CN111393139B - Method for preparing porous water-retaining ceramic material by utilizing spodumene flotation tailings - Google Patents
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Abstract
The invention provides a method for preparing a porous water-retaining ceramic material by utilizing spodumene flotation tailings, which comprises the following steps: (1) weighing 89-93% of spodumene flotation tailings, 6-10% of bonding material and 0.6-1.5% of sodium carboxymethylcellulose according to mass percentage; adding hydrogen peroxide and water into the raw materials, mixing and stirring to prepare slurry; the bonding material is a mixture of common glass powder, bentonite and kaolin according to a weight ratio of 1-3: 1-2, the addition amount of the hydrogen peroxide is 0.01-0.04ml/g, and the addition amount of the water is 30% of the total solid mass; (2) uniformly stirring the slurry obtained in the step (1), standing at 40 ℃ for 30 minutes for foaming, and performing normal-pressure injection molding after foaming; (3) and (3) demolding and drying the product obtained in the step (2), and sintering the blank at 1100-1200 ℃ to obtain the porous water-retaining ceramic material. The ceramic material prepared by the method has excellent mechanical property, high water absorption and high utilization rate of spodumene flotation tailings.
Description
Technical Field
The invention belongs to the technical field of ceramic material preparation from industrial solid waste resources, and particularly relates to a method for preparing a porous water-retaining ceramic material from spodumene flotation tailings.
Background
With the development of society, resource and environment problems are increasingly prominent, how to properly treat solid waste becomes a current hot problem, flotation tailings are used as special solid waste in the solid waste due to the characteristics of the flotation tailings, the yield is high, the pollution problem is complex, the utilization rate is low, and how to recycle the flotation tailings and improve the comprehensive utilization rate becomes a problem to be solved urgently.
The utilization of industrial solid waste as a raw material of the porous water-retaining ceramic industry is an important way for utilizing industrial solid waste on a large scale. The spodumene flotation tailings are solid wastes discharged after lithium resources are selected by lithium production enterprises through flotation or leaching and other processes, contain a large amount of silicate minerals, and mainly comprise SiO as a chemical component2The proportion is up to 79.75%, and the main phase composition is rock-making minerals such as quartz and the like. Patent publication No. CN105541296A proposes a method for preparing ceramic material by using copper tailings, the ceramic material of copper tailings is prepared by pressure forming, and patent publication Nos. CN109626957A and CN109467389A take graphite tailings as raw materials, and ceramic archaized bricks and ceramic tiles are respectively prepared by pressure forming. At present, secondary tailings generated after the spodumene flotation tailings are subjected to re-selection are still mainly treated in a stockpiling mode, and the problem of difficult forming caused by improvement of ridge materials and high granularity after spodumene flotation hinders the application of the spodumene flotation tailings in the aspect of porous ceramic materials.
If the spodumene flotation tailings can be used for preparing the porous water-retaining ceramic material, the burden of treating the tailings of lithium production enterprises can be reduced, and the source of ceramic raw materials can be expanded. Therefore, how to provide a method for preparing a porous water-retaining ceramic material by utilizing spodumene flotation tailings becomes a technical problem to be solved urgently.
Disclosure of Invention
The invention aims to solve the technical problems and provides a method for preparing a porous water-retaining ceramic material by utilizing spodumene flotation tailings. The method solves the problem that the spodumene flotation tailings are difficult to form due to large granularity, omits the ball milling and refining process of raw materials, reduces energy consumption and saves the cost for preparing ceramic materials. The invention also greatly enhances the green strength of the dried porous ceramic material and overcomes the problems of difficult demoulding and easy damage caused by lower strength after the porous ceramic material is dried. The porous water-retaining ceramic material can be successfully prepared by the method, and can be applied to the fields of water-retaining bricks, water-permeable bricks, filtering materials, microorganism carriers and the like.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: a method for preparing a porous water-retaining ceramic material by utilizing spodumene flotation tailings comprises the following steps:
(1) weighing the following raw materials in percentage by mass: 89-93% of spodumene flotation tailings, 6-10% of bonding materials and 0.6-1.5% of sodium carboxymethylcellulose; adding hydrogen peroxide and water into the raw materials, mixing and stirring to prepare slurry; the bonding material is a mixture of common glass powder, bentonite and kaolin, the weight ratio of the common glass powder to the bentonite to the kaolin in the bonding material is 1-3: 1-2, the addition amount of the hydrogen peroxide is 0.01-0.04ml/g based on the total solid mass, and the addition amount of the water is 30% of the total solid mass;
(2) uniformly stirring the slurry obtained in the step (1), standing in a forced air drying oven at 40 ℃ for 30 minutes for foaming, and performing normal-pressure injection molding after foaming;
(3) and (3) demolding and drying the product obtained in the step (2), and sintering the blank at 1100-1200 ℃ to obtain the porous water-retaining ceramic material.
According to the method, common glass powder, bentonite and kaolin are added as bonding materials, and the mixture is subjected to wet injection molding, so that the problem that the spodumene flotation tailings are difficult to form due to large particle size is solved, the ball milling and refining process of raw materials is omitted, the energy consumption is reduced, and the cost for preparing ceramic materials is saved. And a small amount of sodium carboxymethylcellulose is added to be matched with clay mineral kaolin and the like to be used as green body bonding materials, so that the green body strength of the dried porous ceramic material is greatly enhanced, and the problems of difficult demoulding and easy damage caused by low strength after the porous ceramic material is dried are solved. According to the invention, the green body is rapidly expanded and foamed through hydrogen peroxide foaming, and the hydrogen peroxide foaming rate is increased by raising the temperature (40 ℃), so that the addition of manganese dioxide serving as a catalyst is omitted, the test risk is reduced, and the environment is protected (manganese dioxide is decomposed into toxic substances, namely trimmings tetroxide at about 535 ℃, and has pollution). And the selective regulation and control of the porosity of the porous ceramic material can be realized by regulating the adding amount of the hydrogen peroxide, and the regulation and control are carried out before sintering, so that the defect that foaming is invisible and uncontrollable in the conventional high-temperature process is overcome. By regulating and controlling the water injection amount of the raw materials, the invention reduces the water addition amount to the maximum extent under the condition of ensuring that the raw materials can be successfully injected, thereby increasing the content of through holes in air holes in the porous ceramic and overcoming the problem of difficult preparation of the through hole ceramic. The porous ceramic material prepared by the invention has certain mechanical property, the highest water absorption rate can reach 50%, and the apparent porosity is high.
Further, the spodumene flotation tailings are tailings obtained after lithium is extracted by a flotation process or tailings obtained after a leaching process in lithium production enterprises.
Further, the step of demoulding and drying in the step (3) is as follows: drying at 60 deg.C for 48 hr, demoulding, and drying at 120 deg.C for 24 hr.
Further, the sintering process of the green body in the step (3) is as follows: and (3) after the green body sample is cooled to room temperature, placing the green body sample in a high-temperature experimental furnace for normal-pressure sintering, heating to the sintering temperature at the speed of 8 ℃/min, preserving the heat for 1h, cooling to room temperature along with the furnace after sintering is finished, and taking out.
Compared with the prior art, the invention has the following beneficial effects:
(1) the porous water-retaining ceramic material is prepared by using tailings obtained after spodumene flotation as a main raw material, waste is turned into wealth, the spodumene flotation tailings account for 89-93% of the total weight, large-scale resource utilization of industrial solid wastes can be realized, and obvious social benefits, environmental benefits and economic benefits are achieved.
(2) According to the invention, a mixture of common glass powder, bentonite and kaolin is added as a bonding material and is formed by wet injection molding, so that the problem that spodumene flotation tailings are difficult to form due to large particle size is solved, the process of ball milling and refining of raw materials is omitted, the energy consumption is reduced, and the cost for preparing ceramic materials is saved. And a small amount of sodium carboxymethylcellulose is added to be matched with clay mineral kaolin and the like to be used as green body bonding materials, so that the green body strength of the dried porous ceramic material is greatly enhanced, and the problems of difficult demoulding and easy damage caused by low strength after the porous ceramic material is dried are solved. And the porous water-retaining ceramic material with excellent performance is successfully prepared at the temperature of 1100-1200 ℃.
(3) The green body is rapidly expanded and foamed through hydrogen peroxide foaming, the hydrogen peroxide foaming rate is improved through raising the temperature (40 ℃), the addition of a catalyst manganese dioxide is further saved, the test risk is reduced, and the environment is protected (manganese dioxide is decomposed into toxic substances, namely trimmings tetraoxide at about 535 ℃, and has pollution).
(4) And the selective regulation and control of the porosity of the porous ceramic material can be realized by regulating the adding amount of the hydrogen peroxide, and the regulation and control are carried out before sintering, so that the defect that foaming is invisible and uncontrollable in the conventional high-temperature process is overcome.
(5) By regulating and controlling the water injection amount of the raw materials, the invention reduces the water addition amount to the maximum extent under the condition of ensuring that the raw materials can be successfully injected, thereby increasing the content of through holes in air holes in the porous ceramic and overcoming the problem of difficult preparation of the through hole ceramic.
Drawings
FIG. 1 is a schematic diagram of a sintered porous water-retaining ceramic material prepared in example 1 using spodumene flotation tailings as a main raw material; numbers 1, 2 and 3 (or 4, 5, 6 or 7, 8 and 9) in the figure respectively represent that the glass powder, bentonite and kaolin in the binding material at the temperature of 1100 ℃, 1150 ℃ and 1200 ℃ are mixed according to the mass ratio of 2: 1: 1, the numbers in figure 1 correspond to the numbers in table 1. FIG. 2 is a schematic diagram showing a porous water-retaining ceramic material sintered from spodumene flotation tailings prepared in comparative example 1 as a main raw material; in fig. 2, the numbers correspond to the numbers in table 2, the binding material is a mixture of bentonite and kaolin, and the mass ratio of the mixture is 3: 1. the result shows that the shrinkage is severe at high temperature, which is not beneficial to the preparation of porous ceramics.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more clearly understood, the present invention is described in detail below with reference to the following embodiments, and it should be noted that the following embodiments are only for explaining and illustrating the present invention and are not intended to limit the present invention. The invention is not limited to the embodiments described above, but rather, may be modified within the scope of the invention.
Example 1
The porous water-retaining ceramic material is prepared by the following method, wherein the raw materials comprise the following components in parts by weight: the total mass of the solid is 300g, the mass ratios of the spodumene flotation tailings are 89.33%, 91.00% and 92.67%, the mass ratios of the binders are 6.67%, 8.33% and 10%, and the mass ratios of the glass powder, the bentonite and the kaolin in the binders are 2: 1: 1, proportioning 0.67 percent of sodium carboxymethylcellulose by mass, adding 2ml, 3ml and 4ml of hydrogen peroxide by mass respectively, adding water, mixing and stirring, then molding by injection molding, wherein the adding amount of the water is 30 percent of the total solid mass, demolding, drying, and sintering the blank at 1100 ℃, 1150 ℃ and 1200 ℃ respectively. The bending strength, compression strength, porosity, volume weight, water absorption and linear shrinkage test results of the sintered product are shown in the table 1, and the picture of the sample is shown in the attached figure 1.
TABLE 1
Comparative example 1
Weighing the following raw materials in parts by weight: the total mass of the solid is 300g, the mass ratios of the spodumene flotation tailings are 89.33%, 91.00% and 92.67%, the mass ratios of the binders are 6.67%, 8.33% and 10%, and the mass ratio of the binders to the kaolin is 3:1, the mass ratio of the sodium carboxymethylcellulose is 0.67 percent, the adding amount of the hydrogen peroxide is respectively 2ml, 3ml and 4ml, water is added for mixing and stirring, injection molding is carried out, and after demoulding and drying, the blank is sintered at 1100 ℃, 1150 ℃ and 1200 ℃ respectively. The test results of bending strength, compression strength, porosity, volume weight and water absorption of the sintered product are shown in the table 2, and the picture of the sample is shown in the attached figure 2.
TABLE 2
Comparative example 2
The test results, which were obtained by replacing the binder with only ordinary glass frit mixed with kaolin in a weight ratio of 3:1 according to the method of example 1, show that the strength of the ceramic material is reduced compared to that of example 1, with a reduction of 10-15% for each sample.
Comparative example 2
According to the method of the example 1, the bonding material is replaced by only mixing the common glass powder and the bentonite according to the weight ratio of 3:1, and the test result shows that the strength of the ceramic material is slightly increased, the strength increase amplitude is about 10% compared with the example 1, the bentonite can cause the style shrinkage and the strength increase, but can cause the porosity of the material to be remarkably reduced, and the porosity of each sample is reduced by 15-20% compared with the example 1.
Comparative example 3
The preparation was carried out by the method of example 1 without adding hydrogen peroxide, and as a result, it was found that foaming was not caused during the preparation, and the apparent porosity was less than 30% and less than 5% at 1200 ℃.
The bending strength of the ceramic materials prepared in the above example 1 and comparative examples 1 to 3 was tested according to the bending strength test method of the ceramic material of national standard GB/T4741-1999, the compressive strength was tested according to the compressive strength test method of the ceramic material of national standard GB/T4740-1999, the water absorption rate was tested according to the water absorption rate test method of the domestic ceramic of national standard GB/T3299-2011, and the apparent porosity and the volume weight were tested according to the apparent porosity and volume weight test method of the porous water-retaining ceramic of national standard GB/T1966-1996.
Claims (4)
1. A method for preparing a porous water-retaining ceramic material by utilizing spodumene flotation tailings is characterized by comprising the following steps of:
(1) weighing the following raw materials in percentage by mass: 89-93% of spodumene flotation tailings, 6-10% of bonding materials and 0.6-1.5% of sodium carboxymethylcellulose; adding hydrogen peroxide and water into the raw materials, mixing and stirring to prepare slurry; the bonding material is a mixture of common glass powder, bentonite and kaolin, the weight ratio of the common glass powder to the bentonite to the kaolin in the bonding material is 1-3: 1-2, the addition amount of the hydrogen peroxide is 0.01-0.04mL/g based on the total solid mass, and the addition amount of the water is 30% of the total solid mass;
(2) uniformly stirring the slurry obtained in the step (1), standing in a forced air drying oven at 40 ℃ for 30 minutes for foaming, and performing normal-pressure injection molding after foaming;
(3) and (3) demolding and drying the product obtained in the step (2), and sintering the blank at 1100-1200 ℃ to obtain the porous water-retaining ceramic material.
2. The method according to claim 1, wherein the spodumene flotation tailings are tailings obtained after lithium production enterprises extract lithium through a flotation process or tailings obtained after a leaching process.
3. The method according to claim 1, wherein the step of demolding and drying in step (3) is: drying at 60 deg.C for 48 hr, demoulding, and drying at 120 deg.C for 24 hr.
4. The method according to claim 1, wherein the sintering process of the green body in the step (3) is as follows: and (3) after the green body sample is cooled to room temperature, placing the green body sample in a high-temperature experimental furnace for normal-pressure sintering, heating to the sintering temperature at the speed of 8 ℃/min, preserving the heat for 1h, cooling to room temperature along with the furnace after sintering is finished, and taking out.
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