CN110981457A - Lightweight porous mullite ceramic and direct-writing 3D printing preparation method thereof - Google Patents
Lightweight porous mullite ceramic and direct-writing 3D printing preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field related to preparation of inorganic nonmetal ceramics, and discloses a light porous mullite ceramic and a direct-writing 3D printing preparation method thereof, wherein the method comprises the following steps: (1) mixing and stirring kaolin powder and pore-forming agent powder to obtain uniformly mixed powder, adding a plasticizer and a solvent into the mixed powder, stirring to obtain a ceramic paste, and degassing the ceramic paste; (2) and (3) printing a porous ceramic blank (3) by using the ceramic paste as a raw material and adopting a direct-writing 3D printer to dry and sinter the porous ceramic blank so as to obtain the light porous mullite ceramic with a specific shape and structure. The invention has the advantages of lower cost, higher forming speed and simple preparation process, is favorable for solving the problem of recycling the waste coal-series kaolin, and has better application prospect in the fields of chemical industry and the like.
Description
Technical Field
The invention belongs to the technical field related to preparation of inorganic nonmetal ceramics, and particularly relates to a light porous mullite ceramic and a direct-writing 3D printing preparation method thereof.
Background
Coal-based kaolin, also known as coal gangue, is a byproduct of coal mining, and with the high-speed development of the coal industry, the accumulation of coal-based kaolin waste has become a serious environmental problem. The kaolin is accumulated in a large amount, so that the kaolin can occupy agricultural industrial land, and can generate dust and harmful gas, pollute air and water resources and seriously harm human health; metal ions and soluble salts decomposed from kaolin also cause soil acidification and groundwater contamination. However, the recycling rate of the coal-series kaolin is low and the recycling economic benefit is poor at present, so that the reasonable utilization of the waste coal-series kaolin is an urgent need in the industrial aspect.
Kaolin belongs to aluminosilicate, and its main chemical component is Al2O3And SiO2The method can be used for preparing mullite ceramic with high fire resistance, strong pressure resistance and high chemical stability. The porous mullite ceramic can be used in the fields of catalysis, filtration, heat insulation and the like due to the advantages of higher specific surface area, high corrosion resistance, low thermal expansion coefficient and the like. The kaolin powder can be used as an important raw material of mullite ceramic, and the porous mullite ceramic with a complex structure is prepared by combining a proper forming process, so that the treatment problem of coal-series kaolin is solved, the pollution to the environment is reduced, the reprocessing additional value of the coal-series kaolin is improved, and the requirement is provided for industrial production application.
At present, the porous mullite ceramic prepared by the traditional method has some problems, such as difficult formation of complex structures and difficult realization of the cooperative regulation and control of macroscopic microstructures in the traditional process. Accordingly, there is a technical need in the art to develop a light porous mullite ceramic with good applicability and a direct-writing 3D printing preparation method thereof.
Disclosure of Invention
Aiming at the defects or improvement requirements of the prior art, the invention provides a light porous mullite ceramic and a direct-writing 3D printing preparation method thereof, which are based on the preparation characteristics of the existing mullite ceramic, and researches and designs the light porous mullite ceramic with controllable macroscopic microstructure and low cost and the direct-writing 3D printing preparation method thereof. The method adopts kaolin as a material and adopts a direct-writing forming technology, has the advantages of low material consumption cost, low production cost compared with other printing modes, high forming speed, simple preparation process and the like, is favorable for solving the recycling problem of the waste coal-series kaolin, and has better application prospect in the fields of chemical industry and the like.
In order to achieve the above object, according to one aspect of the present invention, a direct-writing 3D printing preparation method of a lightweight porous mullite ceramic is provided, where the direct-writing 3D printing preparation method mainly includes the following steps:
(1) mixing and stirring kaolin powder and pore-forming agent powder to obtain uniformly mixed powder, adding a plasticizer and a solvent into the mixed powder, stirring to obtain a ceramic paste, and degassing the ceramic paste;
(2) printing a porous ceramic blank by using the ceramic paste as a raw material and adopting a direct-writing 3D printer;
(3) and drying and sintering the porous ceramic blank to obtain the light porous mullite ceramic with a specific shape and structure.
Further, the pore-forming agent is one or more of polymethyl methacrylate, polystyrene, polyethylene, polypropylene, calcium carbonate and calcium sulfate.
Further, the plasticizer is one or more of bentonite, cellulose, polyvinyl alcohol, polymethyl methacrylate, high molecular weight polyethylene glycol, polyacrylamide and sorbitol.
Further, the mass percentage of the kaolin powder in the porous ceramic body is 30-50%; the mass of the pore-forming agent accounts for 30-50% of the mass of the porous ceramic blank; the mass percentage of the plasticizer in the porous ceramic body is 1-2%.
Further, the sintering temperature adopted in the step (3) is 1400-1600 ℃, and the heat preservation time is 1-2 h; the temperature rise rate is 5-10 ℃/min.
Further, the sintering temperature adopted in the step (3) is 1400 ℃, the heat preservation time is 2h, and the heating rate is 5 ℃/min.
Further, the solvent is at least one of water, glycerin, low molecular weight polyethylene glycol and liquid paraffin.
According to another aspect of the invention, the lightweight porous mullite ceramic is prepared by adopting the direct-writing 3D printing preparation method of the lightweight porous mullite ceramic.
In general, compared with the prior art, the light porous mullite ceramic and the direct-writing 3D printing preparation method thereof provided by the invention have the following beneficial effects:
1. the preparation method adopts kaolin as a material and adopts a direct-writing forming technology, has the advantages of low material consumption cost, low production cost relative to other printing modes, high forming speed, simple preparation process and the like, is favorable for solving the recycling problem of the waste coal-series kaolin, and has better application prospect in the fields of chemical industry and the like.
2. The preparation method realizes the cooperative regulation and control of the microscopic and macroscopic pore channel structure of the porous mullite ceramic by adjusting the mass ratio of kaolin to the pore-forming agent in the raw materials and combining direct-writing 3D printing.
3. The gas generated by the organic matter added in the preparation process during pyrolysis is easy to discharge from the porous structure, and the prepared sample can be prevented from deformation and cracking, so that the invention does not need to arrange a glue discharging procedure, can effectively shorten the preparation period, simplifies the preparation process and reduces the preparation cost.
4. The invention adopts the coal-series kaolin which is an industrial waste as a raw material, has wide sources, adopts the preparation method of direct-writing 3D printing, has simple printing equipment, reduces the cost, is simple and easy to implement, and is suitable for large-scale production.
Drawings
FIG. 1 is a schematic flow chart of a direct-writing 3D printing preparation method of the lightweight porous mullite ceramic provided by the invention;
fig. 2 is a micro-topography of the lightweight porous mullite ceramic prepared by the direct-writing 3D printing preparation method of the lightweight porous mullite ceramic in fig. 1, wherein (a) and (b) are respectively a low-power micro-topography and a high-power micro-topography of the lightweight porous mullite ceramic.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
Referring to fig. 1 and fig. 2, the direct-writing 3D printing preparation method of the lightweight porous mullite ceramic provided by the present invention mainly includes the following steps:
step one, mixing and stirring kaolin powder and pore-forming agent powder to obtain uniformly mixed powder, adding a plasticizer and a solvent into the mixed powder, stirring to obtain a ceramic paste, and degassing the ceramic paste.
Specifically, the kaolin powder and the pore former powder are mixed and stirred, so that the kaolin powder and the pore former powder are uniformly mixed to obtain mixed powder. Then, a plasticizer and a solvent are added to the mixed powder and stirred so that the plasticizer and the solvent are uniformly distributed in the mixed powder, thereby preparing a ceramic paste having high plasticity. And then, the prepared ceramic paste is put into a centrifuge for degassing, and the ceramic paste for printing can be obtained by vacuum or semi-vacuum degassing.
In this embodiment, the pore-forming agent is one or more of polymethyl methacrylate, polystyrene, polyethylene, polypropylene, calcium carbonate, and calcium sulfate; the plasticizer is one or more of bentonite, cellulose, polyvinyl alcohol, polymethyl methacrylate, high molecular weight polyethylene glycol, polyacrylamide and sorbitol; the solvent is at least one of water, glycerol, low molecular weight polyethylene glycol and liquid paraffin.
And secondly, printing a porous ceramic blank by using the ceramic paste as a raw material and adopting a direct-writing 3D printer.
In the embodiment, the mass of the kaolin powder accounts for 30-50% of the mass of the porous ceramic body; the mass of the pore-forming agent accounts for 30-50% of the mass of the porous ceramic blank; the mass of the plasticizer accounts for 1-2% of the mass of the porous ceramic body; the balance of solvent, and the sum of the mass percentages of the components is 100 percent.
And thirdly, drying and sintering the porous ceramic blank to obtain the light porous mullite ceramic with a specific shape and structure.
In the embodiment, the sintering temperature is 1400-1600 ℃, and the heat preservation time is 1-2 h; the temperature rise rate is 5-10 ℃/min.
The invention also provides the lightweight porous mullite ceramic prepared by the direct-writing 3D printing preparation method of the lightweight porous mullite ceramic.
The invention is described in further detail below with reference to several specific examples.
Example 1
The direct-writing 3D printing preparation method of the light porous mullite ceramic provided by the embodiment 1 of the invention mainly comprises the following steps: firstly, mixing 15g of kaolin powder, 6g of calcium carbonate, 0.291g of bentonite powder and 9g of 1 wt% cellulose solution to prepare a ceramic paste with the solid content of 70 wt%, printing a porous ceramic blank by a direct-writing 3D printer after vacuum degassing, sintering the fully dried ceramic blank at 1400 ℃, keeping the temperature for 2 hours, and increasing the temperature at the rate of 5 ℃/min to prepare the kaolin ceramic sintered part with a complex shape.
Example 2
The direct-writing 3D printing preparation method of the lightweight porous mullite ceramic provided by the embodiment 2 of the invention mainly comprises the following steps: ball-milling and mixing 12g of kaolin powder, 9g of polymethyl methacrylate, 0.45g of high molecular weight polyethylene glycol and 11.55g of liquid paraffin to prepare a ceramic paste with the solid content of 70 wt%, printing the ceramic paste into a porous ceramic blank by a direct-writing 3D printer after vacuum degassing, and sintering the fully dried porous ceramic blank at the temperature of 1500 ℃, wherein the heat preservation time is 1.5h, and the temperature rise rate is 7 ℃/min, so as to prepare the kaolin ceramic sintered piece with a complex shape.
Example 3
The direct-writing 3D printing preparation method of the lightweight porous mullite ceramic provided by the embodiment 3 of the invention mainly comprises the following steps: ball-milling and mixing 9g of kaolin powder, 12g of calcium sulfate, 0.6g of high molecular weight polyethylene glycol and 11.4g of glycerol to prepare ceramic slurry with the solid phase content of 70 wt%, degassing in vacuum, printing the ceramic slurry into a porous ceramic blank by a direct-writing 3D printer, and sintering the fully dried porous ceramic blank at 1600 ℃, wherein the heat preservation time is 1h, and the temperature rise rate is 10 ℃/min to prepare the kaolin ceramic sintered part with a complex shape.
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the present invention, and is not intended to limit the invention, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (8)
1. A direct-writing 3D printing preparation method of light porous mullite ceramic is characterized by comprising the following steps:
(1) mixing and stirring kaolin powder and pore-forming agent powder to obtain uniformly mixed powder, adding a plasticizer and a solvent into the mixed powder, stirring to obtain a ceramic paste, and degassing the ceramic paste;
(2) printing a porous ceramic blank by using the ceramic paste as a raw material and adopting a direct-writing 3D printer;
(3) and drying and sintering the porous ceramic blank to obtain the light porous mullite ceramic with a specific shape and structure.
2. The direct-write 3D printing preparation method of the lightweight porous mullite ceramic of claim 1 wherein: the pore-forming agent is one or more of polymethyl methacrylate, polystyrene, polyethylene, polypropylene, calcium carbonate and calcium sulfate.
3. The direct-write 3D printing preparation method of the lightweight porous mullite ceramic of claim 1 wherein: the plasticizer is one or more of bentonite, cellulose, polyvinyl alcohol, polymethyl methacrylate, high molecular weight polyethylene glycol, polyacrylamide and sorbitol.
4. The direct-write 3D printing preparation method of the lightweight porous mullite ceramic of claim 1 wherein: the mass of the kaolin powder accounts for 30-50% of the mass of the porous ceramic body; the mass of the pore-forming agent accounts for 30-50% of the mass of the porous ceramic blank; the mass percentage of the plasticizer in the porous ceramic body is 1-2%.
5. The method for preparing the lightweight porous mullite ceramic according to any one of claims 1 to 4 by direct-write 3D printing, wherein: the sintering temperature adopted in the step (3) is 1400-1600 ℃, and the heat preservation time is 1-2 h; the temperature rise rate is 5-10 ℃/min.
6. The direct-write 3D printing preparation method of the lightweight porous mullite ceramic of claim 5 wherein: the sintering temperature adopted in the step (3) is 1400 ℃, the heat preservation time is 2h, and the heating rate is 5 ℃/min.
7. The method for preparing the lightweight porous mullite ceramic according to any one of claims 1 to 4 by direct-write 3D printing, wherein: the solvent is at least one of water, glycerol, low molecular weight polyethylene glycol and liquid paraffin.
8. A lightweight porous mullite ceramic characterized by: the lightweight porous mullite ceramic is prepared by the direct-writing 3D printing preparation method of the lightweight porous mullite ceramic according to any one of claims 1 to 7.
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Cited By (10)
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|---|---|---|---|---|
| CN111534796A (en) * | 2020-04-17 | 2020-08-14 | 哈尔滨工业大学 | Nano mullite powder for plasma physical vapor deposition and preparation method thereof |
| CN111943690A (en) * | 2020-08-17 | 2020-11-17 | 山西高速公路工程检测有限公司 | Mullite mixed powder, preparation method thereof and application thereof in 3D printing |
| CN112321318A (en) * | 2020-10-20 | 2021-02-05 | 上海航翼高新技术发展研究院有限公司 | Polymer precursor porous magnetic ceramic system based on 3D printing technology and preparation method thereof |
| CN112341153A (en) * | 2020-10-20 | 2021-02-09 | 上海航翼高新技术发展研究院有限公司 | Waste porous magnetic ceramic system based on 3D printing technology and preparation method thereof |
| CN112620647A (en) * | 2020-12-15 | 2021-04-09 | 华中科技大学 | High-strength part 3D printing method and device for lunar environment |
| CN113275590A (en) * | 2021-04-27 | 2021-08-20 | 江苏大学 | Method for preparing component with through cavity by direct-writing printing and pressure sintering |
| CN113912414A (en) * | 2021-10-28 | 2022-01-11 | 韶关学院 | Method for preparing mullite porous heat-insulating material by using coal gangue |
| CN115745583A (en) * | 2022-12-05 | 2023-03-07 | 中国人民解放军海军工程大学 | Hierarchical porous ceramic material with skeleton filled with hollow microspheres of waste fly ash formed by 3D printing and preparation method of hierarchical porous ceramic material |
| CN115745404A (en) * | 2022-11-28 | 2023-03-07 | 浙江大学温州研究院 | High-solid-content glaze suitable for direct-writing 3D printing and preparation method thereof |
| CN115745570A (en) * | 2022-12-09 | 2023-03-07 | 中国人民解放军海军工程大学 | Porous ceramic with gradient pore structure framework and 3D printing forming method thereof |
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