WO2021056934A1 - Matériau de microsphères à absorption d'eau élevée à durcissement interne de béton armé et son procédé de préparation - Google Patents

Matériau de microsphères à absorption d'eau élevée à durcissement interne de béton armé et son procédé de préparation Download PDF

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Publication number
WO2021056934A1
WO2021056934A1 PCT/CN2020/072209 CN2020072209W WO2021056934A1 WO 2021056934 A1 WO2021056934 A1 WO 2021056934A1 CN 2020072209 W CN2020072209 W CN 2020072209W WO 2021056934 A1 WO2021056934 A1 WO 2021056934A1
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WIPO (PCT)
Prior art keywords
reinforced concrete
stirring
microsphere material
internal curing
superabsorbent
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PCT/CN2020/072209
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English (en)
Chinese (zh)
Inventor
何锐
谈亚文
陈华鑫
房建宏
薛成
王振军
段德峰
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长安大学
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Publication of WO2021056934A1 publication Critical patent/WO2021056934A1/fr

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    • 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
    • C04B14/06—Quartz; Sand
    • C04B14/062—Microsilica, e.g. colloïdal silica
    • 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
    • C04B24/24—Macromolecular compounds
    • C04B24/26—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • C04B24/2641—Polyacrylates; Polymethacrylates
    • 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
    • C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
    • C04B40/0028—Aspects relating to the mixing step of the mortar preparation
    • C04B40/0039—Premixtures of ingredients
    • C04B40/0046—Premixtures of ingredients characterised by their processing, e.g. sequence of mixing the ingredients when preparing the premixtures

Definitions

  • the invention relates to the field of building materials, to concrete internal curing materials, in particular to a reinforced concrete internal curing high water-absorbing microsphere material and a preparation method.
  • SAP as a new type of internal curing material, with its unique water absorption and water retention properties, acts as a reservoir inside the concrete, accompanied by the difference in humidity, pressure and pH value between the inside and outside of SAP particles during the hydration process of cement It will gradually release the water to maintain the internal relative humidity of the cement-based composite material at a higher level. The subsequent hydration of the cementitious material will not stop due to lack of water.
  • the early self-drying and shrinkage cracking phenomenon of the cement-based material It can be effectively relieved and controlled, and the negative impact on other properties of concrete is much lower than the former. Therefore, SAP has become an internal maintenance material that has been continuously researched and applied in recent years. However, due to the limited current technology, the influence of SAP on the strength of concrete is very controversial. In addition, after SAP is incorporated, the workability of concrete becomes worse, and it cannot be effectively controlled during the hydration process of cement concrete. The release rate of water.
  • the purpose of the present invention is to provide a reinforced concrete internal curing superabsorbent microsphere material and a preparation method, which solves the problem of the existing absorbent material, which causes the strength of concrete to decrease on the basis of ensuring the water absorption performance.
  • the present invention adopts the following technical solutions to achieve:
  • a reinforced concrete internal curing super absorbent microsphere material which is characterized in that it is made of the following raw materials: nano silica, chitosan, glutaraldehyde, acacia, methacrylic acid, glacial acetic acid, cumene Hydrogen oxide, ferrous chloride and sodium ethoxide.
  • the invention also has the following technical features:
  • the average particle size of the nano-silica is 20 nm.
  • the present invention also protects a method for preparing the reinforced concrete internal curing superabsorbent microsphere material, which adopts the above-mentioned formula of the reinforced concrete internal curing superabsorbent microsphere material.
  • the method specifically includes the following steps:
  • Step 1 Weigh the ingredients according to the formula weight
  • Step 2 Disperse nano-silica in water, configure it into a nano-silica suspension with a mass concentration of 3%, and stir;
  • Step 3 Dilute glacial acetic acid with water into a dilute solution of glacial acetic acid with a mass concentration of 1%;
  • Step 4 Mix chitosan and gum arabic, add the dilute solution of glacial acetic acid with a mass concentration of 1% prepared in step 3, and stir to form a dilute acid solution A of chitosan and gum arabic;
  • Step 5 add methacrylic acid to water, configure it as a dilute solution with a mass concentration of 15%, add sodium ethoxide and cool to room temperature, while continuing to stir, add cumene hydrogen peroxide and ferrous chloride to fully dissolve Then the mixture B is prepared;
  • Step 6 add cyclopentane and Span 80 to the container, stir at constant temperature to form oil phase C;
  • Step 7 adding the nano-silica suspension prepared in step 2 to oil phase C, protecting with inert gas, stirring at a constant temperature, and continuously stirring, adding the dilute acid solution A and glutaraldehyde prepared in step 4, liters Mix liquid D with rapid stirring;
  • Step 8 adding the mixture B prepared in step 5 to the mixed solution D prepared in step 7 and reacting to obtain a compound E;
  • step 9 the composite E prepared in step 8 is taken out, washed with a solvent, and after the solvent is volatilized, a reinforced concrete inner curing superabsorbent microsphere material is prepared.
  • the stirring adopts magnetic stirring, and the stirring time is 20 minutes.
  • step 4 the stirring adopts magnetic stirring, and the stirring time is 30 minutes.
  • step 6 the constant temperature is a constant temperature water bath environment of 30°C; the stirring is 200 r/min for 20 minutes.
  • Span 80 is 5% to 8% of the mass fraction of cyclopentane.
  • step 7 the inert gas protection is nitrogen; the constant temperature is 40°C constant temperature water bath environment; the stirring is 200r/min stirring for 10min; the rising speed stirring is 400r/min stirring for 30min .
  • the temperature is controlled between 40°C and 45°C during the whole process of the reaction, and the reaction time is 6h.
  • step 9 the solvent is absolute ethanol, and the washing is performed 3 to 5 times.
  • the present invention has the following technical effects:
  • the nano-silica component in the reinforced concrete internal curing superabsorbent microspheres provided by the present invention has a spherical, flocculent and net-like quasi-particle structure, which can not only provide concrete internal curing superabsorbent microspheres
  • the framework of nano-silica has pozzolanic activity and chemically reacts with calcium hydroxide (CH) to generate additional calcium silicate hydrate (CSH).
  • CSH is the main component to enhance the strength and density of cement-based hardened paste. Due to its pozzolanic activity, silica particles reduce the content of Ca(OH) 2 in the slurry and its grain size.
  • the nucleation effect promotes the formation of CSH gels from C 3 S and C 2 S, and the filling effect makes it as a nano-filler. Fill the gaps between CSH gels. Therefore, the pozzolanic activity, nucleation effect and filling effect of nano-silica can promote the early hydration of cement, improve the transition zone between cement paste and aggregate, modify the internal microstructure of cement-based materials, reduce porosity, and improve mechanical properties .
  • the chitosan molecule in the reinforced concrete internal curing superabsorbent microspheres provided by the present invention is a natural polymer with active amino groups in the structure and high chemical activity.
  • the structure contains a large number of hydrophilic groups, which will swell to a certain extent in a solution with high water content, which can not only provide a network skeleton for the graft polymerization of organic monomers during the synthesis process of superabsorbent microspheres for curing in concrete, but also Improve the degree of polymerization of the polymerization reaction and increase the liquid absorption rate of the internally cured super absorbent microspheres.
  • Glutaraldehyde can undergo a cross-linking reaction with glutaraldehyde, and the cross-linking reaction mainly occurs between molecules and also occurs within molecules.
  • the cross-linked product is stable and generally not easy to dissolve.
  • chitosan has good emulsification, film-forming properties and spheroidizing properties, which can effectively mention the synthesis effect of curing superabsorbent microspheres in concrete.
  • the organic monomer methacrylic acid in the reinforced concrete internal curing superabsorbent microspheres provided by the present invention is continuously grafted and polymerized, and the nano-silica is continuously filled and packaged, which can significantly improve the internal curing material Aspiration rate.
  • the excellent liquid absorption and storage effects can more effectively adjust the humidity distribution inside the concrete to a certain extent, ensure the water demand of the concrete in the hydration process, and promote the secondary cement and mineral admixtures. Hydration.
  • the second time can effectively improve the hydration degree of cement-based materials and optimize the internal pores of concrete. Therefore, the preparation of reinforced concrete internal curing superabsorbent microspheres made by the present invention greatly contributes to the strength, durability and service life of cement concrete.
  • Fig. 1 is an SEM image of the reinforced concrete internal curing superabsorbent microsphere material of the present invention.
  • Span 80 namely sorbitan monooleate.
  • the average particle size of nano silica is 20nm, the silica content is ⁇ 99%, the specific surface area is 150-200m 2 /g, and the pH is 4-7.
  • the chitosan is food grade, and the degree of deacetylation is 80% to 90%.
  • This example provides a reinforced concrete internal curing superabsorbent microsphere material, in parts by weight, including the following raw materials: 8% nano silica, 20% chitosan, 30% glutaric acid Aldehydes, 5% gum arabic, 25% methacrylic acid, 3.3% glacial acetic acid, 0.5% cumene hydrogen peroxide, 0.2% ferrous chloride, 8% sodium ethoxide.
  • Step 1 Weigh the ingredients according to the formula weight
  • Step 2 Disperse nano-silica in water, configure it into a nano-silica suspension with a mass concentration of 3%, and stir;
  • the stirring adopts magnetic stirring, and the stirring time is 20 minutes.
  • Step 3 Dilute glacial acetic acid with water into a dilute solution of glacial acetic acid with a mass concentration of 1%;
  • Step 4 Mix chitosan and gum arabic, add the dilute solution of glacial acetic acid with a mass concentration of 1% prepared in step 3, and stir to form a dilute acid solution A of chitosan and gum arabic;
  • step 4 the stirring adopts magnetic stirring, and the stirring time is 30 minutes.
  • Step 5 add methacrylic acid to water, configure it as a dilute solution with a mass concentration of 15%, add sodium ethoxide and cool to room temperature, while continuing to stir, add cumene hydrogen peroxide and ferrous chloride to fully dissolve Then the mixture B is prepared;
  • Step 6 add cyclopentane and Span 80 to the container, stir at constant temperature to form oil phase C;
  • step 6 the constant temperature is a constant temperature water bath environment of 30°C; the stirring is 200 r/min for 20 minutes.
  • Span 80 is 5% to 8% of the mass fraction of cyclopentane.
  • Step 7 adding the nano-silica suspension prepared in step 2 to oil phase C, protecting with inert gas, stirring at a constant temperature, and continuously stirring, adding the dilute acid solution A and glutaraldehyde prepared in step 4, liters Mix liquid D with rapid stirring;
  • step 7 the inert gas protection is nitrogen; the constant temperature is 40°C constant temperature water bath environment; the stirring is 200r/min stirring for 10min; the rising speed stirring is 400r/min stirring for 30min .
  • Step 8 adding the mixture B prepared in step 5 to the mixed solution D prepared in step 7 and reacting to obtain a compound E;
  • the temperature is controlled between 40°C and 45°C during the whole process of the reaction, and the reaction time is 6h.
  • step 9 the composite E prepared in step 8 is taken out, washed with a solvent, and after the solvent is volatilized, a reinforced concrete inner curing superabsorbent microsphere material is prepared.
  • step 9 the solvent is absolute ethanol, and the washing is performed 3 to 5 times.
  • the SEM image of the reinforced concrete internal curing superabsorbent microsphere material prepared in this example is shown in FIG. 1.
  • the mixing amount is 0.2% of the cement mixing amount.
  • the 7d compressive strength of the resulting concrete is the benchmark concrete strength. 110%, 28d compressive strength is 123% of the benchmark concrete strength, the fluidity of 60min concrete is increased by 18% compared to the benchmark concrete, and the autogenous shrinkage of 28d concrete is reduced by 65% compared to the benchmark concrete.
  • This example provides a reinforced concrete internal curing super absorbent microsphere material, in parts by weight, including the following raw materials: 9% nano silica, 18% chitosan, 25% glutaric acid Aldehydes, 4.4% gum arabic, 30% methacrylic acid, 5% glacial acetic acid, 0.4% cumene hydrogen peroxide, 0.2% ferrous chloride, 8% sodium ethoxide.
  • the preparation method of the reinforced concrete inner-curing superabsorbent microsphere material of this embodiment is the same as the preparation method of the reinforced concrete inner-curing superabsorbent microsphere material in Example 1.
  • the SEM image of the reinforced concrete internal curing superabsorbent microsphere material prepared in this example is shown in FIG. 1.
  • the mixing amount is 1.8% of the cement mixing amount
  • the 7d compressive strength of the resulting concrete is the benchmark concrete strength 108%
  • 28d compressive strength is 123% of the benchmark concrete strength
  • the fluidity of 60min concrete is increased by 20% compared to the benchmark concrete
  • the autogenous shrinkage of 28d concrete is reduced by 60% compared to the benchmark concrete.
  • This example provides a reinforced concrete internal curing superabsorbent microsphere material, in parts by weight, including the following raw materials: 10% nano silica, 19% chitosan, 28% glutaric acid Aldehydes, 4% gum arabic, 27% methacrylic acid, 3.3% glacial acetic acid, 0.5% cumene hydrogen peroxide, 0.2% ferrous chloride, 8% sodium ethoxide.
  • the preparation method of the reinforced concrete inner-curing superabsorbent microsphere material of this embodiment is the same as the preparation method of the reinforced concrete inner-curing superabsorbent microsphere material in Example 1.
  • the SEM image of the reinforced concrete internal curing superabsorbent microsphere material prepared in this example is shown in FIG. 1.
  • the mixing amount is 0.25% of the cement mixing amount
  • the 7d compressive strength of the resulting concrete is the benchmark concrete strength 112%
  • 28d compressive strength is 128% of the benchmark concrete strength
  • the fluidity of 60min concrete is increased by 30% relative to the benchmark concrete
  • the autogenous shrinkage of the 28d concrete is reduced by 69% relative to the benchmark concrete.
  • This example provides a reinforced concrete internal curing superabsorbent microsphere material, in parts by weight, including the following raw materials: 10% nano-silica, 15% chitosan, 30% glutaric acid Aldehydes, 4.4% gum arabic, 30% methacrylic acid, 5% glacial acetic acid, 0.5% cumene hydrogen peroxide, 0.1% ferrous chloride, 5% sodium ethoxide.
  • the preparation method of the reinforced concrete inner-curing superabsorbent microsphere material of this embodiment is the same as the preparation method of the reinforced concrete inner-curing superabsorbent microsphere material in Example 1.
  • the SEM image of the reinforced concrete internal curing superabsorbent microsphere material prepared in this example is shown in FIG. 1.
  • the mixing amount is 0.3% of the cement mixing amount
  • the 7d compressive strength of the resulting concrete is the benchmark concrete strength 102%
  • 28d compressive strength is 130% of the benchmark concrete strength
  • the fluidity of 60min concrete is increased by 35% relative to the benchmark concrete
  • the autogenous shrinkage of 28d concrete is reduced by 70% compared to the benchmark concrete.
  • the high-absorbent microspheres cured in the strong concrete can significantly increase the compressive strength of the concrete.
  • the 28d compressive strength is more than 120% of the benchmark concrete strength.
  • the fluidity of 60min concrete has also been significantly improved.
  • the internal curing material can also greatly reduce the autogenous shrinkage of concrete. Therefore, the strong concrete internal curing superabsorbent microspheres of the present invention have good applicability, can effectively solve the problems in the current concrete curing process, and have broad application prospects.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Civil Engineering (AREA)
  • Manufacturing Of Micro-Capsules (AREA)
  • Curing Cements, Concrete, And Artificial Stone (AREA)

Abstract

La présente invention concerne un matériau de microsphères à absorption d'eau élevée à durcissement interne de béton armé et un procédé de préparation de celui-ci. Le matériau de microsphères est préparé à partir des matières premières suivantes : nanosilice, chitosane, glutaraldéhyde, gomme arabique, acide méthacrylique, acide acétique glacial, hydroperoxyde d'isopropylbenzène, chlorure ferreux et éthoxyde de sodium. Celui-ci modifie la microstructure à l'intérieur d'un matériau à base de ciment en améliorant une région de transition entre une pâte de ciment et un agrégat, de sorte que la porosité est réduite et les propriétés mécaniques sont améliorées.
PCT/CN2020/072209 2019-09-23 2020-01-15 Matériau de microsphères à absorption d'eau élevée à durcissement interne de béton armé et son procédé de préparation WO2021056934A1 (fr)

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CN201910898836.0A CN110606690B (zh) 2019-09-23 2019-09-23 增强型混凝土内养护高吸水微球材料及制备方法

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CN110606690B (zh) * 2019-09-23 2020-06-09 长安大学 增强型混凝土内养护高吸水微球材料及制备方法
CN113667061B (zh) * 2021-08-24 2023-06-02 北京建筑材料科学研究总院有限公司 一种吸水树脂及其制备方法与应用
CN117756459A (zh) * 2023-12-25 2024-03-26 万特福建筑构件有限公司 一种绿色环保混凝土及其制备方法

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CN103408778A (zh) * 2013-07-30 2013-11-27 中国石油大学(华东) 一种亲水性包裹的吸水树脂微球及其制备方法
CN103554331A (zh) * 2013-11-05 2014-02-05 中海油能源发展股份有限公司惠州石化分公司 一种反相悬浮聚合制备聚丙烯酸高吸水性树脂微球的方法
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CN110606690A (zh) * 2019-09-23 2019-12-24 长安大学 增强型混凝土内养护高吸水微球材料及制备方法

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