CN110894166A - Preparation method of mullite porous graded fibrous material - Google Patents
Preparation method of mullite porous graded fibrous material Download PDFInfo
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- CN110894166A CN110894166A CN201911222689.1A CN201911222689A CN110894166A CN 110894166 A CN110894166 A CN 110894166A CN 201911222689 A CN201911222689 A CN 201911222689A CN 110894166 A CN110894166 A CN 110894166A
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- 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 title claims abstract description 38
- 229910052863 mullite Inorganic materials 0.000 title claims abstract description 38
- 239000002657 fibrous material Substances 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000000835 fiber Substances 0.000 claims abstract description 113
- 238000002347 injection Methods 0.000 claims abstract description 32
- 239000007924 injection Substances 0.000 claims abstract description 32
- 238000000034 method Methods 0.000 claims abstract description 21
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 108
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 48
- 239000007864 aqueous solution Substances 0.000 claims description 46
- 239000002002 slurry Substances 0.000 claims description 44
- 239000011230 binding agent Substances 0.000 claims description 42
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 40
- 229910052782 aluminium Inorganic materials 0.000 claims description 37
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 28
- 238000003756 stirring Methods 0.000 claims description 22
- 239000003054 catalyst Substances 0.000 claims description 21
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 17
- 235000010469 Glycine max Nutrition 0.000 claims description 15
- 244000068988 Glycine max Species 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 15
- 235000013336 milk Nutrition 0.000 claims description 15
- 239000008267 milk Substances 0.000 claims description 15
- 210000004080 milk Anatomy 0.000 claims description 15
- 238000007710 freezing Methods 0.000 claims description 14
- 230000008014 freezing Effects 0.000 claims description 14
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 14
- 238000004108 freeze drying Methods 0.000 claims description 13
- 239000002893 slag Substances 0.000 claims description 12
- WOZZOSDBXABUFO-UHFFFAOYSA-N tri(butan-2-yloxy)alumane Chemical compound [Al+3].CCC(C)[O-].CCC(C)[O-].CCC(C)[O-] WOZZOSDBXABUFO-UHFFFAOYSA-N 0.000 claims description 12
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 11
- 229910017604 nitric acid Inorganic materials 0.000 claims description 11
- 239000000243 solution Substances 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 239000011259 mixed solution Substances 0.000 claims description 8
- 238000010992 reflux Methods 0.000 claims description 8
- 238000007873 sieving Methods 0.000 claims description 8
- 229910052710 silicon Inorganic materials 0.000 claims description 8
- 239000010703 silicon Substances 0.000 claims description 8
- IRPGOXJVTQTAAN-UHFFFAOYSA-N 2,2,3,3,3-pentafluoropropanal Chemical group FC(F)(F)C(F)(F)C=O IRPGOXJVTQTAAN-UHFFFAOYSA-N 0.000 claims description 7
- KLZUFWVZNOTSEM-UHFFFAOYSA-K Aluminum fluoride Inorganic materials F[Al](F)F KLZUFWVZNOTSEM-UHFFFAOYSA-K 0.000 claims description 7
- 229920001661 Chitosan Polymers 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 4
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 4
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims description 4
- 230000007062 hydrolysis Effects 0.000 claims description 4
- 238000006460 hydrolysis reaction Methods 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 4
- 239000000463 material Substances 0.000 abstract description 8
- 230000001105 regulatory effect Effects 0.000 abstract description 4
- 238000011160 research Methods 0.000 abstract description 4
- 238000004062 sedimentation Methods 0.000 abstract description 4
- 230000001276 controlling effect Effects 0.000 abstract description 2
- 238000012360 testing method Methods 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 235000013322 soy milk Nutrition 0.000 description 2
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 description 1
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 229910000323 aluminium silicate Inorganic materials 0.000 description 1
- 229910001570 bauxite Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 235000005770 birds nest Nutrition 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000010574 gas phase reaction Methods 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- ABTOQLMXBSRXSM-UHFFFAOYSA-N silicon tetrafluoride Chemical compound F[Si](F)(F)F ABTOQLMXBSRXSM-UHFFFAOYSA-N 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000003828 vacuum filtration Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 235000005765 wild carrot Nutrition 0.000 description 1
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- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/0045—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by a process involving the formation of a sol or a gel, e.g. sol-gel or precipitation processes
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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
- C04B35/10—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 aluminium oxide
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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
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3418—Silicon oxide, silicic acids or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
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- 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
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Abstract
A preparation method of mullite porous graded fibrous material relates to a preparation method of mullite graded material. The invention aims to solve the technical problem that the quality of whiskers and fibers cannot be accurately regulated and controlled in a large range in the conventional mullite porous graded fibrous material. Firstly, the invention uses the low-cost polycrystalline mullite fiber to be dedicated to the research of low-cost high-performance samples. The mullite graded fibrous material prepared by combining the control of fiber sedimentation and the injection method can regulate and control the proportion of whiskers and fibers in a graded structure on the premise of controlling low density.
Description
Technical Field
The invention relates to a preparation method of a mullite grading material.
Background
The mullite porous fibrous material is an aluminosilicate material and has the advantages of a three-dimensional network structure similar to a bird nest, good high-temperature mechanical property, good chemical stability, low thermal conductivity, good creep property, good thermal shock resistance and the like. The preparation process can be adjusted to meet the performance requirements of different application occasions, such as gas and wastewater filters, separation membranes, catalyst carriers, heat-insulating materials and other fields with special requirements on pore diameter and structure. At present, a plurality of synthesis methods are used for obtaining a mullite whisker/fiber hierarchical structure with a three-dimensional structure, and mainly comprise a fluorine catalytic gas phase reaction method, a molten salt method and the like. The preparation of mullite whiskers where different aluminum sources (e.g., bauxite, aluminum nitrate), different silicon sources (e.g., silica, tetraethylorthosilicate), different catalysts (e.g., aluminum fluoride, ammonium fluoride, silicon fluoride) have a significant impact on whisker morphology and synthesis conditions has also been attempted by many researchers.
At present, research on the grading material mostly focuses on exploration of a whisker growth mechanism and influence of the proportion of effective components (an aluminum source, a silicon source and a catalyst) in raw materials on the organizational structure and the performance of the grading material, the research on the influence of the whisker to fiber mass ratio in the grading structure on the organizational structure and the performance of the grading material is less, researchers mostly adopt a suction filtration method to change the mass ratio of the whisker to the fiber in the grading material, and the method cannot accurately regulate and control the quality ratio of the whisker to the fiber in a large range. On the basis, the development of a method for preparing the grading material with the adjustable whisker-to-fiber mass ratio is of great significance.
Disclosure of Invention
The invention provides a preparation method of a mullite porous graded fibrous material, aiming at solving the technical problem that the quality of whiskers and fibers cannot be accurately regulated and controlled in a large range in the existing mullite porous graded fibrous material.
The preparation method of the mullite porous graded fibrous material is carried out according to the following steps:
firstly, preparing a fiber blank:
①, cutting the polycrystalline mullite fiber into granular fiber by using scissors, sieving the granular fiber by a 40-mesh sieve, and repeatedly sieving the granular fiber until no slag balls are sieved out, wherein the diameter of the granular fiber is 0.5-3 mm;
②, putting the screened granular fibers obtained in the step ① into a soybean milk machine, adding water, and chopping for 20-22 min, wherein the rotation speed of the soybean milk machine is 10000-11000 r/min, and the mass ratio of the screened granular fibers obtained in the step ① to the water is 1 (100-110);
③, after chopping, pouring the whole mixture in the soybean milk machine in the step ② into a container, standing for 20-25 s, then pouring out and retaining the upper layer of fiber, and removing the slag balls at the bottom;
④, repeating the operation of step ③ four to five times to remove the slag balls, and filtering the upper layer fiber with gauze to remove water to obtain chopped fiber;
⑤, dispersing the fibers chopped in the step ④ into an acetic acid aqueous solution containing a binder, and then stirring for 30-35 min to obtain a slurry, wherein the mass of the chopped fibers is 1.5-2% of that of the acetic acid aqueous solution containing the binder, the concentration of acetic acid in the acetic acid aqueous solution containing the binder is 0.5-0.6 mol/L, the binder in the acetic acid aqueous solution containing the binder is chitosan, and the mass of the binder is 0.5-2% of that of the acetic acid aqueous solution containing the binder;
⑥, pouring the slurry prepared in the step ⑤ into a mould, putting the mould into a refrigerator, freezing at the temperature of-18 to-20 ℃ until the slurry is completely frozen, putting the mould into a freeze dryer, freeze-drying at the temperature of-60 to-65 ℃ and the vacuum degree of 150 to 200Pa for 72 to 74 hours, and finally demoulding to obtain a fiber blank;
secondly, preparing active slurry:
①, preparation of aluminum sol:
mixing aluminum sec-butoxide with water, refluxing and stirring for 1-1.5 h under the condition of 70-100 ℃ water bath, then adding dilute nitric acid aqueous solution to promote further hydrolysis, clarifying the solution from milky color, then continuously refluxing and stirring for 9-10 h under the condition of 70-100 ℃ water bath to obtain mixed sol, and putting the mixed sol into a constant-temperature stirring heater at 100-110 ℃ until the content of Al element in the mixed sol is 1-1.1 mol/L to obtain aluminum sol; the molar ratio of the aluminum sec-butoxide to the water is 0.12 (9.5-10); the mass ratio of the dilute nitric acid aqueous solution to the secondary aluminum butoxide is 1 (6-7);
②, preparation of silica sol:
pouring tetraethoxysilane into a beaker, adding absolute ethyl alcohol, adding deionized water to form a mixed solution, putting the mixed solution into a water bath at the temperature of 40-50 ℃ for heat preservation for 10-15 min, dripping hydrochloric acid aqueous solution, and preserving the heat for 1-1.5 h in the water bath at the temperature of 40-50 ℃ to obtain silica sol; the molar ratio of the ethyl orthosilicate to the deionized water is 1 (4-5); the molar ratio of the ethyl orthosilicate to the absolute ethyl alcohol is 1 (4-5); the molar ratio of the ethyl orthosilicate to the hydrogen chloride in the hydrochloric acid aqueous solution is 1 (7.5 multiplied by 10)-4～10-3) (ii) a The concentration of the hydrochloric acid aqueous solution is 0.2-0.3 mol/L;
③, mixing the aluminum sol obtained in the step II ① with the silica sol obtained in the step II ②, adding a catalyst, and stirring for 12-15 hours to obtain active slurry, wherein the catalyst is aluminum fluoride powder, the molar ratio of aluminum elements in the catalyst to aluminum elements in the aluminum sol is 3 (6-8), and the molar ratio of aluminum elements to silicon elements in the active slurry is 3 (1.1-1.3);
thirdly, injection:
injecting the active slurry in the step two into the fiber blank in the step one by using an injection device, wherein the injection device is provided with an injection head, the side wall of the injection head is provided with a plurality of holes, and the active slurry flows into the fiber blank through the holes in the side wall and the holes at the bottom of the injection head;
fourthly, freezing and freeze drying:
and putting the injected fiber blank into a refrigerator, freezing at the temperature of minus 18-minus 20 ℃ until the fiber blank is completely frozen, putting the sample into a freeze drier, freeze-drying for 72-74 h at the temperature of minus 50-minus 60 ℃ and the vacuum degree of 150-200 Pa, and taking out to obtain a graded sample blank.
Fifthly, heat treatment:
and (3) placing the graded sample blank prepared in the fourth step into a crucible, covering the crucible with a cover, then placing the crucible into a muffle furnace, heating the crucible to 800-1200 ℃ from room temperature at a heating rate of 3-5 ℃/min in the air atmosphere, preserving the heat at 800-1200 ℃ for 2-3 h, and then cooling along with the furnace to obtain the mullite porous graded fibrous material.
The invention is characterized in that:
compared with the porous fibrous material prepared by the traditional process methods such as the gravity precipitation method, the pressurized liquid discharge method, the vacuum filtration method and the like, the invention adopts the freezing injection molding method to change the viscosity of the slurry by adding the chitosan in the step one to control the fiber sedimentation so as to realize more accurate control on the density of the fiber blank; compared with the traditional method for preparing the graded fibrous material by blending and sintering the fiber and the active powder, the method firstly prepares a fiber blank with lower density, and then realizes the regulation and control of the proportion of the whiskers and the fibers in the graded fibrous material by controlling the dosage of the active slurry injected into the network structure of the fiber, thereby realizing the regulation and control of the performance of the graded fibrous material and further realizing the preparation of the optimal graded structure.
The invention has the beneficial effects that:
firstly, the invention uses the low-cost polycrystalline mullite fiber to be dedicated to the research of low-cost high-performance samples. The invention can control the low density (0.03 g/cm) of the mullite graded fibrous material prepared by combining the control of fiber sedimentation and the injection method3～0.08g/cm3) The ratio of whiskers to fibers in the hierarchical structure is regulated and controlled on the premise of (1).
Drawings
Fig. 1 is an SEM image of mullite porous graded fibrous material prepared in run one.
Detailed Description
The first embodiment is as follows: the embodiment is a preparation method of a mullite porous graded fibrous material, which is specifically carried out according to the following steps:
firstly, preparing a fiber blank:
①, cutting the polycrystalline mullite fiber into granular fiber by using scissors, sieving the granular fiber by a 40-mesh sieve, and repeatedly sieving the granular fiber until no slag balls are sieved out, wherein the diameter of the granular fiber is 0.5-3 mm;
②, putting the screened granular fibers obtained in the step ① into a soybean milk machine, adding water, and chopping for 20-22 min, wherein the rotation speed of the soybean milk machine is 10000-11000 r/min, and the mass ratio of the screened granular fibers obtained in the step ① to the water is 1 (100-110);
③, after chopping, pouring the whole mixture in the soybean milk machine in the step ② into a container, standing for 20-25 s, then pouring out and retaining the upper layer of fiber, and removing the slag balls at the bottom;
④, repeating the operation of step ③ four to five times to remove the slag balls, and filtering the upper layer fiber with gauze to remove water to obtain chopped fiber;
⑤, dispersing the fibers chopped in the step ④ into an acetic acid aqueous solution containing a binder, and then stirring for 30-35 min to obtain a slurry, wherein the mass of the chopped fibers is 1.5-2% of that of the acetic acid aqueous solution containing the binder, the concentration of acetic acid in the acetic acid aqueous solution containing the binder is 0.5-0.6 mol/L, the binder in the acetic acid aqueous solution containing the binder is chitosan, and the mass of the binder is 0.5-2% of that of the acetic acid aqueous solution containing the binder;
⑥, pouring the slurry prepared in the step ⑤ into a mould, putting the mould into a refrigerator, freezing at the temperature of-18 to-20 ℃ until the slurry is completely frozen, putting the mould into a freeze dryer, freeze-drying at the temperature of-60 to-65 ℃ and the vacuum degree of 150 to 200Pa for 72 to 74 hours, and finally demoulding to obtain a fiber blank;
secondly, preparing active slurry:
①, preparation of aluminum sol:
mixing aluminum sec-butoxide with water, refluxing and stirring for 1-1.5 h under the condition of 70-100 ℃ water bath, then adding dilute nitric acid aqueous solution to promote further hydrolysis, clarifying the solution from milky color, then continuously refluxing and stirring for 9-10 h under the condition of 70-100 ℃ water bath to obtain mixed sol, and putting the mixed sol into a constant-temperature stirring heater at 100-110 ℃ until the content of Al element in the mixed sol is 1-1.1 mol/L to obtain aluminum sol; the molar ratio of the aluminum sec-butoxide to the water is 0.12 (9.5-10); the mass ratio of the dilute nitric acid aqueous solution to the secondary aluminum butoxide is 1 (6-7);
②, preparation of silica sol:
pouring tetraethoxysilane into a beaker, adding absolute ethyl alcohol, adding deionized water to form a mixed solution, putting the mixed solution into a water bath at the temperature of 40-50 ℃ for heat preservation for 10-15 min, dripping hydrochloric acid aqueous solution, and preserving the heat for 1-1.5 h in the water bath at the temperature of 40-50 ℃ to obtain silica sol; the molar ratio of the ethyl orthosilicate to the deionized water is 1 (4-5); the molar ratio of the ethyl orthosilicate to the absolute ethyl alcohol is 1 (4-5); the molar ratio of the ethyl orthosilicate to the hydrogen chloride in the hydrochloric acid aqueous solution is 1 (7.5 multiplied by 10)-4～10-3) (ii) a The concentration of the hydrochloric acid aqueous solution is 0.2-0.3 mol/L;
③, mixing the aluminum sol obtained in the step II ① with the silica sol obtained in the step II ②, adding a catalyst, and stirring for 12-15 hours to obtain active slurry, wherein the catalyst is aluminum fluoride powder, the molar ratio of aluminum elements in the catalyst to aluminum elements in the aluminum sol is 3 (6-8), and the molar ratio of aluminum elements to silicon elements in the active slurry is 3 (1.1-1.3);
thirdly, injection:
injecting the active slurry in the step two into the fiber blank in the step one by using an injection device, wherein the injection device is provided with an injection head, the side wall of the injection head is provided with a plurality of holes, and the active slurry flows into the fiber blank through the holes in the side wall and the holes at the bottom of the injection head;
fourthly, freezing and freeze drying:
putting the injected fiber blank into a refrigerator, freezing at the temperature of minus 18-minus 20 ℃ until the fiber blank is completely frozen, putting the sample into a freeze dryer, freeze-drying for 72-74 h at the temperature of minus 50-minus 60 ℃ and the vacuum degree of 150-200 Pa, and taking out to obtain a graded sample blank;
fifthly, heat treatment:
and (3) placing the graded sample blank prepared in the fourth step into a crucible, covering the crucible with a cover, then placing the crucible into a muffle furnace, heating the crucible to 800-1200 ℃ from room temperature at a heating rate of 3-5 ℃/min in the air atmosphere, preserving the heat at 800-1200 ℃ for 2-3 h, and then cooling along with the furnace to obtain the mullite porous graded fibrous material.
The second specific embodiment is different from the first specific embodiment in that in the first step ②, the screened granular fibers obtained in the first step ① are put into a soymilk machine, water is added for chopping for 20min, the rotation speed of the soymilk machine is 10000r/min, the mass ratio of the screened granular fibers obtained in the first step ① to the water is 1:100, and the rest is the same as the first specific embodiment.
Third embodiment the third embodiment is different from the first or second embodiment in that the first ⑤ is that the fiber cut in the ④ step is dispersed in an acetic acid aqueous solution containing a binder, and then stirred for 30min to obtain a slurry, wherein the mass of the fiber cut is 1.5% of the mass of the acetic acid aqueous solution containing the binder, the concentration of acetic acid in the acetic acid aqueous solution containing the binder is 0.5mol/L, the binder in the acetic acid aqueous solution containing the binder is chitosan, and the mass of the binder is 0.5% of the mass of the acetic acid aqueous solution containing the binder.
Fourth embodiment this embodiment differs from the first to third embodiments in that in the first ⑥ the slurry prepared in the second step ⑤ is poured into a mold, the mold is placed in a refrigerator and frozen at a temperature of-18 deg.c until the slurry is completely frozen, then the mold is placed in a freeze dryer and freeze dried at-60 deg.c and a vacuum of 150Pa for 72h, and finally the mold is removed to obtain a fiber body.
Fifth embodiment the fifth embodiment is different from the fourth embodiment in that the concentration of the dilute aqueous nitric acid solution in the second step ① is 1 mol/L.
Sixth specific embodiment, the difference between the fourth specific embodiment and the sixth specific embodiment is that in the second step ③, the aluminum sol in the second step ① and the silica sol in the second step ② are mixed, then a catalyst is added, and stirring is carried out for 12 hours, so as to obtain an active slurry, wherein the catalyst is aluminum fluoride powder, the molar ratio of aluminum element in the catalyst to aluminum element in the aluminum sol is 3:7, the molar ratio of aluminum element to silicon element in the active slurry is 3:1.2, and the difference is the same as that in the fourth specific embodiment.
The seventh embodiment: the fourth difference between this embodiment and the specific embodiment is that: and step four, putting the injected fiber blank into a refrigerator, freezing the fiber blank to be completely frozen at the temperature of 18 ℃ below zero, putting the sample into a freeze dryer, freeze-drying the sample for 72 hours at the temperature of 50 ℃ below zero and the vacuum degree of 150Pa, and taking out the sample to obtain a graded sample blank. The rest is the same as the fourth embodiment.
The specific implementation mode is eight: the fourth difference between this embodiment and the specific embodiment is that: and fifthly, placing the graded sample blank prepared in the fourth step into a crucible, covering the crucible with a cover, then placing the crucible into a muffle furnace, heating the crucible to 1000 ℃ from room temperature at a heating rate of 3 ℃/min in the air atmosphere, preserving the heat for 2h at 1000 ℃, and then cooling the crucible along with the furnace to obtain the mullite porous graded fibrous material. The rest is the same as the fourth embodiment.
The invention was verified with the following tests:
test one: the test is a preparation method of mullite porous graded fibrous material, which is specifically carried out according to the following steps:
firstly, preparing a fiber blank:
①, cutting the polycrystalline mullite fiber into granular fiber by using scissors, sieving the granular fiber by a 40-mesh sieve, and repeatedly sieving the granular fiber until no slag balls are sieved out, wherein the diameter of the granular fiber is 2 mm;
②, putting the screened granular fibers obtained in the step ① into a soybean milk machine, adding water, and chopping for 20min, wherein the rotation speed of the soybean milk machine is 10000r/min, and the mass ratio of the screened granular fibers obtained in the step ① to the water is 1: 100;
③, after chopping, pouring the whole mixture in the soybean milk machine in the step ② into a container, standing for 20s, then pouring out and retaining the fibers on the upper layer, and removing the slag balls at the bottom;
④, repeating the operation of step ③ for four times to remove the slag balls, and filtering the upper layer fiber with gauze to remove water to obtain chopped fiber;
⑤, dispersing the fibers chopped in the step ④ into an acetic acid aqueous solution containing a binder, and then stirring for 30min to obtain a slurry, wherein the mass of the chopped fibers is 1.5% of that of the acetic acid aqueous solution containing the binder, the concentration of acetic acid in the acetic acid aqueous solution containing the binder is 0.5mol/, the binder in the acetic acid aqueous solution containing the binder is chitosan, and the mass of the binder is 0.5% of that of the acetic acid aqueous solution containing the binder;
⑥, pouring the slurry prepared in the step ⑤ into a mould, putting the mould into a refrigerator, freezing the mould at the temperature of 18 ℃ below zero until the slurry is completely frozen, putting the mould into a freeze dryer, freeze-drying the mould for 72 hours at the temperature of 60 ℃ below zero and the vacuum degree of 150Pa, and finally demoulding to obtain a fiber blank;
the test shows that the density of the fiber blank is 0.022g/cm3；
The fiber blank is a cylinder, the diameter of the bottom surface is 3.8cm, and the height is 2.8 cm;
secondly, preparing active slurry:
①, preparation of aluminum sol:
mixing aluminum sec-butoxide with water, refluxing and stirring for 1h under the condition of 70 ℃ water bath, then adding dilute nitric acid aqueous solution to promote further hydrolysis, changing the solution from milky color to clear, continuously refluxing and stirring for 9h under the condition of 70 ℃ water bath to obtain mixed sol, and putting the mixed sol into a constant-temperature stirring heater at 100 ℃ until the content of Al element in the mixed sol is 1mol/L to obtain aluminum sol; the molar ratio of the aluminum sec-butoxide to the water is 0.12: 10; the mass ratio of the dilute nitric acid aqueous solution to the secondary aluminum butoxide is 1: 7; the concentration of the dilute nitric acid aqueous solution is 1 mol/L;
②, preparation of silica sol:
pouring tetraethoxysilane into a beaker, adding absolute ethyl alcohol, adding deionized water to form a mixed solution, putting the mixed solution into a water bath at 40 ℃ for heat preservation for 10min, dripping hydrochloric acid aqueous solution, and preserving the heat in the water bath at 40 ℃ for 1h to obtain silica sol; the molar ratio of the ethyl orthosilicate to the deionized water is 1: 4; the molar ratio of the ethyl orthosilicate to the absolute ethyl alcohol is 1: 4; the molar ratio of the ethyl orthosilicate to the hydrogen chloride in the hydrochloric acid aqueous solution is 1:7.5 multiplied by 10-4(ii) a The concentration of the hydrochloric acid aqueous solution is 0.2 mol/L;
③, mixing the aluminum sol obtained in the step II ① with the silica sol obtained in the step II ②, adding a catalyst, and stirring for 12-15 hours to obtain active slurry, wherein the catalyst is aluminum fluoride powder, the molar ratio of aluminum elements in the catalyst to aluminum elements in the aluminum sol is 3:7, and the molar ratio of aluminum elements to silicon elements in the active slurry is 3: 1.2;
thirdly, injection:
injecting the active slurry obtained in the step two into the fiber blank obtained in the step one by using an injection device, wherein the injection device is provided with an injection head, the side wall of the injection head is provided with a plurality of holes, and 3mL of active slurry flows into the fiber blank through the holes in the side wall and the holes at the bottom of the injection head; injection depth: repeatedly moving the injection head up and down within the range of 0.9-2.8 cm away from the bottom layer of the fiber blank body for injection; injection speed: 0.05 mL/s; the injection head is a needle head;
fourthly, freezing and freeze drying:
putting the injected fiber blank into a refrigerator, freezing the fiber blank at the temperature of minus 18 ℃ until the fiber blank is completely frozen, putting the sample into a freeze drier, freeze-drying the sample for 72 hours at the temperature of minus 50 ℃ and the vacuum degree of 150Pa, and taking out the sample to obtain a graded sample blank;
fifthly, heat treatment:
and (3) placing the graded sample blank prepared in the fourth step into a crucible, covering the crucible with a cover, then placing the crucible into a muffle furnace, heating the crucible to 1000 ℃ from room temperature at a heating rate of 3 ℃/min in the air atmosphere, preserving the heat at 1000 ℃ for 2h, and then cooling along with the furnace to obtain the mullite porous graded fibrous material.
Fig. 1 is an SEM image of the mullite porous graded fibrous material prepared in the first experiment, from which it can be seen that the mullite fiber surface is a well-developed whisker secondary structure, which is needle-like and densely grown.
The mullite graded fibrous material prepared by combining the control of fiber sedimentation and the injection method in the test can control the low density (0.06 g/cm)3) And the ratio of the whiskers to the fibers in the hierarchical structure is regulated and controlled on the premise of low thermal conductivity (0.04667W/mK).
Claims (8)
1. A preparation method of a mullite porous graded fibrous material is characterized by comprising the following steps:
firstly, preparing a fiber blank:
①, cutting the polycrystalline mullite fiber into granular fiber by using scissors, sieving the granular fiber by a 40-mesh sieve, and repeatedly sieving the granular fiber until no slag balls are sieved out, wherein the diameter of the granular fiber is 0.5-3 mm;
②, putting the screened granular fibers obtained in the step ① into a soybean milk machine, adding water, and chopping for 20-22 min, wherein the rotation speed of the soybean milk machine is 10000-11000 r/min, and the mass ratio of the screened granular fibers obtained in the step ① to the water is 1 (100-110);
③, after chopping, pouring the whole mixture in the soybean milk machine in the step ② into a container, standing for 20-25 s, then pouring out and retaining the upper layer of fiber, and removing the slag balls at the bottom;
④, repeating the operation of step ③ four to five times to remove the slag balls, and filtering the upper layer fiber with gauze to remove water to obtain chopped fiber;
⑤, dispersing the fibers chopped in the step ④ into an acetic acid aqueous solution containing a binder, and then stirring for 30-35 min to obtain a slurry, wherein the mass of the chopped fibers is 1.5-2% of that of the acetic acid aqueous solution containing the binder, the concentration of acetic acid in the acetic acid aqueous solution containing the binder is 0.5-0.6 mol/L, the binder in the acetic acid aqueous solution containing the binder is chitosan, and the mass of the binder is 0.5-2% of that of the acetic acid aqueous solution containing the binder;
⑥, pouring the slurry prepared in the step ⑤ into a mould, putting the mould into a refrigerator, freezing at the temperature of-18 to-20 ℃ until the slurry is completely frozen, putting the mould into a freeze dryer, freeze-drying at the temperature of-60 to-65 ℃ and the vacuum degree of 150 to 200Pa for 72 to 74 hours, and finally demoulding to obtain a fiber blank;
secondly, preparing active slurry:
①, preparation of aluminum sol:
mixing aluminum sec-butoxide with water, refluxing and stirring for 1-1.5 h under the condition of 70-100 ℃ water bath, then adding dilute nitric acid aqueous solution to promote further hydrolysis, clarifying the solution from milky color, then continuously refluxing and stirring for 9-10 h under the condition of 70-100 ℃ water bath to obtain mixed sol, and putting the mixed sol into a constant-temperature stirring heater at 100-110 ℃ until the content of Al element in the mixed sol is 1-1.1 mol/L to obtain aluminum sol; the molar ratio of the aluminum sec-butoxide to the water is 0.12 (9.5-10); the mass ratio of the dilute nitric acid aqueous solution to the secondary aluminum butoxide is 1 (6-7);
②, preparation of silica sol:
pouring tetraethoxysilane into a beaker, adding absolute ethyl alcohol, adding deionized water to form a mixed solution, putting the mixed solution into a water bath at the temperature of 40-50 ℃ for heat preservation for 10-15 min, dripping hydrochloric acid aqueous solution, and preserving the heat for 1-1.5 h in the water bath at the temperature of 40-50 ℃ to obtain silica sol; the molar ratio of the ethyl orthosilicate to the deionized water is 1 (4-5); the molar ratio of the ethyl orthosilicate to the absolute ethyl alcohol is 1 (4-5); the molar ratio of the ethyl orthosilicate to the hydrogen chloride in the hydrochloric acid aqueous solution is 1 (7.5 multiplied by 10)-4～10-3) (ii) a The concentration of the hydrochloric acid aqueous solution is 0.2-0.3 mol/L;
③, mixing the aluminum sol obtained in the step II ① with the silica sol obtained in the step II ②, adding a catalyst, and stirring for 12-15 hours to obtain active slurry, wherein the catalyst is aluminum fluoride powder, the molar ratio of aluminum elements in the catalyst to aluminum elements in the aluminum sol is 3 (6-8), and the molar ratio of aluminum elements to silicon elements in the active slurry is 3 (1.1-1.3);
thirdly, injection:
injecting the active slurry in the step two into the fiber blank in the step one by using an injection device, wherein the injection device is provided with an injection head, the side wall of the injection head is provided with a plurality of holes, and the active slurry flows into the fiber blank through the holes in the side wall and the holes at the bottom of the injection head;
fourthly, freezing and freeze drying:
putting the injected fiber blank into a refrigerator, freezing at the temperature of minus 18-minus 20 ℃ until the fiber blank is completely frozen, putting the sample into a freeze dryer, freeze-drying for 72-74 h at the temperature of minus 50-minus 60 ℃ and the vacuum degree of 150-200 Pa, and taking out to obtain a graded sample blank;
fifthly, heat treatment:
and (3) placing the graded sample blank prepared in the fourth step into a crucible, covering the crucible with a cover, then placing the crucible into a muffle furnace, heating the crucible to 800-1200 ℃ from room temperature at a heating rate of 3-5 ℃/min in the air atmosphere, preserving the heat at 800-1200 ℃ for 2-3 h, and then cooling along with the furnace to obtain the mullite porous graded fibrous material.
2. The method for preparing the mullite porous graded fibrous material according to claim 1, wherein in the step one ②, the screened granular fibers obtained in the step ① are put into a soybean milk machine, water is added into the soybean milk machine for chopping for 20min, the rotation speed of the soybean milk machine is 10000r/min, and the mass ratio of the screened granular fibers obtained in the step ① to the water is 1: 100.
3. The method for preparing the mullite porous graded fibrous material as claimed in claim 1, wherein the step ⑤ comprises dispersing the fibers chopped in the step ④ into an aqueous acetic acid solution containing a binder, and stirring for 30min to obtain a slurry, wherein the mass of the chopped fibers is 1.5% of that of the aqueous acetic acid solution containing the binder, the concentration of acetic acid in the aqueous acetic acid solution containing the binder is 0.5mol/L, the binder in the aqueous acetic acid solution containing the binder is chitosan, and the mass of the binder is 0.5% of that of the aqueous acetic acid solution containing the binder.
4. The method of claim 1, wherein in step one ⑥, the slurry prepared in step ⑤ is poured into a mold, the mold is placed in a refrigerator and frozen at a temperature of-18 ℃ to completely freeze the slurry, then the mold is placed in a freeze dryer and freeze-dried at-60 ℃ and a vacuum degree of 150Pa for 72h, and finally the fiber blank is obtained after demolding.
5. The method according to claim 1, wherein the concentration of the dilute aqueous nitric acid solution in step two ① is 1 mol/L.
6. The method for preparing the mullite porous graded fibrous material as claimed in claim 1, wherein the aluminum sol obtained in the step two ① and the silica sol obtained in the step two ② are mixed in the step two ③, then the mixture is added with a catalyst, and the mixture is stirred for 12 hours to obtain an active slurry, wherein the catalyst is aluminum fluoride powder, the molar ratio of aluminum elements in the catalyst to aluminum elements in the aluminum sol is 3:7, and the molar ratio of the aluminum elements to the silicon elements in the active slurry is 3: 1.2.
7. The method for preparing the mullite porous graded fibrous material according to claim 1, wherein the step four is to put the injected fiber blank into a refrigerator, freeze the fiber blank at a temperature of 18 ℃ below zero until the fiber blank is completely frozen, put the sample into a freeze dryer, freeze-dry the sample for 72 hours at 50 ℃ below zero and under a vacuum degree of 150Pa, and take out the sample to obtain a graded sample blank.
8. The method for preparing the mullite porous graded fibrous material according to claim 1, wherein in the fifth step, the graded sample blank prepared in the fourth step is placed in a crucible, the crucible is covered by a cover, then the crucible is placed in a muffle furnace, the temperature is raised to 1000 ℃ from room temperature at the heating rate of 3 ℃/min under the air atmosphere, the temperature is kept for 2h at 1000 ℃, and then the mullite porous graded fibrous material is obtained after furnace cooling.
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