CN111270411B - Preparation method of alumina fiber blanket - Google Patents

Preparation method of alumina fiber blanket Download PDF

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Publication number
CN111270411B
CN111270411B CN202010263985.2A CN202010263985A CN111270411B CN 111270411 B CN111270411 B CN 111270411B CN 202010263985 A CN202010263985 A CN 202010263985A CN 111270411 B CN111270411 B CN 111270411B
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fiber
blank
temperature
precursor fiber
blanket
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CN111270411A (en
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李梅
岳耀辉
鹿明
李传勇
王成龙
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Shandong Luyang Hot High Technology Ceramic Fiber Co
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Shandong Luyang Hot High Technology Ceramic Fiber Co
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    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
    • D04H1/4209—Inorganic fibres
    • C—CHEMISTRY; METALLURGY
    • 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
    • C04B35/14—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
    • C—CHEMISTRY; METALLURGY
    • 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
    • C04B35/622—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
    • C04B35/62236—Fibres based on aluminium oxide
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/44—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties the fleeces or layers being consolidated by mechanical means, e.g. by rolling
    • D04H1/46—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties the fleeces or layers being consolidated by mechanical means, e.g. by rolling by needling or like operations to cause entanglement of fibres

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Inorganic Chemistry (AREA)
  • Textile Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Inorganic Fibers (AREA)

Abstract

The invention belongs to the technical field of refractory materials, and particularly relates to a preparation method of an alumina fiber blanket, which comprises the following steps: a) forming fibers from a spinning stock solution containing an aluminum source and a silicon source, and collecting cotton from obtained fiber yarns to obtain a precursor fiber blank with the water content of 5-35%; b) sequentially maintaining and needling the precursor fiber blank to obtain a precursor fiber blanket blank; the curing temperature is 30-200 ℃, the equivalent relative humidity is 20-90 RH%, and the time is 10-60 min; c) and carrying out heat treatment on the precursor fiber blanket blank to obtain the alumina fiber blanket. According to the method provided by the invention, the precursor fiber with specific water content is subjected to maintenance treatment at specific temperature and humidity, so that the fiber has higher strength and the resistance between the fiber is reduced under the condition of ensuring the water content in the fiber, and thus, the needling, interweaving and shaping of the precursor fiber blank into the carpet can be realized under the condition of not adding any lubricating grease.

Description

Preparation method of alumina fiber blanket
Technical Field
The invention belongs to the technical field of refractory materials, and particularly relates to a preparation method of an alumina fiber blanket.
Background
The alumina fiber is a super-light, heat-insulating, energy-saving and fireproof fibrous material which is formed by spinning through a sol-gel chemical method and is converted into a mullite phase as a main crystal phase through high-temperature calcination, and the main component of the alumina fiber is A12O3Containing a small amount of SiO2The maximum service temperature is 1600 ℃, and the long-term service temperature is 1300-1500 ℃. The alumina fiber can be processed into different types of products according to the use requirements, and comprises: alumina fiber cotton, alumina fiber needled blanket, alumina fiber module, alumina fiber liner, alumina fiber board, etc. The alumina fiber needled blanket is prepared by needling a fiber precursor prepared by spinning and forming fibers through a needling process, interweaving and shaping the fibers, and then drying and calcining. By self-crossing between fibresThe high-strength high-resilience high-temperature-resistant sealing material still has high strength, chemical stability and resilience at high temperature, and is widely applied to the fields of high-temperature industrial kilns, high-temperature sealing of automobile exhaust, military aerospace and the like.
The production process of the alumina fiber needle-punched carpet is complex and comprises a plurality of processes of spinning solution preparation, fiber forming, needle punching, drying, calcination and the like. The spinning solution containing the aluminum source and the silicon source is subjected to centrifugal spinning or blowing spinning technology to instantly finish dispersion and drying, and the prepared fiber has relatively poor strength, is influenced by a plurality of parameters, has large fluctuation and is difficult to directly needle into a blanket.
In the production process of the traditional ceramic fiber needled blanket, in order to reduce the needling resistance of a fiber blank, reduce the abrasion of felting needles and realize fiber interweaving into the blanket, a certain amount of organic lubricating grease needs to be added while forming fiber, but the method has two problems: firstly, the lubricating grease can generate tar under the action of high temperature, the tar is gathered on cotton collecting equipment and an induced draft pipeline, the danger of fire hazard is accumulated for a long time, and the potential safety hazard during production is increased; secondly, organic waste gas (VOCs) is generated in the high-temperature treatment process of the organic lubricating grease, so that environmental pollution is caused.
Disclosure of Invention
In view of the above, the present invention provides a method for preparing an alumina fiber blanket, which can be used to needle-punch a precursor fiber blank into a blanket without adding grease, and has low environmental pollution and high production safety.
The invention provides a preparation method of an alumina fiber blanket, which comprises the following steps:
a) forming fibers from a spinning stock solution containing an aluminum source and a silicon source, and collecting cotton from obtained fiber yarns to obtain a precursor fiber blank with the water content of 5-35%;
b) sequentially maintaining and needling the precursor fiber blank to obtain a precursor fiber blanket blank;
the curing temperature is 30-200 ℃; the equivalent humidity of the maintenance is 20-90 RH%; the curing time is 10-60 min;
c) and carrying out heat treatment on the precursor fiber blanket blank to obtain the alumina fiber blanket.
Preferably, in step a), the spinning solution is prepared according to the following steps:
i) mixing and heating aluminum powder, acid and water for reaction to obtain aluminum sol;
ii) mixing the aluminum sol, the acidic silica sol and the water-soluble polymer spinning aid to obtain a spinning solution.
Preferably, the water-soluble polymer spinning aid comprises one or more of polyvinylpyrrolidone, polyvinyl alcohol, polyethylene oxide, syrup, starch and cellulose.
Preferably, in the step a), the viscosity of the spinning solution at 50 ℃ is 500-2000 cP.
Preferably, in step a), the fiber forming manner is blow spinning or centrifugal spinning.
Preferably, in the step a), the temperature of the cotton collection is 30-100 ℃; the relative humidity of the cotton collection is 5-40 RH%.
Preferably, in the step a), the thickness of the precursor fiber blank is 100-400 mm; the surface density of the precursor fiber blank is 0.5-3 kg/m2。
Preferably, in the step b), the needling density is 1-50 needles/cm2。
Preferably, the step c) specifically comprises:
sequentially carrying out heat treatment on the precursor fiber blanket blank in a low-temperature area, a medium-temperature area and a high-temperature area of a heating furnace to obtain an aluminum oxide fiber blanket;
in the heat treatment process, the temperature of the low-temperature zone of the heating furnace is 0-600 ℃, the temperature of the medium-temperature zone is 600-1100 ℃, and the temperature of the high-temperature zone is 1100-1300 ℃.
Preferably, the air displacement of the low-temperature area of the heating furnace in the heat treatment process is set to be 1-2 Nm3/kg/h。
Compared with the prior art, the invention provides a preparation method of an alumina fiber blanket. The preparation method provided by the invention comprises the following steps: a) forming fibers from a spinning stock solution containing an aluminum source and a silicon source, and collecting cotton from obtained fiber yarns to obtain a precursor fiber blank with the water content of 5-35%; b) sequentially maintaining and needling the precursor fiber blank to obtain a precursor fiber blanket blank; the curing temperature is 30-200 ℃; the equivalent humidity of the maintenance is 20-90 RH%; the curing time is 10-60 min; c) and carrying out heat treatment on the precursor fiber blanket blank to obtain the alumina fiber blanket. According to the preparation method provided by the invention, the precursor fiber with specific water content is maintained at specific temperature and humidity, so that the fiber has higher strength and the resistance between the fiber is reduced under the condition of ensuring the water content in the fiber, and thus, the precursor fiber blank can be needled and interwoven to form a blanket under the condition of not adding any lubricating grease, and further, the problems of fire hazard and environmental pollution caused by needling the blanket by adding organic lubricating grease are solved.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a preparation method of an alumina fiber blanket, which comprises the following steps:
a) forming fibers from a spinning stock solution containing an aluminum source and a silicon source, and collecting cotton from obtained fiber yarns to obtain a precursor fiber blank with the water content of 5-35%;
b) sequentially maintaining and needling the precursor fiber blank to obtain a precursor fiber blanket blank;
the curing temperature is 30-200 ℃; the equivalent humidity of the maintenance is 20-90 RH%; the curing time is 10-60 min;
c) and carrying out heat treatment on the precursor fiber blanket blank to obtain the alumina fiber blanket.
In the preparation method provided by the invention, firstly, a spinning solution containing an aluminum source and a silicon source is provided. The viscosity of the spinning solution at 50 ℃ is preferably 500-2000 cP, and specifically can be 500cP, 600cP, 700cP, 800cP, 900cP, 1000cP, 1100cP, 1200cP, 1300cP, 1400cP, 1500cP, 1600cP, 1700cP, 1800cP, 1900cP or 2000 cP. In the present invention, the spinning dope is preferably prepared according to the following steps:
i) mixing and heating aluminum powder, acid and water for reaction to obtain aluminum sol;
ii) mixing the aluminum sol, the acidic silica sol and the water-soluble polymer spinning aid to obtain a spinning solution.
In the above spinning dope preparation step provided by the present invention, in step i), the acid is preferably formic acid and acetic acid; the molar ratio of the aluminum powder, formic acid and acetic acid is preferably 1: (1-5): (1-5), specifically 1:3: 3; the molar ratio of the aluminum powder to water is preferably 1: (10-15), specifically 1: 13; the reaction temperature is preferably 90-100 ℃, and specifically can be 90 ℃, 91 ℃, 92 ℃, 93 ℃, 94 ℃, 95 ℃, 96 ℃, 97 ℃, 98 ℃, 99 ℃ or 100 ℃; the reaction time is preferably 6-20 h, and specifically can be 6h, 7h, 8h, 9h, 10h, 11h, 12h, 13h, 14h, 15h, 16h, 17h, 18h, 19h or 20 h.
In the spinning solution preparation step provided by the present invention, in step ii), the acidic silica sol is preferably a sodium-removed acidic silica sol, and the sodium-removed acidic silica sol is an acidic silica sol treated by a cation exchange resin; the content of the silica in the acidic silica sol is preferably 20-30 wt%, and specifically can be 20 wt%, 21 wt%, 22 wt%, 23 wt%, 24 wt%, 25 wt%, 26 wt%, 27 wt%, 28 wt%, 29 wt% or 30 wt%; the pH value of the acidic silica sol is preferably 3-4, and specifically can be 3, 3.5 or 4; the molar ratio of silica in the acidic silica sol to alumina in the aluminum sol is preferably 1: (2-5), specifically 1:2, 1:2.5, 1:3, 1:3.5, 1:4, 1:4.5 or 1: 5.
In the above spinning dope preparation step provided by the present invention, in step ii), the water-soluble polymer spinning aid preferably includes one or more of polyvinylpyrrolidone, polyvinyl alcohol, polyethylene oxide, syrup, starch, and cellulose; the polymerization degree of the polyvinyl alcohol is preferably 1000-3000, and specifically can be 2099. In the invention, the water-soluble polymer spinning aid is preferably mixed in the form of a water-soluble polymer spinning aid aqueous solution, and the concentration of the water-soluble polymer spinning aid aqueous solution is preferably 3-8 wt%, and specifically can be 3 wt%, 3.5 wt%, 4 wt%, 4.5 wt%, 5 wt%, 5.5 wt%, 6 wt%, 6.5 wt%, 7 wt%, 7.5 wt% or 8 wt%; the amount of the water-soluble polymer spinning aid aqueous solution is preferably 1 to 5 wt% of the total mass of the aluminum sol and the acidic silica sol, and specifically may be 1 wt%, 1.5 wt%, 2 wt%, 2.5 wt%, 3 wt%, 3.5 wt%, 4 wt%, 4.5 wt%, or 5 wt%.
In the above-mentioned spinning dope preparation step provided by the present invention, in the step ii), a certain amount of alcohol is preferably added to the mixed system. Wherein the alcohol is preferably ethanol and/or isobutanol; the amount of the alcohol added is preferably 0.05 to 1.5 wt%, specifically 0.05 wt%, 0.1 wt%, 0.2 wt%, 0.3 wt%, 0.4 wt%, 0.5 wt%, 0.7 wt%, 1 wt%, 1.2 wt%, or 1.5 wt%, based on the total mass of the aluminum sol and the acidic silica sol.
In the preparation step of the spinning solution provided by the invention, in the step ii), the materials are preferably concentrated after being uniformly mixed, so that the spinning solution with the required viscosity is obtained. Wherein the concentration mode is preferably vacuum concentration; the concentration temperature is preferably 50-60 deg.C, specifically 50 deg.C, 51 deg.C, 52 deg.C, 53 deg.C, 54 deg.C, 55 deg.C, 56 deg.C, 57 deg.C, 58 deg.C, 59 deg.C or 60 deg.C.
In the preparation method provided by the invention, after the spinning stock solution is obtained, the spinning stock solution is subjected to fiber forming. Wherein, the fiber forming mode is preferably blow spinning or centrifugal spinning; the rotating speed of a spinning disc of the centrifugal spinning is preferably 1000-5000 r/min, and specifically can be 1000r/min, 1500r/min, 2000r/min, 2500r/min, 3000r/min, 3500r/min, 4000r/min, 4500r/min or 5000 r/min; the drawing wind speed of the centrifugal spinning is preferably 15-30 m/s, and more preferably 20-25 m/s.
In the preparation method provided by the invention, after fiber is formed, the spinning dope forms fiber yarn,the filaments are then collected (i.e., collected and dried). Wherein, the temperature of the cotton collection is preferably 30-100 ℃, more preferably 40-80 ℃, and specifically can be 40 ℃, 45 ℃, 50 ℃, 55 ℃, 60 ℃, 65 ℃, 70 ℃, 75 ℃ or 80 ℃; the relative humidity of the cotton-gathering is preferably 5-40 RH%, more preferably 10-20 RH%, and specifically may be 10 RH%, 11 RH%, 12 RH%, 13 RH%, 14 RH%, 15 RH%, 16 RH%, 17 RH%, 18 RH%, 19 RH% or 20 RH%. After cotton collection is finished, a precursor fiber blank is obtained, wherein the thickness of the precursor fiber blank is preferably 100-400 mm, and specifically can be 100mm, 150mm, 200mm, 250mm, 300mm, 350mm or 400 mm; the preferred surface density of the precursor fiber blank is 0.5-3 kg/m2Specifically, it may be 0.5kg/m2、0.6kg/m2、0.7kg/m2、0.8kg/m2、0.9kg/m2、1kg/m2、1.05kg/m2、1.1kg/m2、1.2kg/m2、1.3kg/m2、1.4kg/m2、1.5kg/m2、1.7kg/m2、2kg/m2、2.05kg/m2、2.5kg/m2Or 3kg/m2(ii) a The moisture content of the precursor fiber blank is 5-35%, preferably 10-30%, more preferably 18-25%, and specifically 18%, 19%, 20%, 21%, 22%, 23%, 24% or 25%. According to the invention, the precursor fiber blank can be sticky when the moisture content is too high, and brittle failure can be generated when the moisture content is too low, and the precursor fiber blank can have better strength due to proper moisture content.
In the preparation method provided by the invention, after the precursor fiber blank is obtained, the precursor fiber blank is maintained. Wherein the curing temperature is 30-200 ℃, preferably 50-150 ℃, more preferably 80-120 ℃, and specifically can be 80 ℃, 85 ℃, 90 ℃, 95 ℃, 100 ℃, 105 ℃, 110 ℃, 115 ℃ or 120 ℃; the relative humidity of the curing is 20-90 RH%, preferably 30-60 RH%, more preferably 30-50 RH%, specifically 30 RH%, 32 RH%, 35 RH%, 37 RH%, 40 RH%, 42 RH%, 45 RH%, 47 RH% or 50 RH%; the curing time is 10-60 min, preferably 10-30 min, and specifically 10min, 13min, 15min, 17min, 20min, 23min, 25min, 27min or 30 min. In the invention, the spinning aid on the surface of the fiber can be further dried and shrunk to form a film through maintenance treatment, so that the flexibility of the fiber is improved, and the strength of the fiber is increased; meanwhile, the surface of the fiber can be further dried, the surface is smoother, the needling resistance is reduced, and the interweaving among fibers during needling is realized.
In the preparation method provided by the invention, after the maintenance is finished, needling is carried out on the precursor fiber blank after the maintenance. Wherein the needling density is preferably 1-50 needles/cm2More preferably 5 to 40 needles/cm2Most preferably 8 to 35 needles/cm2Specifically, it can be 8 needles/cm29 needles/cm210 needles/cm211 needles/cm212 needles/cm213 needles/cm214 needles/cm215 needles/cm216 needles/cm217 needles/cm218 needles/cm219 needles/cm220 needles/cm221 needles/cm222 needles/cm223 needles/cm224 needles/cm225 needles/cm226 needles/cm227 needles/cm228 needles/cm229 needles/cm230 needles/cm231 needles/cm232 needles/cm233 needles/cm234 needles/cm2Or 35 needles/cm2. And after the needling is finished, obtaining a precursor fiber blanket blank, wherein the thickness of the precursor fiber blanket blank is preferably 10-50 mm, and specifically can be 1mm, 15mm, 17mm, 20mm, 25mm, 30mm, 35mm, 40mm, 45mm or 50 mm.
In the preparation method provided by the present invention, after obtaining the precursor fiber blanket blank, the precursor fiber blanket blank is subjected to a heat treatment, and the specific process preferably includes: and carrying out heat treatment on the precursor fiber blanket blank in a low-temperature area, a medium-temperature area and a high-temperature area of a heating furnace in sequence. In the heat treatment process, the temperature of the low-temperature area is 0-600 ℃, and preferably 80-600 ℃; the temperature of the medium temperature zone is 600-1100 ℃, and preferably 700-1100 ℃; the temperature of the high-temperature area is 1100-1300 ℃, and specifically 1250 ℃; the exhaust volume of the low-temperature zone is preferably 1-2 Nm3A/kg/h, in particular 1.5Nm3The ratio of the water to the oil is/kg/h. In the present inventionThe heat treatment time of the precursor fiber blanket blank in the low-temperature zone is preferably 90-150 min, and specifically may be 90min, 100min, 110min, 120min, 130min, 140min or 150 min; the heat treatment time in the middle temperature zone is preferably 60-120 min, and specifically can be 60min, 70min, 80min, 90min, 100min, 110min or 120 min; the heat treatment time in the high-temperature zone is preferably 30-90 min, and specifically can be 30min, 40min, 50min, 60min, 70min, 80min or 90 min. And (4) after the precursor fiber blanket is subjected to heat treatment, obtaining the alumina fiber blanket.
According to the preparation method provided by the invention, the precursor fiber with specific water content is maintained at specific temperature and humidity, so that the fiber has higher strength and the resistance between the fiber is reduced under the condition of ensuring the water content in the fiber, and thus, the precursor fiber blank can be needled and interwoven to form a blanket under the condition of not adding any lubricating grease, and further, the problems of fire hazard and environmental pollution caused by needling the blanket by adding organic lubricating grease are solved.
For the sake of clarity, the following examples are given in detail.
Example 1
Dissolving aluminum powder in a mixture of formic acid and acetic acid, adding deionized water, heating and refluxing at the reflux temperature of 95 ℃ for 9 hours to prepare mixed sol of aluminum formate and aluminum acetate, and filtering to remove impurities; wherein the molar ratio of the aluminum powder, the formic acid, the acetic acid and the water is 1:3:3: 13. In the mixed sol of aluminum formate and aluminum acetate, according to Al2O3/SiO2Adding sodium-removed acidic silica sol with the molar ratio of 3:1, wherein the sodium-removed acidic silica sol contains 25% of silica by mass and has a pH value of 4; after being uniformly mixed, mixed liquid is obtained; adding a polyvinyl alcohol aqueous solution with the concentration of 5 wt% into the mixed solution, wherein the polymerization degree of the polyvinyl alcohol is 2099, and the adding amount of the polyvinyl alcohol aqueous solution is 3% of the mass of the mixed solution; then adding ethanol with the addition amount of 1.0 percent of the mass of the mixed solution, and carrying out vacuum concentration at 60 ℃ to prepare a spinning solution with the viscosity of 2000cP at 50 ℃.
Spinning the aboveForming fiber by using a centrifugal spinning device, wherein the spinning disc rotates at 3000r/min, the drawing wind speed is 20-25 m/s, the temperature of a cotton collecting chamber is controlled at 50 +/-2 ℃, the relative humidity is controlled at 15 +/-2 RH%, and the silk stock solution with the water content of 20 wt%, the thickness of 150mm and the surface density of 1.05kg/m is obtained2The alumina fiber precursor cotton blank.
Maintaining the above alumina fiber precursor cotton blank at 100 deg.C and 45 RH% for 10min, and needling with needling density of 10 needles/cm into blanket2And preparing an alumina fiber precursor blanket blank with the thickness of 17 mm.
Conveying the alumina fiber precursor blanket blank into a blanket heating furnace, and carrying out heat treatment in a low-temperature area, a medium-temperature area and a high-temperature area of the heating furnace in sequence, wherein the temperature of the low-temperature area is 80-600 ℃, the heat treatment time is 120min, and the air exhaust amount is 1.5 Nm/min per kg of precursor fiber exhaust gas3(ii) a The temperature of the medium temperature zone is 700-1100 ℃, and the heat treatment time is 90 min; the heat treatment temperature of the high-temperature zone is 1250 ℃, and the heat treatment time is 60 min. After the heat treatment, the obtained steel sheet had a thickness of 12.5mm and a volume weight of 96kg/m2And the tensile strength of the alumina fiber blanket is 0.08 MPa.
Example 2
Dissolving aluminum powder in a mixture of formic acid and acetic acid, adding deionized water, heating and refluxing at the reflux temperature of 95 ℃ for 9 hours to prepare mixed sol of aluminum formate and aluminum acetate, and filtering to remove impurities; wherein the molar ratio of the aluminum powder, the formic acid, the acetic acid and the water is 1:3:3: 13. In the mixed sol of aluminum formate and aluminum acetate, according to Al2O3/SiO2Adding sodium-removed acidic silica sol with the molar ratio of 3:1, wherein the sodium-removed acidic silica sol contains 25% of silica by mass and has a pH value of 4; after being uniformly mixed, mixed liquid is obtained; adding a polyvinyl alcohol aqueous solution with the concentration of 5 wt% into the mixed solution, wherein the polymerization degree of the polyvinyl alcohol is 2099, and the adding amount of the polyvinyl alcohol aqueous solution is 3% of the mass of the mixed solution; then adding ethanol with the addition amount of 1.0 percent of the mass of the mixed solution, and carrying out vacuum concentration at 60 ℃ to prepare a spinning solution with the viscosity of 2000cP at 50 ℃.
Will be at the topThe spinning solution is formed into fibers by using a centrifugal spinning device, the rotating speed of a spinning disc is 3000r/min, the wind speed of traction wind is 20-25 m/s, the temperature of a cotton collecting chamber is controlled at 55 +/-2 ℃, the relative humidity is controlled at 13 +/-2 RH%, and the spinning solution with the water content of 18 wt%, the thickness of 200mm and the surface density of 1.40kg/m is obtained2The alumina fiber precursor cotton blank.
Maintaining the above alumina fiber precursor cotton blank at 100 deg.C and 45 RH% for 13min, and needling with a needling density of 15 needles/cm into blanket2And preparing an alumina fiber precursor blanket blank with the thickness of 17 mm.
Conveying the alumina fiber precursor blanket blank into a blanket heating furnace, and carrying out heat treatment in a low-temperature area, a medium-temperature area and a high-temperature area of the heating furnace in sequence, wherein the temperature of the low-temperature area is 80-600 ℃, the heat treatment time is 120min, and the air exhaust amount is 1.5 Nm/min per kg of precursor fiber exhaust gas3(ii) a The temperature of the medium temperature zone is 700-1100 ℃, and the heat treatment time is 90 min; the heat treatment temperature of the high-temperature zone is 1250 ℃, and the heat treatment time is 60 min. After the heat treatment, the thickness was 12.5mm and the volume weight was 128kg/m2And the tensile strength of the alumina fiber blanket is 0.12 MPa.
Example 3
Dissolving aluminum powder in a mixture of formic acid and acetic acid, adding deionized water, heating and refluxing at the reflux temperature of 95 ℃ for 9 hours to prepare mixed sol of aluminum formate and aluminum acetate, and filtering to remove impurities; wherein the molar ratio of the aluminum powder to the formic acid to the acetic acid to the water is 1:3:3: 13. In the mixed sol of aluminum formate and aluminum acetate, according to Al2O3/SiO2Adding sodium-removed acidic silica sol with the molar ratio of 3:1, wherein the sodium-removed acidic silica sol contains 25% of silica by mass and has a pH value of 4; after being uniformly mixed, mixed liquid is obtained; adding a polyvinyl alcohol aqueous solution with the concentration of 5 wt% into the mixed solution, wherein the polymerization degree of the polyvinyl alcohol is 2099, and the adding amount of the polyvinyl alcohol aqueous solution is 3% of the mass of the mixed solution; then adding ethanol with the addition amount of 1.0 percent of the mass of the mixed solution, and carrying out vacuum concentration at 60 ℃ to prepare a spinning solution with the viscosity of 2000cP at 50 ℃.
The spinning stock solution is subjected to fiber forming by using a centrifugal spinning device, the rotating speed of a spinning disc is 3000r/min, the wind speed of traction wind is 20-25 m/s, the temperature of a cotton collecting chamber is controlled at 45 +/-2 ℃, the relative humidity is controlled at 20 +/-2 RH%, and the spinning stock solution with the water content of 23 wt%, the thickness of 300mm and the surface density of 2.05kg/m is obtained2The alumina fiber precursor cotton blank.
Maintaining the above alumina fiber precursor cotton blank at 80 deg.C and 45 RH% for 20min, and needling with needling density of 10 needles/cm into blanket2And preparing an alumina fiber precursor blanket blank with the thickness of 35 mm.
Conveying the alumina fiber precursor blanket blank into a blanket heating furnace for heat treatment, and sequentially carrying out heat treatment in a low-temperature area, a medium-temperature area and a high-temperature area of the heating furnace, wherein the temperature in the low-temperature area is 80-600 ℃, the heat treatment time is 120min, and the air exhaust amount is 1.5 Nm/min per kg of precursor fiber exhaust gas3(ii) a The temperature of the medium temperature zone is 700-1100 ℃, and the heat treatment time is 90 min; the heat treatment temperature of the high-temperature zone is 1250 ℃, and the heat treatment time is 60 min. After the heat treatment, the thickness was 25mm and the volume weight was 96kg/m2And the tensile strength of the alumina fiber blanket is 0.08 MPa.
The fiber diameter, tensile strength and water content of the alumina fiber precursor cotton blanks prepared in examples 1 to 3 before and after curing treatment were measured, and the results are shown in table 1:
table 1 performance parameters before and after curing treatment of the alumina fiber precursor cotton blanks of examples 1 to 3.
Figure BDA0002440522610000091
Comparative example 1
The precursor fiber cotton blank with the water content of 20 wt% is prepared by the same method as the example 1, and is sent into a needle loom to be needled into a blanket without high-temperature environmental curing treatment, wherein the needling density is 15 needles/cm2There is no interweaving between the fibers, and the carpet cannot be formed.
Comparative example 2
The same as in example 1 was usedThe method comprises preparing precursor fiber cotton blank with water content of 20 wt%, maintaining at 150 deg.C and humidity of 10 RH% for 10min, and feeding into needle machine for needling with needling density of 15 needles/cm2There is no interweaving between the fibers, and the carpet cannot be formed.
Comparative example 3
The same method as that of example 1 is adopted to prepare spinning solution, centrifugal spinning is utilized to form fibers, the temperature of a cotton collecting chamber is controlled to be 65 +/-2 ℃, the relative humidity is controlled to be 8 +/-2 RH percent, and the spinning solution with the water content of 10wt percent, the thickness of 200mm and the surface density of 1.30kg/m is obtained2The alumina fiber precursor cotton blank.
Maintaining the above alumina fiber precursor cotton blank at 100 deg.C and 45 RH% for 13min, and needling with a needling density of 15 needles/cm into blanket2There is no interweaving between the fibers, and the carpet cannot be formed.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.

Claims (10)

1. A preparation method of an alumina fiber blanket comprises the following steps:
a) forming fibers from a spinning stock solution containing an aluminum source and a silicon source, and collecting cotton from obtained fiber yarns to obtain a precursor fiber blank with the water content of 10-30%;
b) sequentially maintaining and needling the precursor fiber blank to obtain a precursor fiber blanket blank;
the curing temperature is 80-120 ℃; the relative humidity of the maintenance is 30-50 RH%; the curing time is 10-30 min;
c) and carrying out heat treatment on the precursor fiber blanket blank to obtain the alumina fiber blanket.
2. The method according to claim 1, wherein the dope is prepared in step a) by the following steps:
i) mixing and heating aluminum powder, acid and water for reaction to obtain aluminum sol;
ii) mixing the aluminum sol, the acidic silica sol and the water-soluble polymer spinning aid to obtain a spinning solution.
3. The method according to claim 2, wherein the water-soluble polymer spinning aid comprises one or more of polyvinylpyrrolidone, polyvinyl alcohol, polyethylene oxide, syrup, starch and cellulose.
4. The method according to claim 1, wherein the viscosity of the dope at 50 ℃ in the step a) is 500 to 2000 cP.
5. The method according to claim 1, wherein the fiber forming in step a) is performed by blow spinning or centrifugal spinning.
6. The preparation method according to claim 1, wherein in the step a), the temperature of the cotton collection is 30-100 ℃; the relative humidity of the cotton collection is 5-40 RH%.
7. The preparation method according to claim 1, wherein in step a), the thickness of the precursor fiber blank is 100-400 mm; the surface density of the precursor fiber blank is 0.5-3 kg/m2。
8. The method according to claim 1, wherein the needling density in step b) is 1 to 50 needles/cm2。
9. The method according to claim 1, wherein step c) comprises in particular:
sequentially carrying out heat treatment on the precursor fiber blanket blank in a low-temperature area, a medium-temperature area and a high-temperature area of a heating furnace to obtain an aluminum oxide fiber blanket;
in the heat treatment process, the temperature of the low-temperature zone of the heating furnace is 0-600 ℃, the temperature of the medium-temperature zone is 600-1100 ℃, and the temperature of the high-temperature zone is 1100-1300 ℃.
10. The production method according to claim 9, wherein the amount of exhaust gas in the low temperature zone of the heating furnace during the heat treatment is set to 1 to 2Nm3/kg/h。
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