CN106145881B - A kind of hydrophobic type fibrofelt enhancing titanium silicon compound aerogel and preparation method - Google Patents
A kind of hydrophobic type fibrofelt enhancing titanium silicon compound aerogel and preparation method Download PDFInfo
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- CN106145881B CN106145881B CN201510137847.9A CN201510137847A CN106145881B CN 106145881 B CN106145881 B CN 106145881B CN 201510137847 A CN201510137847 A CN 201510137847A CN 106145881 B CN106145881 B CN 106145881B
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Abstract
The invention discloses a kind of hydrophobic type fibrofelt enhancing titanium silicon compound aerogel and preparation methods, belong to the preparing technical field of nano structural material.Hydrophobic type fibrofelt enhancing titanium silicon compound aerogel is made of following components, tetraethyl orthosilicate, absolute ethyl alcohol, deionized water, acid, titanium dioxide and alkali；Tetraethyl orthosilicate with the 2/3 of absolute ethyl alcohol volume is mixed first during preparation, solution A is obtained after stirring evenly；Then remaining absolute ethyl alcohol with deionized water, acid is mixed, solution B is obtained after stirring evenly；Solution B is slowly added into solution A again, avoids and floccule occurs in coal addition position, influences stability and hydrophobic effect.Hydrophobic effect of the present invention is apparent, at the 7th day, hydrophobic rate is 92.4%, and the hydrophobic type fibrofelt enhancing titanium silicon compound aerogel material prepared not only has certain intensity, it can also be folded, available for multiple fields such as national defence, aerospace, military affairs, petroleum production engineerings, and low-carbon environment-friendly, service life are long.
Description
Technical field
The invention belongs to the preparing technical fields of nano structural material, and in particular to a kind of hydrophobic type fibrofelt enhances titanium silicon
Composite aerogel and preparation method.
Background technology
With the high speed development of scientific and technological level, various thermal insulation materials continue to introduce new, and modern thermal insulation material is good with it
Properties of heat preservation and energy saving, obtained in terms of oil, chemical industry, smelting, the equipment pipe of power department and industry and civil buildings
It is widely applied, but higher requirement also is proposed to high-temperature heat insulation heat-insulation system simultaneously, not only requirement has higher thermal effect
Rate improves the utilization rate of efficient heat, reduces waste heat output, and a series of performances such as high temperature resistant, lightweight, efficient, high stability；
Excellent working environment is also provided for worker simultaneously.
SiO2Aeroge is a kind of novel low-density, nanoporous, amorphous state and has continuous three-dimensional net structure
Solid, network diameter be 1~100nm, belong to typical mesoporous material.Due to its special porous property, it is usually used in conduct
Absorption, sound insulation and heat-insulating material.These unique properties have caused the very big emerging of numerous chemists, physicist and material scholar
Interest.Since cryogenic heat transfer is mainly in a manner of convection current and heat transfer, with the raising of temperature, when temperature is more than 100 DEG C or more
When, heat radiation starts to play a major role, and can increase sharply with the raising of temperature.On the other hand due to SiO2Aeroge sheet
Body mechanical strength is low, and density is small, it is easy to lose powder.Therefore silica aerogel cannot be separately as high temperature thermal insulation material, it is necessary to pass through
Doping vario-property, and go out its advantage in high-temperature heat insulation aspect of performance with the compound competence exertion of inorganic reinforcement.
Invention content
The purpose of the present invention overcomes the shortcomings of the prior art, and the first purpose is to provide that a kind of preparation process is simple, system
The standby period is short, it is of low cost, can be continuously produced, there is the hydrophobic type fibrofelt of good hydrophobicity and comprehensive performance enhancing titanium
Silicon compound aerogel；The second purpose is to provide the preparation method of hydrophobic type fibrofelt enhancing titanium silicon compound aerogel.
An object of the present invention can be achieved through the following technical solutions：
Hydrophobic type fibrofelt enhancing titanium silicon compound aerogel is formulated by the following raw material：
Use tetraethyl orthosilicate：Absolute ethyl alcohol：Deionized water：Acid=1：3.5~5：0.32：0.015 parts by volume proportioning system
Into SiO2Colloidal sol；SiO is used again2Colloidal sol：Titanium dioxide=1:Hydrophobic type fibrofelt enhancing titanium silicon is made in 0.05~0.15 proportion by weight
Composite aerogel product.
An object of the present invention can be also achieved through the following technical solutions：
The HCl or HNO that the acid is 0.5mol/L~1.5mol/L3In any one, the titanium dioxide be rutile-type
Any one in titanium dioxide or anatase titanium dioxide.
The second object of the present invention can be achieved through the following technical solutions：
A kind of preparation method of hydrophobic type fibrofelt enhancing titanium silicon compound aerogel recited above, preparation process are as follows：
(1) tetraethyl orthosilicate with the 2/3 of absolute ethyl alcohol volume is mixed, solution A is obtained after stirring evenly；
(2) remaining absolute ethyl alcohol with deionized water, acid is mixed, solution B is obtained after stirring evenly；The purpose done so
It is：If because tetraethyl orthosilicate and absolute ethyl alcohol are first mixed, when adding water or is sour, can all go out in coal addition position
Existing a part of floccule, affects stability and hydrophobic effect, this is because in the too fast water of coal addition position tetraethyl orthosilicate
Caused by solution and polycondensation.(ethyl alcohol is solvent, does not participate in reaction in tetraethyl orthosilicate hydrolytic process；Acid be as catalyst,
Effect is to accelerate the hydrolysis of tetraethyl orthosilicate；Water is the hydrolysis for participating in tetraethyl orthosilicate), therefore absolute ethyl alcohol point
Open plus purpose be to water or acid serve buffer it is diluted.
(3) solution B is slowly added into solution A, 1~2h is reacted at 50~70 DEG C, obtains solution S iO2Colloidal sol；
(4) by SiO2Colloidal sol：Titanium dioxide=1:Titanium dioxide is added to SiO by 0.05~0.15 proportion by weight2In colloidal sol, use
The pH that alkali adjusts solution is 6~7, is stirred continuously obtained titanium silicon composite sol；
(5) the titanium silicon composite sol that step (4) is prepared is poured into the mold of fibrofelt prefabricated component, treats that colloidal sol is impregnated with
Fibrofelt pours out extra colloidal sol, and formation titanium silicon is compound solidifying after titanium silicon composite sol material is stood 1~3h at 50~70 DEG C
Glue material；
(6) it by the titanium silicon plural gel obtained in step (5) at 50~80 DEG C, carries out solvent with ethanol solution and puts
It changes, replaces 2~4 days, surface modification is carried out to titanium silicon composite gel material with surface modifier, it is 2~4 days modified, to be dredged
Water surface, then solvent displacement is carried out with ethanol solution, it replaces 2~4 days, is modified with removing the unreacted surface of material surface
Agent, so as to obtain the titanium silicon composite gel material with hydrophobic surface；
(7) the titanium silicon composite gel material obtained in step (6) is subjected to supercritical drying, obtains hydrophobic type fibrofelt and increase
Strong titanium silicon compound aerogel.
The second object of the present invention can be also achieved through the following technical solutions：
The NH that alkali in the step (4) is 1mol/L~2mol/L3·H2Any one in O or NaOH.
Fibrofelt used in the step (5) is glass mat, mullite fiber felt, carbon fiber felt or basalt are fine
It ties up any in felt.
Surface modifier described in the step (6) is two silicon of trim,ethylchlorosilane, hexamethyldisilazane or hexamethyl
It is any in oxygen alkane.
Supercritical drying mode described in the step (7) is CO2Or it is any in Ethanol supercritical, Ethanol supercritical is done
Dry drying temperature is 260~280 DEG C, and pressure is 10~12MPa, and 2~3 hours, Ran Houfang are maintained under constant temperature and pressure state
Gas takes out sample, CO2The drying temperature of supercritical drying is 40~50 DEG C, and pressure is 10~12MPa, is tieed up under constant temperature and pressure state
10~12 hours are held, then deflates and takes out sample.
Compared with prior art, the invention has the advantages that：
(1) present invention use tetraethyl orthosilicate and titanium dioxide production cost is low, simple for process for raw material, suitable industrial
Metaplasia is produced.
(2) the hydrophobic type fibrofelt enhancing titanium silicon compound aerogel material that prepared by the present invention can effectively barrier material in height
Infrared radiation heat transfer when temperature uses, for room temperature thermal conductivity up to 0.021~0.029W/ (mK), 400 DEG C of thermal conductivity is reachable
0.035~0.042W/ (mK).
(3) hydrophobic effect of the present invention is apparent, and at the 7th day, hydrophobic rate was 92.4%, and the hydrophobic type fibrofelt prepared
Enhancing titanium silicon compound aerogel material not only there is certain intensity can also be folded, available for national defence, aerospace, military affairs etc.
Multiple fields, and low-carbon environment-friendly, service life are long.
Description of the drawings
Fig. 1 is a kind of the infrared of hydrophobic type basalt fibre felt enhancing titanium silicon compound aerogel material prepared by example 1
Test chart；
Fig. 2 is a kind of sample drawing of hydrophobic type glass mat enhancing titanium silicon compound aerogel material prepared by example 2；
Fig. 3 is a kind of hydrophobic of hydrophobic type mullite fiber felt enhancing titanium silicon compound aerogel material prepared by example 3
Rate test chart；
Fig. 4 is that a kind of contact angle of hydrophobic type carbon fiber felt enhancing titanium silicon compound aerogel material prepared by example 4 is surveyed
Attempt.
Specific embodiment
A kind of hydrophobic type fibrofelt enhancing titanium silicon compound aerogel and preparation method, with reference to the accompanying drawings and examples to this
Invention is described further, but invent protection domain and be not so limited.
Embodiment 1
It is 1 by volume by tetraethyl orthosilicate, absolute ethyl alcohol, deionized water, 0.5mol/L hydrochloric acid：3.5：0.32：
0.015 uniformly mixes, and mixing step is：
(1) tetraethyl orthosilicate with the 2/3 of absolute ethyl alcohol volume is mixed, solution A is obtained after stirring evenly；
(2) remaining absolute ethyl alcohol with deionized water, HCl is mixed, solution B is obtained after stirring evenly；
(3) solution B is slowly added into solution A.
1h is reacted at 50 DEG C, under stirring, by SiO2:TiO2(mass ratio)=1:0.05 by rutile titanium dioxide
Powder is added to SiO2In colloidal sol, add 1mol/LNH3·H2It is 6 that O, which adjusts solution ph, is stirred continuously obtained TiO2-SiO2Complex sol；
By TiO2-SiO2Complex sol is poured into the mold of basalt fibre felt prefabricated component, treats that colloidal sol is impregnated with basalt fibre
Felt pours out extra colloidal sol, and gel complex material is formed after colloidal sol composite material is stood 1h at 50 DEG C；The gel that will be obtained
Composite material carries out solvent displacement at 50 DEG C, with ethanol solution, replaces 2 days, gel is answered with hexamethyldisilazane
Condensation material carries out surface and is modified 2 days, to obtain hydrophobic surface, then with ethanol solution carries out solvent displacement, displacement 2 days obtains
Obtain the gel complex material with hydrophobic surface；Obtained gel complex material is dried with Ethanol supercritical, dry temperature
It is 260 DEG C, pressure 10MPa to spend, and 2 hours are maintained under constant temperature and pressure state, then deflates and takes out sample, it is profound to obtain hydrophobic type
Military rock fibrofelt enhances titanium silicon compound aerogel material.
The room temperature thermal conductivity of the material is 0.023W/ (mK), and 400 DEG C of thermal conductivity is 0.036W/ (mK), such as Fig. 1
Shown, as can be seen from the figure there are many hydrophobic methyl groups on the surface of material, hydrophobic well so as to have material
Effect.
Embodiment 2
It is 1 by volume by tetraethyl orthosilicate, absolute ethyl alcohol, deionized water, 0.8mol/L hydrochloric acid：4：0.32：0.015
Uniformly mixing, mixing step is the same as embodiment 1.
1.2h is reacted at 55 DEG C, under stirring, by SiO2:TiO2(mass ratio)=1:0.07 by Detitanium-ore-type titanium
White powder is added to SiO2In colloidal sol, add 1.3mol/LNH3·H2It is 6.3 that O, which adjusts solution ph, is stirred continuously obtained TiO2-SiO2It is multiple
Close colloidal sol；
By TiO2-SiO2Complex sol is poured into the mold of glass mat prefabricated component, treats that colloidal sol is impregnated with glass mat,
Extra colloidal sol is poured out, gel complex material is formed after colloidal sol composite material is stood 1.5h at 60 DEG C；The gel that will be obtained
Composite material carries out solvent displacement at 60 DEG C, with ethanol solution, replaces 2.5 days, gel is answered with trim,ethylchlorosilane
Condensation material carries out surface and is modified 2.5 days, to obtain hydrophobic surface, then with ethanol solution carries out solvent displacement, replaces 2.5
My god, obtain the gel complex material with hydrophobic surface；The gel complex material CO that will be obtained2The dry temperature of supercritical drying
It is 40 DEG C, pressure 10MPa to spend, and 10 hours are maintained under constant temperature and pressure state, then deflates and takes out sample, obtains hydrophobic type glass
Glass fibrofelt enhances titanium silicon compound aerogel material.
The room temperature thermal conductivity of the material is 0.025W/ (mK), and 400 DEG C of thermal conductivity is 0.038W/ (mK), such as Fig. 2
Shown, as can be seen from the figure material is blockiness preferable.
Embodiment 3
It is 1 by volume by tetraethyl orthosilicate, absolute ethyl alcohol, deionized water, 1mol/L nitric acid：4.5：0.32：0.015
Uniformly mixing, mixing step is the same as embodiment 1.
1.5h is reacted at 65 DEG C, under stirring, by SiO2:TiO2(mass ratio)=1:0.1 by rutile titanium dioxide
Powder is added to SiO2In colloidal sol, add 1.6mol/LNH3·H2It is 6.6 that O, which adjusts solution ph, is stirred continuously obtained TiO2-SiO2It is compound
Colloidal sol；
By TiO2-SiO2Complex sol is poured into the mold of mullite fiber felt prefabricated component, treats that colloidal sol is impregnated with mullite fiber
Felt pours out extra colloidal sol, and gel complex material is formed after colloidal sol composite material is stood 2.5h at 65 DEG C；It is solidifying by what is obtained
Glue composite material carries out solvent displacement at 70 DEG C, with ethanol solution, replaces 3 days, gel is answered with trim,ethylchlorosilane
Condensation material carries out surface and is modified 3 days, to obtain hydrophobic surface, then with ethanol solution carries out solvent displacement, displacement 3 days obtains
Obtain the gel complex material with hydrophobic surface；The gel complex material CO that will be obtained2The drying temperature of supercritical drying is
50 DEG C, pressure 12MPa, 11.5 hours are maintained under constant temperature and pressure state, then deflates and takes out sample, hydrophobic type is obtained and does not come
Mineral wool felt enhances titanium silicon compound aerogel material.
The room temperature thermal conductivity of the material is 0.028W/ (mK), and 400 DEG C of thermal conductivity is 0.041W/ (mK), such as Fig. 3
Shown, as can be seen from the figure material has good hydrophobic performance.
Embodiment 4
It is 1 by volume by tetraethyl orthosilicate, absolute ethyl alcohol, deionized water, 1.5mol/L nitric acid：5：0.32：0.015
Uniformly mixing, mixing step is the same as embodiment 1.
2h is reacted at 70 DEG C, under stirring, by SiO2:TiO2(mass ratio)=1:0.15 by rutile titanium dioxide
Powder is added to SiO2In colloidal sol, add 2mol/LNH3·H2It is 7 that O, which adjusts solution ph, is stirred continuously obtained TiO2-SiO2Complex sol；
By TiO2-SiO2Complex sol is poured into the mold of carbon fiber felt prefabricated component, is treated that colloidal sol is impregnated with carbon fiber felt, is poured out
Extra colloidal sol forms gel complex material after colloidal sol composite material is stood 3h at 70 DEG C；The gel composite wood that will be obtained
Material carries out solvent displacement at 80 DEG C, with ethanol solution, replaces 4 days, with hexamethyldisiloxane to gel complex material
It carries out surface to be modified 4 days, to obtain hydrophobic surface, then with ethanol solution carries out solvent displacement, displacement 4 days is had
The gel complex material of hydrophobic surface；Obtained gel complex material is dried with Ethanol supercritical, drying temperature 275
DEG C, pressure 12MPa maintains 3 hours under constant temperature and pressure state, then deflates and takes out sample, obtains hydrophobic type carbon fiber felt
Enhance titanium silicon compound aerogel material.
The room temperature thermal conductivity of the material is 0.025W/ (mK), and 400 DEG C of thermal conductivity is 0.04W/ (mK), such as Fig. 4 institutes
Show, as can be seen from the figure material has good hydrophobic performance.
Claims (1)
1. a kind of hydrophobic type fibrofelt enhances titanium silicon compound aerogel, it is characterised in that it is formulated by the following raw material：
Use tetraethyl orthosilicate：Absolute ethyl alcohol：Deionized water：Acid=1：3.5~5：0.32：SiO is made in 0.015 parts by volume proportioning2
Colloidal sol；SiO is used again2Colloidal sol：Titanium dioxide=1:It is compound that hydrophobic type fibrofelt enhancing titanium silicon is made in 0.05~0.15 proportion by weight
Aerogel products；The HCl or HNO that the acid is 0.5mol/L~1.5mol/L3；The titanium dioxide for rutile type titanium white or
Anatase titanium dioxide；The hydrophobic type fibrofelt enhancing titanium silicon compound aerogel is made as follows：
（1）Tetraethyl orthosilicate with the 2/3 of absolute ethyl alcohol volume is mixed, solution A is obtained after stirring evenly；
（2）Remaining absolute ethyl alcohol with deionized water, acid is mixed, solution B is obtained after stirring evenly；
（3）Solution B is slowly added into solution A, 1~2h is reacted at 50~70 DEG C, obtains solution S iO2Colloidal sol；
（4）Titanium dioxide is added to SiO2In colloidal sol, the pH that solution is adjusted with alkali is 6~7, is stirred continuously obtained titanium silicon composite sol；
（5）By step（4）The titanium silicon composite sol being prepared is poured into the mold of fibrofelt prefabricated component, treats that colloidal sol is impregnated with fibrofelt,
Extra colloidal sol is poured out, titanium silicon composite gel material is formed after 1~3h is then stood at 50~70 DEG C；
（6）By step（5）In obtained titanium silicon plural gel at 50~80 DEG C, carry out solvent displacement with ethanol solution,
Displacement 2~4 days carries out titanium silicon composite gel material surface modification with surface modifier, 2~4 days modified, to obtain hydrophobic table
Face, then solvent displacement is carried out with ethanol solution, it replaces 2~4 days, to remove the unreacted surface modifier of material surface,
So as to obtain the titanium silicon composite gel material with hydrophobic surface；
（7）By step（6）In obtained titanium silicon composite gel material carry out supercritical drying, obtain hydrophobic type fibrofelt enhancing titanium
Silicon compound aerogel；
The step（4）Middle alkali is the NH of 1mol/L~2mol/L3·H2O or NaOH；Step（5）Used in fibrofelt be glass
Any one in glass fibrofelt, mullite fiber felt, carbon fiber felt or basalt fibre felt；Step（6）Described in surface change
Property agent be any in trim,ethylchlorosilane, hexamethyldisilazane or hexamethyldisiloxane；Step（7）Described in it is overcritical
Drying mode is CO2Or it is any in Ethanol supercritical, the drying temperature of ethanol supercritical drying is 260~280 DEG C, and pressure is
10~12 MPa maintain 2~3 hours under constant temperature and pressure state, then deflate and take out sample, CO2The drying of supercritical drying
Temperature is 40~50 DEG C, and pressure is 10~12 MPa, and 10~12 hours are maintained under constant temperature and pressure state, then deflates and takes out sample
Product.
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| CN108191386A (en) * | 2018-03-14 | 2018-06-22 | 宿迁市美达净化科技有限公司 | Polypropylene fibre composite S iO2Aerogel material and preparation method thereof |
| CN108221367A (en) * | 2018-03-21 | 2018-06-29 | 青岛纳博科环保科技有限公司 | Hydrophobic modifier for activated carbon fibre and preparation method thereof, hydrophobic active Carbon fibe and preparation method thereof |
| CN108585922B (en) * | 2018-06-20 | 2021-02-05 | 响水华夏特材科技发展有限公司 | Aerogel ceramic fiber heat-insulating plate and preparation method thereof |
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| CN101691227A (en) * | 2009-10-13 | 2010-04-07 | 厦门大学 | Method for preparing silica aerogel material |
| CN102351494A (en) * | 2011-07-20 | 2012-02-15 | 厦门大学 | Method for preparing foam material reinforced silica aerogel composite material |
| CN103754887A (en) * | 2013-12-25 | 2014-04-30 | 上海纳米技术及应用国家工程研究中心有限公司 | Heat-resisting silica aerogel material and preparation method thereof |
| CN103785369A (en) * | 2014-01-21 | 2014-05-14 | 江苏大学 | Preparation method of composite silicon-based titanium-doped aerogel |
| CN104261797A (en) * | 2014-09-02 | 2015-01-07 | 南京工业大学 | Glass fiber reinforced TiO2-SiO2Preparation method of composite aerogel heat insulation material |
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Patent Citations (5)
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|---|---|---|---|---|
| CN101691227A (en) * | 2009-10-13 | 2010-04-07 | 厦门大学 | Method for preparing silica aerogel material |
| CN102351494A (en) * | 2011-07-20 | 2012-02-15 | 厦门大学 | Method for preparing foam material reinforced silica aerogel composite material |
| CN103754887A (en) * | 2013-12-25 | 2014-04-30 | 上海纳米技术及应用国家工程研究中心有限公司 | Heat-resisting silica aerogel material and preparation method thereof |
| CN103785369A (en) * | 2014-01-21 | 2014-05-14 | 江苏大学 | Preparation method of composite silicon-based titanium-doped aerogel |
| CN104261797A (en) * | 2014-09-02 | 2015-01-07 | 南京工业大学 | Glass fiber reinforced TiO2-SiO2Preparation method of composite aerogel heat insulation material |
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