CN107500800B - Porous ceramic material containing copper tailings and preparation method thereof - Google Patents

Porous ceramic material containing copper tailings and preparation method thereof Download PDF

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CN107500800B
CN107500800B CN201710803769.0A CN201710803769A CN107500800B CN 107500800 B CN107500800 B CN 107500800B CN 201710803769 A CN201710803769 A CN 201710803769A CN 107500800 B CN107500800 B CN 107500800B
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parts
copper
copper tailings
ceramic material
porous ceramic
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CN107500800A (en
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成军
朱晓东
邢跃鹏
张栋平
汪晓明
赵长红
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Nantong University
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    • C04B38/06Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances
    • C04B38/063Preparing or treating the raw materials individually or as batches
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Abstract

The invention discloses a porous ceramic material containing copper tailings and a preparation method thereof, wherein the preparation method comprises the following steps: drying and crushing the copper tailings to prepare copper tailing particles; mixing copper tailing particles, potassium feldspar, sandstone, calcium carbonate, carbon powder, fiber and nano wollastonite powder, and then pressing and molding to prepare a material to be sintered; and sintering the material to be sintered at the temperature of 1140-1180 ℃ to prepare the porous ceramic material containing the copper tailings. The invention dries and crushes the copper tailings, mixes the treated copper tailings particles with potassium feldspar, sandstone, calcium carbonate, carbon powder, fiber and nano wollastonite powder, presses and forms, and then sinters the pressed and formed prototype at the temperature of 1140-plus-1180 ℃, so that the prepared porous ceramic material has good use performance such as strength and the like on the premise of using a large amount of copper tailings, improves the effective utilization of the copper tailings, and has high environmental friendliness.

Description

Porous ceramic material containing copper tailings and preparation method thereof
Technical Field
The invention relates to the field of production and preparation of ceramic materials, in particular to a porous ceramic material containing copper tailings and a preparation method thereof.
Background
Copper tailings, also known as copper tailings, are one of the products of separation operations in mineral separation, are the lowest-content copper fractions of the target components, and are left after the ore is crushed and refined. And every 1t of mineral copper is produced, 400t of waste rocks and tailings are produced, so that the yield is extremely high and the use is not high. But it also tends to put a great strain on the surrounding ecological environment and safety. However, the copper tailings are used in a narrow range, so that a large amount of copper tailings are often treated as waste, the economic cost of treatment is high in the treatment process, and the waste is very large.
Therefore, the present invention provides a copper tailing-containing porous ceramic material and a preparation method thereof, which can effectively utilize copper tailings, and the ceramic material prepared while using a large amount of copper tailings still has good use properties such as strength.
Disclosure of Invention
Aiming at the prior art, the invention aims to solve the problems that a large amount of copper tailings are often treated as waste due to the narrow application range of the copper tailings in the prior art, the treatment process is often high in economic cost and great waste is caused, so that the copper tailings can be effectively utilized, and the ceramic material prepared while the copper tailings are used in large amount still has good strength and other use performances, and the preparation method of the copper tailings-containing porous ceramic material are provided.
In order to achieve the above object, the present invention provides a method for preparing a porous ceramic material containing copper tailings, wherein the method comprises:
1) drying and crushing the copper tailings to prepare copper tailing particles;
2) mixing the prepared copper tailing particles, potassium feldspar, sandstone, calcium carbonate, carbon powder, fiber and nano wollastonite powder, and then pressing and molding to prepare a material to be sintered;
3) and sintering the material to be sintered at the temperature of 1140-1180 ℃ to prepare the porous ceramic material containing the copper tailings.
The invention also provides the porous ceramic material containing the copper tailings prepared by the preparation method.
According to the technical scheme, the copper tailings are dried, crushed and the like, the treated copper tailing particles are mixed with potassium feldspar, sandstone, calcium carbonate, carbon powder, fibers and nano wollastonite powder, the mixture is pressed and formed, and the pressed and formed blank is sintered at the temperature of 1140-1180 ℃.
Additional features and advantages of the invention will be set forth in the detailed description which follows.
Detailed Description
The following describes in detail specific embodiments of the present invention. It should be understood that the detailed description and specific examples, while indicating the present invention, are given by way of illustration and explanation only, not limitation.
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
The invention provides a preparation method of a porous ceramic material containing copper tailings, wherein the preparation method comprises the following steps:
1) drying and crushing the copper tailings to prepare copper tailing particles;
2) mixing the prepared copper tailing particles, potassium feldspar, sandstone, calcium carbonate, carbon powder, fiber and nano wollastonite powder, and then pressing and molding to prepare a material to be sintered;
3) and sintering the material to be sintered at the temperature of 1140-1180 ℃ to prepare the porous ceramic material containing the copper tailings.
According to the invention, the copper tailings are dried, crushed and the like, the treated copper tailing particles are mixed with potassium feldspar, sandstone, calcium carbonate, carbon powder, fiber and nano wollastonite powder, the mixture is pressed and formed, and the pressed and formed blank is sintered at the temperature of 1140-plus 1180 ℃, so that the prepared porous ceramic material still has good use performances such as strength and the like on the premise of using a large amount of copper tailings, the effective utilization of the copper tailings is greatly improved, and the environment-friendly degree is high.
In a preferred embodiment of the present invention, in order to make the prepared ceramic material have better service performance, step 1) may further include acid leaching the copper tailings, and then drying and crushing the filter residue.
In a further preferred embodiment, the acid leaching process comprises at least a first acid leaching, a second acid leaching and a third acid leaching; wherein the content of the first and second substances,
the first acid leaching comprises the following steps: stirring and mixing the copper tailings and the acid liquor for 1-3h, standing for 2-4h, and taking filter residue M1;
the second acid leaching comprises: mixing the filter residue M1 with acid liquor under stirring for 0.5-2h, standing for 1-2h, and collecting the filter residue M2;
the third acid leaching comprises the following steps: and stirring and mixing the filter residue M2 with acid liquor for 0.5-1h, and standing for 0.5-1h to obtain filter residue M3.
The acid solution here may be selected from a wide range, and may be selected from, for example, an aqueous nitric acid solution, an aqueous sulfuric acid solution, an aqueous hydrochloric acid solution, and the like. Of course, the concentration can be selected according to the actual requirement, for example, 0.2-0.5 mol/L.
The amount of the above-mentioned raw materials may be selected within a wide range, for example, in a preferred embodiment of the present invention, the potassium feldspar is used in an amount of 5 to 20 parts by weight, the sandstone is used in an amount of 5 to 15 parts by weight, the calcium carbonate is used in an amount of 5 to 10 parts by weight, the carbon powder is used in an amount of 3 to 5 parts by weight, the fiber is used in an amount of 3 to 10 parts by weight, and the nano-silica wollastonite powder is used in an amount of 1 to 5 parts by weight, with respect to 100 parts by weight of the copper tailing particles.
In a further preferred embodiment, the fibers may be selected from glass fibers and/or carbon fibers.
In a more preferred embodiment of the present invention, step 2) may further comprise adding polyvinyl alcohol.
In a preferred embodiment, the polyvinyl alcohol is used in an amount of 3 to 10 parts by weight, relative to 100 parts by weight of the copper tailings particles.
In a further preferred embodiment, in order to make the ceramic material obtained after sintering better in use performance, the sintering process in step 3) may be further selected to include: a heating process, a heat preservation sintering process and a cooling process.
For example, in a preferred embodiment, the temperature rise process is to raise the temperature to 1140-1180 ℃ at a constant speed, and the temperature rise rate is 4-8 ℃/min;
the temperature in the heat-preservation sintering process is 1140-1180 ℃, and the heat-preservation sintering time is 0.5-2 h;
the temperature reduction process is to reduce the temperature at a constant speed to be not higher than 800 ℃, and the temperature reduction rate is 4-8 ℃/min.
The invention also provides the porous ceramic material containing the copper tailings prepared by the preparation method.
The present invention will be described in detail below by way of examples. Stirring and mixing the copper tailings and a sulfuric acid aqueous solution (the concentration is 0.3mol/L) for 2 hours, standing for 3 hours, and taking a filter residue M1; mixing the filter residue M1 with a sulfuric acid aqueous solution (the concentration is 0.3mol/L) for 1 hour, standing for 1 hour, and taking the filter residue M2; and stirring and mixing the filter residue M2 with a sulfuric acid aqueous solution (the concentration is 0.3mol/L) for 0.5h, and standing for 0.5h to obtain a filter residue M3.
Example 1
Drying and crushing the filter residue M3 to obtain copper tailing particles; mixing 100 parts by weight of the prepared copper tailing particles, 5 parts by weight of potassium feldspar, 5 parts by weight of sandstone, 5 parts by weight of calcium carbonate, 3 parts by weight of carbon powder, 3 parts by weight of glass fiber, 1 part by weight of nano wollastonite powder and 3 parts by weight of polyvinyl alcohol, and then pressing and molding to prepare a material to be sintered; and (3) heating the material to be sintered to 1140 ℃ at the speed of 4 ℃/min, preserving the heat for 0.5h, cooling to 800 ℃ at the speed of 4 ℃/min, and cooling at room temperature to obtain the porous ceramic material A1 containing the copper tailings. The water absorption rate is 13.5% according to GB/T1966, the Shore hardness is 32 ℃ according to a Shore hardness tester, and the compressive strength is 105.6MPa and the breaking strength is 53.2 MPa.
Example 2
Drying and crushing the filter residue M3 to obtain copper tailing particles; mixing 100 parts by weight of the prepared copper tailing particles, 20 parts by weight of potassium feldspar, 15 parts by weight of sandstone, 10 parts by weight of calcium carbonate, 5 parts by weight of carbon powder, 10 parts by weight of glass fiber, 5 parts by weight of nano wollastonite powder and 10 parts by weight of polyvinyl alcohol, and then pressing and molding to prepare a material to be sintered; and (3) heating the material to be sintered to 1180 ℃ at the speed of 8 ℃/min, preserving the heat for 2h, cooling to 800 ℃ at the speed of 8 ℃/min, and cooling at room temperature to obtain the porous ceramic material A2 containing the copper tailings. The water absorption was found to be 14.1%, the Shore hardness was found to be 31 degrees, the compressive strength was found to be 106.5MPa, and the flexural strength was found to be 52.5 MPa.
Example 3
Drying and crushing the filter residue M3 to obtain copper tailing particles; mixing 100 parts by weight of the prepared copper tailing particles, 10 parts by weight of potassium feldspar, 10 parts by weight of sandstone, 8 parts by weight of calcium carbonate, 4 parts by weight of carbon powder, 6 parts by weight of glass fiber, 3 parts by weight of nano wollastonite powder and 6 parts by weight of polyvinyl alcohol, and then pressing and molding to prepare a material to be sintered; and (3) heating the material to be sintered to 1150 ℃ at the speed of 6 ℃/min, preserving the heat for 1h, cooling to 800 ℃ at the speed of 6 ℃/min, and cooling at room temperature to obtain the porous ceramic material A3 containing the copper tailings. The water absorption was found to be 14.3%, the Shore hardness was found to be 30 degrees, the compressive strength was found to be 104.7MPa, and the flexural strength was found to be 53.6 MPa.
Example 4
The preparation was carried out according to the preparation method of example 1, except that polyvinyl alcohol was not added, and the porous ceramic material containing copper tailings a4 was obtained. The water absorption was found to be 13.6%, the Shore hardness was found to be 31 degrees, the compressive strength was found to be 95.7MPa, and the flexural strength was found to be 42.5 MPa.
Example 5
The preparation was carried out according to the preparation method of example 1, except that the potassium feldspar was used in an amount of 2 parts by weight, the sandstone was used in an amount of 2 parts by weight, the calcium carbonate was used in an amount of 2 parts by weight, the carbon powder was used in an amount of 1 part by weight, the fiber was used in an amount of 1 part by weight, and the nano-wollastonite powder was used in an amount of 0.5 part by weight, to prepare the porous ceramic material a5 containing copper tailings. The water absorption was found to be 13.5%, the Shore hardness was found to be 31 degrees, the compressive strength was found to be 97.2MPa, and the flexural strength was found to be 43.6 MPa.
Example 6
The preparation was carried out according to the preparation method of example 2, except that the potassium feldspar was used in an amount of 30 parts by weight, the sandstone was used in an amount of 30 parts by weight, the calcium carbonate was used in an amount of 20 parts by weight, the carbon powder was used in an amount of 10 parts by weight, the fiber was used in an amount of 20 parts by weight, and the nano-wollastonite powder was used in an amount of 10 parts by weight, to prepare the porous ceramic material a6 containing copper tailings. The water absorption was found to be 14.5%, the Shore hardness was found to be 30 degrees, the compressive strength was found to be 93.1MPa, and the flexural strength was found to be 41.7 MPa.
Example 7
The preparation was carried out according to the preparation method of example 3, except that the temperature increase rate in the temperature increase process was 2 ℃/min, to obtain the copper tailing-containing porous ceramic material A7. The water absorption was found to be 13.9%, the Shore hardness was 29 degrees, the compressive strength was 92.5MPa, and the flexural strength was 42.3 MPa.
Example 8
The preparation was carried out according to the preparation method of example 3, except that the copper tailing particles were copper tailing stones which were not subjected to the acid leaching treatment, and a porous ceramic material containing copper tailings A8 was obtained. The water absorption was found to be 13.7%, the Shore hardness was found to be 31 degrees, the compressive strength was found to be 91.6MPa, and the flexural strength was found to be 45.2 MPa.
Comparative example 1
The preparation was carried out according to the preparation method of example 1, except that potassium feldspar and sandstone were not added, and a porous ceramic material D1 was prepared. The water absorption was found to be 13.1%, the Shore hardness was found to be 30 degrees, the compressive strength was found to be 56.7MPa, and the flexural strength was found to be 31.5 MPa.
Comparative example 2
The preparation was carried out according to the preparation method of example 2, except that the porous ceramic material D2 was obtained without adding carbon powder. The water absorption was found to be 12.5%, the Shore hardness was found to be 25 degrees, the compressive strength was found to be 63.5MPa, and the flexural strength was found to be 32.7 MPa.
Comparative example 3
The preparation was carried out according to the preparation method of example 3, except that the glass fiber was not added, to obtain a porous ceramic material D3. The water absorption was found to be 13.6%, the Shore hardness was found to be 30 degrees, the compressive strength was found to be 53.8MPa, and the flexural strength was found to be 21.6 MPa.
Comparative example 4
The preparation was carried out according to the preparation method of example 3, except that the nano wollastonite powder was not added, and the porous ceramic material D4 was obtained. The water absorption was found to be 14.1%, the Shore hardness was found to be 31 degrees, the compressive strength was found to be 62.5MPa, and the flexural strength was found to be 31.5 MPa.
Comparative example 5
Sintering was carried out in accordance with the preparation method of example 1 except that the sintering temperature was 1000 ℃ to obtain a porous ceramic material D5. The water absorption was found to be 17.6%, the Shore hardness was found to be 23 degrees, the compressive strength was found to be 72.5MPa, and the flexural strength was found to be 35.6 MPa.
Comparative example 6
Sintering was carried out in accordance with the preparation method of example 2 except that the sintering temperature was 1500 deg.C to obtain a porous ceramic material D6. The water absorption was 11.2%, the Shore hardness was 32 degrees, the compressive strength was 69.8MPa, and the flexural strength was 37.5 MPa.
The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
It should be noted that the various technical features described in the above embodiments can be combined in any suitable manner without contradiction, and the invention is not described in any way for the possible combinations in order to avoid unnecessary repetition.
In addition, any combination of the various embodiments of the present invention is also possible, and the same should be considered as the disclosure of the present invention as long as it does not depart from the spirit of the present invention.

Claims (7)

1. A preparation method of a porous ceramic material containing copper tailings is characterized by comprising the following steps:
1) drying and crushing the copper tailings to prepare copper tailing particles;
2) mixing the prepared copper tailing particles, potassium feldspar, sandstone, calcium carbonate, carbon powder, fiber and nano wollastonite powder, and then pressing and molding to prepare a material to be sintered;
3) sintering the material to be sintered at the temperature of 1140-1180 ℃ to prepare the porous ceramic material containing the copper tailings; the method comprises the following steps of 1), carrying out acid leaching on copper tailings, and then drying and crushing filter residues; wherein the acid leaching process at least comprises primary acid leaching, secondary acid leaching and tertiary acid leaching; wherein the content of the first and second substances,
the first acid leaching comprises the following steps: stirring and mixing the copper tailings and the acid liquor for 1-3h, standing for 2-4h, and taking filter residue M1;
the second acid leaching comprises: mixing the filter residue M1 with acid liquor under stirring for 0.5-2h, standing for 1-2h, and collecting the filter residue M2;
the third acid leaching comprises the following steps: mixing the filter residue M2 with acid liquor under stirring for 0.5-1h, and standing for 0.5-1h to obtain filter residue M3; the preparation method comprises the following steps of mixing, by weight, 100 parts of copper tailing particles, 5-20 parts of potassium feldspar, 5-15 parts of sandstone, 5-10 parts of calcium carbonate, 3-5 parts of carbon powder, 3-10 parts of fibers and 1-5 parts of nano wollastonite powder, wherein the potassium feldspar is used in an amount of 5-20 parts, the carbon powder is used in an amount of 5-15 parts, and the nano wollastonite powder is used in an amount of 1-5 parts.
2. The production method according to claim 1, wherein the fiber is selected from glass fiber and/or carbon fiber.
3. The method of claim 1, wherein step 2) further comprises adding polyvinyl alcohol.
4. The preparation method according to claim 3, wherein the polyvinyl alcohol is used in an amount of 3 to 10 parts by weight, relative to 100 parts by weight of the copper tailings particles.
5. The production method according to claim 1, wherein the sintering process in step 3) includes: a heating process, a heat preservation sintering process and a cooling process.
6. The method according to claim 5, wherein the temperature is raised to 1140-1180 ℃ at a constant rate and at a rate of 4-8 ℃/min;
the temperature in the heat-preservation sintering process is 1140-1180 ℃, and the heat-preservation sintering time is 0.5-2 h;
the temperature reduction process is to reduce the temperature at a constant speed to be not higher than 800 ℃, and the temperature reduction rate is 4-8 ℃/min.
7. A porous ceramic material containing copper tailings produced by the production method according to any one of claims 1 to 6.
CN201710803769.0A 2017-09-08 2017-09-08 Porous ceramic material containing copper tailings and preparation method thereof Expired - Fee Related CN107500800B (en)

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CN105541296A (en) * 2015-12-29 2016-05-04 江西省科学院能源研究所 Method for preparing ceramic material by virtue of copper tailings

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