CN112745101A - Method for preparing high-performance porous ceramic by using iron tailings - Google Patents
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Abstract
The invention discloses a method for preparing high-performance porous ceramics by using iron tailings in the industrial solid waste comprehensive utilization industry, which aims to solve the problem of unstable performance of the porous ceramics prepared by using the iron tailings. The porous ceramic prepared by the method has the advantages of oxidation resistance, high temperature resistance, good adsorption performance, stable and reliable performance and the like, and is wide in application and high in market value.
Description
The technical field is as follows:
the invention relates to the technical field of comprehensive utilization of iron tailings, in particular to a method for preparing high-performance porous ceramic by using iron tailings, and belongs to the technical field of comprehensive utilization of industrial solid wastes.
Background art:
in recent years, the country pays more and more attention to the field of comprehensive utilization of industrial solid waste, and with the temporary method for comprehensive utilization evaluation management of industrial solid waste resources and the catalogue of national comprehensive utilization products of industrial solid waste resources, which are released by the national ministry of industry and trust in 5 months in 2018, the method aims to establish a scientifically-specified comprehensive utilization evaluation mechanism of industrial solid waste resources and guide enterprises to actively develop the comprehensive utilization of the industrial solid waste resources. The implementation of the policy system promotes the implementation of the comprehensive utilization work of industrial solid wastes in China, and provides powerful support for the development of the comprehensive utilization industry of the relevant industrial solid wastes.
The iron tailings belong to one of large industrial solid wastes, have large production quantity, are difficult to dispose and are mostly stockpiled. At present, billions of tons of iron tailings are accumulated in China, 3 billion tons of iron tailings are continuously generated every year, and the iron tailings are piled up for a long time, so that land is wasted, the surrounding environment is seriously harmed, and harmless and resource treatment is urgently needed. At present, backfilling, building materials, roadbed and the like are generally adopted as a domestic comprehensive utilization mode of iron tailings, and the increasingly growing disposal requirements of the domestic iron tailings are difficult to meet due to the limitation of the doping proportion of the iron tailings, the weak economy and the like.
In recent years, more comprehensive utilization technologies of iron tailings are developed, such as "an iron tailing heat-absorbing functional ceramic material and a preparation method thereof" (application publication No. CN 110194653 a), "an iron tailing based black solar heat-absorbing ceramic and a preparation method thereof" (application publication No. CN 110128105 a), "an iron tailing porous material used as a microorganism ceramsite filter material and a preparation method and application thereof" (publication No. CN 105693277B), "a method for preparing iron tailing porous ceramic by foam injection-coagulation-low-temperature sintering" (publication No. CN 106830989B), and the like. The technology mainly adopts a foaming, injection and coagulation forming-low-temperature sintering method to prepare the porous ceramic product, and the technology has good realizability. However, the iron tailings in most domestic areas have low silicon-aluminum content and complex composition containing associated metals and minerals, so that the prepared porous ceramic has unstable performance and low activity and is difficult to apply on a large scale.
The invention content is as follows:
the invention aims to mainly solve the technical problem of providing a comprehensive utilization method of iron tailings, and solve the problems of difficult disposal and high comprehensive utilization cost of the existing iron tailings.
The purpose of the invention is realized by the following technical scheme:
a method for preparing high-performance porous ceramic by using iron tailings comprises the following steps,
the first step is as follows: grading and sorting the iron tailings by using grading and sorting equipment, and sorting 95-115 meshes of tailings granules according to the condition that the contents of Al2O3 and SiO2 in the iron tailings are in a negative correlation with the strength so as to improve the content of aluminum and silicon in the sorted tailings granules;
the second step is that: adding a certain amount of water into a tailing granule raw material to form slurry, sequentially adding a monomer accounting for 2-5.5 wt.% of the slurry, a cross-linking agent accounting for 0.2-0.6 wt.% of the slurry and a dispersing agent accounting for 0.25-2.5 wt.% of the slurry under stirring to prepare a premixed liquid, and performing ball milling for 6-11 hours to obtain a mixed slurry with a solid content of 30-70%;
the third step: adding a polyurethane raw material serving as a foaming agent into the mixed slurry to perform a foaming reaction; then adding an initiator, stirring uniformly, injecting the mixture into a mold, and curing and forming to obtain a foaming agent-polyurethane raw material;
the fourth step: demoulding the formed material, and heating the formed material in a drying box until the surface of the formed material is completely dried;
the fifth step: and (2) after demoulding and heating and drying the formed material, setting a sintering temperature rise program, starting temperature rise from normal temperature, keeping the temperature rise rate at 2.5 ℃/min, respectively setting three temperature interval points of 300 ℃, 950 ℃ and 1120 ℃, preserving heat for 1-2 h when the temperature rises to 300 ℃, preserving heat for 2-3 h when the temperature rises to 950 ℃, preserving heat for 3-8 h when the temperature rises to 1020 ℃, and naturally cooling to obtain the nano-scale porous ceramic product.
The monomer in the invention refers to acrylamide; the cross-linking agent is N, N-methylene bisacrylamide; the dispersant is ammonium polyacrylate.
The foaming agent is a polyurethane raw material, and the adding amount of the foaming agent is 0.02-0.5 wt% of the slurry; the initiator is ammonium persulfate, and the addition amount of the initiator is 0.1-1.0 wt% of the slurry.
The preparation method of the foaming agent polyurethane raw material comprises the following steps: putting polyether polyol into a vacuum dehydrator, performing vacuum dehydration for 3h at 110 ℃, then cooling to 65 ℃, adding toluene diisocyanate with the stoichiometric number being 1.5 times that of the polyether polyol (the temperature is 65 ℃), controlling the reaction temperature to be 75 ℃ and 85 ℃, wherein the reaction is exothermic reaction, reacting at 75 ℃ for a period of time, adjusting to 85 ℃ after the temperature is stable, and stopping heating after the reaction temperature is stable to obtain the foaming agent-polyurethane raw material.
In the invention, the fine-grained raw materials obtained by crushing and sorting the iron tailings are 95-115 meshes; the iron tailings, water, a monomer, a cross-linking agent and a dispersing agent are prepared into a premixed liquid, and the solid content of the mixed slurry obtained after ball milling is 40-70%.
The aperture of the porous ceramic product is 50-200 nm.
The invention improves the content of silicon and aluminum in the raw materials by crushing and sorting the iron tailings, adopts the polyurethane raw material as a foaming agent, adds a cross-linking agent, a dispersing agent, an initiator and the like, adopts the foaming-gel injection molding process, and carries out the process steps of ball milling, foaming, gelling, drying, sintering and the like on the mixed slurry to obtain the nano-scale porous ceramic. The porous ceramic prepared by the method has the advantages of oxidation resistance, high temperature resistance, strong activity, good adsorption performance, stable performance and the like, and is wide in application and high in market value.
Description of the drawings:
FIG. 1 is a flow chart of a technique for preparing high-performance porous ceramics by using iron tailings according to the invention;
FIG. 2 is a flow chart of the blowing agent-polyurethane raw material preparation technique of the present invention.
The specific implementation mode is as follows:
the present invention is further illustrated by the following examples, which are not intended to limit the scope of the invention.
The chemical compositions of several iron tailings in China are shown in the following table.
Crushing and sorting the iron tailings by adopting a grading sorting crusher according to Al in the iron tailings2O3And SiO2The content and the strength are in a negative correlation relationship, fine grains with low strength are sorted out, and the content of silicon and aluminum in the sorted raw materials is improved. The sorted fine-grained raw material with low strength has a particle size of 95-115 meshes and a silica content of 30-70%.
Example 1
Adding water, a monomer, a cross-linking agent and a dispersing agent into an iron tailing raw material in a mixing tank to prepare a premixed solution according to the following proportion, and adopting a rod-type ball mill to control the ball milling ratio to be 1.5:1 and the ball milling time to be 10 hours to obtain mixed slurry; wherein the monomer acrylamide is added in an amount of 2 wt.% of the slurry; the addition of the cross-linking agent N, N-methylene-bisacrylamide is 0.2 wt.% of the slurry; the addition amount of the ammonium polyacrylate serving as a dispersant is 0.25 wt% of the slurry, and the addition amount of the iron tailings is 40 wt% of the slurry.
Polyurethane raw materials are used as foaming agents and added into the mixed slurry, the mixture is uniformly stirred, and foaming reaction is carried out. Then adding an initiator, stirring uniformly, and injecting the mixture into a mold for curing and forming; wherein the adding amount of the polyurethane raw material is 0.02 wt% of the slurry, and the adding amount of the initiator ammonium persulfate is 0.1 wt% of the slurry.
Demoulding the cured and formed material, and putting the material into a drying box for heating until the surface of the formed material is completely dried; the heating temperature is 105 ℃, and the heating time is 3 h.
And putting the dried forming material into an electric furnace for sintering. Setting a sintering temperature rise program, starting temperature rise from normal temperature, keeping the temperature rise rate at 2.5 ℃/min, respectively setting three temperature interval points of 300 ℃, 950 ℃ and 1120 ℃, preserving heat for 1h when the temperature rises to 300 ℃, preserving heat for 2h when the temperature rises to 950 ℃, and preserving heat for 5h when the temperature rises to 1020 ℃; naturally cooling to obtain the nano-scale porous ceramic product.
The prepared porous ceramic has apparent porosity of 78% and volume density of 0.36g/cm3The compression strength is 0.76MPa, and the aperture is 100-150 nm.
Example 2
Adding water, a monomer, a cross-linking agent and a dispersing agent into an iron tailing raw material in a mixing tank to prepare a premixed solution according to the following proportion, and adopting a rod-type ball mill to control the ball milling ratio to be 1.5:1, wherein the ball milling time is 7 hours, so as to obtain mixed slurry; wherein the monomer acrylamide is added in an amount of 2.5 wt.% of the slurry; the addition of the cross-linking agent N, N-methylene-bisacrylamide is 0.3 wt.% of the slurry; the addition amount of the ammonium polyacrylate serving as a dispersant is 0.5 wt% of the slurry, and the addition amount of the iron tailings is 45 wt% of the slurry.
Polyurethane raw materials are used as foaming agents and added into the mixed slurry, the mixture is uniformly stirred, and foaming reaction is carried out. Then adding an initiator, stirring uniformly, and injecting the mixture into a mold for curing and forming; wherein the polyurethane raw material is added in an amount of 0.1 wt.% of the slurry; the initiator ammonium persulfate was added at 0.2 wt.% of the slurry.
And (4) demolding the cured and formed material, and heating the material in a drying box until the surface of the formed material is completely dried. The heating temperature is 105 ℃, and the heating time is 3 h.
And putting the dried forming material into an electric furnace for sintering. Setting a sintering temperature rise program, starting temperature rise from normal temperature, keeping the temperature rise rate at 2.5 ℃/min, respectively setting three temperature interval points of 300 ℃, 950 ℃ and 1120 ℃, preserving heat for 1h when the temperature rises to 300 ℃, preserving heat for 2h when the temperature rises to 950 ℃, and preserving heat for 5h when the temperature rises to 1020 ℃; naturally cooling to obtain the nano-scale porous ceramic product.
The prepared porous ceramic has the apparent porosity of 83 percent and the volume density of 0.41g/cm3The compression strength is 0.89MPa, and the aperture is 100-130 nm.
Example 3
Adding water, a monomer, a cross-linking agent and a dispersing agent into an iron tailing raw material in a mixing tank to prepare a premixed solution according to the following proportion, and adopting a rod-type ball mill to control the ball milling ratio to be 1.5:1, wherein the ball milling time is 9 hours, so as to obtain mixed slurry; wherein the monomer acrylamide is added at 3.0 wt.% of the slurry; the addition of the cross-linking agent N, N-methylene-bisacrylamide is 0.4 wt.% of the slurry; the addition amount of the ammonium polyacrylate serving as a dispersant is 1.0 wt% of the slurry, and the addition amount of the iron tailings is 45 wt% of the slurry.
Polyurethane raw materials are used as foaming agents and added into the mixed slurry, the mixture is uniformly stirred, and foaming reaction is carried out. Then adding an initiator, stirring uniformly, and injecting the mixture into a mold for curing and forming; wherein the polyurethane raw material is added in an amount of 0.2 wt.% of the slurry; the initiator ammonium persulfate was added at 0.4 wt.% of the slurry.
Demoulding the cured and formed material, and putting the material into a drying box for heating until the surface of the formed material is completely dried; the heating temperature is 105 ℃, and the heating time is 3 h.
And putting the dried forming material into an electric furnace for sintering. Setting a sintering temperature rise program, starting temperature rise from normal temperature, keeping the temperature rise rate at 2.5 ℃/min, respectively setting three temperature interval points of 300 ℃, 950 ℃ and 1120 ℃, preserving heat for 1h when the temperature rises to 300 ℃, preserving heat for 2h when the temperature rises to 950 ℃, and preserving heat for 5h when the temperature rises to 1020 ℃; naturally cooling to obtain the nano-scale porous ceramic product.
The prepared porous ceramic has the apparent porosity of 88 percent and the volume density of 0.82g/cm3The compression strength is 0.91MPa, and the aperture is 80-130 nm.
Example 4
Adding water, a monomer, a cross-linking agent and a dispersing agent into an iron tailing raw material in a mixing tank to prepare a premixed solution according to the following proportion, and adopting a rod-type ball mill to control the ball milling ratio to be 1.5:1 and the ball milling time to be 1.5h to obtain mixed slurry; wherein the monomer acrylamide is added in an amount of 4.0 wt.% of the slurry; the addition of the cross-linking agent N, N-methylene-bisacrylamide is 0.45 wt.% of the slurry; the addition amount of the ammonium polyacrylate serving as a dispersant is 1.5 wt% of the slurry, and the addition amount of the iron tailings is 55 wt% of the slurry.
Polyurethane raw materials are used as foaming agents and added into the mixed slurry, the mixture is uniformly stirred, and foaming reaction is carried out. Then adding an initiator, stirring uniformly, and injecting the mixture into a mold for curing and forming; wherein the polyurethane raw material is added in an amount of 0.3 wt.% of the slurry; the initiator ammonium persulfate was added at 0.6 wt.% of the slurry.
Demoulding the cured and formed material, and putting the material into a drying box for heating until the surface of the formed material is completely dried; the heating temperature is 105 ℃, and the heating time is 3 h.
And putting the dried forming material into an electric furnace for sintering. Setting a sintering temperature rise program, starting temperature rise from normal temperature, keeping the temperature rise rate at 2.5 ℃/min, respectively setting three temperature interval points of 300 ℃, 950 ℃ and 1120 ℃, preserving heat for 2h when the temperature rises to 300 ℃, preserving heat for 3h when the temperature rises to 950 ℃, and preserving heat for 8h when the temperature rises to 1020 ℃; naturally cooling to obtain the nano-scale porous ceramic product.
The prepared porous ceramic has the apparent porosity of 90 percent and the volume density of 0.68g/cm3The compression strength is 2.91MPa, and the aperture is 50-100 nm.
Example 5
Adding water, a monomer, a cross-linking agent and a dispersing agent into an iron tailing raw material in a mixing tank to prepare a premixed solution according to the following proportion, and adopting a rod-type ball mill to control the ball milling ratio to be 1.5:1 and the ball milling time to be 8 hours to obtain mixed slurry; wherein the monomer acrylamide is added in an amount of 4.5 wt.% of the slurry; the addition of the cross-linking agent N, N-methylene-bisacrylamide is 0.5 wt.% of the slurry; the addition amount of the ammonium polyacrylate serving as a dispersant is 2.0 wt% of the slurry, and the addition amount of the iron tailings is 48 wt% of the slurry.
Polyurethane raw materials are used as foaming agents and added into the mixed slurry, the mixture is uniformly stirred, and foaming reaction is carried out. Then adding an initiator, stirring uniformly, and injecting the mixture into a mold for curing and forming; wherein the polyurethane raw material is added in an amount of 0.4 wt.% of the slurry; the initiator ammonium persulfate was added at 0.8 wt.% of the slurry.
Demoulding the cured and formed material, and putting the material into a drying box for heating until the surface of the formed material is completely dried; the heating temperature is 105 ℃, and the heating time is 3 h.
And putting the dried forming material into an electric furnace for sintering. Setting a sintering temperature rise program, starting temperature rise from normal temperature, keeping the temperature rise rate at 2.5 ℃/min, respectively setting three temperature interval points of 300 ℃, 950 ℃ and 1120 ℃, preserving heat for 2h when the temperature rises to 300 ℃, preserving heat for 3h when the temperature rises to 950 ℃, and preserving heat for 8h when the temperature rises to 1020 ℃; naturally cooling to obtain the nano-scale porous ceramic product.
The prepared porous ceramic has an apparent porosity of 94.5% and a volume density of 0.46g/cm3The compression strength is 5.83MPa, and the pore diameter is 50-120 nm.
Example 6
Adding water, a monomer, a cross-linking agent and a dispersing agent into an iron tailing raw material in a mixing tank to prepare a premixed solution according to the following proportion, and adopting a rod-type ball mill to control the ball milling ratio to be 1.5:1 and the ball milling time to be 9.5h to obtain mixed slurry; wherein the amount of monomeric acrylamide added is 5.5 wt.% of the slurry; the addition of the cross-linking agent N, N-methylene-bisacrylamide is 0.6 wt.% of the slurry; the addition amount of the ammonium polyacrylate serving as a dispersant is 2.5 wt% of the slurry, and the addition amount of the iron tailings is 50 wt% of the slurry.
Polyurethane raw materials are used as foaming agents and added into the mixed slurry, the mixture is uniformly stirred, and foaming reaction is carried out. Then adding an initiator, stirring uniformly, and injecting the mixture into a mold for curing and forming; wherein the polyurethane raw material is added in an amount of 0.5 wt.% of the slurry; the initiator ammonium persulfate was added at 1.0 wt.% of the slurry.
And (4) demolding the cured and formed material, and heating the material in a drying box until the surface of the formed material is completely dried. The heating temperature is 105 ℃, and the heating time is 3 h.
And putting the dried forming material into an electric furnace for sintering. Setting a sintering temperature rise program, starting temperature rise from normal temperature, keeping the temperature rise rate at 2.5 ℃/min, respectively setting three temperature interval points of 300 ℃, 950 ℃ and 1120 ℃, preserving heat for 2h when the temperature rises to 300 ℃, preserving heat for 3h when the temperature rises to 950 ℃, and preserving heat for 8h when the temperature rises to 1020 ℃. Naturally cooling to obtain the nano-scale porous ceramic product.
The prepared porous ceramic has the apparent porosity of 95.0 percent and the volume density of 0.61g/cm3The compression strength is 4.09MPa, and the pore diameter is 50-150 nm.
The above-mentioned embodiments are only preferred embodiments of the present invention, and do not limit the scope of the present invention. Any modification and replacement within the principle of the present invention should be included in the protection scope of the present invention.
Claims (5)
1. A method for preparing high-performance porous ceramic by using iron tailings comprises the following steps,
the first step is as follows: grading and sorting the iron tailings by using grading and sorting equipment, and sorting 95-115 meshes of tailings granules according to the condition that the contents of Al2O3 and SiO2 in the iron tailings are in a negative correlation with the strength so as to improve the content of aluminum and silicon in the sorted tailings granules;
the second step is that: adding a certain amount of water into a tailing granule raw material to form slurry, sequentially adding a monomer accounting for 2-5.5 wt.% of the slurry, a cross-linking agent accounting for 0.2-0.6 wt.% of the slurry and a dispersing agent accounting for 0.25-2.5 wt.% of the slurry under stirring to prepare a premixed liquid, performing ball milling, and performing ball milling for 6-11 hours to obtain a mixed slurry with a solid content of 30-70%;
the third step: adding a polyurethane raw material serving as a foaming agent into the mixed slurry to perform a foaming reaction; then adding an initiator, stirring uniformly, injecting the mixture into a mold, and curing and forming to obtain a foaming agent-polyurethane raw material;
the fourth step: demoulding the formed material, and heating the formed material in a drying box until the surface of the formed material is completely dried;
the fifth step: and (2) after demoulding and heating and drying the formed material, setting a sintering temperature rise program, starting temperature rise from normal temperature, keeping the temperature rise rate at 2.5 ℃/min, respectively setting three temperature interval points of 300 ℃, 950 ℃ and 1120 ℃, preserving heat for 1-2 h when the temperature rises to 300 ℃, preserving heat for 2-3 h when the temperature rises to 950 ℃, preserving heat for 3-8 h when the temperature rises to 1020 ℃, and naturally cooling to obtain the nano-scale porous ceramic product.
2. The method for preparing high performance porous ceramic according to claim 1, wherein: the monomer is acrylamide; the cross-linking agent is N, N-methylene bisacrylamide, and the dispersing agent is ammonium polyacrylate.
3. The method for preparing high performance porous ceramic according to claim 1, wherein: the foaming agent is a polyurethane raw material, and the addition amount of the foaming agent is 0.02-0.5 wt% of the slurry; the initiator is ammonium persulfate, and the addition amount of the initiator is 0.1-1.0 wt% of the slurry.
4. The method for preparing high performance porous ceramic according to claim 1, wherein: the method of the third step is as follows: putting polyether polyol into a vacuum dehydrator, performing vacuum dehydration for 3h at 110 ℃, then cooling to 65 ℃, adding toluene diisocyanate with 1.5 times of stoichiometric number, controlling the reaction temperature to be 75 ℃ and 85 ℃, wherein the reaction is exothermic reaction, reacting at 75 ℃ for a period of time until the temperature is stable, adjusting to 85 ℃, stopping heating after the reaction temperature is stable, and obtaining the foaming agent-polyurethane raw material.
5. The method for preparing high performance porous ceramic according to claim 1, wherein: the aperture of the nano-scale porous ceramic product is 50-200 nm.
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