WO2024070814A1 - Accélérateur liquide, et béton projeté - Google Patents

Accélérateur liquide, et béton projeté Download PDF

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Publication number
WO2024070814A1
WO2024070814A1 PCT/JP2023/033922 JP2023033922W WO2024070814A1 WO 2024070814 A1 WO2024070814 A1 WO 2024070814A1 JP 2023033922 W JP2023033922 W JP 2023033922W WO 2024070814 A1 WO2024070814 A1 WO 2024070814A1
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Prior art keywords
setting
quick
mass
liquid quick
liquid
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PCT/JP2023/033922
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English (en)
Japanese (ja)
Inventor
隆行 樋口
昌浩 岩崎
俊一 三島
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デンカ株式会社
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Publication of WO2024070814A1 publication Critical patent/WO2024070814A1/fr

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B14/00—Use of inorganic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of inorganic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
    • C04B14/02—Granular materials, e.g. microballoons
    • C04B14/04—Silica-rich materials; Silicates
    • C04B14/10—Clay
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B22/00—Use of inorganic materials as active ingredients for mortars, concrete or artificial stone, e.g. accelerators, shrinkage compensating agents
    • C04B22/06—Oxides, Hydroxides
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B22/00—Use of inorganic materials as active ingredients for mortars, concrete or artificial stone, e.g. accelerators, shrinkage compensating agents
    • C04B22/08—Acids or salts thereof
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B22/00—Use of inorganic materials as active ingredients for mortars, concrete or artificial stone, e.g. accelerators, shrinkage compensating agents
    • C04B22/08—Acids or salts thereof
    • C04B22/14—Acids or salts thereof containing sulfur in the anion, e.g. sulfides
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
    • C04B24/12—Nitrogen containing compounds organic derivatives of hydrazine
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • C04B28/02—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing hydraulic cements other than calcium sulfates
    • E—FIXED CONSTRUCTIONS
    • E21—EARTH OR ROCK DRILLING; MINING
    • E21D—SHAFTS; TUNNELS; GALLERIES; LARGE UNDERGROUND CHAMBERS
    • E21D11/00—Lining tunnels, galleries or other underground cavities, e.g. large underground chambers; Linings therefor; Making such linings in situ, e.g. by assembling
    • E21D11/04—Lining with building materials
    • E21D11/10—Lining with building materials with concrete cast in situ; Shuttering also lost shutterings, e.g. made of blocks, of metal plates or other equipment adapted therefor

Definitions

  • the present invention relates to a liquid quick-setting agent and sprayed concrete.
  • a method of spraying quick-setting concrete in which a quick-setting agent is mixed into the concrete, has been used to prevent the collapse of exposed ground during tunnel excavation, etc.
  • This method involves measuring and mixing the materials at a measuring plant installed at the excavation site to prepare the sprayed concrete, which is then pumped and mixed with quick-setting agent pumped in from the other side of the junction pipe, and sprayed onto the ground surface until a specified thickness is reached.
  • the set-accelerating agents used in the spraying method can be broadly classified into two types: powder set-accelerating agents whose main components are calcium aluminate or alkali metal aluminate, and liquid set-accelerating agents whose main components are alkali metal aluminate or aluminum sulfate.
  • liquid quick-setting additives have the problem of having lower quick-setting properties compared to powder quick-setting additives. Therefore, to improve quick-setting properties, measures have been taken to improve strength by increasing the sulfate ion concentration, as shown in Patent Document 1, for example.
  • liquid quick-setting agents with a high sulfate ion concentration can sometimes cause unstable precipitates to form in the liquid, the liquid to gel, or suspended particles to settle.
  • the solubility of aluminum sulfate in water is 27% by mass at 20°C, and this varies depending on the coexisting solutes and the liquid temperature.
  • liquid quick-setting agents that contain aluminum sulfate in excess of the solubility limit have poor long-term storage stability of about one month due to the settling of dispersed aluminum sulfate particles (dispersed particles), making it difficult to maintain the properties immediately after production.
  • the object of the present invention is to provide a liquid quick-setting agent that has excellent quick-setting properties, strength development, and long-term storage stability.
  • the present invention is as follows.
  • the liquid quick-setting admixture according to [1] having a viscosity at 30 ° C. of 200 to 3,000 mPa ⁇ s.
  • the present invention provides a liquid quick-setting agent that has excellent quick-setting properties, strength development, and storage stability.
  • the liquid quick-setting admixture according to this embodiment contains 9.0 to 15.0% aluminum calculated as Al2O3 , 22.0 to 35.0% sulfur calculated as SO3 , 0.5 to 2.0% by mass of clay minerals, and 0.5 to 5.0% by mass of amine compounds, assuming the mass of the liquid quick-setting admixture to be 100%.
  • the quick-setting property is insufficient, and if it exceeds 15.0%, the viscosity of the liquid quick-setting admixture increases, causing unstable delivery to the spray nozzle, which may result in reduced quick-setting property and strength development. From the viewpoint of further improving the quick-setting property, strength development, and storage stability, 9.5 to 14.5% is preferable, and 10.0 to 14.0% is even more preferable.
  • the aluminum concentration in terms of Al 2 O 3 in the liquid quick-setting admixture can be measured in accordance with the method described in JIS K1423, Aluminum Sulfate (Aluminum Sulfate).
  • the sulfur content is less than 22.0% in terms of SO3 , the quick-setting property is insufficient, and if it exceeds 35.0%, the viscosity of the liquid quick-setting admixture increases, the liquid delivery to the spray nozzle becomes unstable, and the quick-setting property and strength development may decrease. From the viewpoint of further improving the quick-setting property, strength development, and storage stability, 23.0 to 34.0% is preferable, and 24.0 to 33.0% is more preferable.
  • the sulfur concentration in terms of SO3 can be measured by ion chromatography or the like.
  • the liquid quick-setting admixture according to this embodiment further contains clay minerals such as bentonite, sepiolite, and attapulgite.
  • clay minerals such as bentonite, sepiolite, and attapulgite.
  • sepiolite which is a hydrated magnesium silicate with a unique chain structure, is more preferable.
  • the clay mineral content in the liquid quick-binding agent is 0.5 to 2.0%, preferably 0.7 to 1.8%, and more preferably 1.0 to 1.5%. By having the content of 0.5 to 2.0%, good storage stability can be ensured.
  • the average particle size of the clay mineral is preferably 0.5 to 20 ⁇ m, and more preferably 1 to 10 ⁇ m. The average particle size of the clay mineral can be measured by a laser diffraction method.
  • the clay mineral content can be measured by suction filtration using a membrane filter. Because the separated solid phase may contain aluminum compounds, it is necessary to thoroughly wash it with pure water to separate only the clay minerals that are poorly soluble in pure water.
  • the liquid quick-setting agent of this embodiment contains an amine compound from the viewpoint of good quick-setting ability and strength development.
  • amine compounds include ethanolamine, monoethanolamine, diethanolamine, triethanolamine, triisopropanol, diisopropylamine, etc.
  • diethanolamine is preferred from the viewpoint of better quick-setting ability and strength development.
  • the content of the amine compound in the liquid quick-setting admixture is 0.5 to 5.0%, preferably 1.0 to 4.0%, and more preferably 1.5 to 3.0%. By being 0.5 to 5.0%, better quick-setting properties and strength development can be easily obtained.
  • the content of the amine compound can be measured by high performance liquid chromatography or the like.
  • the Heywood mean particle diameter of dispersed particles is in the range of 3 to 30 ⁇ m.
  • the present inventors have found that the range of the Heywood average diameter of the dispersed particles, together with the concentration of each component described above, is important for the dispersion stability (storage stability) of the dispersed particles while improving the quick-setting property and strength development. That is, if the Heywood average diameter of the dispersed particles is less than 3 ⁇ m, the viscosity of the liquid quick-setting admixture increases, and the liquid delivery to the spray nozzle becomes unstable, which may result in a decrease in quick-setting property and strength development.
  • the Heywood average diameter of the dispersed particles is preferably 3 ⁇ m or more. If the Heywood average diameter of the dispersed particles exceeds 30 ⁇ m, any one of the storage stability, quick-setting property, and strength development is decreased.
  • the Heywood mean diameter is preferably from 3 to 25 ⁇ m, and more preferably from 5 to 20 ⁇ m.
  • the Heywood mean diameter of dispersed particles observed under an optical microscope using transmitted light is determined by analyzing the obtained particle diameter data using the image analysis type particle size distribution measurement software "Mac-View Ver. 4", measuring 300 Heywood diameters converted into the diameter of a circle having the same area as the selected particle, and averaging these values to obtain the mean diameter. Specifically, it is preferable to measure using the method described in the Examples.
  • the liquid quick-setting admixture of this embodiment is in a supersaturated state with aluminum sulfate, and the undissolved aluminum sulfate exists as dispersed particles.
  • the laser diffraction/scattering method measurement in a supersaturated state is impossible, and the concentration must be diluted, but this causes the undissolved aluminum sulfate to dissolve, making it impossible to measure the particle diameter accurately.
  • the Heywood average diameter makes it possible to more accurately measure the particle diameter of the dispersed particles in the liquid quick-setting admixture of this embodiment.
  • the Heywood mean diameter In order to adjust the Heywood mean diameter to 3 to 30 ⁇ m, it is necessary to apply a high shear force at a high speed as described below when mixing and stirring the raw material in a solvent (for example, water or a mixture of water and sulfuric acid). This makes it easier to obtain a good dispersion state with a Heywood mean diameter of 3 to 30 ⁇ m.
  • a solvent for example, water or a mixture of water and sulfuric acid.
  • the amount (concentration) and viscosity of the precipitated dispersed particles may also affect the average diameter. For example, the higher the Al2O3 - converted concentration or the SO3- converted concentration, the greater the amount of dispersed particles and the higher the viscosity, which can cause problems in stirring the liquid quick-setting additive and crushing the particles in the reaction vessel, resulting in a larger Heywood average diameter.
  • the viscosity of the liquid quick-setting admixture is preferably 200 to 3,000 mPa ⁇ s, and more preferably 500 to 2,500 mPa ⁇ s, from the viewpoints of preventing separation of the liquid quick-setting admixture, sending the liquid to the spray concrete nozzle, dispersing in concrete, and quick-setting of concrete.
  • a viscosity of 200 mPa ⁇ s or more suppresses separation of the liquid phase and the solid phase, and a viscosity of 3,000 mPa ⁇ s or less makes it easy to supply a fixed amount using a pump, and can improve dispersibility in concrete and quick-setting power.
  • the viscosity can be adjusted by adding the above-mentioned clay minerals, or can be adjusted by controlling the Heywood mean diameter.
  • the liquid quick-setting agent can contain various additives as long as they do not impair the effects of the present invention.
  • additives include nitric acid and its salts, formic acid and its salts, alkali, and fluorine, which are known to promote the setting and strength of cement.
  • the total alkali content R 2 O (R is an alkali metal) in the liquid quick-setting admixture is preferably 1.0% or less, more preferably 0.8% or less, and even more preferably 0.5% or less, from the viewpoint of worker safety. Alternatively, it may be 0% or more.
  • the total alkali content R 2 O in the liquid quick-setting admixture can be measured by atomic absorption spectrometry.
  • the total alkali content R 2 O can be adjusted by appropriately using raw materials having a low total alkali content R 2 O.
  • the active ingredient concentration of the liquid quick-setting admixture of the present embodiment is preferably 34 to 45%, and more preferably 36 to 43%, from the viewpoints of quick-setting property, strength development, and storage stability.
  • the term "effective component concentration” refers to the total concentration (%) of aluminum concentration in Al2O3 equivalent, sulfur concentration in SO3 equivalent, clay minerals, and amine compounds.
  • the term “effective component amount” refers to the total amount of aluminum in Al2O3 equivalent, sulfur in SO3 equivalent, clay minerals, and amine compounds.
  • the above liquid quick-setting agents can be obtained by appropriately selecting aluminum-containing raw materials or sulfur-containing raw materials such as aluminum sulfate, various alums, and aluminum hydroxide, and mixing and stirring these with any clay mineral or amine compound together with sulfuric acid, water, etc. at a temperature range of 20 to 80°C for 1 to 6 hours.
  • aluminum-containing raw materials or sulfur-containing raw materials such as aluminum sulfate, various alums, and aluminum hydroxide
  • a suitable stirring device is a high-shear mixer.
  • a high-shear mixer is a mixer in which a rotor attached to a rotating shaft rotates at high speed inside a precisely machined stirring head, and the solution and solids at the bottom of the tank are drawn into the stirring head by its strong suction effect, and the solution drawn into the stirring head is swung toward the outer periphery of the work head by the centrifugal force generated by the rotor, and the rotor tip blade and the inner edge of the stirring head create a precise clearance to produce a particle crushing effect.
  • the solution to which high shear force is applied at high speed is pushed outward from a window machined in the stirring head, and this circulation is repeated in the tank, which has the characteristic of enabling a high degree of homogenization of the solution.
  • the high-shear mixer for example, a high-shear batch mixer AX5 series manufactured by Silverson Corporation can be used.
  • the shape of the work head and the blade are also very important for controlling the particle size.
  • the mixer is not limited to a high shear mixer, and a general high speed mixer can also be used.
  • the rotor rotation speed is preferably 1,100 to 10,000 rpm, and more preferably 4,000 to 8,000 rpm.
  • the mixing time depends on the rotation speed, but is preferably about 60 to 200 minutes.
  • the Heywood mean diameter tends to become smaller as the rotation speed increases.
  • the shotcrete according to this embodiment contains the liquid quick-setting admixture of the present invention described above.
  • the liquid quick-setting admixture of the present invention may be used alone or in combination with a powder quick-setting admixture containing calcium aluminate as a main component.
  • Sprayed concrete actually uses cement
  • examples of the cement used in sprayed concrete include various types of Portland cement, such as normal, early strength, extra early strength, low heat, and medium heat, various mixed cements in which Portland cement is mixed with blast furnace slag, fly ash, or silica, filler cements in which limestone powder or finely powdered cooled blast furnace slag is mixed, and environmentally friendly cements (ecocement) made from municipal waste incineration ash and sewage sludge incineration ash.
  • Portland cement such as normal, early strength, extra early strength, low heat, and medium heat
  • various mixed cements in which Portland cement is mixed with blast furnace slag, fly ash, or silica
  • filler cements in which limestone powder or finely powdered cooled blast furnace slag is mixed
  • environmentally friendly cements ecocement
  • sprayed concrete uses aggregate, but there are no particular limitations on the aggregate, and it is preferable to use aggregate with low water absorption and high aggregate strength. There are no particular limitations on the maximum size of the aggregate, as long as it can be sprayed. River sand, mountain sand, sea sand, lime sand, and silica sand can be used as fine aggregate, and river gravel, mountain gravel, and lime gravel can be used as coarse aggregate, and crushed sand and crushed stone can also be used.
  • the amount of liquid quick-setting agent mixed should be such that the amount of active ingredient in the liquid quick-setting agent is 3 to 12 parts by mass, and more preferably 5 to 10 parts by mass, per 100 parts by mass of cement in the concrete.
  • the method of mixing the liquid quick-setting admixture with the cement-containing concrete is not particularly limited, and examples thereof include a method of mixing the liquid quick-setting admixture with the concrete using a mixing pipe such as a Y-shaped pipe, and a method of mixing the liquid quick-setting admixture with the concrete using a double pipe. After producing sprayed concrete using these methods, the concrete is sprayed onto an object to be sprayed.
  • High-speed mixer Three-one motor agitator. The rotation speed and agitation time were as shown in Table 1.
  • High shear mixer Silverson high shear batch mixer L5M-A, mixing head Emulsor Screen, rotation speed and mixing time were as shown in Table 1.
  • ⁇ Density> The sample was filled into a 100 ml measuring cylinder, the mass was measured, and the mass was divided by the volume to obtain the density.
  • ⁇ pH> The pH of the liquid quick-setting admixture was measured using a commercially available pH meter.
  • ⁇ Setting test/compressive strength test> The basic mix was 700 parts by mass of ordinary Portland cement and 2100 parts by mass of surface-dried sand, and the liquid quick-setting agent was added with 28 parts by mass of active ingredients ( 4.0 parts by mass per 100 parts by mass of cement) together with 350 parts by mass of water. The amount of water was adjusted taking into consideration the moisture content of the liquid quick-setting agent. After mixing for 10 seconds at low speed and 10 seconds at high speed, the mixture was molded and subjected to setting and compressive strength tests. The test was conducted in accordance with JIS R5201 "Physical Testing Methods for Cement" and measured the compressive strength at the initial and final setting times and at each age (12 hours, 1 day, 7 days, and 28 days). The test was conducted at 20°C. The results are shown in Table 1 below.
  • Clay mineral b Attapulgite (hydrated aluminum-magnesium silicate), average particle size 5 ⁇ m, commercially available product
  • Amine compound b Diisopropylamine, commercially available product
  • High-speed mixer Three-one motor agitator. The rotation speed and agitation time were as shown in Table 2.
  • High-shear mixer Silverson high-shear batch mixer L5M-A, mixing head Emulsor Screen, rotation speed and mixing time were as shown in Table 2.
  • the liquid quick-setting agent of the present invention can be suitably used for cement concrete that is sprayed onto exposed natural ground surfaces, such as road, railway, and waterway tunnels, as well as slopes, etc.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Civil Engineering (AREA)
  • Architecture (AREA)
  • Mining & Mineral Resources (AREA)
  • Dispersion Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Geology (AREA)
  • Curing Cements, Concrete, And Artificial Stone (AREA)
  • Lining And Supports For Tunnels (AREA)

Abstract

L'invention concerne un accélérateur liquide dans lequel sont incorporés ９,０ à １５,０% en masse en termes de Ａｌ２Ｏ３ d'un aluminium, ２２,０ à ３５,０% en masse en termes de ＳＯ３ d'un soufre, 0,５ à ２,０% en masse d'un minéraux argileux, et ０,５ à ５,０% en masse d'un composé à base d'amine. Le diamètre Heywood moyen de particules de dispersion d'après une observation au microscope optique mettant en œuvre un faisceau transmis, est compris entre ３ et ３０μｍ.
PCT/JP2023/033922 2022-09-27 2023-09-19 Accélérateur liquide, et béton projeté WO2024070814A1 (fr)

Applications Claiming Priority (2)

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JP2022153726A JP7453303B1 (ja) 2022-09-27 2022-09-27 液状急結剤、吹付けコンクリート
JP2022-153726 2022-09-27

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6140853A (ja) * 1984-07-31 1986-02-27 電気化学工業株式会社 セメント急結剤
JP2002053356A (ja) * 2000-08-03 2002-02-19 Denki Kagaku Kogyo Kk セメント急結剤
JP2014152058A (ja) * 2013-02-06 2014-08-25 Denki Kagaku Kogyo Kk 液体急結剤、それを用いたセメント組成物および吹付け工法
WO2014148523A1 (fr) * 2013-03-21 2014-09-25 電気化学工業株式会社 Agent à prise rapide liquide
JP2018030731A (ja) * 2016-08-22 2018-03-01 デンカ株式会社 液体急結剤、吹付け材料及びそれを用いた吹付け工法
CN111499248A (zh) * 2020-05-22 2020-08-07 山西海裕隆建材有限公司 一种中热低热水泥专用高性能无碱液体速凝剂及制备方法
WO2022097495A1 (fr) * 2020-11-09 2022-05-12 デンカ株式会社 Matériau mixte à prise rapide et matériau de pulvérisation

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6140853A (ja) * 1984-07-31 1986-02-27 電気化学工業株式会社 セメント急結剤
JP2002053356A (ja) * 2000-08-03 2002-02-19 Denki Kagaku Kogyo Kk セメント急結剤
JP2014152058A (ja) * 2013-02-06 2014-08-25 Denki Kagaku Kogyo Kk 液体急結剤、それを用いたセメント組成物および吹付け工法
WO2014148523A1 (fr) * 2013-03-21 2014-09-25 電気化学工業株式会社 Agent à prise rapide liquide
JP2018030731A (ja) * 2016-08-22 2018-03-01 デンカ株式会社 液体急結剤、吹付け材料及びそれを用いた吹付け工法
CN111499248A (zh) * 2020-05-22 2020-08-07 山西海裕隆建材有限公司 一种中热低热水泥专用高性能无碱液体速凝剂及制备方法
WO2022097495A1 (fr) * 2020-11-09 2022-05-12 デンカ株式会社 Matériau mixte à prise rapide et matériau de pulvérisation

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