CN113045231B - Calcium-aluminum hydrotalcite structure geopolymer cement based on microwave curing and preparation method thereof - Google Patents
Calcium-aluminum hydrotalcite structure geopolymer cement based on microwave curing and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
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- C04B12/00—Cements not provided for in groups C04B7/00 - C04B11/00
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- 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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- 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
- C04B40/02—Selection of the hardening environment
- C04B40/0204—Selection of the hardening environment making use of electric or wave energy or particle radiation
- C04B40/0213—Electromagnetic waves
- C04B40/0218—Microwaves
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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
- C04B7/00—Hydraulic cements
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- C04B7/147—Metallurgical slag
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- 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
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- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/20—Resistance against chemical, physical or biological attack
- C04B2111/28—Fire resistance, i.e. materials resistant to accidental fires or high temperatures
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Abstract
The invention provides calcium-aluminum hydrotalcite structure geopolymer cement based on microwave curing and a preparation method thereof. The geopolymer cement containing the calcium-aluminum hydrotalcite structure can realize the massive utilization of silicon-aluminum solid waste materials, can also solidify chloride ions, and improves the durability and the anti-erosion capability of concrete in the service process. The geopolymer cement has wide raw material sources and strong operability, and can be used as a green cementing material for replacing cement.
Description
Technical Field
The invention relates to the technical field of preparation of green cementing materials, in particular to calcium-aluminum hydrotalcite structure geopolymer cement based on microwave curing and a preparation method thereof.
Background
The corrosion of the steel bars caused by the corrosion of the chloride is a main reason for causing the rust expansion and the cracking of the reinforced concrete structure. Every year, due to the use of a large amount of deicing salts containing chloride ions and the erosion of seawater and sea wind in coastal areas, a protective layer is peeled off after a large amount of concrete structures are in service, the service life is greatly shortened, and therefore huge economic losses are caused. In fact, the chloride ions do not directly participate in the generation of the tarnish but rather act as a catalyst. Chloride ions are immersed into the surface of the steel bar through the pores or the microcracks of the concrete, and when the concentration of the chloride ions around the steel bar is accumulated to reach a threshold value, an oxide film on the surface of the steel bar is damaged, so that the steel bar is corroded. Therefore, curing chloride ions is one of effective ways to improve the durability of reinforced concrete.
The hydrotalcite structure is a layered compound formed by a positively charged layer and negatively charged anions filled between layers. The anions between the layers can exchange with the anions in the external solution, so that the anions can be solidified. Based on the method, the invention provides novel geopolymer cement with a calcium-aluminum hydrotalcite structure and a preparation method thereof.
Disclosure of Invention
The invention aims to provide microwave curing-based calcium-aluminum hydrotalcite-structured geopolymer cement and a preparation method thereof, which utilize the calcium-aluminum hydrotalcite structure in the geopolymer cement to solidify chloride ions so as to solve the problem that a reinforced concrete structure is damaged in the service life period due to the corrosion of the chloride ions under various environmental conditions, and provide a new technical scheme for improving the durability of the reinforced concrete.
The technical scheme adopted by the invention for solving the technical problem is as follows: the microwave curing-based calcium-aluminum hydrotalcite-structured geopolymer cement comprises the following raw materials in percentage by mass: 50-60% of silicon-aluminum phase material, 12-15% of hydroxyl polymeric aluminum iron, 4-8% of calcium nitrate, 4-8% of sodium hydroxide, 17-22% of sodium metasilicate and 1-3% of steel slag.
Further, the silicon-aluminum phase material is a material rich in active silicon and aluminum elements, the silicon content is more than 35% and the aluminum content is more than 25% according to the mass percentage, and specifically, the silicon-aluminum phase material is one or a mixture of more of slag, fly ash, kaolin and the like.
Further, the hydroxyl polymeric aluminum-iron is hydroxyl polymeric aluminum-iron sulfate or hydroxyl polymeric aluminum-iron chloride, wherein the molar ratio Al: fe = 9.
Further, the steel slag is blast furnace steel slag, the main mineral components are dicalcium silicate, tricalcium silicate, ferric oxide, manganese oxide and a small amount of free calcium oxide, wherein the mass fraction of the ferric oxide is more than 20%, and the mass fraction of the manganese oxide is more than 2%.
The invention also provides a preparation method of geopolymer cement based on the composition, which comprises the following steps:
(1) Uniformly mixing raw materials such as a silicon-aluminum phase material, hydroxyl polymeric aluminum iron, calcium nitrate, sodium hydroxide, sodium metasilicate, steel slag and the like according to a proportion, and grinding to obtain a multi-element composite powder;
(2) Carrying out hydration reaction on the composite powder and water to obtain geopolymer cement slurry;
(3) After the geopolymer cement slurry is hardened, placing the slurry in microwave curing equipment for twice microwave curing, and finally obtaining a hardened body, namely the geopolymer cement with the calcium-aluminum hydrotalcite structure.
Further, the particle size of the mixed powder ground in the step (1) is less than 150 μm.
Furthermore, the water consumption in the step (2) is 40-55% of the mass of the composite powder.
Further, the hardening time of the geopolymerized cement slurry in the step (3) is 12 to 24 hours.
Further, in the step (3), the frequency of the microwave curing equipment is 900 MHz-6000 MHz, the time of the first microwave curing is 2-6 hours, after the first microwave curing is finished, the equipment is taken out and stands for 20-24 hours, then the second microwave curing is carried out, and the time of the second microwave curing is 1-3 hours.
The principle of the invention is as follows: the calcium nitrate and silicon-aluminum phase materials used in the invention contain rich Ca, al and other necessary elements for forming calcium-aluminum hydrotalcite (CaAl-LDHs); hydroxy polymeric aluminum iron, sodium hydroxide, sodium metasilicate can depolymerize the raw materials and release sufficient Al 3+ 、Ca 2+ Ions. At the same time, hydrolysis-depolymerization of aluminum-iron hydroxypolyate produces amorphous gel such as aluminum-hydroxide, iron-hydroxide and aluminum-iron-hydroxide copolymer, which can provide OH - And the group promotes the formation of the CaAl-LDHs structure. In addition, the gel can be dissolved again in a heating environment, and unreacted hydroxyl polymeric aluminum iron further participates in the CaAl-LDHs structural reaction, so that the CaAl-LDHs structure in the geopolymer cement is efficiently constructed in a secondary heating curing mode. Meanwhile, the steel slag has hydration characteristics, can react to produce hydrated calcium silicate, also has electrical characteristics, can improve the dielectric characteristics of geopolymer cement, and is beneficial to improving the microwave curing efficiency. In addition, NO in calcium nitrate 3 - The ions can be used for balancing surplus positive charges in a CaAl-LDHs structure, can replace invading chloride ions and improve the anti-corrosion capability of reinforced concrete.
The invention provides a green cementing material calcium-aluminum hydrotalcite structured geopolymer cement and a preparation method thereof, compared with the prior art, the green cementing material calcium-aluminum hydrotalcite structured geopolymer cement has the following beneficial effects:
(1) The geopolymer cement forms a calcium-aluminum hydrotalcite structure, has the characteristic that the geopolymer cement is different from portland cement, and has good mechanical property and high early strength;
(2) The invention can effectively cure chloride ions, even most heavy metal ions;
(3) The invention has wide raw material source, convenient manufacture and processing, high hardening speed and good durability, and has wide application prospect in the fields of civil engineering, heavy metal curing, high temperature resistance, fire prevention and the like.
Drawings
FIG. 1 is an X-ray diffraction pattern of geopolymer cement with calcium-aluminum hydrotalcite structure obtained by the present invention.
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 following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The microwave curing-based calcium-aluminum hydrotalcite-structured geopolymerized cement and the preparation method thereof are characterized in that the geopolymerized cement comprises the following raw materials in percentage by mass: 50-60% of silicon-aluminum phase material, 12-15% of hydroxyl polymeric aluminum iron, 4-8% of calcium nitrate, 4-8% of sodium hydroxide, 17-22% of sodium metasilicate and 1-3% of steel slag. The silicon-aluminum phase material is a material rich in active silicon and aluminum elements, the silicon content is more than 35 percent, the aluminum content is more than 25 percent according to the mass percentage, and the silicon-aluminum phase material is specifically one or a mixture of more of slag, fly ash, kaolin and the like. The hydroxyl polymeric aluminum-iron is hydroxyl polymeric aluminum-iron sulfate or hydroxyl polymeric aluminum-iron chloride, wherein the molar ratio of Al to Fe =9 is 1-1, the alkalization degree B is less than 2.5, the hydrolysis-polymerization effect is achieved, and the hydrolysis-polymerization product is hydroxyl polymeric aluminum, hydroxyl polymeric iron and hydroxyl aluminum-iron copolymer. The steel slag is blast furnace steel slag, the main mineral components are dicalcium silicate, tricalcium silicate, ferric oxide, manganese oxide and a small amount of free calcium oxide, wherein the mass fraction of the ferric oxide is more than 20%, and the mass fraction of the manganese oxide is more than 2%.
The preparation method of the geopolymer cement specifically comprises the following steps:
(1) Uniformly mixing a silicon-aluminum phase material, hydroxyl polymeric aluminum iron, calcium nitrate, sodium hydroxide, sodium metasilicate, steel slag and other raw materials in proportion, and grinding to obtain multi-element composite powder, wherein the particle size of the powder is less than 150 mu m; (2) Drying the multi-element composite powder, transferring the powder into a stirrer, adding tap water with the powder mass percent of 40-55%, stirring at the speed of 1000 revolutions per minute to obtain geopolymer cement slurry, and transferring the geopolymer cement slurry into a test mold; (3) And (3) after the cement is put into a mold and hardened for 12-24 hours, placing the cement in microwave curing equipment for microwave curing twice, wherein the microwave curing frequencies of 915MHz,2450MHz and 5800MHz are adopted, the first microwave curing time is 2-6 hours, the first microwave curing is finished, taking the cement out of the equipment, standing the cement for 20-24 hours, and then performing second microwave curing for 1-3 hours to finally obtain a hardened body, namely the geopolymer cement with the calcium-aluminum hydrotalcite structure.
Example 1:
(1) silicon-aluminum phase material: metakaolin, inner Mongolia super-brand kaolin factory;
(2) hydroxyl polymeric aluminum iron: hydroxypolyaluminum iron (basification degree 0.4, molar ratio Al: fe = 9;
(3) calcium nitrate: calcium nitrate tetrahydrate (analytical grade), shenyang chemical group Co., ltd;
(4) sodium hydroxide: sodium hydroxide (analytical grade), shenyang chemical group Co., ltd;
(5) sodium metasilicate: sodium metasilicate pentahydrate, sodium metasilicate nonahydrate, shenyang chemical group Co., ltd;
(6) steel slag: blast furnace slag, liaoning Hengwei group
TABLE 1 formulation of geopolymer cement of example 1
| Composition of | Silicon-aluminium phase material | Hydroxy polymeric aluminum iron | Calcium nitrate | Sodium hydroxide (NaOH) | Sodium metasilicate | Steel slag |
| Proportion (wt%) | 50％ | 15％ | 5％ | 8％ | 19％ | 3％ |
Firstly, removing impurities in metakaolin, drying at 105 ℃ for 2 hours, mixing and uniformly stirring raw materials such as a silicon-aluminum phase material, hydroxyl polymeric aluminum iron, calcium nitrate, sodium hydroxide, sodium metasilicate, steel slag and the like according to the mixing ratio shown in the table 1, and grinding the raw materials to be less than 150 micrometers. Drying the multi-element composite powder for 8 hours at 105 ℃, transferring the multi-element composite powder into a stirrer, adding tap water with the powder mass percent of 55%, stirring at the speed of 1000 revolutions per minute to obtain geopolymer cement slurry, demolding the test piece after hardening for 12 hours, and placing the test piece into microwave curing equipment for first microwave curing, wherein the microwave frequency is 915MHz, and the curing time is 6 hours; taking out and standing for 24 hours, and then performing secondary microwave curing, wherein the microwave frequency is 915MHz, and the curing time is 3 hours; the hardened body finally obtained is geopolymer cement with a calcium-aluminum hydrotalcite structure.
TABLE 2 mechanical Properties of Geopolymeric cements example 1
| Index (I) | Compressive strength (3 d) | Compressive strength (7 d) | Compressive strength (14 d) | Compressive strength (28 d) |
| As a result, the | 41.7MPa | 44.8MPa | 45.6MPa | 46.4MPa |
The 28-day sample was pulverized and subjected to X-ray diffraction analysis (XRD), and the analysis results are shown in fig. 1. The product of geocement is a structure in which an amorphous aluminosilicate compound coexists with a crystal structure of calcium aluminum hydrotalcite. It can be clearly seen that the geopolymer cement prepared has an amorphous peak. Multiple diffraction peaks appear on the amorphous peak, indicating that a new crystalline product, calcium aluminium hydrotalcite (nitrate insertion type), is produced upon polymerisation of the geopolymer. This shows that the prepared geopolymer cement contains typical calcium-aluminum hydrotalcite structure.
Example 2:
(1) silicon-aluminum phase material: fly ash, shenyang green building fly ash;
(2) hydroxyl polymeric aluminum iron: aluminum iron hydroxypolyide (degree of alkalization 1.6, molar ratio Al: fe = 1;
(3) calcium nitrate: calcium nitrate tetrahydrate (analytical grade), shenyang chemical group Co., ltd;
(4) sodium hydroxide: sodium hydroxide (analytical grade), shenyang chemical group Co., ltd;
(5) sodium metasilicate: sodium metasilicate pentahydrate, sodium metasilicate nonahydrate, shenyang chemical group Co., ltd;
(6) steel slag: blast furnace slag, liaoning Hengwei group
TABLE 3 mixing ratio of Geopolymeric cement example 2
| Composition of | Silicon-aluminium phase material | Hydroxy polymeric aluminum iron | Calcium nitrate | Sodium hydroxide | Sodium metasilicate | Steel slag |
| Proportion (wt%) | 60％ | 12％ | 4％ | 4％ | 17％ | 3％ |
Firstly, removing impurities in the fly ash, drying the fly ash for 2 hours at 105 ℃, mixing and uniformly stirring raw materials such as a silicon-aluminum phase material, hydroxyl polymeric aluminum iron, calcium nitrate, sodium hydroxide, sodium metasilicate, steel slag and the like according to the mixture ratio in the table 3, and grinding the raw materials to be less than 150 micrometers. Drying the multi-element composite powder at 105 ℃ for 8 hours, transferring the multi-element composite powder into a stirrer, adding tap water with the powder mass percent of 40%, stirring at the speed of 1000 revolutions per minute to obtain geopolymer cement slurry, demolding the hardened test piece after 12 hours, and placing the test piece into microwave curing equipment for first microwave curing, wherein the microwave frequency is 2450MHz, and the curing time is 4 hours; standing for 24 hours after taking out, and performing secondary microwave curing, wherein the microwave frequency is 2450MHz, and the curing time is 2 hours; the hardened body finally obtained is geopolymer cement with a calcium-aluminum hydrotalcite structure.
TABLE 4 mechanical Properties of Geopolymeric Cement example 2
| Index (I) | Compressive strength (3 d) | Compressive strength (7 d) | Compressive strength (14 d) | Compressive strength (28 d) |
| Results | 47.4MPa | 50.3MPa | 51.6MPa | 52.8MPa |
Example 3:
(1) silicon-aluminum phase material: slag, heavy industry slag micropowder of Shenyang;
(2) hydroxyl polymeric aluminum iron: hydroxypolyaluminum iron, (degree of alkalization 1.1, molar ratio Al: fe = 4);
(3) calcium nitrate: calcium nitrate tetrahydrate (analytical grade), shenyang chemical group Co., ltd;
(4) sodium hydroxide: sodium hydroxide (analytical grade), shenyang chemical group Co., ltd;
(5) sodium metasilicate: sodium metasilicate pentahydrate, sodium metasilicate nonahydrate, shenyang chemical group Co., ltd;
(6) steel slag: blast furnace slag, liaoning Hengwei group
TABLE 5 formulation ratio of Geopolymeric cement of example 3
| Composition of | Silicon-aluminium phase material | Hydroxy polymeric aluminum iron | Calcium nitrate | Sodium hydroxide (NaOH) | Sodium metasilicate | Steel slag |
| Proportion (wt%) | 51％ | 12％ | 8％ | 4％ | 22％ | 3％ |
Firstly, removing impurities in slag, drying the slag for 2 hours at 105 ℃, mixing and uniformly stirring raw materials such as a silicon-aluminum phase material, hydroxyl polymeric aluminum iron, calcium nitrate, sodium hydroxide, sodium metasilicate, steel slag and the like according to the mixture ratio of Table 5, and grinding the raw materials to be less than 150 micrometers. Drying the multi-element composite powder for 8 hours at 105 ℃, transferring the multi-element composite powder into a stirrer, adding tap water with the powder mass percent of 48%, stirring at the speed of 1000 revolutions per minute to obtain geopolymer cement slurry, demolding the hardened test piece after 12 hours, and placing the test piece into microwave curing equipment for first microwave curing, wherein the microwave frequency is 5800MHz, and the curing time is 2 hours; taking out and standing for 24 hours, and then carrying out secondary microwave curing, wherein the microwave frequency is 5800MHz, and the curing time is 1 hour; the hardened body finally obtained is geopolymer cement with a calcium-aluminum hydrotalcite structure.
TABLE 6 mechanical Properties of Geopolymeric Cement example 3
| Index (es) | Compressive strength (3 d) | Compressive strength (7 d) | Compressive strength (14 d) | Compressive strength (28 d) |
| As a result, the | 46.4MPa | 49.7MPa | 51.2MPa | 51.8MPa |
The technical idea of the present invention is described in the above technical solutions, and the protection scope of the present invention is not limited thereto, and any changes and modifications made to the above technical solutions according to the technical essence of the present invention belong to the protection scope of the technical solutions of the present invention.
Claims (6)
1. The microwave curing-based calcium-aluminum hydrotalcite-structured geopolymer cement is characterized by comprising the following raw materials in percentage by mass: 50-60% of silicon-aluminum phase material, 12-15% of hydroxyl polymeric aluminum iron, 4-8% of calcium nitrate, 4-8% of sodium hydroxide, 17-22% of sodium metasilicate and 1-3% of steel slag; the microwave curing is twice microwave curing;
the silicon-aluminum phase material is a material rich in active silicon and aluminum elements, the silicon content is more than 35 percent, the aluminum content is more than 25 percent according to the mass percentage, and the silicon-aluminum phase material is specifically one or a mixture of more of slag, fly ash and kaolin;
the hydroxyl polymeric aluminum iron is hydroxyl polymeric aluminum ferric sulfate or hydroxyl polymeric aluminum ferric chloride, wherein the molar ratio Al: fe = 9;
the frequency of the microwave curing equipment is 900MHz to 6000MHz, the time of first microwave curing is 2 to 6 hours, the first microwave curing is finished, the equipment is taken out and stands for 20 to 24 hours, then the second microwave curing is carried out, and the time of the second microwave curing is 1 to 3 hours.
2. The microwave curing-based calcium-aluminum hydrotalcite structured geopolymer cement as claimed in claim 1, wherein the main mineral components are dicalcium silicate, tricalcium silicate, ferric oxide, manganese oxide and a small amount of free calcium oxide, wherein the mass fraction of ferric oxide is more than 20%, and the mass fraction of manganese oxide is more than 2%.
3. The preparation method of the microwave curing-based calcium-aluminum hydrotalcite-structured geopolymer cement according to any one of claims 1 to 2, which is characterized by comprising the following steps:
(1) Uniformly mixing a silicon-aluminum phase material, hydroxyl polymeric aluminum iron, calcium nitrate, sodium hydroxide, sodium metasilicate and a steel slag raw material in proportion, and grinding to obtain a multi-element composite powder;
(2) Carrying out hydration reaction on the composite powder and water to obtain geopolymer cement slurry;
(3) After the geopolymer cement slurry is hardened, placing the slurry in microwave curing equipment for microwave curing twice, and finally obtaining a hardened body, namely the geopolymer cement with the calcium-aluminum hydrotalcite structure.
4. The method for preparing calcium-aluminum hydrotalcite-structured geopolymer cement based on microwave curing as claimed in claim 3, wherein the mixed powder ground in step (1) has a particle size of less than 150 μm.
5. The microwave curing-based preparation method of calcium-aluminum hydrotalcite-structured geopolymer cement according to claim 3, wherein the water consumption in the step (2) is 40-55% of the mass of the composite powder.
6. The preparation method of the calcium aluminum hydrotalcite-structured geopolymer cement based on microwave curing as claimed in claim 3, wherein the hardening time of the geopolymer cement slurry in the step (3) is 12 to 24 hours.
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