JP2020083712A - Cement-based solidification material and manufacturing method therefor - Google Patents

Cement-based solidification material and manufacturing method therefor Download PDF

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JP2020083712A
JP2020083712A JP2018221750A JP2018221750A JP2020083712A JP 2020083712 A JP2020083712 A JP 2020083712A JP 2018221750 A JP2018221750 A JP 2018221750A JP 2018221750 A JP2018221750 A JP 2018221750A JP 2020083712 A JP2020083712 A JP 2020083712A
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cement
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zinc
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solidifying material
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JP7185994B2 (en
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浩大 土肥
Kota Doi
浩大 土肥
武 河野
Takeshi Kono
武 河野
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Mitsubishi Materials Corp
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
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    • Y02W30/50—Reuse, recycling or recovery technologies
    • Y02W30/91—Use of waste materials as fillers for mortars or concrete

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  • Consolidation Of Soil By Introduction Of Solidifying Substances Into Soil (AREA)
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Abstract

To solve the problem in which countermeasures to prevent reduced flowability of slurry under high temperature environment are insufficient in the conventional cement-based solidification material, and to thereby provide a cement-based solidification material with less reduction of flowability even in the high temperature environment.SOLUTION: The present invention relates to a cement-based solidification material which, in a solidification material including portland cement and gypsum, contains zinc and lead and has a total content of zinc and lead of 500 mg/kg or more and 1000 mg/kg or less, and preferably contains particles sieved with a 20 μm sieve of 50 mass% or more and 100 mass% or less and has a zinc content of the particles of 600 mg/kg or more and a lead content of 100 mg/kg or more, and a manufacturing method therefor.SELECTED DRAWING: None

Description

本発明は、高温環境下でもスラリーの流動性の低下が少ない、セメント系固化材およびその製造方法に関する。 TECHNICAL FIELD The present invention relates to a cement-based solidifying material and a method for producing the same, in which the fluidity of a slurry is not significantly reduced even in a high temperature environment.

セメント系固化材は、土壌の液状化防止や軟弱地盤の固化強化などの、土質の固化改良のために使用される、ポルトランドセメントを主材とした固化材である。 The cement-based solidifying material is a solidifying material mainly composed of Portland cement, which is used for improving solidification of soil such as preventing liquefaction of soil and strengthening solidification of soft ground.

一般的なセメント系固化材には硬化促進剤として石膏が配合されており、石膏はセメント中のアルミネート相と反応してエトリンガイトを生成し、セメントだけでは固化し難い軟弱土などを効率的に固化する作用がある。通常、セメント系固化材はスラリーにして用いられるが、夏場の高温環境下において、スラリーの温度が上昇して石膏とアルミネート相との反応が進むとエトリンガイトの生成が多くなり、凝結速度が増してスラリーの流動性が低下する問題を招く。 Gypsum is blended as a hardening accelerator in a general cement-based solidifying material, and gypsum reacts with the aluminate phase in the cement to form ettringite, which effectively hardens soft soil that is hard to solidify with cement alone. Has the effect of solidifying. Cement-based solidifying materials are usually used in the form of slurries, but in a high temperature environment in the summer, when the temperature of the slurries rises and the reaction between gypsum and the aluminate phase progresses, ettringite formation increases and the setting speed increases. As a result, the fluidity of the slurry is reduced.

スラリーの流動性の低下によって、ポンプ圧送速度の低下や圧送ラインの詰まりなどのトラブルが生じるので、このようなトラブルを防止するために、材料の練り混ぜ水や固化材の温度を下げるなどの対策が試みられるが、炎天下の施工現場などでは材料を低温に保つことは難しいため有効な解決策にならないことが多い。 As the fluidity of the slurry decreases, problems such as a decrease in pump pumping speed and clogging of the pumping line may occur.In order to prevent such problems, measures such as lowering the temperature of the material mixing water and the solidifying material are taken. However, since it is difficult to keep the material at a low temperature in a construction site under hot weather, it is often not an effective solution.

高温環境下におけるセメント系固化材スラリーの流動性が低下する問題を解決するために、例えば、従来、以下の対策が知られている。
(１) 特開２００４−２３１４７９号公報（特許文献１）には、セメント系固化材に含まれる三酸化硫黄含有量を６〜１５質量％、塩素含有量を０.１〜２.０質量％の範囲にし、さらに１５〜５０質量部の高炉スラグを配合することによって、高温下でもスラリーの流動性の低下を防止することが提案されている。しかし、この固化材は環境温度が３５℃程度になるとスラリーの流動性が低下するようになり、流動性低下防止の効果は不十分である。 In order to solve the problem that the fluidity of the cementitious solidifying material slurry under a high temperature environment is reduced, for example, the following measures are conventionally known.
(1) In JP-A-2004-231479 (Patent Document 1), the content of sulfur trioxide contained in the cement-based solidifying material is 6 to 15% by mass, and the content of chlorine is 0.1 to 2.0% by mass. It is proposed to prevent the deterioration of the fluidity of the slurry even at a high temperature by blending the blast furnace slag in an amount of 15 to 50 parts by mass in the above range. However, when the solidifying material has an ambient temperature of about 35° C., the fluidity of the slurry decreases, and the effect of preventing fluidity deterioration is insufficient.

（２）特開２０１０−１５９３４７号公報（特許文献２）には、セメントクリンカ、石膏、および消石灰を配合してなる土壌固化材について、この土壌固化材に水を加えたスラリーとして使用する場合、該スラリーの流動性の低下を避けるために消石灰の粒子径を調整し、粒子径３０μｍ以上の粒子を５〜４０体積％、好ましくは１０〜２５体積％の範囲で含有する消石灰を用いることを提案している。しかし、この固化材でも、環境温度が３５℃程度ではスラリーの流動性が低下し、その改善は十分ではない。 (2) Japanese Unexamined Patent Application Publication No. 2010-159347 (Patent Document 2) discloses a soil solidifying material containing a cement clinker, gypsum, and slaked lime, which is used as a slurry in which water is added to the soil solidifying material. It is proposed to adjust the particle size of slaked lime in order to avoid deterioration of the fluidity of the slurry, and to use slaked lime containing particles having a particle size of 30 μm or more in the range of 5 to 40% by volume, preferably 10 to 25% by volume. is doing. However, even with this solidified material, the fluidity of the slurry decreases at an environmental temperature of about 35° C., and the improvement is not sufficient.

特開２００４−２３１４７９号公報JP, 2004-231479, A 特開２０１０−１５９３４７号公報JP, 2010-159347, A

本発明は、従来のセメント系固化材は、高温環境下におけるスラリーの流動性低下の防止対策が不十分であると云う課題を解決したものであり、高温環境下でも流動性の低下が少ないセメント系固化材を提供する。 The present invention is a conventional cement-based solidifying material, which solves the problem that the preventive measures against the deterioration of the fluidity of the slurry in a high temperature environment are insufficient, and the cement has a low fluidity deterioration even in a high temperature environment. Provide a system solidifying material.

本発明は以下の構成を有するセメント系固化材に関する。
〔１〕ポルトランドセメントと石膏を含む固化材において、亜鉛および鉛を含有し、亜鉛および鉛の合計含有量が５００mg/kg以上〜１０００mg/kgg以下であることを特徴とするセメント系固化材。
〔２〕２０μｍ篩下の粒子を５０質量％以上〜１００質量％以下含有し、該粒子の亜鉛含有量が６００mg/kg以上であって鉛含有量が１００mg/kg以上である上記[１]に記載するセメント系固化材。
〔３〕高炉スラグ、石灰石、またはフライアッシュの少なくとも１種類以上を含有し、その合計含有量が５０質量％以下である上記[１]または上記[２]に記載するセメント系固化材。
〔４〕粉体材料のブレーン値が３０００cm２/g以上〜４５００cm２/g以下である上記[１]〜上記[３]の何れかに記載するセメント系固化材。
〔５〕ポルトランドセメントおよび石膏を含む粉体原料に、高炉スラグ、石灰石、またはフライアッシュの少なくとも１種からなる混和材料を配合してセメント系固化材を製造する方法において、上記粉体原料ないし上記混和材料が亜鉛および鉛を含有するものを用い、固化材中の亜鉛および鉛の合計含有量が５００mg/kg以上になるように、上記粉体原料および上記混和材料を配合するセメント系固化材の製造方法。 The present invention relates to a cement-based solidifying material having the following constitution.
[1] A solidification material containing portland cement and gypsum, containing zinc and lead, and having a total content of zinc and lead of 500 mg/kg to 1000 mg/kgg.
[2] In the above [1], which contains particles under 20 μm sieve in an amount of 50% by mass to 100% by mass, the zinc content of the particles is 600 mg/kg or more, and the lead content is 100 mg/kg or more. Cement-based solidifying material to be described.
[3] The cementitious solidifying material according to the above [1] or [2], which contains at least one or more of blast furnace slag, limestone, and fly ash, and the total content thereof is 50% by mass or less.
[4] cement solidifying material according to any one of the Blaine value of the powder material is less than 3000 cm 2 / g or more ~4500cm 2 / g [1] to [3] above.
[5] A method for producing a cementitious solidifying material by mixing a powder material containing Portland cement and gypsum with an admixture material of at least one of blast furnace slag, limestone, and fly ash, wherein The cement-based solidifying material containing the powder material and the admixture is used such that the admixture contains zinc and lead so that the total content of zinc and lead in the solidifying material is 500 mg/kg or more. Production method.

本発明のセメント系固化材は、亜鉛および鉛をその合計含有量５００mg/kg以上〜１０００mg/kg以下を含有することによって、環境温度が３５℃程度になっても、固化材スラリーの流動性の低下を効果的に抑制することができる。さらに、本発明のセメント系固化材は、亜鉛および鉛の合計含有量を５００mg/kg以上含有すると共に、好ましくは、２０μｍ篩下の粒子を５０質量％以上〜１００質量％以下含有し、該粒子の亜鉛含有量が６００mg/kg以上であって鉛含有量が１００mg/kg以上であることによって、上記高温環境下において固化材スラリーの流動性の低下をさらに効果的に抑制することができる。 The cement-based solidifying material of the present invention contains zinc and lead in a total content of 500 mg/kg or more and 1000 mg/kg or less, so that the fluidity of the solidifying material slurry can be improved even when the environmental temperature reaches about 35°C. The decrease can be effectively suppressed. Furthermore, the cementitious solidifying material of the present invention contains a total content of zinc and lead of 500 mg/kg or more, and preferably contains particles of 20 μm sieve down of 50% by mass to 100% by mass. When the zinc content is 600 mg/kg or more and the lead content is 100 mg/kg or more, it is possible to more effectively suppress the decrease in the fluidity of the solidifying material slurry under the high temperature environment.

本発明のセメント系固化材は、上記亜鉛および鉛含有量と共に、高炉スラグ、石灰石、またはフライアッシュなどを所定量含有し、またブレーン値が所定範囲であることによって、上記高温環境下において固化材スラリーの流動性の低下を効果的に抑制することができる。 The cement-based solidifying material of the present invention, together with the zinc and lead contents, contains a predetermined amount of blast furnace slag, limestone, or fly ash, and the Blaine value is within a predetermined range, so that the solidifying material under the high temperature environment. It is possible to effectively suppress the decrease in the fluidity of the slurry.

〔具体的な説明〕
本発明のセメント系固化材は、ポルトランドセメントと石膏を含む固化材において、亜鉛および鉛を含有し、亜鉛および鉛の合計含有量が５００mg/kg以上〜１０００mg/kg以下であることを特徴とし、好ましくは、２０μｍ篩下の粒子を５０質量％以上〜１００質量％以下含有し、該粒子の亜鉛含有量が６００mg/kg以上であって鉛含有量が１００mg/kg以上であるセメント系固化材である。 [Specific explanation]
The cement-based solidifying material of the present invention is a solidifying material containing Portland cement and gypsum, containing zinc and lead, wherein the total content of zinc and lead is 500 mg/kg or more to 1000 mg/kg or less, Preferably, the cement-based solidifying material contains particles under 20 μm sieve in an amount of 50% by mass to 100% by mass, the zinc content of the particles is 600 mg/kg or more, and the lead content is 100 mg/kg or more. is there.

本発明のセメント系固化材は、ポルトランドセメントと石膏を含む。これらの含有量は内割りで、例えば、ポルトランドセメント７０〜９８質量％および石膏（無水石膏換算）２〜３０質量％が好ましい。さらにポルトランドセメント９０〜９５質量％、石膏（無水石膏換算）５〜１０質量％がより好ましい。 The cementitious solidifying material of the present invention contains Portland cement and gypsum. The content of these is an internal ratio, and for example, 70 to 98% by mass of Portland cement and 2 to 30% by mass of gypsum (calculated as anhydrous gypsum) are preferable. Further, 90 to 95 mass% of Portland cement and 5 to 10 mass% of gypsum (calculated as anhydrous gypsum) are more preferable.

ポルトランドセメントは、普通ポルトランドセメント、早強ポルトランドセメント、中庸熱ポルトランドセメント、または低熱ポルトランドセメント等を用いることができる。石膏は無水石膏、二水石膏、半水石膏の何れでも良く、２種以上でも良い。また石膏の産出元は天然無水石膏、排煙脱硫石膏、フッ酸石膏など何れでも良い。 As the Portland cement, normal Portland cement, early-strength Portland cement, moderate heat Portland cement, low heat Portland cement, or the like can be used. The gypsum may be any of anhydrous gypsum, gypsum dihydrate and gypsum hemihydrate, and may be two or more kinds. The source of gypsum may be natural anhydrous gypsum, flue gas desulfurization gypsum, hydrofluoric acid gypsum, or the like.

本発明のセメント系固化材は、ポルトランドセメントおよび石膏と共に高炉スラグ、石灰石、またはフライアッシュの少なくとも１種類以上の混和材料を含有することができる。これらの混和材料は、好ましくは、その合計量が固化材中に内割りで５０質量％以下含むことができる。混和材料の固化材中の含有量は５質量％以上〜５０質量％以下が好ましい。また、この混和材料は規格に適合するものが好ましい。例えば、フライアッシュはＪＩＳ規格（JIS A 6201：コンクリート用フライアッシュII種）に適合するものを用いると良い。 The cementitious solidifying material of the present invention can contain at least one admixture material of blast furnace slag, limestone, or fly ash together with Portland cement and gypsum. Preferably, the total amount of these admixtures is 50% by mass or less in the solidifying material. The content of the admixture in the solidifying material is preferably 5% by mass or more and 50% by mass or less. Further, it is preferable that the admixture material conforms to the standard. For example, it is preferable to use a fly ash that conforms to the JIS standard (JIS A 6201: Fly ash type II for concrete).

本発明のセメント系固化材において、ポルトランドセメント、石膏、および混和材料（高炉スラグ、石灰石、またはフライアッシュ）は粉体原料が用いられる。これらの粉体材料のブレーン値（ブレーン比表面積）は３０００cm２/g以上、４５００cm２/g以下であることが好ましい。ブレーン値が３０００cm２/ｇより小さいと、スラリーにしたときにブリーディング率が高くなる傾向があり、固液分離によって固化体強度のばらつきや強度不足を生じる原因になる。一方、粉体材料のブレーン値が４５００cm２/ｇより高いとスラリーの流動性がやや低下する傾向がある。なお、本発明のセメント系固化材は、これらの粉体原料に水を加え、例えば、水セメント比（Ｗ/Ｃ比）４０〜１００％のスラリーにして使用される。 In the cement-based solidifying material of the present invention, powder raw materials are used for Portland cement, gypsum, and an admixture (blast furnace slag, limestone, or fly ash). The Blaine value (Blaine specific surface area) of these powder materials is preferably 3000 cm 2 /g or more and 4500 cm 2 /g or less. When the Blaine value is less than 3000 cm 2 /g, the bleeding rate tends to be high when it is made into a slurry, which causes variation in strength of the solidified body and insufficient strength due to solid-liquid separation. On the other hand, if the Blaine value of the powder material is higher than 4500 cm 2 /g, the fluidity of the slurry tends to be slightly lowered. The cement-based solidifying material of the present invention is used by adding water to these powder raw materials to form a slurry having a water cement ratio (W/C ratio) of 40 to 100%.

本発明のセメント系固化材は亜鉛および鉛を含み、固化材全体の亜鉛および鉛の合計含有量が５００mg/kg以上〜１０００mg/kg以下である。好ましくは、本発明のセメント系固化材は２０μｍ篩下の粒子を５０質量％以上〜１００質量％以下含有し、この粒子の亜鉛含有量が６００mg/kg以上であって鉛含有量が１００mg/kg以上のものである。本発明のセメント系固化材は、亜鉛および鉛を合計５００mg/kg以上含むことよって、高温環境下でのスラリーの流動性の低下を防止する効果を有する。亜鉛および鉛の合計含有量が５００mg/kg未満ではスラリーの流動性を低下する効果が不十分になる。また、亜鉛および鉛の合計含有量が１０００ｍｇ/kgを超えると凝結遅延が生じるので好ましくない。 The cement-based solidifying material of the present invention contains zinc and lead, and the total content of zinc and lead in the entire solidifying material is 500 mg/kg to 1000 mg/kg. Preferably, the cementitious solidifying material of the present invention contains particles of 20 μm under sieve in an amount of 50% by mass or more and 100% by mass or less, and a zinc content of the particles is 600 mg/kg or more and a lead content is 100 mg/kg. That is all. Since the cement-based solidifying material of the present invention contains zinc and lead in a total amount of 500 mg/kg or more, it has an effect of preventing deterioration of the fluidity of the slurry under a high temperature environment. If the total content of zinc and lead is less than 500 mg/kg, the effect of lowering the fluidity of the slurry becomes insufficient. Further, if the total content of zinc and lead exceeds 1000 mg/kg, delay of setting occurs, which is not preferable.

本発明のセメント系固化材は、より好ましくは、例えば、固化材全体の亜鉛および鉛の合計含有量が５００mg/kg以上〜８５０mg/kg以下であって、２０μｍ篩下の粒子を５０質量％〜６５質量％を含み、この粒子の亜鉛含有量が６００mg/kg以上〜８００mg/kg以下であって鉛含有量が１００mg/kg以上〜２５０mg/kg以下のものである。なお、２０μｍ篩下の粒子は、原料粉体であるポルトランドセメント、石膏、および混和材料について、２０μｍ篩下の粒子が５０質量％以上〜１００質量％以下、好ましくは５０質量％〜６５質量％であればよい。 More preferably, the cement-based solidifying material of the present invention has, for example, a total content of zinc and lead in the solidifying material of 500 mg/kg or more to 850 mg/kg or less, and 50% by mass of particles under a 20 μm sieve. The content of zinc is 65% by mass, the zinc content of the particles is 600 mg/kg to 800 mg/kg and the lead content is 100 mg/kg to 250 mg/kg. The particles under the 20 μm sieve are 50% by mass or more and 100% by mass or less, preferably 50% by mass to 65% by mass, with respect to the raw material powders of Portland cement, gypsum, and admixtures. I wish I had it.

固化材が２０μｍ篩下の粒子を５０質量％以上〜１００質量％以下、好ましくは５０質量％〜６５質量％含むことによって、スラリー作製時に固化材と水の混合が容易になり、短時間で均一なスラリーを作製することができる。また、この粒子に所定量の亜鉛および鉛が含まれることによって、高温下でのスラリーの流動性の低下を効果的に抑制することができる。 Since the solidifying material contains particles of 20 μm sieve under 50% by mass to 100% by mass, preferably 50% by mass to 65% by mass, mixing of the solidifying material and water becomes easy at the time of slurry preparation, and uniform in a short time. It is possible to prepare a simple slurry. Further, by containing a predetermined amount of zinc and lead in these particles, it is possible to effectively suppress the decrease in the fluidity of the slurry at high temperatures.

なお、２０μｍ篩下の粒子に含まれる亜鉛および鉛の合計含有量だけでは固化材全体の亜鉛および鉛の合計含有量が５００mg/kgに満たないときは、固化材に含まれる２０μｍより大きい粒子の亜鉛および鉛の合計含有量を加えたときに、固化材全体の亜鉛および鉛の合計含有量が５００mg/kg以上であれば良い。 If the total content of zinc and lead contained in the particles under the 20 μm sieve is less than 500 mg/kg in the entire solidified material, the particles larger than 20 μm contained in the solidified material are not included. When the total content of zinc and lead is added, the total content of zinc and lead in the entire solidified material should be 500 mg/kg or more.

例えば、固化材が２０μｍ篩下の粒子を５０質量％含み、この粒子の亜鉛含有量が６００mg/kgあって鉛含有量が１００mg/kgであり、固化材全体の亜鉛および鉛の合計含有量が７００mg/kgであるとき、固化材全体では、２０μｍ篩下の粒子によって、亜鉛および鉛の合計含有量７００mg/kgの５０％分の３５０mg/kgが含まれることになるが、５００mg/kgには満たない。しかし、固化材に含まれる２０μｍより大きい粒子の亜鉛および鉛の合計含有量が１５０mg/kg以上であれば、本発明のセメント系固化材として用いることができる。 For example, the solidifying material contains 50% by mass of particles under the 20 μm sieve, the zinc content of the particles is 600 mg/kg and the lead content is 100 mg/kg, and the total content of zinc and lead in the whole solidifying material is When it is 700 mg/kg, the solidified material as a whole contains 350 mg/kg which is 50% of the total content of zinc and lead of 700 mg/kg due to the particles under the 20 μm sieve. Less than. However, if the total content of zinc and lead of particles larger than 20 μm contained in the solidifying material is 150 mg/kg or more, it can be used as the cementitious solidifying material of the present invention.

本発明のセメント系固化材に含まれる亜鉛および鉛は、該セメント系固化材の原料になるポルトランドセメントクリンカー、石灰石、フライアッシュ、石膏に通常含まれている。また、亜鉛および鉛成分を多く含有する鉱物質物質を加えてもよい。亜鉛および鉛成分を多く含有する鉱物質物質としては、例えば、セメント製造工程において発生する塩素バイパスダスト、サイクロンシュート原料、電気集塵機ダスト、バッグフィルターダストなどの２０μｍ篩下の粒子が２０質量％以上〜１００質量％以下のものを用いることができる。なお、亜鉛および鉛成分を多く含有する鉱物質物質これらの物質に限定されない。セメント系固化材組成物中の亜鉛および鉛の合計量が５００mg/kg以上〜１０００mg/kg以下になるように、好ましくは２０μｍ篩下の粒子の亜鉛含有量が６００mg/kg以上であって鉛含有量が１００mg/kg以上になるように、上記原料を選択して配合量を調整すればよい。なお、亜鉛および鉛成分を多く含有する鉱物質物質を補助原料として加える場合には、セメント系固化材に対して内割りで０.１０質量％以上〜１０質量％以下が好ましい。 Zinc and lead contained in the cement-based solidifying material of the present invention are usually contained in Portland cement clinker, limestone, fly ash, and gypsum, which are raw materials for the cement-based solidifying material. Further, a mineral substance containing a large amount of zinc and lead components may be added. Examples of the mineral substances containing a large amount of zinc and lead components include, for example, 20% by mass or more of particles under a 20 μm sieve such as chlorine bypass dust, cyclone chute raw material, electrostatic precipitator dust, and bag filter dust generated in a cement manufacturing process. It is possible to use one having a content of 100% by mass or less. Mineral substances containing a large amount of zinc and lead components are not limited to these substances. In order for the total amount of zinc and lead in the cement-based solidifying material composition to be 500 mg/kg or more to 1000 mg/kg or less, it is preferable that the particles under the 20 μm sieve have a zinc content of 600 mg/kg or more and contain lead. The above raw materials may be selected and the compounding amount adjusted so that the amount becomes 100 mg/kg or more. When a mineral substance containing a large amount of zinc and lead components is added as an auxiliary raw material, the content is preferably 0.10% by mass or more and 10% by mass or less based on the cement solidification material.

〔製造方法〕
本発明のセメント系固化材は、ポルトランドセメントおよび石膏を含む粉体原料に、高炉スラグ、石灰石、またはフライアッシュの少なくとも１種からなる混和材料を配合してセメント系固化材を製造する方法において、上記粉体原料ないし上記混和材料として亜鉛および鉛を含有するものを用い、固化材中の亜鉛および鉛の合計含有量が５００mg/kg以上になるように、上記粉体原料および上記混和材料を配合して製造することができる。 〔Production method〕
The cement-based solidifying material of the present invention is a method for producing a cement-based solidifying material by blending a powdered raw material containing Portland cement and gypsum with an admixture made of at least one of blast furnace slag, limestone, or fly ash, The powder raw material or the admixture containing zinc and lead is used, and the powder raw material and the admixture are blended so that the total content of zinc and lead in the solidifying material is 500 mg/kg or more. Can be manufactured.

上記粉体原料および上記混和材料は、２０μｍ篩下の粒子を５０質量％以上〜１００質量％以下含有するものが好ましく、これらの粒子に亜鉛が６００mg/kg以上および鉛が１００mg/kg以上含まれるものを用いるのが好ましい。また、上記混和材料は固化材中の内割で５０質量％以下になる量を配合するのが良く、５質量％以上〜５０質量％以下がより好ましい。さらに、上記粉体原料および上記混和材料は、ブレーン値が３０００cm２/g以上〜４５００cm２/g以下の粉体を用いるのが好ましい。 It is preferable that the powder raw material and the admixture contain 50% by mass or more and 100% by mass or less of particles under a 20 μm sieve, and these particles contain 600 mg/kg or more of zinc and 100 mg/kg or more of lead. It is preferable to use one. Further, it is preferable to mix the above-mentioned admixture material in an amount of 50% by mass or less in terms of the content in the solidifying material, and more preferably 5% by mass or more and 50% by mass or less. Furthermore, the powder material and the admixture is Blaine is preferable to use a 3000 cm 2 / g or more ~4500cm 2 / g or less powder.

本発明のセメント系固化材は、亜鉛および鉛をその合計含有量５００mg/kg以上〜１０００mg/kg以下を含有することによって、環境温度が３５℃程度になっても、固化材スラリーの流動性の低下を効果的に抑制することができる。さらに、本発明のセメント系固化材は、亜鉛および鉛の合計含有量を５００mg/kg以上〜１０００mg/kg以下含有すると共に、好ましくは、２０μｍ篩下の粒子を５０質量％以上、１００質量％以下含有し、該粒子の亜鉛含有量が６００mg/kg以上であって鉛含有量が１００mg/kg以上であることによって、上記高温環境下において固化材スラリーの流動性の低下をさらに効果的に抑制することができる。 The cement-based solidifying material of the present invention contains zinc and lead in a total content of 500 mg/kg or more to 1000 mg/kg or less, so that the fluidity of the solidifying material slurry can be improved even when the environmental temperature reaches about 35°C. The decrease can be effectively suppressed. Further, the cementitious solidifying material of the present invention contains a total content of zinc and lead of 500 mg/kg or more to 1000 mg/kg or less, and preferably 50% by mass or more and 100% by mass or less of particles under a 20 μm sieve. By containing the zinc content of the particles is 600 mg/kg or more and the lead content is 100 mg/kg or more, it is possible to more effectively suppress the deterioration of the fluidity of the solidifying material slurry under the high temperature environment. be able to.

さらに、本発明のセメント系固化材は、高炉スラグ、石灰石、またはフライアッシュの少なくとも１種類以上からなる混和材料を、その合計量が５０質量％以下、好ましくは５質量％以上〜５０質量％以下（固化材中の内割）含有することによって、上記高温環境下において固化材スラリーの流動性の低下をさらに効果的に抑制することができる。また、本発明のセメント系固化材は、材料のブレーン値が３０００cm２/g以上〜４５００cm２/g以下であることによって、上記高温環境下において固化材スラリーの流動性の低下をさらに効果的に抑制することができるとともに、ブリーディングを抑制することができる。 Furthermore, the cementitious solidifying material of the present invention is a mixed material composed of at least one kind of blast furnace slag, limestone, or fly ash in a total amount of 50 mass% or less, preferably 5 mass% or more and 50 mass% or less. By including (inner ratio in the solidifying material), it is possible to more effectively suppress the decrease in the fluidity of the solidifying material slurry under the high temperature environment. Further, cement-based solidifying material of the present invention, by Blaine value of the material is less than 3000 cm 2 / g or more ~4500cm 2 / g, more effectively the decrease in the fluidity of the solidifying material slurry under the high temperature environment Not only can it be suppressed, but also bleeding can be suppressed.

以下、本発明の実施例を比較試料と共に示す。流動性評価試験およびブリーディング率試験は以下の方法によって行った。
（１）流動性評価試験
固化材について、３５℃環境下において、水セメント比(Ｗ/Ｃ)６０％のスラリーを作製し、土木学会規準JSCE-F-521「プレパックドコンクリートの注入モルタルの流動性試験方法（P漏斗による方法）」に規定されるプレパクトフローコーン(Ｐロート)を使用して、流下時間を測定する。流下時間は３０分毎に測定した。流下時間が１３.０秒以上になるときの練上がりからの経過時間を測定した。この経過時間が長いほど流動性が良い。
（２）ブリーディング率試験
固化材について、３５℃環境下において、水セメント比(Ｗ/Ｃ)６０％のスラリーを作製し、土木学会規準JSCE-F 522「プレパックドコンクリートの注入モルタルのブリーディング率および膨張率試験方法（ポリエチレン袋方法）（案）」に従って、練上がりから３時間経過後のブリーディング率を測定した。ブリーディング率は５％以下が好ましい。 Hereinafter, examples of the present invention will be shown together with comparative samples. The fluidity evaluation test and the bleeding rate test were performed by the following methods.
(1) Fluidity evaluation test Regarding the solidified material, a slurry with a water-cement ratio (W/C) of 60% was prepared in a 35° C. environment, and the JSCE-F-521 “JSCE-F-521” flow of injected mortar of prepacked concrete The run-down time is measured using a prepact flow cone (P funnel) specified in "Sex test method (method using P funnel)". The flow-down time was measured every 30 minutes. The elapsed time from the kneading when the flow-down time was 13.0 seconds or more was measured. The longer this elapsed time, the better the fluidity.
(2) Bleeding rate test Regarding the solidified material, a slurry having a water cement ratio (W/C) of 60% was prepared in an environment of 35° C. The bleeding rate after 3 hours from kneading was measured according to the “Expansion test method (polyethylene bag method) (draft)”. The bleeding rate is preferably 5% or less.

〔実施例〕
ポルトランドセメント９２.０質量％、石膏８.０質量％を含む固化材の粉体原料に、高炉スラグ、石灰石、またはフライアッシュの少なくとも１種類以上からなる混和材料を配合して、亜鉛と鉛の合計含有量が５００mg/kg以上のセメント系固化材を調製した。混和材料の配合量は固化材全体の５質量％〜５０質量％になる量である（試料Ａ１〜Ａ２８、試料Ａ３０〜Ａ３２）。また、混和材料を配合しない試料Ａ２９を調製した。
この固化材に水を加えて水セメント比(Ｗ/Ｃ)６０％のスラリーを作製した。このスラリーについて、流動性評価試験およびブリーディング率試験を行った。この結果を表１に示した。表１の試料Ａ１〜Ａ３２は本発明の試料であり、試料Ａ１〜Ａ１０は本発明の好ましい範囲の試料である。 〔Example〕
A powder material of a solidifying material containing 92.0% by mass of Portland cement and 8.0% by mass of gypsum was mixed with an admixture material of at least one kind of blast furnace slag, limestone, or fly ash to mix zinc and lead. A cement-based solidifying material having a total content of 500 mg/kg or more was prepared. The compounding amount of the admixture material is an amount of 5% by mass to 50% by mass of the entire solidifying material (Samples A1 to A28, Samples A30 to A32). Further, a sample A29 containing no admixture was prepared.
Water was added to this solidified material to prepare a slurry having a water-cement ratio (W/C) of 60%. The slurry was subjected to a fluidity evaluation test and a bleeding rate test. The results are shown in Table 1. Samples A1 to A32 in Table 1 are samples of the present invention, and samples A1 to A10 are samples in the preferred range of the present invention.

〔比較例〕
亜鉛と鉛の合計含有量が５００mg/kg未満である以外は実施例と同様のセメント系固化材を調製した。この固化材に水を加えて水セメント比(Ｗ/Ｃ)６０％のスラリーを作製した。このスラリーについて、流動性評価試験およびブリーディング率試験を行った。この結果を表１に示した。試料Ｂ１〜Ｂ２が本発明から外れる比較試料である。 (Comparative example)
A cement-based solidifying material similar to that of the example was prepared except that the total content of zinc and lead was less than 500 mg/kg. Water was added to this solidifying material to prepare a slurry having a water-cement ratio (W/C) of 60%. The slurry was subjected to a fluidity evaluation test and a bleeding rate test. The results are shown in Table 1. Samples B1 and B2 are comparative samples that depart from the invention.

表１に示すように、固化材中の亜鉛と鉛の合計含有量が５００mg/kg未満の試料Ｂ１、試料Ｂ２は何れも経過時間（Ｐロートからスラリーが流下する時間が１３.０秒以上になった際の練り込みからの経過時間）が９０分であって格段に短く、流動性の経過時間に伴う低下が著しい。一方、固化材中の亜鉛と鉛の合計含有量が５００mg/kg以上〜１０００mg/kg以下の試料Ａ１〜Ａ３２は該経過時間が何れも１１０分以上であり、スラリーの流動性の低下が抑制されている。このなかで試料Ａ１１、Ａ１２は２０μｍ篩下の粒子の含有量が少ないので、経過時間は１２０分、１１５分であるが、比較試料Ｂ１，Ｂ２より経過時間が長く、スラリーの流動性低下の抑制効果がみられる。 As shown in Table 1, both the sample B1 and the sample B2 in which the total content of zinc and lead in the solidifying material is less than 500 mg/kg, the elapsed time (the time for which the slurry flows down from the P funnel is 13.0 seconds or more). The time elapsed since kneading) was 90 minutes, which was remarkably short, and the decrease in fluidity with the elapsed time was remarkable. On the other hand, in Samples A1 to A32 in which the total content of zinc and lead in the solidified material is 500 mg/kg or more to 1000 mg/kg or less, the elapsed time is 110 minutes or more, and the deterioration of the fluidity of the slurry is suppressed. ing. Among them, Samples A11 and A12 had a small content of particles under the 20 μm sieve, and thus the elapsed time was 120 minutes and 115 minutes, but the elapsed time was longer than Comparative Samples B1 and B2, and the deterioration of the fluidity of the slurry was suppressed. The effect can be seen.

一方、試料Ａ１〜Ａ２９のうち、固化材中の亜鉛と鉛の合計含有量が５００mg/kg以上〜１０００mg/kg以下であって、２０μｍ篩下の粒子を５０質量％以上〜１００質量％以下含有し、該粒子の亜鉛含有量が６００mg/kg以上であって鉛含有量が１００mg/kg以上である試料Ａ１〜Ａ１０は、何れも上記経過時間が１８０分であって、試料Ｂ１、試料Ｂ２の２倍程度長く、スラリーの流動性の低下が格段に抑制されている。このように本発明の固化材は、固化材中の亜鉛と鉛の合計含有量が５００mg/kg以上〜１０００mg/kg以下であって、２０μｍ篩下の粒子を５０質量％以上〜１００質量％以下含有し、該粒子の亜鉛含有量が６００mg/kg以上であって鉛含有量が１００mg/kg以上であるものが最も好ましい。 On the other hand, in Samples A1 to A29, the total content of zinc and lead in the solidifying material is 500 mg/kg or more to 1000 mg/kg or less, and the particles under the 20 μm sieve contain 50% by mass to 100% by mass. However, all of the samples A1 to A10 in which the zinc content of the particles is 600 mg/kg or more and the lead content is 100 mg/kg or more, the elapsed time is 180 minutes, and the samples B1 and B2 are It is about twice as long and the deterioration of the fluidity of the slurry is significantly suppressed. As described above, the solidified material of the present invention has a total content of zinc and lead in the solidified material of 500 mg/kg or more to 1000 mg/kg or less, and particles of 20 μm sieve are 50% by mass or more to 100% by mass or less. Most preferably, the particles have a zinc content of 600 mg/kg or more and a lead content of 100 mg/kg or more.

なお、試料Ａ１３〜Ａ１８は固化材中の亜鉛と鉛の合計含有量が５００mg/kg以上、１０００mg/kg以下であるが、固化材に含まれる２０μｍ篩下の粒子の亜鉛含有量が６００mg/kg未満あるいは鉛含有量が１００mg/kg未満の試料であり、これらの上記経過時間は１１５分であって、試料Ａ１〜Ａ１０よりは短いが、試料Ｂ１、試料Ｂ２よりは格段に長く、スラリー流動性の低下が十分に抑制されている。 Samples A13 to A18 have a total content of zinc and lead in the solidifying material of 500 mg/kg or more and 1000 mg/kg or less, but the zinc content of the particles below the 20 μm sieve contained in the solidifying material is 600 mg/kg. Less than or less than 100 mg/kg of lead content, the above elapsed time is 115 minutes, which is shorter than Samples A1 to A10 but much longer than Samples B1 and B2, and has a slurry fluidity. Is sufficiently suppressed.

また、試料Ａ１９〜Ａ２１および試料Ａ２２〜Ａ２３は、固化材に含まれる２０μｍ篩下の粒子の割合が５０質量％未満であり、あるいは高炉スラグ等の含有量が５０質量％未満であるが、固化材中の亜鉛と鉛の合計含有量が５００mg/kg以上〜１０００mg/kg以下であるので、上記経過時間は１１５分であり、試料Ａ１〜Ａ１０よりは短いが、試料Ｂ１、試料Ｂ２よりは格段に長く、スラリー流動性の低下が十分に抑制されている。 Further, in Samples A19 to A21 and Samples A22 to A23, the proportion of particles under the 20 μm sieve contained in the solidifying material is less than 50% by mass, or the content of the blast furnace slag and the like is less than 50% by mass, but the solidification occurs. Since the total content of zinc and lead in the material is 500 mg/kg or more to 1000 mg/kg or less, the above-mentioned elapsed time is 115 minutes, which is shorter than Samples A1 to A10, but much more than Samples B1 and B2. It is very long, and the decrease in slurry fluidity is sufficiently suppressed.

粉体材料のブレーン値が４５００cm２/ｇを超える試料Ａ２４〜Ａ２５は、上記経過時間は１２０分であり、スラリーの流動性の低下は抑制されているが、試料Ａ１〜Ａ１０よりは該経過時間がやや短いので、粉体材料のブレーン値は４５００cm２/ｇ以下が好ましい。また、試料Ａ２６〜Ａ２７は、粉体材料のブレーン値が３０００cm２/ｇ未満であるため、ブリーディング率が５.０％を上回り材料分離が生じやすくなる。材料分離が生じ難い固化材を得るには、粉体材料のブレーン値は３０００cm２/ｇ以上が好ましい。
混和材（高炉スラグ、石灰石、フライアッシュ）を含有しない試料Ａ２９、および混和材の含有量が５質量％のＡ３０〜Ａ３２は、混和材の含有量が少ないものの固化材中の亜鉛と鉛の含有量が多いので、上記経過時間が１１５分であり、試料Ｂ１、試料Ｂ２よりは長く、スラリー流動性の低下が十分に抑制されている。 Samples A24 to A25 in which the Blaine value of the powder material exceeds 4500 cm 2 /g have the above-mentioned elapsed time of 120 minutes, and the deterioration of the fluidity of the slurry is suppressed, but the elapsed time is more than that of Samples A1 to A10. However, the Blaine value of the powder material is preferably 4500 cm 2 /g or less. Further, in the samples A26 to A27, since the Blaine value of the powder material is less than 3000 cm 2 /g, the bleeding rate exceeds 5.0% and the material separation easily occurs. The Blaine value of the powder material is preferably 3000 cm 2 /g or more in order to obtain a solidified material in which material separation hardly occurs.
Sample A29 containing no admixture (blast furnace slag, limestone, fly ash), and A30 to A32 having an admixture content of 5% by mass contained zinc and lead in the solidified material although the admixture content was small. Since the amount is large, the elapsed time is 115 minutes, which is longer than in Samples B1 and B2, and the decrease in slurry fluidity is sufficiently suppressed.

Figure 2020083712
Figure 2020083712

Claims (5)

ポルトランドセメントと石膏を含む固化材において、亜鉛および鉛を含有し、亜鉛および鉛の合計含有量が５００mg/kg以上〜１０００mg/kg以下であることを特徴とするセメント系固化材。 A solidifying material containing portland cement and gypsum, containing zinc and lead, and having a total content of zinc and lead of 500 mg/kg to 1000 mg/kg. ２０μｍ篩下の粒子を５０質量％以上〜１００質量％以下で含み、該粒子の亜鉛含有量が６００mg/kg以上であって鉛含有量が１００mg/kg以上である請求項１に記載するセメント系固化材。 The cement system according to claim 1, which comprises particles of 20 μm sieve under 50% by mass to 100% by mass, the zinc content of the particles is 600 mg/kg or more, and the lead content is 100 mg/kg or more. Solidifying material. 高炉スラグ、石灰石、またはフライアッシュの少なくとも１種類以上を含有し、その合計含有量が５０質量％以下である請求項１または請求項２に記載するセメント系固化材。 The cement-based solidifying material according to claim 1 or 2, containing at least one kind of blast furnace slag, limestone, and fly ash, and the total content thereof is 50% by mass or less. 粉体材料のブレーン値が３０００cm２/g以上、４５００cm２/g以下である請求項１〜請求項３の何れかに記載するセメント系固化材。 The cement-based solidifying material according to claim 1, wherein the powder material has a Blaine value of 3000 cm 2 /g or more and 4500 cm 2 /g or less. ポルトランドセメントおよび石膏を含む粉体原料に、高炉スラグ、石灰石、またはフライアッシュの少なくとも１種からなる混和材料を配合してセメント系固化材を製造する方法において、上記粉体原料ないし上記混和材料が亜鉛および鉛を含有するものを用い、固化材中の亜鉛および鉛の合計含有量が５００mg/kg以上〜１０００mg/kg以下になるように、上記粉体原料および上記混和材料を配合するセメント系固化材の製造方法。

In a method for producing a cementitious solidifying material by mixing an admixture material comprising at least one of blast furnace slag, limestone, and fly ash to a powder raw material containing Portland cement and gypsum, the powder raw material or the admixture material is Cement-based solidification using the powder raw material and the admixture material such that the total content of zinc and lead in the solidifying material is 500 mg/kg to 1000 mg/kg using a material containing zinc and lead. Method of manufacturing wood.

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JP2004041942A (en) * 2002-07-12 2004-02-12 Earth Create Office Co Ltd Cement-based solidifying agent and solidification method using the same
JP2010159347A (en) * 2009-01-08 2010-07-22 Tokuyama Corp Soil-solidifying material
WO2014092101A1 (en) * 2012-12-11 2014-06-19 太平洋セメント株式会社 Method for producing cement-based solidified material and cement-based solidified material
JP2017014350A (en) * 2015-06-30 2017-01-19 宇部興産株式会社 Soil improver and soil improvement method

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JP2004041942A (en) * 2002-07-12 2004-02-12 Earth Create Office Co Ltd Cement-based solidifying agent and solidification method using the same
JP2010159347A (en) * 2009-01-08 2010-07-22 Tokuyama Corp Soil-solidifying material
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