CN110156447A - The preparation method of hollow mullite heat insulation fiber - Google Patents
The preparation method of hollow mullite heat insulation fiber Download PDFInfo
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- CN110156447A CN110156447A CN201910461581.1A CN201910461581A CN110156447A CN 110156447 A CN110156447 A CN 110156447A CN 201910461581 A CN201910461581 A CN 201910461581A CN 110156447 A CN110156447 A CN 110156447A
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- mullite
- aluminium salt
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B35/16—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 silicates other than clay
- C04B35/18—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 silicates other than clay rich in aluminium oxide
- C04B35/185—Mullite 3Al2O3-2SiO2
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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
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/62227—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres
- C04B35/62231—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres based on oxide ceramics
- C04B35/6224—Fibres based on silica
- C04B35/62245—Fibres based on silica rich in aluminium oxide
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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
- C04B2235/6562—Heating rate
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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
- C04B2235/6567—Treatment time
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- C—CHEMISTRY; METALLURGY
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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
- C04B2235/9607—Thermal properties, e.g. thermal expansion coefficient
Abstract
The invention discloses a kind of preparation methods of hollow mullite heat insulation fiber.Aluminium salt and ethyl orthosilicate are first dissolved in dehydrated alcohol by the method is made dipping solution, then bombax cotton is immersed in solution, takes out, extracts and dry, be finally placed under aerobic atmosphere and be sintered, and the mullite fiber of hollow structure is made.Present invention process is simple, stablizes, and the fibre density of preparation is low, degree of hollowness is high, thermal insulation fire-resistant is functional, reduces by 20% compared with traditional solid mullite shape fiber thermal conductivity, is suitable for heat-barrier material field.
Description
Technical field
The invention belongs to technical field of fire-resistant material preparation, are related to a kind of heat-insulated using the hollow mullite of bombax cotton acquisition
The method of fiber.
Background technique
Mullite fiber is a kind of excellent Ultralight high-temperature resistant thermal insulating material, have corrosion-resistant, specific gravity is small, fusing point is high,
The advantages that good thermal shock, thermal conductivity are low and elevated temperature strength is big is widely used in metallurgy, machinery, ceramics, electronics, building materials, stone
(it is inorganic that Li Chengshun, Zhang Yujun, Zhang Jingde sol-gal process prepare polycrystalline mullite fibre [J] in the fields such as change, space flight and aviation
Material journal, 2009,24 (4): 848-852.).Mullite fiber used at present is mostly solid fibre, and thermal coefficient is
0.25w/mk (polycrystalline mullite fibre).The existing method for preparing mullite fiber has sol-gal process, and (Zhang Yabin waits
Sol-gal process prepares technical study [J] artificial lens journal of continuous mullite fiber, 2009 (s1): 203-206.)；It is non-
Solution spinning method (Xiao Z, Mitchell B S.The production ofmullite fibers via inviscid
Melt spinning (IMS) [J] .Materials Letters, 1998,37 (6): 359365).Other methods (Qiao Jian,
Liu and Yi, Cui Hongliang wait mullite fiber preparation method summary [J] silicate notification, 2014,33 (12): 3230-
3234.).Existing method preparation mullite fiber be generally it is solid, in practical applications, this mullite fiber exposes
One problem: the fiber of solid construction is difficult to further decrease density and heat-proof quality.Therefore the heat insulation of mullite fiber
It is difficult further to be promoted.
Summary of the invention
The object of the present invention is to provide a kind of using bombax cotton preparation density is low, degree of hollowness is high, thermal insulation property is good
The method of hollow mullite heat insulation fiber.
The technical solution achieved the object of the present invention is as follows:
The method for obtaining hollow mullite heat insulation fiber using bombax cotton, the specific steps are as follows:
Step 1, it is 5~20:100 by the mass ratio of aluminium salt and dehydrated alcohol, aluminium salt, ethyl orthosilicate is dissolved in anhydrous second
In alcohol, dipping solution is obtained；
Step 2, bombax cotton is immersed in dipping solution, takes out, extracts and dries；
Step 3, bombax cotton step 2 obtained is warming up to 1200~1300 DEG C of sintering, sintering knot under aerobic atmosphere
Hollow mullite heat insulation fiber is made in Shu Hou, furnace cooling.
Preferably, in step 1, the aluminium salt is nine water aluminum nitrates, and the molar ratio of aluminium salt and ethyl orthosilicate is 3:1.
Preferably, in step 1, the mass ratio of the aluminium salt and dehydrated alcohol is 10 ± 1:100.
Preferably, in step 2, the soaking time is 3~5min.
Preferably, described to have oxygen atmosphere for air or pure oxygen atmosphere in step 3.
Preferably, in step 3, the heating rate is 5~20 DEG C/min.
Preferably, in step 3, the sintered heat insulating time is 1h.
Compared with prior art, the present invention having the advantage that
Hollow mullite heat insulation fiber prepared by the present invention is compared with traditional solid mullite fiber, under 300 DEG C of hot faces, heat
Conductance reduces 20%.
Detailed description of the invention
Fig. 1 is mullite fiber X ray diffracting spectrum obtained in embodiment 1.
Fig. 2 is that mullite fiber SEM obtained is low in embodiment 1, high magnification micro-structure diagram.
Fig. 3 is mullite fiber X ray diffracting spectrum obtained in embodiment 2.
Fig. 4 is that mullite fiber SEM obtained is low in embodiment 2, high magnification micro-structure diagram.
Fig. 5 is that mullite fiber SEM obtained is low in embodiment 3, high magnification micro-structure diagram.
Specific embodiment
Below with reference to embodiment and attached drawing, present invention is further described in detail.
The present invention utilizes the hollow feature of bombax cotton, and the ethyl alcohol that bombax cotton is immersed in aluminium salt and ethyl orthosilicate is molten
In liquid.In dipping process, solute is immersed with solution and is stayed in fiber tube wall, is extracted after taking out fiber, is placed in horse after drying
Not it is sintered in furnace.As the temperature rises, aluminium, silicon, oxygen atom phase counterdiffusion generate mullite (3Al through solid-state phase changes2O3·
2SiO2) crystal.Bombax cotton combustion decomposition, the mullite crystal of generation remains the hollow structure of fiber, therefore is sintered and completes
Afterwards, the mullite fiber with hollow structure is obtained.Mullite heat insulation fiber prepared by the present invention is in hollow form, relative to reality
Core fiber density is lower.For heat-proof quality, the thermal conductivity of inside hollow fibre air is extremely low, and overall thermal convective heat transfer
Difference, therefore be obviously improved relative to traditional solid fibrous thermal performance.
It is different that mullite is prepared from conventional sintering, it is other uniform that the method for the present invention guarantees that aluminium silicon atom be in molecular level,
Therefore the mullite purity theoretically prepared is higher.The technique is similar to infusion process, is a kind of side of new mullite synthesizing
Method.
The present invention makees template using bombax cotton, compared to other plant template (as slightly melon, Calotropis gigantea, Yang Xu, cattail
Suede, Chinese parasol tree tree hair etc.) there is apparent advantage.Said from materials, kapok be a kind of most common heat insulating material, annual output compared with
Greatly, industrialized production needs can be met.From fibre property, bombax cotton is more elongated, and degree of hollowness is in known doughnut
It is highest and whole fluffy unordered, it is a kind of heat insulating material that heat-proof quality is excellent.With existing using in similar method preparation
Empty ceramic phase ratio, hollow mullite fiber cost of material prepared by the present invention is lower, and application prospect is wider.In addition, mullite is high
Warm mechanical property is better than aluminium oxide, and thermal shock resistance is better than zirconium oxide, and general performance is excellent.
Embodiment 1 (5:100)
The ethyl orthosilicate of the nine water aluminum nitrates and 0.32g that take 1.76g is dissolved in the ethanol solution of 20ml.It will be wooden
Cotton fiber immerse solution in, impregnate 1min after extract, after by 80 DEG C of fiber dry.By the bombax cotton after drying with 5 DEG C/min
Heating rate rise to 1200 DEG C, keep the temperature 1h, hollow mullite fiber be made.The XRD object phase that Fig. 1 is obtained at this temperature；Fig. 2 a,
For doughnut under the concentration, low, high magnification SEM schemes 2b.From Fig. 2 a, 2b as can be seen that since impregnation concentrations are too low, fiber
Tube wall is relatively thin and has part to curl contraction, and dipping effect is unsatisfactory.
Embodiment 2 (10:100)
The ethyl orthosilicate of the nine water aluminum nitrates and 0.64g that take 3.52g is dissolved in the ethanol solution of 20ml.It will be wooden
Cotton fiber immerse solution in, impregnate 1min after extract, after by 80 DEG C of fiber dry.By the bombax cotton after drying with 5 DEG C/min
Heating rate rise to 1200 DEG C, keep the temperature 1h, hollow mullite fiber be made.Fig. 3 a, 3b are that doughnut is low, high under the concentration
Multiplying power SEM figure.Mullite fiber is low under concentration thus by Fig. 3, high magnification photo.The hollow mullite fiber of the concentration is at 300 DEG C
Under thermal coefficient be 0.19W/ (mK), improve 20% compared with traditional solid mullite.From figure 3, it can be seen that the dipping
Moderate concentration, fibre pipe degree of hollowness is higher and whole fluffy unordered, and mullite fiber has been effectively maintained the pattern of bombax cotton.
Embodiment 3 (20:100)
The ethyl orthosilicate of the nine water aluminum nitrates and 1.30g that take 7.04g is dissolved in the dehydrated alcohol volume fraction of 20ml
In alcoholic solution.Bombax cotton is immersed in solution, is extracted after impregnating 1min, drying is taken out；By the bombax cotton after drying with 5
DEG C/heating rate of min rises to 1300 DEG C, 1h is kept the temperature, hollow mullite fiber is made.Fig. 4 is object phasor at this temperature；Figure
5a, 5b are low under this condition, high magnification SEM figure.It can be seen from the figure that the existing part of mullite fiber is viscous when 20% concentration
Even, fiber tube wall is also thicker, and impregnation concentrations are no more than 20% when practical application.
Claims (7)
1. the preparation method of hollow mullite heat insulation fiber, which is characterized in that specific step is as follows:
Step 1, it is 5~20:100 by the mass ratio of aluminium salt and dehydrated alcohol, aluminium salt, ethyl orthosilicate is dissolved in dehydrated alcohol
In, obtain dipping solution；
Step 2, bombax cotton is immersed in dipping solution, takes out, extracts and dries；
Step 3, bombax cotton step 2 obtained is warming up to 1200~1300 DEG C of sintering, sintering terminates under aerobic atmosphere
Afterwards, hollow mullite heat insulation fiber is made in furnace cooling.
2. preparation method according to claim 1, which is characterized in that in step 1, the aluminium salt is nine water aluminum nitrates,
Aluminium salt and the molar ratio of ethyl orthosilicate are 3:1.
3. preparation method according to claim 1, which is characterized in that in step 1, the matter of the aluminium salt and dehydrated alcohol
Amount is than being 10 ± 1:100.
4. preparation method according to claim 1, which is characterized in that in step 2, the soaking time is 3~5min.
5. preparation method according to claim 1, which is characterized in that described to have oxygen atmosphere for air or pure oxygen in step 3
Gas atmosphere.
6. preparation method according to claim 1, which is characterized in that in step 3, the heating rate be 5~20 DEG C/
min。
7. preparation method according to claim 1, which is characterized in that in step 3, the sintered heat insulating time is 1h.
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| CN201910461581.1A CN110156447A (en) | 2019-05-30 | 2019-05-30 | The preparation method of hollow mullite heat insulation fiber |
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| CN201910461581.1A CN110156447A (en) | 2019-05-30 | 2019-05-30 | The preparation method of hollow mullite heat insulation fiber |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112174690A (en) * | 2020-10-12 | 2021-01-05 | 南京理工大学 | Method for preparing hollow aluminum titanate fiber by using kapok fiber |
| CN112661522A (en) * | 2021-01-12 | 2021-04-16 | 南京理工大学 | Method for improving filling power of ceramic fiber prepared by template method |
| CN113775855A (en) * | 2021-08-06 | 2021-12-10 | 华南理工大学 | Kapok fiber vacuum insulation panel core material and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105536559A (en) * | 2015-12-28 | 2016-05-04 | 中国科学院城市环境研究所 | Mullite ceramic hollow fiber membrane and preparation method for same |
| CN106350899A (en) * | 2016-08-24 | 2017-01-25 | 南京理工大学 | Preparation method for hollow aluminum oxide fiber |
-
2019
- 2019-05-30 CN CN201910461581.1A patent/CN110156447A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105536559A (en) * | 2015-12-28 | 2016-05-04 | 中国科学院城市环境研究所 | Mullite ceramic hollow fiber membrane and preparation method for same |
| CN106350899A (en) * | 2016-08-24 | 2017-01-25 | 南京理工大学 | Preparation method for hollow aluminum oxide fiber |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112174690A (en) * | 2020-10-12 | 2021-01-05 | 南京理工大学 | Method for preparing hollow aluminum titanate fiber by using kapok fiber |
| CN112661522A (en) * | 2021-01-12 | 2021-04-16 | 南京理工大学 | Method for improving filling power of ceramic fiber prepared by template method |
| CN113775855A (en) * | 2021-08-06 | 2021-12-10 | 华南理工大学 | Kapok fiber vacuum insulation panel core material and preparation method and application thereof |
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