JP2011133344A - Evaluation method of expression property of strength of coal ash and improvement method of expression property of strength - Google Patents
Evaluation method of expression property of strength of coal ash and improvement method of expression property of strength Download PDFInfo
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本発明は、セメント、モルタル、コンクリート用の混和材として用いられる石炭灰の強度発現性の評価方法及び強度発現性の改善方法に関する。 The present invention relates to a method for evaluating the strength development of coal ash used as an admixture for cement, mortar and concrete, and a method for improving the strength development.
火力発電所の微粉炭燃焼ボイラからの副産物として大量に産出される石炭灰は、セメント、モルタルまたはコンクリート（以下、これらを総称して「コンクリート」という場合がある。）用の混和材として一部有効利用されているものの、大部分が埋立て等により廃棄処分されている。石炭灰のうち、コンクリート用混和材として用いられるフライアッシュは、その粒子が平滑かつ球状であるためにコンクリートのワーカビリティーを向上させ、コンクリート組織を緻密化させ、コンクリートの長期強度を増大させるとともに、化学薬品に対する抵抗性等を向上させ、その混入によりセメントの水和発熱が緩和されるために白己発熱による温度ひび割れが問題となるマスコンクリート構造物に適しており、アルカリ骨材反応に対する抑制効果を有している等、コンクリート用混和材として優れた特性を多く有している（非特許文献１）。 Coal ash produced in large quantities as a by-product from pulverized coal fired boilers at thermal power plants is partially used as an admixture for cement, mortar, or concrete (hereinafter sometimes collectively referred to as “concrete”). Although it is used effectively, most of it is disposed of by landfill. Among the coal ash, fly ash used as a concrete admixture improves the workability of concrete because its particles are smooth and spherical, densifies the concrete structure, increases the long-term strength of concrete, It is suitable for mass concrete structures where temperature cracking due to white heat generation is a problem because the hydration heat generation of cement is mitigated by improving the resistance to chemicals, etc., and the effect of suppressing alkali-aggregate reaction. It has many excellent properties as a concrete admixture (Non-patent Document 1).
一方、フライアッシュをコンクリートに多量に混合すると、凝結の遅延、初期強度の低下、低温環境下における強度発現の遅れ等の問題が生じ得るため、おのずとその混合量に制限がかけられてしまう。例えば、ＪＩＳ−Ｒ５２１３に規定されているフライアッシュセメントは、セメントに対するフライアッシュの置換割合を最大で３割に制限しており、フライアッシュの大量使用に結びついていないのが現状である。 On the other hand, when a large amount of fly ash is mixed with concrete, problems such as a delay in setting, a decrease in initial strength, a delay in the development of strength in a low-temperature environment, and the like may occur, so that the mixing amount is naturally limited. For example, the fly ash cement defined in JIS-R5213 restricts the replacement ratio of fly ash to cement to 30% at the maximum, and is currently not connected to large-scale use of fly ash.
また、石炭灰の大量使用を妨げる原因の一つとして、火力発電所で使用される石炭が多種に及び、しかもその燃焼条件が同一でないために、得られる石炭灰のポゾラン活性が大きく変わってしまい、その結果、石炭灰を使用したコンクリートの強度発現性も異なってしまうという問題がある。 In addition, as one of the causes that hinder the use of large quantities of coal ash, there are many types of coal used in thermal power plants, and because the combustion conditions are not the same, the pozzolanic activity of the resulting coal ash greatly changes. As a result, there is a problem that the strength development of the concrete using coal ash is also different.
フライアッシュのポゾラン活性を評価する方法としては、ＪＩＳ−Ａ６２０１に規定されるコンクリート用フライアッシュの活性度指数を算出し、当該活性度指数により評価する方法が知られている。この方法は、所定の配合割合でフライアッシュを含む試験モルタル供試体とフライアッシュを含まない基準モルタル供試体とを調製し、両モルタル供試体の圧縮強度を測定し、かかる圧縮強度の比に基づいてフライアッシュの活性度を算出する方法である。 As a method for evaluating the pozzolanic activity of fly ash, a method is known in which the activity index of fly ash for concrete specified in JIS-A6201 is calculated and evaluated based on the activity index. This method prepares a test mortar specimen containing fly ash and a reference mortar specimen not containing fly ash at a predetermined blending ratio, measures the compressive strength of both mortar specimens, and based on the ratio of the compressive strength. This is a method for calculating the activity of fly ash.
前述のＪＩＳ−Ａ６２０１に規定されるコンクリート用フライアッシュの活性度指数を算出する方法は、２８日材齢及び９１日材齢の各時点におけるモルタル供試体の圧縮強度を測定する必要があるため、コンクリート用フライアッシュの評価に３ヶ月程度もの長い期間を要するという問題がある。 Since the method for calculating the activity index of concrete fly ash specified in the above-mentioned JIS-A6201 needs to measure the compressive strength of the mortar specimen at each time point of 28-day age and 91-day age, There is a problem that it takes a long period of about 3 months to evaluate concrete fly ash.
このような課題に鑑みて、本発明は、石炭灰の強度発現性を迅速に評価することができる石炭灰の強度発現性の評価方法を提供することを目的とする。
また、本発明は、石炭灰の強度発現性を簡易にかつ確実に改善することができる石炭灰の強度発現性の改善方法を提供することを目的とする。
In view of such a problem, an object of the present invention is to provide a method for evaluating the strength development of coal ash capable of quickly evaluating the strength development of coal ash.
Another object of the present invention is to provide a method for improving the strength development of coal ash that can easily and reliably improve the strength development of coal ash.
本発明者らは、上記課題を解決するために鋭意検討した結果、石炭灰の物性値として、ホウ素溶出量、フリーライム量、ガラス化率、ガラス相の塩基度、及び４５μｍ篩残分量を測定し、これらの測定値と特定の３つの式を用いることによって、材齢３日、７日、２８日の各時点における圧縮強度を推定することができることなどを見出し、本発明を完成した。
すなわち、本発明は、以下の［１］〜［２］を提供するものである。
As a result of intensive studies to solve the above problems, the present inventors have measured the boron elution amount, the amount of free lime, the vitrification rate, the basicity of the glass phase, and the 45 μm sieve residue as physical properties of coal ash. Then, by using these measured values and specific three formulas, it was found that the compressive strength at each time point of 3 days, 7 days and 28 days of age could be estimated, and the present invention was completed.
That is, the present invention provides the following [1] to [2].
［１］ 石炭灰の物性値として、ホウ素溶出量、フリーライム量、ガラス化率、ガラス相の塩基度、及び４５μｍ篩残分量を測定し、下記式（１）〜（３）を用いて、材齢３日、７日、２８日の各時点における石炭灰含有モルタルの圧縮強度の推定値である圧縮強度１〜３を算出し、該圧縮強度１〜３の算出値を用いて、石炭灰の強度発現性を評価することを特徴とする石炭灰の強度発現性の評価方法。
圧縮強度１（材齢３日；単位：Ｎ／ｍｍ２）＝９．３−０．０２８×ホウ素溶出量（ｍｇ／Ｌ）＋１．２×フリーライム量（質量％）＋１．２×ガラス相の塩基度・・・（１）
圧縮強度２（材齢７日；単位：Ｎ／ｍｍ２）＝１３．６−０．０１２×４５μｍ篩残分量（質量％）＋０．３６３×フリーライム量（質量％）＋４．６７×ガラス相の塩基度・・・（２）
圧縮強度３（材齢２８日；単位：Ｎ／ｍｍ２）＝３１．５−０．０５４×４５μｍ篩残分量（質量％）＋０．０６×ガラス相の塩基度×ガラス化率・・・（３）
［２］ 石炭灰の物性値として、ホウ素溶出量、フリーライム量、ガラス化率、ガラス相の塩基度、及び４５μｍ篩残分量を測定し、下記式（１）〜（３）を用いて、材齢３日、７日、２８日の各時点における石炭灰含有モルタルの圧縮強度の推定値である圧縮強度１〜３を算出し、該圧縮強度１〜３のいずれか１つ以上の算出値が、圧縮強度１〜３の各々について予め定めた基準値よりも小さい場合、前記圧縮強度１〜３の算出値のすべてが、前記予め定めた基準値以上となるように、フリーライム量の増大のための処理、及び／又は、４５μｍ篩残分量の減少のための処理を行なうことを特徴とする石炭灰の強度発現性の改善方法。
圧縮強度１（材齢３日；単位：Ｎ／ｍｍ２）＝９．３−０．０２８×ホウ素溶出量（ｍｇ／Ｌ）＋１．２×フリーライム量（質量％）＋１．２×ガラス相の塩基度・・・（１）
圧縮強度２（材齢７日；単位：Ｎ／ｍｍ２）＝１３．６−０．０１２×４５μｍ篩残分量（質量％）＋０．３６３×フリーライム量（質量％）＋４．６７×ガラス相の塩基度・・・（２）
圧縮強度３（材齢２８日；単位：Ｎ／ｍｍ２）＝３１．５−０．０５４×４５μｍ篩残分量（質量％）＋０．０６×ガラス相の塩基度×ガラス化率・・・（３）
[1] As physical properties of coal ash, boron elution amount, free lime amount, vitrification rate, basicity of glass phase, and 45 μm sieve residue amount are measured, and using the following formulas (1) to (3), Compressive strength 1 to 3, which is an estimated value of the compressive strength of the coal ash-containing mortar at each time point of 3 days, 7 days and 28 days of age, is calculated. Strength evaluation property of coal ash characterized by evaluating strength development property of coal ash.
Compressive strength 1 (material age 3 days; unit: N / mm 2 ) = 9.3-0.028 × boron elution amount (mg / L) + 1.2 × free lime amount (mass%) + 1.2 × glass phase Basicity of (1)
Compressive strength 2 (age 7 days; unit: N / mm 2 ) = 13.6-0.012 × 45 μm sieve residue amount (mass%) + 0.363 × free lime amount (mass%) + 4.67 × glass phase Basicity of (2)
Compressive strength 3 (age 28 days; unit: N / mm 2 ) = 31.5−0.054 × 45 μm sieve residue (mass%) + 0.06 × basicity of glass phase × vitrification rate 3)
[2] As physical properties of coal ash, boron elution amount, free lime amount, vitrification rate, basicity of glass phase, and 45 μm sieve residue amount are measured, and using the following formulas (1) to (3), Calculate compressive strength 1 to 3, which is an estimate of the compressive strength of the coal ash-containing mortar at each time point of 3 days, 7 days and 28 days of age, and calculate one or more of the compressive strengths 1 to 3 Is smaller than a predetermined reference value for each of the compressive strengths 1 to 3, an increase in the amount of free lime so that all the calculated values of the compressive strengths 1 to 3 are equal to or greater than the predetermined reference value. A method for improving the strength development of coal ash, characterized in that a treatment for reducing the amount of residual sieve residue is performed.
Compressive strength 1 (material age 3 days; unit: N / mm 2 ) = 9.3-0.028 × boron elution amount (mg / L) + 1.2 × free lime amount (mass%) + 1.2 × glass phase Basicity of (1)
Compressive strength 2 (age 7 days; unit: N / mm 2 ) = 13.6-0.012 × 45 μm sieve residue amount (mass%) + 0.363 × free lime amount (mass%) + 4.67 × glass phase Basicity of (2)
Compressive strength 3 (age 28 days; unit: N / mm 2 ) = 31.5−0.054 × 45 μm sieve residue (mass%) + 0.06 × basicity of glass phase × vitrification rate 3)
本発明によれば、材齢２８日等の強度を実際に測定することなく、石炭灰の強度発現性を迅速に評価することができる。
また、本発明によれば、石炭灰の強度発現性の評価方法で得られた結果に基き、かつ、該評価方法で用いた特定の式を利用して、簡易にかつ確実に、強度発現性の低い石炭灰を、強度発現性が良好な石炭灰に改質することができる。
According to the present invention, it is possible to quickly evaluate the strength development of coal ash without actually measuring the strength such as the age of 28 days.
Further, according to the present invention, based on the result obtained by the method for evaluating the strength development of coal ash, and using the specific formula used in the evaluation method, the strength development can be performed easily and reliably. The coal ash having a low strength can be reformed into a coal ash having good strength development.
以下、本発明について詳細に説明する。本発明においては、石炭灰の物性値として、ホウ素溶出量、フリーライム量、ガラス化率、ガラス相の塩基度、及び４５μｍ篩残分量を測定する。
［ホウ素溶出量］
ホウ素溶出量は、以下の手順で測定する。
（１） 蒸留水７５ｍｌに石炭灰２５ｇを投入し、ｐＨを８．５±０．２に調整しつつ１０分間撹拌する。この際、ｐＨ調整には、塩酸又は水酸化ナトリウム水溶液を使用する。
（２） 撹拌終了後に固液分離を行い、得られた液中のホウ素濃度を、ＩＣＰを用いて測定する。
Hereinafter, the present invention will be described in detail. In the present invention, boron elution amount, free lime amount, vitrification rate, basicity of glass phase, and 45 μm sieve residue are measured as physical properties of coal ash.
[Boron elution amount]
The boron elution amount is measured by the following procedure.
(1) Add 25 g of coal ash to 75 ml of distilled water and stir for 10 minutes while adjusting the pH to 8.5 ± 0.2. At this time, hydrochloric acid or a sodium hydroxide aqueous solution is used for pH adjustment.
(2) After completion of stirring, solid-liquid separation is performed, and the boron concentration in the obtained liquid is measured using ICP.
［フリーライム量］
フリーライム量は、ＪＩＳ−Ｒ５２０２に準じて測定する。
[Amount of free lime]
The amount of free lime is measured according to JIS-R5202.
［ガラス化率］
石炭灰のガラス化率を測定する方法としては、ガラス化率を測定し得る限り、特に限定されるものではないが、例えば、粉末Ｘ線回折に基づく検量線法、粉末Ｘ線回折に基づくプロファイルフィッティング法等が挙げられる。
これらの方法のうち、粉末Ｘ線回折に基づく検量線法又は粉末Ｘ線回折に基づくプロファイルフィッティング法により、石炭灰のガラス化率を測定するのが好ましい。これらの方法によれば、石炭灰を所定の溶媒に懸濁させる等の化学的操作を要することなく、石炭灰のガラス化率を短時間で測定することができる。
[Vitrification rate]
The method for measuring the vitrification rate of coal ash is not particularly limited as long as the vitrification rate can be measured. For example, a calibration curve method based on powder X-ray diffraction, a profile based on powder X-ray diffraction Examples include a fitting method.
Among these methods, the vitrification rate of coal ash is preferably measured by a calibration curve method based on powder X-ray diffraction or a profile fitting method based on powder X-ray diffraction. According to these methods, the vitrification rate of coal ash can be measured in a short time without requiring a chemical operation such as suspending coal ash in a predetermined solvent.
粉末Ｘ線回折に基づく検量線法においては、ムライト（２θ＝１６．５゜付近に現れる（１１０）ピーク）、α−石英（２θ＝２０．８゜付近に現れる（０１０）ピーク）及びマグネタイト（２θ＝２５．６゜付近に現れる（０２２）ピーク）のそれぞれについての検量線を予め作成する。
次に、被測定試料としての石炭灰を、粉末Ｘ線回折法により回折する。そして、かかる回折強度（ピーク面積）を用い、上記のようにして予め作成した検量線に基づいて、石炭灰に含まれるムライト、α−石英及びマグネタイトのそれぞれを定量する。このようにして得られた定量結果を用いて、下記式に基づいて、石炭灰のガラス化率（質量％）を算出する。
ガラス化率（質量％）＝１００−結晶鉱物の合計量（質量％）
In the calibration curve method based on powder X-ray diffraction, mullite ((110) peak appearing near 2θ = 16.5 °), α-quartz ((010) peak appearing near 2θ = 20.8 °) and magnetite ( A calibration curve is prepared in advance for each of (022 peak) appearing in the vicinity of 2θ = 25.6 °.
Next, the coal ash as the sample to be measured is diffracted by the powder X-ray diffraction method. Then, using the diffraction intensity (peak area), each of mullite, α-quartz, and magnetite contained in the coal ash is quantified based on the calibration curve prepared in advance as described above. The vitrification rate (mass%) of coal ash is calculated based on the following formula using the quantitative result thus obtained.
Vitrification rate (mass%) = 100-total amount of crystal mineral (mass%)
なお、粉末Ｘ線回折は、市販の粉末Ｘ線回折装置（例えば、Ｄ８ ＡＤＶＡＮＣＥ（ＢＲＵＫＥＲ ＡＸＳ社製）等）を用いて、常法により行うことができる。この場合において、粉末Ｘ線回折は、被測定試料としての石炭灰に、Ａｌ２Ｏ３、ＣａＦ２、ＭｇＦ２等の内部標準物質を添加して行い、その添加量は５〜１０質量％であるのが好ましい。 Powder X-ray diffraction can be performed by a conventional method using a commercially available powder X-ray diffractometer (for example, D8 ADVANCE (manufactured by BRUKER AXS) or the like). In this case, powder X-ray diffraction is performed by adding an internal standard substance such as Al 2 O 3 , CaF 2 , MgF 2 to coal ash as a sample to be measured, and the addition amount is 5 to 10% by mass. Preferably there is.
粉末Ｘ線回折に基づくプロファイルフィッティング法としては、例えば、リートベルト解析法等が挙げられる。
リートベルト解析法は、まず、被測定試料としての石炭灰を粉末Ｘ線回折法により回折し、その回折結果から石炭灰に含まれるムライト、α−石英及びマグネタイトの実測プロファイルを求める。なお、粉末Ｘ線回折は、上述した粉末Ｘ線回折に基づく検量線法と同様に、市販の粉末Ｘ線回折装置（例えば、Ｄ８ ＡＤＶＡＮＣＥ（ＢＲＵＫＥＲ ＡＸＳ社製）等）を用いて、常法により行うことができ、この場合において、粉末Ｘ線回折は、被測定試料としての石炭灰に、Ａｌ２Ｏ３、ＣａＦ２、ＭｇＦ２等の内部標準物質を添加して行い、その添加量は５〜１０質量％であるのが好ましい。
次に、得られた実測プロファイルに、石炭灰に含まれるムライト、α−石英及びマグネタイトの理論プロファイルをフィッティングすることにより、石炭灰に含まれるムライト、α−石英及びマグネタイトのそれぞれを定量する。なお、実測プロファイルと理論プロファイルとのフィッティング及び結晶性鉱物の定量は、慣用されているリートベルト解析プログラム（例えば、ＴＯＰＡＳ（ＢＲＵＫＥＲ ＡＸＳ社製）等）等を用いて行うことができる。
このようにして得られた結果から、下記式に基づいて、石炭灰のガラス化率（質量％）を算出する。
ガラス化率（質量％）＝１００−結晶鉱物の合計量（質量％）
Examples of the profile fitting method based on powder X-ray diffraction include a Rietveld analysis method.
In the Rietveld analysis method, first, coal ash as a sample to be measured is diffracted by a powder X-ray diffraction method, and an actual measurement profile of mullite, α-quartz and magnetite contained in the coal ash is obtained from the diffraction result. In addition, powder X-ray diffraction is a conventional method using a commercially available powder X-ray diffractometer (for example, D8 ADVANCE (manufactured by BRUKER AXS), etc.) in the same manner as the calibration curve method based on the above-mentioned powder X-ray diffraction. In this case, powder X-ray diffraction is performed by adding an internal standard substance such as Al 2 O 3 , CaF 2 , MgF 2 to coal ash as a sample to be measured, and the amount added is 5 It is preferable that it is 10 mass%.
Next, by fitting the theoretical profiles of mullite, α-quartz and magnetite contained in the coal ash to the obtained actual measurement profile, each of mullite, α-quartz and magnetite contained in the coal ash is quantified. The fitting between the measured profile and the theoretical profile and the quantification of the crystalline mineral can be performed using a commonly used Rietveld analysis program (for example, TOPAS (manufactured by BRUKER AXS) or the like).
From the result thus obtained, the vitrification rate (mass%) of coal ash is calculated based on the following formula.
Vitrification rate (mass%) = 100-total amount of crystal mineral (mass%)
［ガラス相の塩基度］
ガラス相の塩基度は、下記式に基づいて算出する。
塩基度＝（非晶質Ａｌ２Ｏ３（質量％）＋非晶質ＣａＯ（質量％）＋全ＭｇＯ（質量％））／非晶質ＳｉＯ２（質量％）
ここで、式中の非晶質Ａｌ２Ｏ３、非晶質ＣａＯ、及び非晶質ＳｉＯ２の各質量割合の値は、以下の式に基いて求めることができる。
非晶質Ａｌ２Ｏ３（質量％）＝全Ａｌ２Ｏ３（質量％）−結晶質Ａｌ２Ｏ３（質量％）
非晶質ＣａＯ（質量％）＝全ＣａＯ（質量％）−フリーライム量（質量％）
非晶質ＳｉＯ２＝全ＳｉＯ２（質量％）−結晶質ＳｉＯ２（質量％）
また、結晶質Ａｌ２Ｏ３（質量％）と結晶質ＳｉＯ２（質量％）の値は、上記粉末Ｘ線回折に基づく検量線法やプロファイルフィッティング法において求めたムライト及びα−石英の量から算出することができる。
全ＭｇＯ（質量％））、全Ａｌ２Ｏ３（質量％）、全ＣａＯ（質量％）、全ＳｉＯ２（質量％）は、ＪＩＳ Ｒ５２０２に準じて測定することができる。
[Basicity of glass phase]
The basicity of the glass phase is calculated based on the following formula.
Basicity = (Amorphous Al 2 O 3 (mass%) + Amorphous CaO (mass%) + Total MgO (mass%)) / Amorphous SiO 2 (mass%)
Here, the value of each mass ratio of amorphous Al 2 O 3 , amorphous CaO, and amorphous SiO 2 in the formula can be obtained based on the following formula.
Amorphous Al 2 O 3 (mass%) = total Al 2 O 3 (mass%) − crystalline Al 2 O 3 (mass%)
Amorphous CaO (mass%) = total CaO (mass%) − free lime amount (mass%)
Amorphous SiO 2 = total SiO 2 (mass%) − crystalline SiO 2 (mass%)
The values of crystalline Al 2 O 3 (mass%) and crystalline SiO 2 (mass%) are based on the amounts of mullite and α-quartz obtained by the calibration curve method or profile fitting method based on the above powder X-ray diffraction. Can be calculated.
Total MgO (mass%)), total Al 2 O 3 (mass%), total CaO (mass%), and total SiO 2 (mass%) can be measured according to JIS R5202.
［４５μｍ篩残分量］
４５μｍ篩残分量は、ＪＩＳ−Ａ６２０１の網ふるい方法に準じて測定することができる。
[45 μm sieve residue]
The amount of 45 μm sieve residue can be measured according to the screen screening method of JIS-A6201.
本発明においては、下記式（１）〜（３）を用いて、材齢３日、７日、２８日の各時点における石炭灰含有モルタルの圧縮強度の推定値である圧縮強度１〜３を算出し、該圧縮強度１〜３の算出値を用いて、石炭灰の強度発現性を評価する。
圧縮強度１（材齢３日；単位：Ｎ／ｍｍ２）＝９．３−０．０２８×ホウ素溶出量（ｍｇ／Ｌ）＋１．２×フリーライム量（質量％）＋１．２×ガラス相の塩基度・・・（１）
圧縮強度２（材齢７日；単位：Ｎ／ｍｍ２）＝１３．６−０．０１２×４５μｍ篩残分量（質量％）＋０．３６３×フリーライム量（質量％）＋４．６７×ガラス相の塩基度・・・（２）
圧縮強度３（材齢２８日；単位：Ｎ／ｍｍ２）＝３１．５−０．０５４×４５μｍ篩残分量（質量％）＋０．０６×ガラス相の塩基度×ガラス化率・・・（３）
なお、圧縮強度１〜３は、中庸熱ポルトランドセメント７０質量％と石炭灰３０質量％の混合セメントについて、ＪＩＳ−Ｒ５２０１に準じて測定して得られる材齢３日、７日、２８日の各時点における圧縮強度に相当する推定値である。
石炭灰の評価の一例としては、圧縮強度１が９．５Ｎ／ｍｍ２以上、圧縮強度２が１６．０Ｎ／ｍｍ２以上、圧縮強度３が３３．０Ｎ／ｍｍ２以上、の各条件をすべて満たす石炭灰を、初期〜長期に亘って強度発現性が良好であると評価することが挙げられる。なお、圧縮強度１または圧縮強度２が小さい場合は、初期強度の発現性が劣ると評価することができる。また、圧縮強度３が小さい場合は、長期強度の発現性が劣ると評価することができる。
In the present invention, by using the following formulas (1) to (3), compressive strengths 1 to 3 which are estimated values of the compressive strength of the coal ash-containing mortar at each time point of 3 days, 7 days and 28 days of age are used. It calculates and the strength expression property of coal ash is evaluated using the calculated value of this compression strength 1-3.
Compressive strength 1 (material age 3 days; unit: N / mm 2 ) = 9.3-0.028 × boron elution amount (mg / L) + 1.2 × free lime amount (mass%) + 1.2 × glass phase Basicity of (1)
Compressive strength 2 (age 7 days; unit: N / mm 2 ) = 13.6-0.012 × 45 μm sieve residue amount (mass%) + 0.363 × free lime amount (mass%) + 4.67 × glass phase Basicity of (2)
Compressive strength 3 (age 28 days; unit: N / mm 2 ) = 31.5−0.054 × 45 μm sieve residue (mass%) + 0.06 × basicity of glass phase × vitrification rate 3)
The compressive strengths 1 to 3 are the age of 3 days, 7 days and 28 days obtained by measuring according to JIS-R5201 for the mixed cement of 70% by mass of moderately hot Portland cement and 30% by mass of coal ash. This is an estimated value corresponding to the compression strength at the time.
As an example of the evaluation of coal ash, all the conditions that the compressive strength 1 is 9.5 N / mm 2 or more, the compressive strength 2 is 16.0 N / mm 2 or more, and the compressive strength 3 is 33.0 N / mm 2 or more. It is mentioned that the coal ash to be filled is evaluated as having good strength development from the initial stage to the long term. In addition, when compressive strength 1 or compressive strength 2 is small, it can be evaluated that the initial strength is poor. Moreover, when the compressive strength 3 is small, it can be evaluated that the long-term strength is poor.
次に、本発明の石炭灰の強度発現性の改善方法は、前述の圧縮強度１〜３のいずれか１つ以上の算出値が、圧縮強度１〜３の各々について予め定めた基準値（例えば、圧縮強度１：９．５Ｎ／ｍｍ２以上、圧縮強度２：１６．０Ｎ／ｍｍ２以上、圧縮強度３：３３．０Ｎ／ｍｍ２以上）よりも小さい場合、圧縮強度１〜３の算出値のすべてが、前記予め定めた基準値以上となるように、フリーライム量の増大のための処理、及び／又は、４５μｍ篩残分量の減少のための処理を行なうものである。
フリーライム量の増大のための処理の例としては、フリーライムを含む粉末と石炭灰を混合する方法が挙げられる。フリーライムを含む粉末中のフリーライムの割合は、好ましくは５０質量％以上、より好ましくは６０質量％以上である。フリーライムを含む粉末の例としては、生石灰粉末、塩素バイパスダスト等が挙げられる。該粉末のブレーン比表面積は、好ましくは３０００〜８０００ｃｍ２／ｇである。
なお、石炭灰中のフリーライム量を増大させる場合、該フリーライム量は、０．５〜１．５質量％に調整することが好ましく、０．６〜１．４質量％に調整することがより好ましい。フリーライム量が０．５質量％未満では、強度向上効果がほとんど認められない。フリーライム量が１．５質量％を超えると、流動性の低下等が生じるおそれがある。
Next, in the method for improving the strength development of the coal ash according to the present invention, any one or more calculated values of the compression strengths 1 to 3 described above are predetermined reference values for the compression strengths 1 to 3 (for example, Compressive strength 1: 9.5 N / mm 2 or higher, Compressive strength 2: 16.0 N / mm 2 or higher, Compressive strength 3: 33.0 N / mm 2 or higher) The processing for increasing the amount of free lime and / or the processing for decreasing the amount of 45 μm sieve residue is performed so that all of the above are equal to or greater than the predetermined reference value.
As an example of the treatment for increasing the amount of free lime, there is a method of mixing powder containing free lime and coal ash. The proportion of free lime in the powder containing free lime is preferably 50% by mass or more, more preferably 60% by mass or more. Examples of the powder containing free lime include quick lime powder and chlorine bypass dust. The brane specific surface area of the powder is preferably 3000 to 8000 cm 2 / g.
In addition, when increasing the amount of free lime in coal ash, it is preferable to adjust this amount of free lime to 0.5-1.5 mass%, and to adjust to 0.6-1.4 mass%. More preferred. If the amount of free lime is less than 0.5% by mass, the strength improving effect is hardly recognized. When the amount of free lime exceeds 1.5% by mass, fluidity may be lowered.
４５μｍ篩残分量を減少させる方法としては、石炭灰を粉砕する方法が挙げられる。
なお、４５μｍ篩残分量を減少させる場合、４５μｍ篩残分量は、１２質量％以下に調整することが好ましく、１１質量％以下に調整することがより好ましい。４５μｍ篩残分量が１２質量％を超えている場合は、強度向上効果はほとんど認められない。
As a method for reducing the amount of 45 μm sieve residue, there is a method of pulverizing coal ash.
In addition, when reducing 45 micrometer sieve residue amount, it is preferable to adjust 45 micrometer sieve residue amount to 12 mass% or less, and it is more preferable to adjust to 11 mass% or less. When the amount of 45 μm sieve residue exceeds 12% by mass, the strength improving effect is hardly recognized.
［実施例１］
（１）使用材料
使用した石炭灰Ａ〜Ｇの各物性値を表１に示す。
（２）石炭灰の評価
中庸熱ポルトランドセメント（太平洋セメント社製）７０質量％と上記各石炭灰３０質量％の混合セメントについて、ＪＩＳ−Ｒ５２０１に準じて、モルタルの圧縮強度（材齢：３日、７日、２８日）を測定した。
上記各石炭灰の物性値と上記式（１）〜（３）とに基づいて算出される圧縮強度１〜３の算出値、及び、上記各石炭灰の圧縮強度の実測値を表２に示す。
[Example 1]
(1) Used material Table 1 shows the physical properties of the used coal ash A to G.
(2) Evaluation of coal ash For mixed cement of 70% by mass of medium heat Portland cement (manufactured by Taiheiyo Cement) and 30% by mass of each of the above coal ash, compressive strength of mortar (age: 3 days) according to JIS-R5201 , 7 and 28).
Table 2 shows the calculated values of the compression strengths 1 to 3 calculated based on the physical property values of the coal ash and the formulas (1) to (3), and the measured values of the compression strength of the coal ash. .
［実施例２］
実施例１において、材齢３日の圧縮強度が低かった石炭灰Ｇに生石灰粉末（ブレーン比表面積：３７００ｃｍ２／ｇ）を混合して、フリーライム量が０．９質量％である石炭灰Ｇ２を得た。該石炭灰Ｇ２を使用して、実施例１と同じ方法でモルタルの圧縮強度を測定した。
その結果、材齢３日の圧縮強度は１０．３Ｎ／ｍｍ２、材齢７日の圧縮強度は１６．４Ｎ／ｍｍ２、材齢２８日の圧縮強度は３３．４Ｎ／ｍｍ２であった。結果を表１及び２に示す。
[Example 2]
In Example 1, coal ash G2 having a free lime content of 0.9 mass% by mixing quick lime powder (Brain specific surface area: 3700 cm 2 / g) with coal ash G having a low compressive strength at the age of 3 days in Example 1. Got. Using the coal ash G2, the compressive strength of the mortar was measured in the same manner as in Example 1.
As a result, the compressive strength at the age of three days compressive strength of 10.3N / mm 2, the age 7 days 16.4N / mm 2, compression strength at the age of 28 days was 33.4N / mm 2 . The results are shown in Tables 1 and 2.
［実施例３］
実施例１において、材齢７日及び２８日の圧縮強度が低かった石炭灰Ｆを粉砕して、４５μｍ篩残分量が８．０質量％である石炭灰Ｆ２を得た。該石炭灰Ｆ２を使用して、実施例１と同じ方法でモルタルの圧縮強度を測定した。
その結果、材齢３日の圧縮強度は９．９Ｎ／ｍｍ２、材齢７日の圧縮強度は１６．１Ｎ／ｍｍ２、材齢２８日の圧縮強度は３３．４Ｎ／ｍｍ２であった。結果を表１及び２に示す。
[Example 3]
In Example 1, the coal ash F having a low compressive strength at 7 days and 28 days of age was pulverized to obtain coal ash F2 having a 45 μm sieve residue of 8.0% by mass. Using the coal ash F2, the compressive strength of the mortar was measured in the same manner as in Example 1.
As a result, the compressive strength at the age of 3 days was 9.9 N / mm 2 , the compressive strength at the age of 7 days was 16.1 N / mm 2 , and the compressive strength at the age of 28 days was 33.4 N / mm 2 . . The results are shown in Tables 1 and 2.
［実施例４］
実施例３で調製した石炭灰Ｆ２に生石灰粉末（ブレーン比表面積：３７００ｃｍ２／ｇ）を混合して、フリーライム量が０．９質量％である石炭灰Ｆ３を得た。該石炭灰Ｆ３を使用して、実施例１と同じ方法でモルタルの圧縮強度を測定した。
その結果、材齢３日の圧縮強度は１０．４Ｎ／ｍｍ２、材齢７日の圧縮強度は１６．５Ｎ／ｍｍ２、材齢２８日の圧縮強度は３３．７Ｎ／ｍｍ２であった。結果を表１及び２に示す。
[Example 4]
Quick lime powder (Blaine specific surface area: 3700 cm 2 / g) was mixed with the coal ash F2 prepared in Example 3 to obtain coal ash F3 having a free lime content of 0.9 mass%. Using the coal ash F3, the compressive strength of the mortar was measured in the same manner as in Example 1.
As a result, the compressive strength at the age of 3 days was 10.4 N / mm 2 , the compressive strength at the age of 7 days was 16.5 N / mm 2 , and the compressive strength at the age of 28 days was 33.7 N / mm 2 . . The results are shown in Tables 1 and 2.
表２に示すように、各石炭灰の物性値と上記式（１）〜（３）とに基づいて算出した圧縮強度１〜３（材齢３日、７日、２８日相当）の値は、実測値（材齢３日、７日、２８日）の値とほぼ等しい。
例えば、圧縮強度１が９．５Ｎ／ｍｍ２以上、圧縮強度２が１６．０Ｎ／ｍｍ２以上、及び圧縮強度３が３３．０Ｎ／ｍｍ２以上と算出された石炭灰Ａ〜Ｄでは、実測値においても、初期（３日）〜長期（２８日）に亘って強度発現性が良好であることが分かる。
一方、圧縮強度１が９．０Ｎ／ｍｍ２と算出された石炭灰Ｇでは、初期の強度発現性を示す実測値（３日）も低かった。また、圧縮強度２が１６．０Ｎ／ｍｍ２未満でかつ圧縮強度３が３３．０Ｎ／ｍｍ２未満と算出された石炭灰Ｅ〜Ｆでは、材齢７日、２８日の強度発現性の実測値も低かった。
このように、本発明では、石炭灰の物性値と特定の式とに基づいて、石炭灰の強度発現性を高い信頼性で迅速に評価しうることが分かる。
また、実施例２〜４から、石炭灰のフリーライム量を増大させたり、あるいは、４５μｍ篩残分量を減少させることによって、石炭灰の強度発現性を改善させうることが分かる。
As shown in Table 2, the values of the compressive strengths 1 to 3 (equivalent to 3 days, 7 days, and 28 days of age) calculated based on the physical properties of each coal ash and the above formulas (1) to (3) are The measured values (material age 3 days, 7 days, 28 days) are almost equal.
For example, in the coal ash A to D, in which the compressive strength 1 is calculated to be 9.5 N / mm 2 or more, the compressive strength 2 is 16.0 N / mm 2 or more, and the compressive strength 3 is 33.0 N / mm 2 or more, actual measurement is performed. Also in terms of values, it can be seen that the strength development is good from the initial stage (3 days) to the long term (28 days).
On the other hand, in the coal ash G in which the compressive strength 1 was calculated to be 9.0 N / mm 2 , the actual measurement value (3 days) showing the initial strength development was also low. In addition, in the coal ash E to F in which the compressive strength 2 is less than 16.0 N / mm 2 and the compressive strength 3 is calculated to be less than 33.0 N / mm 2 , the actual strength measurement of the ages 7 days and 28 days is actually measured. The value was also low.
Thus, in this invention, it turns out that the strength expression property of coal ash can be evaluated rapidly with high reliability based on the physical property value of coal ash and a specific formula.
Moreover, from Examples 2-4, it turns out that the intensity | strength expression property of coal ash can be improved by increasing the amount of free lime of coal ash, or reducing the amount of 45 micrometer sieve residue.
Claims (2)
下記式（１）〜（３）を用いて、材齢３日、７日、２８日の各時点における石炭灰含有モルタルの圧縮強度の推定値である圧縮強度１〜３を算出し、該圧縮強度１〜３の算出値を用いて、石炭灰の強度発現性を評価することを特徴とする石炭灰の強度発現性の評価方法。
圧縮強度１（材齢３日；単位：Ｎ／ｍｍ２）＝９．３−０．０２８×ホウ素溶出量（ｍｇ／Ｌ）＋１．２×フリーライム量（質量％）＋１．２×ガラス相の塩基度・・・（１）
圧縮強度２（材齢７日；単位：Ｎ／ｍｍ２）＝１３．６−０．０１２×４５μｍ篩残分量（質量％）＋０．３６３×フリーライム量（質量％）＋４．６７×ガラス相の塩基度・・・（２）
圧縮強度３（材齢２８日；単位：Ｎ／ｍｍ２）＝３１．５−０．０５４×４５μｍ篩残分量（質量％）＋０．０６×ガラス相の塩基度×ガラス化率・・・（３） As physical properties of coal ash, boron elution amount, free lime amount, vitrification rate, basicity of glass phase, and 45 μm sieve residue amount are measured,
Using the following formulas (1) to (3), compressive strengths 1 to 3 that are estimated values of the compressive strength of the coal ash-containing mortar at each time point of 3 days, 7 days, and 28 days are calculated. An evaluation method for strength development of coal ash, wherein strength development of coal ash is evaluated using calculated values of strengths 1 to 3.
Compressive strength 1 (material age 3 days; unit: N / mm 2 ) = 9.3-0.028 × boron elution amount (mg / L) + 1.2 × free lime amount (mass%) + 1.2 × glass phase Basicity of (1)
Compressive strength 2 (age 7 days; unit: N / mm 2 ) = 13.6-0.012 × 45 μm sieve residue amount (mass%) + 0.363 × free lime amount (mass%) + 4.67 × glass phase Basicity of (2)
Compressive strength 3 (age 28 days; unit: N / mm 2 ) = 31.5−0.054 × 45 μm sieve residue (mass%) + 0.06 × basicity of glass phase × vitrification rate 3)
下記式（１）〜（３）を用いて、材齢３日、７日、２８日の各時点における石炭灰含有モルタルの圧縮強度の推定値である圧縮強度１〜３を算出し、該圧縮強度１〜３のいずれか１つ以上の算出値が、圧縮強度１〜３の各々について予め定めた基準値よりも小さい場合、前記圧縮強度１〜３の算出値のすべてが、前記予め定めた基準値以上となるように、フリーライム量の増大のための処理、及び／又は、４５μｍ篩残分量の減少のための処理を行なうことを特徴とする石炭灰の強度発現性の改善方法。
圧縮強度１（材齢３日；単位：Ｎ／ｍｍ２）＝９．３−０．０２８×ホウ素溶出量（ｍｇ／Ｌ）＋１．２×フリーライム量（質量％）＋１．２×ガラス相の塩基度・・・（１）
圧縮強度２（材齢７日；単位：Ｎ／ｍｍ２）＝１３．６−０．０１２×４５μｍ篩残分量（質量％）＋０．３６３×フリーライム量（質量％）＋４．６７×ガラス相の塩基度・・・（２）
圧縮強度３（材齢２８日；単位：Ｎ／ｍｍ２）＝３１．５−０．０５４×４５μｍ篩残分量（質量％）＋０．０６×ガラス相の塩基度×ガラス化率・・・（３） As physical properties of coal ash, boron elution amount, free lime amount, vitrification rate, basicity of glass phase, and 45 μm sieve residue amount are measured,
Using the following formulas (1) to (3), compressive strengths 1 to 3 that are estimated values of the compressive strength of the coal ash-containing mortar at each time point of 3 days, 7 days, and 28 days are calculated. When any one or more calculated values of the strengths 1 to 3 are smaller than a reference value determined in advance for each of the compression strengths 1 to 3, all the calculated values of the compression strengths 1 to 3 are determined in advance. A method for improving the strength development of coal ash, characterized in that a treatment for increasing the amount of free lime and / or a treatment for reducing the amount of 45 μm sieve residue is performed so as to be equal to or greater than a reference value.
Compressive strength 1 (material age 3 days; unit: N / mm 2 ) = 9.3-0.028 × boron elution amount (mg / L) + 1.2 × free lime amount (mass%) + 1.2 × glass phase Basicity of (1)
Compressive strength 2 (age 7 days; unit: N / mm 2 ) = 13.6-0.012 × 45 μm sieve residue amount (mass%) + 0.363 × free lime amount (mass%) + 4.67 × glass phase Basicity of (2)
Compressive strength 3 (age 28 days; unit: N / mm 2 ) = 31.5−0.054 × 45 μm sieve residue (mass%) + 0.06 × basicity of glass phase × vitrification rate 3)
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