CN107904697A - The poly- aikyiaiurnirsoxan beta of solid-state, the preparation method of the poly- aikyiaiurnirsoxan beta of solid-state, alumina fibre cotton and preparation method thereof - Google Patents
The poly- aikyiaiurnirsoxan beta of solid-state, the preparation method of the poly- aikyiaiurnirsoxan beta of solid-state, alumina fibre cotton and preparation method thereof Download PDFInfo
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/10—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material by decomposition of organic substances
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G79/00—Macromolecular compounds obtained by reactions forming a linkage containing atoms other than silicon, sulfur, nitrogen, oxygen, and carbon with or without the latter elements in the main chain of the macromolecule
- C08G79/10—Macromolecular compounds obtained by reactions forming a linkage containing atoms other than silicon, sulfur, nitrogen, oxygen, and carbon with or without the latter elements in the main chain of the macromolecule a linkage containing aluminium
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D10/00—Physical treatment of artificial filaments or the like during manufacture, i.e. during a continuous production process before the filaments have been collected
- D01D10/02—Heat treatment
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/18—Formation of filaments, threads, or the like by means of rotating spinnerets
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
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Abstract
The present invention relates to a kind of poly- aikyiaiurnirsoxan beta of solid-state, the preparation method of the poly- aikyiaiurnirsoxan beta of solid-state, alumina fibre cotton and preparation method thereof, first pass through high temperature bunching and poly- aikyiaiurnirsoxan beta is prepared as the poly- aikyiaiurnirsoxan beta of solid-state, then cellucotton precursor is prepared into fibre by centrifugal drying silk or injection, further by curing, cracking, the technique such as sintering and prepare alumina fibre cotton.The poly- aikyiaiurnirsoxan beta softening point of solid-state and rheological characteristic being prepared are adjustable, and cost is relatively low, and solvent-free, environmentally protective in follow-up spinning operations, fiber precursor is insensitive to humidity in air, easy to large-scale production.And preparation-obtained alumina fibre cotton pliability is splendid, mechanical behavior under high temperature is excellent, and can be widely used in the fields such as vehicle exhaust insulation blanket, high temperature filtration core carrier, Industrial Stoves heat-preservation cotton.
Description
Technical field
The present invention relates to a kind of poly- aikyiaiurnirsoxan beta of solid-state, the preparation method of the poly- aikyiaiurnirsoxan beta of solid-state, alumina fibre cotton and its system
Preparation Method.
Background technology
Alumina fibre cotton is a kind of development situation of high-performance inorganic fibers, its outstanding feature is high intensity, high-modulus, and 1000
There is excellent mechanical property under~1200 DEG C of air atmospheres, at the same it is also small with thermal conductivity, and thermal coefficient of expansion is low, anti-thermal shock
The advantages that property is good.Compared with the non-oxidized substance fiber such as carbon fiber, silicon carbide fibre, alumina fibre has high intensity, heat resistance
And the advantages of high-temperature oxidation, good tensile strength is kept at a higher temperature；It is and easily multiple with metal, ceramic matrix
Close, form many excellent performances, widely used composite material.
Alumina fibre cotton has huge city as high temperature thermal insulation material in aerospace and civilian high end materials field
Field prospect.Such as the thermal insulation tile of space shuttle, solid engines combustion chamber insulated case, the jet pipe in supersonic velocity aircraft,
Packing ring, nuclear reactor in rocket engine are heat-insulated, the heat structure connector between SRM Nozzle and combustion chamber, jet pipe
The related component of outlet cone has all largely used alumina fibre.
The vehicle exhaust insulation blanket of civil field is often with glass fibre, alumina silicate fibre, ceramic alumina fiber at present
Deng high-temperature fibre.This is because the temperature of tail gas is higher, 600 DEG C -800 DEG C are maintained for a long time.Glass fibre has resistance
Combustion, the plurality of advantages such as corrosion-resistant, unit weight is small, thermal conductivity factor is low, hydroscopicity is low, therefore the application in the field is more universal.But
Since glass resistance to elevated temperatures itself is bad, then add its pliability it is poor, hard texture is crisp, easily breaks in the case of continuous vibration
Split, so as to influence sound isolating and heat insulating performance, there is also this drawback for alumina silicate fibre.And glass fibre is using molten condition
Glass centrifugal injection prepares gained into fibre, once the fiber incoming call alveolar produced in preparation process, easily produces carcinogenic risk.
Ceramic alumina fiber resistance to elevated temperatures is better than aluminium silicate fiber peacekeeping glass fibre, and can be by adjusting the crystalloid of fiber
Condition, improves the pliability of alumina fibre, and fracture can not occur in lasting temperature vibration environment, use when can be long.
The country is currently without the commercialization cellucotton product padded suitable for vehicle exhaust high temperature insulating.
Viscosity is low after aluminium oxide ceramics fusing point height and thawing, can not use traditional melt drawing technique productions.Various countries for this
Researcher develops several different production lines successively using chemical method, and wherein precursor process is preparation of industrialization aluminium oxide
The main method of continuous fiber.According to precursor material Species differences, particularly may be divided into organic fiber infusion process, inorganic salts method,
Sol-gel process, organic polymer precursor body method and mud solution method etc..
Sol-gal process is a kind of method more generally used in current alumina fibre preparation of the production process, and China is specially
Sharp CN104005115A discloses a kind of preparation method of ceramic alumina fiber, mainly using following steps：Using containing
The alumina sol and Ludox of Al13 micelles prepare spinnability precursor sol, and gel fibre is prepared using injection fiber-forming process
Dimension, by the ceramic alumina fiber for being thermally treated resulting in diameter 1-7um.But fiber precursor is more quick to the humidity of spinning environment
Sense, is easily adhered simultaneously silk, or even cause precursor to be scrapped in the pasty state, the stability of spinning system is poor.
Method of electrostatic spinning is the effective technical way for preparing nanofiber.Chinese patent CN101982581A is disclosed with second
Acyl acetone aluminium is silicon source, and using polyacrylonitrile or polyurethane as spin finish aid, electrostatic spinning combines 1200 DEG C of high temperature carbon thermal reduction systems
It is standby gone out the alumina fibre of a diameter of hundred nano-scale.Chinese patent CN102167567A has been opened altogether a kind of uses sol-gel
Method prepares the spinning material containing Aluminum sol, by electrostatic spinning process, with reference to double sintering technique, finally prepare it is flexible compared with
Alumina fibre good, that diameter is not waited in 400nm-800nm.But method of electrostatic spinning preparation efficiency is low, cost is higher, it is difficult to real
Existing large-scale production.
For these reasons, it is special to propose the present invention.
The content of the invention
It is an object of the invention to provide a kind of poly- aikyiaiurnirsoxan beta of solid-state, the preparation method of the poly- aikyiaiurnirsoxan beta of solid-state, aluminium oxide are fine
Vinylon and cotton blend and preparation method thereof, the spinning system in the preparation method of the alumina fibre cotton are stablized, and cut fiber precursor to spinning ring
The humidity in border is insensitive, while spin finish aid is free of in this method raw material, and avoiding leaving away for spin finish aid under high temperature causes fibre
Tie up volume contraction and the adverse effect of mechanical property loss.
To reach above-mentioned purpose, the present invention provides following technical solution：A kind of preparation method of the poly- aikyiaiurnirsoxan beta of solid-state, including
Following steps：
Poly- aikyiaiurnirsoxan beta is provided, the poly- aikyiaiurnirsoxan beta is obtained into the poly- aikyiaiurnirsoxan beta of the solid-state by high temperature bunching.
Further, during the high temperature bunching, temperature is 150-220 DEG C.
Further, it is carried out at the same time vacuum distillation during the high temperature bunching.
To reach above-mentioned purpose, the present invention provides also following technical solution：A kind of preparation by the poly- aikyiaiurnirsoxan beta of the solid-state
The poly- aikyiaiurnirsoxan beta of solid-state obtained by method, the softening point of the poly- aikyiaiurnirsoxan beta of solid-state are located at 50-125 DEG C.
To reach above-mentioned purpose, the present invention provides and and for example descends technical solution：A kind of preparation method of alumina fibre cotton, bag
Include following steps：
S1, provide spinning material, and the spinning material includes the poly- aikyiaiurnirsoxan beta of solid-state as claimed in claim 4, by described in
Spinning material obtains cellucotton precursor by spinning technique；
S2, by the cellucotton precursor cured and cracked, to obtain fiber cotton fabric；
S3, by the fiber cotton fabric after cracking be sintered with superhigh temperature processing, to obtain the alumina fibre cotton.
Further, in step S1, the spinning technique includes centrifugal drying silk, the specific steps bag of the centrifugal drying silk
Include：
The spinning material is placed in centrifugation tumbling machine, heat up heating in nitrogen atmosphere, treats that the spinning material melts
After melting as uniform melt and removing residual bubbles, the wire hole high speed of getting rid of of the melt from the centrifugation tumbling machine is thrown away,
To obtain cellucotton precursor.
Further, the condition of the centrifugal drying silk includes：It is described heating heating temperature for 110-180 DEG C, it is described from
The rotating speed of heart tumbling machine is 4000-20000r/min, the wire tray aperture of getting rid of of the centrifugation tumbling machine is 0.1-0.5mm.
Further, in step S1, the spinning technique includes injection into fibre, specific steps bag of the injection into fibre
Include：
The spinning material is placed in blowing device, heating is heated to the spinning material and melts completely, in the spray
Blow and be blown in equipment into fibre to obtain cellucotton precursor.
Further, the injection includes into fine adjusting：Air pressure is 0.05-0.6MPa, hydraulic pressure 0.05-
The angle of 0.15Mpa, spinneret liquid direction and airflow direction are 20-70 °.
Further, in step S2, the cured specific steps include：
The cellucotton precursor is placed in climatic chamber, is first warming up to 30-40 DEG C, in the relative humidity of 30-45%
Lower insulation 20min-2h, then 60-95 DEG C is warming up to, 10min -2h are kept the temperature under the humidity of 60-95%, are cooled to room temperature to obtain
Cured fiber cotton fabric.
Further, in step S2, the specific steps of the cracking include：
Cellucotton fabric after curing is placed in high temperature furnace and is warming up to 500-800 DEG C with 0.5-30 DEG C/min, and is being split
Insulation 30min-2h is cracked in solution atmosphere.
Further, one kind in nitrogen, argon gas, helium and air is included for forming the gas of the cracking atmosphere
Or more than one gases.
Further, in step S3, the specific steps of the sintering include：
Fiber cotton fabric after cracking is warming up to 1000- in air atmosphere with the heating rate of 0.15-100 DEG C/min
1800 DEG C, sintering processes 1min-10h.
Further, in step S3, the specific steps of the superhigh temperature processing include：
The gas flame that fiber cotton fabric after sintering is produced with burner carries out superhigh temperature in flammable atmosphere to it
Handle to obtain the alumina fibre cotton.
Further, one in ethene, propane, acetylene and coal gas is included for forming the gas of the flammable atmosphere
Kind or more than one gases.
To reach above-mentioned purpose, the present invention provides technical solution as follows：A kind of system by the alumina fibre cotton
Alumina fibre cotton obtained by Preparation Method.
The beneficial effects of the present invention are：
(1) poly- aikyiaiurnirsoxan beta is obtained solid-state poly-aluminium oxygen by the preparation method of the poly- aikyiaiurnirsoxan beta of solid-state of the invention by high temperature bunching
Alkane, the poly- aikyiaiurnirsoxan beta of the solid-state is cheap as spinning material, and its softening point and rheological characteristic are adjustable.Meanwhile the present invention is adopted
Spin finish aid is free of in spinning material, avoiding leaving away for spin finish aid under high temperature causes fiber volume contraction and mechanical property
The adverse effect of the loss of energy.
(2) alumina fibre cotton Preparation Method of the invention prepares fiber using centrifugal drying silk or injection fiber-forming process
Cotton, the spinning technique stable system, fiber precursor is insensitive to the humidity of spinning environment, avoids solution and gets rid of prepared by a technique
Fiber precursor is easily adhered and the problem of silk even in the pasty state.
(3) whole technique is environmentally protective, can quickly accomplish scale production, and the cellucotton sample finally prepared is flexible
Property is splendid, and mechanical behavior under high temperature is excellent.
Described above is only the general introduction of technical solution of the present invention, in order to better understand the technological means of the present invention,
And can be practiced according to the content of specification, below with presently preferred embodiments of the present invention and coordinate attached drawing describe in detail as after.
Brief description of the drawings
Fig. 1 is the process step figure of the preparation method of the alumina fibre cotton of the present invention；
Fig. 2 a and Fig. 2 b are the SEM figures of the alumina fibre cotton shown in the embodiment of the present invention one；
Fig. 3 is the XRD diagram of the alumina fibre cotton shown in the embodiment of the present invention one；
Fig. 4 is the SEM figures of the alumina fibre cotton shown in the embodiment of the present invention six；
Fig. 5 is the XRD diagram of the alumina fibre cotton shown in the embodiment of the present invention six.
Embodiment
With reference to the accompanying drawings and examples, the embodiment of the present invention is described in further detail.Implement below
Example is used to illustrate the present invention, but is not limited to the scope of the present invention.
The preparation method of the poly- aikyiaiurnirsoxan beta of solid-state of the present invention, comprises the following steps：
Poly- aikyiaiurnirsoxan beta is provided, is obtained under conditions of being 150-220 DEG C in temperature by the poly- aikyiaiurnirsoxan beta by high temperature bunching
The poly- aikyiaiurnirsoxan beta of solid-state, and it is carried out at the same time vacuum distillation during the high temperature bunching.
By the poly- aikyiaiurnirsoxan beta of solid-state obtained by the preparation method of the poly- aikyiaiurnirsoxan beta of the solid-state, its softening point is located at 50-125
DEG C, its structural formula is as follows：
Fig. 1 is referred to, the preparation method of alumina fibre cotton of the invention, comprises the following steps：
S1, provide spinning material, and the spinning material includes the poly- aikyiaiurnirsoxan beta of solid-state as claimed in claim 4, by described in
Spinning material is placed in centrifugation tumbling machine, and heating up in nitrogen atmosphere is heated to 110-180 DEG C, treats that the spinning material melting is
Uniform melt and after removing residual bubbles, by the melt getting rid of in wire hole with 4000-20000r/ from the centrifugation tumbling machine
The rotating speed of min is thrown away at a high speed, to obtain cellucotton precursor；
Alternatively,
Spinning material is provided, the spinning material includes the poly- aikyiaiurnirsoxan beta of solid-state as claimed in claim 4, by the spinning
Raw material is placed in blowing device, and heating is heated to 110-200 DEG C, is 0.05- in air pressure after the spinning material completely melting
Under conditions of 0.6MPa, hydraulic pressure 0.05-0.15MPa, spinneret liquid flow path direction and airflow direction angle are 20-70 °, it is blown into
Fibre, obtains cellucotton precursor.
The cellucotton precursor, be placed in climatic chamber by S2,30-40 DEG C is first warming up to, in the relatively wet of 30-45%
The lower insulation 20min-2h of degree, then 60-95 DEG C is warming up to, 10min-2h is kept the temperature under the humidity of 60-95%, is cooled to room temperature
To cured fiber cotton fabric；
Cellucotton fabric after curing, be placed in high temperature furnace and be warming up to 800 DEG C of 500- with 0.5-30 DEG C/min by S3, and
Keep the temperature 30min-2h in atmosphere is cracked to be cracked, the gas for forming the cracking atmosphere includes nitrogen, argon gas, helium
And one or more kinds of gases in air；
Fiber cotton fabric after cracking, be warming up to by S4 in air atmosphere with the heating rate of 0.15-100 DEG C/min
1000-1800 DEG C, sintering processes 1min-10h, to obtain the alumina fibre cotton.
S5, the gas flame for producing the fiber cotton fabric after sintering with burner carry out superelevation in flammable atmosphere to it
Temperature processing to obtain the alumina fibre cotton, for formed the flammable atmosphere gas include ethene, propane, acetylene with
And one or more kinds of gases in coal gas.Temperature, gas and the device of the superhigh temperature processing are carried out based on actual conditions
Selection.
Below in conjunction with specific embodiments come to the present invention illustrated in further detail.
Embodiment one
1. the preparation of the poly- aikyiaiurnirsoxan beta of solid-state：
The poly- aikyiaiurnirsoxan betas of 500g (Poly aluminoxane, PAO) are placed in reaction kettle, 80 DEG C are heated under stirring, is subtracted
Pressure distillation 1h, is continuously heating to 120 DEG C, keeps the temperature 1h, be finally warming up to 150 DEG C again, and per 10min, softening point is surveyed in sampling, works as softening
When point reaches 85 DEG C, stop heating, nitrogen protection drops to room temperature and obtains the poly- aikyiaiurnirsoxan beta of solid-state；
2. the preparation of alumina fibre cotton：
Spinning material, be placed in there-necked flask by S1, and heating under nitrogen protection is heated to 130 DEG C, treats that its melting is uniform
Melt and after removing residual bubbles, it is 4000r/min quickly and evenly to pour into rotating speed, and it is that 0.4mm gets rid of silk to get rid of wire tray aperture
Machine, melt spinning raw material are thrown away from wire hole high speed is got rid of, and obtain fiber precursor；
S2, by S1 gained alumina fibre precursor be placed in climatic chamber, 40 DEG C are first warming up to, in 30% phase
To keeping the temperature 30min under humidity, then 90 DEG C are warming up to, 20min is kept the temperature under 80% humidity, be cooled to room temperature to obtain curing fibre
Dimension；
Gained cured fiber in S2, be placed in high temperature furnace and be warming up to 600 DEG C with 1 DEG C/min by S3, keeps the temperature 1h, cracks atmosphere
For air；
S4, by S3 gained cracking after fiber cotton fabric 1000 DEG C of processing are warming up to the heating rate of 30 DEG C/min
20min, sintering atmosphere are air；
S5, using the propane gas flame that 12cm burners produce in S4 gained sintering after fiber superhigh temperature handle 5s.I.e.
It can obtain the γ-Al2O3 ceramic fibres of white fiber cotton form.
Fig. 2 a, Fig. 2 b and Fig. 3 are referred to, according to the alumina fibre obtained by the preparation method of the alumina fibre cotton
The SEM photograph and XRD spectra of cotton are as shown in the figure.As can be seen from Figure, fiber surface is smooth, size uniform, and fibre diameter is 2-5 μ
m；XRD the result shows that, the crystalline phase of fiber composition is γ-Al2O3.
Embodiment two
1. the preparation of the poly- aikyiaiurnirsoxan beta of solid-state：
500g PAO are placed in reaction kettle, 80 DEG C are heated under stirring, are evaporated under reduced pressure 1h, are continuously heating to 120 DEG C, are protected
Warm 1h, is finally warming up to 150 DEG C again, and per 10min, softening point is surveyed in sampling, when softening point reaches 85 DEG C, stops heating, nitrogen is protected
Shield drops to room temperature and obtains the poly- aikyiaiurnirsoxan beta of solid-state.
2. the preparation of alumina fibre cotton：
S1, by spinning material pour into injection device for spinning liquid material pipe in, adjust liquid material pipe temperature to 125 DEG C, treat it
After melting as uniform melt and removing residual bubbles, meltblowns, control pressure 0.45MPa, hydraulic pressure are carried out at 125 DEG C
For 0.08MPa, it is in about 60 ° of angles to keep liquid flow path direction and airflow direction, is blown out precursor fibre precursor, fibre length is about
15cm, size uniform and without slag ball；
S2, by S1 gained alumina fibre precursor be placed in climatic chamber, 40 DEG C are first warming up to, in 30% phase
To keeping the temperature 20min under humidity, then 90 DEG C are warming up to, 20min is kept the temperature under 80% humidity, be cooled to room temperature to obtain curing fibre
Dimension；
Gained cured fiber in S2, be placed in high temperature furnace and be warming up to 600 DEG C with 1 DEG C/min by S3, keeps the temperature 1h, cracks atmosphere
For air；
S4, by S3 gained cracking after fiber cotton fabric 1400 DEG C of processing are warming up to the heating rate of 30 DEG C/min
10min, sintering atmosphere are air；
S5, using the propane gas flame that 12cm burners produce in S4 gained sintering after fiber superhigh temperature handle 5s.I.e.
It can obtain the white α-Al2O3 ceramic fiber cottons that length is 10cm.
Embodiment three
1. the preparation of the poly- aikyiaiurnirsoxan beta of solid-state：
The poly- aikyiaiurnirsoxan betas of 500g (PAO) are placed in reaction kettle, 180 DEG C are heated under stirring, vacuum distillation, takes per 10min
Sample surveys softening point, when softening point reaches 105 DEG C, stops heating, and nitrogen protection drops to the secure satisfactory grades solid-state of sub-ization of room temperature and gathers
Aikyiaiurnirsoxan beta.
2. the preparation of alumina fibre cotton：
Spinning material, be placed in there-necked flask by S1, and heating under nitrogen protection is heated to 150 DEG C, treats that its melting is uniform
Melt and after removing residual bubbles, it is 5000r/min quickly and evenly to pour into rotating speed, and it is that 0.4mm gets rid of silk to get rid of wire tray aperture
Machine, melt spinning raw material are thrown away from wire hole high speed is got rid of, and obtain fiber precursor；
S2, by S1 gained alumina fibre precursor be placed in climatic chamber, 85 DEG C are warming up to, under 90% humidity
10min is kept the temperature, is cooled to room temperature to obtain cured fiber；
Gained cured fiber in S2, be placed in high temperature furnace and be warming up to 600 DEG C with 5 DEG C/min by S3, keeps the temperature 1h, cracks atmosphere
For air；
S4, by S3 gained cracking after fiber with the heating rate of 10 DEG C/min be warming up to 1200 DEG C processing 30min, burn
Knot atmosphere is air；
S5, using the propane gas flame that 12cm burners produce in S4 gained sintering after fiber superhigh temperature handle 5s.I.e.
It can obtain the α-Al2O3 ceramic fiber cottons of white.
Example IV
1. the preparation of the poly- aikyiaiurnirsoxan beta of solid-state：
The poly- aikyiaiurnirsoxan betas of 500g (PAO) are placed in reaction kettle, 180 DEG C are heated under stirring, vacuum distillation, takes per 10min
Sample surveys softening point, when softening point reaches 105 DEG C, stops heating, and nitrogen protection drops to the secure satisfactory grades solid-state of sub-ization of room temperature and gathers
Aikyiaiurnirsoxan beta.
2. the preparation of alumina fibre cotton：
S1, by spinning material pour into injection device for spinning liquid material pipe in, adjust liquid material pipe temperature to 145 DEG C, treat it
After melting as uniform melt and removing residual bubbles, meltblowns, control pressure 0.56MPa, hydraulic pressure are carried out at 145 DEG C
For 0.06MPa, it is in about 55 ° of angles to keep liquid flow path direction and airflow direction, is blown out precursor fibre precursor, fibre length is about
20cm, size uniform and without slag ball；
S2, by S1 gained alumina fibre precursor be placed in climatic chamber, 50 DEG C are first warming up to, in 30% phase
To keeping the temperature 1h min under humidity, then 90 DEG C are warming up to, 20min is kept the temperature under 80% humidity, be cooled to room temperature to obtain curing fibre
Dimension；
Gained cured fiber in S2, be placed in high temperature furnace and be warming up to 600 DEG C with 2 DEG C/min by S3, keeps the temperature 2h, cracks atmosphere
For air；
S4, by S3 gained cracking after fiber with the heating rate of 30 DEG C/min be warming up to 1400 DEG C processing 10min, burn
Knot atmosphere is air；
S5, using the ethylene gaseous fuel flame that 12cm burners produce in S4 gained sintering after fiber superhigh temperature handle 5s.I.e.
It can obtain the white α-Al2O3 ceramic fiber cottons that length is 10cm.
Embodiment five
1. the preparation of the poly- aikyiaiurnirsoxan beta of solid-state：
The poly- aikyiaiurnirsoxan betas of 500g (PAO) are placed in reaction kettle, 220 DEG C are heated under stirring, after being evaporated under reduced pressure 30min, are stopped
Only heat, nitrogen protective atmosphere, which encloses, drops to room temperature, and it is 113 DEG C to obtain softening point, the poly- aikyiaiurnirsoxan beta of solid-state of producing high-molecular.
2. the preparation of alumina fibre cotton：
Spinning material, be placed in there-necked flask by S1, and heating under nitrogen protection is heated to 160 DEG C, treats that its melting is uniform
Melt and after removing residual bubbles, it is 7000r/min quickly and evenly to pour into rotating speed, and it is that 0.4mm gets rid of silk to get rid of wire tray aperture
Machine, melt spinning raw material are thrown away from wire hole high speed is got rid of, and obtain fiber precursor；
S2, by S1 gained alumina fibre precursor be placed in climatic chamber, 85 DEG C are warming up to, under 90% humidity
10min is kept the temperature, is cooled to room temperature to obtain cured fiber；
Gained cured fiber in S2, be placed in high temperature furnace and be warming up to 600 DEG C with 2 DEG C/min by S3, keeps the temperature 2h, cracks atmosphere
For air；
S4, by S3 gained cracking after fiber with the heating rate of 10 DEG C/min be warming up to 1400 DEG C processing 20min, sintering
Atmosphere is air；
S5, using the ethylene gaseous fuel flame that 12cm burners produce in S4 gained sintering after fiber superhigh temperature handle 5s.I.e.
It can obtain the α-Al2O3 ceramic fiber cottons of white.
Embodiment six
1. the preparation of the poly- aikyiaiurnirsoxan beta of solid-state：
The poly- aikyiaiurnirsoxan betas of 500g (PAO) are placed in reaction kettle, 220 DEG C are heated under stirring, after being evaporated under reduced pressure 30min, are stopped
Only heat, nitrogen protective atmosphere, which encloses, drops to room temperature, and it is 113 DEG C to obtain softening point, the poly- aikyiaiurnirsoxan beta of solid-state of producing high-molecular.
2. the preparation of alumina fibre cotton：
S1, by spinning material pour into injection device for spinning liquid material pipe in, adjust liquid material pipe temperature to 165 DEG C, treat it
After melting as uniform melt and removing residual bubbles, meltblowns, control pressure 0.56MPa, hydraulic pressure are carried out at 165 DEG C
For 0.06MPa, it is in about 35 ° of angles to keep liquid flow path direction and airflow direction, is blown out precursor fibre precursor, fibre length is about
30cm, size uniform and without slag ball；
S2, by S1 gained alumina fibre precursor be placed in climatic chamber, 50 DEG C are first warming up to, in 30% phase
To keeping the temperature 1h min under humidity, then 90 DEG C are warming up to, 20min is kept the temperature under 80% humidity, be cooled to room temperature to obtain curing fibre
Dimension；
Gained cured fiber in S2, be placed in high temperature furnace and be warming up to 700 DEG C with 1 DEG C/min by S3, keeps the temperature 1h, cracks atmosphere
For air；
S4, by S3 gained cracking after fiber cotton fabric 1400 DEG C of processing are warming up to the heating rate of 30 DEG C/min
10min, sintering atmosphere are air；
S5, using the ethylene gaseous fuel flame that 12cm burners produce in S4 gained sintering after fiber superhigh temperature handle 5s.I.e.
It can obtain the white α-Al2O3 ceramic fiber cottons that length is 15cm.The SEM photograph and XRD spectra of gained alumina fibre cotton are such as
Shown in Fig. 4 and Fig. 5.
In summary：Poly- aikyiaiurnirsoxan beta is obtained solid-state by the preparation method of the poly- aikyiaiurnirsoxan beta of solid-state of the present invention by high temperature bunching
Poly- aikyiaiurnirsoxan beta, the poly- aikyiaiurnirsoxan beta of the solid-state is cheap as spinning material, and its softening point and rheological characteristic are adjustable.Meanwhile this hair
Be free of spin finish aid in spinning material used by bright, avoid spin finish aid under high temperature leave away cause fiber volume shrink with
The adverse effect of mechanical property loss.
Also, the alumina fibre cotton Preparation Method of the present invention prepares cellucotton using silk and injection fiber-forming process is got rid of, should
Spinning technique stable system, fiber precursor are insensitive to the humidity of spinning environment, avoid solution and get rid of fiber prepared by a technique
Precursor is easily adhered and the problem of silk even in the pasty state.
Meanwhile whole technique of the invention is environmentally protective, can quickly accomplish scale production, and the fiber finally prepared
Cotton sample product pliability is splendid, and mechanical behavior under high temperature is excellent.
Each technical characteristic of embodiment described above can be combined arbitrarily, to make description succinct, not to above-mentioned reality
Apply all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, the scope that this specification is recorded all is considered to be.
Embodiment described above only expresses the several embodiments of the present invention, its description is more specific and detailed, but simultaneously
Cannot therefore it be construed as limiting the scope of the patent.It should be pointed out that come for those of ordinary skill in the art
Say, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the protection of the present invention
Scope.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (16)
1. a kind of preparation method of the poly- aikyiaiurnirsoxan beta of solid-state, it is characterised in that comprise the following steps：
Poly- aikyiaiurnirsoxan beta is provided, the poly- aikyiaiurnirsoxan beta is obtained into the poly- aikyiaiurnirsoxan beta of the solid-state by high temperature bunching.
2. the preparation method of poly- aikyiaiurnirsoxan beta as claimed in claim 1, it is characterised in that during the high temperature bunching, temperature
Spend for 150-220 DEG C.
3. the preparation method of poly- aikyiaiurnirsoxan beta as claimed in claim 2, it is characterised in that during the high temperature bunching at the same time
It is evaporated under reduced pressure.
A kind of 4. solid-state poly-aluminium as obtained by the preparation method of the poly- aikyiaiurnirsoxan beta of the solid-state any one of claims 1 to 3
Oxygen alkane, it is characterised in that the softening point of the poly- aikyiaiurnirsoxan beta of solid-state is located at 50-125 DEG C.
5. a kind of preparation method of alumina fibre cotton, it is characterised in that comprise the following steps：
S1, provide spinning material, and the spinning material includes the poly- aikyiaiurnirsoxan beta of solid-state as claimed in claim 4, by the spinning
Raw material obtains cellucotton precursor by spinning technique；
S2, by the cellucotton precursor cured and cracked, to obtain fiber cotton fabric；
S3, by the fiber cotton fabric after cracking be sintered with superhigh temperature processing, to obtain the alumina fibre cotton.
6. the preparation method of alumina fibre cotton as claimed in claim 5, it is characterised in that in step S1, the spinning work
Skill includes centrifugal drying silk, and the specific steps of the centrifugal drying silk include：
The spinning material is placed in centrifugation tumbling machine, heat up heating in nitrogen atmosphere, treats that the spinning material melting is
Uniform melt and after removing residual bubbles, the wire hole high speed of getting rid of of the melt from the centrifugation tumbling machine is thrown away, with
To cellucotton precursor.
7. the preparation method of alumina fibre cotton as claimed in claim 6, it is characterised in that the condition bag of the centrifugal drying silk
Include：The temperature of the heating heating is 110-180 DEG C, the rotating speed of the centrifugation tumbling machine be 4000-20000r/min, it is described from
The wire tray aperture of getting rid of of heart tumbling machine is 0.1-0.5mm.
8. the preparation method of alumina fibre cotton as claimed in claim 5, it is characterised in that in step S1, the spinning work
Skill includes injection to be included into fibre, the injection into fine specific steps：
The spinning material is placed in blowing device, heating is heated to the spinning material and melts completely, is set in the injection
It is blown for middle into fibre to obtain cellucotton precursor.
9. the preparation method of alumina fibre cotton as claimed in claim 8, it is characterised in that adjusting bag of the injection into fibre
Include：Air pressure is 0.05-0.6MPa, hydraulic pressure 0.05-0.15Mpa, the angle of spinneret liquid direction and airflow direction are 20-70 °.
10. the preparation method of alumina fibre cotton as claimed in claim 5, it is characterised in that described cured in step S2
Specific steps include：
The cellucotton precursor is placed in climatic chamber, is first warming up to 30-40 DEG C, is protected under the relative humidity of 30-45%
Warm 20min-2h, then 60-95 DEG C is warming up to, 10min-2h is kept the temperature under the humidity of 60-95%, is cooled to room temperature to obtain cured
Fiber cotton fabric.
11. the preparation method of alumina fibre cotton as claimed in claim 5, it is characterised in that in step S2, the cracking
Specific steps include：
Cellucotton fabric after curing is placed in high temperature furnace and is warming up to 500-800 DEG C with 0.5-30 DEG C/min, and in cracking gas
30min-2h is kept the temperature in atmosphere to be cracked.
12. the preparation method of alumina fibre cotton as claimed in claim 11, it is characterised in that for forming the cracking gas
The gas of atmosphere includes one or more kinds of gases in nitrogen, argon gas, helium and air.
13. the preparation method of alumina fibre cotton as claimed in claim 5, it is characterised in that in step S3, the sintering
Specific steps include：
Fiber cotton fabric after cracking is warming up to 1000-1800 in air atmosphere with the heating rate of 0.15-100 DEG C/min
DEG C, sintering processes 1min-10h.
14. the preparation method of alumina fibre cotton as claimed in claim 5, it is characterised in that in step S3, the superhigh temperature
The specific steps of processing include：
The gas flame that fiber cotton fabric after sintering is produced with burner carries out superhigh temperature processing in flammable atmosphere to it
To obtain the alumina fibre cotton.
15. the preparation method of alumina fibre cotton as claimed in claim 14, it is characterised in that for forming the combustibility
The gas of atmosphere includes one or more kinds of gases in ethene, propane, acetylene and coal gas.
A kind of 16. aluminium oxide as obtained by the preparation method of the alumina fibre cotton any one of claim 5 to 15
Cellucotton.
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