CN110550932A - method for hydrothermal preparation of high-strength building material from siliceous tailings by steam - Google Patents
method for hydrothermal preparation of high-strength building material from siliceous tailings by steam Download PDFInfo
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- CN110550932A CN110550932A CN201910856954.5A CN201910856954A CN110550932A CN 110550932 A CN110550932 A CN 110550932A CN 201910856954 A CN201910856954 A CN 201910856954A CN 110550932 A CN110550932 A CN 110550932A
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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
- C04B30/00—Compositions for artificial stone, not containing binders
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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
- 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
- C04B40/024—Steam hardening, e.g. in an autoclave
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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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention relates to a method for hydrothermal preparation of a siliceous tailings into a high-strength building material, which comprises the following steps of: calcium additive: an activity activator: 50-80% of water: 10% -30%: 0.5% -5%: 5-15%, uniformly mixing, and pressing and forming to obtain the building material profile green body. Demoulding the green body, carrying out hot pressing treatment for 8-24 h at 110-170 ℃, and then curing for 6-12 h in a normal-temperature high-humidity environment to obtain a building material product; through detection, the compressive strength of the material can reach 25-50 MPa. The invention realizes the high-efficiency reutilization of siliceous tailings represented by tailing, waste ceramic and sand washing bottom mud generated in the production process of glass, ceramics and machine-made sand, realizes the resource utilization of solid wastes, and the synthesized solidified material has higher strength and can be used as wall bricks, floor tiles, square bricks, pavement bricks, permeable bricks, artificial fish reefs, ocean river bank protection materials, retaining wall materials and the like.
Description
Technical Field
The invention relates to a method for hydrothermal preparation of a high-strength building material from siliceous tailings, belonging to the technical field of resource recycling of solid wastes.
Background
The siliceous tailings are defined as industrial tailings with silicon dioxide content of more than 50%, and are general solid wastes generated in the industrial production process, specifically include tailings generated in the glass production process, ceramic wastes generated in the ceramic production process, sand washing bottom mud generated in the machine-made sand production process, and the like. With the rapid development of economic and industrial production in China, the quantity of siliceous tailings is increased explosively. However, the wastes with huge amount, various kinds and complex components are only treated in a rough yard or simple landfill mode, which causes great harm to the production and life of people, but the research on the reutilization of the siliceous tailings in the domestic and foreign documents is less, and the treatment mode in the actual industry is mainly landfill or stacking. How to continuously promote the resource utilization of the siliceous tailings, reduce the landfill capacity to the maximum extent, change the siliceous tailings into a utilizable 'urban mineral product', and become the focus of attention in the field.
Disclosure of Invention
The invention aims to provide a method for hydrothermal preparation of siliceous tailings into a high-strength building material, which fills the domestic blank of research on utilization of the wastes. The novel building material prepared by the invention has the strength far higher than that of common cement concrete building materials, has better durability, and can be widely applied to the aspects of road pavement, building materials, river bank protection retaining walls and the like.
in order to achieve the purpose, the method adopted by the invention is steam hydrothermal, which is a method for rapidly reproducing the long-growing rock-forming process of the natural rock pile in a laboratory, namely, the raw material is placed in a water vapor environment with certain temperature and pressure, and the water in the steam environment is in a supercritical state, so that the dissolving capacity and the reaction activity are greatly enhanced. By the method, siliceous tailings which are difficult to react under the conditions of normal temperature and normal pressure participate in a reaction system, and react with a calcareous additive under the action of an active excitant to generate new crystals so as to improve the strength. The new crystals are in fiber or sheet shape, are interwoven with each other and are filled in the gaps of the raw materials, and play a crucial role in the final improvement of the strength.
The method comprises the following specific steps:
Weighing silicon tailings according to mass percent: calcium additive: an activity activator: water (50-80%): (10-30%): (0.5-5%): (5-15%), uniformly mixing, and pressing and forming to obtain a building material profile green body; after demolding, carrying out hot pressing treatment for 8-24 h at 110-170 ℃, and then curing for 6-12 h in a normal-temperature high-humidity environment to obtain a building material product; through detection, the compressive strength of the material can reach 25-50 MPa.
The siliceous tailings are tailings and tailings generated in the glass production process; ceramic defective products, waste ceramic powder and ceramic polished tile waste materials generated in the ceramic production process; one kind of sand washing bottom mud or a plurality of kinds of silicon tailings mixed according to any proportion in the production process of machine-made sand.
The calcareous additive is one or more of slaked lime, limestone, quicklime and dolomite which are mixed according to any proportion and are sold in commercial industrial grade products.
The activity excitant is a self-made product and is prepared by weighing 15-25 parts of sodium silicate according to parts by weight; 5-30 parts of sodium hydroxide; 5-35 parts of soda ash; 10-30 parts of desulfurized gypsum and 10-55 parts of C-S-H seed crystal are uniformly mixed to obtain a powdery medicament with the particle size of 100 meshes.
The C-S-H seed crystal in the activity excitant is prepared according to the following method: weighing amorphous silica/quicklime 1.5-1.7 in mass ratio, uniformly mixing, then putting into a mechanical stirring reaction kettle, adding water which is 9-12 times of the total mass of the mixture into the reaction kettle, reacting for 4-10 hours at the temperature of 120-160 ℃, and then filtering, vacuum drying, grinding and sieving with a 100-mesh sieve to obtain the C-S-H crystal seed.
The invention has the advantages and effects that:
1. The doping amount of the siliceous tailings reaches 50-80%, the siliceous tailings which are difficult to treat are used as main reaction raw materials for treatment, and compared with the addition amount of less than 30% of siliceous tailings used as fillers in the traditional technology, the method is an efficient method for recycling solid wastes.
2. the invention adopts a steam hydrothermal treatment mode, the reaction temperature is not more than 170 ℃, and compared with the traditional sintering mode, the energy consumption is lower, the energy is saved, the environment is protected, and no secondary pollution is generated.
3. The waste siliceous tailings can be prepared into high-strength building materials by utilizing the method, can be widely used as wall bricks, floor tiles, square bricks, pavement bricks, embankment protection materials, retaining wall materials and the like, and really realizes the high value-added utilization of the siliceous tailings. Meanwhile, the silicon raw material has high mixing amount and low energy consumption at reaction temperature, so that the product has low production cost and strong market competitiveness.
Drawings
FIG. 1 is a schematic process flow diagram of the present invention.
FIG. 2 is a graph showing the effect of calcareous additive content of the present invention on the flexural strength of a siliceous tailings steam hydrothermal building material product.
FIG. 3 is a graph of the infrared profile of a building material product at various calcareous additive levels according to the present invention.
Detailed Description
The invention is further illustrated by the following examples.
Firstly, preparing an activity excitant: 20 parts of sodium silicate measured according to the weight ratio; 10 parts of sodium hydroxide; 15 parts of soda ash; 15 parts of desulfurized gypsum and 40 parts of C-S-H seed crystal are uniformly mixed to obtain a powdery medicament with the particle size of 100 meshes. The sodium silicate, the sodium hydroxide, the soda ash and the desulfurized gypsum are all commercial products.
The C-S-H crystal seed in the active excitant is prepared by taking amorphous silica and quicklime as raw materials, weighing the amorphous silica/quicklime to be 1.5 according to the mass ratio, uniformly mixing, then putting into a mechanical stirring reaction kettle, adding water which is 10 times of the total weight of the raw materials into the reaction kettle, stirring and reacting for 5 hours at the temperature of 140 ℃, and then filtering, vacuum drying, grinding and sieving with a 100-mesh sieve to obtain the C-S-H crystal seed.
Example 1:
Taking a ceramic tailing generated by a certain ceramic enterprise in Zhaoqing, Guangdong province as a siliceous tailing, according to a picture 1, respectively grinding the ceramic tailing and commercial industrial-grade quick lime to 100 meshes, sieving, taking the ground ceramic tailing, the quick lime, an active activator and water as raw materials, weighing 80% of the ceramic tailing, 10% of the quick lime, 3% of the active activator and 7% of the water according to mass percent, fully grinding, stirring and mixing, pressing and molding in an YP1300 static pressure machine to obtain a green body sample, wherein the sample is a cuboid standard brick with the length of about 240mm, the width of about 115mm and the thickness of about 53mm, and the molding pressure is 20 MPa; transferring the molded green body sample to a steam-hydrothermal autoclave, adding a certain volume of water into the autoclave, wherein the specific addition amount is less than 10% of the volume of the autoclave, and then heating at 170 ℃ for 8 h; and taking out the treated sample, and then placing the sample in a high-humidity environment at 25 ℃ for curing for 10 hours to obtain a cured body product. The compressive strength test is carried out according to GB/T2542-2012 'method for testing wall bricks', and the result shows that the compressive strength of the cured product can reach 38MPa, so that the requirement on the strength of the wall brick product is met.
Example 2:
Taking glass tailings generated by a certain glass enterprise in Jiaxing city, Zhejiang province as siliceous tailings, grinding the glass tailings and commercial industrial-grade slaked lime respectively to 100 meshes and sieving according to a diagram shown in a figure 1, taking the ground glass tailings, slaked lime, an active excitant and water as raw materials, weighing 50% of siliceous tailings, 30% of slaked lime, 5% of active excitant and 15% of water according to mass percent, fully grinding, stirring and mixing the raw materials, pressing and molding in an YP1300 static pressure machine to obtain a green body sample, wherein the sample is a cuboid pavement brick sample with the shape of about 200mm long, about 100mm wide and about 60mm thick, and the molding pressure is 15 MPa; transferring the formed green body into a closed steam hydrothermal autoclave, adding a certain volume of water into the autoclave, wherein the specific addition amount is 10% of the volume of the autoclave, and then carrying out heating treatment at 160 ℃ for 16 h; and taking out the treated sample, and then placing the sample in a high-humidity environment at 25 ℃ for curing for 6 hours to obtain a product cured body. The compressive strength test is carried out according to GB/T32987-2016 concrete pavement brick performance test method, and the result shows that the flexural strength of the sample can reach 44MPa, so that the strength requirement of a pavement brick product is met.
Example 3:
Taking sand washing bottom mud generated by a certain mechanism sand production enterprise in Nibo of Zhejiang province as siliceous tailings, firstly respectively grinding and crushing the sand washing bottom mud and commercial industrial-grade slaked lime to 100 meshes and sieving according to a diagram shown in figure 1, taking the ground sand washing bottom mud, slaked lime, an active activator and water as raw materials, weighing 70% of the sand washing bottom mud, 20% of the slaked lime, 2% of the active activator and 8% of the water according to mass percent, fully grinding, stirring and mixing the raw materials, pressing and molding the raw materials in an YP1300 static pressure machine to obtain a green body sample, wherein the sample is a cube slope protection building block with the shape of about 300mm in length, about 300mm in width and about 10mm in thickness, and the molding pressure is 10 MPa; transferring the formed green body into a closed autoclave, adding a certain volume of water into the autoclave, wherein the specific addition amount is 10% of the volume of the autoclave, and then heating at 110 ℃ for 24 hours; and taking out the treated sample, and then placing the sample in a high-humidity environment at 25 ℃ for curing for 12 hours to obtain a cured body product. The compressive strength test is carried out according to a related method in TZZB 0775-2018 concrete ecological block for retaining wall and slope protection, and the result shows that the compressive strength of the cured product can reach 32MPa, so that the strength requirement of the slope protection block is met.
example 4:
The influence of the content of the calcareous additive on the compressive strength of the product is illustrated by treating the glass tailings generated by a certain glass enterprise in Jiaxing city, Zhejiang province as siliceous tailings, and in example 4, the process for preparing the pavement brick product is the same as in example 2 except that the formula for preparing the brick from the glass tailings is prepared according to the formula shown in Table 1.
Table 1 glass tailings brick making formula table
Fig. 2 shows the influence of the content of the calcareous additive on the compressive strength of a construction material sample pavement brick product made of glass tailings, and it can be seen from fig. 2 that the strength of the pavement brick product is continuously increased with the continuous increase of the content of slaked lime, and when the content of the slaked lime is 25%, the flexural strength of the sample is the highest and reaches 47MPa, and the strength is continuously increased and starts to be reduced on the contrary. An optimum slaked lime content of 25% is thus obtained.
FIG. 3 shows the Fourier infrared (FT-IR) curve change of samples with different contents of calcareous additives, the peaks (778cm -1 and 461cm -1) related to quartz in the product of the solidified body are obviously weakened, and the quartz participates in the reaction, researches indicate that the infrared absorption peak related to C-S-H (or tobermorite) appears near 970cm -1, and the peak in the range of 1200-900cm -1 in the spectrum is obviously shifted to 970cm -1 along with the addition of the calcareous additives, which proves that the C-S-H (or tobermorite) is generated along with the reaction, and the intensity change trend of FIG. 2 is also matched, while excessive calcareous additives are easy to form films on the surfaces of raw material particles, so that the hydration reaction of the products is prevented, and the intensity of the samples is reduced.
Claims (2)
1. a method for hydrothermal preparation of high-strength building material from siliceous tailings is characterized by comprising the following steps: firstly, weighing silicon tailings according to mass percentage: calcium additive: an activity activator: 50-80% of water: 10% -30%: 0.5% -5%: 5-15%, uniformly mixing, and pressing and forming to obtain a building material profile green body; after demolding, carrying out hot pressing treatment for 8-24 h at 110-170 ℃, and then curing for 6-12 h in a normal-temperature high-humidity environment to obtain a building material product; through detection, the compressive strength of the material can reach 25-50 MPa;
The siliceous tailings are tailings and tailings generated in the glass production process; ceramic defective products, waste ceramic powder and ceramic polished tile waste materials generated in the ceramic production process; one or more siliceous tailings formed by mixing sand washing bottom mud in any proportion in the production process of machine-made sand;
The calcareous additive is a commercial industrial grade commodity which is prepared by mixing one or more of slaked lime, limestone, quicklime, dolomite and calcium-containing inorganic waste according to any proportion;
The active excitant is a self-made product and is prepared by weighing 15-25 parts of sodium silicate according to the weight ratio; 5-30 parts of sodium hydroxide; 5-35 parts of soda ash; 10-30 parts of desulfurized gypsum and 10-55 parts of C-S-H seed crystal are uniformly mixed to obtain a powdery medicament with the particle size of 100 meshes;
The C-S-H seed crystal in the activity excitant is prepared according to the following method: weighing amorphous silica/quicklime 1.5-1.7 in mass ratio, uniformly mixing, then putting into a mechanical stirring reaction kettle, adding water which is 9-12 times of the total mass of the mixture into the reaction kettle, reacting for 4-10 hours at the temperature of 120-160 ℃, and then filtering, vacuum drying, grinding and sieving with a 100-mesh sieve to obtain the C-S-H crystal seed.
2. The method of claim 1 for steam hydrothermal conversion of siliceous tailings into high strength building materials, comprising: the high-strength building material is a building material profile product for wall bricks, floor tiles, square bricks, pavement bricks, permeable bricks, artificial fish reefs, ocean river bank protection materials and retaining wall materials.
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Cited By (3)
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CN112876148A (en) * | 2021-02-08 | 2021-06-01 | 大连理工大学 | Red mud/yellow river sediment artificial fish reef and preparation method thereof |
CN115304339A (en) * | 2022-08-17 | 2022-11-08 | 鹤山市鸿盛石场有限公司 | Autoclaved aerated concrete based on granite sand washing tail mud and preparation method thereof |
CN117361915A (en) * | 2023-08-16 | 2024-01-09 | 浙江大学 | Method for preparing hydrothermal curing body based on relative content of active calcium and active silicon |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112876148A (en) * | 2021-02-08 | 2021-06-01 | 大连理工大学 | Red mud/yellow river sediment artificial fish reef and preparation method thereof |
CN115304339A (en) * | 2022-08-17 | 2022-11-08 | 鹤山市鸿盛石场有限公司 | Autoclaved aerated concrete based on granite sand washing tail mud and preparation method thereof |
CN117361915A (en) * | 2023-08-16 | 2024-01-09 | 浙江大学 | Method for preparing hydrothermal curing body based on relative content of active calcium and active silicon |
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