CN110759656A - Normal-temperature single red mud geopolymer and preparation method thereof - Google Patents
Normal-temperature single red mud geopolymer 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
- C04B12/00—Cements not provided for in groups C04B7/00 - C04B11/00
- C04B12/005—Geopolymer cements, e.g. reaction products of aluminosilicates with alkali metal hydroxides or silicates
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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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- 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
- C04B2111/00017—Aspects relating to the protection of the environment
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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
- 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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- 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
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Abstract
The invention discloses a normal-temperature single red mud geopolymer and a preparation method thereof, relating to the technical field of solid waste recycling and novel building material preparation; comprises the following raw materials: bayer process red mud, an alkali activator and water, wherein the total Si/Al atomic molar ratio in all raw materials is 1.4, the Na/Al atomic molar ratio is 2.0-2.4, the mass ratio of the water to the solid is 0.7, and the alkali activator is a mixed solution prepared by analyzing and purifying water glass solution and sodium hydroxide; the compressive strength of the single red mud geopolymer prepared at normal temperature is 28d and can reach more than 35MPa, the problem that the intensity of the geopolymer is reduced due to the increase of the mixing amount of the red mud in the production of the geopolymer is solved, the single red mud is used as a material, the geopolymer is prepared at normal temperature, the preparation process is simple, the industrial production is easy to realize, and the method has a positive promotion effect on reducing the harm of the red mud to the environment and the resource utilization of the red mud.
Description
Technical Field
The invention relates to the technical field of solid waste recycling and novel building material preparation, in particular to a normal-temperature single red mud geopolymer and a preparation method thereof.
Background
Red mud is an insoluble solid residue produced after bauxite is melted by caustic soda solution in the production process of alumina, and causes serious pollution to the environment.
In order to minimize the damage of red mud to the environment, a great deal of effort has been put into developing the way of resource utilization of red mud. At present, the red mud can be utilized on a large scale, and the most potential way is to utilize the red mud to produce building materials. The most predominant of the building materials produced from red mud are geopolymer materials. The geopolymer is an alkali-activated cementing material, and is a high-performance cementing material prepared by taking a silicon-aluminum material as a main raw material and activating potential activity of alkali on the raw material. However, since the red mud has large fluctuation of components and performance, it is found that a single red mud has insufficient reactivity in the synthesis of geopolymers, and therefore, the red mud is usually mixed with aluminosilicate materials with stronger reactivity, mainly fly ash, metakaolin, silica powder, slag and the like, so that the mixing amount of the red mud is reduced, and the red mud is difficult to be utilized on a large scale through a way of preparing geopolymers. In actual production, the negative effect is brought by simply increasing the content of the red mud, namely, the strength of the whole polymer is reduced.
Disclosure of Invention
The invention overcomes the defects of the prior art, provides a normal-temperature single red mud geopolymer and a preparation method thereof, and solves the problem of the decrease of the intensity of the geopolymer caused by increasing the mixing amount of red mud in the production of the geopolymer.
In order to achieve the above object, the present invention is achieved by the following technical solutions.
A normal-temperature single red mud geopolymer comprises the following raw materials in parts by weight: 95-110 parts of Bayer process red mud, 115-124 parts of alkali activator and 3-7 parts of water, wherein the total Si/Al atomic molar ratio in all raw materials is 1.4, the Na/Al atomic molar ratio is 2.0-2.4, the mass ratio of water to solid is 0.7, and the alkali activator is a mixed solution prepared by analyzing and purifying water glass solution and sodium hydroxide.
Preferably, the weight part of the water glass solution is 98 parts, and the analytically pure weight part of sodium hydroxide is 17-26 parts.
Preferably, the atomic molar ratio of Si/Al in the raw material is 1.4 and the atomic molar ratio of Na/Al is 2.2.
A preparation method of a normal-temperature single red mud geopolymer specifically comprises the following steps:
a) raw material treatment: drying and crushing Bayer process red mud, sieving to prepare red mud powder, and drying.
b) Sample preparation: weighing corresponding Bayer process red mud according to the parts by mass, adding the Bayer process red mud into a stirrer for stirring at the rotating speed of 150r/min, stirring for 2min, adding an alkali activator after solid materials are uniformly stirred, and continuously stirring for 3min at the rotating speed of 150r/min, so that the solid materials and liquid materials are completely and uniformly stirred to form geopolymer precursor slurry.
c) And (5) maintenance: adding the slurry into a mold, placing the mold on a vibration table for vibration for 20s, scraping the surface of the mold, sealing the mold, removing the mold after 24h, and placing the test block into normal temperature (20-25 ℃) for curing to obtain the geopolymer.
The main minerals in the red mud raw material comprise cancrinite ore, garcinite, hematite, calcite, gibbsite and the like, and the XRD map shows that the red mud raw material has sharp peaks and no obvious humps, which indicates that the red mud raw material contains few amorphous phase substances. Wherein cancrinite ore is one of feldspar-like minerals, and is alkaline aluminosilicate ore, wherein red mud is prepared by mixing multiple cancrinite minerals. The red mud is dissolved in high-alkaline water glass solution by using soluble aluminosilicate which contains less amount, so that structural units of silicon-oxygen tetrahedron and aluminum-oxygen tetrahedron are formed, and finally, polycondensation reaction is carried out, so as to form geopolymer with three-dimensional network structure.
As shown in FIG. 1, the XRD pattern of red mud geopolymer formed by the process of the present invention generates zeolite-like minerals with high strength characteristics relative to red mud, which are similar to the rock in the crust of the earth. The zeolite mineral is OH in strong alkaline environment-And the silicon-aluminum component in the red mud. The substances have chain structures similar to organic polymers and can be matched with [ SiO ] on the surfaces of mineral particles4]4-And [ AlO ]4]4-The tetrahedron forms chemical bonds by dehydroxylation, which is a direct reason for its high strength, and also determines its excellent physicochemical properties. In the research, the generated zeolite mineral has a direct relation with the silicon-aluminum ratio in the raw material, the combined form of the silicon-aluminum ratio is related with the sufficiency of the reaction, and for a single red mud, the Si/Al atomic molar ratio and the Na/Al atomic molar ratio have great influence on the generated amount and the stability of the zeolite mineral, in the figure 1, the Si/Al atomic molar ratio is 1.4, the diffraction peak is firstly increased and then decreased along with the increase of Na/Al, the diffraction peak of Na/Al is 2.2 is the largest, and the compressive strength of the single red mud polymer is indirectly proved to be the best.
Compared with the prior art, the invention has the beneficial effects that.
(1) The invention adopts single red mud as the raw material of the geopolymer, has low price and wide source, can reduce the stacking amount of the red mud and reduce the harm of the red mud to the environment.
(2) According to the invention, through strictly limiting the silicon-aluminum ratio and the sodium-aluminum ratio in the raw materials, the compressive strength of the prepared single red mud geopolymer can reach more than 35MPa in 28 days, the requirement of building materials is met, and a new way for red mud resource utilization is developed.
(3) The invention is a polymer material prepared and maintained at normal temperature, has simple preparation process and is easy to realize industrial production.
Drawings
FIG. 1 shows XRD patterns of red mud and geopolymer samples prepared at Si/Al atomic molar ratios of 1.4 and Na/Al atomic molar ratios of 2.0, 2.2 and 2.4, respectively.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects to be solved by the present invention more clearly apparent, the present invention is further described in detail with reference to the embodiments and the accompanying drawings. 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 technical solution of the present invention is described in detail below with reference to the embodiments and the drawings, but the scope of protection is not limited thereto.
(1) Selecting and processing raw materials:
the used materials comprise Bayer process red mud of Shanxi Hejin aluminum works, and the chemical components of the Bayer process red mud are shown in Table 1.
Table 1 chemical composition of bayer process red mud.
The water glass solution is commercial industrial water glass (SiO)2Content of 24.73%, Na2O content 8.17%, modulus 3.12, baume degree 40, density 1.375g/cm3) The sodium hydroxide is analytically pure sodium hydroxide sold on the market, the purity is over 99 percent, and the distilled water is prepared by adopting laboratory distillation equipment.
(2) Processing raw materials:
naturally drying Bayer process red mud in the air, crushing by a crusher, and sieving by a sieve of 0.075 mm; drying the crushed and sieved red mud powder in an oven at 105 ℃ for 24h to obtain the red mud raw material with the specific surface area average particle size of 2.64 mu m and the specific surface area of 2270m2/kg)。
Weighing 1000g of Bayer process red mud according to the mass for later use;
an aqueous glass solution, sodium hydroxide analytical reagent and distilled water were calculated and named according to the set Si/Al (atomic molar ratio of Si/Al in the raw material is 1.4), Na/Al (atomic molar ratio of Na/Al in the raw material is 2.0, 2.1, 2.2, 2.3, 2.4, respectively) and water-to-solid mass ratio (mass ratio of water to solid is 0.7, mass of water includes the sum of mass of water added to the aqueous glass solution and mass of distilled water added to the raw material, mass of solid includes Bayer process red mud), wherein the aqueous glass solution is 980g, the distilled water is 50g, and analytical reagent of sodium hydroxide is 170g, 200g, 220g, 240g, 260g, respectively.
Respectively adding 170g, 200g, 220g, 240g and 260g of sodium hydroxide analytically pure into 5 980g water glass solutions, respectively adding 50g of distilled water into 5 980g water glass solutions to obtain alkali-activated solutions under different Na/Al conditions, after the alkali-activated solutions are cooled to room temperature, adding water lost due to heat release, and controlling the mass ratio of water to solid to be 0.7 for later use.
(3) Sample preparation and maintenance:
adding Bayer process red mud into a stirrer for stirring at a rotation speed of 150r/min for 2min, adding the alkali excitation solution into the stirrer after solid materials are uniformly stirred, and continuously stirring for 3min at a rotation speed of 150r/min to ensure that the solid materials and the liquid materials are completely and uniformly stirred to form geopolymer precursor slurry.
Adding the slurry into a triple square steel die with the side length of 40mm, placing the triple square steel die on a vibration table, vibrating for 20s, scraping the surface of the die by using a scraper, sealing a steel film by using a plastic film, removing the die after 24h, and placing a test block into normal temperature (20-25 ℃) for maintenance.
And (3) testing the strength of the sample: the compressive strength of the polymer test blocks was tested at 7d, 14d, 21d, 28d age, with a test rate of 2 mm/min.
The strength of the monochite geopolymer at 4 ages for the 5 formulations is shown in Table 2.
Table 2 compressive strengths of polymers of single red mud at different ages.
As can be seen from Table 2, the strength of the geopolymer produced was different in terms of the atomic molar ratio of Na/Al, while controlling the atomic molar ratio of Si/Al to 1.4, when the amount of Bayer process red mud was 100 parts. When the atomic mole of Na/Al is 2.2, namely the analytically pure sodium hydroxide content is 22 parts, the strength of a single red mud polymer is optimal at each age, the 7d compressive strength can reach 28.24MPa, and the 28d compressive strength can reach 37.77 MPa.
FIG. 1 shows XRD patterns of red mud and geopolymer samples prepared at Si/Al atomic molar ratios of 1.4 and Na/Al atomic molar ratios of 2.0, 2.2 and 2.4, respectively.
The main minerals in the red mud raw material comprise cancrinite ore, cancrinite, hematite, calcite, gibbsite and the like, and the displayed minerals are sharp peaks without obvious humps, which indicates that the amorphous phase substances are not much. Wherein cancrinite ore is one of feldspar-like minerals, and is alkaline aluminosilicate ore, wherein red mud is prepared by mixing multiple cancrinite minerals.
The XRD pattern of the red mud geopolymer formed by the method generates zeolite minerals relative to the red mud, and the zeolite minerals have the characteristic of high strength similar to rocks in the crust of the earth. The zeolite mineral is OH in strong alkaline environment-And the silicon-aluminum component in the red mud. The substances have chain structures similar to organic polymers and can be matched with [ SiO ] on the surfaces of mineral particles4]4-And [ AlO ]4]4-The tetrahedron forms chemical bonds by dehydroxylation, which is a direct reason for its high strength, and also determines its excellent physicochemical properties. In the research, the generated zeolite mineral has a direct relation with the silicon-aluminum ratio in the raw material, the combined form of the silicon-aluminum ratio is related with the sufficiency of the reaction, and for a single red mud, the Si/Al atomic molar ratio and the Na/Al atomic molar ratio have great influence on the generated amount and the stability of the zeolite mineral, in the figure 1, the Si/Al atomic molar ratio is 1.4, the diffraction peak is firstly increased and then decreased along with the increase of Na/Al, the diffraction peak of Na/Al is 2.2 is the largest, and the compressive strength of the single red mud polymer is indirectly proved to be the best.
While the invention has been described in further detail with reference to specific preferred embodiments thereof, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (4)
1. The normal-temperature single red mud geopolymer is characterized by comprising the following raw materials in parts by weight: 95-110 parts of Bayer process red mud, 115-124 parts of alkali activator and 3-7 parts of water, wherein the total Si/Al atomic molar ratio in all raw materials is 1.4, the Na/Al atomic molar ratio is 2.0-2.4, the mass ratio of water to solid is 0.7, and the alkali activator is a mixed solution prepared by analyzing and purifying water glass solution and sodium hydroxide.
2. A room temperature single red mud geopolymer as claimed in claim 1, wherein the water glass solution is 98 parts by weight, and the sodium hydroxide analytically pure is 17-26 parts by weight.
3. An ordinary-temperature single red mud polymer as defined in claim 1, wherein the raw material has an atomic mole ratio of Si/Al of 1.4 and an atomic mole ratio of Na/Al of 2.2.
4. The preparation method of the normal-temperature single red mud geopolymer as claimed in claim 1, which is characterized by comprising the following steps:
a) raw material treatment: drying and crushing Bayer process red mud, sieving to prepare red mud powder, and drying;
b) sample preparation: weighing corresponding Bayer process red mud according to the parts by mass, adding the Bayer process red mud into a stirrer for stirring at the rotating speed of 150r/min, stirring for 2min, adding an alkali activator after solid materials are uniformly stirred, and continuously stirring for 3min at the rotating speed of 150r/min to ensure that the solid materials and liquid materials are completely and uniformly stirred to form geopolymer precursor slurry;
c) and (5) maintenance: adding the slurry into a mold, placing the mold on a vibration table for vibration for 20s, scraping the surface of the mold, sealing the mold, removing the mold after 24h, and placing the test block at the normal temperature of 20-25 ℃ for curing to obtain the geopolymer.
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CN115093244A (en) * | 2022-07-05 | 2022-09-23 | 中国矿业大学(北京) | Fireproof heat-insulating material and preparation method thereof |
CN116813257A (en) * | 2023-07-05 | 2023-09-29 | 中冀建勘集团有限公司 | Red mud and fly ash geopolymer material capable of being used for pumping and underwater pouring, preparation method and construction process |
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CN116813257A (en) * | 2023-07-05 | 2023-09-29 | 中冀建勘集团有限公司 | Red mud and fly ash geopolymer material capable of being used for pumping and underwater pouring, preparation method and construction process |
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