CN116813217A - Method for regulating carbonate product in carbonized steel slag - Google Patents
Method for regulating carbonate product in carbonized steel slag Download PDFInfo
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- CN116813217A CN116813217A CN202310759970.9A CN202310759970A CN116813217A CN 116813217 A CN116813217 A CN 116813217A CN 202310759970 A CN202310759970 A CN 202310759970A CN 116813217 A CN116813217 A CN 116813217A
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- steel slag
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- carbonization
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- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 172
- 239000002893 slag Substances 0.000 title claims abstract description 172
- 239000010959 steel Substances 0.000 title claims abstract description 172
- 238000000034 method Methods 0.000 title claims abstract description 24
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 title claims abstract description 23
- 230000001105 regulatory effect Effects 0.000 title claims abstract description 16
- 238000003763 carbonization Methods 0.000 claims abstract description 53
- 238000006243 chemical reaction Methods 0.000 claims abstract description 43
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 40
- 230000001276 controlling effect Effects 0.000 claims abstract description 27
- 239000000203 mixture Substances 0.000 claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000000843 powder Substances 0.000 claims abstract description 22
- 230000000694 effects Effects 0.000 claims abstract description 21
- 229910021532 Calcite Inorganic materials 0.000 claims abstract description 19
- 235000012771 pancakes Nutrition 0.000 claims abstract description 19
- 238000000227 grinding Methods 0.000 claims abstract description 10
- 238000007789 sealing Methods 0.000 claims abstract description 8
- 238000005303 weighing Methods 0.000 claims abstract description 6
- 239000003463 adsorbent Substances 0.000 claims description 20
- 239000004094 surface-active agent Substances 0.000 claims description 15
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 12
- 239000010419 fine particle Substances 0.000 claims description 12
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 7
- 238000007873 sieving Methods 0.000 claims description 7
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 6
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 6
- 239000002808 molecular sieve Substances 0.000 claims description 6
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 6
- RYYKJJJTJZKILX-UHFFFAOYSA-M sodium octadecanoate Chemical compound [Na+].CCCCCCCCCCCCCCCCCC([O-])=O RYYKJJJTJZKILX-UHFFFAOYSA-M 0.000 claims description 6
- 239000004575 stone Substances 0.000 claims description 6
- 239000010457 zeolite Substances 0.000 claims description 6
- HHSPVTKDOHQBKF-UHFFFAOYSA-J calcium;magnesium;dicarbonate Chemical compound [Mg+2].[Ca+2].[O-]C([O-])=O.[O-]C([O-])=O HHSPVTKDOHQBKF-UHFFFAOYSA-J 0.000 claims description 5
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 3
- BCKXLBQYZLBQEK-KVVVOXFISA-M Sodium oleate Chemical compound [Na+].CCCCCCCC\C=C/CCCCCCCC([O-])=O BCKXLBQYZLBQEK-KVVVOXFISA-M 0.000 claims description 2
- 235000021355 Stearic acid Nutrition 0.000 claims description 2
- 229910021536 Zeolite Inorganic materials 0.000 claims description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 2
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 2
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical class O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 2
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 2
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 2
- 229910002027 silica gel Inorganic materials 0.000 claims description 2
- 239000000741 silica gel Substances 0.000 claims description 2
- 235000019982 sodium hexametaphosphate Nutrition 0.000 claims description 2
- 239000002594 sorbent Substances 0.000 claims description 2
- 239000008117 stearic acid Substances 0.000 claims description 2
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 abstract description 10
- 239000000463 material Substances 0.000 abstract description 10
- 239000000395 magnesium oxide Substances 0.000 abstract description 8
- 238000005336 cracking Methods 0.000 abstract description 3
- 238000003756 stirring Methods 0.000 abstract 1
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 14
- 229910000019 calcium carbonate Inorganic materials 0.000 description 14
- 239000001569 carbon dioxide Substances 0.000 description 7
- 229910002092 carbon dioxide Inorganic materials 0.000 description 7
- 239000004568 cement Substances 0.000 description 7
- 239000000292 calcium oxide Substances 0.000 description 6
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 6
- 229910021486 amorphous silicon dioxide Inorganic materials 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 238000006703 hydration reaction Methods 0.000 description 5
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 5
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 230000008901 benefit Effects 0.000 description 4
- 239000004567 concrete Substances 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 239000000499 gel Substances 0.000 description 4
- 238000000643 oven drying Methods 0.000 description 4
- 239000000377 silicon dioxide Substances 0.000 description 4
- 229940029614 triethanolamine stearate Drugs 0.000 description 4
- 239000011575 calcium Substances 0.000 description 3
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 3
- 239000001095 magnesium carbonate Substances 0.000 description 3
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 3
- 230000009257 reactivity Effects 0.000 description 3
- 239000002910 solid waste Substances 0.000 description 3
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- 229920000858 Cyclodextrin Polymers 0.000 description 2
- 239000001116 FEMA 4028 Substances 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- WHGYBXFWUBPSRW-FOUAGVGXSA-N beta-cyclodextrin Chemical compound OC[C@H]([C@H]([C@@H]([C@H]1O)O)O[C@H]2O[C@@H]([C@@H](O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O3)[C@H](O)[C@H]2O)CO)O[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@@H]3O[C@@H]1CO WHGYBXFWUBPSRW-FOUAGVGXSA-N 0.000 description 2
- 235000011175 beta-cyclodextrine Nutrition 0.000 description 2
- 229960004853 betadex Drugs 0.000 description 2
- 239000004566 building material Substances 0.000 description 2
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 2
- 238000010000 carbonizing Methods 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 230000036571 hydration Effects 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 235000019738 Limestone Nutrition 0.000 description 1
- 239000011398 Portland cement Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 235000011116 calcium hydroxide Nutrition 0.000 description 1
- 235000012241 calcium silicate Nutrition 0.000 description 1
- JHLNERQLKQQLRZ-UHFFFAOYSA-N calcium silicate Chemical compound [Ca+2].[Ca+2].[O-][Si]([O-])([O-])[O-] JHLNERQLKQQLRZ-UHFFFAOYSA-N 0.000 description 1
- 229910052918 calcium silicate Inorganic materials 0.000 description 1
- 229910001748 carbonate mineral Inorganic materials 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- BCAARMUWIRURQS-UHFFFAOYSA-N dicalcium;oxocalcium;silicate Chemical compound [Ca+2].[Ca+2].[Ca]=O.[O-][Si]([O-])([O-])[O-] BCAARMUWIRURQS-UHFFFAOYSA-N 0.000 description 1
- 239000010881 fly ash Substances 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 239000005431 greenhouse gas Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000002440 industrial waste Substances 0.000 description 1
- 239000006028 limestone Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000003469 silicate cement Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000009628 steelmaking Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 235000019976 tricalcium silicate Nutrition 0.000 description 1
- 229910021534 tricalcium silicate Inorganic materials 0.000 description 1
- 229960004418 trolamine Drugs 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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
- C04B7/00—Hydraulic cements
- C04B7/14—Cements containing slag
- C04B7/147—Metallurgical slag
-
- 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
- C04B7/00—Hydraulic cements
- C04B7/36—Manufacture of hydraulic cements in general
- C04B7/38—Preparing or treating the raw materials individually or as batches, e.g. mixing with fuel
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention discloses a method for regulating and controlling carbonate products in carbonized steel slag, which comprises the following steps: weighing 85-90wt% of steel slag micropowder, 9.9-14wt% of water and 0.1-1wt% of pre-adsorbed CO 2 Uniformly stirring to form a steel slag mixture; preparing the steel slag mixture into steel slag thin cakes; adding a certain amount of water into the bottom of the carbonization reaction kettle, putting the steel slag thin pancake on a bracket in the kettle, and sealing the reaction kettle; controlling the carbonization temperature in the kettle to be 60-150 ℃ and introducing CO with the concentration of 20-100 percent 2 Gas, CO 2 The partial pressure is 0.2-2.0MPa, the relative humidity is more than or equal to 80 percent, the carbonized steel slag is taken out after carbonization for 0.5-2 hours, and the carbonized steel slag micro powder is obtained after grinding. The invention can control the reaction capacity of carbonized steel slag, generate more high-activity materials such as aragonite or vaterite, avoid generating low-activity or inert carbonate products mainly comprising calcite, consume magnesia basically and solve the potential cracking risk possibly caused by magnesia.
Description
Technical Field
The invention relates to the technical field of comprehensive utilization of industrial waste residues, in particular to a method for regulating and controlling carbonate products in carbonized steel slag.
Background
Steel slag is a solid waste produced in the steel-making process, and in recent years, steel slag is used as a cement mixture, a concrete admixture or coarse and fine aggregate in a building material to a certain extent. However, researchers at home and abroad agree that free calcium oxide and free magnesium oxide in steel slag can generate Ca (OH) in the later hydration reaction 2 And Mg (OH) 2 And the volume expansion is generated, so that the hidden trouble of poor stability exists in the steel slag-containing building material. Therefore, the problem of poor stability of the steel slag is a key point for large-scale resource development and utilization of the steel slag.
The main component of the steel slag is CaO and SiO 2 And Al 2 O 3 Wherein Ca element is mainly contained in dicalcium silicate, tricalcium silicate, calcium hydroxide, a small amount of f-CaO and the like, so that the Ca element is rich in CO 2 Has high carbonization reactivity in the environment, and can be carbonized into carbonate. The early strength of the steel slag serving as a cementing material can be improved by carbonizing the steel slag, f-CaO can be carbonized into calcium carbonate, the adverse effect of the steel slag on the volume stability of concrete is eliminated, and CO generated in industrial production can be absorbed 2 Reduces the emission of greenhouse gases and has certain economic and environmental benefits.
Chinese patent publication No. CN103395812A discloses a method for controlling the morphology of calcium carbonate in a solid carbonization process, which comprises the steps of 2 : beta-cyclodextrin: mixing water=100:3-10:5-15 in proportion, forming under 2.0-15.0MPa, and carbonizing in a closed reaction kettle. The invention introduces a method for controlling the morphology of calcium carbonate crystals in liquid by using polysaccharide to prepare the calcium carbonate with hollow tubular morphology similar to beta-cyclodextrin molecular structure, wherein the calcium carbonate is mainly calcite. However, the technology uses pure reagent to synthesize the calcium carbonate whisker with hollow tubular morphology, the cost is too high, and if the technology is used for improving the strength performance of cement materials, the technology is very uneconomical and even wastes resources.
Zhang Yan et al, free calcium oxide and magnesium oxide in steel slag carbonation reaction [ J ]; university of company university report; in 2018, in 06 period, steel slag powder and water are uniformly mixed according to a water-solid ratio of 0.1, the mixture is placed into a reaction kettle, carbonation treatment is carried out under the pressure of 99.9% and 0.2MPa of carbon dioxide content, a sample is taken out and dried, and carbonated steel slag powder is obtained, wherein under the condition of basically complete carbonization, carbonized steel slag powder taking calcite as a main product is produced, and the calcite product accounts for 88% of the carbonized product. But also contains magnesium carbonate in an amount of 2.4-2.5, which is not completely carbonized, which will create a risk of expansion cracking for the concrete incorporating the carbonized steel slag. In addition, the method is not embodied by a technology for regulating and controlling the proportion of the carbonic acid product.
In summary, the problems of the prior art are as follows:
(1) In the prior art, calcite is mainly generated by carbonization, and the calcite has very weak capability of participating in hydration reaction due to good crystallization.
(2) The pure reagent is used for synthesizing the calcium carbonate whisker with the hollow tubular shape, if the calcium carbonate whisker is doped into cement-based materials, the cost is too high, and the resource is wasted;
(3) The carbonization capability of magnesium oxide is weak, and risks are brought to the use of cementing materials;
(4) At present, no effective technology is available to realize that enough carbonate mineral contents such as striations, vaterites and the like can be generated in the carbonized steel slag, so that the carbonized steel slag-silicate clinker is promoted to conform to the reactivity of cement, and the strength performance of the cementing material is improved.
Therefore, research on the above problems is needed to develop a method capable of controlling carbonate products in carbonized steel slag.
Disclosure of Invention
The invention provides a method for regulating and controlling carbonate products in carbonized steel slag, which is characterized in that similar calcium carbonate whisker materials are prepared by using low-cost or large-scale solid waste raw materials, and carbonized products of the low-cost solid waste materials are controlled by a special process, so that two or more gelled materials of calcium carbonate whiskers can be generated; the method can control the reaction capacity of the carbonized steel slag, generate more high-activity calcium carbonate seed crystal materials such as aragonite or vaterite and the like, avoid generating low-activity or inert carbonate products mainly comprising calcite, consume magnesium oxide, and solve the potential cracking risk possibly caused by the magnesium oxide.
The invention is realized in such a way that a method for regulating and controlling carbonate products in carbonized steel slag comprises the following steps:
firstly, weighing 85-90wt% of steel slag micropowder, 9.9-14wt% of water and 0.1-1wt% of adsorbent, and putting the steel slag micropowder and the adsorbent into a stirrer to be uniformly stirred to form a plastic steel slag mixture; wherein the adsorbent is pre-adsorbed with CO 2 Is a sorbent of (2);
step two, preparing the steel slag mixture prepared in the step one into steel slag thin cakes with the diameter of 200-250mm and the thickness of 2-5 mm;
adding a certain amount of water into the bottom of the carbonization reaction kettle, putting the steel slag thin pancake prepared in the second step on a multi-layer bracket in the carbonization reaction kettle, and then sealing the carbonization reaction kettle;
controlling the carbonization temperature in the carbonization reaction kettle to be 60-150 ℃, and introducing CO with the concentration of 20-100 percent 2 Gas, CO 2 The partial pressure is 0.2-2.0MPa, the relative humidity is more than or equal to 80 percent, the carbonized steel slag thin pancake is taken out after carbonization for 0.5-2 hours, and the powder is ground to the specific surface area of 450-600m 2 And (3) per kg, obtaining carbonized steel slag micropowder.
Preferably, in the first step, the steel slag micropowder is obtained by crushing raw steel slag, sieving with a 1mm square sieve, drying, performing electromagnetic iron removal, and then placing the steel slag micropowder and surfactant accounting for 0.1-1% of the mass of the steel slag micropowder into a mill for grinding to obtain the steel slag micropowder with the specific surface area of 450-600m 2 /kg of steel slag micropowder.
Further preferably, the surfactant is a combination of any two of triethanolamine, isopropanol, propylene glycol, stearic acid, oleate, sodium hexametaphosphate, sodium stearate, and maleic anhydride derivatives.
Preferably, in the first step, the pre-adsorbed CO 2 The adsorbent is one or the combination of any two of molecular sieve (zeolite), active carbon, active alumina and silica gel.
Preferably, in the third step, water with the depth of 10 cm to 15cm is added into the bottom of the carbonization reaction kettle, so that the whole carbonization reaction kettle has enough humidity and water vapor, and the water reacts with CO under the pressure 2 Enters the steel slag thin pancake and carbonizes the steel slag thin pancake.
Preferably, in the fourth step, the content of Chinese stone in the carbonized steel slag micropowder is 3.0-5.0%, the content of calcite is 5.0-8.0%, the content of vaterite is 4.0-7.0%, the content of calcium magnesium carbonate is 1.0-2.0%, the content of amorphous silicon dioxide is 5.0-6.0%, and the 28-day activity index of the carbonized steel slag micropowder is 85-95%.
The invention also provides the carbonized steel slag micro powder, which is prepared by adopting the preparation method.
Compared with the prior art, the invention has the advantages and positive effects that:
1. according to the invention, the adsorbent which is pre-adsorbed with a certain amount of carbon dioxide and the steel slag micropowder are used for preparing the steel slag wafer with a certain thickness, so that the carbon dioxide in the adsorbent is gradually released in the steel slag wafer in the heating process after introducing the carbon dioxide, the carbon dioxide participates in carbonization reaction in the steel slag wafer, and a microscopic region rich in carbon dioxide is formed locally, so that more aragonite and vaterite can be formed, and a large amount of calcite is reduced. The adsorbent selected by the invention has better reactivity in a silicate cement system.
2. The surfactant is used in the preparation process of the steel slag micro powder, so that the grinding efficiency of the steel slag is improved, the Gibbs free energy and chemical reaction activity of the surface of the steel slag micro powder are increased, the carbon dioxide adsorption capacity is improved, and the carbonization reaction process is improved.
3. The invention effectively solves the problem of poor stability of steel slag through carbonization reaction, and simultaneously improves the activity index of the carbonized steel slag micro powder, compared with the original state steel slag, the carbonized steel slag micro powder can greatly improve the early strength of the steel slag composite Portland cement, has low carbon and environmental protection, and has better social benefit and economic benefit.
Drawings
FIG. 1 is an XRD pattern of a carbonized steel slag micropowder obtained in example 1 of the present invention;
FIG. 2 is an XRD pattern of the carbonized steel slag micropowder obtained in example 2 of the present invention;
FIG. 3 is an XRD pattern of the carbonized steel slag micropowder obtained in example 3 of the present invention;
FIG. 4 is an XRD pattern of the carbonized steel slag micropowder obtained in comparative example 1 of the present invention.
Detailed Description
The following description of the present invention will be made clearly and fully, and it is apparent that the embodiments described are some, but not all, of the embodiments of the present invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The composition of the raw steel slag is shown in the following table 1.
TABLE 1 raw slag composition
| Name of the name | L.O.I | SiO 2 | Al 2 O 3 | Fe 2 O 3 | CaO | MgO | K 2 O | Na 2 O | SO 3 | Cl － | Totals to |
| Original state steel slag I | 3.12 | 15.34 | 7.12 | 18.84 | 40.83 | 10.14 | 0.05 | 0.10 | 0.35 | 0.024 | 95.914 |
| Original state steel slag II | 1.42 | 11.84 | 7.55 | 27.54 | 38.64 | 9.24 | 0.06 | 0.08 | 0.34 | 0.01 | 96.720 |
In the following examples, the primary steel slag I in Table 1 was used.
Example 1
A method for regulating and controlling carbonate products in carbonized steel slag, comprising the following steps:
step one: weighing 90.0wt% of steel slag micropowder, 9.9wt% of water and 0.1wt% of adsorbent; putting the mixture into a stirrer to be stirred uniformly to form a plastic steel slag mixture;
wherein the steel slag micropowder is prepared by crushing raw steel slag, sieving with 1mm square sieve, oven drying, electromagnetic deironing, grinding the steel slag fine particles and surfactant accounting for 0.1% of the mass of the fine particles in a mill to obtain a specific surface area of 450-600m 2 /kg of steel slag micropowder. The surfactant is a combination of triethanolamine and sodium stearate. The adsorbent is pre-adsorbed with CO 2 Molecular sieves (zeolites) and silica gels.
Step two: and (3) preparing the steel slag mixture prepared in the step one into steel slag thin cakes with the diameter of 200-250mm and the thickness of 2-5 mm.
And thirdly, adding water with the depth of 10-15cm into the carbonization reaction kettle, putting the steel slag thin pancake prepared in the second step into a multi-layer bracket in the carbonization reaction kettle, and then sealing the reaction kettle.
Controlling the carbonization temperature in the carbonization reaction kettle to be 150 ℃, and introducing CO with the concentration of 100 percent 2 Gas, CO 2 The partial pressure is 2.0MPa, the relative humidity is more than or equal to 80 percent, the carbonized steel slag thin pancake is taken out after carbonization for 0.5h, and the powder is ground to the specific surface area of 450-600m 2 And (3) per kg, obtaining carbonized steel slag micropowder.
The 28-day activity index of the carbonized steel slag micropowder is 85-95%, wherein the carbonized steel slag micropowder comprises 3.0% of Chinese stone, 8.0% of calcite, 5.0% of vaterite, 2.0% of calcium magnesium carbonate and 5.0% of amorphous silicon dioxide.
Example 2
A method for regulating and controlling carbonate products in carbonized steel slag, comprising the following steps:
step one: weighing 85.0wt% of steel slag micropowder, 14.0wt% of water and 1.0wt% of adsorbent; putting the mixture into a stirrer to be stirred uniformly to form a plastic steel slag mixture;
wherein the steel slag micropowder is obtained by crushing raw steel slag, sieving with a 1mm square sieve, drying, performing electromagnetic iron removal, and grinding the steel slag fine particles and surfactant accounting for 1% of the mass of the fine particles in a millThe specific surface area is 450-600m 2 /kg of steel slag micropowder. The surfactant is a combination of triethanolamine and sodium stearate. The adsorbent is pre-adsorbed with CO 2 Molecular sieves (zeolites) and silica gels.
Step two: and (3) preparing the steel slag mixture prepared in the step one into steel slag thin cakes with the diameter of 200-250mm and the thickness of 2-5 mm.
And thirdly, adding water with the depth of 10-15cm into the carbonization reaction kettle, putting the steel slag thin pancake prepared in the second step into a multi-layer bracket in the carbonization reaction kettle, and then sealing the reaction kettle.
Controlling the carbonization temperature in the carbonization reaction kettle to be 80 ℃, and introducing CO with concentration of 80 percent 2 Gas, CO 2 The partial pressure is 1.0MPa, the relative humidity is more than or equal to 80 percent, the carbonized steel slag thin pancake is taken out after carbonization for 0.8h, and the powder is ground to the specific surface area of 450-600m 2 And (3) per kg, obtaining carbonized steel slag micropowder.
The 28-day activity index of the carbonized steel slag micropowder is 85-95 percent, wherein the carbonized steel slag micropowder comprises 5.0 percent of Chinese stone, 5.0 percent of calcite, 6.0 percent of vaterite, 1.0 percent of calcium and magnesium carbonate and 6.0 percent of amorphous silicon dioxide.
Example 3
A method for regulating and controlling carbonate products in carbonized steel slag, comprising the following steps:
step one: 86.0wt% of steel slag micropowder, 13.2wt% of water and 0.8wt% of adsorbent are weighed; putting the mixture into a stirrer to be stirred uniformly to form a plastic steel slag mixture;
wherein the steel slag micropowder is prepared by crushing raw steel slag, sieving with 1mm square sieve, oven drying, electromagnetic deironing, grinding the steel slag fine particles and surfactant accounting for 0.8% of the mass of the fine particles in a mill to obtain a powder with a specific surface area of 450-600m 2 /kg of steel slag micropowder. The surfactant is a combination of triethanolamine and sodium stearate. The adsorbent is pre-adsorbed with CO 2 Molecular sieves (zeolites) and silica gels.
Step two: and (3) preparing the steel slag mixture prepared in the step one into steel slag thin cakes with the diameter of 200-250mm and the thickness of 2-5 mm.
And thirdly, adding water with the depth of 10-15cm into the carbonization reaction kettle, putting the steel slag thin pancake prepared in the second step into a multi-layer bracket in the carbonization reaction kettle, and then sealing the reaction kettle.
Controlling the carbonization temperature in the carbonization reaction kettle to be 100 ℃, and introducing CO with the concentration of 70 percent 2 Gas, CO 2 The partial pressure is 0.6MPa, the relative humidity is more than or equal to 80 percent, the carbonized steel slag thin pancake is taken out after carbonization for 1 hour, and the powder is ground to the specific surface area of 450-600m 2 And (3) per kg, obtaining carbonized steel slag micropowder.
The 28-day activity index of the carbonized steel slag micropowder is 85-95%, wherein the carbonized steel slag micropowder comprises 4.0% of Chinese stone, 6.0% of calcite, 7.0% of vaterite, 1.6% of calcium and magnesium carbonate, 5.5% of amorphous silicon dioxide.
Example 4
A method for regulating and controlling carbonate products in carbonized steel slag, comprising the following steps:
step one: 89.0wt% of steel slag micropowder, 10.8wt% of water and 0.2wt% of adsorbent are weighed; putting the mixture into a stirrer to be stirred uniformly to form a plastic steel slag mixture;
wherein the steel slag micropowder is prepared by crushing raw steel slag, sieving with 1mm square sieve, oven drying, electromagnetic deironing, grinding the steel slag fine particles and surfactant accounting for 0.3% of the mass of the fine particles in a mill to obtain a specific surface area of 450-600m 2 /kg of steel slag micropowder. The surfactant is a combination of triethanolamine and sodium stearate. The adsorbent is pre-adsorbed with CO 2 Molecular sieves (zeolites) and silica gels.
Step two: and (3) preparing the steel slag mixture prepared in the step one into steel slag thin cakes with the diameter of 200-250mm and the thickness of 2-5 mm.
And thirdly, adding water with the depth of 10-15cm into the carbonization reaction kettle, putting the steel slag thin pancake prepared in the second step into a multi-layer bracket in the carbonization reaction kettle, and then sealing the reaction kettle.
Controlling the carbonization temperature in the carbonization reaction kettle to be 60 ℃, and introducing CO with the concentration of 20 percent 2 Gas, CO 2 The partial pressure is 0.2MPa, the relative humidity is more than or equal to 80 percent, and the mixture is taken out after carbonization for 2 hoursGrinding the carbonized steel slag thin pancake to a specific surface area of 450-600m 2 And (3) per kg, obtaining carbonized steel slag micropowder.
The 28-day activity index of the carbonized steel slag micropowder is 85-95%, wherein the carbonized steel slag micropowder comprises 4.5% of Chinese stone, 7.0% of calcite, 4.0% of vaterite, 1.2% of calcium magnesium carbonate and 5.0% of amorphous silicon dioxide.
Comparative example 1
A method for regulating and controlling carbonate products in carbonized steel slag, comprising the following steps:
step one: weighing 90.0wt% of steel slag micropowder, 14.0wt% of water and 0.0wt% of adsorbent; putting the mixture into a stirrer to be stirred uniformly to form a plastic steel slag mixture;
wherein the steel slag micropowder is prepared by crushing raw steel slag, sieving with 1mm square sieve, oven drying, electromagnetic deironing, grinding the steel slag fine particles and surfactant accounting for 0.0% of the mass of the fine particles in a mill to obtain a specific surface area of 450-600m 2 /kg of steel slag micropowder.
Step two: and (3) preparing the steel slag mixture prepared in the step one into steel slag thin cakes with the diameter of 200-250mm and the thickness of 2-5 mm.
And thirdly, adding water with the depth of 10-15cm into the carbonization reaction kettle, putting the steel slag thin pancake prepared in the second step into a multi-layer bracket in the carbonization reaction kettle, and then sealing the reaction kettle.
Controlling the carbonization temperature in the carbonization reaction kettle to be 150 ℃, and introducing CO with the concentration of 100 percent 2 Gas, CO 2 The partial pressure is 2.0MPa, the relative humidity is more than or equal to 80 percent, the carbonized steel slag thin pancake is taken out after carbonization for 0.5h, and the powder is ground to the specific surface area of 450-600m 2 And (3) per kg, obtaining carbonized steel slag micropowder.
The 28-day activity index of the carbonized steel slag micropowder is 79.4%, wherein the carbonized steel slag micropowder comprises 14.0% of calcite, 1.4% of aragonite, 0.8% of vaterite, 1.0% of calcium magnesium carbonate and 5.5% of amorphous silica.
The amounts of carbonate ores of different crystal forms, as measured by activity index and XRD quantitative analysis, were measured for the fine powder of carbonized steel slag prepared in examples 1 to 4 and comparative example 1 according to GB/T1596-2017 fly ash for cement and concrete, and the results are shown in Table 2.
Table 2 performance indexes of the carbonized steel slag micropowder prepared in examples 1 to 4 and comparative example 1
As can be seen from table 2, when the calcite content is increased, the activity index tends to decrease, which means that the hydration activity of calcite is lower than that of other carbonic acid products with poor crystallization degree, whereas the case of comparative example 1 without adding the surfactant and the adsorbent produces carbonized steel slag micropowder based on calcite, the activity of which is significantly lower than that of examples 1 to 4 in which the difference in calcium carbonate crystal form content is not large, and the carbonized steel slag micropowder based on calcite is equivalent to direct limestone powder addition, and the improvement of cement hydration activity is limited. The hydration reaction activity of the carbonized steel slag micropowder in cement is regulated and controlled by regulating and controlling the contents of different carbonate products in the carbonized steel slag micropowder, so that the 28-day activity index and early strength of the carbonized steel slag micropowder are greatly improved, the test result is far higher than that of original steel slag, and the basic requirement of not less than 70% in national standard is met.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and not for limiting the same; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the invention.
Claims (7)
1. A method for regulating and controlling carbonate products in carbonized steel slag, which is characterized by comprising the following steps:
step one, weighing 85 to 90 weight percent of steel slag micro powder, 9.9 to 14 weight percent of water and 0.1 to 1 weight percent of adsorbent,putting the mixture into a stirrer to be stirred uniformly to form a plastic steel slag mixture; wherein the adsorbent is pre-adsorbed with CO 2 Is a sorbent of (2);
step two, preparing the steel slag mixture prepared in the step one into steel slag thin cakes with the diameter of 200-250mm and the thickness of 2-5 mm;
adding a certain amount of water into the bottom of the carbonization reaction kettle, putting the steel slag thin pancake prepared in the second step on a multi-layer bracket in the carbonization reaction kettle, and then sealing the carbonization reaction kettle; controlling the carbonization temperature in the carbonization reaction kettle to be 60-150 ℃, and introducing CO with the concentration of 20-100 percent 2 Gas, CO 2 The partial pressure is 0.2-2.0MPa, the relative humidity is more than or equal to 80 percent, the carbonized steel slag thin pancake is taken out after carbonization for 0.5-2 hours, and the powder is ground to the specific surface area of 450-600m 2 And (3) per kg, obtaining carbonized steel slag micropowder.
2. The method for controlling carbonate products in carbonized steel slag according to claim 1, wherein in the first step, the steel slag micro powder is obtained by crushing raw steel slag, sieving with a square sieve of 1mm, drying, then carrying out electromagnetic iron removal, and then grinding the steel slag fine particles and a surfactant accounting for 0.1-1% of the mass of the fine particles in a grinding machine to obtain the steel slag micro powder with a specific surface area of 450-600m 2 /kg of steel slag micropowder.
3. The method for controlling carbonate products in carbonized steel slag according to claim 2, wherein the surfactant is any two of triethanolamine, isopropanol, propylene glycol, stearic acid, oleate, sodium hexametaphosphate, sodium stearate, and maleic anhydride derivatives.
4. The method according to claim 1, wherein in the first step, the pre-adsorbed CO is used for controlling carbonate products in the carbonized steel slag 2 The adsorbent is one or the combination of any two of molecular sieve (zeolite), active carbon, active alumina and silica gel.
5. Regulated carbonization according to claim 1The method for preparing carbonate product in steel slag is characterized by that in step three, water with depth of 10-15cm is added into bottom portion of carbonization reaction kettle so as to make the whole carbonization reaction kettle possess enough humidity and water vapour, and under the action of pressure it can be reacted with CO 2 Enters the steel slag thin pancake and carbonizes the steel slag thin pancake.
6. The method for controlling carbonate products in carbonized steel slag according to claim 1, wherein in the fourth step, the fine powder of carbonized steel slag has a chinese stone content of 3.0-5.0%, calcite content of 5.0-8.0%, vaterite content of 4.0-7.0%, calcium magnesium carbonate content of 1.0-2.0%, amorphous silica content of 5.0-6.0% and 28-day activity index of 85-95%.
7. A carbonized steel slag micropowder, characterized in that it is produced by the production method according to any one of claims 1 to 6.
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