JP4592165B2 - Adjustment method for setting time of hydraulic material - Google Patents
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Description
【０００１】
【発明の属する技術分野】
本発明は、急硬性セメント、速硬性セメント、急結材、地盤改良材、マスキング材等に使用される水硬性材料、及びその製造方法に関する。
【０００２】
【従来の技術】
カルシウムアルミネートは、水硬性を有することが知られており、アルミナセメント、急硬性セメント、急結材、速硬性セメント、地盤改良材、マスキング材等の材料として用いられている。
【０００３】
しかしながら、カルシウムアルミネートは、実用に際し、注水と同時に硬化が進行するため、作業時間を確保できず、練り混ぜ不十分となり易く、良好なコンクリートを得ることが困難であった。
【０００４】
そこで、凝結時間が長く作業性の改善された水硬性材料の製造方法として、１２ＣａＯ・７Ａｌ2Ｏ3を主成分とするカルシウムアルミネートを溶融した後、急冷して非晶質カルシウムアルミネート類を製造し、次いで、これを粉砕した後、焼成して、結晶質のカルシウムアルミネート類を得る方法が報告されている（特開平４−２０９７３８号）。
【０００５】
しかしながら、この製造方法では、高温においてカルシウムアルミネート類を溶融させるために、電力費や設備費が高くなり、製造コストが高騰するという問題点がある。しかも、溶融、粉砕、焼成という工程を含むために、製造方法が煩雑である。
【０００６】
【発明が解決しようとする課題】
本発明の主な目的は、複雑な工程を要することなく製造可能な水硬性材料であって、良好な水硬性を有し、しかも凝結速度の調整が可能な材料を提供することである。
【０００７】
【課題を解決するための手段】
本発明者は、上記した目的を達成すべく、鋭意研究を重ねてきた。その結果、石灰質原料、アルミナ質原料及びフッ化カルシウム質原料からなるカルシウムアルミネート焼結用原料を、１１ＣａＯ・７Ａｌ2Ｏ3・ＣａＦ2固溶体の融点を下回る温度で焼成することによって、優れた水硬性を有する結晶質の１１ＣａＯ・７Ａｌ2Ｏ3・ＣａＦ2固溶体を含む焼結体をクリンカーとして製造できることを見出した。そして、この製造方法によれば、焼結体中の結晶質１１ＣａＯ・７Ａｌ2Ｏ3・ＣａＦ2固溶体は、従来の溶融法によって得られるものと比べて大きい格子定数を有するものとなり、しかも、焼成温度を調整することによって、その格子定数を変化させることができ、それに伴って、凝結速度が変化するため、使用目的に応じた凝結時間を有する水硬性材料を簡単に製造できることを見出し、ここに本発明を完成するに至った。
【０００８】
即ち、本発明は、以下の水硬性材料の凝結時間の調整方法を提供するものである。
１．石灰質原料、アルミナ質原料及びフッ化カルシウム質原料を含むカルシウムアルミネート焼結用原料を、１１ＣａＯ・７Ａｌ 2 Ｏ 3 ・ＣａＦ 2 固溶体の溶融温度を下回る温度で焼成して、１１ＣａＯ・７Ａｌ 2 Ｏ 3 ・ＣａＦ 2 固溶体を含有する焼結体を製造する際に、焼成温度を変化させて１１ＣａＯ・７Ａｌ 2 Ｏ 3 ・ＣａＦ 2 の格子定数を変化させることによる、１１ＣａＯ・７Ａｌ 2 Ｏ 3 ・ＣａＦ 2 固溶体を含有する焼結体からなる水硬性材料の凝結時間の調整方法であって、
カルシウムアルミネート焼結用原料が、１２６５〜１３２０℃の範囲の温度で焼成した際に、格子定数が１．１９７９ｎｍ〜１．１９８１ｎｍの結晶質の１１ＣａＯ・７Ａｌ 2 Ｏ 3 ・ＣａＦ 2 固溶体を形成し、１３４０〜１３９０℃の範囲の温度で焼成した際に、格子定数が１．１９８３ｎｍ〜１．１９８５ｎｍの結晶質の１１ＣａＯ・７Ａｌ 2 Ｏ 3 ・ＣａＦ 2 固溶体を形成するものであり、該原料を１２６５〜１３２０℃の範囲の温度で焼成して、格子定数が１．１９７９ｎｍ〜１．１９８１ｎｍの結晶質の１１ＣａＯ・７Ａｌ 2 Ｏ 3 ・ＣａＦ 2 固溶体を形成することによって急硬性セメント用の水硬性材料とすることを特徴とする凝結時間の調整方法。
２． 石灰質原料、アルミナ質原料及びフッ化カルシウム質原料を含むカルシウムアルミネート焼結用原料を、１１ＣａＯ・７Ａｌ 2 Ｏ 3 ・ＣａＦ 2 固溶体の溶融温度を下回る温度で焼成して、１１ＣａＯ・７Ａｌ 2 Ｏ 3 ・ＣａＦ 2 固溶体を含有する焼結体を製造する際に、焼成温度を変化させて１１ＣａＯ・７Ａｌ 2 Ｏ 3 ・ＣａＦ 2 の格子定数を変化させることによる、１１ＣａＯ・７Ａｌ 2 Ｏ 3 ・ＣａＦ 2 固溶体を含有する焼結体からなる水硬性材料の凝結時間の調整方法であって、
カルシウムアルミネート焼結用原料が、１２６５〜１３２０℃の範囲の温度で焼成した際に、格子定数が１．１９７９ｎｍ〜１．１９８１ｎｍの結晶質の１１ＣａＯ・７Ａｌ 2 Ｏ 3 ・ＣａＦ 2 固溶体を形成し、１３４０〜１３９０℃の範囲の温度で焼成した際に、格子定数が１．１９８３ｎｍ〜１．１９８５ｎｍの結晶質の１１ＣａＯ・７Ａｌ 2 Ｏ 3 ・ＣａＦ 2 固溶体を形成するものであり、該原料を１３４０〜１３９０℃の範囲の温度で焼成して、格子定数が１．１９８３ｎｍ〜１．１９８５ｎｍの結晶質の１１ＣａＯ・７Ａｌ 2 Ｏ 3 ・ＣａＦ 2 固溶体を形成することによって速硬性セメント用の水硬性材料とすることを特徴とする凝結時間の調整方法。
【０００９】
【発明の実施の形態】
本発明の水硬性材料は、格子定数が１．１９７２ｎｍ以上の結晶質の１１ＣａＯ・７Ａｌ2Ｏ3・ＣａＦ2固溶体を含有する焼結体からなるものである。このような焼結体は、石灰質原料、アルミナ質原料及びフッ化カルシウム質原料からなるカルシウムアルミネート焼結用原料を、１１ＣａＯ・７Ａｌ2Ｏ3・ＣａＦ2固溶体の溶融温度を下回る温度で焼結させることによって製造することが可能である。以下に、該焼結体の製造方法の一例を説明する。
【００１０】
まず、石灰質原料、アルミナ質原料及びフッ化カルシウム質原料を、目的物である１１ＣａＯ・７Ａｌ2Ｏ3・ＣａＦ2固溶体の組成比となるように配合する。
【００１１】
石灰質原料としては、石灰石等を用いることができ、アルミナ質原料としては、ボーキサイト、バンド頁岩等を用いることができ、フッ化カルシウム質原料としては、蛍石等を用いることができる。
【００１２】
これらの各原料成分を１１ＣａＯ・７Ａｌ2Ｏ3・ＣａＦ2固溶体の組成比となるように配合したカルシウムアルミネート焼結用原料に、添加剤としてＦｅ2Ｏ3とＴｉＯ2を配合する。Ｆｅ2Ｏ3の配合量は、全原料成分中０．１〜９重量％程度とすることが好ましく、ＴｉＯ2の配合量は全原料成分中０．５〜９重量％程度とすることが好ましい。これらの添加剤を配合する場合には、低温融液相が形成され、１１ＣａＯ・７Ａｌ2Ｏ3・ＣａＦ2の溶融温度を下回る温度において、融液を媒体とする焼結方法によって、結晶質の１１ＣａＯ・７Ａｌ2Ｏ3・ＣａＦ2 を含む焼結体を得ることができる。
【００１３】
焼成には、例えば、融液を媒体として焼結させる方式を採るロータリーキルン等を用ることができる。焼成温度は、１１ＣａＯ・７Ａｌ2Ｏ3・ＣａＦ2固溶体の溶融温度を下回る温度とすることが必要である。具体的な焼成温度は、形成するカルシウムアルミネートの種類、焼成方法等によって異なるが、通常、１２４０〜１４１５℃程度とすればよく、好ましくは１２６０〜１４００℃程度とすればよい。焼成時間は、通常、１〜２時間程度とすればよい。
【００１４】
焼成により、結晶質の１１ＣａＯ・Ａｌ2Ｏ3・ＣａＦ2系固溶体を含む焼結体を得た後、空気で急冷することによって、目的とする焼結体をクリンカーとして得ることができる。
【００１５】
上記した製造方法によれば、得られる焼結体（クリンカー）中の１１ＣａＯ・７Ａｌ2Ｏ3・ＣａＦ2固溶体は、格子定数が１．１９７２ｎｍ以上となり、原料を溶融して得た非晶質のカルシウムアルミネートを焼成して得られる１１ＣａＯ・７Ａｌ2Ｏ3・ＣａＦ2固溶体と比べて、大きい格子定数を有するものとなる。このような焼結体は、優れた水硬性を有し、適度な凝結速度を有するものとなる。格子定数の上限値については、良好な水硬性を発揮するためには、１．１９９５ｎｍ程度以下であることが好ましい。
本発明では、焼結体中における格子定数が１．１９７２〜１．１９９５ｎｍの結晶質の１１ＣａＯ・７Ａｌ2Ｏ3・ＣａＦ2固溶体の存在量は、良好な水硬性を発揮するためには、４０重量％程度以上であることが好ましく、６０重量％程度以上であることがより好ましく、７０重量％程度以上であることが更に好ましい。該焼結体中には、上記した結晶質の１１ＣａＯ・７Ａｌ2Ｏ3・ＣａＦ2固溶体以外の成分として、原料中に含まれる不純物や焼成条件に応じて、１２ＣａＯ・７Ａｌ2Ｏ3、３ＣａＯ・Ａｌ2Ｏ3、ＣａＯ・Ａｌ2Ｏ3等の各種カルシウムアルミネートや非晶質成分が含まれる。
【００１６】
上記した方法で得られる焼結体では、焼成温度を変化させることによって、該焼結体中の結晶質の１１ＣａＯ・７Ａｌ2Ｏ3・ＣａＦ2固溶体の格子定数を変化させることができる。具体的には、上記した焼成温度範囲において、焼成温度を高くすることによって、格子定数を大きくすることができる。通常は、１２４０〜１３２０℃程度の焼結温度において、１．１９７２ｎｍ〜１．１９８１ｎｍ程度の格子定数の１１ＣａＯ・７Ａｌ2Ｏ3・ＣａＦ2固溶体が形成され、１３３０〜１４１５℃程度の焼結温度において、１．１９８２ｎｍ〜１．１９９０ｎｍ程度の格子定数の１１ＣａＯ・７Ａｌ2Ｏ3・ＣａＦ2固溶体が形成される。
【００１７】
本発明の処理対象とする水硬性材料は、焼結体中に含まれる結晶質１１ＣａＯ・７Ａｌ2Ｏ3・ＣａＦ2固 溶体の格子定数の相違によって、凝結速度が異なるものとなる。具体的には、格子定数が１．１９７９ｎｍ〜１．１９８１ｎｍ程度の範囲にある場合に、注水後すぐに凝結が始まる急硬性セメント用の水硬性材料として適度な凝結速度を有するものとなり、格子定数が１．１９８３ｎｍ〜１．１９８５ｎｍ程度の範囲にある場合に、注水後 ３０〜６０分程度経過後に凝結が始まる速硬性セメント用の水硬性材料として適度な凝結速度を有するものとなる。
【００１８】
本発明の水硬性材料は、目的に応じた適度な粒度に粉砕して用いればよい。粒度については、特に限定的ではないが、通常、ブレーン比表面積で２０００〜８０００ｃｍ2／ｇ程度とすればよい。
【００１９】
本発明の水硬性材料は、良好な水硬性を有するものであり、急硬性セメント、速硬性セメント、急結材、地盤改良材、マズキング材等に使用される水硬性材料として有用である。
【００２０】
【発明の効果】
本発明によれば、複雑な製造工程を要すること無く、原料成分を焼成するという簡単な方法によって、優れた水硬性を有する材料を得ることができる。
【００２１】
本発明では、焼結温度に応じて焼結体中のカルシウムアルミネートの格子定数を変化させることができ、それにより水硬性材料の凝結時間の調整が可能である。よって、目的に応じた作業時間を有する水硬性材料を容易に得ることができる。
【００２２】
【実施例】
以下、実施例を挙げて本発明を更に詳細に説明する。
実施例１
石灰質原料として、石灰石を用い、アルミナ質原料として、ボーキサイトを用い、フッ化カルシウム質原料として、蛍石を用い、更に、添加剤としてＴｉＯ2とＦｅ2Ｏ3を用いて、これらの原料を下記表１に示す配合組成となる様に混合した。
【００２３】
【表１】
これらの原料を、電気炉中で下記表３に示す焼成温度で１時間焼成した後、直ちに炉外に取り出すことによって急冷し、その後、ブレーン比表面積５０００±１００ｃｍ2／ｇに粉砕して、水硬性材料を得た。
【００２５】
これらの全ての試料についてｆ−ＣａＯ量は０．５％以下であり、クリンカー生成反応が十分に進行していることを確認した。また、クリンカー（焼結体）中のカルシウムアルミネート相を分離し、フッ素量を測定することで、１１ＣａＯ・７Ａｌ2Ｏ3・ＣａＦ2固溶体を含有するカルシウムアルミネート類の生成を確認した。
【００２６】
更に、下記の条件でカルシウムアルミネート相の格子定数を測定した。
＊格子定数測定方法
格子定数は、高純度化学研究所製金属シリコン粉末を内部標準とし、理学電機社製ＲＡＤ−ｒＣシステムを用い、粉末Ｘ線回折にて測定した。
回折角度は半価幅中点法により求め、回折角の補正は、得られた内部標準試料の回折線から補正値を算出し、最小二乗法によって行った。
【００２７】
上記した方法において、走査範囲（２θ）は下記表２に示す通りである。また、格子定数の測定結果を下記表３に示す。
【００２８】
また、住友大阪セメント（株）製普通ポルトランドセメントと愛知県瀬戸市産珪砂を使用して、モルタルの強度試験方法（ＪＩＳ Ｒ ５２０１）に従ってモルタルを混練し、３０分間静置した後、上記した方法で作製した各急硬性材料を添加して３０秒間混練した。これらのモルタルについて、コンクリートの凝結試験方法（ＪＩＳ Ａ ６２０４）に準じたプロクター貫入試験によって始発時間を測定し、凝結性状を評価した。試験温度は５℃とした。結果を下記表３に示す。
【００２９】
また、上記したセメントと砂を用いてモルタルの強度試験方法（ＪＩＳ Ｒ ５２０１）に従ってモルタルを混練し、３０分間静置した後、上記した方法で得た各水硬性材料を添加して３０秒間混練し、このモルタルを強度試験に供して強度発現性状を評価した。材齢２８日の圧縮強度試験結果を下記表３に示す。
【００３０】
【表２】
【表３】
BACKGROUND OF THE INVENTION
The present invention relates to a hydraulic material used for quick-hardening cement, quick-hardening cement, quick-setting material, ground improvement material, masking material, and the like, and a manufacturing method thereof.
[0002]
[Prior art]
Calcium aluminate is known to have hydraulic properties, and is used as a material for alumina cement, quick hardening cement, quick setting material, quick hardening cement, ground improvement material, masking material and the like.
[0003]
However, since calcium aluminate is hardened simultaneously with water injection in practical use, working time cannot be secured, kneading tends to be insufficient, and it is difficult to obtain good concrete.
[0004]
Therefore, as a method for producing a hydraulic material having a long setting time and improved workability, after melting calcium aluminate containing 12CaO · 7Al 2 O 3 as a main component, it is rapidly cooled to obtain amorphous calcium aluminates. A method for producing a crystalline calcium aluminate after being produced and then pulverized and then fired has been reported (Japanese Patent Laid-Open No. 4-209738).
[0005]
However, in this manufacturing method, there is a problem that power costs and equipment costs increase because the calcium aluminates are melted at a high temperature, and the manufacturing costs increase. In addition, the manufacturing method is complicated because it includes steps of melting, crushing, and firing.
[0006]
[Problems to be solved by the invention]
A main object of the present invention is to provide a hydraulic material that can be manufactured without requiring a complicated process, has a good hydraulic property, and can adjust a setting speed.
[0007]
[Means for Solving the Problems]
The present inventor has intensively studied to achieve the above-described object. As a result, excellent water is obtained by firing a calcium aluminate sintering raw material comprising a calcareous raw material, an alumina raw material and a calcium fluoride raw material at a temperature below the melting point of 11CaO · 7Al 2 O 3 · CaF 2 solid solution. It has been found that a sintered body containing a crystalline 11CaO · 7Al 2 O 3 · CaF 2 solid solution having hardness can be produced as a clinker. According to this manufacturing method, the crystalline 11CaO.7Al 2 O 3 .CaF 2 solid solution in the sintered body has a larger lattice constant than that obtained by the conventional melting method, and further, firing. By adjusting the temperature, the lattice constant can be changed, and accordingly, the setting speed changes, and it has been found that a hydraulic material having a setting time according to the purpose of use can be easily produced. The present invention has been completed.
[0008]
That is, the present invention provides the following method for adjusting the setting time of a hydraulic material.
1. A calcium aluminate sintering raw material including a calcareous raw material, an alumina raw material, and a calcium fluoride raw material is fired at a temperature lower than the melting temperature of 11CaO · 7Al 2 O 3 · CaF 2 solid solution, and 11CaO · 7Al 2 O 3 · in making a sintered body containing CaF 2 solid solution, changing the firing temperature by varying the lattice constant of 11CaO · 7Al 2 O 3 · CaF 2 and, 11CaO · 7Al 2 O 3 · CaF 2 solid solution A method for adjusting the setting time of a hydraulic material comprising a sintered body containing
Calcium aluminate sintering raw material is, when fired at a temperature in the range of from 1265 to 1320 ° C., the lattice constant is formed a 11CaO · 7Al 2 O 3 · CaF 2 solid solution of crystalline 1.1979nm~1.1981nm , when fired at a temperature in the range of 1,340 to 1390 ° C., are those lattice constant to form a 11CaO · 7Al 2 O 3 · CaF 2 solid solution of crystalline 1.1983Nm～1.1985Nm, the raw material 1265 ～1320 and fired at a temperature in the range of ° C., and hydraulic material for rapid hardening cement by lattice constant to form a 11CaO · 7Al 2 O 3 · CaF 2 solid solution of crystalline 1.1979nm~1.1981nm A method for adjusting the setting time, characterized by:
2. A calcium aluminate sintering raw material including a calcareous raw material, an alumina raw material, and a calcium fluoride raw material is fired at a temperature lower than the melting temperature of 11CaO · 7Al 2 O 3 · CaF 2 solid solution, and 11CaO · 7Al 2 O 3 · in making a sintered body containing CaF 2 solid solution, changing the firing temperature by varying the lattice constant of 11CaO · 7Al 2 O 3 · CaF 2 and, 11CaO · 7Al 2 O 3 · CaF 2 solid solution A method for adjusting the setting time of a hydraulic material comprising a sintered body containing
Calcium aluminate sintering raw material is, when fired at a temperature in the range of from 1265 to 1320 ° C., the lattice constant is formed a 11CaO · 7Al 2 O 3 · CaF 2 solid solution of crystalline 1.1979nm~1.1981nm , when fired at a temperature in the range of 1,340 to 1390 ° C., are those lattice constant to form a 11CaO · 7Al 2 O 3 · CaF 2 solid solution of crystalline 1.1983Nm～1.1985Nm, the raw material 1340 ～1390 and fired at a temperature in the range of ° C., and hydraulic material for quick-setting cement by lattice constant to form a 11CaO · 7Al 2 O 3 · CaF 2 solid solution of crystalline 1.1983nm~1.1985nm A method for adjusting the setting time, characterized by:
[0009]
DETAILED DESCRIPTION OF THE INVENTION
The hydraulic material of the present invention is composed of a sintered body containing a crystalline 11CaO.7Al 2 O 3 .CaF 2 solid solution having a lattice constant of 1.1972 nm or more. Such a sintered body is obtained by sintering a calcium aluminate sintering raw material composed of a calcareous raw material, an alumina raw material and a calcium fluoride raw material at a temperature lower than the melting temperature of the 11CaO · 7Al 2 O 3 · CaF 2 solid solution. Can be manufactured. Below, an example of the manufacturing method of this sintered compact is demonstrated.
[0010]
First, a calcareous raw material, an alumina raw material, and a calcium fluoride raw material are blended so as to have a composition ratio of 11CaO · 7Al 2 O 3 · CaF 2 solid solution as a target product.
[0011]
Limestone or the like can be used as the calcareous material, bauxite, band shale or the like can be used as the alumina material, and fluorite or the like can be used as the calcium fluoride material.
[0012]
Fe 2 O 3 and TiO 2 are added as additives to a calcium aluminate sintering raw material in which these raw material components are blended so as to have a composition ratio of 11CaO · 7Al 2 O 3 · CaF 2 solid solution. The blending amount of Fe 2 O 3 is preferably about 0.1 to 9% by weight in all raw material components, and the blending amount of TiO 2 is preferably about 0.5 to 9% by weight in all raw material components. . When these additives are blended, a low-temperature melt phase is formed, and at a temperature lower than the melting temperature of 11CaO · 7Al 2 O 3 · CaF 2 , a crystalline process is performed by a sintering method using the melt as a medium. A sintered body containing 11CaO · 7Al 2 O 3 · CaF 2 can be obtained.
[0013]
For the firing, for example, a rotary kiln that employs a method of sintering using a melt as a medium can be used. The firing temperature must be lower than the melting temperature of the 11CaO · 7Al 2 O 3 · CaF 2 solid solution. The specific firing temperature varies depending on the type of calcium aluminate to be formed, the firing method, and the like, but is usually about 1240 to 1415 ° C, and preferably about 1260 to 1400 ° C. The firing time may normally be about 1 to 2 hours.
[0014]
After obtaining a sintered body containing a crystalline 11CaO.Al 2 O 3 .CaF 2 solid solution by firing, the objective sintered body can be obtained as a clinker by quenching with air.
[0015]
According to the manufacturing method described above, the 11CaO · 7Al 2 O 3 · CaF 2 solid solution in the obtained sintered body (clinker) has a lattice constant of 1.1972 nm or more, and is an amorphous material obtained by melting the raw material. Compared with the 11CaO · 7Al 2 O 3 · CaF 2 solid solution obtained by firing calcium aluminate, it has a large lattice constant. Such a sintered body has excellent hydraulic properties and an appropriate setting speed. About the upper limit of a lattice constant, in order to exhibit favorable hydraulic property, it is preferable that it is about 1.1995 nm or less.
In the present invention, the abundance of the crystalline 11CaO · 7Al 2 O 3 · CaF 2 solid solution having a lattice constant of 1.972 to 1.1995 nm in the sintered body is 40 in order to exhibit good hydraulic properties. It is preferably about wt% or more, more preferably about 60 wt% or more, and even more preferably about 70 wt% or more. During sintered body, as above-mentioned 11CaO · 7Al 2 O 3 · CaF 2 components other than the solid solution of crystalline, depending on the impurities and firing conditions contained in the raw material, 12CaO · 7Al 2 O 3, 3CaO · Various calcium aluminates such as Al 2 O 3 and CaO.Al 2 O 3 and amorphous components are included.
[0016]
In the sintered body obtained by the above-described method, the lattice constant of the crystalline 11CaO · 7Al 2 O 3 · CaF 2 solid solution in the sintered body can be changed by changing the firing temperature. Specifically, the lattice constant can be increased by increasing the firing temperature in the above firing temperature range. Usually, at a sintering temperature of about 1240 to 1320 ° C., an 11CaO · 7Al 2 O 3 · CaF 2 solid solution having a lattice constant of about 1.1972 nm to 1.1981 nm is formed, and at a sintering temperature of about 1330 to 1415 ° C. 11CaO.7Al 2 O 3 .CaF 2 solid solution having a lattice constant of about 1.1982 nm to 1.1990 nm is formed.
[0017]
The hydraulic material to be treated according to the present invention has different setting speeds due to the difference in the lattice constant of the crystalline 11CaO · 7Al 2 O 3 · CaF 2 solid solution contained in the sintered body. Specifically, the lattice constant is 1 . When it is in the range of about 1979 nm to 1.1981 nm, it has an appropriate setting speed as a hydraulic material for rapid hardening cement which starts setting immediately after water injection, and the lattice constant is 1 . When it is in the range of about 1983 nm to 1.1985 nm, it has an appropriate setting speed as a hydraulic material for fast-setting cement that starts setting after about 30 to 60 minutes after water injection.
[0018]
The hydraulic material of the present invention may be used after being pulverized to an appropriate particle size according to the purpose. The particle size is not particularly limited, but is usually about 2000 to 8000 cm 2 / g in terms of the specific surface area of branes.
[0019]
The hydraulic material of the present invention has good hydraulic properties, and is useful as a hydraulic material used for quick setting cement, quick setting cement, quick setting material, ground improvement material, muzzking material and the like.
[0020]
【The invention's effect】
According to the present invention, a material having excellent hydraulic properties can be obtained by a simple method of firing raw material components without requiring a complicated manufacturing process.
[0021]
In the present invention, the lattice constant of the calcium aluminate in the sintered body can be changed according to the sintering temperature, whereby the setting time of the hydraulic material can be adjusted. Therefore, a hydraulic material having a working time according to the purpose can be easily obtained.
[0022]
【Example】
Hereinafter, the present invention will be described in more detail with reference to examples.
Example 1
Limestone is used as the calcareous raw material, bauxite is used as the alumina raw material, fluorite is used as the calcium fluoride raw material, and further TiO 2 and Fe 2 O 3 are used as additives. It mixed so that it might become a formulation composition shown in Table 1.
[0023]
[Table 1]
These raw materials were fired in an electric furnace at the firing temperature shown in Table 3 below for 1 hour, and then immediately cooled by taking them out of the furnace, and then ground to a specific surface area of 5000 ± 100 cm 2 / g in water. A hard material was obtained.
[0025]
For all these samples, the amount of f-CaO was 0.5% or less, and it was confirmed that the clinker formation reaction proceeded sufficiently. Further, clinker (sintered) in the calcium aluminate phase was separated, by measuring the amount of fluorine was confirmed the formation of calcium aluminates containing 11CaO · 7Al 2 O 3 · CaF 2 solid solution.
[0026]
Furthermore, the lattice constant of the calcium aluminate phase was measured under the following conditions.
* Lattice constant measurement method The lattice constant was measured by powder X-ray diffraction using RAD-rC system manufactured by Rigaku Corporation with metal silicon powder manufactured by High Purity Chemical Laboratory as an internal standard.
[0027]
In the above method, the scanning range (2θ) is as shown in Table 2 below. The measurement results of the lattice constant are shown in Table 3 below.
[0028]
In addition, using the normal Portland cement manufactured by Sumitomo Osaka Cement Co., Ltd. and silica sand from Seto City, Aichi Prefecture, the mortar was kneaded according to the strength test method for mortar (JIS R 5201) and allowed to stand for 30 minutes. Each quick-hardening material prepared in (1) was added and kneaded for 30 seconds. About these mortars, the initial time was measured by the proctor penetration test according to the concrete setting test method (JIS A6204), and the setting property was evaluated. The test temperature was 5 ° C. The results are shown in Table 3 below.
[0029]
In addition, mortar was kneaded according to the mortar strength test method (JIS R 5201) using the above cement and sand, allowed to stand for 30 minutes, and then each hydraulic material obtained by the above method was added and kneaded for 30 seconds. The mortar was subjected to a strength test to evaluate the strength development property. Table 3 below shows the results of the compressive strength test on the material age 28 days.
[0030]
[Table 2]
[Table 3]
Claims (2)
カルシウムアルミネート焼結用原料が、１２６５〜１３２０℃の範囲の温度で焼成した際に、格子定数が１．１９７９ｎｍ〜１．１９８１ｎｍの結晶質の１１ＣａＯ・７Ａｌ 2 Ｏ 3 ・ＣａＦ 2 固溶体を形成し、１３４０〜１３９０℃の範囲の温度で焼成した際に、格子定数が１．１９８３ｎｍ〜１．１９８５ｎｍの結晶質の１１ＣａＯ・７Ａｌ 2 Ｏ 3 ・ＣａＦ 2 固溶体を形成するものであり、該原料を１２６５〜１３２０℃の範囲の温度で焼成して、格子定数が１．１９７９ｎｍ〜１．１９８１ｎｍの結晶質の１１ＣａＯ・７Ａｌ2Ｏ3・ＣａＦ2固溶体を形成することによって急硬性セメント用の水硬性材料とすることを特徴とする凝結時間の調整方法。A calcium aluminate sintering raw material including a calcareous raw material, an alumina raw material, and a calcium fluoride raw material is fired at a temperature lower than the melting temperature of 11CaO · 7Al 2 O 3 · CaF 2 solid solution, and 11CaO · 7Al 2 O 3 · in making a sintered body containing CaF 2 solid solution, changing the firing temperature by varying the lattice constant of 11CaO · 7Al 2 O 3 · CaF 2 and, 11CaO · 7Al 2 O 3 · CaF 2 solid solution A method for adjusting the setting time of a hydraulic material comprising a sintered body containing
Calcium aluminate sintering raw material is, when fired at a temperature in the range of from 1265 to 1320 ° C., the lattice constant is formed a 11CaO · 7Al 2 O 3 · CaF 2 solid solution of crystalline 1.1979nm~1.1981nm , when fired at a temperature in the range of 1,340 to 1390 ° C., are those lattice constant to form a 11CaO · 7Al 2 O 3 · CaF 2 solid solution of crystalline 1.1983Nm～1.1985Nm, the raw material 1265 Calcinated at a temperature in the range of ˜1320 ° C. to form a crystalline 11CaO.7Al 2 O 3 .CaF 2 solid solution having a lattice constant of 1.1979 nm to 1.1981 nm, A method for adjusting the setting time, characterized by:
カルシウムアルミネート焼結用原料が、１２６５〜１３２０℃の範囲の温度で焼成した際に、格子定数が１．１９７９ｎｍ〜１．１９８１ｎｍの結晶質の１１ＣａＯ・７Ａｌ 2 Ｏ 3 ・ＣａＦ 2 固溶体を形成し、１３４０〜１３９０℃の範囲の温度で焼成した際に、格子定数が１．１９８３ｎｍ〜１．１９８５ｎｍの結晶質の１１ＣａＯ・７Ａｌ 2 Ｏ 3 ・ＣａＦ 2 固溶体を形成するものであり、該原料を１３４０〜１３９０℃の範囲の温度で焼成して、格子定数が１．１９８３ｎｍ〜１．１９８５ｎｍの結晶質の１１ＣａＯ・７Ａｌ2Ｏ3・ＣａＦ2固溶体を形成することによって速硬性セメント用の水硬性材料とすることを特徴とする凝結時間の調整方法。A calcium aluminate sintering raw material including a calcareous raw material, an alumina raw material, and a calcium fluoride raw material is fired at a temperature lower than the melting temperature of 11CaO · 7Al 2 O 3 · CaF 2 solid solution, and 11CaO · 7Al 2 O 3 · in making a sintered body containing CaF 2 solid solution, changing the firing temperature by varying the lattice constant of 11CaO · 7Al 2 O 3 · CaF 2 and, 11CaO · 7Al 2 O 3 · CaF 2 solid solution A method for adjusting the setting time of a hydraulic material comprising a sintered body containing
Calcium aluminate sintering raw material is, when fired at a temperature in the range of from 1265 to 1320 ° C., the lattice constant is formed a 11CaO · 7Al 2 O 3 · CaF 2 solid solution of crystalline 1.1979nm~1.1981nm , when fired at a temperature in the range of 1,340 to 1390 ° C., are those lattice constant to form a 11CaO · 7Al 2 O 3 · CaF 2 solid solution of crystalline 1.1983Nm～1.1985Nm, the raw material 1340 Calcination at a temperature in the range of ˜1390 ° C. to form a crystalline 11CaO.7Al 2 O 3 .CaF 2 solid solution having a lattice constant of 1.1983 nm to 1.1985 nm; A method for adjusting the setting time, characterized by:
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