CN106747267B - 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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- CN106747267B CN106747267B CN201611100591.5A CN201611100591A CN106747267B CN 106747267 B CN106747267 B CN 106747267B CN 201611100591 A CN201611100591 A CN 201611100591A CN 106747267 B CN106747267 B CN 106747267B
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Abstract
The present invention relates to a kind of Carbon Fiber Rigid thermal insulation tiles, the chopped carbon fiber including constituting skeleton, and the Si/C/O glass for being bonded the chopped carbon fiber is bonded phase.The present invention also provides the preparation methods of the Carbon Fiber Rigid thermal insulation tile.The present invention prepares the bonding phase between carbon fiber using silicone resin, Si/C/O glass, which is generated, when being carbonized cracking is bonded phase, play the role of being bonded chopped carbon fiber skeleton, and after mutually being aoxidized under high temperature aerobic environment due to Si/C/O glass bonding, surface can generate layer of silicon dioxide glass-film, to prevent oxygen atom from further aoxidizing internal substance, therefore there is stronger inoxidizability, and the carbon yield that silicone resin cracks under an inert atmosphere is high, with use starch as binder compared with, 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 sides
Method.
Background technique
Carbon Fiber Rigid thermal insulation tile has many advantages, such as that heatproof is high, light porous, good heat-insulation effect, can be directly as superhigh temperature
Heat-barrier material uses, 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 uses the oxide ceramic fibres such as chopped carbon fiber, quartz fibre or alumina silicate to be raw material, solubility is used to form sediment
Powder is bonding agent, prepares corresponding fibrous insulating material green body by wet therapy forming process, and then makes the starch after gelatinization polymerization
Cracking forms bonding charcoal phase in high temperature furnace.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 cracks in high temperature furnace is lower, 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 disclosed in U.S. Department of Energy in United States Patent (USP) 4152482
Tie up the preparation process amelioration of heat-barrier material.United States Patent (USP) 4152482, by layered filtration, multi-shell curing technique, eliminate viscous
The stress accumulation generated in fibrous matrix when connecing phase resin solidification.In addition, layered filtration technique makes the light fibre heat-insulated
The structure of material is more controllable, and different fibrous matrixes, high emissivity filler etc. can be used to realize product in different layers
It can change of gradient.Fibrous material partnership of the U.S. (Fiber Materials Incorporation, FMI) produces one kind
The trade mark isCarbon fiber light rigidity thermal insulation tile.The carbon fiber that diameter is 14-16 microns is chopped to 1.6mm
It is long, rear wet forming is mixed with beating with water soluble phenol resin and solvent, after phenolic resin curing under 1440 ℉ (782.2 DEG C)
Carbonization, and then be made 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. is prepared for a kind of carbon fiber-based ablator PICA (phenolic impregnated 3-
D fine-woven pierced carbon fabric ablator), density is 0.352~0.701g/cm3,
4.5MW/m2Oxygen/acetylene torch ablation test in, 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 by 3D and punctures the preparation of carbon fiber precast body composite phenolic resin.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, lead to it
Inoxidizability is not high, and temperature tolerance is insufficient.
Summary of the invention
The purpose of the present invention is overcoming the disadvantage that existing Carbon Fiber Rigid thermal insulation tile mechanical strength is inadequate, temperature tolerance is insufficient,
Finally provide that a kind of temperature tolerance is higher, carbon fiber light rigidity lightweight, that intensity is bigger using different technical solutions
Thermal insulation tile and preparation method thereof can be used as oxygen-free atmosphere super high sintering temperature furnace, nuclear power station high-temperature service, chemical reactor etc.
Thermally protective materials use.
For this purpose, the present invention achieves the object of the present invention by following technical solution:
1, a kind of Carbon Fiber Rigid thermal insulation tile, wherein the chopped carbon fiber including constituting skeleton, and it is described for being bonded
The Si/C/O glass of chopped carbon fiber is bonded phase.
2, Carbon Fiber Rigid thermal insulation tile according to technical solution 1, wherein the Si/C/O glass bonding is mutually by silicon tree
Rouge prepolymer, crosslinking agent, catalyst and organic solvent are according to 10:(0.1~10): (0.1~10): the mass ratio of (10~100)
It is sucked in carbon fiber dry body after being configured to silicone precursor mixed liquor by Vacuum infusion techniques, using room temperature curing, carbon
Change and is obtained after high-temperature heat treatment.
3, the Carbon Fiber Rigid thermal insulation tile according to technical solution 2, in which:
The silicone prepolymer be selected from by hydroxyl endblocked polydimethylsiloxane, hydroxy-end capped polydiphenylsiloxane,
Dimethyl silicone polymer, amino-terminated dimethyl silicone polymer and the epoxy radicals end-blocking poly dimethyl silicon that hydroxy-end capped phenyl replaces
One of group of oxygen alkane composition or several mixtures；The viscosity of the silicone prepolymer is 200~100000cst；With/
Or
The crosslinking agent is selected from by ethyl orthosilicate, methyl orthosilicate, methyltrimethoxysilane, methyltriethoxy silane
One of group of alkane and dimethyl diethoxysilane composition or several mixtures；And/or
The catalyst is dibutyl tin dilaurate or γ-amine propyl-triethoxysilicane；And/or
The organic solvent is selected from one of group being made of benzene, dimethylbenzene, styrene and acetone or several mixing
Object.
4, the Carbon Fiber Rigid thermal insulation tile according to technical solution 1 or 2, wherein the length of the carbon fiber be 1~
5mm, diameter are 8~12 μm.
5, a kind of preparation method of Carbon Fiber Rigid thermal insulation tile, wherein the following steps are included:
(1) the wet base of chopped carbon fiber is obtained by wet forming, carbon fiber dry body is obtained after drying；
(2) silicone precursor is made 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, using room temperature curing, carbonization and high temperature
Carbon Fiber Rigid thermal insulation tile is obtained after heat treatment.
6, the preparation method of the Carbon Fiber Rigid thermal insulation tile according to technical solution 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 made after agent and organic solvent mixing.
7, the preparation method of the Carbon Fiber Rigid thermal insulation tile according to technical solution 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 the epoxy radicals end-blocking poly dimethyl silicon that hydroxy-end capped phenyl replaces
One of group of oxygen alkane composition or several mixtures；The viscosity of the silicone prepolymer is 200~100000cst；With/
Or
The crosslinking agent is selected from by ethyl orthosilicate, methyl orthosilicate, methyltrimethoxysilane, methyltriethoxy silane
One of group of alkane and dimethyl diethoxysilane composition or several mixtures；And/or
The catalyst is dibutyl tin dilaurate or γ-amine propyl-triethoxysilicane；And/or
The organic solvent is selected from one of group being made of benzene, dimethylbenzene, styrene and acetone or several mixing
Object.
8, the preparation method of the Carbon Fiber Rigid thermal insulation tile according to technical solution 5, wherein in the step (1):
Chopped carbon fiber is mixed with water according to the mass ratio of 1:150~250, wet base is obtained by filtration after stirring to pulp, then
Wet base is packed into shaping mould, wet base is depressed by preset height according to the target density of material, dry 4 at 60~150 DEG C~
36 hours, obtain carbon fiber dry body.
9, the preparation method of the Carbon Fiber Rigid thermal insulation tile according to technical solution 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, is 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 treating agent, obtain chopped carbon fiber then by strainer filtering, then after making acetone volatilize.
10, the preparation method of the Carbon Fiber Rigid thermal insulation tile according to technical solution 5, wherein in the step (3):
Vacuum impregnation and room temperature curing specifically: be first placed in the carbon fiber dry body that step (1) obtains together with shaping mould
In vacuum impregnation tank, the vacuum impregnation tank is sealed and is evacuated to 10-2~10-4atm；By silicone resin made from step (2)
Presoma mixed liquor injects in the vacuum impregnation tank, and liquid level is made not have the shaping mould upper surface, and opening blow valve makes tank
Internal air pressure balance stands 24~100 hours, so that silicone resin crosslinking curing to 1atm；And/or
The carbonization is heated to 600~1000 DEG C in argon gas atmosphere stove and keeps the temperature 1~10 hour；And/or
The high-temperature heat treatment is heated to 1500~2200 DEG C in argon gas atmosphere stove and keeps the temperature 1~10 hour.
Implement Carbon Fiber Rigid thermal insulation tile and preparation method thereof of the invention, has the advantages that
1, the present invention prepares the bonding phase between carbon fiber using silicone resin, and it is viscous to generate Si/C/O glass when being carbonized cracking
Phase is connect, which is bonded the point of intersection for being mutually covered on carbon fiber surface and carbon fiber and carbon fiber, plays bonding and is chopped
The effect of carbon fiber skeleton, and since Si/C/O glass bonding is mutually under high temperature aerobic environment after oxidation, surface can generate one
Layer silica glass film has inoxidizability so that oxygen atom be prevented further to aoxidize internal substance.Therefore, with use
Phenolic resinoid residue carbon of biomass pyrolysis is compared as the material of bonding phase, the inoxidizability of Carbon Fiber Rigid thermal insulation tile produced by the present invention
It is stronger.On the other hand, with use starch as binder compared with, carbon yield that silicone resin of the invention cracks under an inert atmosphere
Higher than the starch of gelatinization, therefore mechanical strength is also higher by 20%~50%.
2, the present invention makes silicone precursor mixed liquor sufficiently in conjunction with carbon fiber dry body by vacuum impregnation technique, is formed
Carbon Fiber Rigid thermal insulation tile it is uniform in material, overall performance stablize, be more advantageous to Si/C/O glass bonding mutually play its bonding make
With.
3, present invention optimizes the proportions of each raw material in the silicone precursor mixed liquor used, when silicone resin pre-polymerization
Object, 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 of cracking mutually to more uniformly spread, mechanical strength is higher, and antioxygenic property is more preferable.
Detailed description of the invention
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 the shooting picture in kind of the Carbon Fiber Rigid thermal insulation tile according to made from the preferred embodiment of the present invention；
Fig. 3 is the Carbon Fiber Rigid thermal insulation tile stereoscan photograph according to made from the preferred embodiment of the present invention.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention
In attached drawing, technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described embodiment is
A part of the embodiments of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, ordinary skill people
Member's every other embodiment obtained without making creative work, shall fall within the protection scope of the present 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 the chopped carbon fiber for constituting skeleton, and the Si/C/O glass for being bonded the chopped carbon fiber is bonded phase.
In some preferred embodiments, the length of chopped carbon fiber is 1~5mm, and diameter is 8~12 μm.Further
Preferably, the length of chopped carbon fiber is 2mm, and diameter is 10 μm.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 embodiments, Si/C/O glass bonding mutually by silicone prepolymer A, crosslinking agent B,
Catalyst C and organic solvent D is sucked in carbon fiber dry body after being configured to silicone precursor mixed liquor by Vacuum infusion techniques,
Using being obtained after room temperature curing, carbonization and high-temperature heat treatment.Preferably, silicone prepolymer in silicone precursor mixed liquor
A, the mass ratio of crosslinking agent B, catalyst C and organic solvent D is 10:(0.1~10): (0.1~10): (10~100).Such as it can
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 silicone resin.Silicone resin disperse phase is after hardening in carbon fiber surface
Face and carbon fiber and carbon fiber point of intersection are evenly dispersed.When 800 DEG C of carbonizations crack, it is viscous that silicone resin is cracked to form Si/C/O glass
Connect phase, i.e. SiCxOyGlass phase, the glass phase are covered on the point of intersection of carbon fiber surface and carbon fiber and carbon fiber, play bonding
The effect of chopped carbon fiber skeleton.After mutually being aoxidized under high temperature aerobic environment due to Si/C/O glass bonding, surface can generate one
Layer silica glass film, to prevent oxygen atom from further aoxidizing internal substance, therefore Si/C/O glass bonding mutually has
Inoxidizability, when undergoing high temperature, ablation shrinkage is smaller, high reliablity；If replacing silicon using epoxy resin or phenolic aldehyde
If resin, oxygen abundance under conditions of ablation after basic noresidue, ablation shrinkage is big, thus reliability obviously compared with
It is low.
In some preferred embodiments, the silicone prepolymer A is selected from by hydroxy-end capped polydimethylsiloxanes
Dimethyl silicone polymer, the amino-terminated poly dimethyl silicon that alkane, hydroxy-end capped polydiphenylsiloxane, hydroxy-end capped phenyl replace
One of group of oxygen alkane and epoxy radicals end-blocking dimethyl silicone polymer composition or several mixtures.Wherein hydroxy-end capped phenyl
Substituted dimethyl silicone polymer can replace for part phenyl, and degree of substitution can be 30% to 70%.It may further be preferable that
The viscosity of the silicone prepolymer is 200~100000cst；Further preferably 10000~20000CSt；In addition further excellent
It is selected as 2000~4000CSt.
In some preferred embodiments, the crosslinking agent B is selected from by ethyl orthosilicate, methyl orthosilicate, methyl
One of group of trimethoxy silane, methyltriethoxysilane and dimethyl diethoxysilane composition or several mixing
Object；It may further be preferable that the crosslinking agent B is ethyl orthosilicate.
In some preferred embodiments, the catalyst C is dibutyl tin dilaurate or γ-three second of amine propyl
Oxysilane.The inventors discovered that using dibutyl tin dilaurate as catalyst in system of the invention, capable of making
It obtains curing reaction speed faster, the time is fully cured no more than 24 hours；If using other catalyst such as γ-amine propyl
For triethoxysilane as catalyst, being fully cured the time then needs 48 hours or more.Therefore in some preferred embodiments
In, the catalyst C is dibutyl tin dilaurate.
In some preferred embodiments, the organic solvent D is selected from and is made of benzene, dimethylbenzene, styrene and acetone
One of group or several mixtures；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 ethyl orthosilicate, catalyst C
For dibutyl tin dilaurate, organic solvent D is dimethylbenzene, obtains silicon after mixing according to the mass ratio of 10:1:0.1:50
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 includes such as
Lower step:
(1) the wet base of chopped carbon fiber is obtained by wet forming, carbon fiber dry body is obtained after drying；
(2) silicone precursor is made after mixing silicone prepolymer, crosslinking agent, catalyst and organic solvent to mix
Liquid；
(3) silicone precursor mixed liquor impregnation of carbon fibers dry body is used, such as carbon fiber is impregnated by vacuum impregnation technique
Dry body is tieed up, to make carbon fiber dry body absorb the silicone precursor mixed liquor, using room temperature curing, carbonization and high warm
Carbon Fiber Rigid thermal insulation tile is obtained after processing.
In some preferred embodiments, in the step (1): by chopped carbon fiber and water according to 1:150~250
Mass ratio mixes, and wet base is obtained by filtration after stirring to pulp, then wet base is packed into shaping mould, will be wet according to the target density of material
Base is depressed into preset height, 4~36 hours dry at 60~150 DEG C, obtains carbon fiber dry body.It specifically, will be except short after glue
It cuts carbon fiber to mix with deionized water, mashing is sufficiently stirred in agitator, slurry is transferred in filtering tooling, filter off big absolutely
Then wet base is packed into shaping mould, wet base is depressed into scheduled height according to the target density of material by partial water, 60~
Dry 4~36 hours (4,10,20,30 or 36), it is dry to obtain carbon fiber under 150 DEG C (such as 60 DEG C, 80 DEG C, 100 DEG C or 150 DEG C)
Base；Chopped carbon fiber and the mass ratio of deionized water are 1:150~250 (such as 1:150,1:200 or 1:250), further excellent
It is selected as 1:200.
Further include except glue step in some preferred embodiments, in the step (1): i.e. by diameter for 8~
12 μm of carbon fiber obtains chopped carbon fiber after prescinding to 1~5mm long.Chopped carbon fiber is mixed with acetone then, is being stirred
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 treating agent on surface obtains chopped carbon fiber then by strainer filtering, then after making acetone volatilize.Tool
Body, chopped carbon fiber is placed in the kettle for filling acetone, kettle top is equipped with stirring and water cooled reflux device.Opening stirs mixing water
Acetone is heated to 55~60 DEG C (such as 55 DEG C, 58 DEG C or 60 DEG C) and flowed back 24~72 hours (24,36,48 by cold reflux device
Or 72 hours), the epoxy resin adhesive for being attached to carbon fiber surface is thoroughly washed.A kind of optimization except glue program is perseverance
60 DEG C of temperature are flowed back 48 hours, which is enough thoroughly to clean up the epoxy resin adhesive for being attached to carbon fiber surface.With
Afterwards, the carbon fiber cleaned in kettle is come out by strainer filtering, is dried in draught cupboard, so that acetone sufficiently volatilizees.
In some preferred embodiments, 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 made silicone precursor mix
Liquid.It such as 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
Rouge prepolymer A, crosslinking agent B, catalyst C and organic solvent D are as described in the first aspect of the invention.
In some preferred embodiments, vacuum impregnation and room temperature curing in the step (3) specifically: first by step
(1) the carbon fiber dry body obtained is placed in vacuum impregnation tank together with shaping mould, and the vacuum impregnation tank is sealed and is locked, and is taken out
Vacuum is to 10-2~10-4Atm, more preferably 10-4atm；It again will be described in the injection of silicone precursor mixed liquor made from step (2)
In vacuum impregnation tank, liquid level is made not have the shaping mould upper surface, opening blow valve keeps air pressure balance in tank body quiet to 1atm
It sets 24~100 hours, so that silicone resin full cross-linked solidification at room temperature.
In some preferred embodiments, carbonization treatment in the step (3) specifically: the carbon fiber after solidification is rigid
Property thermal insulation tile blank is put into carbide furnace, is warming up to 600~1000 DEG C (such as 600 DEG C, 800 DEG C or 1000 under an argon atmosphere
DEG C), 1~10 hour (such as 1,2,5 or 10 hour) is kept the temperature, so that silicone resin carbonization, generates Si/C/O glass and be bonded phase.
In one more preferably embodiment, it is heated to 800 DEG C in argon gas atmosphere stove, keeps the temperature 2 hours, obtains Carbon Fiber Rigid
The ripe base of thermal insulation tile.
In some preferred embodiments, step (3) the high temperature heat treatment specifically: add in argon gas atmosphere stove
Heat is to 1500~2200 DEG C (such as 1500 DEG C, 1800 DEG C or 2200 DEG C) and keeps the temperature 1~10 hour (such as 1,2,5 or 10 are small
When).For example, the ripe base of Carbon Fiber Rigid thermal insulation tile is put into the pyrolysis furnace of argon atmosphere, 1800 DEG C are warming up to, keeps the temperature 1 hour,
With the thermal stress for eliminating resin solidification, carbonisation accumulates in thermal insulation tile green body, the production of Carbon Fiber Rigid thermal insulation tile is finally obtained
Product.
Fig. 2 and Fig. 3 are please referred to, is the Carbon Fiber Rigid thermal insulation tile according to made from the preferred embodiment of the present invention
Material object shooting 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 bonding phase of the cracking that is distributed between chopped carbon fiber, Si/C/O glass bonding are mutually covered on carbon
The point of intersection of fiber surface and carbon fiber and carbon fiber plays the role of being bonded chopped carbon fiber skeleton.
The present invention will be hereafter further detailed in the form of embodiment, but since the present inventor can not
Present inventive concept all technical solutions obtained are based on It is not necessary to exhaustively show, protection scope of the present invention should not necessarily be limited by
Following examples, and should include being based on present inventive concept all technical solutions obtained.
Embodiment 1
1. prescinding the carbon fiber that diameter is 10 μm to 2mm long, 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 is heated to 55 DEG C and is flowed back 48 hours,
The epoxy resin adhesive for being attached to carbon fiber surface is thoroughly washed.The carbon fiber cleaned in kettle is gone out by strainer filtering
Come, is dried in draught cupboard, so that acetone sufficiently volatilizees.
2. abundant in agitator by according to mass ratio being that 1:150 is mixed with deionized water except the chopped carbon fiber after glue
Slurry is transferred in filtering tooling, filters off the water of the overwhelming majority, wet base is then packed into shaping mould by stirring to pulp, according to
Wet base is depressed into preset height by the target density of material, 24 hours dry 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. preparing silicone resin precursor mixed liquor: by hydroxyl endblocked polydimethylsiloxane, ethyl orthosilicate, tin dilaurate
Dibutyl tin and dimethylbenzene are spare after mixing according to the mass ratio of 10:1:0.1:50.Wherein, hydroxy-end capped poly dimethyl silicon
The viscosity of oxygen alkane is 4000cst.
5. making liquid level not have the setting in step 4. silicone precursor mixed liquor injection vacuum impregnation tank obtained
Mould upper surface, opening blow valve makes air pressure balance in tank body 24 hours be stood, so that silicone resin is full cross-linked solid to 1atm
Change.
6. the Carbon Fiber Rigid thermal insulation tile blank after solidification is put into carbide furnace, it is warming up to 800 DEG C under an argon atmosphere,
Heat preservation 2 hours, so that silicone resin carbonization, generates Si/C/O glass and be bonded phase.
7. the 6. ripe base of Carbon Fiber Rigid thermal insulation tile that step is prepared is put into the pyrolysis furnace of argon atmosphere, it is warming up to 1800
DEG C, 2 hours are kept the temperature, with the thermal stress for eliminating resin solidification, carbonisation accumulates in thermal insulation tile green body, finally obtains carbon fiber
Rigid thermal insulation tile product.
Embodiment 2 to 22
Other than the content shown in the lower table 1 and table 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 also use United States Patent (USP) 3577344 disclosed in fibrous insulating material as a comparison case 1.Specifically prepared
Journey is as follows: it is 0.25 inch long to be that 0.5~0.7 μm of carbon fiber is cut into for average diameter, then will be after carbon fiber, starch and water mixes
It is beaten, the mass ratio of starch and carbon fiber is 0.75:1 in slurry obtained, and the ratio of carbon fiber and water is every 1kg carbon fiber
Tie up corresponding 380L water.Slurry is filtered by 0.25 inch of strainer, and continues stirring 30 minutes, is then poured into mold
In.It is dehydrated 7 minutes by vacuum tank in communication, and the temperature of mold increases to 95 degrees Celsius.In the atmosphere of saturated steam
Lower persistently standing 4 hours are enclosed, starch gelatinization is made.It is later, compound obtained is 24 hours dry in the environment of compared with low humidity,
Then at 1000 degrees Centigrade 16 hours to realize carbonization.Through detecting, 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 prepared by the present invention in thickness direction
The fibrous insulating material prepared than comparative example 1 is generally higher by 20%~50%, and some is even higher by 100% or more.This is because
The carbon yield that silicone resin cracks under an inert atmosphere in Carbon Fiber Rigid thermal insulation tile produced by the present invention is higher than the starch of gelatinization.
The present invention also use United States Patent (USP) 4152482 disclosed in Carbon Fiber Rigid thermal insulation tile 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 it is 250 μm long, then by carbon fiber and phenolic resin according to 1:
0.35 mass ratio is mixed, and wherein the partial size of phenolic resin is 10 μm or so, and by the strainer of 0.5mm to carbon fiber
It is filtered.It is beaten after water then is added in the mixture, wherein 300L water is added in every 1kg mixture, slurry is continued to stir
It 20 minutes, is then poured into mold.It is dehydrated 15 minutes by vacuum tank in communication, and carbon fiber and phenolic resin are constituted
Compound tiles molding under the action of vacuum.Mold temperature is heated to 130 DEG C.Standing 24 hours under air atmosphere makes phenolic aldehyde
Resin solidification, and remove extra moisture.Material obtained is heated to 1000 DEG C under nitrogen atmosphere, and continuous heating 30 divides
Carbonization is realized after clock, and the Carbon Fiber Rigid thermal insulation tile of comparative example 2 is made.5min detection pair is heated at 1200 DEG C, under air atmosphere
The antioxygenic property of the Carbon Fiber Rigid thermal insulation tile of ratio 2.The experimental results showed that Carbon Fiber Rigid prepared by comparative example 2 is heat-insulated
Watt in 1200 DEG C of generation combustion phenomena, final residual quality is 0.5%.And the present invention is cracked under an inert atmosphere due to silicone resin
Product Si/C/O glass bonding mutually there is inoxidizability, therefore Carbon Fiber Rigid thermal insulation tile made from embodiment 1-11 is 1200
DEG C heating 5min after structure do not collapse, quality increase be 10%~20%.
Claims (9)
1. a kind of Carbon Fiber Rigid thermal insulation tile, which is characterized 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；
Si/C/O glass bonding mutually by silicone prepolymer, crosslinking agent, catalyst and organic solvent according to 10:(0.1~
10): (0.1~10): the mass ratio of (10~100) is sucked after being configured to silicone precursor mixed liquor by Vacuum infusion techniques
In carbon fiber dry body, using being obtained after room temperature curing, carbonization and high-temperature heat treatment.
2. Carbon Fiber Rigid thermal insulation tile according to claim 1, it is characterised in that:
The silicone prepolymer is selected from by hydroxyl endblocked polydimethylsiloxane, hydroxy-end capped polydiphenylsiloxane, hydroxyl
Block dimethyl silicone polymer, amino-terminated dimethyl silicone polymer and epoxy radicals end-blocking dimethyl silicone polymer that phenyl replaces
One of group of composition or several mixtures；The viscosity of the silicone prepolymer is 200~100000cst；And/or
The crosslinking agent be selected from by ethyl orthosilicate, methyl orthosilicate, methyltrimethoxysilane, methyltriethoxysilane and
One of group of dimethyl diethoxysilane composition or several mixtures；And/or
The catalyst is dibutyl tin dilaurate or γ-amine propyl-triethoxysilicane；And/or
The organic solvent is selected from one of group being made of benzene, dimethylbenzene, styrene and acetone or several mixtures.
3. Carbon Fiber Rigid thermal insulation tile according to claim 1, which is characterized in that the length of the carbon fiber be 1~
5mm, diameter are 8~12 μm.
4. a kind of preparation method of Carbon Fiber Rigid thermal insulation tile, which comprises the following steps:
(1) the wet base of chopped carbon fiber is obtained by wet forming, carbon fiber dry body is obtained after drying；
(2) silicone precursor mixed liquor is made after mixing silicone prepolymer, crosslinking agent, catalyst and organic solvent；
(3) the carbon fiber dry body is impregnated using silicone precursor mixed liquor, at room temperature curing, carbonization and high warm
Carbon Fiber Rigid thermal insulation tile is obtained after reason.
5. the preparation method of Carbon Fiber Rigid thermal insulation tile according to claim 4, which is characterized 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 made with after organic solvent mixing.
6. the preparation method of Carbon Fiber Rigid thermal insulation tile according to claim 4, which is characterized in that in the step (2):
The silicone prepolymer is selected from by hydroxyl endblocked polydimethylsiloxane, hydroxy-end capped polydiphenylsiloxane, hydroxyl
Block dimethyl silicone polymer, amino-terminated dimethyl silicone polymer and epoxy radicals end-blocking dimethyl silicone polymer that phenyl replaces
One of group of composition or several mixtures；The viscosity of the silicone prepolymer is 200~100000cst；And/or
The crosslinking agent be selected from by ethyl orthosilicate, methyl orthosilicate, methyltrimethoxysilane, methyltriethoxysilane and
One of group of dimethyl diethoxysilane composition or several mixtures；And/or
The catalyst is dibutyl tin dilaurate or γ-amine propyl-triethoxysilicane；And/or
The organic solvent is selected from one of group being made of benzene, dimethylbenzene, styrene and acetone or several mixtures.
7. the preparation method of Carbon Fiber Rigid thermal insulation tile according to claim 4, which is characterized in that in the step (1):
Chopped carbon fiber is mixed with water according to the mass ratio of 1:150~250, wet base is obtained by filtration after stirring to pulp, then will be wet
Base is packed into shaping mould, and wet base is depressed into preset height according to the target density of material, and dry 4~36 is small at 60~150 DEG C
When, obtain carbon fiber dry body.
8. the preparation method of Carbon Fiber Rigid thermal insulation tile according to claim 4, which is characterized in that in the step (1)
Further include except glue step:
Carbon fiber is prescinded to 1~5mm, chopped carbon fiber is obtained, chopped carbon fiber is mixed with acetone, is returned in stirring and water cooling
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 resinae surface treating agent obtains chopped carbon fiber then by strainer filtering, then after so that acetone is volatilized.
9. the preparation method of Carbon Fiber Rigid thermal insulation tile according to claim 4, which is characterized in that in the step (3):
Vacuum impregnation and room temperature curing specifically: the carbon fiber dry body that step (1) obtains first is placed in vacuum together with shaping mould
In impregnating autoclave, the vacuum impregnation tank is sealed and is evacuated to 10-2~10-4atm；By silicone resin forerunner made from step (2)
Body mixed liquor injects in the vacuum impregnation tank, and liquid level is made not have the shaping mould upper surface, and opening blow valve makes in tank body
Air pressure balance stands 24~100 hours, so that silicone resin crosslinking curing to 1atm；And/or
The carbonization is heated to 600~1000 DEG C in argon gas atmosphere stove and keeps the temperature 1~10 hour；And/or
The high-temperature heat treatment is heated to 1500~2200 DEG C in argon gas atmosphere stove and keeps the temperature 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 |
| CN114213156B (en) * | 2021-12-28 | 2023-06-16 | 山东工业陶瓷研究设计院有限公司 | Preparation method of ceramic heat-insulating tile surface coating |
| 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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| CN104494225A (en) * | 2014-12-16 | 2015-04-08 | 山东工业陶瓷研究设计院有限公司 | Machinable silica aerogel composite rigid thermal insulating tile and preparation method thereof |
| CN105272322A (en) * | 2015-09-30 | 2016-01-27 | 航天特种材料及工艺技术研究所 | Light-weight, high temperature-resistance and heat-insulation ceramic fiber tile and making method thereof |
| CN105565845A (en) * | 2015-12-14 | 2016-05-11 | 天津大学 | Preparation method for porous ceramic fiber heat-insulation tile |
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| CN100415690C (en) * | 2006-06-30 | 2008-09-03 | 中国科学院上海硅酸盐研究所 | Process for preparing composite materials capable of forming oxidation-resisting structure on the surface of fiber by in-situ reaction |
| CN101591178B (en) * | 2008-05-30 | 2012-08-08 | 鞍山塞诺达碳纤维有限公司 | Method for manufacturing rigid carbon fiber heat insulating material and surface treatment method |
| WO2010104534A1 (en) * | 2009-03-12 | 2010-09-16 | Dow Corning Corporation | Thermal interface materials and mehtods for their preparation and use |
| CN102295465B (en) * | 2011-06-10 | 2013-05-01 | 陕西科技大学 | Hot-press preparation method of short carbon fiber/silicon carbide composite material |
| CN104610753B (en) * | 2015-01-26 | 2017-03-29 | 山东省科学院新材料研究所 | A kind of silicones coating layer material and its preparation and application |
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| CN104494225A (en) * | 2014-12-16 | 2015-04-08 | 山东工业陶瓷研究设计院有限公司 | Machinable silica aerogel composite rigid thermal insulating tile and preparation method thereof |
| CN105272322A (en) * | 2015-09-30 | 2016-01-27 | 航天特种材料及工艺技术研究所 | Light-weight, high temperature-resistance and heat-insulation ceramic fiber tile and making method thereof |
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