CN116606161A - Method for preparing porous ceramic from titanium-containing blast furnace slag and silicon slag - Google Patents

Method for preparing porous ceramic from titanium-containing blast furnace slag and silicon slag Download PDF

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CN116606161A
CN116606161A CN202310598791.1A CN202310598791A CN116606161A CN 116606161 A CN116606161 A CN 116606161A CN 202310598791 A CN202310598791 A CN 202310598791A CN 116606161 A CN116606161 A CN 116606161A
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slag
titanium
blast furnace
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furnace slag
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丁满堂
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Panzhihua University
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    • C04B38/02Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by adding chemical blowing agents
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    • C04B33/00Clay-wares
    • C04B33/02Preparing or treating the raw materials individually or as batches
    • C04B33/13Compounding ingredients
    • C04B33/132Waste materials; Refuse; Residues
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    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3205Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
    • C04B2235/3208Calcium oxide or oxide-forming salts thereof, e.g. lime
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    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/34Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3409Boron oxide, borates, boric acids, or oxide forming salts thereof, e.g. borax
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    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/34Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3418Silicon oxide, silicic acids, or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
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    • C04B2235/44Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
    • C04B2235/447Phosphates or phosphites, e.g. orthophosphate, hypophosphite
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Abstract

The invention provides a method for preparing porous ceramics from titanium-containing blast furnace slag and silicon slag, belonging to the technical fields of recycling of metallurgical slag resources, preparation of porous materials and preparation of light materials. The invention relates to a method for preparing porous ceramics from titanium-containing blast furnace slag and silicon slag, which comprises the following steps: uniformly mixing titanium-containing blast furnace slag, silicon slag, shale, quartz sand, limestone, boric acid and phosphate according to the mass ratio of 100:10-25:70:30:2-10:10-30:10-20, and sintering at 1000-1200 ℃ for 0.5-2 h with the balance of unavoidable impurities; after sintering, cooling the sintered product to room temperature to obtain the product with apparent density of 0.4-0.52 g/cm ‑3 The compressive strength is 7.5-8.2 MPa, and the flexural strength is 3.5-4.0 MPa. The method for preparing the porous ceramic from the titanium-containing blast furnace slag and the silicon slag has the advantages of obviously reducing energy consumption and simplifying the process flowAnd has good social and economic benefits.

Description

Method for preparing porous ceramic from titanium-containing blast furnace slag and silicon slag
Technical Field
The invention relates to a method for preparing porous ceramics from titanium-containing blast furnace slag and silicon slag, belonging to the technical fields of recycling metallurgical slag resources, preparing porous materials and preparing light materials.
Background
The use of titanium-containing blast furnace slag is classified into 2 directions of titanium extraction use and non-titanium extraction use. Titanium extraction utilization is in a research stage and cannot realize industrial utilization. Non-titanium extraction utilization realizes industrial utilization, but fails to realize deep utilization with high added value. At present, the main mode of utilizing the titanium-containing blast furnace slag is used as coarse and fine aggregate of buildings, paving materials and the like, and the utilization value of the titanium-containing blast furnace slag is not high. The research on non-titanium extraction mainly includes microcrystalline glass, photocatalytic materials, fertilizer use and the like, but the research has not been popularized and applied.
The patent application of CN110256047A discloses a method for preparing foamed ceramics by utilizing titanium-containing blast furnace slag and shale waste residues, which comprises the following specific steps: s1, preparing titanium-containing blast furnace slag, shale waste residue and silicon dioxide powder as raw materials; s2, preparing borax, ball clay, a foaming agent, magnesium oxide, manganese oxide and sodium metaphosphate as additives; s3, mixing all the raw materials and additives, and wet-grinding to prepare slurry; s4, placing the slurry into a baking oven for drying, and then crushing in a crusher to prepare powder, wherein the particle size of the powder is 200-300 meshes; s5, filling the powder particles into a die, and then carrying out roasting foaming and crystallization processes by using a medium-temperature box type resistance furnace; and then cooling to obtain the foamed ceramic. The method has the following defects: the method has the advantages of multiple raw materials, complex types, multiple process links and long process flow.
The patent application of CN101323503A discloses a method for preparing microcrystalline foam glass from titanium-containing blast furnace slag, which comprises the following specific steps: preparing a glassy material, sintering the glassy material, preparing a foam glass material, preparing foam glass, crystallizing the foam glass, and obtaining the foam glass with full microcrystallization. The method has the following defects: the method has long and complex process flow, and the middle part needs to be subjected to multiple heating, cooling, heat preservation, annealing and other hot processing processes, so that the energy consumption is high.
Disclosure of Invention
The first technical problem to be solved by the invention is to provide a method for preparing porous ceramics from titanium-containing blast furnace slag and silicon slag.
The method for preparing the porous ceramic from the titanium-containing blast furnace slag and the silicon slag comprises the following steps:
a. uniformly mixing titanium-containing blast furnace slag, silicon slag, shale, quartz sand, limestone, boric acid and phosphate according to the mass ratio of 100:10-25:70:30:2-10:10-30:10-20, and sintering at 1000-1200 ℃ for 0.5-2 h with the balance of unavoidable impurities;
b. and after the sintering is finished, cooling the sintered product to room temperature to obtain the porous ceramic.
Preferably, in the step a, the titanium-containing blast furnace slag, the silicon slag, the shale, the quartz sand, the limestone, the boric acid and the phosphate are uniformly mixed according to the mass ratio of 100:15-25:70:30:2-4:10-15:20.
Wherein the granularity of the titanium-containing blast furnace slag, the silicon slag, the shale, the quartz sand, the limestone, the boric acid and the phosphate in the step a is less than or equal to 0.5mm.
Wherein the mixing uniformity of the titanium-containing blast furnace slag, the silicon slag, the shale, the quartz sand, the limestone, the boric acid and the phosphate in the step a is more than or equal to 98.5 percent.
Preferably, the sintering time in step a is 0.5 to 1h.
The second technical problem to be solved by the invention is to provide the porous ceramic prepared by the method for preparing the porous ceramic from the titanium-containing blast furnace slag and the silicon slag.
Wherein the apparent density of the porous ceramic is 0.4-0.52 g/cm -3 The compressive strength is 7.5-8.2 MPa, and the flexural strength is 3.5-4.0 MPa.
The invention has the beneficial effects that:
1. the method for preparing the porous ceramic from the titanium-containing blast furnace slag and the silicon slag solves the problem that the porous material is prepared through repeated heating and heat preservation, and the porous material can be directly obtained through one-time heating and sintering, so that the energy consumption is remarkably reduced.
2. The method for preparing the porous ceramic from the titanium-containing blast furnace slag and the silicon slag provided by the invention avoids the preparation process of slurry, correspondingly eliminates the processes of drying the slurry, crushing and pulverizing the dried body and the like, and obviously improves and simplifies the technological process.
3. The method for preparing the porous ceramic from the titanium-containing blast furnace slag and the silicon slag directly uses the silicon slag waste, comprehensively utilizes industrial waste slag such as the titanium-containing blast furnace slag and the silicon slag, avoids the use of new materials as much as possible, avoids the use of expensive materials such as silicon carbide, lithium carbonate, management and control materials such as potassium permanganate, and has good social and economic benefits.
Drawings
FIG. 1 is a SEM microstructure morphology graph of a porous ceramic section obtained by the method for preparing the porous ceramic by using the titanium-containing blast furnace slag and the silica slag
FIG. 2 is a photograph of a porous ceramic section obtained by the method for preparing porous ceramic from titanium-containing blast furnace slag and silica slag according to the present invention
Detailed Description
Embodiments of the present invention will be described in detail below with reference to specific examples, but it will be understood by those skilled in the art that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention. The examples were conducted under conventional conditions, except that the specific conditions were not specified.
The method for preparing porous ceramics from the titanium-containing blast furnace slag and the silicon slag comprises the following steps:
A. respectively crushing titanium-containing blast furnace slag, silicon slag, shale, quartz sand, limestone (carbonate), boric acid and phosphate to a granularity of 0.5mm, and uniformly mixing until the mixing degree is more than or equal to 98.5%; sintering in a high temperature furnace for 0.5-2 h;
B. after the reaction is completed, cooling to room temperature to obtain the porous ceramic.
Example 1
Respectively crushing 5g of titanium-containing blast furnace slag, 0.5g of silica slag, 3.5g of shale, 1.5g of quartz sand, 0.5g of limestone (carbonate), 1.5g of boric acid and 0.5g of phosphate to 0.5mm of granularity, and uniformly mixing until the uniformity is more than or equal to 98.5%; placing the mixture into a high-temperature furnace, and sintering the mixture for 2 hours at 1000 ℃; after the reaction is completed, cooling to room temperature to obtain the porous ceramic. The apparent density of the ceramic is 0.43g cm -3 The compressive strength is 7.7MPa, and the flexural strength is 3.5MPa. The experimental data are shown in table 1.
Example 2
Respectively crushing 5g of titanium-containing blast furnace slag, 0.75g of silica slag, 3.5g of shale, 1.5g of quartz sand, 0.3g of limestone (carbonate), 1.5g of boric acid and 0.5g of phosphate to 0.5mm of granularity, and uniformly mixing until the uniformity is more than or equal to 98.5%; sintering in a high temperature furnace at 1070 deg.c for 1 hr; reactionAnd after cooling to room temperature, obtaining the porous ceramic. The apparent density of the ceramic is 0.47g cm -3 The compressive strength is 7.8MPa, and the flexural strength is 4.0MPa. The experimental data are shown in table 1.
Example 3
Respectively crushing 5g of titanium-containing blast furnace slag, 0.75g of silica slag, 3.5g of shale, 1.5g of quartz sand, 0.3g of limestone (carbonate), 1.5g of boric acid and 0.5g of phosphate to 0.5mm of granularity, and uniformly mixing until the uniformity is more than or equal to 98.5%; placing the mixture into a high-temperature furnace, and sintering the mixture for 1h at 1150 ℃; after the reaction is completed, cooling to room temperature to obtain the porous ceramic. The apparent density of the ceramic is 0.42g cm -3 The compressive strength is 7.9MPa, and the flexural strength is 3.9MPa. The experimental data are shown in table 1.
Example 4
Respectively crushing 5g of titanium-containing blast furnace slag, 1.0g of silica slag, 3.5g of shale, 1.5g of quartz sand, 0.2g of limestone (carbonate), 0.5g of boric acid and 1.0g of phosphate to 0.5mm of granularity, and uniformly mixing until the uniformity is more than or equal to 98.5%; sintering in a high temperature furnace at 1170 ℃ for 0.5h; after the reaction is completed, cooling to room temperature to obtain the porous ceramic. The apparent density of the ceramic is 0.5g cm -3 The compressive strength is 8.0MPa, and the flexural strength is 4.0MPa. The experimental data are shown in table 1.
Example 5
Respectively crushing 5g of titanium-containing blast furnace slag, 1.25g of silica slag, 3.5g of shale, 1.5g of quartz sand, 0.1g of limestone (carbonate), 0.5g of boric acid and 1.0g of phosphate to 0.5mm of granularity, and uniformly mixing until the uniformity is more than or equal to 98.5%; placing the mixture into a high-temperature furnace, and sintering the mixture for 0.3h at 1200 ℃; after the reaction is completed, cooling to room temperature to obtain the porous ceramic. The apparent density of the ceramic is 0.52g cm -3 The compressive strength is 8.1MPa, and the flexural strength is 3.8MPa. The experimental data are shown in table 1.
TABLE 1
The present embodiment is merely illustrative of the invention and not intended to be limiting, and those skilled in the art will make modifications or improvements on the basis of the present invention after reading the description of the invention, but are protected by the patent laws within the scope of the claims of the present invention.

Claims (7)

1. The method for preparing the porous ceramic from the titanium-containing blast furnace slag and the silicon slag is characterized by comprising the following steps of:
a. uniformly mixing titanium-containing blast furnace slag, silicon slag, shale, quartz sand, limestone, boric acid and phosphate according to the mass ratio of 100:10-25:70:30:2-10:10-30:10-20, and sintering at 1000-1200 ℃ for 0.5-2 h with the balance of unavoidable impurities;
b. and after the sintering is finished, cooling the sintered product to room temperature to obtain the porous ceramic.
2. The method for preparing porous ceramics from titanium-containing blast furnace slag and silica slag according to claim 1, wherein the titanium-containing blast furnace slag, silica slag, shale, quartz sand, limestone, boric acid and phosphate in the step a are uniformly mixed according to the mass ratio of 100:15-25:70:30:2-4:10-15:20.
3. The method for preparing porous ceramics from titanium-containing blast furnace slag and silica slag according to claim 1, wherein the granularity of the titanium-containing blast furnace slag, silica slag, shale, quartz sand, limestone, boric acid and phosphate in the step a is less than or equal to 0.5mm.
4. The method for preparing porous ceramics from titanium-containing blast furnace slag and silica slag according to claim 1, wherein the mixing uniformity of the titanium-containing blast furnace slag, silica slag, shale, quartz sand, limestone, boric acid and phosphate in the step a is more than or equal to 98.5%.
5. The method for preparing porous ceramics from titanium-containing blast furnace slag and silica slag according to claim 1, wherein the sintering time in the step a is 0.5-1 h.
6. The porous ceramic produced by the method for producing porous ceramic from titanium-containing blast furnace slag and silica slag according to any one of claims 1 to 5.
7. The porous ceramic according to claim 6, wherein: the apparent density of the porous ceramic is 0.4-0.52 g/cm -3 The compressive strength is 7.5-8.2 MPa, and the flexural strength is 3.5-4.0 MPa.
CN202310598791.1A 2023-05-25 2023-05-25 Method for preparing porous ceramic from titanium-containing blast furnace slag and silicon slag Pending CN116606161A (en)

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CN108529887A (en) * 2018-04-02 2018-09-14 四川大学 A kind of preparation method of high intensity, porous sound-absorbing material
CN110256047A (en) * 2019-07-11 2019-09-20 东北大学 A method of foamed ceramic is prepared using titanium-containing blast furnace slag and shale waste residue
CN110668786A (en) * 2019-09-25 2020-01-10 攀钢集团攀枝花钢铁研究院有限公司 Foamed ceramic and preparation method and application thereof
CN112898045A (en) * 2021-03-31 2021-06-04 成渝钒钛科技有限公司 High-titanium blast furnace slag porous sound-absorbing ceramic and preparation method thereof
CN113045291A (en) * 2021-03-31 2021-06-29 成渝钒钛科技有限公司 High-titanium blast furnace slag external thermal insulation material and preparation method thereof
CN113087543A (en) * 2021-03-31 2021-07-09 成渝钒钛科技有限公司 High-titanium blast furnace slag high-strength lightweight aggregate and preparation method thereof

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2001253765A (en) * 2000-03-08 2001-09-18 Kurosaki Harima Corp Magnesia-alumina-titania-based brick
CN105461346A (en) * 2015-11-23 2016-04-06 攀钢集团攀枝花钢铁研究院有限公司 Method for preparing porous material by use of blast furnace slag titanium-extracting tailings
CN108529887A (en) * 2018-04-02 2018-09-14 四川大学 A kind of preparation method of high intensity, porous sound-absorbing material
CN110256047A (en) * 2019-07-11 2019-09-20 东北大学 A method of foamed ceramic is prepared using titanium-containing blast furnace slag and shale waste residue
CN110668786A (en) * 2019-09-25 2020-01-10 攀钢集团攀枝花钢铁研究院有限公司 Foamed ceramic and preparation method and application thereof
CN112898045A (en) * 2021-03-31 2021-06-04 成渝钒钛科技有限公司 High-titanium blast furnace slag porous sound-absorbing ceramic and preparation method thereof
CN113045291A (en) * 2021-03-31 2021-06-29 成渝钒钛科技有限公司 High-titanium blast furnace slag external thermal insulation material and preparation method thereof
CN113087543A (en) * 2021-03-31 2021-07-09 成渝钒钛科技有限公司 High-titanium blast furnace slag high-strength lightweight aggregate and preparation method thereof

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