CN114940623B - Open-cell foamed ceramic board and preparation method thereof - Google Patents

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

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CN114940623B
CN114940623B CN202210411815.3A CN202210411815A CN114940623B CN 114940623 B CN114940623 B CN 114940623B CN 202210411815 A CN202210411815 A CN 202210411815A CN 114940623 B CN114940623 B CN 114940623B
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open
temperature
foamed ceramic
foaming agent
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CN114940623A (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 board 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 talcum, 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 molybdenum tailings, shale, perlite, zinc oxide, talcum, foaming agent and additive, and grinding to obtain a product A; (2) granulating the product A; (3) Setting the powder particles obtained in the step (2), and calcining to obtain an open-cell foamed ceramic plate; the prepared open-cell foamed ceramic plate has higher water absorption performance and fire resistance.

Description

Open-cell foamed ceramic board and preparation method thereof
Technical Field
The invention belongs to the field of foamed ceramics, and relates to an open-cell foamed ceramic plate and a preparation method thereof.
Background
At present, most of the inorganic foaming plates in the industry are closed-pore structure materials such as foaming ceramic or foam glass materials and the like, contain closed pores, have lower water absorption and fire resistance limit and have weaker sound absorption capability. There are also open cell ceramic foam materials that are made by precursor impregnation and which release harmful gases during firing and cause environmental pollution.
Chinese patent application 201910365909.X discloses a method for preparing foamed ceramics. The preparation method comprises the steps of taking polishing slag, waste brick scraps, tailings and potassium feldspar as raw materials, adding a composite foaming agent and a high-temperature oxidant to obtain mixed powder, and performing ball milling, granulation, distribution and sintering; wherein the components are as follows according to parts 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 oxidizing agent. The Chinese patent application 201811552548.1 discloses an ultra-thick foaming ceramic plate and a production process thereof, and belongs to the technical field of foaming ceramics, wherein the ultra-thick foaming ceramic plate comprises raw materials, a foaming agent, a foam stabilizer and a thermal inertia modifier; wherein: the components of 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 inert modifier is at least one of high borosilicate glass, potash calcium glass, silicon dioxide, aluminum oxide 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 agents of the foaming ceramics are single in type, cannot be subjected to open-cell foaming, and can only obtain closed-cell foaming ceramics, and the water absorption rate and the fire resistance limit are low, so that it is necessary to explore a foaming ceramic plate with simple raw material sources and high water absorption rate and fire resistance limit and a preparation method thereof.
Disclosure of Invention
Aiming at the problems existing in the prior art, the invention provides an open-cell foamed ceramic plate with wide component sources, high water absorption and high fire resistance and a preparation method thereof.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
firstly, an open-cell foamed ceramic board is provided, which comprises the following components: molybdenum tailings, shale, perlite, zinc oxide, talc, foaming agents and admixtures.
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 talcum, 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 (SiO) 2 50-70 parts of Al 2 O 3 10-20 parts, 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 silicate 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 molybdenum tailings, shale, perlite, zinc oxide, talcum, foaming agent and additive, and grinding to obtain a product A;
(2) Granulating the product A;
(3) And (3) shaping and calcining the powder particles obtained in the step (2) 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 for two times, the low-temperature foaming is performed at the temperature of 600-1000 ℃, the pore diameter is 0.2-1mm, the high-temperature foaming is performed at the temperature of 1080-1140 ℃, and the pore diameter is 1-3mm.
Further, the temperature rising rate in the low-temperature foaming process is 7-10 ℃/min, and the heat preservation time is 10-20min.
Further, the heating rate in the high-temperature foaming process is 2-5 ℃/min, and the heat preservation time is 40min.
In some specific embodiments, a method for preparing an open-cell foamed ceramic board specifically includes the following steps:
(1) According to the proportion of molybdenum tailings, shale, perlite, zinc oxide, talcum, foaming agent and additive, respectively weighing and metering the above raw materials, and then putting the raw materials into a closed ball mill for wet grinding until the fineness of the slurry is less than or equal to 1.2% after 250 mesh screen residue;
(2) Pumping the slurry obtained in the step (1) into a spray granulation tower for granulation;
(3) The powder particles obtained in the step (2) are distributed into a refractory mould with required specification;
(4) Feeding the refractory mould with the powder particles distributed in the step (3) into a roller kiln for high-temperature sintering, foaming twice in the sintering process, foaming at low temperature in the temperature stage of 600-1000 ℃, heating up at 8 ℃/min, keeping the temperature for 15min, foaming at high temperature in the temperature stage of 1080-1140 ℃, heating up at 3 ℃/min, and keeping the temperature for 40min;
(5) And (3) carrying out dry cutting on the blank 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 board and the preparation method thereof, and the open-cell foamed ceramic board 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-pore foamed ceramic provided by the invention contains a large number of open and mutually communicated micropores, can better conduct heat and has stronger fire resistance.
Drawings
FIG. 1 is a process diagram of the preparation of an open-celled foamed ceramic finished board;
FIG. 2 is a microstructure diagram of example 1;
fig. 3 is a microstructure diagram of example 2.
Detailed Description
It is to 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 raw material sources are exemplary illustrations: the molybdenum tailings are tailings in Fengning local Xinyuan mining tailings pond, and the shale and the perlite are Fengning local shale and the perlite.
Example 1
Preparing an open-cell foamed ceramic plate:
(1) According to the mass ratio of 50 of molybdenum tailings, shale, perlite, zinc oxide, talcum, foaming agent and admixture: 20:10:3:3:15: mixing 0.5, and then putting into a closed ball mill for wet grinding until the screen residue of the slurry fineness of 250 meshes 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 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) The powder particles obtained in the step (2) are distributed into a refractory mould with required specification;
(4) Feeding the refractory mould with the powder particles distributed in the step (3) into a roller kiln for high-temperature sintering, foaming twice in the sintering process, foaming at low temperature in the temperature stage of 600-1000 ℃, heating up at 8 ℃/min, keeping the temperature for 15min, foaming at high temperature in the temperature stage of 1080-1140 ℃, heating up at 3 ℃/min, and keeping the temperature for 40min;
(5) And (3) carrying out dry cutting on the blank obtained in the step (4) to obtain the required open-cell foamed ceramic finished plate (the preparation process diagram is shown in figure 1).
As can be seen from FIG. 2, the open-cell foamed ceramic finished product plate of the embodiment is subjected to microscopic characterization, and the air holes of the foamed ceramic section layer are uniform, and a structure that 1 air hole structure is that 5-15 air holes with the diameter of 0.2-1mm exist on the wall of 1-3mm air hole is realized.
Example 2
Preparing an open-cell foamed ceramic plate:
(1) According to the mass ratio 66 of molybdenum tailings, shale, perlite, zinc oxide, talcum, foaming agent and admixture: 15:8:2:2:14: mixing 0.6, and then putting into a closed ball mill for wet grinding until the screen residue of the slurry fineness of 250 meshes 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 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) The powder particles obtained in the step (2) are distributed into a refractory mould with required specification;
(4) Feeding the refractory mould with the powder particles distributed in the step (3) into a roller kiln for high-temperature sintering, foaming twice in the sintering process, foaming at low temperature in the temperature stage of 600-1000 ℃, heating up at 9 ℃/min, keeping the temperature for 17min, foaming at high temperature in the temperature stage of 1080-1140 ℃, heating up at 3 ℃/min, and keeping the temperature for 40min;
(5) And (3) carrying out dry cutting on the blank obtained in the step (4) to obtain the required open-cell foamed ceramic finished plate (the preparation process diagram is shown in figure 1).
As can be seen from FIG. 3, the open-pore foamed ceramic finished product plate of the embodiment is subjected to microscopic characterization, and the air holes of the foamed ceramic section layer are uniform, and a structure that 1 air hole structure is that 5-15 air holes with the diameter of 0.2-1mm exist on the wall of 1-3mm air hole is realized.
Example 3
Preparing an open-cell foamed ceramic plate:
(1) According to the mass ratio of 65 of molybdenum tailings, shale, perlite, zinc oxide, talcum, foaming agent and admixture: 15:6:2:2:12: mixing 0.3, and then putting into a closed ball mill for wet grinding until the screen residue of the slurry fineness of 250 meshes 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) The powder particles obtained in the step (2) are distributed into a refractory mould with required specification;
(4) Feeding the refractory mould with the powder particles distributed in the step (3) into a roller kiln for high-temperature sintering, foaming twice in the sintering process, foaming at low temperature in the temperature stage of 600-1000 ℃, heating up at 8 ℃/min, keeping the temperature for 15min, foaming at high temperature in the temperature stage of 1080-1140 ℃, heating up at 3 ℃/min, and keeping the temperature for 40min;
(5) And (3) carrying out dry cutting on the blank obtained in the step (4) to obtain the required open-cell foamed ceramic finished plate (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, shale, perlite, zinc oxide, talcum, foaming agent and additive 70:10:5:1:1:10: mixing 0.6, and then putting into a closed ball mill for wet grinding until the screen residue of the slurry fineness of 250 meshes is less than or equal to 1.2%; 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) The powder particles obtained in the step (2) are distributed into a refractory mould with required specification;
(4) Feeding the refractory mould with the powder particles distributed in the step (3) into a roller kiln for high-temperature sintering, foaming twice in the sintering process, foaming at low temperature in the temperature stage of 600-1000 ℃, heating up at 10 ℃/min, keeping the temperature for 19min, foaming at high temperature in the temperature stage of 1080-1140 ℃, heating up at 3 ℃/min, and keeping the temperature for 40min;
(5) And (3) carrying out dry cutting on the blank obtained in the step (4) to obtain the required open-cell foamed ceramic finished plate (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, shale, perlite, zinc oxide, talcum, foaming agent and additive of 75:10:11:3.5:3.1:9: mixing 0.8, and then putting into a closed ball mill for wet grinding until the screen residue of the slurry fineness of 250 meshes 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 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) The powder particles obtained in the step (2) are distributed into a refractory mould with required specification;
(4) Feeding the refractory mould with the powder particles distributed in the step (3) into a roller kiln for high-temperature sintering, foaming twice in the sintering process, foaming at low temperature in the temperature stage of 600-1000 ℃, heating up at 8 ℃/min, keeping the temperature for 15min, foaming at high temperature in the temperature stage of 1080-1140 ℃, heating up at 3 ℃/min, and keeping the temperature for 40min;
(5) And (3) carrying out dry cutting on the blank obtained in the step (4) to obtain the required open-cell foamed ceramic finished plate (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 66 of molybdenum tailings, shale, perlite, zinc oxide, talcum, foaming agent and admixture: 15:8:2:2:14: mixing 0.6, and then putting into a closed ball mill for wet grinding until the screen residue of the slurry fineness of 250 meshes is less than or equal to 1.2%; 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) The powder particles obtained in the step (2) are distributed into a refractory mould with required specification;
(4) Feeding the refractory mould with the powder particles distributed in the step (3) into a roller kiln for high-temperature sintering, foaming twice in the sintering process, foaming at low temperature in the temperature stage of 600-1000 ℃, heating up at 8 ℃/min, keeping the temperature for 15min, foaming at high temperature in the temperature stage of 1080-1140 ℃, heating up at 3 ℃/min, and keeping the temperature for 40min;
(5) And (3) carrying out dry cutting on the blank obtained in the step (4) to obtain the required open-cell foamed ceramic finished plate (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 of molybdenum tailings, shale, perlite, zinc oxide, talcum, foaming agent and admixture: 15:6:2:2:12: mixing 0.3, and then putting into a closed ball mill for wet grinding until the screen residue of the slurry fineness of 250 meshes 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) The powder particles obtained in the step (2) are distributed into a refractory mould with required specification;
(4) Feeding the refractory mould with the powder particles distributed in the step (3) into a roller kiln for high-temperature sintering, foaming twice in the sintering process, foaming at low temperature in the temperature stage of 600-1000 ℃, heating up at 8 ℃/min, keeping the temperature for 15min, foaming at high temperature in the temperature stage of 1080-1140 ℃, heating up at 3 ℃/min, and keeping the temperature for 40min;
(5) And (3) carrying out dry cutting on the blank obtained in the step (4) to obtain the required open-cell foamed ceramic finished plate (the preparation process diagram is shown in figure 1).
Performance tests were carried out on the open-cell foamed ceramic finished boards prepared in examples 1 to 5 and comparative examples 1 to 3, wherein the water absorption was tested according to GB/T3810.3 (vacuum method); bulk density, compressive strength according to GB/T5486; fire resistance tests were according to GB/T9978.8-2008. The test results are shown in table 1:
TABLE 1 Performance test results
Finally, it should be noted that the above description is only for illustrating the technical solution of the present invention, and not for limiting the scope of the present invention, and that the simple modification and equivalent substitution of the technical solution of the present invention can be made by those skilled in the art without departing from the spirit and scope of the technical solution of the present invention.

Claims (8)

1. The open-cell foamed ceramic board is characterized by comprising the following components: molybdenum tailings, shale, perlite, zinc oxide, talc, foaming agents and additives; the open-cell foamed ceramic board 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 talcum, 10-15 parts of foaming agent and 0.3-0.7 part of additive; 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.
2. The open-celled foamed ceramic board according to claim 1, wherein the molybdenum tailings comprise the following chemical components in parts by weight: siO (SiO) 2 50-70 parts of Al 2 O 3 10-20 parts, K 2 O1-3 parts, na 2 O1-3。
3. The open-cell foamed ceramic board according to claim 1, wherein the additive is one or more of sodium silicate pentahydrate, sodium carbonate, gum arabic, methylcellulose, and sodium tripolyphosphate.
4. A method for producing an open-celled foamed ceramic sheet as defined in any one of claims 1 to 3, comprising the steps of:
(1) Mixing molybdenum tailings, shale, perlite, zinc oxide, talcum, foaming agent and additive, and grinding to obtain a product A;
(2) Granulating the product A;
(3) And (3) shaping and calcining the powder particles obtained in the step (2) to obtain the open-cell foamed ceramic plate.
5. The process according to claim 4, wherein the fineness of the product A in step (1) is less than 250 mesh.
6. The method according to claim 4, wherein the calcination step (3) is performed with two foaming steps, low-temperature foaming at 600-1000deg.C, pore size of 0.2-1mm, and high-temperature foaming at 1080-1140 deg.C, pore size of 1-3mm.
7. The method according to claim 6, wherein the temperature rise rate in the low-temperature foaming process is 7-10 ℃/min and the heat preservation time is 10-20min.
8. The method according to claim 6, wherein the temperature rise rate in the high-temperature foaming process is 2-5 ℃/min and the heat preservation time is 40min.
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