CN111196713A - Method for preparing high-strength support semi-vitrified ceramsite by using low-siliceous red mud raw material - Google Patents

Method for preparing high-strength support semi-vitrified ceramsite by using low-siliceous red mud raw material Download PDF

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CN111196713A
CN111196713A CN202010022147.6A CN202010022147A CN111196713A CN 111196713 A CN111196713 A CN 111196713A CN 202010022147 A CN202010022147 A CN 202010022147A CN 111196713 A CN111196713 A CN 111196713A
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red mud
ceramsite
low
preparing high
siliceous
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CN111196713B (en
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王艳秀
孙伟
王丽
曾华
温雅杰
唐鸿鹄
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Central South University
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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
    • C04B33/00—Clay-wares
    • C04B33/02—Preparing or treating the raw materials individually or as batches
    • C04B33/13—Compounding ingredients
    • C04B33/132—Waste materials; Refuse; Residues
    • C04B33/1321—Waste slurries, e.g. harbour sludge, industrial muds
    • C04B33/1322—Red mud
    • 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
    • C04B33/00—Clay-wares
    • C04B33/02—Preparing or treating the raw materials individually or as batches
    • C04B33/13—Compounding ingredients
    • C04B33/132—Waste materials; Refuse; Residues
    • C04B33/1328—Waste materials; Refuse; Residues without additional clay
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P40/00—Technologies relating to the processing of minerals
    • Y02P40/60—Production of ceramic materials or ceramic elements, e.g. substitution of clay or shale by alternative raw materials, e.g. ashes

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Dispersion Chemistry (AREA)
  • Environmental & Geological Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Treatment Of Sludge (AREA)

Abstract

The invention discloses a method for preparing high-strength support semi-vitrified ceramic granules by using a low-silicon red mud raw material, which comprises the steps of dealkalizing, drying and grinding the red mud to obtain red mud powder; uniformly mixing the red mud powder and a plasticizer, and pressing and molding to obtain a cylindrical ceramsite green body; the method comprises the steps of dealkalizing the red mud, forming a multi-component co-fused semi-vitrified ceramic support body by adopting pressure forming and sintering parameter control means, replacing a mullite crystal phase support body in the traditional ceramsite, and breaking through the problem that the ceramsite has high SiO content2The limitation of component requirements, the limitation of large fluctuation of red mud components and high alkali-containing property on the production of the ceramsite is overcome, the strength of the support ceramsite is ensured, the addition amount of the red mud is greatly increased, the reduction and the resource utilization of the red mud are facilitated, and the problem of red mud stacking is solved.

Description

Method for preparing high-strength support semi-vitrified ceramsite by using low-siliceous red mud raw material
Technical Field
The invention relates to a preparation method of ceramsite, in particular to a method for directly preparing high-strength support semi-vitrified ceramsite by using low-siliceous raw material red mud, belonging to the technical field of comprehensive utilization of metallurgical solid waste,
background
Red mud is alkaline solid waste generated in the production process of alumina. By 2018, the worldwide red mud inventory estimate has reached 36 million tons and has grown at a rate of approximately 1.2 million tons per year. The average utilization rate of the red mud in the world is 15 percent, and the utilization rate of the red mud is only 4 percent when the red mud is used as a major country for producing alumina and red mud in China. A great deal of research is carried out on the treatment of the red mud at home and abroad, and most methods are difficult to realize industrialization due to the limitations of red mud treatment capacity, process economy, potential product risks and practical application performance, so most of the red mud is still treated in a stockpiling mode. Obviously, this is not a long term. Red mud is required to be piled up intensively by building a red mud dam, so that a large amount of land is required to be occupied, and huge amount of construction and maintenance cost of a yard is required to be paid. The key to solve the problem of red mud is to research and develop a comprehensive utilization technology of red mud.
The preparation of the ceramsite by utilizing the solid waste is an excellent comprehensive utilization mode of the solid waste, but the relative content of the main chemical components of the red mud is greatly different from the requirement of the ceramsite, and the ceramsite requires that the raw materials have higher SiO content2The content (generally 53-79%) is beneficial to forming mullite skeleton components at high temperature (over 1200 ℃), and the strength of the ceramsite is increased. SiO in red mud2The content of the red mud is only 15-25%, which is far lower than the component requirement of the ceramsite, the alkali content in the red mud is higher, and if the existing ceramsite preparation method is adopted, the strength of the ceramsite is reduced due to the overlarge addition proportion of the red mud, so that the red mud can only be added as a small amount of auxiliary materials in the ceramsite production process at present.
Disclosure of Invention
Aiming at the problem that the process for preparing the ceramsite by using the red mud in the prior art has low utilization rate due to the limitation of the red mud component and can only be used as an auxiliary material for doping to prepare the ceramsite, the invention aims to provide the method for preparing the high-strength ceramsite by using the single red mud as the raw material.
In order to realize the technical purpose, the invention provides a method for preparing high-strength support semi-vitrified ceramic granules by using a low-silicon red mud raw material, which comprises the steps of dealkalizing, drying and grinding the red mud to obtain red mud powder; uniformly mixing the red mud powder and a plasticizer, and pressing and molding to obtain a cylindrical ceramsite green body; and drying and sintering the green body to form the green body.
In a preferred scheme, the dealkalization adopts a water washing method, an acid washing method or a calcification dealkalization method. These methods are common red mud dealkalization methods in the prior art. If an acid washing method is adopted for dealkalization, acid radical ions need to be removed by water washing after dealkalization.
In a preferred scheme, the dealkalization is to remove Na in the red mud2The content of O is reduced to below 3 percent by mass. The dealkalization is beneficial to reducing the influence of alkali on the strength of the ceramsite.
In a preferred scheme, the red mud powder mainly comprises the following components in percentage by mass: SiO 2211～25％，Fe2O35～35％，Al2O315～25％，CaO 3～15％，H25-20% of O, and the balance of other mineral impurity components. In the preferred composition range, the multi-component eutectic semi-vitreous ceramic support is advantageously produced.
Preferably, the plasticizer comprises at least one of paraffin, polyvinyl alcohol aqueous solution, benzene glue, deionized water, starch solution and biological organic waste liquid. The plasticizer is favorable for the press molding of the red mud powder, and the strength of the ceramsite is improved.
Preferably, the dosage of the plasticizer is not higher than 10% of the mass of the red mud powder. The dosage of the plasticizer is within 10 percent of the mass of the red mud powder, and the proper increase of the dosage of the plasticizer is beneficial to the press molding of the red mud powder and the improvement of the strength of the ceramsite, but the opposite effect can be generated when the dosage is higher than 10 percent.
Preferably, the forming pressure adopted in the compression forming process is more than 10 MPa. More preferably 10 to 30 MPa.
In the preferred scheme, the diameter of the cylindrical ceramsite green body is 0.5-2 cm, and the height-diameter ratio is 0.5-2.
Preferably, the sintering conditions are as follows: the sintering temperature is 950-1250 ℃, and the heat preservation time is 0.5-2 h. It is difficult to obtain a multi-component eutectic semi-vitreous ceramic support if the temperature is too high or too low.
The compression strength of the ceramsite prepared by the method is more than 80MPa, and can reach 335MPa to the maximum.
The method for preparing the ceramsite by using the red mud comprises the following specific steps of:
1) removing free Na in red mud by adopting conventional red mud dealkalization method2O, making Na in slag phase2The content of O is reduced to below 3 percent.
2) Drying the dealkalized red mud to ensure that the dealkalized red mud comprises the following main components in percentage by mass: SiO 2211～25％，Fe2O35～35％，Al2O315～25％，CaO 3～15％，H2O 5～20％。
3) Grinding the dried red mud to be below 100 meshes, adding 0-10% of plasticizer, and uniformly mixing.
4) And (3) adding the red mud material into a pressure die, and shaping on a press machine at a pressure of more than 10MPa to prepare a cylindrical ceramsite green compact.
5) And drying the green body sample in an oven at 105 ℃ for 2 hours, then placing the green body sample in a high-temperature furnace for sintering, wherein the sintering temperature is 950-1250 ℃, preserving the heat for 0.5-2 hours, and then air cooling to the normal temperature to obtain the high-strength ceramsite product.
Compared with the prior art, the technical scheme of the invention has the following beneficial effects:
(1) the invention utilizes red mud raw material to form multi-component co-fused semi-vitrified ceramic branch by means of dealkalization treatment, pressure forming, sintering parameter control and the likeThe support replaces a mullite crystal phase support in the traditional ceramsite, and breaks through the ceramsite to high SiO2Limitations in the requirements of the ingredients.
(2) The invention comprehensively considers Na in the red mud ceramic process2The O has solidification capacity, adopts a partial dealkalization mode, overcomes the problem of 'alkali return' of the red mud-based ceramsite, and has economic applicability.
(3) The invention omits the traditional batching link for preparing the ceramsite, has wider application range for the red mud components, has simple process and can be implemented by utilizing the existing industrial equipment.
(4) The temperature of the multi-component eutectic semi-vitrified ceramic support body generated in the ceramsite preparation process is lower than that of the mullite crystal phase support body, so that the method is more beneficial to energy conservation and consumption reduction in the ceramsite preparation process.
(5) The invention ensures the strength of the support ceramsite, greatly increases the red mud addition amount, contributes to the reduction and reclamation of the red mud, and solves the problem of red mud stacking.
Drawings
FIG. 1 is an XRD pattern of a semi-vitrified ceramic body prepared in example 1.
Detailed Description
The following examples are intended to further illustrate the present disclosure, but not to limit the scope of the claims.
Example 1
Red mud from alumina plant of Guangxi province is washed with water to eliminate alkali (to Na)2O content of 2.8 percent) and drying, wherein the main components and the content of the main components are SiO211％，Fe2O329％，Al2O315％，CaO 14％，H2And (4) O15%. Grinding the dried red mud to be below 100 meshes, adding 5% of deionized water and uniformly mixing. And adding the red mud material into a pressure die, shaping the red mud material on a press machine at the pressure of 20MPa to prepare a cylindrical ceramsite green body with the diameter of 0.6cm and the height-diameter ratio of 0.8, drying the cylindrical ceramsite green body again, placing the cylindrical ceramsite green body into a high-temperature furnace, sintering the cylindrical ceramsite green body for 1h at the temperature of 1150 ℃, and then air-cooling the cylindrical ceramsite green body to the normal temperature to obtain a high-strength red mud-based ceramsite product, wherein the compression peak. XR from ceramsite productsIt can be seen in panel D that it produces a high iron low silicon multicomponent eutectic semi-vitrified ceramic body.
Example 2
Red mud from alumina plant of Guangxi province is washed with water to eliminate alkali (to Na)2O content of 2.8 percent) and drying, wherein the main components and the content of the main components are SiO211％，Fe2O329％，Al2O315％，CaO 14％，H2And (4) O15%. Grinding the dried red mud to be below 100 meshes, adding 5% of deionized water and uniformly mixing. And adding the red mud material into a pressure die, shaping the red mud material on a press machine at the pressure of 20MPa to prepare a cylindrical ceramsite green body with the diameter of 0.6cm and the height-diameter ratio of 0.8, drying the cylindrical ceramsite green body again, placing the cylindrical ceramsite green body into a high-temperature furnace, sintering the cylindrical ceramsite green body for 2 hours at 950 ℃, and then air-cooling the cylindrical ceramsite green body to the normal temperature to obtain a high-strength red mud-based ceramsite product, wherein the compression peak strength of the.
Example 3
Red mud from alumina plant of Shandong is used to remove alkali (to Na) by water washing2O content of 2.6 percent) and drying, the main component and content are SiO217％，Fe2O332％，Al2O318％，CaO 10％，H2And (3) O11%. Grinding the dried red mud to be below 100 meshes, adding 10% of biological organic waste liquid, and uniformly mixing. And adding the red mud material into a pressure die, shaping the red mud material on a press machine at the pressure of 10MPa to prepare a cylindrical ceramsite green body with the diameter of 0.6cm and the height-diameter ratio of 0.8, drying the cylindrical ceramsite green body again, placing the cylindrical ceramsite green body into a high-temperature furnace, sintering the cylindrical ceramsite green body at 1250 ℃ for 1h, and then air-cooling the cylindrical ceramsite green body to the normal temperature to obtain a high-strength red mud-based ceramsite product, wherein the compression peak strength of.
Example 4
Red mud from alumina plant of Guizhou is water washed to eliminate alkali (to Na)2O content of 2.6 percent) and drying, the main component and content are SiO217％，Fe2O323％，Al2O320％，CaO 11％，H2And O18 percent. Grinding the dried red mud to be below 100 meshes, adding the red mud material into a pressure die, shaping the red mud material on a press machine at the pressure of 25MPa to prepare a cylindrical ceramsite green body with the diameter of 0.6cm and the height-diameter ratio of 0.8, and drying the cylindrical ceramsite green body againAnd after drying, placing the dried mixture in a high-temperature furnace, sintering the mixture for 1h at 1150 ℃, and then air-cooling the mixture to normal temperature to obtain the high-strength red mud-based ceramsite product with the compression peak strength of 178 MPa.
Comparative example 1
The other conditions are the same as the example 3, the pressure of 5MPa is only adopted when the green ceramsite is subjected to pressure setting, and the compression peak strength of the fired red mud-based ceramsite product is 56 MPa.
Comparative example 2
The other conditions are the same as the example 3, the sintering temperature is only 800 ℃, and the compression peak strength of the fired red mud-based ceramsite product is 49 MPa.
Comparative example 3
The other conditions are the same as the example 3, the plasticizer is not used only before the pressure forming, and the compression peak strength of the fired red mud-based ceramsite product is 73 MPa.

Claims (9)

1. A method for preparing high-strength support semi-vitrified ceramsite by using a low-silicon red mud raw material is characterized by comprising the following steps of: dealkalizing, drying and grinding the red mud to obtain red mud powder; uniformly mixing the red mud powder and a plasticizer, and pressing and molding to obtain a cylindrical ceramsite green body; and drying and sintering the green body to form the green body.
2. The method for preparing high-strength support semi-vitrified ceramic grains by using low-siliceous red mud raw materials according to claim 1, which is characterized by comprising the following steps: the dealkalization adopts a water washing method, an acid washing method or a calcification dealkalization method.
3. The method for preparing high-strength support semi-vitrified ceramic grains by using the low-siliceous red mud raw material according to claim 1 or 2, which is characterized in that: the dealkalization is to remove Na in the red mud2The content of O is reduced to below 3 percent by mass.
4. The method for preparing high-strength support semi-vitrified ceramic grains by using low-siliceous red mud raw materials according to claim 1, which is characterized by comprising the following steps: the red mud powder mainly comprises the following components in percentage by mass: SiO 2211～25％，Fe2O35～35％，Al2O315～25％，CaO 3～15％，H2O 5～20％。
5. The method for preparing high-strength support semi-vitrified ceramic grains by using low-siliceous red mud raw materials according to claim 1, which is characterized by comprising the following steps: the plasticizer comprises at least one of paraffin, polyvinyl alcohol aqueous solution, benzene glue, deionized water, starch solution and biological organic waste liquid.
6. The method for preparing high-strength support semi-vitrified ceramic grains by using the low-siliceous red mud raw material according to claim 1 or 5, which is characterized in that: the dosage of the plasticizer is not higher than 10% of the mass of the red mud powder.
7. The method for preparing high-strength support semi-vitrified ceramic grains by using low-siliceous red mud raw materials according to claim 1, which is characterized by comprising the following steps: the forming pressure adopted in the pressing forming process is more than 10 MPa.
8. The method for preparing high-strength support semi-vitrified ceramic grains by using low-siliceous red mud raw materials according to claim 1, which is characterized by comprising the following steps: the diameter of the cylindrical ceramsite green body is 0.5-2 cm, and the height-diameter ratio is 0.5-2.
9. The method for preparing high-strength support semi-vitrified ceramic grains by using low-siliceous red mud raw materials according to claim 1, which is characterized by comprising the following steps: the sintering conditions are as follows: the sintering temperature is 950-1250 ℃, and the heat preservation time is 0.5-2 h.
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CN112028608A (en) * 2020-09-07 2020-12-04 山东理工大学 Ceramic filtering membrane prepared from red mud and preparation method thereof
CN112279668A (en) * 2020-10-12 2021-01-29 济南大学 Red mud-based high-strength ceramsite and preparation method thereof
CN113402250A (en) * 2021-06-23 2021-09-17 中国矿业大学 Red mud granulation, solidification and dealkalization method
CN114702299A (en) * 2022-03-03 2022-07-05 武汉理工大学 Heat storage ceramic produced by dealkalized red mud and preparation method thereof
CN115637242A (en) * 2022-10-20 2023-01-24 中南大学 Microbial composite microbial inoculum, preparation method thereof and red mud in-situ biological dealkalization method

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112028608A (en) * 2020-09-07 2020-12-04 山东理工大学 Ceramic filtering membrane prepared from red mud and preparation method thereof
CN112028608B (en) * 2020-09-07 2022-08-05 山东理工大学 Ceramic filtering membrane prepared from red mud and preparation method thereof
CN112279668A (en) * 2020-10-12 2021-01-29 济南大学 Red mud-based high-strength ceramsite and preparation method thereof
CN113402250A (en) * 2021-06-23 2021-09-17 中国矿业大学 Red mud granulation, solidification and dealkalization method
CN114702299A (en) * 2022-03-03 2022-07-05 武汉理工大学 Heat storage ceramic produced by dealkalized red mud and preparation method thereof
CN115637242A (en) * 2022-10-20 2023-01-24 中南大学 Microbial composite microbial inoculum, preparation method thereof and red mud in-situ biological dealkalization method

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