JP2006297285A - Low alkali hardner for water-containing soil and hardening treatment method - Google Patents
Low alkali hardner for water-containing soil and hardening treatment method Download PDFInfo
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- JP2006297285A JP2006297285A JP2005122823A JP2005122823A JP2006297285A JP 2006297285 A JP2006297285 A JP 2006297285A JP 2005122823 A JP2005122823 A JP 2005122823A JP 2005122823 A JP2005122823 A JP 2005122823A JP 2006297285 A JP2006297285 A JP 2006297285A
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- 239000002689 soil Substances 0.000 title claims abstract description 61
- 239000003513 alkali Substances 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 9
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 43
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 28
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims abstract description 19
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims abstract description 18
- 229910052808 lithium carbonate Inorganic materials 0.000 claims abstract description 18
- 238000000634 powder X-ray diffraction Methods 0.000 claims abstract description 4
- 238000001228 spectrum Methods 0.000 claims abstract description 4
- 239000000463 material Substances 0.000 claims description 48
- 238000007711 solidification Methods 0.000 claims description 38
- 230000008023 solidification Effects 0.000 claims description 38
- 238000010438 heat treatment Methods 0.000 claims description 21
- 238000002156 mixing Methods 0.000 claims description 9
- 229910052782 aluminium Inorganic materials 0.000 claims description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 5
- 230000002776 aggregation Effects 0.000 claims description 4
- -1 aluminum hydroxide compound Chemical class 0.000 claims description 4
- 238000007743 anodising Methods 0.000 claims description 4
- 238000006386 neutralization reaction Methods 0.000 claims description 4
- 238000005054 agglomeration Methods 0.000 claims description 2
- 229940024545 aluminum hydroxide Drugs 0.000 abstract description 18
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 abstract description 17
- 229910001385 heavy metal Inorganic materials 0.000 abstract description 3
- 239000002585 base Substances 0.000 abstract 1
- 239000006227 byproduct Substances 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 14
- 238000002441 X-ray diffraction Methods 0.000 description 12
- 239000002245 particle Substances 0.000 description 8
- 238000001035 drying Methods 0.000 description 7
- 239000004568 cement Substances 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 230000009257 reactivity Effects 0.000 description 5
- 241000196324 Embryophyta Species 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 239000010802 sludge Substances 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000012669 compression test Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 241001465754 Metazoa Species 0.000 description 2
- MXRIRQGCELJRSN-UHFFFAOYSA-N O.O.O.[Al] Chemical compound O.O.O.[Al] MXRIRQGCELJRSN-UHFFFAOYSA-N 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 2
- 229910001680 bayerite Inorganic materials 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 description 2
- IIPYXGDZVMZOAP-UHFFFAOYSA-N lithium nitrate Chemical compound [Li+].[O-][N+]([O-])=O IIPYXGDZVMZOAP-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000003672 processing method Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 239000011398 Portland cement Substances 0.000 description 1
- 240000008042 Zea mays Species 0.000 description 1
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 1
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 1
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 1
- SMYKVLBUSSNXMV-UHFFFAOYSA-K aluminum;trihydroxide;hydrate Chemical class O.[OH-].[OH-].[OH-].[Al+3] SMYKVLBUSSNXMV-UHFFFAOYSA-K 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 238000009614 chemical analysis method Methods 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 238000005056 compaction Methods 0.000 description 1
- 235000005822 corn Nutrition 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000002542 deteriorative effect Effects 0.000 description 1
- 230000000816 effect on animals Effects 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000010440 gypsum Substances 0.000 description 1
- 229910052602 gypsum Inorganic materials 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 239000002075 main ingredient Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000003002 pH adjusting agent Substances 0.000 description 1
- 238000001139 pH measurement Methods 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 238000007655 standard test method Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
- Soil Conditioners And Soil-Stabilizing Materials (AREA)
- Processing Of Solid Wastes (AREA)
- Treatment Of Sludge (AREA)
Abstract
Description
本発明は、浚渫底泥や建設汚泥、汚染土壌等の含水土を固化・不溶化するために適した含水土用低アルカリ固化材およびそれを用いた固化処理方法に関する。 The present invention relates to a low alkali solidification material for hydrous soil suitable for solidifying and insolubilizing hydrous soil such as dredged bottom mud, construction sludge, and contaminated soil, and a solidification treatment method using the same.
軟弱土の土質改良には、固化材を使用する固化処理が施される。また、土木工事等に伴って発生する建設汚泥等を搬出する際、流動性が高くそのままでの搬送が困難な場合があるので、固化材を使用して固化処理した後、搬出するという方法が採用される。何れの目的においても、固化材には、固化処理後の土が目的に合った十分な強度を有していること、適度の固化速度を有していること、固化材が化学的に安定であり有害物質が溶出しないこと等の特性が要求される。 To improve the soil quality of soft soil, a solidification process using a solidifying material is performed. In addition, when carrying out construction sludge, etc. generated by civil engineering work, etc., there are cases where it is difficult to carry it as it is because of its high fluidity. Adopted. For any purpose, the solidified material should have sufficient strength that suits the purpose of the soil after solidification, a suitable solidification rate, and the solidified material is chemically stable. Certain characteristics such as no toxic substances eluting are required.
これら複数の特性が要求される固化材に関し、既に多くの技術が開示されている。このうちセメントを主成分とするセメント系固化材では高強度は得られるものの、セメント自体のアルカリにより固化処理土のpH値が11〜12程度となる。このアルカリによる動植物への影響、アンモニアの発生、近年では、鉛などの両性重金属汚染土の処理時に鉛の再溶出が問題となる場合がある。 Many techniques have already been disclosed for solidifying materials that require a plurality of properties. Among them, a cement-based solidified material mainly composed of cement can provide high strength, but the pH value of the solidified soil becomes about 11 to 12 due to the alkali of the cement itself. The effects of alkali on animals and plants, the generation of ammonia, and, in recent years, re-elution of lead may be a problem during the treatment of amphoteric heavy metal contaminated soil such as lead.
これらの問題を解決するために、マグネシア系固化材が提案されている。特許文献1〜3では、酸化マグネシウムとpH調整剤として硫酸アルミニウムなどの酸性材料や強度改良材としての高炉スラグ、せっこう、燐酸塩などを組合せたマグネシア系固化材が開示されている。 In order to solve these problems, a magnesia-based solidifying material has been proposed. Patent Documents 1 to 3 disclose a magnesia-based solidified material in which magnesium oxide and an acidic material such as aluminum sulfate as a pH adjusting agent and blast furnace slag, gypsum, and phosphate as a strength improving material are combined.
一方、非特許文献1に示すpHと各種重金属の溶解度の関係から、特に鉛の不溶化性能面で固化処理土のpHは9〜10が望ましいと推定される。しかし、酸化マグネシウム自体のpHはこれよりやや高く、このpH調整のために、酸性材料を添加すると固化強度が低下するなどの問題もある。 On the other hand, from the relationship between the pH shown in Non-Patent Document 1 and the solubility of various heavy metals, it is presumed that the pH of the solidified soil is preferably 9 to 10 particularly in terms of insolubilization performance of lead. However, the pH of magnesium oxide itself is slightly higher than this, and there is a problem that the solidification strength decreases when an acidic material is added to adjust the pH.
本発明は、動植物への影響などの環境負荷が比較的小さく、固化処理土のpHが、鉛汚染土壌を効果的に不溶化可能なpH9〜10程度の低アルカリとなり、且つ、十分な強度を有するように、含水土を固化することができる含水土用低アルカリ固化材およびそれを用いた固化処理方法に関する。 The present invention has a relatively low environmental load such as an effect on animals and plants, and the pH of the solidified soil becomes a low alkali of about pH 9 to 10 that can effectively insolubilize lead-contaminated soil, and has sufficient strength. Thus, it is related with the low alkali solidification material for hydrous soil which can solidify hydrous soil, and the solidification processing method using the same.
本発明に係る含水土用低アルカリ固化材は、酸化マグネシウムを15質量%を超えて60質量%以下、波長1.5405Åにおける粉末X線回折スペクトルが、2θ=22±5°にブロードなピークの頂点を有し、該ブロードなピークのベースラインを基準とした半値幅が6°〜20°である水硬性アルミナを30質量%〜82質量%、及び炭酸リチウムを2質量%〜15質量%含むことを特徴とする。 The low alkali solidification material for hydrous soil according to the present invention has a broad peak at 2θ = 22 ± 5 ° with a powder X-ray diffraction spectrum at a wavelength of 1.5405 mm, exceeding 15% by mass of magnesium oxide. 30% to 82% by mass of hydraulic alumina having a peak and a half width of 6 ° to 20 ° with respect to the baseline of the broad peak, and 2% to 15% by mass of lithium carbonate It is characterized by that.
この含水土用低アルカリ固化材によれば、含水土中で酸化マグネシウム、水硬性アルミナおよび炭酸リチウムが相互に反応し、低アルカリで高い強度が得られる。ここで、酸化マグネシウムの添加量が15質量%より小さいと、十分な固化強度が得られないか、あるいは処理土のpHが低くなりすぎる。一方、60質量%より多くても、固化強度が低下するか、pHが高くなりすぎる。また、水硬性アルミナの添加量が30質量%より小さいと、十分な固化強度が得られないか、処理土のpHが高くなる。一方、82質量%より多い場合、処理土のpHが低くなりすぎる。また、炭酸リチウムの添加量が2質量%より小さいと、十分な固化強度が得られず、一方、炭酸リチウムを15質量%より多く添加しても、コストに見合う強度増進効果が得られず、経済的にも好ましくない。 According to this low alkali solidifying material for hydrous soil, magnesium oxide, hydraulic alumina and lithium carbonate react with each other in the hydrous soil, and high strength can be obtained with low alkali. Here, when the addition amount of magnesium oxide is less than 15% by mass, sufficient solidification strength cannot be obtained, or the pH of the treated soil becomes too low. On the other hand, even if it exceeds 60 mass%, solidification intensity | strength falls or pH becomes high too much. Moreover, when the addition amount of hydraulic alumina is smaller than 30% by mass, sufficient solidification strength cannot be obtained or the pH of the treated soil becomes high. On the other hand, when it is more than 82% by mass, the pH of the treated soil becomes too low. In addition, when the amount of lithium carbonate added is less than 2% by mass, sufficient solidification strength cannot be obtained. On the other hand, even if lithium carbonate is added in an amount of more than 15% by mass, an effect of increasing the strength commensurate with the cost cannot be obtained. It is not economically preferable.
本発明に係る水硬性アルミナは、アルミニウムの陽極酸化処理工程の中和・凝集により副生した非晶質の水酸化アルミニウム化合物を、50℃〜400℃で恒量となるまで加熱することにより得られたものであることが好ましい。なお、この方法によって得られる生成物は、厳密にはアルミナではないが、本発明では水硬性アルミナと称する。 The hydraulic alumina according to the present invention is obtained by heating an amorphous aluminum hydroxide compound by-produced by neutralization / aggregation in an anodizing treatment step of aluminum until a constant weight is obtained at 50 ° C. to 400 ° C. It is preferable that The product obtained by this method is not strictly alumina, but is called hydraulic alumina in the present invention.
ここで、加熱温度が50℃よりも低いと、水硬性アルミナの反応性が十分でなく、固化材とした場合、十分な固化強度を得ることができない。また、恒量(乾燥する)となるまでに長時間がかかり、製造コストの増加を招くことになる。一方、400℃よりも高い温度で長時間加熱すると、同様に水硬性アルミナの反応性が低下し、固化強度が低下する。 Here, when the heating temperature is lower than 50 ° C., the reactivity of the hydraulic alumina is not sufficient, and when the solidified material is used, sufficient solidification strength cannot be obtained. Moreover, it takes a long time to reach a constant weight (drying), resulting in an increase in manufacturing cost. On the other hand, when heated at a temperature higher than 400 ° C. for a long time, similarly, the reactivity of hydraulic alumina is lowered, and the solidification strength is lowered.
また、本発明に係る固化処理方法は、含水土1m3当たり、上記の含水土用低アルカリ固化材を50kg〜200kg混合することを特徴とする。この方法により、処理土がpH9〜10の低アルカリで、且つ、十分な固化強度を得ることが出来る。 Moreover, the solidification processing method according to the present invention is characterized in that 50 kg to 200 kg of the above-mentioned low alkali solidification material for hydrous soil is mixed per 1 m 3 of hydrous soil. By this method, the treated soil is a low alkali having a pH of 9 to 10, and sufficient solidification strength can be obtained.
本発明によれば、動植物への影響などの環境負荷が小さく、また、含水土を鉛の不溶化に適したpH9〜10の低アルカリで、且つ、十分な強度を有するように固化処理することができる。 According to the present invention, the environmental load such as the influence on animals and plants is small, and the hydrous soil is solidified so as to have a low alkali of pH 9 to 10 suitable for lead insolubilization and sufficient strength. it can.
以下、本発明に係る含水土用低アルカリ固化材およびそれを用いた固化処理方法について説明する。 Hereinafter, the low alkali solidification material for hydrous soil according to the present invention and the solidification treatment method using the same will be described.
<含水土用低アルカリ固化材>
本発明に係る含水土用低アルカリ固化材の好適な実施形態について説明する。含水土用低アルカリ固化材は、酸化マグネシウムが15質量%を超えて60質量%以下、好ましくは25質量%〜50質量%、水硬性アルミナが30質量%〜82質量%、好ましくは35質量%〜75質量%、炭酸リチウムが2質量%〜15質量%、好ましくは2.5質量%〜5質量%の割合で混合されている。
<Low alkali solidifying material for hydrous soil>
A preferred embodiment of the low alkali solidifying material for hydrous soil according to the present invention will be described. The low-alkali solidified material for hydrous soil has magnesium oxide in excess of 15% by mass and 60% by mass or less, preferably 25% by mass to 50% by mass, and hydraulic alumina by 30% by mass to 82% by mass, preferably 35% by mass. -75 mass% and lithium carbonate are mixed in a proportion of 2 mass% to 15 mass%, preferably 2.5 mass% to 5 mass%.
この含水土用低アルカリ固化材によれば、含水土中で酸化マグネシウム、水硬性アルミナおよび炭酸リチウムが相互に反応し、低アルカリで高い強度が得られる。ここで、酸化マグネシウムの添加量が15質量%以下であると、十分な固化強度が得られないか、あるいは処理土のpHが低くなりすぎる。一方、60質量%より多くても、固化強度が低下するか、pHが高くなりすぎる。また、水硬性アルミナの添加量が30質量%より小さいと、十分な固化強度が得られないか、処理土のpHが高くなる。一方、82質量%より多い場合、処理土のpHが低くなりすぎる。また、炭酸リチウムの添加量が2質量%より小さいと、十分な固化強度が得られず、一方、炭酸リチウムを15質量%より多く添加しても、コストに見合う強度増進効果が得られず、経済的にも好ましくない。 According to this low alkali solidifying material for hydrous soil, magnesium oxide, hydraulic alumina and lithium carbonate react with each other in the hydrous soil, and high strength can be obtained with low alkali. Here, when the addition amount of magnesium oxide is 15% by mass or less, sufficient solidification strength cannot be obtained, or the pH of the treated soil becomes too low. On the other hand, even if it exceeds 60 mass%, solidification intensity | strength falls or pH becomes high too much. Moreover, when the addition amount of hydraulic alumina is smaller than 30% by mass, sufficient solidification strength cannot be obtained or the pH of the treated soil becomes high. On the other hand, when it is more than 82% by mass, the pH of the treated soil becomes too low. In addition, when the amount of lithium carbonate added is less than 2% by mass, sufficient solidification strength cannot be obtained. On the other hand, even if lithium carbonate is added in an amount of more than 15% by mass, an effect of increasing the strength commensurate with the cost cannot be obtained. It is not economically preferable.
固化材の主成分の1つとして用いられる酸化マグネシウムは、か焼温度により軽焼マグネシアと硬焼マグネシアの2種に大別できるが、本発明においては、軽焼マグネシアを使用するのが好ましい。硬焼マグネシアは水和活性に乏しいことから、非晶質な水硬性アルミナの固化助剤として使用した場合に目標強度への到達に時間がかかるためである。この軽焼マグネシアは、粒度の細かいものが好ましく、そのBET比表面積は20〜50m2/g程度である。なお、ハンドリング性を悪化させない範囲で更に粒度の細かい軽焼マグネシアを使用するとより好ましい結果が得られる。 Magnesium oxide used as one of the main components of the solidifying material can be roughly classified into two types, light-burned magnesia and hard-burned magnesia, depending on the calcination temperature. In the present invention, it is preferable to use light-burned magnesia. This is because hard-fired magnesia is poor in hydration activity, so that it takes time to reach the target strength when used as a solidification aid for amorphous hydraulic alumina. The light-burned magnesia preferably has a fine particle size, and its BET specific surface area is about 20 to 50 m 2 / g. It should be noted that more preferable results can be obtained by using lightly-burned magnesia with a finer particle size within a range not deteriorating handling properties.
また、固化材のもう一つの主成分である水硬性アルミナは、波長1.5405Åにおける粉末X線回折スペクトルが、2θ=22±5°、そのブロードなピークのベースラインを基準とした半値幅が6°〜20°である特性をもつものである。このような特性を有すると、酸化マグネシウムと炭酸リチウムと好適に反応して高い強度が得られるとともに、pHを適切に調整できる。 In addition, hydraulic alumina, which is another main component of the solidified material, has a powder X-ray diffraction spectrum at a wavelength of 1.5405 mm, 2θ = 22 ± 5 °, and a half-value width based on the baseline of the broad peak. It has the characteristic which is 6 degrees-20 degrees. With such characteristics, magnesium oxide and lithium carbonate react appropriately to obtain high strength, and the pH can be adjusted appropriately.
水硬性アルミナの反応性は粒度に影響されるため、レーザー回折式粒度分布計により測定される水硬性アルミナの平均粒径は1μm〜20μmのものが好ましく、2μm〜15μmものの使用は更に望ましい。平均粒径が20μmより大きい場合、十分な固化強度が得られにくく材料分離を生じる傾向がある。1μmより小さいと、粉体流動性が好ましくなく輸送時のハンドリング性や固化助剤との混合性に問題が生じる場合がある。 Since the reactivity of hydraulic alumina is affected by particle size, the average particle size of hydraulic alumina measured by a laser diffraction particle size distribution meter is preferably 1 μm to 20 μm, and more preferably 2 μm to 15 μm. When the average particle size is larger than 20 μm, sufficient solidification strength is difficult to obtain, and there is a tendency to cause material separation. If it is smaller than 1 μm, the powder flowability is not preferred, and there may be a problem in handling properties during transportation and mixing with the solidification aid.
固化材の補助成分として使用する炭酸リチウムは、純度90質量%以上のものが望ましい。90質量%未満の製品も使用可能であるが、その場合、水硬性アルミナに対する割合を調整する必要がある。また、その粒度は平均粒径で2μm〜20μmのものが好ましく、2μm〜15μmのものが更に好ましい。20μmより大では十分な促進効果が得られないか、材料分離を生じる傾向があり、また、2μmより小では、上述の水硬性アルミナと同様に、粉体流動性が好ましくなく輸送時のハンドリング性や固化助剤との混合性に問題が生じる場合がある。なお、固化助剤として、炭酸リチウムの他に、塩化リチウム、硝酸リチウム等の無機塩等も使用可能である。ただし、入手の容易さで炭酸リチウムの使用が最も好ましい。 The lithium carbonate used as an auxiliary component of the solidifying material preferably has a purity of 90% by mass or more. Although a product of less than 90% by mass can be used, in that case, it is necessary to adjust the ratio relative to the hydraulic alumina. The average particle size is preferably 2 μm to 20 μm, more preferably 2 μm to 15 μm. If it is larger than 20 μm, a sufficient accelerating effect is not obtained or there is a tendency to cause material separation, and if it is smaller than 2 μm, like the above-mentioned hydraulic alumina, the powder fluidity is not preferable, and handling property during transportation In some cases, there is a problem in the mixing property with the solidification aid. In addition to lithium carbonate, inorganic salts such as lithium chloride and lithium nitrate can be used as the solidification aid. However, it is most preferable to use lithium carbonate because of its availability.
固化材として混合されたこれらの材料、すなわち酸化マグネシウム、水硬性アルミナ、及び炭酸リチウムは何れも粉末状であればよく、その調製に当たっては特別な機器、手段を必要とせず、ミキサー等公知の粉体混合用の機器を使った公知の粉体混合方法が適用できる。更に好ましくは、これらの粉体の混合と粉砕をボールミル等公知の粉砕機で同時に行うことで、より固化特性に優れた混合物を得ることが出来る。 These materials mixed as a solidifying material, that is, magnesium oxide, hydraulic alumina, and lithium carbonate may all be in the form of powder, and no special equipment or means is required for the preparation, and known powder such as a mixer is used. A known powder mixing method using a body mixing device can be applied. More preferably, these powders can be mixed and pulverized simultaneously with a known pulverizer such as a ball mill to obtain a mixture with more excellent solidification characteristics.
本発明に用いる水硬性アルミナは、次の方法によって好適に得られる。すなわち、水硬性アルミナを製造するに当たっては、アルミニウム製造産業の副産物として生成する非晶質の水酸化アルミニウム含水物等(アルミニウムの陽極酸化処理工程の中和・凝集により副生する水酸化アルミニウム)を主成分とするスラッジを原料とする。このスラッジを50℃〜400℃、好ましくは110℃〜350℃で恒量になるまで加熱する。これにより、水硬性アルミナが得られる。加熱温度が50℃よりも低いと、水硬性アルミナの反応性が十分でなく、固化材とした場合、十分な固化強度を得ることができない。また、恒量(乾燥する)となるまでに長時間がかかり、製造コストの増加を招くことになる。一方、400℃よりも高い温度で長時間加熱すると、同様に水硬性アルミナの反応性が低下し、固化強度が低下する。なお、水硬性アルミナの製造装置としては、通常の各種の電気加熱式、熱風式乾燥機、或いはロータリーキルン等の加熱装置を好適に使用することができる。 The hydraulic alumina used in the present invention is suitably obtained by the following method. In other words, in producing hydraulic alumina, amorphous aluminum hydroxide hydrates and the like produced as a by-product of the aluminum manufacturing industry (aluminum hydroxide by-produced by neutralization / aggregation of the anodizing process of aluminum) are produced. The main ingredient is sludge. The sludge is heated at 50 ° C. to 400 ° C., preferably 110 ° C. to 350 ° C. until a constant weight is obtained. Thereby, hydraulic alumina is obtained. When the heating temperature is lower than 50 ° C., the reactivity of the hydraulic alumina is not sufficient, and sufficient solidification strength cannot be obtained when the solidified material is used. Moreover, it takes a long time to reach a constant weight (drying), resulting in an increase in manufacturing cost. On the other hand, when heated at a temperature higher than 400 ° C. for a long time, similarly, the reactivity of hydraulic alumina is lowered, and the solidification strength is lowered. In addition, as a manufacturing apparatus of hydraulic alumina, heating apparatuses, such as a normal various electric heating type, a hot air dryer, or a rotary kiln, can be used conveniently.
<固化処理方法>
次に、本発明に係る含水土の固化処理方法の好適な実施形態について説明する。上記方法により得られた低アルカリ固化材は目標強度、処理コストなどを考慮して、含水土1m3当たりに50kg〜200kg、好ましくは50kg〜150kg添加して混合する。固化材の混合には、バックホウ、クラムシェル、プラント混合装置などの一般的な混合装置を用いることが出来る。
<Solidification method>
Next, a preferred embodiment of the method for solidifying hydrous soil according to the present invention will be described. The low alkali solidified material obtained by the above method is added and mixed in an amount of 50 kg to 200 kg, preferably 50 kg to 150 kg per 1 m 3 of hydrous soil in consideration of target strength, processing cost, and the like. For mixing the solidifying material, a general mixing apparatus such as a backhoe, a clam shell, a plant mixing apparatus, or the like can be used.
以下に実施例を示し本発明を具体的に詳細に説明するが、本発明は、下記実施例に限定されるものではない。 EXAMPLES Hereinafter, the present invention will be described in detail with reference to examples. However, the present invention is not limited to the following examples.
(1)水硬性アルミナの製造
アルミニウムの陽極酸化処理工程の中和・凝集により副生した非晶質の水酸化アルミニウム含水物をPasolina(株)製(TYO-300)乾燥機またはヤマト科学(株)製の電気炉を用いて、JIS R 5202 「ポルトランドセメントの化学分析方法」 8.強熱減量の定量方法 に則り、50〜400℃で15分間ずつ加熱を繰返し、恒量(最後の15分間の加熱前後の質量差が乾燥前の水酸化アルミニウム含有物の0.05質量%以下)になるまで加熱した後、通常のボールミルを用いて粉砕することにより、粉体状の水硬性アルミナを得た。そして、得られた水硬性アルミナを、(株)堀場製作所製レーザー回折式粒度分布測定装置LA−500Aによって測定したところ、非晶質な水硬性アルミナの平均粒径は15μmであった。
(1) Manufacture of hydraulic alumina Amorphous aluminum hydroxide hydrate produced as a by-product of neutralization and agglomeration in the anodizing process of aluminum is manufactured by Pasolina (TYO-300) dryer or Yamato Science Co., Ltd. ) JIS R 5202 "Chemical analysis method of Portland cement" using an electric furnace manufactured by Repeated heating at 50 to 400 ° C for 15 minutes in accordance with the quantitative method for loss on ignition, constant weight (mass difference before and after heating for the last 15 minutes is 0.05 mass% or less of the aluminum hydroxide-containing material before drying) After heating to pulverize, a powdery hydraulic alumina was obtained by pulverization using a normal ball mill. And when the obtained hydraulic alumina was measured by the laser diffraction type particle size distribution measuring device LA-500A made by Horiba, Ltd., the average particle diameter of the amorphous hydraulic alumina was 15 μm.
ここで、図1に、原料に使用した副生水酸化アルミニウムの自然乾燥(天日乾燥)におけるX線回折測定結果を示し、図2、図3および図4に、その副生水酸化アルミニウムを加熱温度110℃、200℃および400℃として得られた非晶質な水硬性アルミナのX線回折測定結果を示す。また、表1に、副生水酸化アルミニウムの110℃加熱後の化学分析結果、並びに強熱減量を示す。 Here, FIG. 1 shows the result of X-ray diffraction measurement in natural drying (sun drying) of by-product aluminum hydroxide used as a raw material, and FIGS. 2, 3 and 4 show the by-product aluminum hydroxide. The X-ray-diffraction measurement result of the amorphous hydraulic alumina obtained by heating temperature 110 degreeC, 200 degreeC, and 400 degreeC is shown. Table 1 shows the chemical analysis results of the by-product aluminum hydroxide after heating at 110 ° C. and the ignition loss.
なお、X線回折測定には、X線回折装置として理学電気(株)製RINT−2500Vを用いた。X線回折装置における測定条件は次の通りとした。 For the X-ray diffraction measurement, RINT-2500V manufactured by Rigaku Corporation was used as the X-ray diffraction apparatus. The measurement conditions in the X-ray diffractometer were as follows.
管球:Cu、管電流:130mA、管電圧:50kV、サンプリング幅:0.02°、走査速度:4°/min、波長:1.5405Å、測定回折角範囲(2θ):5°〜70° Tube: Cu, tube current: 130 mA, tube voltage: 50 kV, sampling width: 0.02 °, scanning speed: 4 ° / min, wavelength: 1.5405 mm, measurement diffraction angle range (2θ): 5 ° to 70 °
図1に示すX線回折の結果、加熱前の副生水酸化アルミニウムには、少量のギブサイト(Al(OH)3):Gi及びバイヤライト(Al2O3):Baのピークが確認されるものの、副生水酸化アルミニウムの大半は非晶質のアルミニウム化合物であることが確認された。図2に示すX線回折の結果では、副生水酸化アルミニウム含水物を110℃で加熱することによって得られた水硬性アルミナには、2θ=約13°〜33°にブロードなピークが認められ、2θ=20°にその頂点を有している。さらに、このブロードなピークの左右のボトムにベースラインBを引き(ブロードなピークの裾野を線で結び)、このベースラインBからのブロードなピークの高さを基準にして半値幅を求めたところ、2θ=17°と2θ=26°で半値となり、半値幅は9°であった。図3に示すX線回折の結果でも、副生水酸化アルミニウム含水物を200℃の温度で加熱することによって得られた水硬性アルミナには、2θ=約14°〜38°にブロードなピークが認められ、2θ=22°にその頂点を有している。また、ベースラインBからのブロードなピークの高さを基準にして半値幅を求めたところ、2θ=18°と2θ=29°で半値となり、半値幅は11°であった。図4に示すX線回折の結果でも、副生水酸化アルミニウム含水物を400℃の温度で加熱することによって得られた水硬性アルミナには、2θ=約13°〜40°にブロードなピークが認められ、2θ=24°にその頂点を有している。また、ベースラインBからのブロードなピークの高さを基準にして半値幅を求めたところ、2θ=19°と2θ=31°で半値となり、半値幅は12°であった。 As a result of the X-ray diffraction shown in FIG. 1, a small amount of gibbsite (Al (OH) 3 ): Gi and bayerite (Al 2 O 3 ): Ba peaks are confirmed in the byproduct aluminum hydroxide before heating. However, most of the by-product aluminum hydroxide was confirmed to be an amorphous aluminum compound. As a result of X-ray diffraction shown in FIG. 2, a broad peak at 2θ = about 13 ° to 33 ° is recognized in hydraulic alumina obtained by heating the byproduct aluminum hydroxide hydrate at 110 ° C. It has its apex at 2θ = 20 °. Furthermore, the baseline B was drawn on the left and right bottoms of this broad peak (the broad peak skirt was connected by a line), and the half width was obtained based on the height of the broad peak from this baseline B. The half value was 2θ = 17 ° and 2θ = 26 °, and the half value width was 9 °. Also in the result of X-ray diffraction shown in FIG. 3, the hydraulic alumina obtained by heating the by-product aluminum hydroxide hydrate at a temperature of 200 ° C. has a broad peak at 2θ = about 14 ° to 38 °. Is recognized and has its apex at 2θ = 22 °. Further, when the half width was obtained based on the height of the broad peak from the baseline B, the half width was 2θ = 18 ° and 2θ = 29 °, and the half width was 11 °. Also in the result of X-ray diffraction shown in FIG. 4, the hydraulic alumina obtained by heating the byproduct aluminum hydroxide hydrate at a temperature of 400 ° C. has a broad peak at 2θ = about 13 ° to 40 °. Is recognized and has its apex at 2θ = 24 °. Further, when the full width at half maximum was determined based on the height of the broad peak from the baseline B, the full width at half maximum was 2θ = 19 ° and 2θ = 31 °, and the full width at half maximum was 12 °.
(2)固化材等の調製
中国産の軽焼マグネシアと、非晶質の副生水酸化アルミニウム含水物を表2に示す温度で恒量になるまで加熱することにより得られた水硬性アルミナ、そして、本荘ケミカル(株)製工業品の炭酸リチウムを用い、表2に示す割合で混合して調製した(実施例1〜24)。また、比較用として、水硬性アルミナ単味(比較例1、8)、酸化マグネシウムの添加量が少ない固化材(比較例2、9)、酸化マグネシウムの添加量の多い固化材(比較例3、10)、加熱温度が高すぎる水硬性アルミナを配合した固化材(比較例4、11)、加熱温度が低すぎる水硬性アルミナを用いた固化材(比較例5、12)さらに軽焼マグネシア(酸化マグネシウム)単味(比較例6、13)、宇部三菱セメント(株)製セメント系固化材ユースタビラー10(比較例7、14)をそれぞれ用意した。
(2) Preparation of solidified material, etc. Lightly burned magnesia made in China and hydraulic alumina obtained by heating amorphous by-product aluminum hydroxide hydrate to a constant weight at the temperature shown in Table 2, and The mixture was prepared by using lithium carbonate manufactured by Honjo Chemical Co., Ltd. at the ratio shown in Table 2 (Examples 1 to 24). In addition, as a comparative example, hydraulic alumina simple (Comparative Examples 1 and 8), solidified material with a small amount of magnesium oxide added (Comparative Examples 2 and 9), solidified material with a large amount of magnesium oxide added (Comparative Example 3, 10) Solidified material blended with hydraulic alumina whose heating temperature is too high (Comparative Examples 4 and 11), Solidified material using hydraulic alumina whose heating temperature is too low (Comparative Examples 5 and 12), and light calcined magnesia (oxidation) Magnesium) simple (Comparative Examples 6 and 13) and Ube Mitsubishi Cement Co., Ltd. cement-based solidified material youth tabiler 10 (Comparative Examples 7 and 14) were prepared.
(3)供試体の調製
固化試験用供試体の調整:表3および4に示すように、上記(2)において調製した固化材を2種類の試料土1m3に対し100kgの割合で添加した後、ホバート型ミキサーで3分間混合して改良土壌を調製した。このとき、土質の異なる2種の試料土としては、表3の「試料土」の欄に示す試料土A(含水比50.0%、pH7.49),および表4の「試料土」の欄に示す試料土B(黒ぼく)(含水比96.7%、pH6.82)を対象とした。その後、セメント協会標準試験方法JCAS L−01−2003「セメント系固化材による安定処理土の試験方法」に則り、改良土壌から、直径5cm×高さ10cmの成型体を得た。成型体は、温度20℃、湿度96%の恒温恒湿槽内で7日間養生して供試体を得た。
(3) Specimen Preparation solidification test specimen Adjustment: As shown in Table 3 and 4, after the addition of solidified material prepared in the above (2) with respect to two samples soil 1 m 3 at a rate of 100kg The improved soil was prepared by mixing for 3 minutes with a Hobart mixer. At this time, as the two types of sample soils having different soil properties, sample soil A (water content ratio 50.0%, pH 7.49) shown in the column of “sample soil” in Table 3 and “sample soil” in Table 4 Sample soil B (Kuroboku) (water content ratio 96.7%, pH 6.82) shown in the column was used as a target. Thereafter, a molded body having a diameter of 5 cm and a height of 10 cm was obtained from the improved soil in accordance with the Cement Association Standard Test Method JCAS L-01-2003 “Test Method for Stabilized Soil Using Cement-Based Solidified Material”. The molded body was cured for 7 days in a constant temperature and humidity chamber at a temperature of 20 ° C. and a humidity of 96% to obtain a specimen.
(4)改良土壌の評価:一軸圧縮試験
上記(3)で得られた供試体を、JIS A1216:1998「土の一軸圧縮試験方法」に則り一軸圧縮試験を行った。一軸圧縮強さについては、第3種改良土相当であるコーン指数400kN/m2を一軸圧縮強さに換算した値である160kN/m2以上を目標とした。コーン指数の一軸圧縮強さへの換算は以下のとおりとした。表3及び表4の「一軸圧縮強さ」の欄に測定結果を示す。
〔一軸圧縮強さ換算値=400(コーン指数)/10(一軸換算係数)/0.5(現場室内強度比)/0.5(ときほぐし・締固めによる強度低下)〕
(4) Evaluation of improved soil: uniaxial compression test The specimen obtained in the above (3) was subjected to a uniaxial compression test in accordance with JIS A1216: 1998 "Soil uniaxial compression test method". About uniaxial compressive strength, 160 kN / m < 2 > or more which is the value which converted the corn index 400 kN / m < 2 > equivalent to 3rd type | mold improved soil into uniaxial compressive strength was aimed. Conversion to the uniaxial compressive strength of the cone index was as follows. The measurement results are shown in the column of “uniaxial compressive strength” in Tables 3 and 4.
[Uniaxial compressive strength conversion value = 400 (cone index) / 10 (uniaxial conversion coefficient) /0.5 (in-situ indoor strength ratio) /0.5 (strength reduction due to occasional loosening and compaction)]
(5)改良土壌の評価:pH測定
上記(3)で得られた改良土壌について材齢7日で、地盤工学会基準JGS0211−2000「土懸濁液のpH試験方法」に則りpHを測定した。pH値については、非特許文献1に示される鉛の溶解度が最も低い9〜10の範囲内に在ることを目標とした。表3および表4の「改良土のpH」の欄に測定結果を示す。
(5) Evaluation of improved soil: pH measurement The pH of the improved soil obtained in (3) above was measured in accordance with JGS0211-2000 “Ground test method for soil suspension” at the age of 7 days. . About pH value, it aimed at existing in the range of 9-10 in which the solubility of lead shown in nonpatent literature 1 is the lowest. The measurement results are shown in the column of “pH of improved soil” in Tables 3 and 4.
[固化試験について]
(3)で述べたように、水硬性アルミナ、炭酸リチウム及び酸化マグネシウムより成る固化材を調製し、土質の異なる2種の粘性土A,黒ぼくBを対象とした場合の固化試験結果を表3及び表4に示している。
[About solidification test]
As described in (3), the solidification test results when solidified material consisting of hydraulic alumina, lithium carbonate, and magnesium oxide was prepared and two types of clay soil A and blackboku B with different soil properties were used as a target. 3 and Table 4.
比較例1、8に示すように、水硬性アルミナ単独で構成される固化材を用いた供試体の一軸圧縮強さは、160N/m2以下の低い値を示した。また、pHは9未満であった。また、比較例2、9及び比較例3、10に示すように、酸化マグネシウムの添加量が15質量%以下あるいは60質量%を超える量で構成される固化材を用いた供試体の一軸圧縮強さは、160kN/m2以上の強度が得られるものの、pHが9未満となるか、または、pHが10を超える。 As shown in Comparative Examples 1 and 8, the uniaxial compressive strength of the specimen using the solidified material composed of hydraulic alumina alone showed a low value of 160 N / m 2 or less. Moreover, pH was less than 9. Further, as shown in Comparative Examples 2 and 9 and Comparative Examples 3 and 10, the uniaxial compressive strength of the specimen using the solidified material in which the amount of magnesium oxide added is 15% by mass or less or exceeds 60% by mass. Although the strength of 160 kN / m 2 or more can be obtained, the pH is less than 9 or the pH exceeds 10.
一方、実施例1〜24に示すように、酸化マグネシウム、水硬性アルミナおよび炭酸リチウムが所定量添加、混合された固化材を使用した場合、得られた供試体の一軸圧縮強さは、目標とする160kN/m2を十分超えていた。そのうえ、pHは9〜10の低アルカリを示した。 On the other hand, as shown in Examples 1 to 24, when using a solidified material in which a predetermined amount of magnesium oxide, hydraulic alumina and lithium carbonate was added and mixed, the uniaxial compressive strength of the obtained specimen was the target and 160 kN / m 2 was sufficiently exceeded. Moreover, the pH showed a low alkali of 9-10.
これに対し、水硬性アルミナの製造(加熱)温度が、50℃以下、または400℃を超える場合、比較例4、5で示すように、供試体の強度は160kN/m2以下の低い値を示す場合がある。また、比較例6、13および比較例7、14で示す、酸化マグネシウム単味およびセメント系固化材を用いた供試体は、pHは10を超える。 On the other hand, when the production (heating) temperature of the hydraulic alumina exceeds 50 ° C. or exceeds 400 ° C., as shown in Comparative Examples 4 and 5, the strength of the specimen has a low value of 160 kN / m 2 or less. May show. Moreover, the specimens using the magnesium oxide simple substance and the cement-based solidified material shown in Comparative Examples 6 and 13 and Comparative Examples 7 and 14 have a pH exceeding 10.
Ba…バイヤライト(Al2O3)、Gi…ギブサイト(Al(OH)3)、B…ベースライン。
Ba ... bayerite (Al 2 O 3), Gi ... gibbsite (Al (OH) 3), B ... baseline.
Claims (3)
波長1.5405Åにおける粉末X線回折スペクトルが、2θ=22±5°にブロードなピークの頂点を有し、該ブロードなピークのベースラインを基準とした半値幅が6°〜20°である水硬性アルミナを30質量%〜82質量%、
及び炭酸リチウムを2質量%〜15質量%、
含むことを特徴とする含水土用低アルカリ固化材。 Magnesium oxide more than 15% by mass and 60% by mass or less,
A powder X-ray diffraction spectrum at a wavelength of 1.5405 mm has a peak of a broad peak at 2θ = 22 ± 5 °, and water having a half width of 6 ° to 20 ° with reference to the baseline of the broad peak 30% by mass to 82% by mass of hard alumina,
And 2% to 15% by weight of lithium carbonate,
A low alkali solidifying material for hydrous soil characterized by containing.
Wet soil 1 m 3 per solidification method characterized by mixing 50kg~200kg hydrous doyo low alkali solidifying material according to claim 1 or 2.
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