、乾燥・焼成を行った後に、表層部と中心部とで異なる材質の比率を有する複層構造を有する耐火物を製造することも可能である。 Furthermore, as a pre Symbol refractory raw material particles, when using a plurality of materials having different specific gravities, in the present invention, by the vibration is not applied when poured into the mold, after the drying and baking, the surface portion It is also possible to manufacture a refractory having a multilayer structure having different material ratios in the central portion.

(実施例)
次に、本発明に沿った実施例、およびこれとの比較を示すための比較例を実際にいくつか行ったので以下に説明する。
(Example)
Next, some examples in accordance with the present invention and some comparative examples for comparison with the present invention were actually performed and will be described below.

耐火物原料粒子粉末として、1mm以上の粒径を有する粗大粒子粉末30重量%、100μm以下の粒径を有する微細粉末40重量%を含み、残りの30重量%は100μmより大きくかつ1mm未満の粉末である市販のアルミナ質不定形耐火物を用いた。   As refractory raw material powder, 30% by weight of coarse particle powder having a particle size of 1 mm or more, 40% by weight of fine powder having a particle size of 100 μm or less, and the remaining 30% by weight is a powder larger than 100 μm and less than 1 mm A commercially available alumina-based amorphous refractory was used.

(比較例1)
不定形耐火物に、JIS R 2553に記載の水量の決定方法により求められる水量(以下標準添加量と称する)に相当する量の水を加えた。この不定形耐火物においては、水の標準添加量は、不定形耐火物重量に対して10重量%であった。
(Comparative Example 1)
An amount of water corresponding to the amount of water determined by the method for determining the amount of water described in JIS R 2553 (hereinafter referred to as standard addition amount) was added to the amorphous refractory. In this amorphous refractory, the standard amount of water added was 10% by weight based on the weight of the irregular refractory.

標準添加量(10重量%)の水を加えた後、これをミキサーに投入し、このミキサーにおいて混合し、その後、加振台にセットした木枠(500×1000mm)に流し込んだ。   After adding a standard addition amount (10% by weight) of water, it was put into a mixer, mixed in this mixer, and then poured into a wooden frame (500 × 1000 mm) set on a shaking table.

一昼夜自然乾燥後、10℃/時間の昇温速度で600℃まで加熱して乾燥した後に50時間かけて1500℃まで加熱して焼成を行い、耐火物を得た。   After natural drying all day and night, it was heated to 600 ° C. at a heating rate of 10 ° C./hour and dried, and then heated to 1500 ° C. over 50 hours to obtain a refractory.

得られた耐火物の大きさは、495×990×30mmであった。   The size of the obtained refractory was 495 × 990 × 30 mm.

(実施例1)
標準添加量の1.5倍に相当する量の水、すなわち、15重量%の水を加え、また、木枠に流し込む際に加振しなかった他は、比較例1と同様にして耐火物を得た。得られた耐火物の大きさは、比較例1と同様に、495×990×30mmであった。
Example 1
A refractory similar to Comparative Example 1 except that an amount of water corresponding to 1.5 times the standard addition amount, that is, 15% by weight of water was added and was not vibrated when poured into a wooden frame. Got. The size of the obtained refractory was 495 × 990 × 30 mm as in Comparative Example 1.

(実施例2〜4および比較例2〜7)
上記比較例1および実施例1と同様にして耐火物を製造したが、材質をアルミナ質のものから炭化ケイ素に変更したり(比較例4および実施例4)、添加水分量を種々変更したり、木枠に流し込む際に加振を加えたり加えなかったり等による製造時の条件を種々変更して複数種の耐火物を得た。
(Examples 2 to 4 and Comparative Examples 2 to 7)
Although the refractory was produced in the same manner as in Comparative Example 1 and Example 1, the material was changed from alumina to silicon carbide (Comparative Example 4 and Example 4), and the amount of added water was variously changed. A plurality of types of refractories were obtained by variously changing the manufacturing conditions by adding or not adding vibration when pouring into the wooden frame.

実施例1〜4および比較例1〜7による11種の耐火物を製造する際の条件を表1にまとめる。   The conditions for producing 11 types of refractories according to Examples 1 to 4 and Comparative Examples 1 to 7 are summarized in Table 1.

上記11種の各耐火物を焼成用治具として用いてジルコニアセラミックスの焼成を大気中1400℃、電気炉にて実施する工程を繰り返した。   Using each of the 11 types of refractories as a firing jig, the process of firing zirconia ceramics in the atmosphere at 1400 ° C. in an electric furnace was repeated.

工程後の耐火物の表面状態および肉厚を下記表2に示す。   Table 2 below shows the surface state and thickness of the refractory after the process.

上記実施例1および比較例1の耐火物により得られた結果を、実施例2〜4および比較例2〜7の耐火物により得られた結果と共に表2に示す。   The results obtained with the refractories of Example 1 and Comparative Example 1 are shown in Table 2 together with the results obtained with the refractories of Examples 2-4 and Comparative Examples 2-7.

表2中、○は、使用前と比較して表面状態が変化ない場合であり、△は、骨材の脱落が発生した場合であり、×は、骨材の脱落が著しく進行した場合である。また、肉厚は、10%以上低下した場合は×とした。   In Table 2, ◯ indicates a case where the surface state does not change compared to before use, △ indicates a case where the aggregate has fallen, and X indicates a case where the aggregate has significantly dropped. . In addition, when the wall thickness decreased by 10% or more, it was evaluated as x.

比較例1で製作した耐火物は、5回目から骨材の割れによる脱落が生じ始め、9回目で焼成後のジルコニアセラミックスの表面に骨材が焼き付くことを確認することができた。骨材の脱落はその後も進行し、30回目で当初の厚みが減肉していることが分かった(当初30mm→27mm)。   The refractory manufactured in Comparative Example 1 began to drop off due to cracking of the aggregate from the fifth time, and it was confirmed that the aggregate was seized on the surface of the zirconia ceramic after firing at the ninth time. It was found that the dropping of the aggregate continued and the initial thickness was reduced at the 30th time (initial 30 mm → 27 mm).

一方、実施例1で製作した耐火物は骨材の脱落もなく、30回目の使用においても表面状態、肉厚とも初期と大差ないことを確認した。   On the other hand, it was confirmed that the refractory produced in Example 1 did not drop off the aggregate, and even in the 30th use, the surface state and thickness were not significantly different from the initial.

他の実施例および比較例の結果は表2が参照される。表2に示されるように、良好な表面状態と耐火物の長期耐用の双方を得るためには標準添加量の1.2〜1.7倍の水分を添加する必要がある。また、同様の結果が、アルミナ質もの(酸化物)の他炭化ケイ素(非酸化物)でも得られた。
Table 2 is referred to for the results of other examples and comparative examples. As shown in Table 2, it is necessary to add 1.2 to 1.7 times as much water as the standard addition amount in order to obtain both a good surface condition and long-term durability of the refractory. The same results, other silicon carbide (non-oxide) ones of alumina (oxide) is obtained even.

一方、成形時の加振の効果については、実施例1と比較例6とを比較すれば明らかなように、標準添加量よりも多い量の水を加えた場合には、加振しないことにより良好な結果が得られた。なお、標準添加量よりも少ない量の水を加えた場合には、加振の有無に拘わらず表面状態は悪いという結果となった。   On the other hand, as is clear from the comparison between Example 1 and Comparative Example 6 regarding the effect of vibration during molding, when adding more water than the standard addition amount, Good results were obtained. In addition, when the amount of water smaller than the standard addition amount was added, the result was that the surface condition was bad regardless of the presence or absence of vibration.

以上に示したように、耐火物を流し込み成形にて製造する場合は、標準添加量の1.2〜1.7倍の水を添加し、かつ、成形時に加振を行わないことにより良好な性質が得られることが分かった。   As shown above, when the refractory is produced by casting, it is preferable to add 1.2 to 1.7 times as much water as the standard addition amount and not perform vibration during molding. It was found that properties were obtained.

Claims (2)

耐火物原料粒子粉末に水を添加して混合した後に生じた混合物を型枠に流し込み、乾燥および焼成を行うことによる、耐火物の製造方法であって、
添加される水の量が、JIS R 2553に記載の水量の決定方法により求められる水量の1.2〜1.7倍であり、
該混合物を型枠に流し込む際に振動を加えない
ことを特徴とする、耐火物の製造方法。
A method for producing a refractory by pouring a mixture formed after adding and mixing water to a refractory raw material particle powder into a mold, drying and firing,
The amount of water added is 1.2 to 1.7 times the amount of water determined by the method for determining the amount of water described in JIS R 2553,
A method for producing a refractory material, characterized in that no vibration is applied when the mixture is poured into a mold.
前記耐火物原料粒子粉末として、比重の異なる複数の材質を用いる、請求項1に記載の耐火物の製造方法。
The method for producing a refractory according to claim 1, wherein a plurality of materials having different specific gravities are used as the refractory raw material particle powder.
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