CN110862243B - Low-cost high-strength red mud-coal series metakaolin geopolymer - Google Patents

Low-cost high-strength red mud-coal series metakaolin geopolymer Download PDF

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CN110862243B
CN110862243B CN201911136174.XA CN201911136174A CN110862243B CN 110862243 B CN110862243 B CN 110862243B CN 201911136174 A CN201911136174 A CN 201911136174A CN 110862243 B CN110862243 B CN 110862243B
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CN110862243A (en
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刘剑平
白晓红
付鹏臣
袁超
武涛
卢仪思
马富丽
何斌
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Taiyuan University of Technology
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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
    • 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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    • Y02P40/10—Production of cement, e.g. improving or optimising the production methods; Cement grinding
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    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
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Abstract

The invention discloses a red mud-coal series metakaolin geopolymer with low cost and high strength, relating to the technical field of solid waste recycling and novel building material preparation; comprises the following raw materials: 50-85 parts of Bayer process red mud, 15-50 parts of coal series metakaolin, 51-62 parts of alkali activator consisting of water glass and sodium hydroxide, 4-12 parts of water, and 100 parts of Bayer process red mud and coal series metakaolin, wherein the total Si/Al atomic molar ratio in all raw materials is 1.1, and the mass ratio of water to solid is 0.4; the compression strength of the red mud-coal series metakaolin geopolymer can reach more than 40MPa in 28 days, the problem that the cost of the metakaolin is high, and the intensity of the geopolymer is reduced by simply increasing the doping amount of the red mud is solved.

Description

Low-cost high-strength red mud-coal series metakaolin geopolymer
Technical Field
The invention relates to the technical field of solid waste recycling and novel building material preparation, in particular to a red mud-coal series metakaolin geopolymer with low cost and high strength.
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-based kaolin, also known as coal gangue, is an associated mineral of coal. If the coal-series kaolin is not accumulated in a large amount, the coal-series kaolin not only occupies the land area, but also pollutes the atmosphere, soil and water. In addition, spontaneous combustion of coal-series kaolin can also cause fire disasters, even landslides and other geological disasters. 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 coal-series metakaolin is an amorphous aluminosilicate substance formed by calcining coal-series metakaolin at the temperature of 600-900 ℃, and the coal-series metakaolin prepared by adopting the coal-series metakaolin has high cost due to the high-temperature calcination, so that the market price is high, and how to economically utilize the coal-series metakaolin becomes a hotspot problem.
The most predominant of the building materials produced from red mud are geopolymer materials. The geopolymer is an alkali-activated cementing material and mainly adopts a silicon-aluminum materialThe raw material is excited by the potential activity of alkali on the raw material 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, materials such as metakaolin and the like are high in price, so that the production cost of the geopolymer is obviously increased, a negative effect is brought by simply increasing the mixing amount of the red mud, and the compressive strength of the whole geopolymer is reduced.
Disclosure of Invention
The invention overcomes the defects of the prior art, provides a raw material formula for preparing the red mud-coal series metakaolin geopolymer, utilizes Bayer process red mud to the maximum extent and reduces the use of coal series metakaolin on the premise of ensuring the compressive strength of the geopolymer, and solves the problems of low red mud mixing amount, insufficient red mud utilization and high production cost in the production of the geopolymer.
In order to achieve the above object, the present invention is achieved by the following technical solutions.
A low-cost high-strength red mud-coal series metakaolin geopolymer comprises the following raw materials in parts by weight: 50-85 parts of Bayer process red mud, 15-50 parts of coal-series metakaolin, 51-62 parts of an alkali activator, 4-12 parts of water, and 100 parts of Bayer process red mud and coal-series metakaolin, wherein the total Si/Al atomic molar ratio in all raw materials is 1.1, the mass ratio of water to solid is 0.4, and the alkali activator is a mixed solution prepared from water glass and sodium hydroxide.
Preferably, the weight parts of the water glass are 42-53 parts, and the weight parts of the sodium hydroxide are 9 parts.
Preferably, the bayer process red mud is 70 parts by weight, and the coal-series metakaolin is 30 parts by weight.
A preparation method of a low-cost high-strength red mud-coal series metakaolin geopolymer 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 is a kind of feldspar-like mineral, and is alkali-containing aluminosilicate ore, wherein red mud is composed of many kinds of red mudA cancrinite mineral is mixed. 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 research, the generated zeolite minerals have a direct relation with the silica-alumina ratio in the raw materials, the combination form of the silica-alumina ratio is related with the sufficiency of the reaction, and for the red mud-coal series metakaolin, the diffraction peak is the largest when the coal series metakaolin mixing amount is 30 parts, the red mud mixing amount is 70 parts and the Si/Al atomic molar ratio is 1.1, which indirectly proves that the compressive strength of the red mud-coal series metakaolin polymer is the best.
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, the industrial production can be realized, and in addition, geopolymer products with different strength grades are obtained by changing the mixing amount of the coal-series metakaolin and are selected by actual engineering personnel, so that the geopolymer 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 40MPa, the requirement of building materials is met, and a new way for resource utilization of the red mud is developed.
(3) Compared with the traditional cementing material, the red mud-coal series metakaolin geopolymer developed by the invention 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-series metakaolin geopolymer sample when coal-series metakaolin, the molar ratio of red mud to Si/Al atoms is 1.1, and the mixing amount of coal-series metakaolin is 15, 30 and 50 parts by mass 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.
Example 1
(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.
Figure DEST_PATH_IMAGE001
Table 2 chemical composition of coal-based metakaolin.
Figure DEST_PATH_IMAGE002
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）。
And weighing Bayer process red mud, coal series metakaolin and sodium hydroxide according to the mass for analytical purification, wherein 850g of Bayer process red mud, 150g of coal series metakaolin and 90g of sodium hydroxide are analyzed and purified for later use.
The sodium silicate solution and the sodium hydroxide analytically pure distilled water were calculated and named according to the set Si/Al (atomic molar ratio of Si/Al in the raw material is 1.1) and the mass ratio of water to solid (mass ratio of water to solid is 0.4, mass of water includes the sum of mass of water added to the sodium silicate solution and mass of distilled water added, mass of solid includes the sum of mass of Bayer process red mud and coal-series metakaolin), wherein the sodium silicate solution is 530g, and the distilled water is 40 g.
Adding 90g of sodium hydroxide analytically pure into 530g of water glass solution, adding 40g of distilled water to prepare alkali-activated solution, adding water lost due to heat release after the alkali-activated solution is cooled to room temperature, and controlling the mass ratio of water to solid to be 0.4 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 compressive strengths of the obtained geopolymer test pieces 7d, 14d, 21d and 28d were 7.26MPa, 9.17MPa, 11.37MPa and 12.39MPa, respectively.
Example 2
(1) Selecting and processing raw materials: the same procedure as in example 1 was repeated except for the fact that (1)
(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, coal series metakaolin and sodium hydroxide according to the mass for analytical purification, wherein 700g of Bayer process red mud, 300g of coal series metakaolin and 90g of sodium hydroxide are analyzed and purified for later use.
The sodium silicate solution and the sodium hydroxide analytically pure distilled water were calculated and named according to the set Si/Al (atomic molar ratio of Si/Al in the raw material is 1.1) and the mass ratio of water to solid (mass ratio of water to solid is 0.4, mass of water includes the sum of mass of water added to the sodium silicate solution and mass of distilled water added, mass of solid includes the sum of mass of Bayer process red mud and coal-series metakaolin), wherein the sodium silicate solution is 480g, and the distilled water is 70 g.
Adding 90g of sodium hydroxide analytical reagent into 480g of water glass solution, adding 70g of distilled water to prepare alkali-activated solution, cooling the alkali-activated solution to room temperature, adding water lost due to heat release, and controlling the mass ratio of water to solid to be 0.4 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 compressive strengths of the obtained geopolymer test pieces 7d, 14d, 21d and 28d were 37.81MPa, 38.74MPa, 39.52MPa and 40.13MPa, respectively.
Example 3
(1) Selecting and processing raw materials: the same procedure as in example 1 was repeated except for the fact that (1)
(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）。
And weighing Bayer process red mud, coal series metakaolin and sodium hydroxide according to the mass for analytical purification, wherein 500g of Bayer process red mud, 500g of coal series metakaolin and 90g of sodium hydroxide are analyzed and purified for later use.
The sodium silicate solution and the sodium hydroxide analytically pure distilled water were calculated and called according to the set Si/Al (atomic molar ratio of Si/Al in the raw material is 1.1) and the mass ratio of water to solid (mass ratio of water to solid is 0.4, mass of water includes the sum of mass of water added to the sodium silicate solution and mass of distilled water added, mass of solid includes the sum of mass of Bayer process red mud and coal-series metakaolin), wherein the sodium silicate solution is 420g, and the distilled water is 120 g.
Adding 90g of sodium hydroxide analytically pure into 420g of water glass solution, adding 120g of distilled water to prepare alkali-activated solution, adding water lost due to heat release after the alkali-activated solution is cooled to room temperature, and controlling the mass ratio of water to solid to be 0.4 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 compressive strengths of the obtained geopolymer test pieces 7d, 14d, 21d and 28d were 11.64MPa, 16.83MPa, 18.39MPa and 20.95MPa, respectively.
FIG. 1 is an XRD spectrum of a red mud-coal-series metakaolin geopolymer sample when coal-series metakaolin, the molar ratio of red mud to Si/Al atoms is 1.1, and the mixing amount of coal-series metakaolin is 15, 30 and 50 parts by mass 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 XRD pattern of the red mud-coal series metakaolin geopolymer formed by the method of the invention generates zeolite minerals relative to the red mud, and the zeolite mineralsThe object has high strength similar to the rock in the 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 minerals have a direct relation with the silica-alumina ratio in the raw materials, the combination form of the silica-alumina ratio is related with the sufficiency of the reaction, and for the red mud-coal series metakaolin, the diffraction peak is the largest when the coal series metakaolin mixing amount is 30 parts, the red mud mixing amount is 70 parts and the Si/Al atomic molar ratio is 1.1, which indirectly proves that the compressive strength of the red mud-coal series metakaolin polymer is 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 (2)

1. The low-cost high-strength red mud-coal series metakaolin geopolymer is characterized by comprising the following raw materials in parts by weight: 70 parts of Bayer process red mud, 30 parts of coal-series metakaolin, 51-62 parts of an alkali activator, 100 parts of Bayer process red mud and coal-series metakaolin, wherein the total Si/Al atomic molar ratio in all raw materials is 1.1, the mass ratio of water to solid is 0.4, the alkali activator is a mixed solution prepared from water glass and sodium hydroxide, and the Bayer process red mud comprises the following chemical components in percentage by mass: SiO 22：21.05%，Al2O3：27.38%，Fe2O3：6.42%，TiO2：4.04%，CaO：14.91%，MgO： 0.53%，K2O：0.77%，Na2O：11.86%，SO2：0.36%，CO2: 3.90%, LOI: 8.78 percent; the coal series metakaolin comprises the following chemical components in percentage by mass: SiO 22：52.62%，Al2O3：45.42%，Fe2O3：0.45%，TiO2：0.85%，CaO：0.17%，MgO：0.11%，K2O：0.13%，Na2O：0.25%。
2. The low-cost high-strength red mud-coal-series metakaolin geopolymer as claimed in claim 1, wherein the weight parts of the water glass are 42-53 parts, and the weight parts of the sodium hydroxide are 9 parts.
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