CN114940623A - Open-cell foamed ceramic plate and preparation method thereof - Google Patents

Open-cell foamed ceramic plate and preparation method thereof Download PDF

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CN114940623A
CN114940623A CN202210411815.3A CN202210411815A CN114940623A CN 114940623 A CN114940623 A CN 114940623A CN 202210411815 A CN202210411815 A CN 202210411815A CN 114940623 A CN114940623 A CN 114940623A
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open
foamed ceramic
temperature
foaming agent
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CN114940623B (en
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牛艳宁
窦园园
池宗鹏
孔德华
康艳蕊
杨焱鑫
张金青
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Hebei Hengzhen Building Materials Co ltd
North China Institute of Science and Technology
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Hebei Hengzhen Building Materials Co ltd
North China Institute of Science and Technology
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Abstract

The invention provides an open-cell foamed ceramic plate which comprises the following components in parts by weight: 50-70 parts of molybdenum tailings, 10-20 parts of shale, 5-10 parts of perlite, 1-3 parts of zinc oxide, 0.01-3 parts of talc, 10-15 parts of foaming agent and 0.3-0.7 part of additive; the preparation method of the open-cell foamed ceramic plate comprises the following steps: (1) mixing and grinding molybdenum tailings, shale, perlite, zinc oxide, talc, a foaming agent and an additive to obtain a product A; (2) granulating the product A; (3) shaping the powder particles obtained in the step (2), and then calcining to obtain an open-cell foamed ceramic plate; the prepared open-cell foamed ceramic board has high water absorption performance and fire resistance.

Description

Open-cell foamed ceramic plate and preparation method thereof
Technical Field
The invention belongs to the field of foamed ceramics, and relates to a perforated foamed ceramic plate and a preparation method thereof.
Background
At present, most inorganic foaming plates in the industry are closed-cell structural materials such as foaming ceramic or foam glass materials and the like, contain closed pores, and have low water absorption and fire resistance limit and weak sound absorption capacity. Some open-cell foam ceramic materials are prepared by impregnating precursors, and can release harmful gases in the firing process to pollute the environment.
Chinese patent application 201910365909.X discloses a preparation method of foamed ceramics. The preparation method comprises the steps of taking polishing slag, waste brick scraps, tailings and potash feldspar as raw materials, adding a composite foaming agent and a high-temperature oxidant to obtain mixed powder, and carrying out ball milling, granulation, material distribution and sintering; wherein the components are as follows by weight: 25-30 parts of polishing slag, 20-25 parts of waste brick scraps, 40-45 parts of tailings, 5-10 parts of potassium feldspar, 0.3-0.7 part of composite foaming agent and 0.1-0.3 part of high-temperature oxidant. Chinese patent application 201811552548.1 discloses a super-thick foamed ceramic plate and a production process thereof, belonging to the technical field of foamed ceramics, wherein the components of the super-thick foamed ceramic plate comprise a raw material, a foaming agent, a foam stabilizer and a thermal inertia modifier; wherein: the raw materials comprise 40-60 parts of fluorite tailings, 5-15 parts of potassium feldspar, 10-20 parts of green stone powder and 15-30 parts of waste porcelain powder; the foaming agent is at least one of silicon carbide, carbon powder, calcium carbonate, manganese dioxide, sodium nitrate and potassium nitrate; the foam stabilizer is at least one of borax, boric acid, zinc oxide and barium carbonate; the thermal inertia modifier is at least one of high borosilicate glass, potassium calcium glass, silicon dioxide, alumina and glass fiber powder; the mass percentage ratio of the raw materials, the foaming agent, the foam stabilizer and the thermal inertia modifier is 100: 0.5-2: 1-3: 2-10. However, the two foaming ceramic foaming agents are single in type, open-cell foaming cannot be performed, only closed-cell foamed ceramics can be obtained, and the water absorption rate and the fire resistance limit are low, so that a foamed ceramic plate with simple raw material source and high water absorption rate and fire resistance limit and a preparation method thereof need to be searched.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides the open-cell foamed ceramic plate with wide component sources, high water absorption and high fire resistance and the preparation method thereof.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
firstly, an open-cell foamed ceramic plate is provided, which comprises the following components: molybdenum tailings, shale, perlite, zinc oxide, talc, a foaming agent and an additive.
Further, the open-cell foamed ceramic plate comprises the following components in parts by weight: 50-70 parts of molybdenum tailings, 10-20 parts of shale, 5-10 parts of perlite, 1-3 parts of zinc oxide, 0.01-3 parts of talc, 10-15 parts of foaming agent and 0.3-0.7 part of additive.
Further, the molybdenum tailings comprise the following chemical components in parts by weight: SiO 2 2 50-70 parts of Al 2 O 3 10-20 parts of K 2 O1-3 parts, Na 2 O 1-3。
Further, the foaming agent comprises a low-temperature foaming agent and a high-temperature foaming agent; the low-temperature foaming agent is at least two of calcium carbonate, barium carbonate and sodium nitrate; the high-temperature foaming agent is silicon carbide; the mass ratio of the low-temperature foaming agent to the high-temperature foaming agent is 100-200: 2-5.
Further, the additive is one or more of sodium pentahydrate, industrial soda ash, gum arabic, methylcellulose and sodium tripolyphosphate.
Secondly, a preparation method of the open-cell foamed ceramic plate is provided, which comprises the following steps:
(1) mixing and grinding molybdenum tailings, shale, perlite, zinc oxide, talc, a foaming agent and an additive to obtain a product A;
(2) granulating the product A;
(3) and (3) shaping the powder particles obtained in the step (2), and then calcining to obtain the open-cell foamed ceramic plate.
Further, the fineness of the product A in the step (1) is lower than 250 meshes.
Further, in the step (3), the calcination process is performed with two foaming processes, wherein the low-temperature foaming process is performed at the temperature stage of 600-1000 ℃ and the pore diameter is 0.2-1mm, and the high-temperature foaming process is performed at the temperature stage of 1080-1140 ℃ and the pore diameter is 1-3 mm.
Further, the heating rate is 7-10 ℃/min and the heat preservation time is 10-20min in the low-temperature foaming process.
Furthermore, the heating rate is 2-5 ℃/min and the heat preservation time is 40min in the high-temperature foaming process.
In some embodiments, a method for preparing an open-cell foamed ceramic plate comprises the following steps:
(1) according to the mixture ratio of molybdenum tailings, shale, perlite, zinc oxide, talc, foaming agent and additive, the raw materials are weighed and weighed respectively and then put into a closed ball mill for wet milling until the fineness of slurry is 250 meshes and the residue is less than or equal to 1.2%;
(2) pumping the slurry obtained in the step (1) into a spray granulation tower for granulation;
(3) distributing the powder particles obtained in the step (2) into a refractory mould with required specification;
(4) sending the refractory mould distributed with the powder particles in the step (3) into a roller kiln for high-temperature sintering, carrying out foaming twice in the sintering process, carrying out low-temperature foaming in a temperature stage of 600-plus-one and 1000 ℃, wherein the heating rate is 8 ℃/min, the heat preservation time is 15min, carrying out high-temperature foaming in a temperature stage of 1080-plus-one and 1140 ℃, the heating rate is 3 ℃/min, and the heat preservation time is 40 min;
(5) and (4) carrying out dry cutting on the rough board obtained in the step (4) to obtain the required open-cell foamed ceramic finished board.
Compared with the prior art, the invention provides the open-cell foamed ceramic plate and the preparation method thereof, and the open-cell foamed ceramic plate has the following beneficial effects:
(1) the open-cell foamed ceramic provided by the invention has good water absorption, the water absorption rate is up to 300%, and the open-cell foamed ceramic can be applied to the field of sewage treatment;
(2) the open-cell foamed ceramic provided by the invention contains a large number of open mutually-communicated micropores, can better conduct heat and has stronger fire resistance.
Drawings
FIG. 1 is a diagram of a process for preparing an open-cell foamed ceramic finished plate;
FIG. 2 is a view showing a microstructure of example 1;
FIG. 3 is a microstructure diagram of example 2.
Detailed Description
It should be noted that the raw materials used in the present invention are all common commercial products, and the sources thereof are not particularly limited.
The following sources of raw materials are exemplary: the molybdenum tailings are tailings of a Fengning local Xinyuan mining industry tailings pond, and the shale and the perlite are shale and perlite in the Fengning local area.
Example 1
Preparing an open-cell foamed ceramic plate:
(1) according to the mass ratio of the molybdenum tailings, the shale, the perlite, the zinc oxide, the talc, the foaming agent and the additive to be 50: 20: 10: 3: 3: 15: 0.5, mixing and putting into a closed ball mill for wet milling until the fineness of the slurry is 250 meshes and the residue is less than or equal to 1.2 percent; wherein the foaming agent is calcium carbonate, barium carbonate and silicon carbide, and the mass ratio is 80: 70: 3, the additive is sodium silicate pentahydrate;
(2) pumping the slurry obtained in the step (1) into a spray granulation tower for granulation;
(3) distributing the powder particles obtained in the step (2) into a refractory mould with required specification;
(4) sending the refractory mould distributed with the powder particles in the step (3) into a roller kiln for high-temperature sintering, foaming twice in the sintering process, foaming at low temperature in the stage of 600-plus-one temperature of 1000 ℃, wherein the temperature rise rate is 8 ℃/min, the heat preservation time is 15min, foaming at high temperature in the stage of 1080-plus-one temperature of 1140 ℃, the temperature rise rate is 3 ℃/min, and the heat preservation time is 40 min;
(5) and (3) carrying out dry cutting on the rough board obtained in the step (4) to obtain the required open-cell foamed ceramic finished board (the preparation process diagram is shown in figure 1).
The open-cell foamed ceramic product plate of the present embodiment is subjected to microscopic characterization, and as can be seen from fig. 2, the pores of the cross-sectional layer of the foamed ceramic are uniform, and a structure in which 5 to 15 pores of 0.2 to 1mm exist on the pore wall of 1 to 3mm in the pore-shaped structure is realized.
Example 2
Preparing an open-cell foamed ceramic plate:
(1) according to the mass ratio of the molybdenum tailings, the shale, the perlite, the zinc oxide, the talc, the foaming agent and the additive, 66: 15: 8: 2: 2: 14: 0.6, mixing, putting into a closed ball mill, and wet milling until the fineness of the slurry is 250 meshes and the residue is less than or equal to 1.2 percent; wherein the foaming agent is calcium carbonate, barium carbonate and silicon carbide, and the mass ratio is 90: 80: 4, the additive is sodium silicate pentahydrate;
(2) pumping the slurry obtained in the step (1) into a spray granulation tower for granulation;
(3) distributing the powder particles obtained in the step (2) into a refractory mould with required specification;
(4) sending the refractory mould distributed with the powder particles in the step (3) into a roller kiln for high-temperature sintering, carrying out foaming twice in the sintering process, carrying out low-temperature foaming in a temperature stage of 600-plus-one and 1000 ℃, wherein the heating rate is 9 ℃/min, the heat preservation time is 17min, carrying out high-temperature foaming in a temperature stage of 1080-plus-one and 1140 ℃, the heating rate is 3 ℃/min, and the heat preservation time is 40 min;
(5) and (3) carrying out dry cutting on the rough board obtained in the step (4) to obtain the required open-cell foamed ceramic finished board (the preparation process diagram is shown in figure 1).
The open-cell foamed ceramic product plate of the present embodiment is subjected to microscopic characterization, and as can be seen from fig. 3, the pores of the foamed ceramic cross-section layer are uniform, and a structure in which 5 to 15 pores of 0.2 to 1mm exist on the pore wall of 1 to 3mm in a pore-shaped structure is realized.
Example 3
Preparing an open-cell foamed ceramic plate:
(1) according to the mass ratio of 65: 15: 6: 2: 2: 12: 0.3, mixing, putting into a closed ball mill, and wet-milling until the fineness of the slurry is 250 meshes and the residue is less than or equal to 1.2%; wherein the foaming agent is calcium carbonate, sodium nitrate and silicon carbide, and the mass ratio is 100: 90: 2.5, the additive is gum arabic;
(2) pumping the slurry obtained in the step (1) into a spray granulation tower for granulation;
(3) distributing the powder particles obtained in the step (2) into a refractory mould with required specification;
(4) sending the refractory mould distributed with the powder particles in the step (3) into a roller kiln for high-temperature sintering, carrying out foaming twice in the sintering process, carrying out low-temperature foaming in a temperature stage of 600-plus-one and 1000 ℃, wherein the heating rate is 8 ℃/min, the heat preservation time is 15min, carrying out high-temperature foaming in a temperature stage of 1080-plus-one and 1140 ℃, the heating rate is 3 ℃/min, and the heat preservation time is 40 min;
(5) and (3) carrying out dry cutting on the rough board obtained in the step (4) to obtain the required open-cell foamed ceramic finished board (the preparation process diagram is shown in figure 1).
Example 4
Preparing an open-cell foamed ceramic plate:
(1) according to the mass ratio of the molybdenum tailings, the shale, the perlite, the zinc oxide, the talc, the foaming agent and the additive of 70: 10: 5: 1: 1: 10: 0.6 percent of the mixture is put into a closed ball mill for wet milling until the fineness of the slurry is 250 meshes and the residue is less than or equal to 1.2 percent; wherein the foaming agent is barium carbonate, sodium nitrate and silicon carbide, and the mass ratio is 65: 40: 4.5, the additive is methyl cellulose;
(2) pumping the slurry obtained in the step (1) into a spray granulation tower for granulation;
(3) distributing the powder particles obtained in the step (2) into a refractory mould with required specification;
(4) sending the refractory mould distributed with the powder particles in the step (3) into a roller kiln for high-temperature sintering, carrying out foaming twice in the sintering process, carrying out low-temperature foaming in the temperature stage of 600-plus-one temperature of 1000 ℃, wherein the heating rate is 10 ℃/min, the heat preservation time is 19min, carrying out high-temperature foaming in the temperature stage of 1080-plus-one 1140 ℃, the heating rate is 3 ℃/min, and the heat preservation time is 40 min;
(5) and (3) carrying out dry cutting on the rough board obtained in the step (4) to obtain the required open-cell foamed ceramic finished board (the preparation process diagram is shown in figure 1).
Comparative example 1
Preparing an open-cell foamed ceramic plate:
(1) according to the mass ratio of the molybdenum tailings, the shale, the perlite, the zinc oxide, the talc, the foaming agent and the additive of 75: 10: 11: 3.5: 3.1: 9: 0.8, putting the mixture into a closed ball mill for wet milling until the fineness of the slurry is 250 meshes and the residue is less than or equal to 1.2 percent; wherein the foaming agent is calcium carbonate, barium carbonate and silicon carbide, and the mass ratio is 90: 80: 4, the additive is sodium pentahydrate;
(2) pumping the slurry obtained in the step (1) into a spray granulation tower for granulation;
(3) distributing the powder particles obtained in the step (2) into a refractory mould with required specification;
(4) sending the refractory mould distributed with the powder particles in the step (3) into a roller kiln for high-temperature sintering, carrying out foaming twice in the sintering process, carrying out low-temperature foaming in a temperature stage of 600-plus-one and 1000 ℃, wherein the heating rate is 8 ℃/min, the heat preservation time is 15min, carrying out high-temperature foaming in a temperature stage of 1080-plus-one and 1140 ℃, the heating rate is 3 ℃/min, and the heat preservation time is 40 min;
(5) and (3) carrying out dry cutting on the rough board obtained in the step (4) to obtain the required open-cell foamed ceramic finished board (the preparation process diagram is shown in figure 1).
Comparative example 2
Preparing an open-cell foamed ceramic plate:
(1) according to the mass ratio of the molybdenum tailings, the shale, the perlite, the zinc oxide, the talc, the foaming agent and the additive, 66: 15: 8: 2: 2: 14: 0.6 percent of the mixture is put into a closed ball mill for wet milling until the fineness of the slurry is 250 meshes and the residue is less than or equal to 1.2 percent; wherein the foaming agent is calcium carbonate and silicon carbide, and the mass ratio of the calcium carbonate to the silicon carbide is 150: 5, the additive is sodium silicate pentahydrate;
(2) pumping the slurry obtained in the step (1) into a spray granulation tower for granulation;
(3) distributing the powder particles obtained in the step (2) into a refractory mould with required specification;
(4) sending the refractory mould distributed with the powder particles in the step (3) into a roller kiln for high-temperature sintering, carrying out foaming twice in the sintering process, carrying out low-temperature foaming in a temperature stage of 600-plus-one and 1000 ℃, wherein the heating rate is 8 ℃/min, the heat preservation time is 15min, carrying out high-temperature foaming in a temperature stage of 1080-plus-one and 1140 ℃, the heating rate is 3 ℃/min, and the heat preservation time is 40 min;
(5) and (3) carrying out dry cutting on the rough board obtained in the step (4) to obtain the required open-cell foamed ceramic finished board (the preparation process diagram is shown in figure 1).
Comparative example 3
Preparing an open-cell foamed ceramic plate:
(1) according to the mass ratio of 65: 15: 6: 2: 2: 12: 0.3, mixing, putting into a closed ball mill, and wet-milling until the fineness of the slurry is 250 meshes and the residue is less than or equal to 1.2%; wherein the foaming agent is calcium carbonate, barium carbonate and silicon carbide, and the mass ratio is 120: 90: 1.5, the additive is sodium silicate pentahydrate;
(2) pumping the slurry obtained in the step (1) into a spray granulation tower for granulation;
(3) distributing the powder particles obtained in the step (2) into a refractory mould with required specification;
(4) sending the refractory mould distributed with the powder particles in the step (3) into a roller kiln for high-temperature sintering, carrying out foaming twice in the sintering process, carrying out low-temperature foaming in a temperature stage of 600-plus-one and 1000 ℃, wherein the heating rate is 8 ℃/min, the heat preservation time is 15min, carrying out high-temperature foaming in a temperature stage of 1080-plus-one and 1140 ℃, the heating rate is 3 ℃/min, and the heat preservation time is 40 min;
(5) and (3) carrying out dry cutting on the rough board obtained in the step (4) to obtain the required open-cell foamed ceramic finished board (the preparation process diagram is shown in figure 1).
The open-cell foamed ceramic finished plates prepared in examples 1 to 5 and comparative examples 1 to 3 were subjected to a performance test, wherein the water absorption was measured according to GB/T3810.3 (vacuum method); the test of the volume density and the compressive strength is carried out according to GB/T5486; the fire resistance was tested according to GB/T9978.8-2008. The test results are shown in table 1:
table 1 results of performance testing
Figure BDA0003604039730000071
Figure BDA0003604039730000081
Finally, it should be noted that the above-mentioned contents are only used for illustrating the technical solutions of the present invention, and do not limit the protection scope of the present invention, and those skilled in the art can make simple modifications or equivalent substitutions on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.

Claims (10)

1. An open-cell foamed ceramic plate is characterized by comprising the following components: molybdenum tailings, shale, perlite, zinc oxide, talc, a foaming agent and an additive.
2. The open-cell foamed ceramic panel according to claim 1, comprising the following components in parts by weight: 50-70 parts of molybdenum tailings, 10-20 parts of shale, 5-10 parts of perlite, 1-3 parts of zinc oxide, 0.01-3 parts of talc, 10-15 parts of foaming agent and 0.3-0.7 part of additive.
3. The open-cell foamed ceramic panel according to any one of claims 1 to 2, wherein the molybdenum tailings comprise the following chemical components in parts by weight: SiO 2 2 50-70 parts of Al 2 O 3 10-20 parts of K 2 O1-3 parts, Na 2 O 1-3。
4. The open-cell foamed ceramic panel according to any one of claims 1-2, wherein said foaming agent comprises a low temperature foaming agent and a high temperature foaming agent; the low-temperature foaming agent is at least two of calcium carbonate, barium carbonate and sodium nitrate; the high-temperature foaming agent is silicon carbide; the mass ratio of the low-temperature foaming agent to the high-temperature foaming agent is 100-200: 2-5.
5. The open-cell foamed ceramic panel according to any one of claims 1 to 2, wherein the additive is one or more of sodium pentahydrate, industrial soda ash, gum arabic, methylcellulose and sodium tripolyphosphate.
6. The method for preparing an open-cell foamed ceramic sheet according to any one of claims 1 to 5, comprising the steps of:
(1) mixing and grinding molybdenum tailings, shale, perlite, zinc oxide, talc, a foaming agent and an additive to obtain a product A;
(2) granulating the product A;
(3) and (3) shaping the powder particles obtained in the step (2), and then calcining to obtain the open-cell foamed ceramic plate.
7. The process according to claim 6, wherein the fineness of the product A in the step (1) is less than 250 mesh.
8. The method as claimed in claim 6, wherein the step (3) comprises foaming twice, wherein the foaming is performed at a temperature of 600-1000 ℃ and a pore size of 0.2-1mm, and the foaming is performed at a temperature of 1080-1140 ℃ and a pore size of 1-3 mm.
9. The preparation method of claim 8, wherein the heating rate is 7-10 ℃/min and the holding time is 10-20min in the low-temperature foaming process.
10. The preparation method according to claim 8, wherein the temperature rise rate in the high-temperature foaming process is 2-5 ℃/min, and the holding time is 40 min.
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