CN106747267A - A kind of Carbon Fiber Rigid thermal insulation tile and preparation method thereof - Google Patents
A kind of Carbon Fiber Rigid thermal insulation tile and preparation method thereof Download PDFInfo
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- CN106747267A CN106747267A CN201611100591.5A CN201611100591A CN106747267A CN 106747267 A CN106747267 A CN 106747267A CN 201611100591 A CN201611100591 A CN 201611100591A CN 106747267 A CN106747267 A CN 106747267A
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Abstract
The present invention relates to a kind of Carbon Fiber Rigid thermal insulation tile, including the chopped carbon fiber of skeleton is constituted, and phase is bonded for being bonded the Si/C/O glass of the chopped carbon fiber.Present invention also offers the preparation method of the Carbon Fiber Rigid thermal insulation tile.The present invention prepares the bonding phase between carbon fiber using silicones, the generation Si/C/O glass bonding phase when cracking is carbonized, play a part of to be bonded chopped carbon fiber skeleton, and after being aoxidized under high temperature aerobic environment due to Si/C/O glass bonding, surface can generate layer of silicon dioxide glass-film, so as to prevent oxygen atom from further aoxidizing the material of inside, therefore there is stronger inoxidizability, and the carbon yield that silicones is cracked under an inert atmosphere is high, with use starch as binder phase ratio, mechanical strength is also higher.
Description
Technical field
The present invention relates to functional composite material technical field, more particularly to a kind of Carbon Fiber Rigid thermal insulation tile and its preparation side
Method.
Background technology
Carbon Fiber Rigid thermal insulation tile has the advantages that heatproof is high, light porous, good heat-insulation effect, can be directly as superhigh temperature
Heat-barrier material is used, and is also used as raw material, prepares light ablative material by compound resin or anti-oxidant carbon base ceramics are multiple
Condensation material.
United States Atomic Energy Commission discloses a kind of preparation side of fibrous insulating material in United States Patent (USP) 3577344
Method.The patent is raw material using oxide ceramic fibres such as chopped carbon fiber, quartz fibre or alumina silicate, is formed sediment using solubility
Powder is bonding agent, prepares corresponding fibrous insulating material base substrate by wet therapy forming process, and then make the starch after gelatinization polymerization
Cracked in high temperature furnace and form bonding charcoal phase.The fibrous insulating material is used for nuclear power field high-temperature hot protection.Due to the fiber
Heat-barrier material is bonding agent using soluble starch, and the carbon yield after the starch after polymerization is cracked in high temperature furnace is relatively low, causes
The Carbon Fiber Rigid thermal insulation tile mechanical strength of preparation is inadequate.
No. 3577344 lightweight fibres of above-mentioned United States Patent (USP) are disclosed in United States Patent (USP) disclosed in USDOE 4152482
Tie up the preparation process amelioration of heat-barrier material.United States Patent (USP) 4152482 is eliminated viscous by layered filtration, multi-shell curing technique
Connect the stress accumulation produced in fibrous matrix during phase resin solidification.Additionally, layered filtration technique causes that the light fibre is heat-insulated
The structure of material is more controllable, can realize product using different fibrous matrixes, high emissivity filler etc. in different layers
Can graded.Fibrous material partnership of the U.S. (Fiber Materials Incorporation, FMI) produces one kind
The trade mark isCarbon fiber light rigidity thermal insulation tile.A diameter of 14-16 microns carbon fiber is chopped to 1.6mm
It is long, wet moulding after mashing is mixed with water soluble phenol resin and solvent, after phenolic resin curing under 1440 ℉ (782.2 DEG C)
Carbonization, and then be obtained after 3240 ℉ (1782.2 DEG C) high-temperature heat treatmentCarbon Fiber Rigid thermal insulation tile.The density of Carbon Fiber Rigid thermal insulation tile is 0.15-0.23g/cm3, thickness direction compressive strength is 0.2-
0.6MPa.Changqing Hong etc. are prepared for a kind of carbon fiber-based ablator PICA (phenolic impregnated 3-
D fine-woven pierced carbon fabric ablator), its density is 0.352~0.701g/cm3,
4.5MW/m2Oxygen/acetylene torch ablation test in, its linear ablative rate is 0.019~0.036mm/s, and mass ablative rate is
0.045~0.061g/s.This kind of PICA material is carefully compiled puncture carbon fiber precast body composite phenolic resin by 3D and prepared.But, this
A little materials using phenolic resin residue carbon of biomass pyrolysis as bonding phase, can burn under 1200 DEG C of high temperature air atmosphere, cause it
Inoxidizability is not high, and temperature tolerance is not enough.
The content of the invention
The purpose of the present invention is to overcome that existing Carbon Fiber Rigid thermal insulation tile mechanical strength is inadequate, the shortcoming that temperature tolerance is not enough,
The carbon fiber light rigidity that a kind of temperature tolerance is higher, lightweight, intensity is bigger is finally provided using different technical schemes
Thermal insulation tile and preparation method thereof, can be as oxygen-free atmosphere super high sintering temperature stove, nuclear power station high-temperature service, chemical reactor etc.
Thermally protective materials are used.
Therefore, the present invention realizes the purpose of the present invention by following technical solution：
1st, a kind of Carbon Fiber Rigid thermal insulation tile, wherein, including the chopped carbon fiber of skeleton is constituted, and it is described for being bonded
The Si/C/O glass bonding phase of chopped carbon fiber.
2nd, the Carbon Fiber Rigid thermal insulation tile according to technical scheme 1, wherein, the Si/C/O glass bonding is by silicon tree
Fat prepolymer, crosslinking agent, catalyst and organic solvent are according to 10:(0.1~10):(0.1~10):The mass ratio of (10~100)
In being configured to after silicone precursor mixed liquor suck carbon fiber dry body by Vacuum infusion techniques, then by cold curing, carbon
Change and obtained with after high-temperature heat treatment.
3rd, the Carbon Fiber Rigid thermal insulation tile according to technical scheme 2, wherein：
The silicone prepolymer be selected from by hydroxyl endblocked polydimethylsiloxane, hydroxy-end capped polydiphenylsiloxane,
Dimethyl silicone polymer, amino-terminated dimethyl silicone polymer and epoxy radicals end-blocking poly dimethyl silicon that hydroxy-end capped phenyl replaces
The mixture of one or several in the group of oxygen alkane composition；The viscosity of the silicone prepolymer is 200~100000cst；With/
Or
The crosslinking agent is selected from by tetraethyl orthosilicate, methyl silicate, MTMS, methyltriethoxy silane
The mixture of one or several in the group of alkane and dimethyldiethoxysilane composition；And/or
The catalyst is dibutyl tin laurate or γ-amine propyl-triethoxysilicane；And/or
The organic solvent is selected from the mixing of one or several in the group being made up of benzene, dimethylbenzene, styrene and acetone
Thing.
4th, the Carbon Fiber Rigid thermal insulation tile according to technical scheme 1 or 2, wherein, the length of the carbon fiber for 1~
5mm, a diameter of 8~12 μm.
5th, a kind of preparation method of Carbon Fiber Rigid thermal insulation tile, wherein, comprise the following steps：
(1) the wet base of chopped carbon fiber is obtained by wet moulding, carbon fiber dry body is obtained after drying；
(2) silicone precursor is obtained after mixing silicone prepolymer, crosslinking agent, catalyst and organic solvent to mix
Liquid；
(3) the carbon fiber dry body is impregnated using silicone precursor mixed liquor, then by cold curing, carbonization and high temperature
Carbon Fiber Rigid thermal insulation tile is obtained after heat treatment.
6th, the preparation method of the Carbon Fiber Rigid thermal insulation tile according to technical scheme 5, wherein, in the step (2)：
According to 10:(0.1~10):(0.1~10):The mass ratio of (10~100) by silicone prepolymer, crosslinking agent, urge
Silicone precursor mixed liquor is obtained after agent and organic solvent mixing.
7th, the preparation method of the Carbon Fiber Rigid thermal insulation tile according to technical scheme 5 or 6, wherein, the step (2)
In：
The silicone prepolymer be selected from by hydroxyl endblocked polydimethylsiloxane, hydroxy-end capped polydiphenylsiloxane,
Dimethyl silicone polymer, amino-terminated dimethyl silicone polymer and epoxy radicals end-blocking poly dimethyl silicon that hydroxy-end capped phenyl replaces
The mixture of one or several in the group of oxygen alkane composition；The viscosity of the silicone prepolymer is 200~100000cst；With/
Or
The crosslinking agent is selected from by tetraethyl orthosilicate, methyl silicate, MTMS, methyltriethoxy silane
The mixture of one or several in the group of alkane and dimethyldiethoxysilane composition；And/or
The catalyst is dibutyl tin laurate or γ-amine propyl-triethoxysilicane；And/or
The organic solvent is selected from the mixing of one or several in the group being made up of benzene, dimethylbenzene, styrene and acetone
Thing.
8th, the preparation method of the Carbon Fiber Rigid thermal insulation tile according to technical scheme 5, wherein, in the step (1)：
By chopped carbon fiber and water according to 1:150~250 mass ratio mixing, is filtrated to get wet base after stirring to pulp, then
Wet base is loaded into shaping mould, wet base is depressed into preset height by the target density according to material, dry 4 at 60~150 DEG C~
36 hours, obtain carbon fiber dry body.
9th, the preparation method of the Carbon Fiber Rigid thermal insulation tile according to technical scheme 5, wherein, in the step (1) also
Including removing glue step：
Carbon fiber is prescinded to 1~5mm, chopped carbon fiber is obtained, chopped carbon fiber is mixed with acetone, stirring mixing water
Under conditions of cold reflux, acetone is heated to 55~60 DEG C and is flowed back 24~72 hours, cleaning is attached to chopped carbon fiber surface
Epoxy resin surface conditioning agent, then by strainer filtering, then cause acetone volatilization after obtain chopped carbon fiber.
10th, the preparation method of the Carbon Fiber Rigid thermal insulation tile according to technical scheme 5, wherein, in the step (3)：
Vacuum impregnation and cold curing are specially：First the carbon fiber dry body that step (1) is obtained is placed in together with shaping mould
In vacuum impregnation tank, the vacuum impregnation tank is sealed and 10 are evacuated to-2~10-4atm；By silicones obtained in step (2)
Presoma mixed liquor is injected in the vacuum impregnation tank, liquid level was not had the shaping mould upper surface, and opening atmospheric valve makes tank
Internal air pressure balance stands 24~100 hours so that silicones crosslinking curing to 1atm；And/or
The carbonization is heated to 600~1000 DEG C in argon gas atmosphere stove and is incubated 1~10 hour；And/or
The high-temperature heat treatment is heated to 1500~2200 DEG C in argon gas atmosphere stove and is incubated 1~10 hour.
Implement Carbon Fiber Rigid thermal insulation tile of the invention and preparation method thereof, have the advantages that：
1st, the present invention prepares the bonding phase between carbon fiber using silicones, and when cracking is carbonized, generation Si/C/O glass glues
Phase is connect, Si/C/O glass bonding is mutually covered in the point of intersection of carbon fiber surface and carbon fiber and carbon fiber, play bonding and be chopped
The effect of carbon fiber skeleton, and because Si/C/O glass bonding is after oxidation under high temperature aerobic environment, surface can generate one
Layer silica glass film, so that prevent oxygen atom from further aoxidizing the material of inside, with inoxidizability.Therefore, with use
Phenolic resinoid residue carbon of biomass pyrolysis is compared as the material of bonding phase, the inoxidizability of the obtained Carbon Fiber Rigid thermal insulation tile of the present invention
It is stronger.On the other hand, with use starch as binder phase ratio, the carbon yield that silicones of the invention is cracked under an inert atmosphere
Higher than the starch of gelatinization, therefore mechanical strength is also higher by 20%~50%.
2nd, the present invention makes silicone precursor mixed liquor fully be combined with carbon fiber dry body by vacuum impregnation technique, is formed
Carbon Fiber Rigid thermal insulation tile uniform in material, overall performance stabilization, be more beneficial for Si/C/O glass bonding mutually play its bond make
With.
3rd, present invention optimizes the proportioning of each raw material in the silicone precursor mixed liquor for using, when silicones pre-polymerization
Thing, crosslinking agent, catalyst and organic solvent are according to 10:(0.1~10):(0.1~10):The mass ratio of (10~100) is prepared
When, enable to the Si/C/O glass bonding distributed mutually of cracking to be more uniformly distributed, mechanical strength is higher, and antioxygenic property is more preferable.
Brief description of the drawings
Fig. 1 is the Carbon Fiber Rigid thermal insulation tile preparation technology flow chart according to the preferred embodiment of the present invention；
Fig. 2 is that the in kind of the Carbon Fiber Rigid thermal insulation tile according to obtained in the preferred embodiment of the present invention shoots picture；
Fig. 3 is the Carbon Fiber Rigid thermal insulation tile stereoscan photograph according to obtained in the preferred embodiment of the present invention.
Specific embodiment
To make the purpose, technical scheme and advantage of the embodiment of the present invention clearer, below in conjunction with the embodiment of the present invention
In accompanying drawing, the technical scheme in the embodiment of the present invention is clearly and completely described, it is clear that described embodiment is
A part of embodiment of the invention, rather than whole embodiments.Based on the embodiment in the present invention, ordinary skill people
The every other embodiment that member is obtained on the premise of creative work is not made, belongs to the scope of protection of the invention.
As described above, the present invention provides a kind of Carbon Fiber Rigid thermal insulation tile in first aspect, wherein, the Carbon Fiber Rigid
Thermal insulation tile includes constituting the chopped carbon fiber of skeleton, and is bonded phase for being bonded the Si/C/O glass of the chopped carbon fiber.
Some preferred embodiment in, the length of chopped carbon fiber is 1~5mm, a diameter of 8~12 μm.Further
Preferably, the length of chopped carbon fiber is 2mm, a diameter of 10 μm.The carbon fiber used in the present invention can be but not limited to
The carbon fiber of the trades mark such as T-300, T-700, T-800, T-1000.
In some preferred implementation methods, Si/C/O glass bonding by silicone prepolymer A, crosslinking agent B,
During catalyst C and organic solvent D are configured to after silicone precursor mixed liquor suck carbon fiber dry body by Vacuum infusion techniques,
Obtained by after cold curing, carbonization and high-temperature heat treatment again.Preferably, silicone prepolymer in silicone precursor mixed liquor
The mass ratio of A, crosslinking agent B, catalyst C and organic solvent D is 10:(0.1~10):(0.1~10):(10~100).For example may be used
Think 10：(0.1,0.5,2,5 or 10):(0.1,0.5,2,5 or 10):(10,20,50 or 100).
The present invention prepares the bonding phase between carbon fiber using silicones.Silicones disperse phase is after hardening in carbon fiber surface
Face and carbon fiber are dispersed with carbon fiber point of intersection.In 800 DEG C of carbonization cracking, silicones is cracked to form Si/C/O glass and glues
Connect phase, i.e. SiCxOyGlass phase, the glass is mutually covered in the point of intersection of carbon fiber surface and carbon fiber and carbon fiber, plays bonding
The effect of chopped carbon fiber skeleton.After being aoxidized under high temperature aerobic environment due to Si/C/O glass bonding, surface can generate one
Layer silica glass film, so that prevent oxygen atom from further aoxidizing the material of inside, therefore Si/C/O glass bonding mutually has
Inoxidizability, when high temperature is experienced, ablation amount of contraction is smaller, and reliability is high；If replacing silicon using epoxy resin or phenolic aldehyde
If resin, the basic noresidue after ablation under conditions of oxygen abundance, ablation amount of contraction is big, thus reliability substantially compared with
It is low.
In some preferred implementation methods, the silicone prepolymer A is selected from by hydroxy-end capped polydimethylsiloxanes
Alkane, hydroxy-end capped polydiphenylsiloxane, dimethyl silicone polymer, the amino-terminated poly dimethyl silicon of the substitution of hydroxy-end capped phenyl
The mixture of one or several in the group of oxygen alkane and epoxy radicals end-blocking dimethyl silicone polymer composition.Wherein hydroxy-end capped phenyl
Substituted dimethyl silicone polymer can replace for part phenyl, and substitution value can be 30% to 70%.It may further be preferable that
The viscosity of the silicone prepolymer is 200~100000cst；More preferably 10000~20000CSt；It is further excellent in addition
Elect 2000~4000CSt as.
In some preferred implementation methods, the crosslinking agent B is selected from by tetraethyl orthosilicate, methyl silicate, methyl
The mixing of one or several in the group of trimethoxy silane, MTES and dimethyldiethoxysilane composition
Thing；It may further be preferable that the crosslinking agent B is tetraethyl orthosilicate.
In some preferred implementation methods, the catalyst C is dibutyl tin laurate or γ-second of amine propyl group three
TMOS.The inventors discovered that, in system of the invention, using dibutyl tin laurate as catalyst, can make
Obtain curing reaction speed faster, the time is fully cured no more than 24 hours；If using other catalyst such as γ-amine propyl group
Used as catalyst, the time that is fully cured then needs more than 48 hours to triethoxysilane.Therefore at some preferred embodiment
In, the catalyst C is dibutyl tin laurate.
Some preferred embodiment in, the organic solvent D be selected from be made up of benzene, dimethylbenzene, styrene and acetone
Group in the mixture of one or several；It may further be preferable that organic solvent D is dimethylbenzene.It is more highly preferred at one
Embodiment in, silicone prepolymer A be hydroxyl endblocked polydimethylsiloxane, crosslinking agent B is tetraethyl orthosilicate, catalyst C
It is dibutyl tin laurate, organic solvent D is dimethylbenzene, according to 10:1:0.1:Silicon is obtained after 50 mass ratio is well mixed
Resin precursor mixed liquor.
The present invention provides a kind of preparation method of Carbon Fiber Rigid thermal insulation tile in second aspect.Fig. 1 is please referred to, is
Carbon Fiber Rigid thermal insulation tile preparation technology flow chart according to the preferred embodiment of the invention.Wherein, the preparation method is included such as
Lower step：
(1) the wet base of chopped carbon fiber is obtained by wet moulding, carbon fiber dry body is obtained after drying；
(2) silicone precursor is obtained after mixing silicone prepolymer, crosslinking agent, catalyst and organic solvent to mix
Liquid；
(3) use silicone precursor mixed liquor impregnation of carbon fibers dry body, such as it is fine by vacuum impregnation technique impregnated carbon
Dimension dry body, so that carbon fiber dry body absorbs the silicone precursor mixed liquor, then by cold curing, carbonization and warm high
Carbon Fiber Rigid thermal insulation tile is obtained after treatment.
Some preferred embodiment in, in the step (1)：By chopped carbon fiber and water according to 1:150~250
Mass ratio mixes, and wet base is filtrated to get after stirring to pulp, then wet base is loaded into shaping mould, and the target density according to material will be wet
Base is depressed into preset height, is dried 4~36 hours at 60~150 DEG C, obtains carbon fiber dry body.Specifically, by removing glue after it is short
Cut carbon fiber to mix with deionized water, mashing is sufficiently stirred in agitator, slurry is transferred in filtering frock, filter off big absolutely
Partial water, then loads shaping mould by wet base, and wet base is depressed into predetermined height by the target density according to material, 60~
4~36 hours (4,10,20,30 or 36) are dried under 150 DEG C (such as 60 DEG C, 80 DEG C, 100 DEG C or 150 DEG C), carbon fiber is obtained and is done
Base；Chopped carbon fiber is 1 with the mass ratio of deionized water：150~250 (such as 1:150、1:200 or 1:250) it is, further excellent
Elect 1 as:200.
In some preferred implementation methods, removing glue step is also included in the step (1)：I.e. by a diameter of 8~
12 μm of carbon fiber prescind to 1~5mm it is long after obtain chopped carbon fiber.Then chopped carbon fiber is mixed with acetone, in stirring
Under conditions of water cooled reflux, acetone is heated to 55~60 DEG C and is flowed back 24~72 hours, cleaning is attached to chopped carbon fiber
The epoxy resin surface conditioning agent on surface, then by strainer filtering, then causes that acetone obtains chopped carbon fiber after volatilizing.Tool
Body ground, chopped carbon fiber is placed in the kettle for filling acetone, and kettle top is provided with stirring and water cooled reflux device.Opening stirs mixing water
Cold reflux device, is heated to acetone 55~60 DEG C (such as 55 DEG C, 58 DEG C or 60 DEG C) and flows back 24~72 hours (24,36,48
Or 72 hours), the epoxy resin adhesive thoroughly cleaning that will be attached to carbon fiber surface is fallen.A kind of removing glue program of optimization is perseverance
60 DEG C of temperature flows back 48 hours, and the epoxy resin adhesive thoroughly cleaning that the program is enough to will be attached to carbon fiber surface is clean.With
Afterwards, the carbon fiber that will be cleaned in kettle out, is dried so that acetone fully volatilizees by strainer filtering in fume hood.
Some preferred embodiment in, in step (2)：According to 10:(0.1~10):(0.1~10):(10~100)
Mass ratio will silicone prepolymer A, crosslinking agent B, catalyst C and organic solvent D mix after be obtained silicone precursor mix
Liquid.For example can be 10：(0.1,0.5,2,5 or 10):(0.1,0.5,2,5 or 10):(10,20,50 or 100).Wherein silicon tree
Fat prepolymer A, crosslinking agent B, catalyst C and organic solvent D are as described in the first aspect of the invention.
Some preferred embodiment in, vacuum impregnation and cold curing are specially in the step (3)：First by step
(1) the carbon fiber dry body for obtaining is placed in vacuum impregnation tank together with shaping mould, the vacuum impregnation tank is sealed and is locked, and taken out
Vacuum is to 10-2~10-4Atm, more preferably 10-4atm；It is again that silicone precursor mixed liquor injection obtained in step (2) is described
In vacuum impregnation tank, liquid level is set not have the shaping mould upper surface, opening atmospheric valve makes air pressure balance in tank body quiet to 1atm
Put 24~100 hours so that silicones full cross-linked solidification at room temperature.
Some preferred embodiment in, carbonization treatment is specially in the step (3)：Carbon fiber after solidification is firm
Property thermal insulation tile blank is put into carbide furnace, and 600~1000 DEG C (such as 600 DEG C, 800 DEG C or 1000 are warming up under an argon atmosphere
DEG C), it is incubated 1~10 hour (such as 1,2,5 or 10 hours) so that silicones carbonization, generation Si/C/O glass bonding phases.
In an implementation method being more highly preferred to, 800 DEG C are heated in argon gas atmosphere stove, are incubated 2 hours, obtain Carbon Fiber Rigid
The ripe base of thermal insulation tile.
Some preferred embodiment in, step (3) high temperature heat treatment is specially：Add in argon gas atmosphere stove
Heat to 1500~2200 DEG C (such as 1500 DEG C, 1800 DEG C or 2200 DEG C) and be incubated (such as 1,2,5 or 10 are small within 1~10 hour
When).For example, the ripe base of Carbon Fiber Rigid thermal insulation tile is put into the pyrolysis furnace of argon gas atmosphere, 1800 DEG C are warming up to, are incubated 1 hour,
To eliminate the thermal stress that resin solidification, carbonisation are accumulated in thermal insulation tile base substrate, Carbon Fiber Rigid thermal insulation tile product is finally given
Product.
Fig. 2 and Fig. 3 is please referred to, is the Carbon Fiber Rigid thermal insulation tile according to obtained in the preferred embodiment of the present invention
Material object shoots picture and stereoscan photograph.From fig. 2 it can be seen that the Carbon Fiber Rigid thermal insulation tile includes chopped carbon fiber bone
Frame, and the Si/C/O glass of the cracking being distributed between chopped carbon fiber is bonded phase, and Si/C/O glass bonding is mutually covered in carbon
Fiber surface and carbon fiber and the point of intersection of carbon fiber, play a part of to be bonded chopped carbon fiber skeleton.
The present invention will be hereafter further detailed in the form of embodiment, but because the present inventor can not possibly
There is no need exhaustively to show all technical schemes obtained based on present inventive concept, protection scope of the present invention should not necessarily be limited by
Following examples, and all technical schemes obtained based on present inventive concept should be included.
Embodiment 1
1. a diameter of 10 μm of carbon fiber is prescinded long to 2mm, chopped carbon fiber is placed in the kettle for filling acetone, kettle top
Stirring and water cooled reflux device are installed.Stirring and water cooled reflux device are opened, acetone are heated to 55 DEG C and are flowed back 48 hours,
The epoxy resin adhesive thoroughly cleaning that will be attached to carbon fiber surface is fallen.The carbon fiber that will be cleaned in kettle is gone out by strainer filtering
Come, dried in fume hood so that acetone fully volatilizees.
2. by the chopped carbon fiber after removing glue according to mass ratio be 1:150 mix with deionized water, in agitator fully
Stirring to pulp, slurry is transferred in filtering frock, filters off the water of the overwhelming majority, and wet base then is loaded into shaping mould, according to
Wet base is depressed into default height by the target density of material, is dried 24 hours at 120 DEG C, obtains carbon fiber dry body.
3. the carbon fiber dry body with shaping mould is placed in vacuum impregnation tank, impregnating autoclave is sealed and locked, then
Impregnating autoclave is evacuated to 10-2atm。
4. silicones precursor mixed liquor is prepared：By hydroxyl endblocked polydimethylsiloxane, tetraethyl orthosilicate, tin dilaurate
Dibutyl tin and dimethylbenzene are according to 10:1:0.1:It is standby after 50 mass ratio is well mixed.Wherein, hydroxy-end capped poly dimethyl silicon
The viscosity of oxygen alkane is 4000cst.
5. by step 4. obtained silicone precursor mixed liquor injection vacuum impregnation tank, liquid level is made not have the setting
Mould upper surface, opening atmospheric valve makes air pressure balance in tank body to 1atm, stand 24 hours so that silicones is full cross-linked solid
Change.
6. the Carbon Fiber Rigid thermal insulation tile blank after solidification is put into carbide furnace, 800 DEG C is warming up under an argon atmosphere,
Insulation 2 hours so that silicones carbonization, generation Si/C/O glass bonding phases.
7. the ripe base of Carbon Fiber Rigid thermal insulation tile for 6. step being prepared is put into the pyrolysis furnace of argon gas atmosphere, is warming up to 1800
DEG C, 2 hours are incubated, to eliminate the thermal stress that resin solidification, carbonisation are accumulated in thermal insulation tile base substrate, finally give carbon fiber
Rigid thermal insulation tile product.
Embodiment 2 to 22
In addition to the content shown in lower form 1 and form 2, carry out in the same manner as example 1 embodiment 2 to
22.The mechanical strength of the obtained Carbon Fiber Rigid thermal insulation tile of test, as a result referring to table 2.
Comparative example 1~2
The present invention is also using fibrous insulating material disclosed in United States Patent (USP) 3577344 as a comparison case 1.Specifically prepared
Journey is as follows：The carbon fiber that average diameter is 0.5~0.7 μm is cut into 0.25 inch long, then by after the mixing of carbon fiber, starch and water
Mashing, starch and the mass ratio of carbon fiber are 0.75 in obtained slurry:1, and the ratio of carbon fiber and water is fine every 1kg carbon
Dimension correspondence 380L water.Slurry is filtered by 0.25 inch of filter screen, and continues stirring 30 minutes, to be then poured into mould
In.It is dehydrated 7 minutes by vacuum tank in communication, and the temperature of mould increases to 95 degrees Celsius.In the atmosphere of saturated steam
Lower persistently standing 4 hours are enclosed, makes starch gelatinization.Afterwards, obtained compound is dried 24 hours in the environment of compared with low humidity,
Then in 1000 degrees Centigrade 16 hours realizing being carbonized.After testing, the thickness direction pressure of the fibrous insulating material of comparative example 1
Contracting intensity is specially 0.1~0.2MPa.Therefore compressive strength of the Carbon Fiber Rigid thermal insulation tile that prepared by the present invention in thickness direction
The fibrous insulating material prepared than comparative example 1 is generally higher by 20%~50%, and what is had is even higher by more than 100%.Because
Starch of the carbon yield higher than gelatinization that silicones is cracked under an inert atmosphere in obtained Carbon Fiber Rigid thermal insulation tile of the invention.
The present invention is also using Carbon Fiber Rigid thermal insulation tile disclosed in United States Patent (USP) 4152482 as a comparison case 2.Specific system
Standby process is as follows：The carbon fiber that average diameter is 5~7 μm is cut into 250 μm long, then by carbon fiber and phenolic resin according to 1:
0.35 mass ratio is mixed, and wherein the particle diameter of phenolic resin is 10 μm or so, and by the filter screen of 0.5mm to carbon fiber
Filtered.It is beaten after then adding water in the mixture, wherein adding 300L water per 1kg mixtures, slurry is persistently stirred
20 minutes, it is then poured into mould.It is dehydrated 15 minutes by vacuum tank in communication, and carbon fiber and phenolic resin are constituted
Compound tiles shaping in the presence of vacuum.Mold temperature is heated to 130 DEG C.Being stood under air atmosphere makes phenolic aldehyde in 24 hours
Resin solidification, and remove unnecessary moisture.Obtained material is heated to 1000 DEG C, and 30 points of continuous heating under nitrogen atmosphere
Carbonization is realized after clock, the Carbon Fiber Rigid thermal insulation tile of comparative example 2 is obtained.5min detections are heated at 1200 DEG C, under air atmosphere right
The antioxygenic property of the Carbon Fiber Rigid thermal insulation tile of ratio 2.Test result indicate that, Carbon Fiber Rigid prepared by comparative example 2 is heat-insulated
Watt 1200 DEG C occur combustion phenomena, final residual quality be 0.5%.And the present invention is cracked under an inert atmosphere due to silicones
Product Si/C/O glass bonding mutually there is inoxidizability, therefore Carbon Fiber Rigid thermal insulation tile obtained in embodiment 1-11 is 1200
DEG C heating 5min after structure do not cave in, quality increase be 10%~20%.
Claims (10)
1. a kind of Carbon Fiber Rigid thermal insulation tile, it is characterised in that the chopped carbon fiber including constituting skeleton, and for being bonded
State the Si/C/O glass bonding phase of chopped carbon fiber.
2. Carbon Fiber Rigid thermal insulation tile according to claim 1, it is characterised in that the Si/C/O glass bonding is by silicon
Resin prepolymer, crosslinking agent, catalyst and organic solvent are according to 10:(0.1~10):(0.1~10):The quality of (10~100)
In being configured to after silicone precursor mixed liquor suck carbon fiber dry body by Vacuum infusion techniques, then by cold curing,
Obtained after carbonization and high-temperature heat treatment.
3. Carbon Fiber Rigid thermal insulation tile according to claim 2, it is characterised in that：
The silicone prepolymer is selected from by hydroxyl endblocked polydimethylsiloxane, hydroxy-end capped polydiphenylsiloxane, hydroxyl
Dimethyl silicone polymer, amino-terminated dimethyl silicone polymer and epoxy radicals end-blocking dimethyl silicone polymer that end-blocking phenyl replaces
The mixture of one or several in the group of composition；The viscosity of the silicone prepolymer is 200~100000cst；And/or
The crosslinking agent be selected from by tetraethyl orthosilicate, methyl silicate, MTMS, MTES and
The mixture of one or several in the group of dimethyldiethoxysilane composition；And/or
The catalyst is dibutyl tin laurate or γ-amine propyl-triethoxysilicane；And/or
The organic solvent is selected from the mixture of one or several in the group being made up of benzene, dimethylbenzene, styrene and acetone.
4. Carbon Fiber Rigid thermal insulation tile according to claim 1 and 2, it is characterised in that the length of the carbon fiber is 1~
5mm, a diameter of 8~12 μm.
5. a kind of preparation method of Carbon Fiber Rigid thermal insulation tile, it is characterised in that comprise the following steps：
(1) the wet base of chopped carbon fiber is obtained by wet moulding, carbon fiber dry body is obtained after drying；
(2) silicone precursor mixed liquor is obtained after mixing silicone prepolymer, crosslinking agent, catalyst and organic solvent；
(3) impregnate the carbon fiber dry body using silicone precursor mixed liquor, then by cold curing, carbonization and warm high at
Carbon Fiber Rigid thermal insulation tile is obtained after reason.
6. the preparation method of Carbon Fiber Rigid thermal insulation tile according to claim 5, it is characterised in that in the step (2)：
According to 10:(0.1~10):(0.1~10):The mass ratio of (10~100) is by silicone prepolymer, crosslinking agent, catalyst
Silicone precursor mixed liquor is obtained with after organic solvent mixing.
7. the preparation method of the Carbon Fiber Rigid thermal insulation tile according to claim 5 or 6, it is characterised in that the step (2)
In：
The silicone prepolymer is selected from by hydroxyl endblocked polydimethylsiloxane, hydroxy-end capped polydiphenylsiloxane, hydroxyl
Dimethyl silicone polymer, amino-terminated dimethyl silicone polymer and epoxy radicals end-blocking dimethyl silicone polymer that end-blocking phenyl replaces
The mixture of one or several in the group of composition；The viscosity of the silicone prepolymer is 200~100000cst；And/or
The crosslinking agent be selected from by tetraethyl orthosilicate, methyl silicate, MTMS, MTES and
The mixture of one or several in the group of dimethyldiethoxysilane composition；And/or
The catalyst is dibutyl tin laurate or γ-amine propyl-triethoxysilicane；And/or
The organic solvent is selected from the mixture of one or several in the group being made up of benzene, dimethylbenzene, styrene and acetone.
8. the preparation method of Carbon Fiber Rigid thermal insulation tile according to claim 5, it is characterised in that in the step (1)：
By chopped carbon fiber and water according to 1:150~250 mass ratio mixing, is filtrated to get wet base after stirring to pulp, then will be wet
Base loads shaping mould, and wet base is depressed into preset height by the target density according to material, 4~36 is dried at 60~150 DEG C small
When, obtain carbon fiber dry body.
9. the preparation method of Carbon Fiber Rigid thermal insulation tile according to claim 5, it is characterised in that in the step (1)
Also include removing glue step：
Carbon fiber is prescinded to 1~5mm, chopped carbon fiber is obtained, chopped carbon fiber is mixed with acetone, returned in stirring and water-cooled
Under conditions of stream, acetone is heated to 55~60 DEG C and is flowed back 24~72 hours, cleaning is attached to the ring on chopped carbon fiber surface
Oxygen tree Lipophylic surfaces inorganic agent, then by strainer filtering, then makes acetone obtain chopped carbon fiber after volatilizing.
10. the preparation method of Carbon Fiber Rigid thermal insulation tile according to claim 5, it is characterised in that the step (3)
In：
Vacuum impregnation and cold curing are specially：The carbon fiber dry body that step (1) is obtained first is placed in vacuum together with shaping mould
In impregnating autoclave, the vacuum impregnation tank is sealed and 10 are evacuated to-2~10-4atm；By silicones forerunner obtained in step (2)
Body mixed liquor is injected in the vacuum impregnation tank, liquid level was not had the shaping mould upper surface, and opening atmospheric valve makes in tank body
Air pressure balance stands 24~100 hours so that silicones crosslinking curing to 1atm；And/or
The carbonization is heated to 600~1000 DEG C in argon gas atmosphere stove and is incubated 1~10 hour；And/or
The high-temperature heat treatment is heated to 1500~2200 DEG C in argon gas atmosphere stove and is incubated 1~10 hour.
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| CN114014685B (en) * | 2021-11-26 | 2023-06-23 | 航天特种材料及工艺技术研究所 | Antioxidant porous carbon ceramic composite material and preparation method thereof |
| CN114524680B (en) * | 2022-01-19 | 2023-05-02 | 东华大学 | Ceramic nanofiber material with internally overlapped nano film and preparation method thereof |
| CN115991608B (en) * | 2022-12-26 | 2024-05-10 | 内蒙古航天红岗机械有限公司 | Preparation method of endogenous fiber reinforced carbon/Tao Hou lining material |
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