JP2019174240A - Calculation method of specific surface of fly ash in terms of ball, prediction method of activity index of fly ash, fly ash blended cement, and production method of fly ash blended cement - Google Patents
Calculation method of specific surface of fly ash in terms of ball, prediction method of activity index of fly ash, fly ash blended cement, and production method of fly ash blended cement Download PDFInfo
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本発明は、フライアッシュの球換算比表面積を算出する方法、該球換算比表面積を用いてフライアッシュの活性度指数を予測する方法、該活性度指数に基づき選択したフライアッシュを含むフライアッシュ混合セメント、および該フライアッシュ混合セメントの製造方法に関する。 The present invention relates to a method for calculating the sphere equivalent specific surface area of fly ash, a method for predicting an activity index of fly ash using the sphere equivalent specific surface area, and a fly ash mixture containing fly ash selected based on the activity index The present invention relates to a cement and a method for producing the fly ash mixed cement.
セメントの一部をフライアッシュで置換したフライアッシュ混合セメントは、フライアッシュから溶出するＳｉやＡｌがフライアッシュ粒子の近傍にあるセメント水和物の中に取り込まれ、低Ｃａ型のＣ−Ｓ−Ｈ（カルシウムシリケート水和物）相を生成する。この生成反応はポゾラン反応と呼ばれ、Ｃ−Ｓ−Ｈ相がアルカリシリカ反応（ＡＳＲ）を抑制するなど、コンクリートの耐久性を高める効果がある。 In the fly ash mixed cement in which a part of the cement is replaced with fly ash, Si and Al eluted from the fly ash are incorporated into the cement hydrate in the vicinity of the fly ash particles, and the low Ca type CS— An H (calcium silicate hydrate) phase is produced. This generation reaction is called a pozzolanic reaction, and the C—S—H phase has an effect of enhancing the durability of the concrete, for example, suppressing the alkali silica reaction (ASR).
ところで、一般社団法人石炭エネルギーセンターのフライアッシュ全国実態調査報告書によれば、平成２７年度のフライアッシュの発生量は１２７２万トン（この発生量の内訳は、電気事業で９３４万トン、一般産業で３３８万トンである。）に達した。しかも、電源を火力発電に大きく依存せざるを得ない我が国では、フライアッシュが多量に発生する状況は、今後もしばらく続くと予想される。
このフライアッシュの内、セメント混合材やコンクリート混和材として有効活用された量は約１５万トンであり、これはフライアッシュの発生量全体の１．２％に過ぎない。このように、フライアッシュのポゾラン反応性を積極的に活用する分野で、フライアッシュの利用率が低い理由の一つに、フライアッシュの化学組成や粉体特性に強く影響する炭種や燃焼プロセス等の因子が、石炭火力発電所のライン毎に異なるため、フライアッシュの品質（物理・化学的性質）が安定しないことが挙げられる。そのため、フライアッシュの品質を安定化する方法が研究されてきた。
By the way, according to the report on the nationwide survey of fly ash conducted by the Japan Coal Energy Center, the amount of fly ash generated in FY2015 was 12.72 million tons (the breakdown of this amount was 9.34 million tons in the electric business, general industry It was 3.38 million tons.) Moreover, in Japan, where the power source must largely depend on thermal power generation, the situation where a large amount of fly ash is generated is expected to continue for a while.
Of this fly ash, the amount effectively used as cement admixture or concrete admixture is about 150,000 tons, which is only 1.2% of the total amount of fly ash generated. In this way, one of the reasons for the low utilization rate of fly ash in the field of actively utilizing fly ash's pozzolanic reactivity is the type of coal and combustion process that strongly affect the chemical composition and powder characteristics of fly ash. This is because the quality (physical and chemical properties) of fly ash is not stable because factors such as these differ for each line of a coal-fired power plant. For this reason, methods for stabilizing the quality of fly ash have been studied.
例えば、非特許文献１に記載のフライアッシュの品質の安定化方法は、フライアッシュを分級して粗粒分を除去して、粒度を調整する方法である。また、これに関連して、非特許文献２では、分級により粒度を調整したフライアッシュの特性と、該フライアッシュの粒度の関係について報告している。該報告によれば、分級して粗粒分を除去して粒度を調整したフライアッシュの活性度指数と、球換算比表面積との間に直線関係があるとされている。ここで、活性度指数とは、ＪＩＳ Ａ ６２０１「コンクリート用フライアッシュ」の附属書Ｃに規定するフライアッシュのポゾラン反応性を評価するための特性値であって、フライアッシュを含まない基準モルタルに対するフライアッシュを含む試験モルタルの圧縮強度の比である。また、球換算比表面積とは、粒子の形状を球と仮定した場合に球の直径と密度から算出されるパラメータである。
しかし、球換算比表面積を測定するためには、高価なレーザー回折・散乱式 粒子径分布測定装置が必要なため、球換算比表面積に代えて、製造現場でより簡便に取得できるパラメータが求められる。
For example, the fly ash quality stabilization method described in Non-Patent Document 1 is a method of classifying fly ash to remove coarse particles and adjusting the particle size. In relation to this, Non-Patent Document 2 reports the relationship between the characteristics of fly ash whose particle size is adjusted by classification and the particle size of the fly ash. According to this report, it is said that there is a linear relationship between the activity index of fly ash, which is classified and coarse particles are removed to adjust the particle size, and the sphere equivalent specific surface area. Here, the activity index is a characteristic value for evaluating pozzolanic reactivity of fly ash as defined in Annex C of JIS A 6201 “Fly Ash for Concrete”, and is based on a reference mortar that does not include fly ash. Compressive strength ratio of test mortar containing fly ash. The spherical equivalent surface area is a parameter calculated from the diameter and density of the sphere when the shape of the particle is assumed to be a sphere.
However, in order to measure the specific surface area in terms of spheres, an expensive laser diffraction / scattering particle size distribution measuring device is required, so parameters that can be obtained more easily at the manufacturing site are required instead of the specific surface area in terms of spheres. .
したがって、本発明は、球換算比表面積よりも簡易に取得できるフライアッシュの特性値を用いて球換算比表面積を算出し、この算出した球換算比表面積を用いて活性度指数を予測する方法等を提供することを目的とする。 Therefore, the present invention calculates a sphere-equivalent specific surface area using fly ash characteristic values that can be obtained more easily than a sphere-equivalent specific surface area, and predicts an activity index using the calculated sphere-equivalent specific surface area. The purpose is to provide.
そこで、本発明者は、前記目的に適う球換算比表面積を算出する方法を検討したところ、下記の構成を有する球換算比表面積の算出方法等は、前記目的を達成できることを見い出し、本発明を完成させた。
［１］フライアッシュの球換算比表面積（実測値）、該フライアッシュのブレーン比表面積（実測値）および４５μｍ篩い残分（実測値）に基づき、下記（１）式を用いて回帰分析を行い、下記の回帰係数ａ、ｂおよびｃの値を求めた後、回帰係数ａ、ｂおよびｃの値を代入した下記（１）式に、球換算比表面積が未知のフライアッシュのブレーン比表面積（実測値）および４５μｍ篩い残分（実測値）を代入して、フライアッシュの球換算比表面積を算出する、フライアッシュの球換算比表面積の算出方法。
Ｓ＝ａ×ＢＬ＋ｂ×Ｒ４５＋ｃ ・・・（１）
ただし、（１）式中、Ｓはフライアッシュの球換算比表面積（ｃｍ２／ｃｍ３）、ＢＬはフライアッシュのブレーン比表面積（ｃｍ２／ｇ）、Ｒ４５はフライアッシュの４５μｍ篩い残分（質量％）を表す。
［２］前記［１］で算出したフライアッシュの球換算比表面積と、フライアッシュの活性度指数（実測値）に基づき、下記（２）式を用いて回帰分析を行い、下記の回帰係数ｄおよびｅの値を求めた後、回帰係数ｄおよびｅの値を代入した下記（２）式に、活性度指数が未知のフライアッシュの球換算比表面積（計算値）を代入して、フライアッシュの活性度指数の予測値を算出して予測する、フライアッシュの活性度指数の予測方法。
ＡＩ＝ｄ×Ｓ＋ｅ ・・・（２）
ただし、（２）式中、ＡＩはフライアッシュの活性度指数（％）、Ｓはフライアッシュの球換算比表面積（ｃｍ２／ｃｍ３）を表す。
［３］前記［２］に記載のフライアッシュの活性度指数の予測方法を用いて求めた、材齢９１日のモルタル中のフライアッシュの活性度指数の予測値が７０％以上のフライアッシュとセメントを含む、フライアッシュ混合セメント。
［４］前記［２］に記載の活性度指数の予測値が７０％以上であるフライアッシュとセメントを混合する、フライアッシュ混合セメントの製造方法。
Therefore, the present inventor examined a method for calculating a sphere-equivalent specific surface area suitable for the above purpose, and found that a method for calculating a sphere-equivalent specific surface area having the following configuration can achieve the above object, and the present invention. Completed.
[1] Based on the fly ash equivalent surface area (measured value), the fly ash brain specific surface area (actual value), and the 45 μm sieve residue (actual value), regression analysis was performed using the following equation (1). After obtaining the values of the following regression coefficients a, b and c, the following formula (1) into which the values of the regression coefficients a, b and c were substituted, the fly ash brain specific surface area with unknown spherical equivalent surface area ( A method for calculating the fly ash equivalent surface area of the fly ash by substituting the actual measurement value) and the 45 μm sieve residue (actual value) to calculate the sphere equivalent specific surface area of the fly ash.
S = a × B L + b × R 45 + c (1)
However, in the formula (1), S is the fly ash equivalent surface area (cm 2 / cm 3 ), BL is the fly ash brain specific surface area (cm 2 / g), and R 45 is the fly ash 45 μm sieve residue. It represents minutes (mass%).
[2] Based on the fly ash equivalent surface area calculated in [1] above and the fly ash activity index (actual measurement value), regression analysis is performed using the following equation (2), and the regression coefficient d After calculating the values of e and e, the sphere equivalent specific surface area (calculated value) of fly ash with unknown activity index is substituted into the following equation (2) into which the values of regression coefficients d and e are substituted, and fly ash A method for predicting the activity index of fly ash, which calculates and predicts the predicted value of the activity index of the fly ash.
A I = d × S + e (2)
However, expressed through the equation (2), A I is the fly ash activity index (%), S is the fly ash spherical equivalent specific surface area (cm 2 / cm 3).
[3] A fly ash having a predicted activity index of fly ash in a mortar of 91 days of age having a predicted value of 70% or more obtained using the method for predicting an activity index of fly ash according to [2] above Fly ash mixed cement, including cement.
[4] A method for producing fly ash-mixed cement, comprising mixing fly ash and cement having a predicted activity index of 70% or more according to [2].
本発明のフライアッシュの球換算比表面積の算出方法は、セメントの製造現場で簡易に取得できるフライアッシュの特性値（フライアッシュのブレーン比表面積および４５μｍ篩残分）を用いて、フライアッシュの球換算比表面積を精度よく算出できる。また、本発明のフライアッシュの活性度指数の予測方法は、算出したフライアッシュの球換算比表面積を用いてフライアッシュの活性度指数を精度よく予測できる。 The fly ash equivalent surface area of fly ash according to the present invention is calculated using fly ash characteristic values (fly ash specific surface area and 45 μm sieve residue) that can be easily obtained at the cement manufacturing site. The converted specific surface area can be calculated with high accuracy. In addition, the fly ash activity index predicting method according to the present invention can accurately predict the fly ash activity index using the calculated fly ash equivalent surface area of the sphere.
以下、本発明について、フライアッシュの球換算比表面積の算出方法、フライアッシュの活性度指数の予測方法、フライアッシュ混合セメント、およびフライアッシュ混合セメントの製造方法に分けて具体的に説明する。 Hereinafter, the present invention will be specifically described by dividing it into a method for calculating a fly ash equivalent surface area of a fly ash, a method for predicting an activity index of fly ash, a fly ash mixed cement, and a method for producing a fly ash mixed cement.
１．フライアッシュの球換算比表面積の算出方法
本発明のフライアッシュの球換算比表面積の算出方法は、フライアッシュの球換算比表面積（実測値）、該フライアッシュのブレーン比表面積（実測値）および４５μｍ篩い残分（実測値）に基づき、前記（１）式を用いて回帰分析を行い、回帰係数ａ、ｂおよびｃの値を求めた後、回帰係数ａ、ｂおよびｃの値を代入した前記（１）式に、球換算比表面積が未知のフライアッシュのブレーン比表面積（実測値）およびフライアッシュの４５μｍ篩い残分（実測値）を代入して、フライアッシュの球換算比表面積を算出する方法である。
ここで、本発明の算出方法の対象であるフライアッシュは、特に限定されず、石炭火力発電所、石油精製工場、その他の化学工場等で微粉炭を燃焼したときに発生する燃焼ガスから、集塵器により捕集された微粉末である。
また、フライアッシュの球換算比表面積はレーザー回折・散乱式 粒子径分布測定装置を用いて求めることができる。また、フライアッシュのブレーン比表面積および４５μｍ篩残分は、ＪＩＳ Ａ ６２０１「コンクリート用フライアッシュ」に準拠して測定する。
1. Calculation method of fly ash equivalent surface area of spheres The calculation method of fly ash equivalent surface area of spheres of the present invention is as follows: fly ash equivalent surface area (measured value), fly ash brain specific surface area (actual value), and 45 μm Based on the sieving residue (actual value), the regression analysis was performed using the equation (1) to obtain the values of the regression coefficients a, b and c, and then the values of the regression coefficients a, b and c were substituted. By substituting the fly ash brain specific surface area (actually measured value) and the fly ash 45 μm sieving residue (actually measured value) into the equation (1), the spherical equivalent surface area of fly ash is calculated. Is the method.
Here, the fly ash which is the object of the calculation method of the present invention is not particularly limited, and is collected from the combustion gas generated when pulverized coal is burned in a coal-fired power plant, an oil refinery plant, other chemical factories, etc. It is a fine powder collected by a duster.
The fly ash equivalent surface area in terms of sphere can be determined using a laser diffraction / scattering particle size distribution measuring apparatus. The specific surface area of the fly ash and the residue of the 45 μm sieve are measured according to JIS A 6201 “Fly Ash for Concrete”.
２．フライアッシュの活性度指数の予測方法
本発明のフライアッシュの活性度指数の予測方法は、前記算出したフライアッシュの球換算比表面積と、フライアッシュの活性度指数（実測値）に基づき、前記（２）式を用いて回帰分析を行い、回帰係数ｄおよびｅの値を求めた後、回帰係数ｄおよびｅの値を代入した前記（２）式に、活性度指数が未知のフライアッシュの球換算比表面積（計算値）を代入して、フライアッシュの活性度指数の予測値を算出して予測する方法である。
2. Fly Ash Activity Index Prediction Method The fly ash activity index prediction method according to the present invention is based on the calculated fly ash equivalent surface area of the fly ash and the fly ash activity index (actual value). 2) After performing regression analysis using the equation, the values of the regression coefficients d and e are obtained, and then the fly ash sphere whose activity index is unknown to the equation (2) in which the values of the regression coefficients d and e are substituted. This is a method of substituting the converted specific surface area (calculated value) to calculate and predict the predicted value of the fly ash activity index.
３．フライアッシュ混合セメント、およびフライアッシュ混合セメントの製造方法
本発明のフライアッシュ混合セメントは、前記フライアッシュの活性度指数の予測方法を用いて求めた、材齢９１日のモルタル中のフライアッシュの活性度指数の予測値が７０％以上のフライアッシュと、セメントを混合した混合セメントである。なお、前記フライアッシュの活性度指数の予測値は、好ましくは８０％以上、より好ましくは９０％以上、さらに好ましくは１００％以上である。
また、前記セメントは、特に制限されず、普通ポルトランドセメント、早強ポルトランドセメント、超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、低熱ポルトランドセメント、耐硫酸塩ポルトランドセメント、エコセメント、および高炉セメントから選ばれる１種以上が挙げられる。
また、本発明のフライアッシュ混合セメントの製造方法は、前記フライアッシュの活性度指数の予測方法を用いて求めた、材齢９１日のモルタル中のフライアッシュの活性度指数の予測値が７０％以上のフライアッシュと前記セメントを混合して製造する方法である。前記フライアッシュおよびセメントの混合に用いる混合装置は、セメント工場において混合セメントの製造に通常用いる装置であり、連続式またはバッチ式を問わず、容器回転型、容器固定型、粒体運動型等の各種混合装置を使用できる。
3. Fly ash mixed cement and method for producing fly ash mixed cement The fly ash mixed cement of the present invention is obtained by using the fly ash activity index predicting method described above, and the activity of fly ash in a 91-day-old mortar. This is a mixed cement obtained by mixing fly ash with a predicted value of the degree index of 70% or more and cement. The predicted value of the activity index of the fly ash is preferably 80% or more, more preferably 90% or more, and further preferably 100% or more.
The cement is not particularly limited, and is selected from ordinary Portland cement, early-strength Portland cement, ultra-early strong Portland cement, medium heat Portland cement, low heat Portland cement, sulfate-resistant Portland cement, eco-cement, and blast furnace cement. 1 type or more is mentioned.
Moreover, the manufacturing method of the fly ash mixed cement of the present invention has a predicted value of the activity index of fly ash in the mortar of 91 days of age obtained by the method for predicting the activity index of fly ash of 70%. This is a method for producing a mixture of the above fly ash and the cement. The mixing device used for mixing the fly ash and cement is a device that is usually used for manufacturing mixed cement in a cement factory, whether it is a continuous type or a batch type, such as a container rotating type, a container fixing type, and a particle motion type. Various mixing devices can be used.
以下、本発明を実施例により説明するが、本発明はこれらの実施例に限定されない。
１．前記（１）式を用いた回帰分析
表１に示すフライアッシュの球換算比表面積（実測値）、該フライアッシュのブレーン比表面積（実測値）、および該フライアッシュの４５μｍ篩い残分（実測値）に基づき、前記（１）式を用いて回帰分析を行い、回帰係数ａ、ｂおよびｃの値を求め、下記（３）式を得た。
Ｓ＝1.42ＢＬ＋99.12×Ｒ４５＋2729.44 ・・・（３）
なお、フライアッシュの球換算比表面積は、レーザー回折・散乱式 粒子径分布測定装置（製型番：MT3300 EX II、マイクロトラック・ベル社製）を用いて求めた。また、フライアッシュのブレーン比表面積、および該フライアッシュの４５μｍ篩い残分は、ＪＩＳ Ａ ６２０１「コンクリート用フライアッシュ」に準拠して測定した。
EXAMPLES Hereinafter, although an Example demonstrates this invention, this invention is not limited to these Examples.
1. Regression analysis using the equation (1) The sphere equivalent specific surface area (actual measurement value) of fly ash shown in Table 1, the brain specific surface area (actual measurement value) of the fly ash, and the 45 μm sieve residue (actual measurement value) of the fly ash ) Based on the above equation (1), regression analysis was performed to determine the values of the regression coefficients a, b and c, and the following equation (3) was obtained.
S = 1.42B L + 99.12 × R 45 +2729.44 (3)
The spherical equivalent surface area of fly ash was determined using a laser diffraction / scattering particle size distribution measuring device (manufactured model: MT3300 EX II, manufactured by Microtrack Bell). Further, the specific surface area of fly ash and the residue of the fly ash sieved by 45 μm were measured according to JIS A 6201 “Fly Ash for Concrete”.
表１に示すフライアッシュの球換算比表面積（実測値）と、前記（３）式から求めた球換算比表面積（計算値）の相関を図１に示す。この決定係数（Ｒ２）は0.75であるから、（３）式はフライアッシュの球換算比表面積を高い精度で算出することができる。 FIG. 1 shows the correlation between the sphere equivalent specific surface area (measured value) of fly ash shown in Table 1 and the sphere equivalent specific surface area (calculated value) obtained from the equation (3). Since this determination coefficient (R 2 ) is 0.75, Equation (3) can calculate the spherical equivalent surface area of fly ash with high accuracy.
２．前記（２）式を用いた回帰分析
表１に示すフライアッシュの活性度指数（実測値）と前記（３）式を用いて算出した球換算比表面積（計算値）に基づき、前記（２）式を用いて回帰分析を行い、回帰係数ｄおよびｅの値を求め、下記（４）式を得た。
ＡＩ＝0.0035Ｓ＋73.98 ・・・（４）
また、フライアッシュの活性度指数（実測値）と前記（３）式を用いて算出した球換算比表面積（計算値）の相関を図２に示す。
図２に示すように、決定係数は（Ｒ２）は0.78であり、フライアッシュの活性度指数（実測値）と球換算比表面積（計算値）の間には高い相関がある。
2. Regression analysis using the above equation (2) Based on the fly ash activity index (measured value) shown in Table 1 and the sphere equivalent specific surface area (calculated value) calculated using the above equation (3), the above (2) Regression analysis was performed using the equation to determine the values of the regression coefficients d and e, and the following equation (4) was obtained.
A I = 0.0035S + 73.98 (4)
Further, FIG. 2 shows the correlation between the fly ash activity index (actually measured value) and the sphere equivalent specific surface area (calculated value) calculated using the equation (3).
As shown in FIG. 2, the coefficient of determination (R 2 ) is 0.78, and there is a high correlation between the fly ash activity index (actual value) and the sphere equivalent specific surface area (calculated value).
前記（３）式を用いて表２に示すフライアッシュの球換算比表面積（表２中の球換算比表面積の計算値）を算出した。また、前記算出した球換算比表面積を用いて上記（４）式から表２に示すフライアッシュの活性度指数（表２中の活性度指数の予測値）を予測した。なお、表２に示すフライアッシュ１１〜１３は、表１に示すフライアッシュ１〜１０とは異なるものである。
表２に示すように、本発明の方法は、フライアッシュの球換算比表面積を高い精度で算出でき、また、フライアッシュの活性度指数を高い精度で予測することができる。
Using the above equation (3), the sphere equivalent specific surface area of fly ash shown in Table 2 (calculated value of the sphere equivalent specific surface area in Table 2) was calculated. Moreover, the activity index of the fly ash shown in Table 2 (predicted value of the activity index in Table 2) was predicted from the above formula (4) using the calculated sphere-equivalent specific surface area. In addition, the fly ash 11-13 shown in Table 2 is different from the fly ash 1-10 shown in Table 1.
As shown in Table 2, the method of the present invention can calculate the fly ash equivalent surface area of spheres with high accuracy, and can predict the activity index of fly ash with high accuracy.
Claims (4)
Ｓ＝ａ×ＢＬ＋ｂ×Ｒ４５＋ｃ ・・・（１）
ただし、（１）式中、Ｓはフライアッシュの球換算比表面積（ｃｍ２／ｃｍ３）、ＢＬはフライアッシュのブレーン比表面積（ｃｍ２／ｇ）、Ｒ４５はフライアッシュの４５μｍ篩い残分（質量％）を表す。 Based on the fly ash equivalent surface area (measured value), the fly ash brain specific surface area (actual value) and the 45 μm sieve residue (actual value), regression analysis was performed using the following formula (1). After obtaining the values of the regression coefficients a, b and c, the fly ash brane specific surface area (actual measurement value) whose sphere equivalent specific surface area is unknown is substituted into the following equation (1) into which the values of the regression coefficients a, b and c are substituted. And the calculation method of the spherical equivalent specific surface area of fly ash which substitutes the 45 micrometer sieve residue (actual value) of fly ash, and calculates the spherical equivalent specific surface area of fly ash.
S = a × B L + b × R 45 + c (1)
However, in the formula (1), S is the fly ash equivalent surface area (cm 2 / cm 3 ), BL is the fly ash brain specific surface area (cm 2 / g), and R 45 is the fly ash 45 μm sieve residue. It represents minutes (mass%).
ＡＩ＝ｄ×Ｓ＋ｅ ・・・（２）
ただし、（２）式中、ＡＩはフライアッシュの活性度指数（％）、Ｓはフライアッシュの球換算比表面積（ｃｍ２／ｃｍ３）を表す。 Based on the fly ash equivalent surface area calculated in claim 1 and the fly ash activity index (actual measurement value), regression analysis is performed using the following formula (2), and the values of the following regression coefficients d and e: After substituting the sphere equivalent specific surface area (calculated value) of fly ash with unknown activity index into the following equation (2) into which the values of regression coefficients d and e are substituted, the fly ash activity index is calculated. A method for predicting the activity index of fly ash that calculates and predicts the predicted value of.
A I = d × S + e (2)
However, expressed through the equation (2), A I is the fly ash activity index (%), S is the fly ash spherical equivalent specific surface area (cm 2 / cm 3).
The manufacturing method of the fly ash mixing cement which mixes the fly ash and the cement whose predicted value of the activity index of Claim 2 is 70% or more.
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