JP5172222B2 - Calcia material and method for producing the same - Google Patents
Calcia material and method for producing the same Download PDFInfo
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Description
本発明は、耐水和性の高いカルシア質材料およびその製造方法に関する。 The present invention relates to a calciatic material having high hydration resistance and a method for producing the same.
カルシア（ＣａＯ）は、自然界に豊富にあり、耐火度が高く、塩基性溶融スラグなどの溶融物に対する耐食性も良いなどの優れた特性を有するため、製鋼用耐火物やセメント製造用耐火物などの耐火物の製造分野に原料として使用することができるが、水和しやすい欠点があるため、その実用が制限されている。 Calcia (CaO) is abundant in nature, has high fire resistance, and has excellent properties such as good corrosion resistance against melts such as basic molten slag. Although it can be used as a raw material in the field of refractory production, its practical use is limited due to the drawback of being easily hydrated.
カルシアの耐水和性を改善すべく、従来から種々の検討がなされている。例えば、カルシアにＡｌ、Ｃｒ、Ｔｉ、Ｚｒ、Ｆｅ、Ｙ、Ｗ、ＮｉおよびＣｕの金属またはＢ、ＳｉおよびＣの半金属をコーティングし、大気雰囲気、酸化雰囲気、カーボン雰囲気、一酸化炭素雰囲気、窒素雰囲気またはシリコン雰囲気のいずれか の雰囲気中で加熱処理することによりカルシア原料に金属反応物の被覆層を形成させる方法が特許文献１に開示されている。また、カルシア質原料の表面にチタン系有機金属化合物またはコロイド状チタニアを被覆、乾燥、熱処理する方法が特許文献２に開示されている。 Various studies have been made to improve the hydration resistance of calcia. For example, calcia is coated with Al, Cr, Ti, Zr, Fe, Y, W, Ni and Cu metals or B, Si and C metalloids, air atmosphere, oxidizing atmosphere, carbon atmosphere, carbon monoxide atmosphere, Patent Document 1 discloses a method of forming a coating layer of a metal reactant on a calcia raw material by heat treatment in either a nitrogen atmosphere or a silicon atmosphere. Further, Patent Document 2 discloses a method in which a surface of a calcia material is coated with a titanium-based organometallic compound or colloidal titania, dried, and heat-treated.
以上に述べた従来の水和防止技術では、添加物の被覆効果が不十分で、カルシアに十分な耐水和性を付与することが困難である。さらに、高価な添加物の使用でコストが高い問題も含まれている。 With the conventional hydration prevention techniques described above, the coating effect of the additive is insufficient, and it is difficult to impart sufficient hydration resistance to calcia. Furthermore, the problem of high cost due to the use of expensive additives is also included.
本発明は、従来の水和防止技術が有していた課題を解決しようとするものであり、安価な添加物を使用し、カルシアに十分な耐水和性を付与する方法および高耐水和性カルシア質材料を実現することを目的とするものである。 The present invention seeks to solve the problems of conventional hydration prevention techniques, and uses a low-cost additive to provide sufficient hydration resistance to calcia and a high hydration resistance calcia. The purpose is to realize a quality material.
本発明は、鉄成分およびカルシウム成分を含む出発原料からなる混合物に対して段階的な熱処理を行うことにより、ＣａＯ−ＦｅＯ系固溶体を形成させた後、固溶体にＣａＯ−Ｆｅ２Ｏ３−Ｆｅ３Ｏ４系化合物を析出させ、最終的にはＣａＯ−ＦｅＯ系固溶体表面に２ＣａＯ・Ｆｅ ２ Ｏ ３ の結晶相からなる被覆層を形成させる製造方法およびそれから得られる高耐水和性のカルシア質材料とすることを特徴とする。 In the present invention, a CaO—FeO-based solid solution is formed by performing a stepwise heat treatment on a mixture of starting materials including an iron component and a calcium component, and then the CaO—Fe 2 O 3 —Fe 3 is formed in the solid solution. the O 4 compound to precipitate, eventually high water miscible calcia material obtained from the manufacturing method and it Ru to form a coating layer comprising a crystal phase of 2CaO · Fe 2 O 3 to CaO-FeO-based solid solution surface characterized by a.
すなわち、本発明に係る製造方法は、鉄成分およびカルシウム成分を含む出発原料からなる混合物として、炭酸カルシウムの粉体に酸化鉄の粉体をＦｅ２Ｏ３換算で［Ｆｅ２Ｏ３／（ＣａＯ＋Ｆｅ２Ｏ３）］×１００％＝０.３〜１５質量％の比率で添加混合した後、所定の形状に成形し、得られた成形物を酸素分圧が１０−３０〜０．１ａｔｍの雰囲気で全圧力は１ａｔｍ中において８００〜２５００℃の範囲で前段階熱処理をすることにより、ＣａＯ−ＦｅＯ系固溶体を生成させ、次に、酸素分圧が１０−２５〜１ａｔｍの雰囲気で全圧力は１ａｔｍ中において８００〜２５００℃の範囲で前記固溶体生成条件の前段階と異なる雰囲気および／又は加熱温度下で後段階熱処理をして、ＣａＯ−Ｆｅ２Ｏ３−Ｆｅ３Ｏ４系化合物を前記固溶体表面に析出させたのち冷却して、２ＣａＯ・Ｆｅ２Ｏ３の結晶相からなる被覆層を形成させることを特徴とする高耐水和性のカルシア質材料の製造方法である。 That is, in the production method according to the present invention, as a mixture of starting materials including an iron component and a calcium component, iron oxide powder is converted into [Fe 2 O 3 / (CaO + Fe] in terms of Fe 2 O 3 as a calcium carbonate powder. 2 O 3 )] × 100% = 0.3 to 15% by mass, and after mixing and molding into a predetermined shape, the resulting molded product has an oxygen partial pressure of 10 −30 to 0.1 atm. Then, a pre-stage heat treatment is performed in the range of 800 to 2500 ° C. at 1 atm to generate a CaO—FeO-based solid solution, and then the total pressure is 1 atm in an atmosphere having an oxygen partial pressure of 10 −25 to 1 atm. In the range of 800 to 2500 ° C., post-stage heat treatment is performed under an atmosphere and / or heating temperature different from the pre-stage of the solid solution generation conditions, and the CaO—Fe 2 O 3 —Fe 3 O 4 -based compound This is a method for producing a highly hydration resistant calcia material, wherein a product is deposited on the surface of the solid solution and then cooled to form a coating layer composed of a crystal phase of 2CaO · Fe 2 O 3 .
また、上記の製造方法により製造され、熱処理後のカルシア質材料中の酸化鉄含有量がＦｅ ２ Ｏ ３ 換算で０．３〜１５質量％であることを特徴とする高耐水和性のカルシア質材料が得られる。 Further, the highly hydrated calcia having a ferric oxide content of 0.3 to 15% by mass in terms of Fe 2 O 3 produced by the above-described production method and after heat treatment A material is obtained .
上述したように本発明の水和防止技術は、安価な添加物を使用し、カルシアに十分な耐水和性を付与することができ、耐水和性の高いカルシア質材料を提供できる。 As described above, the hydration prevention technology of the present invention can provide a calciaaceous material having high hydration resistance by using an inexpensive additive and imparting sufficient hydration resistance to calcia.
以下、本発明の実施の形態について説明する。本発明においては、鉄成分およびカルシウム成分を含む出発原料からなる混合物を段階的に熱処理するところに特徴がある。 Embodiments of the present invention will be described below. The present invention is characterized in that a mixture of starting materials containing an iron component and a calcium component is heat-treated stepwise.
鉄成分含有の出発原料としては、金属鉄および鉄化合物の中の１種または２種以上を用いることができる。鉄化合物には、鉄の酸化物、炭化物、窒化物、硫化物、塩化物やフッ化物などが含まれる。ただし、低コスト面から酸化鉄が好ましい。また、鉄成分含有原料以外の原料中の鉄成分、例えば炭酸カルシウム原料中の酸化鉄不純物も含まれる。カルシウム成分含有の出発原料としては、カルシア、炭酸カルシウムや水酸化カルシウムなどを用いることができる。 As a starting material containing an iron component, one or more of metallic iron and iron compounds can be used. Iron compounds include iron oxides, carbides, nitrides, sulfides, chlorides and fluorides. However, iron oxide is preferable from the viewpoint of low cost. Moreover, the iron component in raw materials other than an iron component containing raw material, for example, the iron oxide impurity in a calcium carbonate raw material, is also contained. As a starting material containing a calcium component, calcia, calcium carbonate, calcium hydroxide, or the like can be used.
前段階の熱処理として、上述した出発原料からなる混合物を加熱し、Ｃａ、ＦｅおよびＯ元素が均一に分布するＣａＯ−ＦｅＯ系固溶体を形成させる。加熱温度 を８００〜２５００℃の範囲にすることが好ましく、加熱温度が８００℃未満であると、ＣａＯ−ＦｅＯ系固溶体の形成速度が遅く、ＦｅＯ固溶量も小さすぎる。温度が２５００℃を超えると、鉄成分の蒸発が問題となる。 As a heat treatment in the previous stage, the mixture composed of the above starting materials is heated to form a CaO—FeO-based solid solution in which Ca, Fe and O elements are uniformly distributed. The heating temperature is preferably in the range of 800 to 2500 ° C. If the heating temperature is less than 800 ° C, the formation rate of the CaO-FeO solid solution is slow and the FeO solid solution amount is too small. When the temperature exceeds 2500 ° C., evaporation of the iron component becomes a problem.
また、雰囲気中の酸素分圧を１０−３０〜０．１ａｔｍの範囲にすることが好ましく、酸素分圧が１０−３０ａｔｍ未満であると、あるいは０．１ａｔｍを超えると、ＦｅＯが不安定となり、ＣａＯ−ＦｅＯ系固溶体は形成されない可能性がある。 The oxygen partial pressure in the atmosphere is preferably in the range of 10 −30 to 0.1 atm. If the oxygen partial pressure is less than 10 −30 atm or exceeds 0.1 atm, FeO becomes unstable. The CaO—FeO solid solution may not be formed.
後段階の熱処理においては、前段階の熱処理で得られたＣａＯ−ＦｅＯ系固溶体を前段階と異なる雰囲気および／又は加熱温度下で熱処理し、固溶体中のＦｅＯを雰囲気中の酸素と反応させ、ＣａＯ−Ｆｅ２Ｏ３−Ｆｅ３Ｏ４系化合物で析出させる。雰囲気と接する固溶体粒の表面にその化合物が優先的に生成するため、表面被覆層が形成する。 In the subsequent heat treatment, the CaO—FeO-based solid solution obtained in the previous heat treatment is heat-treated at an atmosphere and / or a heating temperature different from that in the previous step, and the FeO in the solid solution is reacted with oxygen in the atmosphere, thereby causing CaO Precipitation is performed with a -Fe 2 O 3 -Fe 3 O 4 -based compound. Since the compound is preferentially generated on the surface of the solid solution particles in contact with the atmosphere, a surface coating layer is formed.
また、その表面被覆層を介して粒の内部へ拡散する酸素が結晶粒間の界面へ集積しやすいため、結晶粒界にもＣａＯ−Ｆｅ２Ｏ３−Ｆｅ３Ｏ４系化合物の被覆層が生じる。 Further, since oxygen diffusing into the grains through the surface coating layer easily accumulates at the interface between the crystal grains, a coating layer of the CaO—Fe 2 O 3 —Fe 3 O 4 compound is also present at the crystal grain boundary. Arise.
ＣａＯ−Ｆｅ２Ｏ３−Ｆｅ３Ｏ４系化合物は、熱処理中において液相または固相を呈し室温まで冷却されると２ＣａＯ・Ｆｅ２Ｏ３やＣａＯ・Ｆｅ２Ｏ３などの結晶相または非結晶相となる。このように形成される耐水和性が高いＣａＯ−Ｆｅ２Ｏ３−Ｆｅ３Ｏ４系化合物の被覆層により、良い被覆効果が現れ、得られるカルシア質材料が高い耐水和性を示す。ただし、後段階の熱処理では、前段階と同様に加熱温度が８００〜２５００℃の範囲であることが好ましい。 The CaO—Fe 2 O 3 —Fe 3 O 4 -based compound exhibits a liquid phase or a solid phase during the heat treatment, and when cooled to room temperature, a crystalline phase such as 2CaO · Fe 2 O 3 or CaO · Fe 2 O 3 It becomes a crystalline phase. The coating layer of the CaO—Fe 2 O 3 —Fe 3 O 4 -based compound having high hydration resistance formed in this way exhibits a good coating effect, and the resulting calcia material exhibits high hydration resistance. However, in the subsequent heat treatment, it is preferable that the heating temperature is in the range of 800 to 2500 ° C. as in the previous step .
また、雰囲気中の酸素分圧を１０−２５〜１ａｔｍの範囲にすることが好ましい。加熱温度は前段階の温度範囲が８００℃未満であると、ＣａＯ−Ｆｅ２Ｏ３−Ｆｅ３Ｏ４系化合物の析出が遅すぎ、２５００℃を超えると、鉄成分の蒸発が問題となる。 In addition, the oxygen partial pressure in the atmosphere is preferably in the range of 10 −25 to 1 atm. When the heating temperature is less than 800 ° C. in the previous stage, precipitation of the CaO—Fe 2 O 3 —Fe 3 O 4 compound is too slow, and when it exceeds 2500 ° C., evaporation of the iron component becomes a problem.
さらに、酸素分圧が１０−２５ａｔｍ未満になると、ＣａＯ−Ｆｅ２Ｏ３−Ｆｅ３Ｏ４系化合物が析出せず、１ａｔｍを超えると、ＣａＯ−Ｆｅ２Ｏ３−Ｆｅ３Ｏ４系化合物は析出するが、耐高圧処理装置が必要となり処理コストが高くなる。 Further, when the oxygen partial pressure is less than 10 −25 atm, the CaO—Fe 2 O 3 —Fe 3 O 4 compound does not precipitate, and when it exceeds 1 atm, the CaO—Fe 2 O 3 —Fe 3 O 4 compound Is deposited, but a high-pressure-resistant processing apparatus is required, which increases the processing cost.
なお、熱処理で得られるカルシア質材料中酸化鉄の含有量が０．３〜１５質量％であることが好ましい。０．３質量％未満であると、均一なＣａＯ−Ｆｅ２Ｏ３−Ｆｅ３Ｏ４系化合物の被覆層が生成できず、あるいはその層の厚みが薄すぎるため、カルシア質材料の耐水和性が低下する可能性がある。 In addition, it is preferable that content of the iron oxide in the calcia material obtained by heat processing is 0.3-15 mass%. If it is less than 0.3% by mass, a uniform coating layer of CaO—Fe 2 O 3 —Fe 3 O 4 compound cannot be formed, or the thickness of the layer is too thin. May be reduced.
酸化鉄の含有量が１５質量％を超えると、その量が多すぎてカルシア材料の耐食性などの特性が損なわれる可能性がある。 If the content of iron oxide exceeds 15% by mass, the amount is too large, and properties such as corrosion resistance of the calcia material may be impaired.
［実施例１］
炭酸カルシウムの粉体に酸化鉄（Ｆｅ２Ｏ３）の粉体を［Ｆｅ２Ｏ３／（ＣａＯ＋Ｆｅ２Ｏ３）］×１００％＝５質量％の比率で添加し、混合した後、直径２５ｍｍ×高さ１０ｍｍの円柱体に成形した。円柱体を酸素分圧が１０−６ａｔｍの（Ａｒ＋Ｏ２）雰囲気（全圧力は１ａｔｍ）中において１６００℃で５時間加熱し、ＣａＯ−ＦｅＯ固溶体を生成させた。次に、雰囲気を大気（酸素分圧が約０．２ａｔｍ）に変更し温度を変更せずに５時間加熱して、ＣａＯ−Ｆｅ２Ｏ３−Ｆｅ３Ｏ４系化合物を前記固溶体表面に析出させた。室温まで冷却するとき、２ＣａＯ・Ｆｅ２Ｏ３の結晶相からなる被覆層が生じた。熱処理後のカルシア質材料を温度が７０℃、湿度が９０％の恒温恒湿装置の中に４８時間静置し、質量増加率から耐水和性を評価した。質量増加率が小さいほど耐水和性が良くなる。
[Example 1]
The powder of iron oxide (Fe 2 O 3 ) was added to the calcium carbonate powder at a ratio of [Fe 2 O 3 / (CaO + Fe 2 O 3 )] × 100% = 5% by mass, and after mixing, the diameter was 25 mm. X Molded into a cylindrical body having a height of 10 mm. The cylindrical body was heated at 1600 ° C. for 5 hours in an (Ar + O 2 ) atmosphere (total pressure: 1 atm) with an oxygen partial pressure of 10 −6 atm to generate a CaO—FeO solid solution. Next, the atmosphere is changed to air (oxygen partial pressure is about 0.2 atm) and heated for 5 hours without changing the temperature, so that the CaO—Fe 2 O 3 —Fe 3 O 4 -based compound is deposited on the surface of the solid solution. I let you. When cooled to room temperature, a coating layer composed of a crystalline phase of 2CaO · Fe 2 O 3 was formed. The calcia material after the heat treatment was allowed to stand for 48 hours in a constant temperature and humidity apparatus having a temperature of 70 ° C. and a humidity of 90%, and the hydration resistance was evaluated from the mass increase rate. The smaller the mass increase rate, the better the hydration resistance.
［実施例２］
炭酸カルシウムの粉体に酸化鉄（Ｆｅ２Ｏ３）の粉体を［Ｆｅ２Ｏ３／（ＣａＯ＋Ｆｅ２Ｏ３）］×１００％＝５質量％の比率で添加し、混合した後、直径２５ｍｍ×高さ１０ｍｍの円柱体に成形した。円柱体を酸素分圧が１０−５ａｔｍの（Ａｒ＋Ｏ２）雰囲気（全圧力は１ａｔｍ）中において１６００℃で５時間加熱し、ＣａＯ−ＦｅＯ固溶体を生成させた後、雰囲気を変更せずに温度を１２００℃まで下げて５時間保持し、２ＣａＯ・Ｆｅ２Ｏ３結晶相の被覆層を形成させた。熱処理後のカルシア質材料を実施例１に示した方法で耐水和性を評価した。
[Example 2]
The powder of iron oxide (Fe 2 O 3 ) was added to the calcium carbonate powder at a ratio of [Fe 2 O 3 / (CaO + Fe 2 O 3 )] × 100% = 5% by mass, and after mixing, the diameter was 25 mm. X Molded into a cylindrical body having a height of 10 mm. The cylindrical body was heated at 1600 ° C. for 5 hours in an (Ar + O 2 ) atmosphere with an oxygen partial pressure of 10 −5 atm (total pressure is 1 atm) to form a CaO—FeO solid solution, and then the temperature was changed without changing the atmosphere. The temperature was lowered to 1200 ° C. and held for 5 hours to form a coating layer of 2CaO · Fe 2 O 3 crystal phase. The calcia material after the heat treatment was evaluated for hydration resistance by the method shown in Example 1.
［比較例１］
酸化鉄が添加されていない炭酸カルシウムの粉体を直径２５ｍｍ×高さ１０ｍｍの円柱体に成形した後、円柱体を大気雰囲気中において１６００℃で５時間加熱した。熱処理後のカルシア材料を実施例１に示した方法で耐水和性を評価した。
[Comparative Example 1]
After forming calcium carbonate powder to which iron oxide was not added into a cylindrical body having a diameter of 25 mm and a height of 10 mm, the cylindrical body was heated in air at 1600 ° C. for 5 hours. The calcia material after the heat treatment was evaluated for hydration resistance by the method shown in Example 1.
［比較例２］
炭酸カルシウムの粉体に酸化鉄（Ｆｅ２Ｏ３）の粉体を［Ｆｅ２Ｏ３／（ＣａＯ＋Ｆｅ２Ｏ３）］×１００％＝５質量％の比率で添加し、混合した後、直径２５ｍｍ×高さ１０ｍｍの円柱体に成形した。円柱体を大気雰囲気中において１６００℃で５時間加熱した。加熱後の試料中酸化鉄は、２ＣａＯ・Ｆｅ２Ｏ３粒の状態でＣａＯ粒の間に分布した。熱処理後のカルシア質材料を実施例１に示した方法で耐水和性を評価した。
[Comparative Example 2]
The powder of iron oxide (Fe 2 O 3 ) was added to the calcium carbonate powder at a ratio of [Fe 2 O 3 / (CaO + Fe 2 O 3 )] × 100% = 5% by mass, and after mixing, the diameter was 25 mm. X Molded into a cylindrical body having a height of 10 mm. The cylinder was heated at 1600 ° C. for 5 hours in an air atmosphere. The iron oxide in the sample after heating was distributed among the CaO grains in the form of 2CaO · Fe 2 O 3 grains. The calcia material after the heat treatment was evaluated for hydration resistance by the method shown in Example 1.
実施例１、２および比較例１、２に対する水和試験結果を図１に示す。図中の水和指数は、水和テスト前後における各材料の質量増加率と比較例１のカルシア材料のそれとの比である。図１から本発明のカルシア質材料は高い耐水和性を示すことがわかる。これは、段階的熱処理によりＣａＯ−ＦｅＯ固溶体に被覆効果の良いＣａＯ−Ｆｅ２Ｏ３−Ｆｅ３Ｏ４系化合物の被覆層を析出させたためで、この被覆層が冷却により高耐水和性の２ＣａＯ・Ｆｅ ２ Ｏ ３ の結晶相からなる被覆層が形成された結果である。 The hydration test results for Examples 1 and 2 and Comparative Examples 1 and 2 are shown in FIG . The hydration index in the figure is the ratio between the mass increase rate of each material before and after the hydration test and that of the calcia material of Comparative Example 1. 1 that the calcia material of the present invention exhibits high hydration resistance. This is because to precipitate a coating layer of CaO-FeO good solid solution coating effect CaO-Fe 2 O 3 -Fe 3 O 4 compounds by stepwise heat treatment, 2CaO the coating layer is highly water-dispersible by cooling This is a result of the formation of a coating layer made of a crystal phase of Fe 2 O 3 .
本発明のカルシア質材料は、浸漬ノズルなどの製鉄・製鋼用耐火物へ応用できるし、セメント製造用耐火物などの分野にも応用できる。 The calcia material of the present invention can be applied to refractories for iron and steel making such as immersion nozzles, and can also be applied to fields such as refractories for cement production.
Claims (2)
得られた成形物を酸素分圧が１０−３０〜０．１ａｔｍの雰囲気で全圧力は１ａｔｍ中において８００〜２５００℃の範囲で前段階熱処理をすることにより、ＣａＯ−ＦｅＯ系固溶体を生成させ、次に、酸素分圧が１０−２５〜１ａｔｍの雰囲気で全圧力は１ａｔｍ中において８００〜２５００℃の範囲で前記固溶体生成条件の前段階と異なる雰囲気および／又は加熱温度下で後段階熱処理をして、ＣａＯ−Ｆｅ２Ｏ３−Ｆｅ３Ｏ４系化合物を前記固溶体表面に析出させたのち冷却して、
２ＣａＯ・Ｆｅ２Ｏ３の結晶相からなる被覆層を形成させることを特徴とする高耐水和性のカルシア質材料の製造方法。 [Fe 2 O 3 / (CaO + Fe 2 O 3 )] × 100% = 0 in terms of Fe 2 O 3 , as a mixture of starting materials including an iron component and a calcium component. After adding and mixing at a ratio of 3 to 15% by mass, it is molded into a predetermined shape,
The obtained molded product is subjected to pre-stage heat treatment in an atmosphere with an oxygen partial pressure of 10 −30 to 0.1 atm and a total pressure of 800 to 2500 ° C. in 1 atm to generate a CaO—FeO-based solid solution, Next, post-stage heat treatment is performed in an atmosphere having an oxygen partial pressure of 10 −25 to 1 atm and a total pressure in the range of 800 to 2500 ° C. in 1 atm and under an atmosphere and / or heating temperature different from the previous stage of the solid solution generation conditions. Then, the CaO—Fe 2 O 3 —Fe 3 O 4 -based compound is deposited on the surface of the solid solution and then cooled,
A method for producing a highly hydration resistant calcia material, characterized in that a coating layer comprising a crystal phase of 2CaO · Fe 2 O 3 is formed.
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