LU503728B1 - Preparation method for tungsten tailing-based geopolymer - Google Patents
Preparation method for tungsten tailing-based geopolymer Download PDFInfo
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- LU503728B1 LU503728B1 LU503728A LU503728A LU503728B1 LU 503728 B1 LU503728 B1 LU 503728B1 LU 503728 A LU503728 A LU 503728A LU 503728 A LU503728 A LU 503728A LU 503728 B1 LU503728 B1 LU 503728B1
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- tungsten
- geopolymer
- powder
- preparation
- na2co3
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- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 title claims abstract description 76
- 229910052721 tungsten Inorganic materials 0.000 title claims abstract description 76
- 239000010937 tungsten Substances 0.000 title claims abstract description 76
- 229920000876 geopolymer Polymers 0.000 title claims abstract description 67
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 72
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 36
- 235000017550 sodium carbonate Nutrition 0.000 claims abstract description 36
- 239000010881 fly ash Substances 0.000 claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000012423 maintenance Methods 0.000 claims abstract description 8
- 230000000694 effects Effects 0.000 claims abstract description 5
- 239000000843 powder Substances 0.000 claims description 62
- 239000002243 precursor Substances 0.000 claims description 20
- 239000000203 mixture Substances 0.000 claims description 17
- 239000002245 particle Substances 0.000 claims description 12
- 239000002002 slurry Substances 0.000 claims description 10
- 238000000227 grinding Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 4
- 239000002994 raw material Substances 0.000 abstract description 4
- 239000004566 building material Substances 0.000 abstract description 3
- 238000009825 accumulation Methods 0.000 description 6
- 238000012360 testing method Methods 0.000 description 5
- 239000012190 activator Substances 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 239000002985 plastic film Substances 0.000 description 4
- 229920006255 plastic film Polymers 0.000 description 4
- 239000003513 alkali Substances 0.000 description 3
- 239000012670 alkaline solution Substances 0.000 description 3
- 150000004645 aluminates Chemical class 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 229910000323 aluminium silicate Inorganic materials 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 235000010755 mineral Nutrition 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical class [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- CQBLUJRVOKGWCF-UHFFFAOYSA-N [O].[AlH3] Chemical compound [O].[AlH3] CQBLUJRVOKGWCF-UHFFFAOYSA-N 0.000 description 1
- OBNDGIHQAIXEAO-UHFFFAOYSA-N [O].[Si] Chemical compound [O].[Si] OBNDGIHQAIXEAO-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 229920000592 inorganic polymer Polymers 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- 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
- C04B7/00—Hydraulic cements
- C04B7/24—Cements from oil shales, residues or waste other than slag
- C04B7/243—Mixtures thereof with activators or composition-correcting additives, e.g. mixtures of fly ash and alkali activators
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B7/00—Hydraulic cements
- C04B7/36—Manufacture of hydraulic cements in general
- C04B7/43—Heat treatment, e.g. precalcining, burning, melting; Cooling
- C04B7/44—Burning; Melting
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- Chemical & Material Sciences (AREA)
- Ceramic Engineering (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Geology (AREA)
- Geochemistry & Mineralogy (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention relates to a preparation technology of building materials, in particular to a preparation method for tungsten tailing-based geopolymer. In the invention, geopolymer is prepared with tungsten tailings and fly ash as the main raw materials. Na2CO3, tungsten tailings and fly ash are respectively calcined and activated to generate calcined products with relatively high activity of Na 6.8 (Al6.3Si9.7O32) as the main phase. The two calcined products are ground and mixed evenly, and then directly mixed with water, and tungsten tailing-based geopolymer with high compressive strength is prepared through pressing and maintenance. After curing for 28 days, the minimum compressive strength of the geopolymer in the invention can reach 110 MPa. The geopolymer in the invention has high compressive strength, and the preparation process of the invention is safer, simpler, more convenient and more operable.
Description
DESCRIPTION 0503728
PREPARATION METHOD FOR TUNGSTEN TAILING-BASED GEOPOLYMER
The invention relates to a preparation technology of building materials, in particular to a preparation method for a tungsten tailing-based geopolymer.
Geopolymer is a kind of inorganic polymer structural cementing material formed by silicon- oxygen tetrahedron and aluminum-oxygen tetrahedron, which was first developed by French professor J-Davidovits in the late 1970s. Because of its three-dimensional network polymer structure, this kind of material has stable physical and chemical properties, high strength, high temperature resistance, acid and alkali corrosion resistance and other excellent properties, so geopolymer has great application potential as a building material.
Tungsten tailings are the main solid wastes produced in the mineral processing of tungsten ore.
Due to the low content of valuable metals in tungsten ore, the utilization rate of tungsten ore in the mineral processing 1s low, resulting in a large number of tungsten tailings. At present, the accumulation amount of tungsten tailings in China has reached more than 30 million tons. The accumulation of a large number of tungsten tailings not only occupies land, but also pollutes the environment, which has great security risks. At present, the utilization rate of tungsten tailings 1s only about 10%, which seriously restricts the sustainable development of mines. The main components of tungsten tailings are silicon and aluminum oxides, which meet the requirements of geopolymer preparation. Therefore, geopolymer preparation with tungsten tailings can turn waste into treasure, and at the same time, it can effectively solve the environmental pollution problem caused by long-term accumulation of tungsten tailings, which has great and far-reaching economic and social benefits.
At present, the preparation of geopolymer is mainly based on the interaction of solid silicon, aluminate materials and high concentration alkaline solution activator. The obvious disadvantages of this preparation method are that solid silicon and aluminate raw materials need to be prepared,
and high-concentration alkaline activator needs to be prepared, which adds to the complexity Sr 503728 the process. The strong alkaline solution used is difficult to handle and store because of its strong corrosiveness and viscosity, which poses a serious threat to the safety of operators and the environment. In addition, due to the use of high-concentration alkaline solution for excitation, geopolymers are prone to "saltpetering" phenomenon after long-term storage, which reduces the performance of geopolymer. At the same time, the compressive strength of geopolymer prepared is generally not high, which is less than 100 MP. These shortcomings make this method not suitable for cast-in-place and large-scale application, which limits its application potential in practical engineering.
Therefore, it is of positive practical and economic significance to develop a simple, safe and convenient process and prepare geopolymer with high compressive strength from tungsten tailings, which will solve the problems of accumulation and pollution of tungsten tailings and promote the large-scale popularization and application of geopolymers.
The purpose of the invention is to provide a preparation method for tungsten tailing-based geopolymer. Geopolymer is prepared with tungsten tailings and fly ash as the main raw materials.
The Na2CO3, tungsten tailings and fly ash are respectively calcined and activated to generate calcined products with relatively high activity of Na 6.8 (Al6.3S19.7032) as the main phase (in which Na6.8 (Al6.3 Si9.7 032) is dissolved in water to form simple silicate and aluminate). The two calcined products are ground and mixed evenly, and then directly mixed with water, and tungsten tailing-based geopolymer with high mechanical properties is prepared through sample preparation and maintenance to solve the problem of accumulation pollution of tungsten tailings.
The technical scheme of the invention is as follows:
A preparation method for tungsten tailing-based geopolymer comprises the steps: (1) First, grind tungsten tailing, fly ash and Na2CO3 into powders respectively, and then mix the tungsten tailings powder and fly ash powder with Na2CO3 powder and calcine them respectively to obtain two kinds of calcined products;
. . . . . . LU503728 (2) Grind the two calcined products obtained in step (1) into powders respectively, and then mix them evenly to form the geopolymer precursor; (3) Add water into the geopolymer precursor in step (2) to form slurry, stir for 5~30 min, inject into a mold, press under the pressure of 10~20 MPa for 10~30 s, demould, seal and maintain at the temperature of 900C for 15-24 h to obtain the tungsten tailing-based geopolymer;
After maintenance at room temperature for 28 d, the compressive strength of tungsten tailing- based geopolymer is above 110 MPa.
In the step (1), the mass ratio of tungsten tailings to fly ash is 10:4~10, and the mass ratios of tungsten tailings to Na2CO3 and fly ash to Na2CO3 are all 10:2-10.
In the step (1), the calcination temperature of tungsten tailings powder, fly ash powder and
Na2CO3 powder is 700~10000C , and the calcination time is 1~3 h.
In the step (1), the two kinds of calcined products are the calcined products with Na 6.8 (A16.3S19.7032) with good activity as the main phase.
In the step (1), the particle sizes of tungsten tailings powder, fly ash powder and Na2CO3 powder are all below 100 meshes.
In the step (2), the particle sizes of the two calcined products after grinding are both below 100 meshes.
In the step (3), the mass ratio of the geopolymer precursor to water is 10:2~5.
The invention has the beneficial effects that:
After maintenance at room temperature for 28 d, the compressive strength of tungsten tailing- based geopolymer is above 110 MPa, as shown in Table 1. In the invention, Na2CO3, tungsten tailings and fly ash are respectively calcined and activated, and a mixture of two calcined products with relatively good activity, namely Na 6.8 (A16.3519.7032), is used as a raw material, and water is directly added and stirred, and geopolymer is prepared through sample preparation and maintenance. After maintenance for 28 d, the minimum compressive strength of the geopolymer of the present invention can reach 110 MPa. See Table 1 for details. The compression resistance is
. . . . . 1, LU503728 excellent. And the invention provides strong technical support for realizing large-scale utilization of tungsten tailings and solving the problem of accumulation pollution of tungsten tailings.
In the invention, the dangerous process is removed. And in the traditional geopolymer preparation process, because the alkaline activator solution needs to be prepared on site, and the alkaline activator solution has strong corrosiveness, the preparation workers are easily corroded and burned by strong alkali. The invention eliminates this high-risk factor. In the invention, tungsten tailings and fly ash are calcined and activated by Na2CO3, and then mixed to obtain a geopolymer aluminosilicate precursor. After directly adding water to the aluminosilicate precursor, mixing and maintenance, the geopolymer with excellent compression resistance can be obtained. The problems that the operation is complicated, the concentrated alkali is not easy to configure on site and is difficult to popularize are solved.
The preparation process of the invention is safer, simpler, more convenient and more operable.
Embodiment 1
A preparation method for tungsten tailing-based geopolymer: (1) Tungsten tailings, fly ash and Na2CO3 were respectively ground and sieved by a 100-mesh sieve to obtain powder with a particle size of less than 100 meshes, 100 g of tungsten tailings powder and 40 g of Na2CO3 powder were taken and evenly mixed, and 100 g of fly ash powder and 40 g of Na2CO3 powder were evenly mixed; Then the mixture of tungsten tailings powder and Na2CO3 powder was calcined at 8000C for 1 h, and the mixture of fly ash powder and
Na2CO3 powder was calcined at 9000C for 1h for later use; (2) The two calcined products obtained in the step (1) were respectively put into a ball mill for grinding finer, screened by a 100-mesh sieve to obtain powder with a particle size of less than 100 meshes, and then uniformly mixed to form a geopolymer precursor; (3) Water was added into the geopolymer precursor in step (2), and the ratio of water to geopolymer precursor is 1:4. After stirring for 5 min, the mixture was fully mixed to form slurry; Then the slurry was poured into a mold, pressed at a pressure of 15 MPa for 15 s, then demoulded, sealéd” 503728 by a plastic film and maintained at 900C for 24 h to obtain the tungsten tailing-based geopolymer, and then cured at room temperature for 3 d, 7 d and 28 d, and then the compressive strength was tested. The test results are shown in Table 1.
Embodiment 2
A preparation method for tungsten tailing-based geopolymer: (1) Tungsten tailings, fly ash and Na2CO3 were respectively ground and sieved by a 100-mesh sieve to obtain powder with a particle size of less than 100 meshes, 100 g of tungsten tailings powder and 40 g of Na2CO3 powder were taken and evenly mixed, and 100 g of fly ash powder and 40 g of Na2CO3 powder were evenly mixed; Then the mixture of tungsten tailings powder and Na2CO3 powder was calcined at 9000C for 1 h, and the mixture of fly ash powder and
Na2CO3 powder was calcined at 10000C for 1h for later use; (2) The two calcined products obtained in the step (1) were respectively put into a ball mill for grinding finer, screened by a 100-mesh sieve to obtain powder with a particle size of less than 100 meshes, and then uniformly mixed to form a geopolymer precursor; (3) Water was added into the geopolymer precursor in step (2), and the ratio of water to geopolymer precursor is 1:4. After stirring for 5 min, the mixture was fully mixed to form slurry; Then the slurry was poured into a mold, pressed at a pressure of 15 MPa for 15 s, then demoulded, sealed by a plastic film and maintained at 900C for 24 h to obtain the tungsten tailing-based geopolymer, and then cured at room temperature for 3 d, 7 d and 28 d, and then the compressive strength was tested. The test results are shown in Table 1.
Embodiment 3
A preparation method for tungsten tailing-based geopolymer: (1) Tungsten tailings, fly ash and Na2CO3 were respectively ground and sieved by a 100-mesh sieve to obtain powder with a particle size of less than 100 meshes, 100 g of tungsten tailings powder and 30 g of Na2CO3 powder were taken and evenly mixed, and 100 g of fly ash powder and 50 g of Na2CO3 powder were evenly mixed; Then the mixture of tungsten tailings powder and Na2CO3 powder was calcined at 8000C for 1 h, and the mixture of fly ash powder and
Na2CO3 powder was calcined at 9000C for 1h for later use; (2) The two calcined products obtained” 503728 in the step (1) were respectively put into a ball mill for grinding finer, screened by a 100-mesh sieve to obtain powder with a particle size of less than 100 meshes, and then uniformly mixed to form a geopolymer precursor; (3) Water was added into the geopolymer precursor in step (2), and the ratio of water to geopolymer precursor is 1:4. After stirring for 5 min, the mixture was fully mixed to form slurry; Then the slurry was poured into a mold, pressed at a pressure of 15 MPa for 15 s, then demoulded, sealed by a plastic film and maintained at 900C for 24 h to obtain the tungsten tailing-based geopolymer, and then cured at room temperature for 3 d, 7 d and 28 d, and then the compressive strength was tested. The test results are shown in Table 1.
Embodiment 4
A preparation method for tungsten tailing-based geopolymer: (1) Tungsten tailings, fly ash and Na2CO3 were respectively ground and sieved by a 100-mesh sieve to obtain powder with a particle size of less than 100 meshes, 100 g of tungsten tailings powder and 30 g of Na2CO3 powder were taken and evenly mixed, and 80 g of fly ash powder and 40 g of Na2CO3 powder were evenly mixed; Then the mixture of tungsten tailings powder and Na2CO3 powder was calcined at 8000C for 1 h, and the mixture of fly ash powder and
Na2CO3 powder was calcined at 9000C for 1h for later use; (2) The two calcined products obtained in the step (1) were respectively put into a ball mill for grinding finer, screened by a 100-mesh sieve to obtain powder with a particle size of less than 100 meshes, and then uniformly mixed to form a geopolymer precursor; (3) Water was added into the geopolymer precursor in step (2), and the ratio of water to geopolymer precursor is 1:4. After stirring for 5 min, the mixture was fully mixed to form slurry; Then the slurry was poured into a mold, pressed at a pressure of 15 MPa for 15 s, then demoulded, sealed by a plastic film and maintained at 900C for 24 h to obtain the tungsten tailing-based geopolymer, and then cured at room temperature for 3 d, 7 d and 28 d, and then the compressive strength was tested. The test results are shown in Table 1.
. or LU503728
Table 1 Test results of compressive strength of tungsten tailing-based geopolymers prepared in various embodiments:
Embodiments Compressive strength/MPa 3d 7d 28 d 1 99 105 111 2 97 107 112 3 111 114 119 4 86 102 110
According to the data of compressive strength in Table 1, the minimum compressive strength of the tungsten tailing-baesd geopolymer of the invention can reach more than 110 MPa after curing for 28 d, and the compressive performance is excellent.
Claims (7)
1. À preparation method for tungsten tailing-based geopolymer, wherein, it comprises the steps: (1) first, grind tungsten tailings, fly ash and Na2CO3 into powders respectively, and then mix the tungsten tailings powder and fly ash powder with Na2CO3 powder and calcine them respectively to obtain two kinds of calcined products; (2) grind the two calcined products obtained in step (1) into powders respectively, and then mix them evenly to form the geopolymer precursor; (3) add water into the geopolymer precursor in step (2) to form slurry, stir for 5~30 min, inject into a mold, press under the pressure of 10-20 MPa for 10-30 s, demould, seal and maintain at the temperature of 900C for 15-24 h to obtain the tungsten tailing-based geopolymer; after maintenance at room temperature for 28 d, the compressive strength of tungsten tailing-based geopolymer is above 110 MPa.
2. The preparation method for tungsten tailing-based geopolymer, as claimed in claim 1, wherein, in the step (1), the mass ratio of tungsten tailings to fly ash is 10:4~10, and the mass ratios of tungsten tailings to Na2CO3 and fly ash to Na2CO3 are all 10:2-10.
3. The preparation method for tungsten tailing-based geopolymer, as claimed in claim 1, wherein, in the step (1), the calcination temperature of tungsten tailings powder, fly ash powder and Na2CO3 powder is 700~10000C , and the calcination time is 1-3 h.
4. The preparation method for tungsten tailing-based geopolymer, as claimed in claim 1, wherein, in the step (1), the two kinds of calcined products are the calcined products with Na 6.8 (AI6.3S19.7032) with good activity as the main phase.
5. The preparation method for tungsten tailing-based geopolymer, as claimed in claim 1, wherein, in the step (1), the particle sizes of tungsten tailings powder, fly ash powder and Na2CO3 powder are all below 100 meshes.
6. The preparation method for tungsten tailing-based geopolymer, as claimed in claim 1 to 5, wherein, in the step (2), the particle sizes of the two calcined products after grinding are both below 100 meshes.
. oe . . . .LU503728
7. The preparation method for tungsten tailing-based geopolymer, as claimed in claim 1, wherein, in the step (3), the mass ratio of the geopolymer precursor to water is 10:2~5.
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LU503728A LU503728B1 (en) | 2023-03-24 | 2023-03-24 | Preparation method for tungsten tailing-based geopolymer |
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- 2023-03-24 LU LU503728A patent/LU503728B1/en active IP Right Grant
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