WO2024078182A1 - 一种高透气性陶瓷纤维过滤管的制备方法 - Google Patents
一种高透气性陶瓷纤维过滤管的制备方法 Download PDFInfo
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- WO2024078182A1 WO2024078182A1 PCT/CN2023/116375 CN2023116375W WO2024078182A1 WO 2024078182 A1 WO2024078182 A1 WO 2024078182A1 CN 2023116375 W CN2023116375 W CN 2023116375W WO 2024078182 A1 WO2024078182 A1 WO 2024078182A1
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- ceramic fiber
- fiber filter
- filter tube
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- silica sol
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- 239000000835 fiber Substances 0.000 title claims abstract description 108
- 239000000919 ceramic Substances 0.000 title claims abstract description 77
- 230000035699 permeability Effects 0.000 title abstract description 18
- 238000002360 preparation method Methods 0.000 title abstract description 5
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910052863 mullite Inorganic materials 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 25
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000003365 glass fiber Substances 0.000 claims abstract description 19
- 230000008569 process Effects 0.000 claims abstract description 13
- 238000003825 pressing Methods 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 25
- 238000003756 stirring Methods 0.000 claims description 12
- 238000000465 moulding Methods 0.000 claims description 9
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 8
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 8
- 238000001354 calcination Methods 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 238000009413 insulation Methods 0.000 claims 1
- 238000005245 sintering Methods 0.000 abstract description 18
- 239000012528 membrane Substances 0.000 abstract description 11
- 238000004108 freeze drying Methods 0.000 abstract description 5
- 239000002105 nanoparticle Substances 0.000 abstract description 2
- 230000005012 migration Effects 0.000 abstract 1
- 238000013508 migration Methods 0.000 abstract 1
- 239000011148 porous material Substances 0.000 description 13
- 239000006185 dispersion Substances 0.000 description 10
- 239000000243 solution Substances 0.000 description 9
- 238000001878 scanning electron micrograph Methods 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 239000002002 slurry Substances 0.000 description 4
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 3
- 229910010271 silicon carbide Inorganic materials 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- CFOAUMXQOCBWNJ-UHFFFAOYSA-N [B].[Si] Chemical compound [B].[Si] CFOAUMXQOCBWNJ-UHFFFAOYSA-N 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000002657 fibrous material Substances 0.000 description 2
- 238000001746 injection moulding Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- YKTSYUJCYHOUJP-UHFFFAOYSA-N [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] Chemical compound [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] YKTSYUJCYHOUJP-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000012700 ceramic precursor Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000009766 low-temperature sintering Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 229920003257 polycarbosilane Polymers 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 239000011863 silicon-based powder Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000003828 vacuum filtration Methods 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/71—Ceramic products containing macroscopic reinforcing agents
- C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
- C04B35/80—Fibres, filaments, whiskers, platelets, or the like
- C04B35/82—Asbestos; Glass; Fused silica
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0039—Inorganic membrane manufacture
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/04—Tubular membranes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/14—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silica
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- C—CHEMISTRY; METALLURGY
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/71—Ceramic products containing macroscopic reinforcing agents
- C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
- C04B35/80—Fibres, filaments, whiskers, platelets, or the like
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/0051—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof characterised by the pore size, pore shape or kind of porosity
- C04B38/0054—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof characterised by the pore size, pore shape or kind of porosity the pores being microsized or nanosized
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/52—Constituents or additives characterised by their shapes
- C04B2235/5208—Fibers
- C04B2235/5216—Inorganic
- C04B2235/522—Oxidic
- C04B2235/5228—Silica and alumina, including aluminosilicates, e.g. mullite
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6567—Treatment time
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
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- Y02A50/2351—Atmospheric particulate matter [PM], e.g. carbon smoke microparticles, smog, aerosol particles, dust
Definitions
- the present invention relates to a method for preparing a highly air-permeable ceramic fiber filter tube, which belongs to the field of membrane material preparation.
- Ceramic fiber membrane is a type of ceramic filter material prepared with high-temperature resistant ceramic fibers, such as alumina fiber, aluminum silicate fiber, mullite fiber, etc. as aggregates.
- the three-dimensional network-like porous structure formed by mutual bridging between ceramic fibers gives the ceramic fiber membrane the characteristics of high porosity, good thermal stability, and high gas permeability, making it one of the most promising ceramic membrane materials.
- Traditional ceramic fiber filter tubes are usually prepared by a wet vacuum filtration molding process. However, due to the suction effect of negative pressure, it is easy to cause unevenness inside the fiber porous ceramic material, which has an adverse effect on the air permeability of the ceramic fiber membrane. Therefore, it is very important to improve the preparation process of ceramic fiber filter tubes to prepare highly permeable ceramic fiber filter tubes.
- Mold molding technology (including dry pressing, gel injection molding, filter pressing, etc.) is simple to operate and highly efficient, and has broad application prospects in the field of ceramic fiber membrane preparation. Although the strength of the ceramic fiber filter material prepared by dry pressing technology is significantly improved, due to the high molding pressure, the porous fiber skeleton structure will be compacted, resulting in a large loss of gas permeability.
- Xu et al. [Ceramics International, 2017, 43(1): 228-233] used gel injection molding to add mullite fiber and sintering aid to a tert-butyl alcohol-based gel premix solution. Under the action of the initiator, the organic monomer polymerized to solidify the slurry, thereby obtaining a high-strength green body.
- Liquid phase sintering aids have the characteristics of small particle size and good dispersibility. They can be evenly wrapped on the aggregate surface and intersections, which helps to promote the low-temperature sintering process. Sols and ceramic precursor solutions can be used to assist the sintering process of porous ceramics. Hai et al. [Refractories and Industrial Ceramics, 2012, 53: 157-161] used polycarbosilane as the precursor solution. After drying, they sintered at 1000 °C without adding any sintering aids to obtain pure silicon carbide porous ceramics with an average porosity of 33.4%, a fracture strength of ⁇ 16 MPa, and an average pore size of 2.275 ⁇ m.
- the neck connection strength formed by a small amount of inorganic sol at the fiber connection point is low, which is not conducive to the long-term use of ceramic fiber membranes.
- Low melting point solid sintering aids can effectively enhance the mechanical properties of porous materials.
- Xu et al. [Ceramics International, 2017, 43(1): 228-233] investigated the effects of different solid sintering aids (silicon powder, silicon dioxide powder, and boron-silicon mixture) on the mechanical properties of prepared fiber porous ceramic materials. The results showed that the porous ceramic fiber material prepared with boron-silicon mixture as a sintering aid had the highest compressive strength of about 2.08 MPa at 1500 °C.
- the purpose of the present invention is to improve the defects of the prior art and to propose a method of preparing ceramic fiber filter tubes by combining two sintering aids with different properties, solid and liquid, to replace the common liquid sintering aids.
- the use of sintering aids with different properties solves the problem of weak neck connection at the fiber connection point.
- the green body is treated with freeze-drying technology to effectively improve the uniformity of the ceramic fiber tube and prepare a ceramic fiber filter tube with high air permeability.
- the technical solution of the present invention is: a method for preparing a highly air-permeable ceramic fiber filter tube, and the specific steps are as follows: A. First, a certain mass fraction of silica sol is mixed with water in a certain volume ratio and fully stirred, and then mullite short fiber and glass fiber are added, wherein the mass ratio of silica sol, mullite short fiber and glass fiber is (30-45): (1.5-9): 1, an organic molding aid is added and stirred for a certain time, and then quickly injected into a filter press mold after stirring for a certain time, and pressure is slowly applied until water is filtered out to obtain a ceramic fiber filter tube green body; B.
- the demolded green body is placed in a refrigerator to freeze for 12-24 hours, and then placed in a -60 °C to -20 °C environment to dry for 12-24 hours, and then subjected to a calcination process to obtain a ceramic fiber filter tube.
- the mass fraction of the silica sol is 20 wt%-40 wt%, and the volume ratio of the silica sol to water is 1:(1.5-9); the aspect ratio of the mullite short fiber is 50-200; the organic molding aid is a polyvinyl alcohol (PVA) solution with a concentration of 8 wt%-12 wt%, and the added amount is 60%-80% of the total mass of the mullite short fiber and the glass fiber.
- PVA polyvinyl alcohol
- the stirring time of the membrane-making liquid is 3-10 min.
- the preferred pressure in the filter pressing process is 2-4 MPa.
- the preferred calcination process is: calcining the green body at 800-1400 °C, controlling the heating rate and cooling rate at 0.5-3 °C/min, and the holding time is 1-3 h.
- the ceramic fiber filter tube prepared by the invention has an average pore size of 34.1-35.2 ⁇ m, a porosity of 74-75.2%, a gas permeability of 642-787 m 3 ⁇ m -2 ⁇ h -1 ⁇ kPa -1 , and a bending strength of 1.86-2.88 MPa.
- the present invention improves the uniformity of the ceramic fiber filter tube by combining two sintering aids with different properties, namely silica sol and glass fiber, and freeze-drying the green body before calcination, thereby successfully preparing a ceramic fiber filter tube with good air permeability.
- the reduction in sintering temperature also reduces the sintering energy consumption for preparing the ceramic fiber filter tube.
- the combined use of two sintering aids with different properties can effectively improve the performance of the ceramic fiber filter tube prepared by the wet molding technology.
- the freeze-drying treatment can block the path of the nanoparticles in the silica sol migrating to the surface of the ceramic fiber filter tube due to capillary force, thereby making the properties of the prepared ceramic fiber filter tube more uniform. It provides a reference for preparing high-throughput ceramic fiber membranes.
- Figure 1 is a SEM image of the microscopic morphology of the glass fiber used in Example 3.
- Figure 2 is a macroscopic morphology of the ceramic fiber filter tube prepared in Example 3.
- Figure 3 is an SEM image of the cross-sectional morphology, outer surface, and middle part of the ceramic fiber filter tube prepared in Example 3.
- Figure 4 is a SEM image of the surface and cross-section of the ceramic fiber filter tube prepared in Example 3 after fracture.
- Figure 5 is the pore size distribution diagram of the ceramic fiber filter tube prepared in Example 3.
- Figure 6 is a comparison chart of the relationship between Darcy permeability, porosity and pore size of the ceramic fiber filter tube prepared in Example 3 and the ceramic fiber membrane prepared in other research works.
- the ceramic fiber filter tube green body After stirring for 10 min, it was quickly injected into the filter press mold, and the pressure was slowly applied to 2 MPa. After the water was filtered out, the ceramic fiber filter tube green body was obtained.
- the demolded green body was placed in a refrigerator and frozen for 24 h, placed in a -60 °C vacuum freeze dryer and dried for 24 h, and then heated to 800 °C at a rate of 0.5 °C/min in an air atmosphere and kept warm for 3 h.
- the prepared ceramic fiber filter tube has an average pore size of 34.1 ⁇ m, a porosity of about 74%, a gas permeability of 642 m 3 ⁇ m -2 ⁇ h -1 ⁇ kPa -1 , and an average flexural strength of about 1.86 MPa.
- the ceramic fiber filter tube green body After stirring for 8 min, it was quickly injected into the filter press mold, and the pressure was slowly applied to 3 MPa. After the water was filtered out, the ceramic fiber filter tube green body was obtained.
- the demolded green body was placed in a refrigerator and frozen for 12 h, placed in a -50 °C vacuum freeze dryer and dried for 24 h, and then heated to 1000 °C at a rate of 2 °C/min in an air atmosphere and kept warm for 2 h.
- the prepared ceramic fiber filter tube has an average pore size of 34.6 ⁇ m, a porosity of about 74.6%, a gas permeability of 680 m 3 ⁇ m -2 ⁇ h -1 ⁇ kPa -1 , and an average flexural strength of about 2.34 MPa.
- the ceramic fiber filter tube green body After stirring for 5 min, it was quickly injected into the filter press mold, and the pressure was slowly applied to 3 MPa. After the water was filtered out, the ceramic fiber filter tube green body was obtained.
- the demolded green body was placed in a refrigerator and frozen for 24 h, placed in a -40 °C vacuum freeze dryer and dried for 12 h, and then heated to 1200 °C at a rate of 2 °C/min in an air atmosphere and kept warm for 2 h.
- the prepared ceramic fiber filter tube has an average pore size of 35.2 ⁇ m, a porosity of about 75%, a gas permeability of 787 m 3 ⁇ m -2 ⁇ h -1 ⁇ kPa -1 , and an average flexural strength of about 2.68 MPa.
- Table 1 is a performance comparison between the mullite fiber tube prepared in this example and the silicon carbide particle ceramic tube in the literature.
- the mullite fiber tube has an obvious advantage of high air permeability.
- Figure 1 is a microscopic SEM image of the glass fiber used in this example. The glass fiber diameter is about 10 ⁇ m and the average length is about 60 ⁇ m.
- Figure 2 is a macroscopic morphology of the ceramic fiber filter tube prepared in this example. The fiber filter tube is 80 mm long, 39 mm in outer diameter, and 12 mm in wall thickness.
- Figure 3 is a cross-sectional morphology, outer surface, and a magnified SEM image of the middle part of the ceramic fiber filter tube prepared in this example. The sintering aid is evenly distributed in the ceramic fiber filter tube.
- Figure 4 is a SEM image of the surface and cross section of the ceramic fiber filter tube prepared in this example after fracture. A large number of fibers extend to the outside of the fracture surface. Combined with the uniform dispersion of the sintering aid inside the ceramic fiber material, it is proved that the bridging mechanism of the fiber plays a certain role in the fracture process.
- Figure 5 is a pore size distribution diagram of the ceramic fiber filter tube prepared in this example. The pore size distribution is concentrated, and the average pore size is about 35.2 ⁇ m.
- FIG6 shows the relationship between the Darcy permeability, porosity and pore size of the ceramic fiber filter tube prepared in this example and the ceramic fiber membrane prepared in other research works. It can be seen that the air permeability of the ceramic fiber filter tube prepared in this work is better than the average level.
- the ceramic fiber filter tube green body After stirring for 3 min, it was quickly injected into the filter press mold, and the pressure was slowly applied to 4 MPa. After the water was filtered out, the ceramic fiber filter tube green body was obtained.
- the demolded green body was placed in a refrigerator and frozen for 12 h, placed in a -20 °C vacuum freeze dryer and dried for 24 h, and then heated to 1400 °C at a rate of 3 °C/min in an air atmosphere and kept warm for 1 h.
- the prepared ceramic fiber filter tube has an average pore size of 34.8 ⁇ m, a porosity of about 75.2%, a gas permeability of 740 m 3 ⁇ m -2 ⁇ h -1 ⁇ kPa -1 , and an average flexural strength of about 2.88 MPa.
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- Chemical Kinetics & Catalysis (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Nanotechnology (AREA)
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Abstract
本发明公开了一种高透气性陶瓷纤维过滤管的制备方法，以莫来石短纤维为骨料，添加玻璃纤维和硅溶胶作为烧结助剂，采用压滤成型工艺得到陶瓷纤维滤管生坯，依次通过冷冻干燥和热处理得到高透气性的陶瓷纤维过滤管。两种不同性质烧结助剂的结合使用能有效改善湿法成型技术制备的陶瓷纤维过滤管性能。同时，冷冻干燥处理能够阻断硅溶胶中的纳米颗粒由于毛细作用力向陶瓷纤维过滤管表面迁移的路径，从而使制备得的陶瓷纤维过滤管的性质更均匀。为制备高通量的陶瓷纤维膜提供了参考。
Description
本发明涉及一种高透气性陶瓷纤维过滤管的制备方法，属于膜材料的制备领域。
陶瓷纤维膜是以耐高温陶瓷纤维，如氧化铝纤维、硅酸铝纤维、莫来石纤维等为骨料制备的一类陶瓷过滤材料。陶瓷纤维之间通过相互桥连形成的三维网络状多孔结构，赋予了陶瓷纤维膜孔隙率高、热稳定性好、气体渗透性高的特点，使其成为最具发展前景的陶瓷膜材料之一。传统的陶瓷纤维过滤管通常是以湿法真空抽滤成型工艺制备的，然而由于负压的抽吸作用，容易造成纤维多孔陶瓷材料内部不均的问题，从而对陶瓷纤维膜的透气性产生不利影响。因此，如何改善陶瓷纤维过滤管的制备工艺，以制备高透气性的陶瓷纤维过滤管十分重要。
模具成型技术（包括干压成型、凝胶注模、压滤成型等）具备操作简单、高效的特点，在陶瓷纤维膜制备领域有广泛的应用前景。干压成型技术制备得到的陶瓷纤维过滤材料，虽然强度明显提高，但是由于成型压力较大，多孔纤维骨架结构会被压实而导致气体渗透性损失较大。Xu等人[Ceramics International, 2017, 43(1): 228-233]采用凝胶注模法，将莫来石纤维和烧结助剂添加到叔丁醇基的凝胶预混溶液中，在引发剂的作用下有机单体聚合使料浆凝固，从而得到高强度的生坯。王树海等人[现代陶瓷技术, 1995(04): 19-25]介绍了压滤成型工艺的工艺原理以及浆料体系、工艺参数对成品性能的影响，指出在受到压力和摩擦阻力的影响下，固相颗粒的团聚性降低，增加了浆料的均匀性；分散度高的浆料成型的固化层因渗透系数低而成型缓慢，可能引起密度梯度导致整体均匀性不佳；较大的成型压力可以得到更均匀的陶瓷成品，然而压力过高往往会造成脱模及干燥过程中的开裂，比较理想的压力范围为1-4 MPa。
液相烧结助剂具有粒径小、分散性好的特点，可以均匀包裹在骨料表面和交叉点处，有助于促进低温烧结过程，溶胶以及陶瓷前驱体溶液均可以用于辅助多孔陶瓷烧结过程。Hai等人[Refractories and Industrial Ceramics, 2012, 53: 157-161]以聚碳硅烷为前驱体溶液，干燥后，在1000 ℃不添加任何烧结助剂的条件下烧结得到了纯质的碳化硅多孔陶瓷，平均孔隙率为33.4%，断裂强度~16 MPa，平均孔径为2.275 μm。依靠纤维连接点处少量无机溶胶形成的颈部连接强度较低，不利于陶瓷纤维膜的长时间使用，而低熔点的固体烧结助剂能够有效强化多孔材料的机械性能。Xu等人[Ceramics International, 2017, 43(1): 228-233]考察了不同的固体烧结助剂（硅粉末、二氧化硅粉末以及硼硅混合物）对制备的纤维多孔陶瓷材料机械性能的影响。结果表明，在1500 °C烧结下，以硼硅混合物作为烧结助剂制备得到的多孔陶瓷纤维材料抗压强度最高，约为2.08 MPa。
本发明的目的是为改进现有技术的缺陷而提出结合固态和液态两种不同性质的烧结助剂代替常见的液态烧结助剂制备陶瓷纤维过滤管，通过不同性质烧结助剂的使用，解决了纤维连接点处颈部连接弱的不足；同时以冷冻干燥技术处理生坯，有效提高陶瓷纤维管的均一性，制备出高透气性的陶瓷纤维过滤管。
本发明的技术方案为：一种高透气性陶瓷纤维过滤管的制备方法，其具体步骤如下：A首先将一定质量分数的硅溶胶与水按一定体积比混合并进行充分搅拌，随后加入莫来石短纤维、玻璃纤维，其中硅溶胶、莫来石短纤维和玻璃纤维的质量比为（30-45）：（1.5-9）：1，加入有机成型助剂并搅拌一定时间，搅拌一定时间后迅速注入压滤模具中，缓慢施加压力至水滤出后得到陶瓷纤维滤管生坯；B将脱模后的生坯放入冰箱冷冻12-24 h，再置于-60 ℃至-20 ℃环境中干燥12-24 h，随后经煅烧过程得到陶瓷纤维过滤管。
优选所述的硅溶胶的质量分数为20 wt%-40 wt%，其与水混合的体积比为1：（1.5-9）；莫来石短纤维的长径比为50-200；有机成型助剂为聚乙烯醇（PVA）溶液，浓度为8 wt%-12 wt%，添加量为莫来石短纤维和玻璃纤维总质量的60%-80%。
优选所述的制膜液搅拌时间为3-10 min。
优选所述的压滤成型过程中的压力为2-4 MPa。
优选所述的煅烧过程为：将生坯在800-1400 ℃下煅烧，升温速率和降温速率控制在0.5-3 ℃/min，保温时间为1-3 h。
本发明制得的陶瓷纤维过滤管平均孔径为34.1-35.2 μm，孔隙率为74-75.2％，气体渗透率为642-787 m
3·m
-2·h
-1·kPa
-1，抗弯强度为1.86-2.88 MPa。
有益效果：
本发明通过结合硅溶胶和玻璃纤维两种性质不同的烧结助剂，以及通过煅烧前对生坯进行冷冻干燥处理，提高陶瓷纤维过滤管的均匀性，成功制备出透气性良好的陶瓷纤维过滤管，烧结温度的降低也降低了制备陶瓷纤维过滤管的烧结能耗。两种不同性质烧结助剂的结合使用能有效改善湿法成型技术制备的陶瓷纤维过滤管性能。同时，冷冻干燥处理能够阻断硅溶胶中的纳米颗粒由于毛细作用力向陶瓷纤维过滤管表面迁移的路径，从而使制备得的陶瓷纤维过滤管的性质更均匀。为制备高通量的陶瓷纤维膜提供了参考。
图1是实例3中所使用的玻璃纤维的微观形貌SEM图。
图2是实例3中制备的陶瓷纤维滤管的宏观形貌图。
图3是实例3中制备的陶瓷纤维过滤管断面形貌、外表面以及中间局部放大的SEM图。
图4是实例3中制备的陶瓷纤维过滤管断裂后表面和断面的SEM图。
图5是实例3中制备的陶瓷纤维过滤管的孔径分布图。
图6是实例3中制备的陶瓷纤维过滤管与其他研究工作制备的陶瓷纤维膜的达西渗透率与孔隙度以及孔径之间的关系对比图。
实施例1
首先将团聚的莫来石短纤维置于水中进行搅拌分散，过滤掉多余的水分后置于120 °C烘箱内烘干，得到分散性良好的短纤维（长径比为50）。然后将40 wt%硅溶胶与水按一定体积比混合并充分搅拌，其中硅溶胶：水=1：9，随后加入莫来石短纤维和玻璃纤维，使硅溶胶、莫来石短纤维和玻璃纤维的质量比为30：1.5：1，继续添加质量为上述两种纤维总质量60%的12 wt%PVA溶液，搅拌10 min后迅速注入压滤模具中，缓慢施加压力至2 MPa，待水滤出后得到陶瓷纤维滤管生坯，将脱模后的生坯放入冰箱冷冻24 h，置于-60 ℃真空冷冻干燥机中干燥24 h，然后在空气气氛下以0.5 ℃/min的速率升温至800 ℃并保温3 h，制备出的陶瓷纤维过滤管平均孔径为34.1 μm，孔隙率约为74 %，气体渗透性为642 m
3·m
-2·h
-1·kPa
-1，平均抗弯强度约为1.86 MPa。
实施例2
首先将团聚的莫来石短纤维置于水中进行搅拌分散，过滤掉多余的水分后置于120 °C烘箱内烘干，得到分散性良好的短纤维（长径比为200）。然后将35 wt%硅溶胶与水按一定体积比混合并充分搅拌，其中硅溶胶：水=1：4，随后加入莫来石短纤维和玻璃纤维，使硅溶胶、莫来石短纤维和玻璃纤维的质量比为35：2.33：1，继续添加质量为上述两种纤维总质量70%的10 wt%PVA溶液，搅拌8 min后迅速注入压滤模具中，缓慢施加压力至3 MPa，待水滤出后得到陶瓷纤维滤管生坯，将脱模后的生坯放入冰箱冷冻12 h，置于-50 ℃真空冷冻干燥机中干燥24 h，然后在空气气氛下以2 ℃/min的速率升温至1000 ℃并保温2 h，制备出的陶瓷纤维过滤管平均孔径为34.6 μm，孔隙率约为74.6 %，气体渗透性为680 m
3·m
-2·h
-1·kPa
-1，平均抗弯强度约为2.34 MPa。
实施例3
首先将团聚的莫来石短纤维置于水中进行搅拌分散，过滤掉多余的水分后置于120 °C烘箱内烘干，得到分散性良好的短纤维（长径比为100）。然后将30 wt%硅溶胶与水按一定体积比混合并充分搅拌，其中硅溶胶：水=1：2.33，随后加入莫来石短纤维和玻璃纤维，使硅溶胶、莫来石短纤维和玻璃纤维的质量比为40：4：1，继续添加质量为上述两种纤维总质量75%的10wt %PVA溶液，搅拌5 min后迅速注入压滤模具中，缓慢施加压力至3 MPa，待水滤出后得到陶瓷纤维滤管生坯，将脱模后的生坯放入冰箱冷冻24 h，置于-40 ℃真空冷冻干燥机中干燥12 h，然后在空气气氛下以2 ℃/min的速率升温至1200 ℃并保温2 h，制备出的陶瓷纤维过滤管平均孔径为35.2 μm，孔隙率约为75 %，气体渗透性为787 m
3·m
-2·h
-1·kPa
-1，平均抗弯强度约为2.68 MPa。
表1是本实例中制备的莫来石纤维管与文献中碳化硅颗粒陶瓷管的性能对比，莫来石纤维管具有明显的高透气性优势。图1是本实例中使用的玻璃纤维的微观形貌SEM图，玻璃纤维直径约为10 μm，平均长度约为60 μm。图2是本实例中制备的陶瓷纤维滤管的宏观形貌图，纤维滤管的长度80 mm，外径为39 mm，壁厚为12 mm。图3是本实例中制备的陶瓷纤维过滤管断面形貌、外表面以及中间局部放大的SEM图，陶瓷纤维过滤管中烧结助剂分布均匀。图4是本实例中制备的陶瓷纤维过滤管断裂后表面和断面的SEM图，大量的纤维延伸到断裂面外侧，结合烧结助剂在陶瓷纤维材料内部分散的均匀性，证明了纤维的桥连机制在断裂过程中起一定作用。图5是本实例中制备的陶瓷纤维过滤管的孔径分布图，孔径分布集中，平均孔径约为35.2 μm。图6是本实例中制备的陶瓷纤维过滤管与其他研究工作制备的陶瓷纤维膜的达西渗透率与孔隙度以及孔径之间的关系，可见本工作制备的陶瓷纤维过滤管透气性优于平均水平。
实施例4
首先将团聚的莫来石短纤维置于水中进行搅拌分散，过滤掉多余的水分后置于120 °C烘箱内烘干，得到分散性良好的短纤维（长径比为150）。然后将20 wt%硅溶胶与水按一定体积比混合并充分搅拌，其中硅溶胶：水=1：1.5，随后加入莫来石短纤维和玻璃纤维，使硅溶胶、莫来石短纤维和玻璃纤维的质量比为45：9：1，继续添加质量为上述两种纤维总质量80%的8 wt%PVA溶液，搅拌3 min后迅速注入压滤模具中，缓慢施加压力至4 MPa，待水滤出后得到陶瓷纤维滤管生坯，将脱模后的生坯放入冰箱冷冻12 h，置于-20 ℃真空冷冻干燥机中干燥24 h，然后在空气气氛下以3 ℃/min的速率升温至1400 ℃并保温1 h，制备出的陶瓷纤维过滤管平均孔径为34.8 μm，孔隙率约为75.2 %，气体渗透性为740 m
3·m
-2·h
-1·kPa
-1，平均抗弯强度约为2.88 MPa。
表1 实例3中制备的莫来石纤维管与文献中碳化硅颗粒陶瓷管的性能对比：
。
Claims (6)
- 一种高透气性陶瓷纤维过滤管的制备方法，其特征在于，具体操作步骤如下：A、将一定质量分数的硅溶胶与水按体积比混合后加入莫来石短纤维与玻璃纤维，其中硅溶胶、莫来石短纤维和玻璃纤维的质量比为（30-45）：（1.5-9）：1，加入有机成型助剂并搅拌一定时间，随后通过压滤成型法得到陶瓷纤维滤管生坯；选用的莫来石短纤维长径比为50-200；B、将脱模后的生坯放入冰箱冷冻12-24 h，再置于-60 ℃至-20 ℃环境中干燥12-24 h，随后经煅烧过程得到陶瓷纤维过滤管。
- 根据权利要求1所述的一种高透气性陶瓷纤维过滤管的制备方法，其特征在于：步骤A中所述硅溶胶的质量分数为20 wt%-40 wt%，其与水混合的体积比为1：（1.5-9）。
- 根据权利要求1所述的一种高透气性陶瓷纤维过滤管的制备方法，其特征在于：步骤A中所述的有机成型剂为聚乙烯醇（PVA）溶液，浓度为8 wt%-12 wt%，添加量为莫来石短纤维和玻璃纤维总质量的60%-80%。
- 根据权利要求1所述的一种高透气性陶瓷纤维过滤管的制备方法，其特征在于：制膜液搅拌时间为3-10 min。
- 根据权利要求1所述的一种高透气性陶瓷纤维过滤管的制备方法，其特征在于：压滤成型过程中的压力为2-4 MPa。
- 根据权利要求1所述的一种高透气性陶瓷纤维过滤管的制备方法，其特征在于：煅烧过程为将生坯在800-1400 ℃下煅烧，升温速率和降温速率控制在0.5-3 ℃/min，保温时间为1-3 h。
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| CN110038368B (zh) * | 2019-04-17 | 2021-04-02 | 合肥合意环保科技工程有限公司 | 一种陶瓷纤维滤管、制备方法及加压抽吸成型装置 |
| CN112892238A (zh) * | 2019-11-15 | 2021-06-04 | 山东工业陶瓷研究设计院有限公司 | 一种连续玻璃纤维增强的陶瓷纤维过滤元件及制备方法 |
| CN111908932B (zh) * | 2020-07-21 | 2023-06-20 | 山东工业陶瓷研究设计院有限公司 | 一种轻质高效防隔热一体化热防护材料及制备方法 |
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| CN115521158A (zh) | 2022-12-27 |
| CN115521158B (zh) | 2023-08-18 |
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