CN108358519B - Alkali-activated fly ash slag conductive concrete with pressure-sensitive characteristic and preparation method thereof - Google Patents
Alkali-activated fly ash slag conductive concrete with pressure-sensitive characteristic and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/006—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing mineral polymers, e.g. geopolymers of the Davidovits type
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- 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
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- 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
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/50—Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength
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Abstract
The invention discloses alkali-activated fly ash slag conductive concrete with pressure-sensitive characteristics and a preparation method thereof, and relates to the technical field of concrete. The invention adjusts the conductivity of concrete and the performance of the material by adding a certain amount of carbon fiber and graphite, adds emulsified tetrasiloxane quaternary ammonium chloride solution as a dispersing agent, and adopts a graphite surface modifier to pretreat graphite powder. The carbon fiber and graphite are doped into the alkali-activated concrete, so that the overall mechanical property of the concrete is improved. The finally prepared concrete has small resistivity and stable conductivity, becomes a good conductive material, and has good stability along with the development of age on pressure sensitivity. The tetrasiloxane quaternary ammonium chloride salt emulsified solution can promote the dispersion of conductive materials such as carbon fibers and the like in the alkali-activated fly ash slag gelled material. Meanwhile, the graphite powder is pretreated, so that the hydrophilicity of the graphite can be enhanced, and the formation of a barrier film on the surface of the graphite or carbon black by the alkali-activated fly ash slag material is prevented.
Description
Technical Field
The invention relates to the technical field of concrete, in particular to alkali-activated fly ash slag conductive concrete with pressure-sensitive characteristics and a preparation method thereof.
Background
The concrete is a widely used building material, and has the advantages of convenient material acquisition, low price, high compressive strength, good moldability and the like. The alkali-activated fly ash-slag cementing material is a cementing material formed by reacting latent hydraulic raw material slag or fly ash with an alkali activator. The performances of the cementing material such as compression resistance, breaking strength, acid and alkali erosion resistance, freeze-thaw resistance, carbonization resistance and the like are superior to those of common portland cement. In addition, the alkali-activated slag fly ash cementing material has the advantages of simple preparation process, capability of treating a large amount of industrial waste residues, no need of firing, low energy consumption, low cost and wide market, and can be said to be an environment-friendly green material and be a cementing material with great development potential at present. This property can be used to gauge the health of the structure due to its good pressure sensitivity.
In the research of the hydration process of the alkali slag fly ash slag cementing material, the hydration heat curve is similar to that of ordinary portland cement, so that the hydration process of the alkali slag fly ash cement can be divided into five stages: the initial hydration phase, induction phase, acceleration phase, decay phase and finally the slow phase. Compared with the common cement concrete material, the alkali slag, fly ash and slag cementing material has the following characteristics: early strength, wherein the initial setting time is only 20-30 minutes; the structure is very compact, the strength is high but the elastic modulus is low. One very important application of conductive concrete is as a sensor for stress monitoring of structural members. However, since concrete itself contains aggregates such as sand and gravel, various defects such as holes and microcracks are inevitably present therein, and these defects cause a large error in the stress-resistivity curve finally generated. The alkali-activated material is selected to replace concrete to manufacture the conductive concrete, so that errors caused by defects of the base material can be avoided.
From the tests, we find that the preparation of the alkali-activated fly ash slag conductive concrete has the following difficulties: 1. the setting time is too short, the construction process of the conductive concrete is relatively complex compared with the common concrete, and the steps of pouring in different times, vibrating in different layers, placing electrodes and the like are involved, so that the setting time of the alkali-activated fly ash slag material is too short, and great difficulty is brought to construction. 2. The conductive material is difficult to disperse, and the alkali-activated fly ash slag material has a compact structure, high viscosity and poor fluidity, so that the additional conductive material such as carbon fiber, graphite, carbon black and the like is difficult to uniformly disperse in the alkali-activated fly ash slag matrix material. 3. In the experiment, the alkali-excited material can form a film around the powdery conductive material graphite, so that the mutual overlapping conduction of the powdery conductive material graphite is hindered, and the conductivity of the powdery conductive material graphite is greatly influenced.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention mainly aims to provide a preparation method of alkali-activated fly ash slag conductive concrete with pressure-sensitive characteristics.
The invention also aims to provide the alkali-activated fly ash slag conductive concrete with pressure-sensitive characteristics prepared by the preparation method.
The purpose of the invention is realized by the following technical scheme:
a preparation method of alkali-activated fly ash slag conductive concrete with pressure-sensitive characteristics comprises the following steps:
step A: preparation of test materials: the main materials are as follows: carbon fiber (the length of a monofilament is 3cm), natural graphite powder, tetrasiloxane quaternary ammonium chloride salt, dimethyl silicone oil, water glass, sodium hydroxide, fly ash, slag, tetraethyl silane, ethanol and deionized water;
and B: preparing an alkali activator: mixing water, water glass and sodium hydroxide according to the mass ratio of 100: 2: 4, mixing, stirring for 10-15 min, and standing for 24-28 h;
step C, performing surface treatment on natural graphite, namely mixing tetraethylsilane, ethanol and deionized water in a mass ratio of 1: 1: 2, stirring for 30-35 min, slowly dropwise adding 5 g/L hydrochloric acid solution until the pH value of the mixture is 2.4-2.6, continuously stirring for 1-1.2 h to obtain a graphite surface modifier, mixing graphite and the graphite surface modifier in a ratio of 1:0.2, placing the mixture in a planetary ball mill for ball milling for 30-35 min, taking out the mixture, placing the mixture in the air for 12-14 h, and drying the mixture at 100-120 ℃ for 6-8 h to obtain modified graphite;
step D: preparing a conductive material dispersant: the matching mass ratio is as follows: tetrasiloxane quaternary ammonium chloride salt: dimethyl silicone oil: deionized water 5:1: 15; putting the tetrasiloxane quaternary ammonium chloride salt and the dimethyl silicone oil into a glass beaker, and stirring for 2-3 min to enable the tetrasiloxane quaternary ammonium chloride salt and the dimethyl silicone oil to be in a uniform phase; then slowly adding water, and continuously stirring for 15-18 min; placing the mixture on an emulsifying machine, and emulsifying for 15-30 min at a rotating speed of 3000-3500 r/min to obtain a conductive material dispersing agent;
step E: dispersing the conductive material: mixing carbon fibers and a conductive material dispersing agent in a mass ratio of 1:1, and stirring for 3-4 min to fully disperse the carbon fibers to prepare a carbon fiber suspension; mixing the modified graphite and the conductive material dispersant in a mass ratio of 1:1.5, and stirring for 15-18 min to prepare a modified graphite suspension;
step F: preparing a conductive concrete member: the mass ratio of the fly ash to the slag is 7: 3-3.5, wherein the mass ratio of the ash body to the alkali activator is 1: 0.35 to 0.4; mixing the fly ash and the slag in a clean slurry stirrer, and dry-stirring for 2-3 min to fully mix the ash, adding an alkali activator, stirring for 4-5 min, adding a carbon fiber suspension and a modified graphite suspension, and stirring for 3-4 min to fully and uniformly mix the materials; pouring the mixture into a prepared mould for three times, vibrating the mixture on a vibrating table for 20-25 sec each time, and adjusting the position of an electrode at any time; after vibrating, lightly screeding the surface of the component by using a scraper;
step H: removing the mold and maintaining: curing the concrete after vibrating at 20 ℃ and 95% humidity for 24h, then demolding, and curing for 28d under the environmental condition; a final concrete element is obtained.
In the step (B), the step (A),
preferably, the stirring time is 10 min;
preferably, the standing time is 24 hours;
in the step C, the step C is carried out,
preferably, the stirring time is 30 min;
preferably, the pH is 2.5;
preferably, the continuous stirring time is 1 h;
preferably, the ball milling time is 30 min;
preferably, the time for placing in the air is 12 hours;
preferably, the drying condition is drying at 120 ℃ for 6 h;
in the step D, the step of the method is carried out,
preferably, the stirring time is 2 min;
preferably, the time for continuing stirring is 15 min;
preferably, the emulsification condition is emulsification for 15min at the rotating speed of 3000 r/min;
in the step E, the step of the method is carried out,
preferably, the stirring time after the carbon fibers and the conductive material dispersing agent are mixed is 3 min;
preferably, the time for stirring the modified graphite and the conductive material dispersant after mixing is 15 min;
in the step F, the step of the method is carried out,
preferably, the mass ratio of the fly ash to the slag is 7: 3;
preferably, the mass ratio of the ash body to the alkali activator is 1: 0.35;
preferably, the dry mixing time is 2 min;
preferably, the stirring time is 4 min;
preferably, the time for re-stirring is 3 min;
preferably, the vibration time is 20 sec.
The alkali-activated fly ash slag conductive concrete with the pressure-sensitive characteristic is prepared by the preparation method.
Compared with the prior art, the invention has the following advantages and effects:
the invention is based on the principle of preparing alkali-activated fly ash slag cementing material, breaks through the traditional alkali-activated material principle and the preparation method, and prepares the alkali-activated conductive concrete doped with carbon fiber and graphite. In the manufacturing process, a certain amount of carbon fiber and graphite are added to adjust the conductivity of concrete and the performance of the material, emulsified tetrasiloxane quaternary ammonium chloride solution is added to serve as a dispersing agent, and graphite powder is pretreated by a graphite surface modifier. The carbon fiber and graphite are doped into the alkali-activated concrete, so that the overall mechanical property of the concrete is improved. The finally prepared concrete has small resistivity and stable conductivity, becomes a good conductive material, and has good stability along with the development of age on pressure sensitivity. The tetrasiloxane quaternary ammonium chloride salt emulsified solution can promote the dispersion of conductive materials such as carbon fibers and the like in the alkali-activated fly ash slag gelled material. Meanwhile, the graphite powder is pretreated, so that the hydrophilicity of the graphite can be enhanced, and the formation of a barrier film on the surface of the graphite or carbon black by the alkali-activated fly ash slag material is prevented.
Drawings
FIG. 1 is a pressure-sensitive graph of alkali-activated fly ash slag conductive concrete.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the present invention is not limited thereto.
Example 1
Step A: test materials were prepared. The main materials for preparing the alkali-activated fly ash slag conductive concrete comprise: carbon fiber (the length of a monofilament is 3cm), natural graphite powder, tetrasiloxane quaternary ammonium chloride salt, dimethyl silicone oil, water glass, sodium hydroxide, fly ash, slag, tetraethyl silane, ethanol and deionized water.
And B: preparing the alkali activator. 100g of water, 2g of water glass and 4g of sodium hydroxide are stirred for 10min and then are kept stand for 24 h.
And step C, performing surface treatment on natural graphite, mixing 10g of tetraethyl silane, 10g of ethanol and 20g of deionized water, stirring for 30min, slowly dropwise adding 5 g/L hydrochloric acid solution until the pH value of the mixture is 2.5, continuously stirring for 1h to obtain a graphite surface modifier, mixing 50g of graphite and 10g of graphite surface modifier, putting the mixture in a planetary ball mill for ball milling for 30min, taking out the mixture, placing the mixture in the air for 12h, and drying the mixture in an oven at 120 ℃ for 6h to obtain the modified graphite.
Step D: a conductive material dispersant is disposed. Putting 15g of tetrasiloxane quaternary ammonium chloride salt and 3g of dimethyl silicone oil into a glass beaker, and stirring for 2min to enable the tetrasiloxane quaternary ammonium chloride salt and the dimethyl silicone oil to form a uniform phase; then 45g of water was slowly added and stirring was continued for 15 min. And (3) putting the mixture on an emulsifying machine to emulsify for 15min at the rotating speed of 3000r/min to obtain the conductive material dispersing agent.
Step E: a conductive material is dispersed. Mixing 10g of carbon fiber and 10g of conductive material dispersing agent, stirring for 3min to fully disperse the carbon fiber, and preparing carbon fiber suspension. And mixing 30g of modified graphite and 45g of conductive material dispersing agent, and stirring for 15min to prepare modified graphite suspension.
Step F: and preparing the alkali-activated conductive concrete member. 210g of fly ash, 90g of slag ash and 105g of alkali activator are weighed. Mixing the fly ash and the slag in a clean slurry stirrer, and dry-stirring for 2min to fully mix the ash, adding the alkali activator, stirring for 4min, adding the dispersed carbon fiber and graphite, and stirring for 3min to fully and uniformly mix the materials. The mixture was poured into prepared 40mm by 40mm molds in three portions, each of which was vibrated on a vibrating table for 20sec, and the electrode position was adjusted at any time. After the vibration is finished, the surface of the component is lightly smoothed by a scraper.
Step H: and (5) removing the mold and maintaining. And curing the concrete after vibrating at the temperature of 20 ℃ and the humidity of 95% for 24h, then demolding, and curing for 28d under the environmental condition. A final concrete element is obtained.
The sample number of the non-additive conductive material is G1, the conductive material is non-dispersed, and the sample number of the graphite which is not subjected to surface treatment is G2; the conductive material is not dispersed, but the sample number of the graphite subjected to surface treatment is G3; the conductive material was dispersed, and the graphite surface-treated sample was numbered G4. The compressive strength and resistivity of the four groups of samples are shown in table 1. The strength was tested according to the national standard GB/T17671-1999 and the resistivity was tested according to voltammetry.
TABLE 1 compressive Strength and resistivity of the G1-G4 samples
Sample numbering | Compressive strength (MPa) | Resistivity (omega. m) |
G1 | 60.8 | 358.4 |
G2 | 54.7 | 112.2 |
G3 | 55.2 | 31.8 |
G4 | 54.2 | 25.6 |
The experimental results show that the resistivity of the sample prepared by the construction process provided by the invention is greatly reduced. Meanwhile, as can be seen from the pressure-sensitive curve of fig. 1, the resistivity change curve of the sample (G4) with the surface treated conductive material is substantially linear with the compressive stress, which is greatly improved compared with the pressure-sensitive performance of G1, G2 and G3.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. A preparation method of alkali-activated fly ash slag conductive concrete with pressure-sensitive characteristics is characterized by comprising the following steps:
step A: preparation of test materials: the main materials are as follows: carbon fiber with the monofilament length of 3cm, natural graphite powder, tetrasiloxane quaternary ammonium chloride salt, dimethyl silicone oil, water glass, sodium hydroxide, fly ash, slag, tetraethyl silane, ethanol and deionized water;
and B: preparing an alkali activator: mixing water, water glass and sodium hydroxide according to the mass ratio of 100: 2: 4, mixing, stirring for 10-15 min, and standing for 24-28 h;
step C, performing surface treatment on natural graphite, namely mixing tetraethylsilane, ethanol and deionized water in a mass ratio of 1: 1: 2, stirring for 30-35 min, slowly dropwise adding 5 g/L hydrochloric acid solution until the pH value of the mixture is 2.4-2.6, continuously stirring for 1-1.2 h to obtain a graphite surface modifier, mixing graphite and the graphite surface modifier in a ratio of 1:0.2, placing the mixture in a planetary ball mill for ball milling for 30-35 min, taking out the mixture, placing the mixture in the air for 12-14 h, and drying the mixture at 100-120 ℃ for 6-8 h to obtain modified graphite;
step D: preparing a conductive material dispersant: the matching mass ratio is as follows: tetrasiloxane quaternary ammonium chloride salt: dimethyl silicone oil: deionized water 5:1: 15; putting the tetrasiloxane quaternary ammonium chloride salt and the dimethyl silicone oil into a glass beaker, and stirring for 2-3 min to enable the tetrasiloxane quaternary ammonium chloride salt and the dimethyl silicone oil to be in a uniform phase; then slowly adding water, and continuously stirring for 15-18 min; placing the mixture on an emulsifying machine, and emulsifying for 15-30 min at a rotating speed of 3000-3500 r/min to obtain a conductive material dispersing agent;
step E: dispersing the conductive material: mixing carbon fibers and a conductive material dispersing agent in a mass ratio of 1:1, and stirring for 3-4 min to fully disperse the carbon fibers to prepare a carbon fiber suspension; mixing the modified graphite and the conductive material dispersant in a mass ratio of 1:1.5, and stirring for 15-18 min to prepare a modified graphite suspension;
step F: preparing a conductive concrete member: the mass ratio of the fly ash to the slag is 7: 3-3.5, wherein the mass ratio of the ash body to the alkali activator is 1: 0.35 to 0.4; mixing the fly ash and the slag in a clean slurry stirrer, and dry-stirring for 2-3 min to fully mix the ash, adding an alkali activator, stirring for 4-5 min, adding a carbon fiber suspension and a modified graphite suspension, and stirring for 3-4 min to fully and uniformly mix the materials; pouring the mixture into a prepared mould for three times, vibrating the mixture on a vibrating table for 20-25 sec each time, and adjusting the position of an electrode at any time; after vibrating, lightly screeding the surface of the component by using a scraper;
step H: removing the mold and maintaining: curing the concrete after vibrating at 20 ℃ and 95% humidity for 24h, then demolding, and curing for 28d under the environmental condition; a final concrete element is obtained.
2. The method for preparing the alkali-activated fly ash slag conductive concrete with pressure-sensitive characteristics according to claim 1, wherein the method comprises the following steps:
in the step (B), the step (A),
the stirring time is 10 min;
the standing time is 24 hours.
3. The method for preparing the alkali-activated fly ash slag conductive concrete with pressure-sensitive characteristics according to claim 1, wherein the method comprises the following steps:
in the step C, the step C is carried out,
the stirring time is 30 min;
the pH value is 2.5;
the continuous stirring time is 1 h.
4. The method for preparing the alkali-activated fly ash slag conductive concrete with pressure-sensitive characteristics according to claim 1, wherein the method comprises the following steps:
in the step C, the step C is carried out,
the ball milling time is 30 min;
the time for placing in the air is 12 hours;
the drying condition is drying at 120 ℃ for 6 h.
5. The method for preparing the alkali-activated fly ash slag conductive concrete with pressure-sensitive characteristics according to claim 1, wherein the method comprises the following steps:
in the step D, the step of the method is carried out,
the stirring time is 2 min;
the time for continuing stirring is 15 min.
6. The method for preparing the alkali-activated fly ash slag conductive concrete with pressure-sensitive characteristics according to claim 1, wherein the method comprises the following steps:
in the step D, the step of the method is carried out,
the emulsification condition is that emulsification is carried out for 15min at the rotating speed of 3000 r/min.
7. The method for preparing the alkali-activated fly ash slag conductive concrete with pressure-sensitive characteristics according to claim 1, wherein the method comprises the following steps:
in the step E, the step of the method is carried out,
the carbon fibers and the conductive material dispersing agent are mixed and stirred for 3 min;
the time for stirring the modified graphite and the conductive material dispersant after mixing is 15 min.
8. The method for preparing the alkali-activated fly ash slag conductive concrete with pressure-sensitive characteristics according to claim 1, wherein the method comprises the following steps:
in the step F, the step of the method is carried out,
the mass ratio of the fly ash to the slag is 7: 3;
the mass ratio of the ash body to the alkali activator is 1: 0.35.
9. the method for preparing the alkali-activated fly ash slag conductive concrete with pressure-sensitive characteristics according to claim 1, wherein the method comprises the following steps:
in the step F, the step of the method is carried out,
the dry mixing time is 2 min;
the stirring time is 4 min;
the re-stirring time is 3 min;
the vibration time is 20 sec.
10. An alkali-activated fly ash slag conductive concrete with pressure-sensitive characteristics, which is characterized by being prepared by the preparation method of any one of claims 1 to 9.
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