CN114890705A - Micro silicon powder-based composite excitant for geopolymer grouting material and preparation method thereof - Google Patents
Micro silicon powder-based composite excitant for geopolymer grouting material and preparation method thereof Download PDFInfo
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 229920000876 geopolymer Polymers 0.000 title claims abstract description 58
- 239000011863 silicon-based powder Substances 0.000 title claims abstract description 54
- 239000000463 material Substances 0.000 title claims abstract description 52
- 239000002131 composite material Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 129
- 239000011734 sodium Substances 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000002994 raw material Substances 0.000 claims abstract description 16
- 229910021487 silica fume Inorganic materials 0.000 claims description 18
- 239000010881 fly ash Substances 0.000 claims description 15
- 230000000694 effects Effects 0.000 claims description 13
- 239000002245 particle Substances 0.000 claims description 12
- 239000003795 chemical substances by application Substances 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 7
- 229910019142 PO4 Inorganic materials 0.000 claims description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 6
- 239000010452 phosphate Substances 0.000 claims description 6
- 239000011159 matrix material Substances 0.000 claims description 2
- 230000007547 defect Effects 0.000 abstract description 3
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 20
- 239000003513 alkali Substances 0.000 description 18
- 235000019353 potassium silicate Nutrition 0.000 description 15
- 238000012360 testing method Methods 0.000 description 13
- 229910052710 silicon Inorganic materials 0.000 description 10
- 239000003518 caustics Substances 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 8
- 239000010703 silicon Substances 0.000 description 8
- 239000012190 activator Substances 0.000 description 7
- 239000002002 slurry Substances 0.000 description 7
- 239000004115 Sodium Silicate Substances 0.000 description 6
- 229910052782 aluminium Inorganic materials 0.000 description 6
- 238000006116 polymerization reaction Methods 0.000 description 6
- 229910052911 sodium silicate Inorganic materials 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 239000000203 mixture Substances 0.000 description 5
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 238000011049 filling Methods 0.000 description 4
- 229910052500 inorganic mineral Inorganic materials 0.000 description 4
- 239000011707 mineral Substances 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 239000000377 silicon dioxide Substances 0.000 description 4
- 235000012239 silicon dioxide Nutrition 0.000 description 4
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 238000003723 Smelting Methods 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 239000002956 ash Substances 0.000 description 3
- 238000005336 cracking Methods 0.000 description 3
- 238000004090 dissolution Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000011574 phosphorus Substances 0.000 description 3
- 229910052698 phosphorus Inorganic materials 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229910000519 Ferrosilicon Inorganic materials 0.000 description 2
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000015271 coagulation Effects 0.000 description 2
- 238000005345 coagulation Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 229910052909 inorganic silicate Inorganic materials 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 description 2
- 239000002910 solid waste Substances 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000010183 spectrum analysis Methods 0.000 description 2
- 239000012798 spherical particle Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 239000011398 Portland cement Substances 0.000 description 1
- 239000004111 Potassium silicate Substances 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- KMWBBMXGHHLDKL-UHFFFAOYSA-N [AlH3].[Si] Chemical class [AlH3].[Si] KMWBBMXGHHLDKL-UHFFFAOYSA-N 0.000 description 1
- CQBLUJRVOKGWCF-UHFFFAOYSA-N [O].[AlH3] Chemical compound [O].[AlH3] CQBLUJRVOKGWCF-UHFFFAOYSA-N 0.000 description 1
- OBNDGIHQAIXEAO-UHFFFAOYSA-N [O].[Si] Chemical compound [O].[Si] OBNDGIHQAIXEAO-UHFFFAOYSA-N 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 description 1
- 229910021486 amorphous silicon dioxide Inorganic materials 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 239000011083 cement mortar Substances 0.000 description 1
- 239000002734 clay mineral Substances 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000010459 dolomite Substances 0.000 description 1
- 229910000514 dolomite Inorganic materials 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000006253 efflorescence Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 239000003546 flue gas Substances 0.000 description 1
- 229910052587 fluorapatite Inorganic materials 0.000 description 1
- 229940077441 fluorapatite Drugs 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 238000001879 gelation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- VSIIXMUUUJUKCM-UHFFFAOYSA-D pentacalcium;fluoride;triphosphate Chemical compound [F-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O VSIIXMUUUJUKCM-UHFFFAOYSA-D 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 238000012643 polycondensation polymerization Methods 0.000 description 1
- NNHHDJVEYQHLHG-UHFFFAOYSA-N potassium silicate Chemical compound [K+].[K+].[O-][Si]([O-])=O NNHHDJVEYQHLHG-UHFFFAOYSA-N 0.000 description 1
- 229910052913 potassium silicate Inorganic materials 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 206010037844 rash Diseases 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 238000009864 tensile test Methods 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
Images
Classifications
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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
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
-
- 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
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/70—Grouts, e.g. injection mixtures for cables for prestressed concrete
-
- 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
Abstract
The invention discloses a micro silicon powder-based composite excitant for a geopolymer grouting material and a preparation method thereof, wherein the micro silicon powder-based composite excitant is prepared by taking micro silicon powder, sodium hydroxide and water as raw materials, and the dosage of the raw materials is as follows: water and sodium hydroxide (as Na) 2 O) is 5 to 20, and the micro silicon powder (calculated by SiO) 2 Calculated as Na) and sodium hydroxide (calculated as Na) 2 O) is 1-2, the micro silicon powder-based composite excitant can make up for the defects of the existing geopolymer excitant, the cost is low, the preparation operation is convenient, and the prepared geopolymer grouting material has excellent mechanical properties such as compressive strength and the like.
Description
Technical Field
The invention belongs to the technical field of constructional engineering, and particularly relates to a micro silicon powder-based composite excitant for a geopolymer grouting material and a preparation method thereof.
Background
Geopolymers (geopolymers) are three-dimensional network polymeric gelled materials composed of silicon-oxygen tetrahedrons and aluminum-oxygen tetrahedrons, which are formed by mineral condensation polymerization under high alkaline conditions by using natural minerals or solid wastes and artificial silicon-aluminum compounds as raw materials. Compared with portland cement, the geopolymer has the advantages of rich raw material source, simple preparation process, low production energy consumption, low discharge of three wastes, high strength, good durability, easily obtained raw materials, low cost and the like, and becomes a hot point for researching novel green cementing materials at home and abroad.
The alkali activator is a necessary condition for promoting the reaction of the silicon-aluminum raw materials to form the geopolymer, on one hand, the high-alkaline environment provided by the alkali activator accelerates the dissolution of Si and Al components in the raw materials, and on the other hand, the formation and solidification of geopolymer are promoted by the SiO4 with low polymerization degree in some alkali activators. Researchers at home and abroad have conducted a great deal of research and research on the reaction mechanism and working performance of activators such as caustic alkali, water glass, sodium hydroxide/silica fume, organic alkali, sodium carbonate and the like, and currently, the most common alkali activators include caustic alkali (sodium hydroxide or potassium hydroxide), water glass (sodium silicate or potassium silicate) and a mixture of caustic alkali and water glass. However, both caustic alkali and water glass have obvious defects in the using process, for example, the strong basicity of the caustic alkali can cause the dissolution of the silica-alumina material on the surface of the raw material and the subsequent polymerization reaction to be too violent, a small amount of formed geopolymer material is covered on the surface of the silica-alumina material more densely, the contact of the alkali activator and the raw material and the subsequent reaction are prevented from proceeding, and in addition, the strong basicity of the caustic alkali can cause the problems of late-stage efflorescence of the geopolymer grouting material and the like; compared with caustic alkali, the alkali of the sodium silicate solution is softer, but the sodium silicate solution is easy to undergo self-polymerization under the alkaline condition, so that the coagulation speed of the geopolymer grouting material is too fast and uncontrollable, the viscosity is too high, and the workability is poor.
The micro silicon powder is a superfine amorphous powder which is obtained by generating a large amount of high-volatility silicon dioxide and silicon gas in an ore-smelting electric furnace in ferrosilicon or industrial silicon smelting industry, quickly contacting air after the gas is discharged, oxidizing, condensing and precipitating, and recycling (dry discharging method) through dust removal environment-friendly equipment, wherein the main component of the superfine amorphous powder is silicon dioxide which is a tail gas byproduct of silicon smelting products and is industrial solid waste. Thousands of ferrosilicon and industrial silicon furnaces exist in China, and generate a large amount of micro silicon powder every year, which brings serious influence to the environment and economy. The main component of the micro silicon powder is amorphous silicon dioxide, the purity can reach more than 85%, the particle size is fine, the particle size is less than 1 mu m and accounts for more than 80%, the average particle size is 0.1-0.3 mu m, the micro silicon powder is 1/50-1/100 of common cement particles, the specific surface area is 15000-25000m2/kg, and the micro silicon powder is a superfine amorphous substance. The chemical components and the particle fineness of the micro silicon powder can be used as a high-activity pozzolanic admixture, so that the waste can be changed into valuable, and the resource recycling is promoted.
Disclosure of Invention
Based on the background, in order to improve the working performance and the cost performance of the geopolymer excitant and make up for the obvious defects of the most common alkaline excitants such as caustic alkali, water glass and the like used at present, the invention provides the micro silicon powder-based composite excitant for the geopolymer grouting material and the preparation method thereof.
The technical scheme of the invention is as follows:
the micro silicon powder-based composite excitant for the geopolymer grouting material is prepared by taking micro silicon powder, sodium hydroxide and water as raw materials, wherein the dosage of the raw materials is as follows: water and sodium hydroxide (as Na) 2 O) is 5 to 20, and the micro silicon powder (calculated by SiO) 2 Calculated as Na) and sodium hydroxide (calculated as Na) 2 Calculated as O) is 1-2.
Preferably, the water and sodium hydroxide (as Na) 2 O) is 20, and the micro silicon powder (calculated as SiO) 2 Calculated as Na) and sodium hydroxide (calculated as Na) 2 Calculated as O) is 1.
Preferably, the average particle size of the micro silicon powder is 0.2 um.
Preferably, the purity of the micro silicon powder is 85% -95%.
The invention also provides a preparation method of the micro silicon powder-based composite excitant for the geopolymer grouting material, which comprises the following steps:
1) taking micro silicon powder, sodium hydroxide and water according to the amount;
2) adding sodium hydroxide into water, stirring to prepare a sodium hydroxide solution, and then adding the micro silicon powder into the sodium hydroxide solution, and stirring;
3) the micro silicon powder and sodium hydroxide solution are put into a sealed high-temperature resistant container and heated for 10 to 15 hours at the temperature of 65 to 80 ℃ to prepare the micro silicon powder-based composite excitant.
The invention also provides a preparation method of the geopolymer grouting material, which is characterized in that the geopolymer grouting material prepared by the microsilica-based composite excitant is adopted.
Further, the geopolymer grouting material matrix material consists of fly ash and phosphate tailings.
Furthermore, the fly ash with low volcanic ash activity dug in a river channel is adopted as the fly ash.
Preferably, the weight ratio of the fly ash to the phosphate tailings is 0.5-1.5.
Compared with the prior art, the invention has the beneficial effects that:
1) the composite exciting agent prepared by the micro silicon powder and the sodium hydroxide can play a remarkable role in exciting and promoting the reaction process of the geopolymer, the high-alkalinity environment provided by the sodium hydroxide can enable Si and Al components in the raw materials to be dissolved out to provide a material base for the formation of the geopolymer, and the volcanic ash activity of the micro silicon powder and the filling effect of the micro aggregate play an important role in the gelation, reconstruction, polymerization, hardening and other stages of the geopolymer: on one hand, sodium silicate formed in the reaction process of the high-activity silica fume and sodium hydroxide can form SiO4 with low polymerization degree to promote the formation and solidification of geopolymer, and on the other hand, the special high activity and surface energy of the superfine silica fume enrich the peripheral free phase on the surface of the nano material, so that the dissolution rate of silicon and aluminum phases in an alkaline environment can be improved by forming a seed crystal nucleation effect, and the polymerization reaction is accelerated. In addition, residual silica fume particles after reaction with sodium hydroxide can be filled in gaps of geopolymers, so that the stacking compactness of the whole slurry system is high, and due to the superfine size characteristic of the silica fume particles, the micro aggregate filling effect can remarkably improve the contractibility, the macroscopic mechanical property, the chemical erosion resistance and the durability of geopolymer grouting materials and can also inhibit or reduce alkali aggregate reaction.
2) At present, most of water glass used as an excitant is stored for a long time, and the chemical composition of the water glass is easy to change and difficult to predict along with the time migration; the composite exciting agent is prepared only 24 hours before use, can effectively control the sodium silicate to be easily self-polymerized under the alkaline condition, has more stable chemical composition, controllable coagulation speed of the geopolymer grouting material and better viscosity and construction performance.
3) In addition, the most widely applied water glass excitant probably needs high temperature (dry method) of 1100-1200 ℃ or autoclaving reaction (wet method) under 2-3 atmospheric pressures in the industrial preparation process, and needs huge energy consumption.
Drawings
Fig. 1 is an energy spectrum/scanning electron microscope analysis of the microsilica of example 1 of the present invention, wherein fig. (a) is an energy spectrum plane scanning analysis result, and fig. (b) is a scanning electron microscope analysis result;
FIG. 2 shows the macro and micro morphologies of a geopolymer grouting material prepared by the composite exciting agent and water glass in example 1 of the invention; wherein (a), (b) and (c) are respectively the macro morphology of the geopolymer grouting material test block prepared by the composite exciting agent and the micro morphology under 150-time and 1000-time scanning electron microscope; (d) and (e) and (f) are respectively the macroscopic morphology of the geopolymer grouting material test block prepared by the water glass and the microscopic morphology of the geopolymer grouting material test block under a scanning electron microscope of 200 times and 2000 times.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the embodiments thereof; it should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1: in the embodiment, the micro silicon powder-based composite excitant is adopted to prepare the geopolymer grouting material
(1) The raw materials adopted in this example:
sodium hydroxide: the selected sodium hydroxide is purchased from Hebei Tongsheng chemical product sales Limited company, industrial grade, purity of 99 percent and sheet structure.
Silica fume: the selected silica fume is derived from the silica fume which is captured and collected in a flue gas duct of a certain steel plant, and the energy spectrum analysis shows that the main component of the silica fume is silicon dioxide, the purity is about 90 percent, and in addition, a small amount of carbon elements are contained (table 1); the silica fume is amorphous spherical particles under a scanning electron microscope, and has a smooth surface with an average particle diameter of about 0.2um (see table 2), and some of the silica fume is an aggregate formed by bonding a plurality of spherical particles together (see fig. 1).
Table 1: microsilica energy spectrum analysis result
| Element(s) | Weight (percentage) | Atom (percentage) |
| C | 8.79 | 13.09 |
| O | 60.04 | 67.08 |
| Si | 31.17 | 19.84 |
| Total amount of | 100 |
Table 2: particle size distribution of micro silicon powder
| Particle diameter/um | Percent/%) | Cumulative percent/%) |
| 0.2-0.4 | 18 | 18 |
| 0.4-0.6 | 30 | 48 |
| 0.6-0.8 | 14 | 62 |
| 0.8-1.0 | 9 | 71 |
| 1.0-1.2 | 7 | 78 |
| 1.2-1.4 | 6 | 84 |
| 1.4-1.6 | 6 | 90 |
| 1.6-1.8 | 6 | 96 |
| 1.8-2.0 | 4 | 100 |
In the embodiment, sodium hydroxide and silica fume with different proportions are adopted to prepare various composite exciting agents, and the quality of the composite exciting agents is compared with that of a geopolymer grouting material prepared from water glass with the same composition conditions, and the result is shown in table 3.
(2) The preparation steps of the composite excitant of the embodiment are as follows:
1) taking micro silicon powder, sodium hydroxide and water according to the amount;
2) adding sodium hydroxide into water, stirring to prepare a sodium hydroxide solution, and then adding the micro silicon powder into the sodium hydroxide solution, and stirring; after the micro silicon powder is mixed with the sodium hydroxide solution, an obvious exothermic process is generated (the exothermic temperature can exceed 80 ℃ at most).
3) The micro silicon powder and the sodium hydroxide solution are put into a sealed high-temperature resistant container and heated for 12 hours at 65-80 ℃ to ensure that the micro silicon powder and the sodium hydroxide fully react.
(3) The geopolymer grouting material in this example was prepared as follows:
1) preparing fly ash, phosphate tailings, an excitant and water into slurry, and then putting the slurry into a cement mortar stirrer for stirring;
2) analyzing the fluidity of the slurry by using a net slurry fluidity test model, and testing the water precipitation rate (calculus rate) of the slurry by using a measuring cylinder;
meanwhile, placing the grouting material into a triple mold for curing at room temperature, demolding after the slurry is initially solidified, placing the test block into a standard curing box (the curing temperature is 20 +/-2 ℃, and the relative humidity is more than 90 percent), and continuously curing for 28 days.
3) And testing the compressive strength of the test block by using an electronic tensile testing machine after the test block is maintained for 28 d.
4) The geopolymer grouting material is characterized from the aspects of element mineral composition, microstructure, functional group change and the like by means of an energy spectrum-scanning electron microscope (EDS-SEM), Fourier transform infrared spectroscopy (FTIR), an X-ray diffractometer (XRD) and the like (the result is shown in a table 3 and a figure 2), so that the micro reaction mechanism of the geopolymer grouting material can be researched.
The weight ratio of the fly ash to the phosphate tailings in this example is 0.5-1.5.
In this embodiment, the fly ash excavated from the river is selected as the fly ash, and the fly ash is seriously altered in clay minerals due to accumulation in the river for years, and part of sludge and organic carbon are mixed in the fly ash, so that the volcanic ash activity is obviously lower than that of the common fly ash, and thus the compressive strength of the geopolymer grouting material prepared by using the common activator (single caustic alkali, water glass, organic alkali and sodium carbonate) is generally poor.
The main mineral components of the used phosphorus tailings are dolomite, and a small amount of fluorapatite and quartz, the content of CaO is high but the content of silicon and aluminum is low, the phosphorus tailings can be mixed with raw materials with high content of silicon and aluminum but low content of calcium, such as fly ash and the like to form the optimal element proportion of the CaO-Al2O3-SiO2 ternary cementing material, so that the phosphorus tailings not only have the silicon and aluminum components required by geopolymers, but also meet the Ca required by the formation and hardening of the geopolymers 2+ 。
Table 3: micro silicon powder/sodium hydroxide composite excitant proportion and excitation effect
nH 2 O/nNa 2 O is water and sodium hydroxide (as Na) 2 Calculated as O), nSiO 2 /nNa 2 O is micro silicon powder (SiO) 2 Calculated as Na) and sodium hydroxide (calculated as Na) 2 Calculated as O).
From table 3, it is apparent that the 28-day compressive strength of the geopolymer grouting material prepared by the invention respectively reaches 4.5Mpa, 2.1Mpa and 25.5Mpa, which is obviously higher than the calculus body coring compressive strength 2Mpa after 3-6 months of grouting required by goaf filling and grouting, and except for the comparison test of serial number 1, the 28-day compressive strength of other geopolymer grouting materials prepared by the excitant of the invention is obviously higher than that prepared by water glass.
And it is obvious from the macro and micro morphology photographs of the prepared geopolymer grouting material shown in fig. 2 that the test block of the geopolymer grouting material prepared from water glass is very tightly cemented, but the phenomena of volume shrinkage and surface cracking can be observed (see fig. 2(d)), the phenomenon of cracks of the cementing material on the micro scale can also be observed under a scanning electron microscope (see fig. 2(e) and fig. 2(f)), and the cracking of the geopolymer is mainly caused by the drying shrinkage of the sodium silicate colloid. The geopolymer grouting material test block prepared by the composite exciting agent is very tightly cemented, the phenomenon of volume shrinkage and cracking is not observed (figure 2(a)), the phenomenon that the cementing material has obvious cracks under the microscale is not observed under a scanning electron microscope (figure 2(b) and figure 2(c)), and the accumulation compactness and the anti-shrinkage property of the geopolymer grouting material are improved mainly by analyzing the pozzolanic activity and the micro-aggregate filling effect of the micro-silica powder, so that the geopolymer grouting material prepared by the micro-silica powder/sodium hydroxide composite exciting agent has no obvious cracks, and the compression strength of the test block is very high.
The above description is only of the preferred embodiments of the present invention, and it should be noted that: it will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the principles of the invention and these are intended to be within the scope of the invention.
Claims (9)
1. The micro silicon powder-based composite excitant for the geopolymer grouting material is characterized by being prepared from micro silicon powder, sodium hydroxide and water as raw materials, wherein the dosage of the raw materials is as follows: water and sodium hydroxide (as Na) 2 O) is 5 to 20, and the micro silicon powder (calculated by SiO) 2 Calculated as Na) and sodium hydroxide (calculated as Na) 2 Calculated as O) is 1-2.
2. The micro silicon powder-based composite excitant for geopolymer grouting material as claimed in claim 1, characterized in that water and sodium hydroxide (as Na) 2 O) is 20, and the micro silicon powder (calculated as SiO) 2 Calculated as Na) and sodium hydroxide (calculated as Na) 2 Calculated as O) is 1.
3. The micro silicon powder-based composite excitant for the geopolymer grouting material as claimed in claim 1, wherein the average particle size of the micro silicon powder is 0.2 um.
4. The micro silicon powder-based composite excitant for the geopolymer grouting material as claimed in claim 1, wherein the purity of the micro silicon powder is 85% -95%.
5. A preparation method of a micro silicon powder-based composite excitant for a geopolymer grouting material is characterized in that,
which comprises the following steps:
1) taking micro silicon powder, sodium hydroxide and water according to the amount;
2) adding sodium hydroxide into water, stirring to prepare a sodium hydroxide solution, and then adding the micro silicon powder into the sodium hydroxide solution, and stirring;
3) the micro silicon powder and sodium hydroxide solution are put into a sealed high-temperature resistant container and heated for 10 to 15 hours at the temperature of 65 to 80 ℃ to prepare the micro silicon powder-based composite excitant.
6. A preparation method of a geopolymer grouting material is characterized in that the geopolymer grouting material prepared by the microsilica-based composite exciting agent of any one of claims 1 to 5 is adopted.
7. The method for preparing geopolymer grouting material of claim 6, characterized in that the matrix material is composed of fly ash and phosphate tailings.
8. The method for preparing the geopolymer grouting material as claimed in claim 7, wherein the fly ash is low in pozzolanic activity and is dug in a river channel.
9. The method for preparing the geopolymer grouting material as claimed in claim 7, wherein the weight ratio of the fly ash to the phosphate tailings is 0.5-1.5.
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| CN115818994A (en) * | 2022-11-22 | 2023-03-21 | 南通河海大学海洋与近海工程研究院 | Silica fume base alkali activator and preparation method thereof |
| CN116002999A (en) * | 2022-12-12 | 2023-04-25 | 福州大学 | Silica fume-based alkali solution-excited slag cement and preparation method and use method thereof |
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| CN113735472A (en) * | 2021-08-09 | 2021-12-03 | 中能化江苏地质矿产设计研究院有限公司 | Preparation of fly ash-phosphorus tailing sand-based cementing material and method for inhibiting saltpetering |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113735472A (en) * | 2021-08-09 | 2021-12-03 | 中能化江苏地质矿产设计研究院有限公司 | Preparation of fly ash-phosphorus tailing sand-based cementing material and method for inhibiting saltpetering |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115818994A (en) * | 2022-11-22 | 2023-03-21 | 南通河海大学海洋与近海工程研究院 | Silica fume base alkali activator and preparation method thereof |
| CN115818994B (en) * | 2022-11-22 | 2023-11-21 | 南通河海大学海洋与近海工程研究院 | Silica fume base alkali excitant and preparation method thereof |
| CN116002999A (en) * | 2022-12-12 | 2023-04-25 | 福州大学 | Silica fume-based alkali solution-excited slag cement and preparation method and use method thereof |
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