CN110803890A - High-red-mud-content geopolymer and preparation method thereof - Google Patents
High-red-mud-content geopolymer and preparation method thereof Download PDFInfo
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- CN110803890A CN110803890A CN201911137338.0A CN201911137338A CN110803890A CN 110803890 A CN110803890 A CN 110803890A CN 201911137338 A CN201911137338 A CN 201911137338A CN 110803890 A CN110803890 A CN 110803890A
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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
- 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 a high red mud content 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, coal series metakaolin, an alkali activator and water, wherein the total Si/Al atomic molar ratio in all raw materials is 1.2, the Na/Al atomic molar ratio is 0.8-1.3, 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 a water glass solution and sodium hydroxide; the compression strength of the red mud-coal series metakaolin geopolymer can reach more than 56MPa in 28 days, and the problem of decrease of the intensity of the geopolymer caused by increasing the mixing amount of the red mud in the production of the geopolymer is solved.
Description
Technical Field
The invention relates to the technical field of solid waste recycling and novel building material preparation, in particular to a high red mud content geopolymer and a preparation method thereof.
Background
Red mud is an insoluble solid residue produced after bauxite is melted with a caustic soda solution in the alumina production process. About 1-1.5 tons of red mud are produced per 1 ton of alumina produced, and even 2.5 tons of red mud are produced for low-grade bauxite. Currently, 90% of the world's alumina is produced by the bayer process. A large amount of red mud cannot be fully and effectively utilized, and can only be stacked by a large-area yard, thereby occupying a large amount of land and causing serious pollution to the environment. At present, the main treatment mode of red mud in China is damming and stockpiling, which not only wastes a large amount of land resources, but also causes serious pollution to the surrounding environment. With the annual increase of the output of the red mud, the improvement of the comprehensive utilization of the red mud is imminent.
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. Coal-based metakaolin is an amorphous material formed by calcining coal-based kaolin at a suitable temperature. Coal-series kaolin is a unique kaolin resource in China. The coal-series kaolin is effectively utilized, so that the environmental pollution caused by the storage of polluted coal gangue can be reduced, and the additional value in some fields can be increased.
The most predominant of the building materials produced from red mud are geopolymer materials. The geopolymer is an alkali-activated cementing material, which takes a silicon-aluminum material as a main raw material and is prepared byThe base excites the potential activity of the raw materials to prepare the high-performance gel material. The geopolymerization technology is a promising innovative technology, and industrial solid wastes (red mud, kaolin, fly ash, steel slag and the like) containing the aluminosilicate composition can be treated by a proper process, and a new material with similar performance to ceramic is obtained through chemical reaction. The geological polymerization reaction comprises that under the condition of strong alkalinity, aluminosilicate compounds and the solution react to generate a precursor of geopolymer, and the precursor is condensed into monomers; the monomers are subjected to polycondensation reaction to polymerize amorphous to semi-crystalline aluminosilicate polymer, the obtained geopolymer is a member of inorganic polymer family, and compared with the common silicate gel material, the geopolymer has the advantages of good physical and mechanical properties, low hydration heat, small shrinkage and expansion rate, good impermeability and frost resistance, strong corrosion resistance, simple production process, low production energy consumption, almost no pollution and zero CO2And (5) discharging.
However, since the red mud has a large fluctuation in the components and performance, it has been found that increasing the proportion of red mud in the raw material is not sufficient in the synthesis of geopolymers, and therefore, it is generally mixed with more reactive aluminosilicate materials, mainly fly ash, metakaolin, silica fume, slag, etc., so that the amount of red mud added is reduced, and it is difficult to utilize red mud on a large scale by a route for producing 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 raw material formula for preparing red mud-coal series metakaolin geopolymer and a preparation method thereof, utilizes Bayer process red mud to the maximum extent on the premise of ensuring the compressive strength of the geopolymer, and solves the problems of low red mud mixing amount and insufficient red mud utilization in the production of the geopolymer.
In order to achieve the above object, the present invention is achieved by the following technical solutions.
A polymer with high red mud content comprises the following raw materials in parts by weight: 70-80 parts of Bayer process red mud, 30-20 parts of coal-series metakaolin, 65-78 parts of an alkali activator and 8-10 parts of water, wherein the total Si/Al atomic molar ratio in all raw materials is 1.2, the Na/Al atomic molar ratio is 0.8-1.3, the mass ratio of water to solid is 0.5, 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 is 62 parts, and the weight part of the sodium hydroxide is 3-16 parts.
Preferably, the atomic molar ratio of Si/Al in the raw material is 1.2 and the atomic molar ratio of Na/Al is 1.0.
A preparation method of a polymer with high red mud content specifically comprises the following steps:
a) raw material treatment: air-drying and crushing Bayer process red mud, sieving the crushed Bayer process red mud to prepare red mud powder, drying the red mud powder, and uniformly mixing the treated Bayer process red mud and coal-series metakaolin according to parts by mass to obtain a raw material mixture.
b) Sample preparation: weighing the corresponding raw material mixture according to the parts by weight, adding the raw material mixture 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 the 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 a standard curing box for curing, wherein the temperature is 18-22 ℃, the humidity is 100%, and the geopolymer is obtained.
As shown in fig. 1, the main minerals in the red mud raw material include cancrinite ore, garcinia stone, hematite, calcite, gibbsite and the like, and the XRD spectrum shows that the red mud raw material has sharp peaks and no obvious hump, 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 coal-series metakaolin is a diffusion peak in X-ray diffraction peaks, has a remarkable wide hump between 18 and 32 degrees (2 theta) and has a plurality of small peaks, and shows that the coal-series metakaolin basically comprises amorphous SiO2Mainly amorphous substances.
The XRD pattern of the red mud-coal series metakaolin 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 earth crust. 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 study, it is found that the generated zeolite mineral has a direct relationship with the silica-alumina ratio in the raw material, and the form of silica-alumina ratio combination is related with the sufficiency of reaction, and for the polymer produced by using the red mud and coal-series metakaolin as the raw materials, the Si/Al atomic molar ratio and the Na/Al atomic molar ratio have great influence on the generation amount and stability of the zeolite mineral, in FIG. 1, the Si/Al atomic molar ratio is 1.2, the diffraction peak is increased and then decreased along with the increase of Na/Al, and the diffraction peak of Na/Al is maximum, thus indirectly proving that the red mud-series metakaolin polymer has the best compressive strength.
Compared with the prior art, the invention has the beneficial effects that.
(1) The red mud and the coal-series metakaolin are used as raw materials of the geopolymer, the raw materials are wide in source, the preparation process is simple, industrial production can be realized, and the method has good economic value.
(2) According to the invention, the Bayer process red mud is fully utilized, the content of the Bayer process red mud is up to 70%, the coal-series metakaolin which is a secondary processing product of coal gangue is indirectly utilized, the compressive strength of the produced geopolymer is 28 days and can reach more than 56MPa, the requirement of building materials is met, and a new way for resource utilization of the red mud is developed.
(3) The red mud-coal series metakaolin geopolymer phase ratio developed by the inventionThe traditional cementing material has excellent mechanical property, high early strength and no CO in the production process2The emission is small, the environmental pollution is small, and the method has certain environmental value.
Drawings
FIG. 1 is an XRD spectrum of a red mud-coal-based metakaolin polymer sample when coal-based metakaolin, red mud, Si/Al atomic molar ratio are 1.2, and Na/Al is 0.8, 1.0, and 1.3, 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 materials used include red mud from Bayer process of Shanxi Hejin aluminum plant and coal-series metakaolin from HP-90B (average particle size of 1.34 μm and specific surface area of 4480 m) from Shanxi Xinjiang Kaolin calcining Kaolin plant2/kg) is formed by roasting coal-series kaolin at 800 ℃ for 40min, belongs to hard metakaolin, and the chemical components of the coal-series kaolin and the hard metakaolin are respectively shown in tables 1 and 2.
Table 1 chemical composition of bayer process red mud.
Table 2 chemical composition of coal-based metakaolin.
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, and the purity is more than 99 percentThe 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 Bayer process red mud and coal series metakaolin according to the mass, wherein 700g of Bayer process red mud and 300g of coal series metakaolin are used for standby.
The waterglass solution, sodium hydroxide analytically pure and distilled water were calculated and named according to the set Si/Al (atomic molar ratio of Si/Al in the raw material is 1.2), Na/Al (atomic molar ratio of Na/Al in the raw material is 0.8, 0.9, 1.0, 1.1, 1.2, 1.3 respectively) and water-solid mass ratio (mass ratio of water to solid is 0.5, mass of water includes the sum of mass of water added to the waterglass solution and mass of distilled water added, mass of solid includes the sum of mass of Bayer process red mud and coal-based metakaolin), wherein the waterglass solution is 620g, the distilled water is 90g, and sodium hydroxide analytically pure is 30g, 60g, 80g, 110g, 130g respectively.
30g, 60g, 80g, 110g and 130g of sodium hydroxide analytical reagent are respectively added into 6 620g of water glass solutions, 90g of distilled water is respectively added into the 6 620g of water glass solutions to obtain alkali-activated solutions under different Na/Al conditions, after the alkali-activated solutions are cooled to room temperature, water lost due to heat release is added, and the mass ratio of water to solid is controlled to be 0.5 for later use.
(3) Sample preparation and maintenance:
adding Bayer process red mud and coal series metakaolin into a stirrer for stirring at the rotation speed of 150r/min for 2min, adding the alkali-activated solution into the stirrer after solid materials are uniformly stirred, and continuously stirring for 3min at the 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 a standard curing box for curing, wherein the temperature is 20 +/-2 ℃, and the humidity is 100%.
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 red mud-coal-based metakaolin geopolymer at 4 ages for 6 formulations is shown in table 3.
Table 3 Polymer compressive strengths of the red mud of each age, coal series metakaolin.
As can be seen from Table 3, under the precondition that the Bayer process red mud content is 70 parts and the coal-based metakaolin content is 30 parts, the Si/Al atomic molar ratio is controlled to be 1.2, and the intensity of geopolymers generated by different Na/Al atomic molar ratios is different. When the atomic mole of Na/Al is 1.0, namely the analytic pure mixing amount of sodium hydroxide is 8 parts, the polymer strength of the red mud-coal series metakaolin reaches the best at each age, the 7d compressive strength can reach 45.05MPa, and the 28d compressive strength can reach 56.20 MPa.
FIG. 1 is an XRD spectrum of a red mud-coal-based metakaolin polymer sample when coal-based metakaolin, red mud, Si/Al atomic molar ratio are 1.2, and Na/Al is 0.8, 1.0, and 1.3, respectively.
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 coal-series metakaolin is a diffusion peak in X-ray diffraction peaks, has a remarkable wide hump between 18 and 32 degrees (2 theta) and has a plurality of small peaks, and shows that the coal-series metakaolin basically comprises amorphous SiO2Mainly amorphous substances.
The red mud-coal metakaolin formed by the method of the inventionThe XRD pattern of the geopolymer generates zeolite minerals relative to the red mud, and the zeolite minerals have the characteristic of high strength similar to rocks in the earth crust. 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 silica-alumina ratio in the raw material, the combination form of the silica-alumina ratio is related with the sufficiency of the reaction, and for single red mud, the Si/Al atomic molar ratio and the Na/Al atomic molar ratio have great influence on the generation amount and the stability of the zeolite mineral, in the figure 1, the Si/Al atomic molar ratio is 1.2, the diffraction peak is increased and then decreased along with the increase of Na/Al, the diffraction peak of the Na/Al is maximum at 1.0, and the compressive strength of the polymer of the coal-series metakaolin is indirectly proved to be optimal at the moment.
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 polymer with high red mud content is characterized by comprising the following raw materials in parts by weight: 70-80 parts of Bayer process red mud, 30-20 parts of coal-series metakaolin, 65-78 parts of an alkali activator and 8-10 parts of water, wherein the total Si/Al atomic molar ratio in all raw materials is 1.2, the Na/Al atomic molar ratio is 0.8-1.3, the mass ratio of water to solid is 0.5, and the alkali activator is a mixed solution prepared by analyzing and purifying water glass solution and sodium hydroxide.
2. The polymer with high red mud content according to claim 1, wherein the weight part of the water glass is 62 parts, and the weight part of the sodium hydroxide is 3-16 parts.
3. The high red mud content polymer according to claim 1, wherein the raw material has an atomic mole ratio of Si/Al of 1.2 and an atomic mole ratio of Na/Al of 1.0.
4. The method for preparing the polymer with high red mud content according to claim 1, which is characterized by comprising the following steps:
a) raw material treatment: air-drying and crushing Bayer process red mud, sieving the crushed Bayer process red mud to prepare red mud powder, drying the red mud powder, and uniformly mixing the treated Bayer process red mud and coal-series metakaolin according to parts by mass to obtain a raw material mixture;
b) sample preparation: weighing corresponding raw material mixtures according to the parts by mass, adding the raw material mixtures 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 into a standard curing box for curing, wherein the temperature is 18-22 ℃, the humidity is 100%, and the geopolymer is obtained.
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| CN112979230A (en) * | 2021-05-08 | 2021-06-18 | 太原理工大学 | Polypropylene fiber reinforced red mud-based polymer material and preparation method thereof |
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