CN115259702A - Slag fly ash-based alkali-activated cementing material and preparation method thereof - Google Patents
Slag fly ash-based alkali-activated cementing material and preparation method thereof Download PDFInfo
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- 239000002893 slag Substances 0.000 title claims abstract description 58
- 239000000463 material Substances 0.000 title claims abstract description 57
- 239000010881 fly ash Substances 0.000 title claims abstract description 53
- 239000003513 alkali Substances 0.000 title claims abstract description 52
- 238000002360 preparation method Methods 0.000 title abstract description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 48
- 239000001488 sodium phosphate Substances 0.000 claims abstract description 22
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 21
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 21
- 235000019353 potassium silicate Nutrition 0.000 claims abstract description 21
- 229910000162 sodium phosphate Inorganic materials 0.000 claims abstract description 20
- 239000004576 sand Substances 0.000 claims abstract description 18
- 239000002131 composite material Substances 0.000 claims abstract description 17
- 239000002994 raw material Substances 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims abstract description 16
- 239000000843 powder Substances 0.000 claims abstract description 11
- 239000012190 activator Substances 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims description 24
- 235000011008 sodium phosphates Nutrition 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 11
- 239000011734 sodium Substances 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- 238000005303 weighing Methods 0.000 claims description 5
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 4
- 229910052708 sodium Inorganic materials 0.000 claims description 4
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- ASTWEMOBIXQPPV-UHFFFAOYSA-K trisodium;phosphate;dodecahydrate Chemical group O.O.O.O.O.O.O.O.O.O.O.O.[Na+].[Na+].[Na+].[O-]P([O-])([O-])=O ASTWEMOBIXQPPV-UHFFFAOYSA-K 0.000 claims description 2
- 239000010754 BS 2869 Class F Substances 0.000 claims 1
- 239000011148 porous material Substances 0.000 abstract description 7
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 abstract description 6
- 229910019142 PO4 Inorganic materials 0.000 abstract description 5
- 239000010452 phosphate Substances 0.000 abstract description 5
- 239000004094 surface-active agent Substances 0.000 abstract description 4
- 239000002956 ash Substances 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 11
- 239000004568 cement Substances 0.000 description 8
- 239000004570 mortar (masonry) Substances 0.000 description 6
- 238000001035 drying Methods 0.000 description 5
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- 239000011083 cement mortar Substances 0.000 description 4
- 238000011056 performance test Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 239000004566 building material Substances 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 238000006703 hydration reaction Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 230000000704 physical effect Effects 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 2
- 239000000378 calcium silicate Substances 0.000 description 2
- 229910052918 calcium silicate Inorganic materials 0.000 description 2
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 239000003638 chemical reducing agent Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000003245 coal Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000036571 hydration Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000007790 scraping Methods 0.000 description 2
- 239000002910 solid waste Substances 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 229910000406 trisodium phosphate Inorganic materials 0.000 description 2
- 235000019801 trisodium phosphate Nutrition 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical group [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 239000011398 Portland cement Substances 0.000 description 1
- 229910001294 Reinforcing steel Inorganic materials 0.000 description 1
- 239000004115 Sodium Silicate Substances 0.000 description 1
- 102100040791 Zona pellucida-binding protein 1 Human genes 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 150000004645 aluminates Chemical class 0.000 description 1
- 229910001579 aluminosilicate mineral Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 125000003636 chemical group Chemical group 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- JYIMWRSJCRRYNK-UHFFFAOYSA-N dialuminum;disodium;oxygen(2-);silicon(4+);hydrate Chemical compound O.[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[Na+].[Na+].[Al+3].[Al+3].[Si+4] JYIMWRSJCRRYNK-UHFFFAOYSA-N 0.000 description 1
- 150000004683 dihydrates Chemical class 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- JEGUKCSWCFPDGT-UHFFFAOYSA-N h2o hydrate Chemical compound O.O JEGUKCSWCFPDGT-UHFFFAOYSA-N 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 229910052909 inorganic silicate Inorganic materials 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 235000011121 sodium hydroxide Nutrition 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- 239000008399 tap water Substances 0.000 description 1
- 235000020679 tap water Nutrition 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000008883 yougui Substances 0.000 description 1
Images
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
-
- 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
- C04B7/24—Cements from oil shales, residues or waste other than slag
- C04B7/243—Mixtures thereof with activators or composition-correcting additives, e.g. mixtures of fly ash and alkali activators
-
- 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
-
- 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
Abstract
The invention discloses a slag fly ash-based alkali-activated cementing material and a preparation method thereof. The alkali-activated cementing material provided by the invention takes slag powder and fly ash as main ash materials, water glass-sodium phosphate as a composite activator and polyethylene glycol surfactant as an introduced component, and the weight parts of the raw materials are as follows: 300-330 parts of slag powder, 120-150 parts of fly ash, 95-105 parts of water glass, 20-25 parts of sodium hydroxide, 5-12 parts of sodium phosphate, 4-9 parts of polyethylene glycol, 100-120 parts of water and 1200-1250 parts of standard sand. Compared with the prior art, the phosphate and the surfactant are introduced into the slag fly ash alkali-activated composite gelling system, the phosphate and the surfactant are comprehensively utilized to optimize the pore structure of the gelling system and compensate the shrinkage, the bottleneck problem that the alkali-activated gelling material shrinks and cracks seriously is obviously improved, the mechanical property is excellent, the average 28d compressive strength is 65MPa, and the composite gelling material has obvious economic benefit and application prospect.
Description
Technical Field
The invention relates to the technical field of building materials, in particular to a slag fly ash-based alkali-activated cementing material and a preparation method thereof.
Background
With the continuous deepening of the sustainable development strategy of China in the capital construction industry and the urgent need of the cement industry to reduce the environmental pollution, the alkali-activated cementing material has received extensive attention and research as a substitute material of a cement-based material. The material is usually prepared by reacting amorphous aluminosilicate minerals with an alkaline activator, wherein the reaction product is calcium silico (aluminate) or sodium silicoaluminate gel, and common raw materials comprise industrial solid wastes such as blast furnace slag, fly ash, metakaolin, red mud, steel slag, coal gangue and the like and natural active materials such as volcanic ash and the like. Compared with portland cement, the alkali-activated cementing material has the characteristics of wide material sources, low comprehensive energy consumption and low carbon dioxide emission, and also has the mechanical properties similar to or even more excellent than those of cement-based materials, and the characteristics of fire resistance, acid and alkali corrosion resistance, high reinforcing steel bar binding power, high protective capacity and the like. With the rapid development of the steel industry in China and the increase of the utilization amount of coal resources, the annual slag production in China is about 2.4 hundred million tons, the yield of the fly ash in 2024 years is estimated to reach 9.25 hundred million tons, and the slag and the fly ash become industrial byproducts with huge yield in China. The slag, the fly ash and other industrial solid wastes are used as raw materials, and a cementing material formed by the excitation of an alkaline excitant replaces a cement-based material, so that the carbon dioxide emission in the cement production can be obviously reduced, the sustainable development capability of the building material industry is improved, and the method is necessary for building an environment-friendly society in China.
However, at present, the alkali-activated cementing material still has many limitations, wherein the material characteristic with excessive drying shrinkage deformation is one of the bottleneck problems limiting the popularization and application of the alkali-activated material, the shrinkage of the material is usually more than 2 times that of the cement-based material, and the shrinkage can even exceed 6 times that of the cement-based material in the absence of design guidance. The shrinkage behavior of the alkali-activated gel material is a gradual change process combining physical action as a main factor and physical-chemical factors, and the high capillary pressure and the free water content brought by the unique phase composition and the gel structure characteristics of the material are main reasons for causing excessive shrinkage deformation. For alkali-activated cementitious materials, the most intensive research at present is that sodium hydroxide is used for adjusting alkali equivalent and water glass modulus, liquid water glass is used as a single alkali activator, granulated blast furnace slag powder is used as a single raw material to form the alkali-activated slag cementitious material, and the alkali-activated slag cementitious material has the advantages of high early compressive strength, good durability and the like, but also has the defects of short setting time, serious shrinkage cracking phenomenon and the like. Therefore, although the alkali-activated cementing material has a plurality of excellent characteristics, the bottleneck problem that the material shrinks too much cannot be effectively broken through at the present stage, so that the large-scale application of the material is limited to a great extent.
Disclosure of Invention
The invention provides a slag fly ash-based alkali-activated cementing material and a preparation method thereof, wherein phosphate and a shrinkage reducing agent are introduced into an alkali-activated slag fly ash composite cementing system, so that the advantages of the phosphate and the shrinkage reducing agent are expected to be integrated, the pore structure characteristics and the shrinkage compensation capability of the system are optimized, the aim that the volume stability of the composite alkali-activated cementing system is superior to that of a traditional cement-based material after regulation and control is realized, and the application of the alkali-activated cementing material in actual engineering is further effectively promoted.
The scheme for solving the technical problems is as follows: the slag fly ash-based alkali-activated cementing material comprises the following raw material components in parts by weight: 300-330 parts of slag powder, 120-150 parts of fly ash, 95-105 parts of water glass, 20-25 parts of sodium hydroxide, 5-12 parts of sodium phosphate, 4-9 parts of polyethylene glycol, 100-120 parts of water and 1200-1250 parts of sand.
Preferably, the slag is S95 grade slag powder with the density being more than or equal to 2.8g/cm 3 The specific surface area is more than or equal to 400m 2 /kg。
Preferably, the fly ash is F-class second-grade fly ash, and the fineness (the screen residue of a 45-um square-hole sieve) is less than or equal to 25wt%.
Preferably, the water glass has a modulus (SiO) 2 With Na 2 Molar ratio of O) is 3.3 2 O content 8.54wt%, siO 2 The content was 27.3wt%.
Preferably, the purity grade of the sodium hydroxide is analytically pure, and the content is more than or equal to 98wt%; the sodium phosphate is trisodium phosphate (Na) dodecahydrate 3 PO 4 ·12H 2 O), the purity grade is analytically pure, and the content is more than or equal to 98wt%.
Preferably, the polyethylene glycol has an average molecular mass of 2000 and a pH (50 g/L,25 ℃) of 6.0.
Preferably, the standard sand meets the relevant requirements of cement mortar strength test method (ISO method) GB/T17671-1999, wherein SiO is 2 The content is more than or equal to 98wt%, and the particle size range is 0.08-2mm.
Preferably, the raw material components of the slag fly ash-based alkali-activated cementing material comprise, by weight: 310-330 parts of slag powder, 130-150 parts of fly ash, 95-100 parts of water glass, 20-25 parts of sodium hydroxide, 6-10 parts of sodium phosphate, 5-8 parts of polyethylene glycol, 105-115 parts of water and 1200-1250 parts of standard sand.
Preferably, the raw material components of the slag fly ash-based alkali-activated cementing material comprise, by weight: 325 parts of slag powder, 150 parts of fly ash, 97 parts of water glass, 25 parts of sodium hydroxide, 7.4 parts of sodium phosphate, 6.9 parts of polyethylene glycol, 107 parts of water and 1244 parts of standard sand.
The preparation method of the slag fly ash-based alkali-activated cementing material specifically comprises the following steps:
1) Weighing various raw materials according to the mass ratio for later use;
2) Placing sodium hydroxide, sodium phosphate, water glass and water in a container, and primarily stirring and mixing to obtain a composite alkali activator;
3) And adding the weighed polyethylene glycol into the composite excitant, primarily stirring, and then placing in heating equipment to heat up and fully dissolve the polyethylene glycol. Preferably, a magnetic stirrer is heated at a constant temperature and the temperature is raised to 80-100 ℃. And (3) placing the compound excitant in a constant-temperature heating magnetic stirrer at the rotating speed of 20r/min, heating and stirring for 3min to fully dissolve polyethylene glycol, uniformly mixing, and cooling to room temperature to obtain the sodium silicate-sodium phosphate compound excitant.
4) Firstly, adding the excitant cooled to room temperature into a stirring container, then adding weighed slag and fly ash, immediately starting a stirrer to stir at low speed (140 +/-5 r/min) for 30s so as to mix uniformly. Standard sand was added to the stirred vessel evenly and slowly over the next 30s, after which the machine was adjusted to high speed (280. + -.10 r/min) and stirring was stopped for 30 s. And scraping the mortar on the inner wall of the stirring container and the blades into the middle of the pot by using a triangular scraper within 15s, manually mixing the mortar at the bottom of the pot uniformly, starting the machine, and continuously stirring at a high speed (280 +/-10 r/min) for 60s to obtain the slag fly ash-based low-shrinkage alkali-activated cementing material.
The beneficial effects of the invention are:
the phosphate and the surfactant are introduced into the composite alkali-activated cementing material system, so that the bound water content of the system can be increased, the phase composition and the pore structure of the system are optimized, and the shrinkage behavior of the alkali-activated composite cementing material system is effectively improved on the premise of ensuring the basic mechanical property. Meanwhile, the fly ash contains stable Al 2 O 3 The addition of the low doping amount can make up the defect of a single raw material, promote the hydration reaction of the alkali-activated slag system, improve the compactness of the system and further improve the shrinkage characteristic of the alkali-activated slag system.
The foregoing description is only an overview of the technical solutions of the present invention, and in order to make the technical solutions of the present invention more clearly understood and to implement them in accordance with the contents of the description, the following detailed description is given with reference to the preferred embodiments of the present invention and the accompanying drawings. The detailed description of the present invention is given in detail by the following examples and the accompanying drawings.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the invention and together with the description serve to explain the invention and do not constitute a limitation of the invention. In the drawings:
FIG. 1 is a flow chart of preparation of a slag fly ash-based alkali-activated cementitious material in an embodiment of the present invention.
Detailed Description
The principles and features of this invention are described below in conjunction with the following drawings, which are set forth to illustrate, but are not to be construed to limit the scope of the invention.
The sources of the raw materials used in the following examples of the invention are as follows:
1. the water glass is provided by Yougui refractory Co., ltd, jiashan county, and has the model of SP38 water glass and SiO 2 27.3wt% of Na 2 O content 8.54wt%, modulus (SiO) 2 /Na 2 O molar ratio) of 3.30, a specific gravity of 1.362, and a colorless, transparent, viscous liquid at room temperature.
2. The sodium hydroxide reagent is provided by Shanghai Aladdin Biotechnology GmbH, the purity grade is analytically pure, the content is 98.15%, and the character is white blocky crystal.
3. The sodium phosphate is trisodium phosphate (Na) dihydrate provided by national drug group chemical reagent limited 3 PO 4 ·12H 2 O), the purity grades are analytically pure, and the content is over 98.0 percent.
4. Polyethylene glycol was provided by the national chemical group, chemical reagents, ltd, and had an average molecular mass of 2000.
5. The water is tap water.
6. The slag is S95 grade slag with the density of 2850kg/m 3 Specific surface area of 1.47m 2 (iv)/g, median particle diameter of 10.109um.
7. The fly ash is F-class secondary fly ash with the density of 2200kg/m 3 Specific surface area of 1.35m 2 (iv) a median particle diameter of 13.197um.
8. The standard sand adopts Chinese ISO standard sand provided by Xiamen EsiO standard sand limited company, conforms to the GB/T17671-1999 standard, and has a particle size range of 0.08-2mm.
The chemical compositions and physical properties of the slag and fly ash are shown in table 1.
TABLE 1 chemical composition and physical Properties of slag and fly Ash
Examples 1 to 8
As shown in FIG. 1, the slag fly ash-based alkali-activated cementitious materials of examples 1-8 were prepared, and the raw material formulation for each example is shown in Table 2:
1) Weighing water glass (liquid sodium silicate), sodium hydroxide particles, sodium phosphate solid and water in sequence according to the mass ratio; firstly, placing sodium hydroxide particles, trisodium phosphate dodecahydrate solid and weighed water glass into a glass beaker for mixing, manually stirring by adopting a glass rod and uniformly mixing, and finally adding the weighed water into the beaker and uniformly stirring by using the glass rod.
2) The constant temperature heating magnetic stirrer (DF-101S type heat collection type constant temperature heating magnetic stirrer provided by Shanghai Cheng West instruments science and technology Co., ltd.) is started to raise the temperature to 100 ℃ for use. Weighing polyethylene glycol according to the mass ratio, adding the polyethylene glycol into the compound alkali activator, primarily stirring and mixing, placing a beaker into a constant-temperature heating magnetic stirrer, adding a rotor of the tetrafluoro magnetic stirrer, adjusting the rotating speed to be 20r/min, and heating and stirring in a constant-temperature water bath for 3min. After the components are fully and uniformly mixed, the magnetic rotor is taken out, and the exciting agent is cooled to room temperature for later use, so that the sodium silicate-sodium phosphate composite exciting agent is obtained.
3) Weighing slag, fly ash and standard sand according to the mass ratio; firstly, adding the excitant cooled to room temperature into a stirring pot, then adding the weighed slag and fly ash, immediately starting a planetary mortar stirrer, and stirring at a low speed (140 +/-5 r/min) for 30s to mix uniformly. Adding standard sand into the stirring pot uniformly within the next 30s, taking care to prevent the standard sand from leaking out during the adding process of the standard sand, then adjusting the stirring machine to a high speed (280 +/-10 r/min), and stopping stirring after 30 s. And scraping the mortar on the inner wall of the stirring container and the blades into the middle of the pot by using a triangular scraper within 15s, manually mixing the mortar at the bottom of the pot uniformly, starting the machine, and continuously stirring for 60s at a high speed (280 +/-10 r/min) to obtain the slag fly ash-based alkali-activated cementing material. And then placing the prepared cementing material into a mold, curing for 24 hours under standard conditions to obtain a corresponding test piece, and carrying out a related performance test.
Comparative example 1
Without the incorporation of sodium phosphate and polyethylene glycol, water glass and solid sodium hydroxide were mixed and the water glass modulus Ms (SiO) was adjusted 2 /Na 2 Molar ratio of O) of 1.5, na in solution 2 The O content is 6wt% as the alkali activator of the comparative example, the mass part ratio of each component of the comparative example is shown in the table 2, and the preparation process is the same as that of the examples 1 to 8.
TABLE 2 raw material mass ratios (/ parts) of examples and comparative examples
The performance tests were performed for examples 1-8 and comparative example 1.
The fluidity, the compressive strength at 28d and the drying shrinkage at 60d of examples 1 to 8 and comparative example 1 were measured with reference to methods for measuring fluidity of cement mortar (GB/T2419-2005), method for testing strength of cement mortar (ISO method) (GB/T17671-1999), and method for testing dry shrinkage of cement mortar (JCT 603-2004), respectively. The results of the relevant performance tests for examples 1-8 and comparative example 1 are shown in Table 3.
Table 3 results of performance test of each example
As can be seen from the test results in Table 3, compared with comparative example 1, the drying shrinkage of examples 1-8 is significantly improved (the drying shrinkage micro strain of 60d is substantially maintained in the range of 1401-1543u epsilon, and can be reduced by 66% compared with the comparative example at most), and the fluidity of examples 1-8 is 185mm or more, which meets the requirements of the working performance of the mortar. The compression strength of the examples 1 to 8 is reduced compared with that of the comparative example, but the 28d compression strength is up to 72.5MPa, and still has higher mechanical property. In summary, example 8 has the best fluidity, the minimum dry shrinkage microstrain of 60d and the highest compressive strength of 28d, and can be used as a preferred example in building materials.
The compressive strength of examples 1-8 is reduced compared to that of comparative example 1, because the invention adopts water glass-sodium phosphate composite excitant and introduces PO 3 4 The ions can improve the viscosity of the water glass, hinder the hydrolysis of the water glass and reduce free SiO4 in the system 4 The quantity of-and OH < - > is reduced, so that the disintegration rate of the slag and the fly ash and the generation rate of calcium silicate hydrate gel are reduced, the hydration degree of the system is reduced, and the mechanical property of the slag fly ash-based alkali-activated cementing material is reduced.
According to the capillary pressure theory, a large amount of loose porous calcium silicate hydrate gel is generated on the slag particle surface which is not completely hydrated, the compactness degree of an alkali-activated gelling system can be reduced, the pore structure of a hydration product can be coarsened, the capillary pressure can be reduced by the coarser pore structure, and meanwhile, the polyethylene glycol molecules introduced by the method exist in the pore structure of the gel system, and the capillary pressure in pores can also be weakened. Therefore, the drying shrinkage of the composite alkali-activated gelling system can be effectively improved by the double shrinkage reduction effect of the phosphate ions and the polyethylene glycol molecules.
The foregoing is merely a preferred embodiment of the invention and is not intended to limit the invention in any manner; the present invention may be readily implemented by those of ordinary skill in the art as illustrated in the accompanying drawings and described above; however, those skilled in the art should appreciate that they can readily use the disclosed conception and specific embodiments as a basis for designing or modifying other structures for carrying out the same purposes of the present invention without departing from the scope of the invention as defined by the appended claims; meanwhile, any changes, modifications, and evolutions of the equivalent changes of the above embodiments according to the actual techniques of the present invention are still within the protection scope of the technical solution of the present invention.
Claims (10)
1. The slag fly ash-based alkali-activated cementing material is characterized by comprising the following raw material components in parts by weight: 300-330 parts of slag powder, 120-150 parts of fly ash, 95-105 parts of water glass, 20-25 parts of sodium hydroxide, 5-12 parts of sodium phosphate, 4-9 parts of polyethylene glycol, 100-120 parts of water and 1200-1250 parts of standard sand.
2. The slag fly ash-based alkali-activated cementitious material of claim 1, wherein the slag powder grade is S95 grade or above, and the density is not less than 2.8g/cm 3 The specific surface area is more than or equal to 400m 2 /kg。
3. The slag fly ash-based alkali-activated cementitious material of claim 1, wherein the fly ash is class F fly ash with fineness less than or equal to 25%.
4. The slag fly ash-based alkali-activated cementitious material of claim 1, wherein said water glass has a modulus of 3.0 to 3.3;
wherein: na (Na) 2 The content of O is 8-9wt%; siO 2 2 The content is 25-30wt%.
5. The slag fly ash-based alkali-activated cementitious material of claim 1, wherein the sodium hydroxide purity is greater than or equal to 98wt%; the sodium phosphate is trisodium phosphate dodecahydrate, and the purity is more than or equal to 98wt%.
6. The slag fly ash-based alkali-activated cementitious material of claim 1, wherein the polyethylene glycol has an average molecular mass of 1900 to 2200 and a pH of 4.0 to 7.0.
7. The slag fly ash-based alkali-activated cementitious material of claim 1, wherein the standard sand is SiO 2 The content is more than or equal to 98wt%, the moisture content is less than 0.2wt%, and the particle size range is 0.08-2mm.
8. The slag fly ash-based alkali-activated cementing material of claim 1, wherein the raw material components thereof comprise, in parts by weight: 310-330 parts of slag powder, 130-150 parts of fly ash, 95-100 parts of water glass, 20-25 parts of sodium hydroxide, 6-10 parts of sodium phosphate, 5-8 parts of polyethylene glycol, 105-115 parts of water and 1200-1250 parts of standard sand.
9. The slag fly ash-based alkali-activated cementitious material of claim 8, comprising the following raw material components in parts by weight: 325 parts of slag powder, 150 parts of fly ash, 97 parts of water glass, 25 parts of sodium hydroxide, 7.4 parts of sodium phosphate, 6.9 parts of polyethylene glycol, 107 parts of water and 1244 parts of standard sand.
10. The method for preparing the slag fly ash-based alkali-activated cementing material according to any one of the claims 1 to 9, which comprises the following specific steps:
1) Weighing various raw materials according to the mass ratio for later use;
2) Mixing and stirring the weighed water glass, sodium hydroxide particles, sodium phosphate and water uniformly to prepare a composite excitant;
3) Adding the weighed polyethylene glycol into the composite activator, heating to 80-100 ℃, keeping the temperature, stirring to fully and uniformly mix the polyethylene glycol and the composite activator, and then cooling to room temperature to obtain a sodium silicate-sodium phosphate composite activator;
4) Mixing the weighed slag, the weighed fly ash and the sodium silicate-sodium phosphate composite excitant, placing the mixture into a stirrer, and stirring the mixture for 30s at the autorotation speed of 140 +/-5 r/min; then adding the weighed standard sand, setting the rotation speed to 280 +/-10 r/min, stirring for 30s, and stopping; and (3) uniformly mixing the raw materials, setting the autorotation speed to be 280 +/-10 r/min, and stirring for 60s to obtain the slag fly ash-based alkali-activated cementing material.
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Application publication date: 20221101 |