CN106495169A - A kind of hydrophobic type aerosil and preparation method thereof - Google Patents
A kind of hydrophobic type aerosil and preparation method thereof Download PDFInfo
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- CN106495169A CN106495169A CN201610963506.1A CN201610963506A CN106495169A CN 106495169 A CN106495169 A CN 106495169A CN 201610963506 A CN201610963506 A CN 201610963506A CN 106495169 A CN106495169 A CN 106495169A
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- 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
- C01B33/16—Preparation of silica xerogels
- C01B33/163—Preparation of silica xerogels by hydrolysis of organosilicon compounds, e.g. ethyl orthosilicate
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/10—Solid density
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/32—Thermal properties
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Abstract
The present invention relates to a kind of preparation method of hydrophobic type aerosil, it is related to a kind of aerosil and preparation method thereof, with tetraethyl orthosilicate, MTES as co-precursor, ethanol is solvent, water is hydrolytic reagent, sodium hydroxide solution is catalyst, and the ethanol for adding fc-surfactant is Ageing solution, and the bulk silicon dioxide aeroge with good hydrophobic rate has been obtained through supercritical drying process.This preparation method process is simple, need not introduce that hexamethyldisiloxane etc. is inflammable, have the dressing agent of abnormal flavour by make sample hydrophobic, and resulting product density is relatively low, and hydrophobicity is good, and hot property is stable, and heat-proof quality is excellent.
Description
Technical field
The present invention relates to a kind of aerosil and preparation method thereof, and in particular to a kind of hydrophobic type silicon dioxide gas
Gel and preparation method thereof.
Background technology
Aeroge is a kind of novel low density, structure-controllable, and being cross-linked with each other by colloidal particle or high-polymer molecular is constituted
There is the light nanoporous amorphous solid-state material of spacial framework, due to its unique nano grade pore architectural feature, make it
There is the characteristics such as low-density, high-specific surface area, high porosity, lower thermal conductivity, low-k, carry in effectively insulating, catalyst
The aspects such as body, absorption have broad application prospects.
The preparation of aerosil is typically with organosilane precursor（Methyl silicate, tetraethyl orthosilicate etc.）Or it is inorganic
Class presoma（Sodium silicate, Ludox etc.）As raw material, formed using sol-gel process and there is nanometer porous network structure
Wet gel, and with reference to appropriate drying process（Supercritical drying or the constant pressure and dry of surface modification）Remove molten in gel
Liquid, so that obtain aeroge.Contain a large amount of hydrophilic radical silicone hydroxyls in the conventional aerosil surface for preparing so as to
The easy moisture absorption in air, chance water are easy to crack, affect its heat, sound, electric property and practical application.
Currently the hydroxyl reactive group on aerosil surface is carried out by surface post-processing approach mostly lazy
Propertyization is replaced, but the method process cycle is lengthened, complex procedures.If the Chinese patent of publication number CN102179230A is with waterglass
For raw material, constant pressure and dry is prepared for a kind of tax magnetic silica aeroge, with water contact angle up to 110 ~ 1200, but preparation process
Middle using a large amount of organic modifiers（Trim,ethylchlorosilane, hexamethyldisiloxane, dimethyldichlorosilane etc.）, preparation cost
Height, complex procedures.
Main using addition organosilan in aging process in current common process（Trim,ethylchlorosilane, hexamethyl
Disilazane, dimethyldichlorosilane etc.）Hydrophobically modified is carried out to aeroge, using the methyl of organosilan（-CH3）Replace wet
Oh group on gel in Si-OH, but due to containing a certain amount of water, hydrophobically modified mistake of the moisture to gel in wet gel
Journey has a major impact, this is because organosilane-modified dose with the reactivity of water than with Si- on silica dioxide gel skeleton
The reactivity of OH is strong, therefore modifying agent is first consumed in a large number with water reaction, and then affects gel hydrophobically modified, it is necessary to using big
Amount modifying agent just can reach purpose.A large amount of interpolation trim,ethylchlorosilanes, hexamethyldisiloxane, dimethyldichlorosilane etc. are easily
Combustion, organosilicon modifier that is explosive, having abnormal flavour, not only bring potential safety hazard, and are manufactured into aeroge because addition is big
Originally significantly improve.
Content of the invention
The purpose of the present invention overcomes defect mentioned above and deficiency, and provides a kind of hydrophobic type aerosil.
Another object of the present invention is to providing the preparation method of above-mentioned water type aerosil.
A kind of hydrophobic type aerosil, its raw material contain the composition of volumes below portion rate：Tetraethyl orthosilicate：First
Ethyl triethoxy silicane alkane：Dehydrated alcohol：Water=1：0.5~1：2~5：0.5~1.5.
A kind of hydrophobic type aerosil, its raw material is by volumes below portion rate into being grouped into：Tetraethyl orthosilicate：
MTES：Dehydrated alcohol：Water=1：0.5~1：2~5：0.5~1.5.
A kind of method for preparing hydrophobic type aerosil, comprises the following steps：
Step one：Volume parts ratio is pressed, by tetraethyl orthosilicate：MTES：Dehydrated alcohol：Water=1：0.5~1：2~
5：0.5 ~ 1.5 ratio mixing, stirs and obtains mixture；
Step 2：The mixture of step one is heated to 50 DEG C ~ 60 DEG C, Deca sodium hydroxide solution to pH is 7.5 ~ 8.0, stirring
Seal after uniform, continue insulation more than 1.5 hours, until forming wet gel；
Step 3：The wet gel of step 2 gained impregnated in 50 DEG C ~ 60 DEG C and with the addition of the anhydrous second of fc-surfactant
In alcohol, aging 1 ~ 2 day after sealing, supercritical drying after taking-up, is carried out, that is, obtain complete bulk silicon dioxide aeroge.
The percent concentration of the sodium hydroxide solution is 0.2% ~ 1%.
The dehydrated alcohol that with the addition of fc-surfactant refers to as Ageing solution, fc-surfactant therein
It is the surface activity for by the hydrogen moiety in hc-surfactant molecule hydrocarbon chain or all being replaced with fluorine atom and being made
Agent；The mass fraction that fc-surfactant accounts for dehydrated alcohol in Ageing solution is 0.005% ~ 0.01%.
In supercritical drying supercritical medium used be carbon dioxide, ethanol, the one kind in methanol.
In supercritical drying, when medium is carbon dioxide, supercritical temperature, pressure are respectively 50 DEG C ~ 60 DEG C, 13 ~
15MPa；When medium is ethanol, supercritical temperature, pressure are respectively 260 DEG C ~ 270 DEG C, 7 ~ 8MPa；When medium is methanol, surpasses and face
Boundary's temperature, pressure are respectively 290 DEG C ~ 300 DEG C, 7 ~ 8MPa.
With tetraethyl orthosilicate and MTES as co-precursor in the present invention, it is in collosol-gelatum system
In introduce silicon alkoxide containing hydrophobic group, teos hydrolysis-polycondensation speed is faster than three ethoxy of methyl in the basic conditions
Base silane, initial reaction stage tetraethyl orthosilicate selective hydrolysis form primary micelle, mutually form secondary micelle, finally between primary micelle
Form gel.Subsequently-the OH on hydrophilic gel surface is by the hydrophobic-CH of MTES hydrolysis3Replaced, so as to shape
Into organophilic gel.
Generally for Monolithic aerogel is prepared, need to be replaced using dehydrated alcohol repeatedly after gel is aging, with as far as possible
To replace out containing the liquid of a certain amount of water in gel hole, this is because the surface tension of water is much larger than ethanol, it deposits
When causing gel drying, collapse of pore structure and block is broken.Using with the addition of with reducing water and wine in the present invention
The ethanol of the fc-surfactant of smart surface tension effect is not required to carry out multiple dehydrated alcohol replacement as Ageing solution, you can
Monolithic aerogel is prepared, preparation process is more simple and convenient.
Specific embodiment
The present invention is described below by way of case is embodied as.
Embodiment 1.
With tetraethyl orthosilicate, MTES as co-precursor, ethanol is solvent to the present embodiment, and water is hydrolysis
Agent, sodium hydroxide solution are catalyst, and the ethanol for adding fc-surfactant is Ageing solution, adopts ethanol for medium supercritical
Dry, prepare hydrophobic type aerosil block.
The preparation method of the hydrophobic type aerosil block is as follows：
a）Tetraethyl orthosilicate is pressed in beaker：MTES：Dehydrated alcohol：Water=1：0.5：2：0.5 volume parts
Than sequentially adding above-mentioned material, beaker is placed on the magnetic stirring apparatuss with heating, is stirred.
b）By step a）Mixture be heated to 50 DEG C, Deca concentration be 0.2% sodium hydroxide solution to pH be 7.5, stirring
Seal after uniform, continue insulation 2 hours, form wet gel.
c）By step b）Gained wet gel impregnated in 50 DEG C and with the addition of mass fraction containing fc-surfactant
In 0.005% dehydrated alcohol, aging 2 days after sealing, are incubated.
d）Take out aging after gel, with ethanol as supercritical drying medium, in 265 DEG C of supercritical temperature, pressure
Supercritical drying under 7.5MPa, that is, obtain complete bulk silicon dioxide aeroge.
The Monolithic aerogel made and water contact angle are up to 110 ~ 1130, room temperature heat conductivity reaches 0.018W/m.k.
Embodiment 2.
With tetraethyl orthosilicate, MTES as co-precursor, ethanol is solvent to the present embodiment, and water is hydrolysis
Agent, sodium hydroxide solution are catalyst, and the ethanol for adding fc-surfactant is Ageing solution, adopt carbon dioxide super for medium
Critical drying, prepares hydrophobic type aerosil block.
The preparation method of the hydrophobic type aerosil block is as follows：
a）Tetraethyl orthosilicate is pressed in beaker：MTES：Dehydrated alcohol：Water=1：1：5：1.5 volume parts ratio
Above-mentioned material is sequentially added, beaker is placed on the magnetic stirring apparatuss with heating, is stirred.
b）By step a）Mixture be heated to 60 DEG C, Deca concentration be 1% sodium hydroxide solution to pH be 8.0, stirring
Seal after uniform, continue insulation 1.5 hours, form wet gel.
c）By step b）Gained wet gel impregnated in 60 DEG C and with the addition of mass fraction containing fc-surfactant for 0.01%
Dehydrated alcohol in, be incubated aging 1 day after sealing.
d）Take out aging after gel, with carbon dioxide as supercritical drying medium, in 55 DEG C of supercritical temperature, pressure
Supercritical drying under 14MPa, that is, obtain complete bulk silicon dioxide aeroge.
The Monolithic aerogel made and water contact angle are up to 118 ~ 1200, room temperature heat conductivity reaches 0.016W/m.k.
Embodiment 3.
With tetraethyl orthosilicate, MTES as co-precursor, ethanol is solvent to the present embodiment, and water is hydrolysis
Agent, sodium hydroxide solution are catalyst, and the ethanol for adding fc-surfactant is Ageing solution, adopts methanol for medium supercritical
Dry, prepare hydrophobic type aerosil block.
The preparation method of the hydrophobic type aerosil block is as follows：
a）Tetraethyl orthosilicate is pressed in beaker：MTES：Dehydrated alcohol：Water=1：0.75：3：1 ratio is successively
Above-mentioned material is added, beaker is placed on the magnetic stirring apparatuss with heating, is stirred.b）By step a）Mixture add
To 55 DEG C, it is 7.8 to pH that Deca concentration is 0.5% sodium hydroxide solution to heat, seals, continue insulation 1.8 little after stirring
When, form wet gel.
c）By step b）Gained wet gel impregnated in 55 DEG C and with the addition of mass fraction containing fc-surfactant
In 0.008% dehydrated alcohol, aging 1.5 days after sealing, are incubated.
d）Take out aging after gel, with methanol as supercritical drying medium, in 290 DEG C of supercritical temperature, pressure 8MPa
Lower supercritical drying, that is, obtain complete bulk silicon dioxide aeroge.
Tetraethyl orthosilicate and MTES is employed in the present invention as co-precursor, by adding catalyst
The suitable poly-condensation and hydrolysis speed of two kinds of presomas of control so as to just defined in gel process substantial amounts of hydrophobic
Si-CH3Group, thus make silica dioxide gel have been equipped with hydrophobicity when being formed, so as to simplify technique, reduce into
This.
With water contact angle up to 115 ~ 1180, room temperature heat conductivity reaches 0.019W/m.k to the Monolithic aerogel that makes.
Fc-surfactant has following performance：The high heat-resistant stability of high surface and high chemical stability；It
Fluorine-containing alkyl not only hydrophobic but also had hated oil.
The lowest surface tension of fc-surfactant its aqueous solution can reach below 20mN/m, or even left to 15mN/m
Right.Fc-surfactant mass fraction in the solution is 0.005%～0.1%, so that it may make the reduction in surface tension of water extremely
Below 20mN/m.And general hc-surfactant mass fraction in the solution is the table that 0.1%～1.0% scope can just make water
Face tension force drops to 30mN/m～35mN/m.The so prominent high surface of fc-surfactant is so that its aqueous solution can be
Hydrocarbon ils surface spreading.
Fc-surfactant has a very high thermostability, such as the perfluoro alkyl sulfonic acid potassium of solid-state, is heated to more than 420 DEG C
Start to decompose, thus can use under the temperature more than 300 DEG C.Fc-surfactant has very high chemical stability, and it can
Opposing strong oxidizer strong acid and the effect of highly basic, and remain to keep good surface activity in this solution.If being made
The surface tension of organic solvent can also be reduced into oil soluble surfactant.
Ethanol preparation method containing fc-surfactant is as follows：
Fc-surfactant is measured by addition, is added drop-wise in ethanol, stirred and can be used as Ageing solution carbon containing
The ethanol of fluorine surfactant.
Following table is the performance test results of three embodiments：
| Embodiment | Density（kg/m3) | Heat conductivity (w/m.k) | With water contact angle (0) |
| 1 | 98 | 0.016 | 118~120 |
| 2 | 109 | 0.018 | 115~118 |
| 3 | 116 | 0.019 | 110~113 |
The buyer of fc-surfactant is Si Luoke（China）Enterprise operation center, the trade mark are Silok-200 and Silok-100
Perfluorinated surfactant.
This preparation method process is simple, need not introduce that hexamethyldisiloxane etc. is inflammable, have the dressing agent of abnormal flavour by make
Sample hydrophobic, and resulting product density is relatively low, hydrophobicity is good, and hot property is stable, and heat-proof quality is excellent.
The present invention is illustrated according to embodiment, on the premise of without departing from present principles, if this device can also be made
Dry deformation and improvement.It should be pointed out that the technical scheme obtained by the mode such as all employing equivalents or equivalent transformation, all falls within this
In the protection domain of invention.
Claims (7)
1. a kind of hydrophobic type aerosil, it is characterised in that its raw material contains the composition of volumes below portion rate：Positive silicon
Acetoacetic ester：MTES：Dehydrated alcohol：Water=1：0.5~1：2~5：0.5~1.5.
2. a kind of hydrophobic type aerosil as claimed in claim 1, it is characterised in that its raw material is by volumes below part
Number ratios into being grouped into：Tetraethyl orthosilicate：MTES：Dehydrated alcohol：Water=1：0.5~1：2~5：0.5~1.5.
3. a kind of method for preparing hydrophobic type aerosil as claimed in claim 1, it is characterised in that including following
Step：
Step one：Volume parts ratio is pressed, by tetraethyl orthosilicate：MTES：Dehydrated alcohol：Water=1：0.5~1：2~
5：0.5 ~ 1.5 ratio mixing, stirs and obtains mixture；
Step 2：The mixture of step one is heated to 50 DEG C ~ 60 DEG C, Deca sodium hydroxide solution to pH is 7.5 ~ 8.0, stirring
Seal after uniform, continue insulation more than 1.5 hours, until forming wet gel；
Step 3：The wet gel of step 2 gained impregnated in 50 DEG C ~ 60 DEG C and with the addition of the anhydrous second of fc-surfactant
In alcohol, aging 1 ~ 2 day after sealing, supercritical drying after taking-up, is carried out, that is, obtain complete bulk silicon dioxide aeroge.
4. a kind of preparation method of hydrophobic type aerosil as claimed in claim 3, it is characterised in that the hydrogen-oxygen
The percent concentration for changing sodium solution is 0.2% ~ 1%.
5. a kind of preparation method of hydrophobic type aerosil as claimed in claim 3, it is characterised in that the interpolation
Used as Ageing solution, fc-surfactant therein refers to hydrocarbon surface activity the dehydrated alcohol of fc-surfactant
Hydrogen moiety in agent molecule hydrocarbon chain or the surfactant for all being replaced with fluorine atom and being made；Carbon fluorine table in Ageing solution
It is 0.005% ~ 0.01% that face activating agent accounts for the mass fraction of dehydrated alcohol.
6. a kind of preparation method of hydrophobic type aerosil as claimed in claim 3, it is characterised in that supercritical drying
In dry supercritical medium used be carbon dioxide, ethanol, the one kind in methanol.
7. a kind of preparation method of hydrophobic type aerosil as claimed in claim 6, it is characterised in that supercritical drying
In dry, when medium is carbon dioxide, supercritical temperature, pressure are respectively 50 DEG C ~ 60 DEG C, 13 ~ 15MPa；When medium is ethanol, surpass
Critical temperature, pressure are respectively 260 DEG C ~ 270 DEG C, 7 ~ 8MPa；When medium is methanol, supercritical temperature, pressure are respectively 290 DEG C
~ 300 DEG C, 7 ~ 8MPa.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108147416A (en) * | 2018-01-16 | 2018-06-12 | 天津摩根坤德高新科技发展有限公司 | The preparation method of nanometer titanium dioxide silica aerogel and nanometer titanium dioxide silica aerogel |
| CN108609621A (en) * | 2018-07-28 | 2018-10-02 | 西安建筑科技大学 | A kind of preparation method of aerosil |
| CN109336545A (en) * | 2018-12-10 | 2019-02-15 | 航天特种材料及工艺技术研究所 | A kind of silicon dioxide silica aerogel composite material, preparation method and application |
| CN109437832A (en) * | 2018-12-18 | 2019-03-08 | 贵州航天乌江机电设备有限责任公司 | A kind of preparation method from hydrophobic type silicon dioxide silica aerogel composite material |
| CN109680485A (en) * | 2018-12-18 | 2019-04-26 | 贵州航天乌江机电设备有限责任公司 | The compound preparation method from hydrophobic silica aerogel insulation quilt of oxidization fiber |
| CN110339814A (en) * | 2018-04-04 | 2019-10-18 | 天津大学 | Modified dioxide composite silica aerogel of methyl with hierarchical porous structure and its preparation method and application |
| CN111021629A (en) * | 2019-12-24 | 2020-04-17 | 贵州航天乌江机电设备有限责任公司 | Simple preparation method of aerogel lighting glass |
| CN111039295A (en) * | 2019-12-20 | 2020-04-21 | 爱彼爱和新材料有限公司 | Method for preparing silicon dioxide aerogel and self-hydrophobic silicon dioxide aerogel heat-insulating felt pad by one-step method |
| CN113264532A (en) * | 2021-05-08 | 2021-08-17 | 南京工业大学 | Super-hydrophobic light transparent high-strength SiO2Method for producing aerogels |
| CN114477193A (en) * | 2022-01-12 | 2022-05-13 | 西安理工大学 | Anisotropic silicon dioxide aerogel with birefringence effect and preparation method thereof |
| CN114751418A (en) * | 2022-05-05 | 2022-07-15 | 中建材科创新技术研究院(山东)有限公司 | Aerogel transparent sheet and preparation method thereof |
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Cited By (14)
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|---|---|---|---|---|
| CN108147416B (en) * | 2018-01-16 | 2019-10-29 | 天津摩根坤德高新科技发展有限公司 | The preparation method and nanometer titanium dioxide silica aerogel of nanometer titanium dioxide silica aerogel |
| CN108147416A (en) * | 2018-01-16 | 2018-06-12 | 天津摩根坤德高新科技发展有限公司 | The preparation method of nanometer titanium dioxide silica aerogel and nanometer titanium dioxide silica aerogel |
| CN110339814A (en) * | 2018-04-04 | 2019-10-18 | 天津大学 | Modified dioxide composite silica aerogel of methyl with hierarchical porous structure and its preparation method and application |
| CN108609621A (en) * | 2018-07-28 | 2018-10-02 | 西安建筑科技大学 | A kind of preparation method of aerosil |
| CN108609621B (en) * | 2018-07-28 | 2020-03-17 | 西安建筑科技大学 | Preparation method of silicon dioxide aerogel |
| CN109336545A (en) * | 2018-12-10 | 2019-02-15 | 航天特种材料及工艺技术研究所 | A kind of silicon dioxide silica aerogel composite material, preparation method and application |
| CN109437832A (en) * | 2018-12-18 | 2019-03-08 | 贵州航天乌江机电设备有限责任公司 | A kind of preparation method from hydrophobic type silicon dioxide silica aerogel composite material |
| CN109680485A (en) * | 2018-12-18 | 2019-04-26 | 贵州航天乌江机电设备有限责任公司 | The compound preparation method from hydrophobic silica aerogel insulation quilt of oxidization fiber |
| CN111039295A (en) * | 2019-12-20 | 2020-04-21 | 爱彼爱和新材料有限公司 | Method for preparing silicon dioxide aerogel and self-hydrophobic silicon dioxide aerogel heat-insulating felt pad by one-step method |
| CN111039295B (en) * | 2019-12-20 | 2022-04-12 | 爱彼爱和新材料有限公司 | Method for preparing silicon dioxide aerogel and self-hydrophobic silicon dioxide aerogel heat-insulating felt pad by one-step method |
| CN111021629A (en) * | 2019-12-24 | 2020-04-17 | 贵州航天乌江机电设备有限责任公司 | Simple preparation method of aerogel lighting glass |
| CN113264532A (en) * | 2021-05-08 | 2021-08-17 | 南京工业大学 | Super-hydrophobic light transparent high-strength SiO2Method for producing aerogels |
| CN114477193A (en) * | 2022-01-12 | 2022-05-13 | 西安理工大学 | Anisotropic silicon dioxide aerogel with birefringence effect and preparation method thereof |
| CN114751418A (en) * | 2022-05-05 | 2022-07-15 | 中建材科创新技术研究院(山东)有限公司 | Aerogel transparent sheet and preparation method thereof |
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Application publication date: 20170315 |