CN106829972A - A kind of hydrophobic aerogels and preparation method thereof, aerogel blanket - Google Patents
A kind of hydrophobic aerogels and preparation method thereof, aerogel blanket Download PDFInfo
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- CN106829972A CN106829972A CN201710077749.XA CN201710077749A CN106829972A CN 106829972 A CN106829972 A CN 106829972A CN 201710077749 A CN201710077749 A CN 201710077749A CN 106829972 A CN106829972 A CN 106829972A
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- hydrophobic aerogels
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- hydrophobic
- aerosil
- fluoroform
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- 230000002209 hydrophobic effect Effects 0.000 title claims abstract description 38
- 239000004964 aerogel Substances 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- XPDWGBQVDMORPB-UHFFFAOYSA-N Fluoroform Chemical compound FC(F)F XPDWGBQVDMORPB-UHFFFAOYSA-N 0.000 claims abstract description 52
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 45
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 42
- 238000006243 chemical reaction Methods 0.000 claims abstract description 33
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 21
- 229910002012 Aerosil® Inorganic materials 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000000047 product Substances 0.000 claims abstract description 14
- 238000012986 modification Methods 0.000 claims abstract description 10
- 230000004048 modification Effects 0.000 claims abstract description 9
- 125000002023 trifluoromethyl group Chemical group FC(F)(F)* 0.000 claims abstract description 8
- 230000003197 catalytic effect Effects 0.000 claims abstract description 5
- 239000012467 final product Substances 0.000 claims abstract 2
- 239000000463 material Substances 0.000 claims description 46
- 239000000835 fiber Substances 0.000 claims description 16
- 239000000377 silicon dioxide Substances 0.000 claims description 12
- 241000790917 Dioxys <bee> Species 0.000 claims description 2
- 229910003978 SiClx Inorganic materials 0.000 claims description 2
- 239000003365 glass fiber Substances 0.000 claims description 2
- 239000003292 glue Substances 0.000 claims description 2
- 238000007254 oxidation reaction Methods 0.000 claims description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims 1
- 230000004888 barrier function Effects 0.000 abstract description 4
- 239000011148 porous material Substances 0.000 abstract description 3
- 239000002131 composite material Substances 0.000 description 22
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical compound FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 description 16
- 238000000034 method Methods 0.000 description 12
- 230000008859 change Effects 0.000 description 10
- 238000010574 gas phase reaction Methods 0.000 description 10
- 238000009423 ventilation Methods 0.000 description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- 239000003795 chemical substances by application Substances 0.000 description 7
- 239000000499 gel Substances 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 7
- 230000000694 effects Effects 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- 230000008569 process Effects 0.000 description 4
- 239000011240 wet gel Substances 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 3
- 230000008878 coupling Effects 0.000 description 3
- 238000010168 coupling process Methods 0.000 description 3
- 238000005859 coupling reaction Methods 0.000 description 3
- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical compound C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 description 3
- 239000011810 insulating material Substances 0.000 description 3
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 2
- ZHNUHDYFZUAESO-UHFFFAOYSA-N Formamide Chemical compound NC=O ZHNUHDYFZUAESO-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- 125000000217 alkyl group Chemical group 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 239000004566 building material Substances 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 239000002274 desiccant Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 206010013786 Dry skin Diseases 0.000 description 1
- 239000004965 Silica aerogel Substances 0.000 description 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- 235000012255 calcium oxide Nutrition 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 1
- 229910000366 copper(II) sulfate Inorganic materials 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- NASVITFAUKYCPM-UHFFFAOYSA-N ethanol;tetraethyl silicate Chemical compound CCO.CCO[Si](OCC)(OCC)OCC NASVITFAUKYCPM-UHFFFAOYSA-N 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000001879 gelation Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 description 1
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 description 1
- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 description 1
- 239000000017 hydrogel Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 150000003961 organosilicon compounds Chemical class 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 229960001866 silicon dioxide Drugs 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- HUAUNKAZQWMVFY-UHFFFAOYSA-M sodium;oxocalcium;hydroxide Chemical group [OH-].[Na+].[Ca]=O HUAUNKAZQWMVFY-UHFFFAOYSA-M 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
- C01B33/157—After-treatment of gels
- C01B33/159—Coating or hydrophobisation
Landscapes
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
The invention provides a kind of hydrophobic aerogels and preparation method thereof, aerogel blanket.A kind of hydrophobic aerogels, have trifluoromethyl CF in the surface modification of aerosil3‑.Its preparation method is：Aerosil is set to be reacted with fluoroform under the catalytic action of ammonia, reaction temperature is 10 50 DEG C, obtains final product product.Innovative point of the invention be ingenious property aerosil surface connection on CF3, on the one hand only improve its surface hydrophobic, i.e., the barrier that blocks water is formed on its surface, the barrier also has good heat-resisting quantity, resistance to more than 900 DEG C of high temperature；On the other hand do not destroy the internal pore structure of aeroge again, it is kept the good characteristics such as specific surface area, porosity, density, the thermal conductivity of script level.
Description
Technical field
The present invention relates to chemical industry and building materials field, more particularly, to a kind of hydrophobic aerogels and preparation method thereof, airsetting
Rubber mat.
Background technology
Aerosil is the light nanoporous amorphous solid material of a kind of low-density, high porosity.Aeroge
The pore space structure (1~100nm) of nanoscale is included, with great specific surface area (200~1000m2/ g), hole very high
Rate (80~99.8%), very low density (1~500kg/m3) and the features such as small thermal conductivity factor, mechanics, acoustics, calorifics,
The aspects such as optics show the property of uniqueness.
Aerosil has shown that wide potential application foreground in many aspects, such as：Ultra heat insulating material,
Cerenkov detectors, efficient rechargeable battery, ultracapacitor, acoustic impedance coupling material, catalyst and carrier etc..But,
Without the SiO of surface modification2Aeroge surface is connected with hydrophilic radical-OH, and with porous structure, can cause SiO2Gas
Gel is easy to adsorption moisture or vapor.The moisture re-evaporation process of absorption can cause the avalanche of Silica hydrogel structure；The water of absorption
Steam condenses between silica skeleton, due to the effect of surface tension, can collapse the nanometer micropore of aerosil, shows
Write the heat-proof quality for reducing aeroge.It is all irreversible that both the above is collapsed, and the heat-proof quality of loss cannot be recovered, these limits
The application of aerosil is made.Therefore prepare hydrophobic aerosil has weight to improving its application value
Want meaning.
At present, the R such as dimethyldichlorosilane, trim,ethylchlorosilane are commonly usednSiX4nType organo-silicon compound (n=1~3, R
=CH3,C2H5Or phenyl etc., X=OCH3,OC2H5, or Cl etc.), HMDS or HMDO etc. be to two
Silica aerogel is modified, and improves its hydrophobicity.Above modification mode has the following disadvantages：
First, method of modifying all must during aeroge is prepared reaction modifying, or in the solution to finished product airsetting
Glue is modified, and both the above technique has a disadvantage that：One is often to immerse in modification liquid wet gel to react, because modifying agent must
Could be reacted during wet gel must be penetrated into by molecular motion, therefore the reaction time is more long.Two is to prepare a large amount of aeroges
When, the aeroge-fiber felt composite material of such as big volume, modifying agent often only reacts with the aeroge on top layer, and internal layer of getting along well
Aeroge reaction, cause the hydrophobicity of internal layer aeroge bad.Three is that the solvent slop obtained after wet gel is dried is difficult to reclaim.
Because hydrophobic drier is present.Often boiling point is very low for hydrophobic drier, it is difficult to and ethanol equal solvent passes through rectifying
Separate.And failing the clean water-repelling agent of removal can influence the gel reaction of next time, lead to not gel or gel turns white, by force
Spend low defect.
By taking trim,ethylchlorosilane as an example, conventional technique is：With tetraethyl orthosilicate ethanol, ammoniacal liquor and water mixed liquor
It is middle heating occur poly-condensation and hydrolysis, then by ageing obtain wet gel, backward solution in add trim,ethylchlorosilane
And ethanol, after carrying out surface modified a period of time, then replaced by solvent, dried, can be only achieved modified product.
By taking dimethyldichlorosilane as an example, conventional technique is：By tetraethyl orthosilicate, absolute ethyl alcohol, formamide, deionization
Water, hydrochloric acid are reacted by the amount proportioning mixing of certain material under rapid mixing conditions, and solution is changed into limpid transparent from muddiness.With
Appropriate weak aqua ammonia adjusts the pH value of solution, and quickly stirring is allowed to well mixed, then mixed liquor is poured into beaker, after sealing
It is placed in and make at room temperature its gelation, is aged.Dimethyldichlorosilane/hexamethylene is added, at room temperature reaction a period of time, makes it
With it is aging after aeroge surface hydroxyl reaction, substituted hydroxy group.Displaced with absolute ethyl alcohol again remaining molten in product
Agent；Finally carry out supercritical CO2It is dried to obtain product.
2nd, the heat-resisting quantity of modifying agent is poor, is unfavorable for playing the effect of heat insulation of aeroge.Because no matter which kind of is foregoing hydrophobic
Agent, finally all with the addition of alkyl group on silica skeleton, and the heat-resisting quantity of alkyl is poor.
In view of this, it is special to propose the present invention.
The content of the invention
The first object of the present invention is to provide a kind of hydrophobic aerogels, and described hydrophobic aerogels are solved simultaneously to be had
Low and heat-resisting quantity difference the problem of existing aeroge hydrophobicity.
The second object of the present invention is the preparation method for providing above-mentioned hydrophobic aerogels, and described preparation method is utilized
Very the simple and very low flow of cost is modified to aerosil, improves its hydrophobicity, maintains its resistance to height
Temperature characteristics.
The third object of the present invention is to provide a kind of aerogel blanket, and the aerogel blanket hydrophobicity is high, and stable performance is resistance to
High temperature, it is applied widely, and suitable for existing production line.
In order to realize the above object the invention provides following technical scheme：
A kind of hydrophobic aerogels, have trifluoromethyl CF in the surface modification of aerosil3-。
Innovative point of the invention be ingenious property aerosil surface connection on CF3-, on the one hand only
Improve its surface hydrophobic, i.e., formed on its surface and blocked water barrier, the barrier also has a good heat-resisting quantity, resistance to 900 DEG C with
On high temperature；On the other hand do not destroy the internal pore structure of aeroge again, it is kept specific surface area, the hole of script level
The good characteristics such as rate, density, thermal conductivity.
Count after testing, the contact angle of hydrophobic aerogels water of the invention is whole for more than more than 100 degree, or even 130 degree
The heat-resisting quantity of body is at least at 900 DEG C.
In order to obtain heat-resisting quantity and hydrophobicity higher, it is preferable that the trifluoromethyl CF3- content for 0.1~
10wt%, preferably 1~10wt%, preferably 5~10wt%.
Aerosil of the present invention can pass through compound aeroge finished product, such as coiled material or plate
Material, or pure aerogel powder etc..
The purposes of hydrophobic aerogels provided by the present invention is widely, although by being modified, but have no effect on it
Use, still can be used for any field used by original aeroge, for example ultra heat insulating material, Cerenkov detectors, efficiently
Rechargeable battery, ultracapacitor, acoustic impedance coupling material, catalyst and carrier etc..By taking heat-insulating heat-preserving material as an example, the present invention
Aerogel blanket can be made with reference to base material, base material used can be glass fibre or pre-oxidized fibers.
The preparation method of hydrophobic aerogels provided by the present invention is very simple, specific as follows：
Aerosil is set to be reacted with fluoroform under the catalytic action of ammonia, reaction temperature is 10-50 DEG C, i.e.,
Obtain product.
Contrast technique of the invention and existing process understands, the present invention reacts completely without under solution state, therefore
Eliminate solvent displacement, except operations such as solvent, dryings, and then the increased sky high cost of these operations institute is eliminated, while realizing
The production model all harmless to environment and human body.
For in terms of the actual production, because the reaction involved by present invention process is very simple, it is not necessary to which complicated sets
It is standby, make larger transformation without to existing production line, need to only increase the container of supply gel and fluoroform reaction, therefore
It is applied widely, easily promote, and easily realize quality control.
Process above can also be improved further, to reach more technique effects：
Preferably, the aerosil, the volume ratio of fluoroform are 60-90:100, preferably 60-90:100,
It is preferred that 70-90:100, preferably 70-80:100.
Preferably, the ammonia and the volume ratio of fluoroform are 0.1-1:0.1-5, preferably 0.3-1:0.1-5, preferably
0.3-1:0.1-1, such as 0.1:5,1:5,0.1:0.1,1:0.1,0.3:0.1,0.3:5,0.3:1,0.2:2.5 etc..
Preferably, the reaction temperature is 25-50 DEG C；The pressure of i.e. described reaction is preferably 0.1Mpa~1Mpa.This hair
It is bright to react at normal temperatures and pressures.
Preferably, the time of the reaction is 10min-2h, preferably 10min-1h.
Proportioning between reaction raw materials and influenced each other between reaction temperature, time, and influence to be mainly reflected in anti-
The aspects such as speed, product amount are answered, it is necessary to consider each side factor in actual production process, appropriate proportioning, temperature is selected
Degree and time.
Wherein, the proportioning between reaction raw materials is also to CF3- modification amount have a major impact, it is preferred that the dioxy
SiClx aeroge, the volume ratio of fluoroform are 60-90:100, preferably 60-90:100, preferably 70-90:100, preferably 70-80:
100, such as 90:100,60:100,70:100,75:100,80:100.
Preferably, the humidity during reaction is less than 1%, and ammonia can be avoided to absorb water, and influences catalytic efficiency.
Preferably, enough drier can be added, to keep the humidity of reaction environment below 1%, to ensure reaction
Stabilization is carried out.
Preferably, drier can be soda lime, quick lime, silica-gel desiccant, and molecular sieve desiccant etc., should not be chlorination
The material that calcium, anhydrous cupric sulfate, concentrated sulfuric acid etc. can react or be complexed with ammonia.
To sum up, compared with prior art, invention achieves following technique effect：
(1) hydrophobicity is greatly improved：In aeroge surface modification CF3- group makes its contact angle reach more than 130 degree, very
To 150 degree.
(2) heat-resisting quantity is improved：The CF for being connected3- group has heat-resisting quantity higher, makes modified gel resistance to
More than 900 DEG C of high temperature, can more play the heat-resisting quantity of aerosil；Aerosil itself bone
Frame can be with resistance to 1000 DEG C of high temperature, but existing base material or modified group only up to resistance to 600 DEG C of high temperature, this serious system
The about performance of silica thermal insulation.
(3) simple production process, low cost, easily promote：If technique of the invention is extended into market, will obtain huge
Business success.
(4) modified aerogels is widely used：Can be used to make ultra heat insulating material, Cerenkov detectors, efficiently may be used
Rechargeable battery, ultracapacitor, acoustic impedance coupling material, catalyst and carrier etc..
Specific embodiment
Technical scheme is clearly and completely described below in conjunction with specific embodiment, but ability
Field technique personnel will be understood that, following described embodiment is a part of embodiment of the invention, rather than whole embodiments,
The present invention is merely to illustrate, and is not construed as limiting the scope of the present invention.Based on the embodiment in the present invention, the common skill in this area
The every other embodiment that art personnel are obtained under the premise of creative work is not made, belongs to the model of present invention protection
Enclose.Unreceipted actual conditions person in embodiment, the condition advised according to normal condition or manufacturer is carried out.Agents useful for same or instrument
Unreceipted production firm person, is the conventional products that can be obtained by commercially available purchase.
Primary motivitation of the invention is in aerosil surface modification trifluoromethyl, and to the type of aeroge
It is not construed as limiting, can is sterling, or by composite building material finished product.Specific modified technique is as follows：
Aerosil is set to be reacted with fluoroform under the catalytic action of ammonia, reaction temperature is 10-50 DEG C, i.e.,
Obtain product.
In above key foundation, optimize each reaction condition and material rate, with obtain yield higher, speed,
CF3- content and other properties of product or reduces cost, for example：
Preferably, the reaction temperature is 25-50 DEG C；The pressure of the reaction is preferably 0.1Mpa~1Mpa.
Preferably, the fluoroform, the volume ratio of aerosil are 60-90:100, preferably 60-90:100,
It is preferred that 70-90:100, preferably 70-80:100.
Preferably, the ammonia and the volume ratio of fluoroform are 0.1-1:0.1-5, preferably 0.3-1:0.1-5, preferably
0.3-1:0.1-1。
Preferably, the time of the reaction is 10min-2h, preferably 10min-1h.
Preferably, the humidity during reaction is less than 1%.
With reference to above technical scheme, there is provided following examples.
Embodiment 1
Hydrophobic treatment will not be done, aeroge-glass composite sheet material is placed in normal pressure gas phase reaction kettle.The volume of coiled material is accounted for
The 60-80% of reactor volume.Fluoroform is passed through, volume is the 60% of composite sheet material, then passes to ammonia, and volume is trifluoro
0.3 times of methane.The lid of reactor will have air-tightness.At 25 DEG C at room temperature, react 1 hour.Uncap and take out airsetting film
Material.Hung 2 hours in ventilation.
The contact angle for measuring water is 130 degree.900 DEG C are heated in Muffle furnace, and are kept for 4 hours, be visible by naked eyes
Change.
Embodiment 2
From the difference of embodiment 1 be fluoroform intake it is different, it is specific as follows.
Hydrophobic treatment will not be done, aeroge-oxidization fiber fiber composite coiled material is placed in normal pressure gas phase reaction kettle.Coiled material
Volume accounts for the 60-80% of reactor volume.Fluoroform is passed through, volume is the 90% of composite sheet material, then passes to ammonia, volume
It is 0.3 times of fluoroform.The lid of reactor will have air-tightness.At 25 DEG C at room temperature, react 1 hour.Uncap taking-up gas
Gel coiled material.Hung 2 hours in ventilation.
The contact angle for measuring water is 134 degree.900 DEG C are heated in Muffle furnace, and are kept for 4 hours, be visible by naked eyes
Change.
Embodiment 3
From the difference of embodiment 1 be fluoroform intake it is different, it is specific as follows.
Hydrophobic treatment will not be done, aeroge-high silica fiber composite sheet material is placed in normal pressure gas phase reaction kettle, is passed through three
Fluoromethane, volume is the 70% of composite sheet material, then passes to ammonia, and volume is 0.3 times of fluoroform.The lid of reactor will
There is air-tightness.At 25 DEG C at room temperature, react 1 hour.Uncap and take out aeroge coiled material.Hung 2 hours in ventilation.
The contact angle for measuring water is 150 degree.950 DEG C are heated in Muffle furnace, and are kept for 4 hours, be visible by naked eyes
Change.
Embodiment 4
From the difference of embodiment 1 be fluoroform intake it is different, it is specific as follows.
Hydrophobic treatment will not be done, aeroge-high silica fiber composite sheet material is placed in normal pressure gas phase reaction kettle, is passed through three
Fluoromethane, volume is the 80% of composite sheet material, then passes to ammonia, and volume is 0.3 times of fluoroform.The lid of reactor will
There is air-tightness.At 25 DEG C at room temperature, react 1 hour.Uncap and take out aeroge coiled material.Hung 2 hours in ventilation.
The contact angle for measuring water is 155 degree.950 DEG C are heated in Muffle furnace, and are kept for 4 hours, be visible by naked eyes
Change.
Embodiment 5
From the difference of embodiment 4 be ammonia intake it is different, it is specific as follows.
Hydrophobic treatment will not be done, aeroge-high silica fiber composite sheet material is placed in normal pressure gas phase reaction kettle, is passed through three
Fluoromethane, volume is the 80% of composite sheet material, then passes to ammonia, and volume is identical with fluoroform.The lid of reactor will have
Air-tightness.At 25 DEG C at room temperature, react 10 minutes.Uncap and take out aeroge coiled material.Hung 2 hours in ventilation.
The contact angle for measuring water is 152 degree.920 DEG C are heated in Muffle furnace, and are kept for 4 hours, be visible by naked eyes
Change.
Embodiment 6
From the difference of embodiment 4 be ammonia intake it is different, it is specific as follows.
Hydrophobic treatment will not be done, aeroge-high silica fiber composite sheet material is placed in normal pressure gas phase reaction kettle, is passed through three
Fluoromethane, volume is the 80% of composite sheet material, then passes to ammonia, and volume is 0.1 times of fluoroform.The lid of reactor will
There is air-tightness.At 25 DEG C at room temperature, react 1 hour.Uncap and take out aeroge coiled material.Hung 2 hours in ventilation.
The contact angle for measuring water is 153 degree.930 DEG C are heated in Muffle furnace, and are kept for 4 hours, be visible by naked eyes
Change.
Embodiment 7
It is different reaction temperature from the difference of embodiment 4, it is specific as follows.
Hydrophobic treatment will not be done, aeroge-high silica fiber composite sheet material is placed in normal pressure gas phase reaction kettle, is passed through three
Fluoromethane, volume is the 80% of composite sheet material, then passes to ammonia, and volume is 0.2 times of fluoroform.The lid of reactor will
There is air-tightness.50 DEG C are heated to, are reacted 1 hour.Uncap and take out aeroge coiled material.Hung 2 hours in ventilation.
The contact angle for measuring water is 154 degree.930 DEG C are heated in Muffle furnace, and are kept for 4 hours, be visible by naked eyes
Change.
Embodiment 8
It is different reaction temperature from the difference of embodiment 4, it is specific as follows.
Hydrophobic treatment will not be done, aeroge-high silica fiber composite sheet material is placed in normal pressure gas phase reaction kettle, is passed through three
Fluoromethane, volume is the 80% of composite sheet material, then passes to ammonia, and volume is 0.02 times of fluoroform.The lid of reactor
There is air-tightness.50 DEG C are heated to, are reacted 3 hours.Uncap and take out aeroge coiled material.Hung 2 hours in ventilation.
The contact angle for measuring water is 153 degree.930 DEG C are heated in Muffle furnace, and are kept for 4 hours, be visible by naked eyes
Change.
Embodiment 9
It is different reaction temperature from the difference of embodiment 4, it is specific as follows.
Hydrophobic treatment will not be done, aeroge-high silica fiber composite sheet material is placed in normal pressure gas phase reaction kettle, is passed through three
Fluoromethane, volume is the 80% of composite sheet material, then passes to ammonia, and volume is 0.1 times of fluoroform.The lid of reactor will
There is air-tightness.50 DEG C are heated to, are reacted 20 minutes.Uncap and take out aeroge coiled material.Hung 2 hours in ventilation.
The contact angle for measuring water is 154 degree.930 DEG C are heated in Muffle furnace, and are kept for 4 hours, be visible by naked eyes
Change.
Embodiment 10
It is different reaction temperature from the difference of embodiment 4, it is specific as follows.
Hydrophobic treatment will not be done, aeroge-high silica fiber composite sheet material is placed in normal pressure gas phase reaction kettle, is passed through three
Fluoromethane, volume is the 80% of composite sheet material, then passes to ammonia, and volume is 0.1 times of fluoroform.The lid of reactor will
There is air-tightness.Reacted 2 hours at 15 DEG C.Uncap and take out aeroge coiled material.Hung 2 hours in ventilation.
The contact angle for measuring water is 153 degree.930 DEG C are heated in Muffle furnace, and are kept for 4 hours, be visible by naked eyes
Change.
Finally it should be noted that：Various embodiments above is merely illustrative of the technical solution of the present invention, rather than its limitations；To the greatest extent
Pipe has been described in detail with reference to foregoing embodiments to the present invention, it will be understood by those within the art that：Its according to
The technical scheme described in foregoing embodiments can so be modified, or which part or all technical characteristic are entered
Row equivalent；And these modifications or replacement, the essence of appropriate technical solution is departed from various embodiments of the present invention technology
The scope of scheme.
Claims (10)
1. a kind of hydrophobic aerogels, it is characterised in that have trifluoromethyl CF in the surface modification of aerosil3-。
2. hydrophobic aerogels according to claim 1, it is characterised in that the trifluoromethyl CF3- content for 0.1~
10wt%, preferably 1~10wt%, preferably 5~10wt%.
3. hydrophobic aerogels according to claim 1 and 2, it is characterised in that the water of the hydrophobic aerogels connects
Feeler is more than 100 degree.
4. the preparation method of the hydrophobic aerogels described in any one of claim 1-3, it is characterised in that comprise the following steps：
Aerosil is set to be reacted with fluoroform under the catalytic action of ammonia, reaction temperature is 10-50 DEG C, obtains final product product
Product.
5. the preparation method of hydrophobic aerogels according to claim 4, it is characterised in that the reaction temperature is 25-
50℃；The pressure of the reaction is preferably 0.1Mpa~1Mpa.
6. the preparation method of hydrophobic aerogels according to claim 4, it is characterised in that the fluoroform, dioxy
The volume ratio of SiClx aeroge is 60-90:100, preferably 60-90:100, preferably 70-90:100, preferably 70-80:100.
7. the preparation method of the hydrophobic aerogels according to claim any one of 4-6, it is characterised in that the ammonia with
The volume ratio of fluoroform is 0.1-1:0.1-5, preferably 0.3-1:0.1-5, preferably 0.3-1:0.1-1.
8. the preparation method of hydrophobic aerogels according to claim 4, it is characterised in that the time of the reaction is
10min-2h, preferably 10min-1h.
9. the preparation method of hydrophobic aerogels according to claim 4, it is characterised in that the humidity during reaction is
Less than 1%.
10. a kind of aerogel blanket, it is characterised in that the main hydrophobicity airsetting as described in base material and claim any one of 1-3
Glue is composited, and the base material is preferably selected from glass fibre, high silica fiber, alumina silicate fibre or oxidization fiber fiber.
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Cited By (4)
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| CN107935540A (en) * | 2017-12-19 | 2018-04-20 | 贵州航天乌江机电设备有限责任公司 | A kind of preparation process of oxidization fiber fiber composite type aerosil insulation blanket |
| TWI741746B (en) * | 2020-08-20 | 2021-10-01 | 趙國昇 | Manufacturing method of silica aerogel composite fiber blanket |
| CN114477194A (en) * | 2022-01-18 | 2022-05-13 | 中国科学院工程热物理研究所 | Method for preparing hydrophobic silica aerogel based on chemical vapor deposition |
| CN114773027A (en) * | 2022-06-16 | 2022-07-22 | 巩义市泛锐熠辉复合材料有限公司 | Aerogel felt prepared at low cost and preparation method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107935540A (en) * | 2017-12-19 | 2018-04-20 | 贵州航天乌江机电设备有限责任公司 | A kind of preparation process of oxidization fiber fiber composite type aerosil insulation blanket |
| TWI741746B (en) * | 2020-08-20 | 2021-10-01 | 趙國昇 | Manufacturing method of silica aerogel composite fiber blanket |
| CN114477194A (en) * | 2022-01-18 | 2022-05-13 | 中国科学院工程热物理研究所 | Method for preparing hydrophobic silica aerogel based on chemical vapor deposition |
| CN114477194B (en) * | 2022-01-18 | 2023-09-05 | 中国科学院工程热物理研究所 | Method for preparing hydrophobic silica aerogel based on chemical vapor deposition |
| CN114773027A (en) * | 2022-06-16 | 2022-07-22 | 巩义市泛锐熠辉复合材料有限公司 | Aerogel felt prepared at low cost and preparation method thereof |
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| CN106829972B (en) | 2019-06-25 |
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