WO2022203641A2 - Production method of geopolymer concrete - Google Patents

Production method of geopolymer concrete Download PDF

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Publication number
WO2022203641A2
WO2022203641A2 PCT/TR2022/050270 TR2022050270W WO2022203641A2 WO 2022203641 A2 WO2022203641 A2 WO 2022203641A2 TR 2022050270 W TR2022050270 W TR 2022050270W WO 2022203641 A2 WO2022203641 A2 WO 2022203641A2
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Prior art keywords
slag
geopolymer
production method
mixture
concrete
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PCT/TR2022/050270
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French (fr)
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WO2022203641A3 (en
Inventor
Nihat KABAY
Hakan OZKAN
Nausad MIYAN
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Yildiz Teknik Universitesi
Oyak Beton Sanayi Ve Ticaret Anonim Sirketi
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Publication of WO2022203641A2 publication Critical patent/WO2022203641A2/en
Publication of WO2022203641A3 publication Critical patent/WO2022203641A3/en

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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
    • 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
    • C04B28/006—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 mineral polymers, e.g. geopolymers of the Davidovits type
    • 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
    • C04B28/24—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 alkyl, ammonium or metal silicates; containing silica sols
    • C04B28/26—Silicates of the alkali metals
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P40/00—Technologies relating to the processing of minerals
    • Y02P40/10—Production of cement, e.g. improving or optimising the production methods; Cement grinding
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00—Technologies for solid waste management
    • Y02W30/50—Reuse, recycling or recovery technologies
    • Y02W30/91—Use of waste materials as fillers for mortars or concrete

Definitions

  • This invention relates to the production of geopolymer concrete using blast furnace and basic oxygen furnace slags generated during iron and steel production.
  • BFS blast furnace slag
  • BOF basic oxygen furnace
  • the object of this invention is to develop a method that enables the production of geopolymer concrete by using slags originating from blast furnace and basic oxygen furnace generated during iron and steel production.
  • Another object of this invention is to develop a method that enables the use of BOF slag as a binder component, which is generally stored in waste sites and poses a significant environmental problem, in the production of geopolymer concrete.
  • Another object of this invention is to develop a method that enables the production of geopolymer concrete that does not require processes such as thermal curing, water curing, and steam curing.
  • Another object of the invention is to develop a geopolymer concrete produced from slag from blast furnace and basic oxygen furnace.
  • geopolymer concrete of the invention basically the mixture of blast furnace slag generated during iron production and basic oxygen furnace slag generated during steel production is mixed with alkali activator. At least one of aqueous sodium hydroxide and potassium hydroxide and sodium silicate solution are used as alkali activators. According to this method, geopolymer concretes with high compressive strength can be obtained without applying processes such as thermal curing, water curing, and steam curing.
  • the blast furnace slag content varies depending on the ore, fuel and flux content and the details of the process.
  • this slag is rich in oxides of mainly flux-derived elements such as silica, calcium oxide and aluminum oxide.
  • the BOF slag content also varies depending on the loaded iron and flux content and the details of the pre-treatment and oxidation processes. As a result of the oxidation of some of the iron together with the undesirable substances in the loaded iron, this slag contains various metal oxides, especially various iron (III) oxide, as well as calcium oxide originating from flux.
  • the BOF slag used for the realization of the invention may be weathered in the atmospheric conditions and/or not weathered.
  • the steps of the production method of the geopolymer concrete of the invention includes the steps of preparing a slag mixture by mixing blast furnace slag and BOF slag, preparing an aqueous solution containing sodium hydroxide or potassium hydroxide and sodium silicate, mixing the slag mixture, the solution and fine and coarse aggregate.
  • the step of pouring the mixture of the slag mixture, solution and aggregate into a mold and keeping in the mold is also applied.
  • the geopolymer precast concrete is obtained.
  • the mixture is cured without any special process during its aging.
  • the mixture is kept in the mold for a certain period of time, it can also be kept in the outdoor environment for a certain period of time.
  • reinforcements are also placed in the mold prior to pouring the mixture into the mold.
  • the step of grinding at least one of the blast furnace slag and basic oxygen furnace slag can also be applied before the step of preparing the slag mixture.
  • the fineness of the BOF slag positively affects the reactivity of this material in the geopolymer binder and its contribution to the mechanical properties.
  • the diameter of 50% of the BOF slag particles may be smaller than a value between 10 and 60 pm.
  • blast furnace slag with a Blaine specific surface of 5000 ⁇ 500 cm 2 /g and BOF slag, in which the largest particle diameter is less than 200 pm and the diameter of 50% of the particles are less than a value between 10 and 50 pm, are used.
  • the step of drying at least one of the blast furnace slag and BOF slag can also be applied. This step is applicable where stored slag, particularly BOF slag, needs to be dehumidified.
  • the solution is prepared comprising a slag mixture containing 20% to 60% BOF slag by volume and sodium hydroxide with a molarity of 4 to 10 M and sodium silicate with a silica modulus of 0.8 to 1.6.
  • Natural sand with a particle diameter of less than 2 mm and crushed sand with a particle diameter of less than 4 mm can be used as fine aggregate, and crushed stone aggregate in the range of 4 and 11.2 mm and 11.2 and 22.4 mm as coarse aggregate.
  • natural sand and/or crushed sand in the range of 0 and 4 mm can be used as fine aggregate, and in the range of 4 and 63 mm as coarse aggregate.
  • the largest particle size of the coarse aggregate can be increased depending on the mold in which the concrete will be poured and the reinforcement ratio.
  • the solution / slag mixture is mixed at a ratio between 0.30 and 0.50 by weight.
  • the aggregate ratio is adjusted so that the binder consisting of a mixture of solution and slag is 300 to 500 kg per cubic meter.
  • a superplasticizer can be added to the mixture at a ratio between 0.5% and 2.0% by weight of the binder.
  • the tests were also carried out with concrete samples that were kept for certain periods. During these tests, the slags, the contents of which are given in Table 1, were used. Table 1 - Chemical compositions of blast furnace slag and basic oxygen furnace slag
  • the samples were prepared for the tests such that the slag mixture contains 10% to 90% BOF slag by volume and the solution comprises a sodium hydroxide with a molarity of 4 to 14 M and sodium silicate with a silica modulus of 0.6 to 2.5, a binder with a solution / slag mixture ratio of 0.20 to 0.60 by weight and natural sand with a particle diameter of less than 2 mm and crushed sand with a particle diameter of less than 4 mm as fine aggregate, crushed stone aggregate in the range of 4 and 11.2 mm and 11.2 and 22.4 mm as coarse aggregate and the amount of slag mixture as binder is 200 to 600 kg per cubic meter.
  • the solution comprises a sodium hydroxide with a molarity of 4 to 14 M and sodium silicate with a silica modulus of 0.6 to 2.5, a binder with a solution / slag mixture ratio of 0.20 to 0.60 by weight and natural sand with a particle diameter of less than 2 mm and crushed sand
  • the invention paved the way for the production of geopolymer concretes with properties comparable to concretes obtained from Portland cement by using sodium hydroxide or potassium hydroxide and sodium silicate as activators of blast furnace slag and BOF slag, which are wastes of the iron and steel industry, without requiring special curing processes.
  • the comparison of the compressive strength of the geopolymer concretes according to the invention with the concrete and geopolymer concretes known in the prior art can also be seen in Table 2.

Abstract

This invention relates to the production of geopolymer concrete using blast furnace and basic oxygen furnace slags generated during iron and steel production. With this invention, geopolymer concretes that do not require processes such as thermal curing, water curing, steam curing and showing high compressive strength can be produced. With the invention, it is possible to use basic oxygen furnace slag, which is a serious waste, as a geopolymer binder material and to reduce the environmental and economic problems it causes. The concrete obtained by the invention has mechanical properties comparable to the concrete obtained with Portland cement. Geopolymer ready-mixed concrete and geopolymer precast concrete obtained by the invention are also disclosed.

Description

PRODUCTION METHOD OF GEOPOLYMER CONCRETE
Technical Field
This invention relates to the production of geopolymer concrete using blast furnace and basic oxygen furnace slags generated during iron and steel production.
Prior Art
There are various solutions and studies for the evaluation of blast furnace slag (BFS) and basic oxygen furnace (BOF) slag, which are wastes of the iron and steel industry. The blast furnace slag is among the inputs of cement production. On the other hand, BOF slag is used in cement production and can also be used as aggregate, however, it can be used in limited application areas such as road aggregate and railway ballast, since it causes cracks in the mortar or concrete it is used together with due to expansion. Therefore, most of the generated BOF slag is disposed of.
Since a large amount of fossil fuel is consumed during its production and high carbon dioxide emissions are realized, there is a need to develop concrete production from alternative materials to cement. For this, geopolymers are particularly emphasized. Some studies are carried out on the use of blast furnace slag or BOF slag in the production of geopolymer concrete. The widespread use of such concretes requires that they have at least similar strength to concretes obtained from Portland cement.
Lee et al. (2020) [1] added BOF slag as aggregate to the geopolymer matrix obtained from fly ash and BFS and experimentally determined that the negative expansion effects that can be caused by BOF slag could be eliminated.
In the study where they used fly ash and BFS as binders, Bellum et al. (2019) [2] combined these two materials at different ratios and activated them with sodium hydroxide and sodium silicate solution (sodium silicate / sodium hydroxide ratio was taken as 2,5), and the prepared concrete samples were cured under ambient conditions until the day 28. The compressive strength of the concrete samples varied between about 3 MPa and 38 MPa, and the modulus of elasticity varied between about 13300 MPa and 20200 MPa on the day 28.
In the study where they used fly ash and BFS as binders, Reddy et al. (2018) [3] combined these two materials at different ratios and activated them with sodium hydroxide and sodium silicate solution, and the sodium hydroxide molarity was taken as 14 M and the sodium silicate / sodium hydroxide ratio as 1,5. The concrete samples were cured under ambient conditions, and the compressive strength was determined at 28 and 56 days. According to the test results, it was determined that the compressive strength varied between about 33 MPa and 66 MPa at 28 days, and between 35 MPa and 68 MPa at 56 days.
In the study where they used fly ash and slag separately, Farhan et al. (2019) [4] used sodium hydroxide and sodium silicate as alkali activators, produced normal strength and high strength geopolymer concretes and compared the test results with Portland cement concrete.
The Objects of the Invention
The object of this invention is to develop a method that enables the production of geopolymer concrete by using slags originating from blast furnace and basic oxygen furnace generated during iron and steel production.
Another object of this invention is to develop a method that enables the use of BOF slag as a binder component, which is generally stored in waste sites and poses a significant environmental problem, in the production of geopolymer concrete.
Another object of this invention is to develop a method that enables the production of geopolymer concrete that does not require processes such as thermal curing, water curing, and steam curing.
Another object of this invention is to develop a method that enables the production of geopolymer concrete with high compressive strength. It is aimed that the produced geopolymer concretes will exhibit strength at least comparable to the concretes obtained from Portland cement. Another object of this invention is to develop a method that enables the production of geopolymer concretes suitable for various engineering applications and which can be used in the ready-mixed concrete and precast concrete industry.
Another object of the invention is to develop a geopolymer concrete produced from slag from blast furnace and basic oxygen furnace.
Detailed Description of the Invention
According to production method of the geopolymer concrete of the invention, basically the mixture of blast furnace slag generated during iron production and basic oxygen furnace slag generated during steel production is mixed with alkali activator. At least one of aqueous sodium hydroxide and potassium hydroxide and sodium silicate solution are used as alkali activators. According to this method, geopolymer concretes with high compressive strength can be obtained without applying processes such as thermal curing, water curing, and steam curing.
The blast furnace slag content varies depending on the ore, fuel and flux content and the details of the process. As a result of the reduction of iron oxides in the ore content, this slag is rich in oxides of mainly flux-derived elements such as silica, calcium oxide and aluminum oxide.
The BOF slag content also varies depending on the loaded iron and flux content and the details of the pre-treatment and oxidation processes. As a result of the oxidation of some of the iron together with the undesirable substances in the loaded iron, this slag contains various metal oxides, especially various iron (III) oxide, as well as calcium oxide originating from flux. The BOF slag used for the realization of the invention may be weathered in the atmospheric conditions and/or not weathered.
The steps of the production method of the geopolymer concrete of the invention includes the steps of preparing a slag mixture by mixing blast furnace slag and BOF slag, preparing an aqueous solution containing sodium hydroxide or potassium hydroxide and sodium silicate, mixing the slag mixture, the solution and fine and coarse aggregate.
As a result of these steps, ready-mixed concrete to be poured in the usage area is obtained. The geopolymer ready-mixed concrete obtained according to the invention is cured without any special process.
In an embodiment of the invention, after the mixing step of the slag mixture, solution and fine and coarse aggregate, the step of pouring the mixture of the slag mixture, solution and aggregate into a mold and keeping in the mold is also applied. As a result of this step, the geopolymer precast concrete is obtained. The mixture is cured without any special process during its aging. After the mixture is kept in the mold for a certain period of time, it can also be kept in the outdoor environment for a certain period of time. Preferably, reinforcements are also placed in the mold prior to pouring the mixture into the mold.
Depending on the initial particle sizes of the slags to be used, the step of grinding at least one of the blast furnace slag and basic oxygen furnace slag can also be applied before the step of preparing the slag mixture. The fineness of the BOF slag positively affects the reactivity of this material in the geopolymer binder and its contribution to the mechanical properties. The diameter of 50% of the BOF slag particles may be smaller than a value between 10 and 60 pm. In a preferred embodiment of the invention, blast furnace slag with a Blaine specific surface of 5000±500 cm2/g and BOF slag, in which the largest particle diameter is less than 200 pm and the diameter of 50% of the particles are less than a value between 10 and 50 pm, are used.
Before preparing the slag mixture, the step of drying at least one of the blast furnace slag and BOF slag can also be applied. This step is applicable where stored slag, particularly BOF slag, needs to be dehumidified.
In a preferred embodiment of the invention, the solution is prepared comprising a slag mixture containing 20% to 60% BOF slag by volume and sodium hydroxide with a molarity of 4 to 10 M and sodium silicate with a silica modulus of 0.8 to 1.6. Natural sand with a particle diameter of less than 2 mm and crushed sand with a particle diameter of less than 4 mm can be used as fine aggregate, and crushed stone aggregate in the range of 4 and 11.2 mm and 11.2 and 22.4 mm as coarse aggregate. In the concrete mixture, depending on the mold dimensions and concrete volume; natural sand and/or crushed sand in the range of 0 and 4 mm can be used as fine aggregate, and in the range of 4 and 63 mm as coarse aggregate. The largest particle size of the coarse aggregate can be increased depending on the mold in which the concrete will be poured and the reinforcement ratio.
In this embodiment of the invention, the solution / slag mixture is mixed at a ratio between 0.30 and 0.50 by weight. On the other hand, the aggregate ratio is adjusted so that the binder consisting of a mixture of solution and slag is 300 to 500 kg per cubic meter. In order for the concrete to have sufficient workability, that is, corresponding to a slump value between 10 and 25 cm, a superplasticizer can be added to the mixture at a ratio between 0.5% and 2.0% by weight of the binder. In order to evaluate the effectiveness of the method of the invention and the geopolymer concrete obtained by this method, the tests were also carried out with concrete samples that were kept for certain periods. During these tests, the slags, the contents of which are given in Table 1, were used. Table 1 - Chemical compositions of blast furnace slag and basic oxygen furnace slag
Figure imgf000006_0001
Figure imgf000007_0001
The samples were prepared for the tests such that the slag mixture contains 10% to 90% BOF slag by volume and the solution comprises a sodium hydroxide with a molarity of 4 to 14 M and sodium silicate with a silica modulus of 0.6 to 2.5, a binder with a solution / slag mixture ratio of 0.20 to 0.60 by weight and natural sand with a particle diameter of less than 2 mm and crushed sand with a particle diameter of less than 4 mm as fine aggregate, crushed stone aggregate in the range of 4 and 11.2 mm and 11.2 and 22.4 mm as coarse aggregate and the amount of slag mixture as binder is 200 to 600 kg per cubic meter. After these samples were kept in the molds for 24 hours, they were taken out of the molds and kept at ambient conditions of 60±20% relative humidity and 22±10°C for certain periods. Compression tests were carried out on the samples that were kept for 3, 7, 14 and 28 days and their compressive strength, modulus of elasticity and Poisson’s ratio values are given in Table 2.
The invention paved the way for the production of geopolymer concretes with properties comparable to concretes obtained from Portland cement by using sodium hydroxide or potassium hydroxide and sodium silicate as activators of blast furnace slag and BOF slag, which are wastes of the iron and steel industry, without requiring special curing processes. The comparison of the compressive strength of the geopolymer concretes according to the invention with the concrete and geopolymer concretes known in the prior art can also be seen in Table 2.
Table 2 - Compressive strengths, modulus of elasticity and poisson’s ratios of concrete and geopolymer concretes measured at different ages according to the invention and prior art
Figure imgf000008_0001
References
[1] Lee W-H, Cheng T-W, Lin K-Y, Lin K-L, Wu C-C, Tsai C-T. Geopolymer Technologies for Stabilization of Basic Oxygen Furnace Slags and Sustainable Application as Construction Materials. Sustainability. 2020; 12(12):5002.
[2] Bellum, Ramamohana Reddy & Muniraj, Karthikeyan & Madduru, Sri Rama. (2019). Investigation on modulus of elasticity of fly ash-ground granulated blast furnace slag blended geopolymer concrete. Materials Today: Proceedings. 27.
[3] Srinivasula Reddy, Maddula & Dinakar, P. & Rao, Bh. (2018). Mix Design Development of Fly Ash and Ground Granulated Blast Furnace Slag based Geopolymer Concrete. Journal of Building Engineering. 20. [4] Farhan, Nabeel & Sheikh, Md & Hadi, Muhammad. (2019). Investigation of engineering properties of normal and high strength fly ash based geopolymer and alkali-activated slag concrete compared to ordinary Portland cement concrete. Construction and Building Materials. 196. 26-42. [5] Ozcan, F. (2017). Farkli dayamm simflarina ait betonlann basm dayammlarina degi§en kiir §artlarinm etkisi. Omer Halisdemir Oniversitesi Muhendislik Bilimleri Dergisi, 6(1), 115-121.
[6] Betonarme yapilarm tasarim ve yapim kurallan. TS 500/T3. 2014

Claims

1. A production method of geopolymer concrete using slag, alkali activator and aggregate; characterized in that a mixture of blast furnace slag and BOF slag is used as slag, at least one of sodium hydroxide and potassium hydroxide and sodium silicate aqueous solution as alkali activators.
2. A production method of geopolymer concrete according to Claim 1; characterized in that the BOF slag, in which the largest particle diameter is less than 200 pm and the diameter of 50% of the particles are less than a value between 10 and 60 pm, are used.
3. A production method of geopolymer concrete according to Claim 1; characterized in that the blast furnace slag with a Blaine specific surface of 5000±500 cm2/g is used.
4. A production method of geopolymer concrete according to Claim 1; characterized in that a slag mixture containing BOF slag between 10% and 90% by volume is used.
5. A production method of geopolymer concrete according to Claim 1; characterized in that a solution containing sodium hydroxide with a molarity of 4 to 14 M and sodium silicate with a silica modulus of 0.6 to 2.5 is used.
6. A production method of geopolymer concrete according to Claim 1; characterized in that the ratio of solution / slag mixture is in the range of 0.20 and 0.60 by weight.
7. A production method of geopolymer concrete according to Claim 1 ; characterized by the steps of; preparing a slag mixture by mixing blast furnace slag and BOF slag, preparing an aqueous solution containing sodium hydroxide or potassium hydroxide and sodium silicate, mixing the slag mixture, the solution and fine and coarse aggregate, ageing the mixture of slag mixture, solution and aggregate.
8. A production method of geopolymer concrete according to Claim 5; characterized by the step of pouring the mixture of the slag mixture, solution and aggregate applied after the mixing step of the slag mixture, solution and fine and coarse aggregate into a mold and keeping in the mold.
9. A geopolymer ready-mixed concrete produced with the geopolymer concrete production method according to Claim 7.
10. A geopolymer precast concrete produced with the geopolymer concrete production method according to Claim 8.
PCT/TR2022/050270 2021-03-26 2022-03-25 Production method of geopolymer concrete WO2022203641A2 (en)

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Cited By (2)

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WO2023146489A1 (en) * 2022-01-28 2023-08-03 Yildiz Teknik Universitesi Production of rapid hardening geopolymer repair material
CN116730668A (en) * 2023-08-02 2023-09-12 广东中寓再生建筑科技有限公司 Geopolymer and preparation method thereof

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Publication number Priority date Publication date Assignee Title
KR102342008B1 (en) * 2019-03-25 2021-12-22 중앙대학교 산학협력단 Manufacturing method of precast geopolymer concrete member
CN111620665A (en) * 2020-06-18 2020-09-04 湘潭大学 Low-shrinkage and carbonization-resistant steel slag geopolymer concrete
TR202020058A2 (en) * 2020-12-08 2021-03-22 Oyak Beton Sanayi Ve Ticaret Anonim Sirketi Geopolymer binder production method

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2023146489A1 (en) * 2022-01-28 2023-08-03 Yildiz Teknik Universitesi Production of rapid hardening geopolymer repair material
CN116730668A (en) * 2023-08-02 2023-09-12 广东中寓再生建筑科技有限公司 Geopolymer and preparation method thereof
CN116730668B (en) * 2023-08-02 2024-04-02 广东中寓再生建筑科技有限公司 Geopolymer and preparation method thereof

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