CN106145881A - A kind of hydrophobic type fiber felt strengthens titanium silicon compound aerogel and preparation method - Google Patents
A kind of hydrophobic type fiber felt strengthens titanium silicon compound aerogel and preparation method Download PDFInfo
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- CN106145881A CN106145881A CN201510137847.9A CN201510137847A CN106145881A CN 106145881 A CN106145881 A CN 106145881A CN 201510137847 A CN201510137847 A CN 201510137847A CN 106145881 A CN106145881 A CN 106145881A
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- fiber felt
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Abstract
The invention discloses a kind of hydrophobic type fiber felt and strengthen titanium silicon compound aerogel and preparation method, belong to the preparing technical field of nano structural material.Hydrophobic type fiber felt strengthens titanium silicon compound aerogel and is made up of following components, tetraethyl orthosilicate, dehydrated alcohol, deionized water, acid, titanium dioxide and alkali；First tetraethyl orthosilicate is mixed with the 2/3 of dehydrated alcohol volume during preparation, after stirring, obtain solution A；Then residue dehydrated alcohol is mixed with deionized water, acid, after stirring, obtain solution B；Again solution B is slowly added in solution A, it is to avoid at coal addition position, floccule occurs, affects stability and hydrophobic effect.Hydrophobic effect of the present invention is obvious, when the 7th day, hydrophobic rate is 92.4%, and the hydrophobic type fiber felt prepared strengthens titanium silicon compound aerogel material and not only has certain intensity, can also be folded, can be used for multiple fields such as national defence, Aero-Space, military affairs, petroleum production engineering, and low-carbon environment-friendly, service life are long.
Description
Technical field
The invention belongs to the preparing technical field of nano structural material, be specifically related to a kind of hydrophobic type fiber felt enhancing titanium silicon and be combined
Aeroge and preparation method.
Background technology
Along with the high speed development of scientific and technological level, various insulation materials are constantly weeded out the old and bring forth the new, and modern insulation material is with its good guarantor
Temperature energy-efficient performance, obtains in terms of oil, chemical industry, smelting, the equipment pipe of power department and industry and civil buildings
It is widely applied, but also high-temperature heat insulation heat-insulation system is had higher requirement simultaneously, not only require there is the higher thermal efficiency,
Improve the utilization rate of efficient heat, reduce a series of performances such as waste heat output, and high temperature resistant, lightweight, efficient, high stability；
The most also to provide excellent working environment for workman.
SiO2Aeroge is a kind of novel low-density, nanoporous, amorphous state and has consolidating of continuous print three-dimensional net structure
Body, network diameter is 1～100nm, belongs to typical mesoporous material.Due to the character of its special porous, it is usually used in as suction
Attached, sound insulation and adiabator.The character of these uniquenesses has caused that numerous chemists, physicist and material scholar's is the most emerging
Interest.Owing to cryogenic heat transfer is mainly in the way of convection current and conduction of heat, along with the rising of temperature, when temperature more than 100 DEG C with
Time upper, heat radiation starts to play a major role, and can increase sharply along with the rising of temperature.On the other hand due to SiO2Airsetting
The mechanical strength of glue own is low, and density is little, it is easy to dry linting.Therefore silica aerogel can not be separately as high temperature thermal insulation material, must
By doping vario-property, and competence exertion must be combined with inorganic reinforcement and goes out its advantage at high-temperature heat insulation aspect of performance.
Summary of the invention
The purpose of the present invention is intended to overcome the deficiencies in the prior art, one of purpose to be to provide, and a kind of preparation technology is simple, preparation is all
Phase is short, with low cost, can be continuously produced, and the hydrophobic type fiber felt with good hydrophobicity and combination property strengthens titanium silicon
Composite aerogel；The two of purpose are to provide this hydrophobic type fiber felt and strengthen the preparation method of titanium silicon compound aerogel.
An object of the present invention can be achieved through the following technical solutions:
This hydrophobic type fiber felt strengthens titanium silicon compound aerogel and is formed by following preparation of raw material:
With tetraethyl orthosilicate: dehydrated alcohol: deionized water: acid=1:3.5～5:0.32:0.015 parts by volume proportioning system
Become SiO2Colloidal sol；Use SiO again2Colloidal sol: titanium dioxide=1:0.05～0.15 proportion by weight are made hydrophobic type fiber felt and strengthened titanium
Silicon compound aerogel product.
An object of the present invention realizes also by techniques below scheme:
Described acid is HCl or HNO of 0.5mol/L～1.5mol/L3In any one, described titanium dioxide is rutile type titanium
In white lead or Detitanium-ore-type titanium dioxide any one.
The two of the purpose of the present invention can be achieved through the following technical solutions:
A kind of hydrophobic type fiber felt recited above strengthens the preparation method of titanium silicon compound aerogel, and preparation process is as follows:
(1) tetraethyl orthosilicate is mixed with the 2/3 of dehydrated alcohol volume, after stirring, obtain solution A；
(2) residue dehydrated alcohol is mixed with deionized water, acid, after stirring, obtain solution B；The purpose of do so is:
If because tetraethyl orthosilicate and dehydrated alcohol are first mixed, the when of adding water or be sour, all can occur at coal addition position
A part of floccule, have impact on stability and hydrophobic effect, this is because in the too fast hydrolysis of coal addition position tetraethyl orthosilicate
Cause with polycondensation.(ethanol is solvent, does not participate in reaction in tetraethyl orthosilicate hydrolytic process；Acid is as catalyst,
Effect is the hydrolysis accelerating tetraethyl orthosilicate；Water is the hydrolysis participating in tetraethyl orthosilicate), therefore dehydrated alcohol
The purpose separately added is that water or acid play the effect of buffering dilution.
(3) solution B is slowly added in solution A, at 50～70 DEG C, reacts 1～2h, obtain solution S iO2Colloidal sol；
(4) SiO is pressed2Colloidal sol: titanium dioxide=1:0.05～0.15 proportion by weight, is added to SiO by titanium dioxide2In colloidal sol,
It is 6～7 with the pH of alkali regulation solution, is stirred continuously prepared titanium silicon composite sol；
(5) the titanium silicon composite sol that step (4) prepares is poured in the mould of fiber felt prefabricated component, treat that colloidal sol is impregnated with
Fiber felt, pours out unnecessary colloidal sol, forms titanium silicon and be combined after titanium silicon composite sol material is stood 1～3h at 50～70 DEG C
Gel rubber material；
(6) by the titanium silicon pluralgel that obtains in step (5) at 50～80 DEG C, carry out solvent with ethanol solution and put
Changing, replace 2～4 days, with surface modifier, titanium silicon composite gel material is carried out surface modification, modification 2～4 days, to obtain
Obtain hydrophobic surface, then carry out solvent displacement with ethanol solution, replace 2～4 days, to remove the unreacted table of material surface
Face modifying agent, thus obtain the titanium silicon composite gel material with hydrophobic surface；
(7) the titanium silicon composite gel material obtained in step (6) is carried out supercritical drying, it is thus achieved that hydrophobic type fiber felt increases
Strong titanium silicon compound aerogel.
The two of the purpose of the present invention realize also by techniques below scheme:
The NH that alkali is 1mol/L～2mol/L in described step (4)3·H2In O or NaOH any one.
Fiber felt used in described step (5) is that glass mat, mullite fiber felt, carbon fiber felt or basalt are fine
Tie up any one in felt.
Surface modifier described in described step (6) is trim,ethylchlorosilane, hexamethyldisiloxane or hexamethyl two silica
In alkane any one.
Described in described step (7), supercritical drying mode is CO2Or in Ethanol supercritical any one, Ethanol supercritical do
Dry baking temperature is 260～280 DEG C, and pressure is 10～12MPa, maintains 2～3 hours under constant temperature and pressure state, then
Sample, CO are taken out in venting2The baking temperature of supercritical drying is 40～50 DEG C, and pressure is 10～12MPa, constant temperature and pressure shape
Maintaining 10～12 hours under state, then sample is taken out in venting.
Compared to existing technology, the method have the advantages that
(1) present invention uses tetraethyl orthosilicate and titanium dioxide to be raw material, and production cost is low, and technique is simple, is suitable for industrialization
Produce.
(2) the hydrophobic type fiber felt that prepared by the present invention strengthens titanium silicon compound aerogel material can be made at high temperature by barrier material effectively
The infrared radiation heat transfer of used time, room temperature thermal conductivity up to 0.021～0.029W/ (m K), the thermal conductivity of 400 DEG C up to
0.035～0.042W/ (m K).
(3) hydrophobic effect of the present invention is obvious, and when the 7th day, hydrophobic rate was 92.4%, and the hydrophobic type fiber felt prepared
Enhancing titanium silicon compound aerogel material not only has certain intensity and can also be folded, and can be used for national defence, Aero-Space, military affairs
Etc. multiple fields, and low-carbon environment-friendly, service life are long.
Accompanying drawing explanation
Fig. 1 is the infrared test that a kind of hydrophobic type basalt fibre felt prepared by example 1 strengthens titanium silicon compound aerogel material
Figure；
Fig. 2 is the sample drawing that a kind of hydrophobic type glass mat prepared by example 2 strengthens titanium silicon compound aerogel material；
Fig. 3 is the hydrophobic rate survey that a kind of hydrophobic type mullite fiber felt prepared by example 3 strengthens titanium silicon compound aerogel material
Attempt；
Fig. 4 is the contact angle test that a kind of hydrophobic type carbon fiber felt prepared by example 4 strengthens titanium silicon compound aerogel material
Figure.
Detailed description of the invention
A kind of hydrophobic type fiber felt strengthens titanium silicon compound aerogel and preparation method, below in conjunction with the accompanying drawings with embodiment to the present invention
Be described further, but invention protection domain and be not so limited.
Embodiment 1
It is 1:3.5:0.32:0.015 by volume by tetraethyl orthosilicate, dehydrated alcohol, deionized water, 0.5mol/L hydrochloric acid
Uniformly mixing, blend step is:
(1) tetraethyl orthosilicate is mixed with the 2/3 of dehydrated alcohol volume, after stirring, obtain solution A；
(2) residue dehydrated alcohol is mixed with deionized water, HCl, after stirring, obtain solution B；
(3) solution B is slowly added in solution A.
1h is reacted, under stirring, by SiO at 50 DEG C2:TiO2(mass ratio)=1:0.05 is by rutile titanium dioxide
Powder is added to SiO2In colloidal sol, add 1mol/LNH3·H2O regulation solution ph is 6, is stirred continuously prepared TiO2-SiO2Multiple
Close colloidal sol；
By TiO2-SiO2Complex sol is poured in the mould of basalt fibre felt prefabricated component, treats that colloidal sol is impregnated with basalt fibre felt,
Pour out unnecessary colloidal sol, after colloidal sol composite is stood at 50 DEG C 1h, form gel complex material；The gel that will obtain
Composite, at 50 DEG C, carries out solvent displacement with ethanol solution, replaces 2 days, with HMDS to gel
Composite carries out surface modification 2 days, to obtain hydrophobic surface, then carries out solvent displacement with ethanol solution, replaces 2
My god, it is thus achieved that there is the gel complex material of hydrophobic surface；The gel complex material Ethanol supercritical obtained is dried,
Baking temperature is 260 DEG C, and pressure is 10MPa, maintains 2 hours under constant temperature and pressure state, and then sample is taken out in venting,
Obtain hydrophobic type basalt fibre felt and strengthen titanium silicon compound aerogel material.
The room temperature thermal conductivity of this material is 0.023W/ (m K), and the thermal conductivity of 400 DEG C is 0.036W/ (m K), as it is shown in figure 1,
As can be seen from the figure there is a lot of hydrophobic methyl groups on the surface of material, so that material has good hydrophobic effect.
Embodiment 2
It is 1:4:0.32:0.015 by volume by tetraethyl orthosilicate, dehydrated alcohol, deionized water, 0.8mol/L hydrochloric acid
Uniformly mixing, blend step is with embodiment 1.
1.2h is reacted, under stirring, by SiO at 55 DEG C2:TiO2(mass ratio)=1:0.07 is by Detitanium-ore-type titanium white
Powder is added to SiO2In colloidal sol, add 1.3mol/LNH3·H2O regulation solution ph is 6.3, is stirred continuously prepared TiO2-SiO2
Complex sol；
By TiO2-SiO2Complex sol is poured in the mould of glass mat prefabricated component, treats that colloidal sol is impregnated with glass mat, falls
Go out unnecessary colloidal sol, after colloidal sol composite is stood at 60 DEG C 1.5h, form gel complex material；The gel that will obtain
Composite, at 60 DEG C, carries out solvent displacement with ethanol solution, replaces 2.5 days, with trim,ethylchlorosilane to gel
Composite carries out surface modification 2.5 days, to obtain hydrophobic surface, then carries out solvent displacement with ethanol solution, displacement
2.5 days, it is thus achieved that there is the gel complex material of hydrophobic surface；The gel complex material CO that will obtain2Supercritical drying
Baking temperature is 40 DEG C, and pressure is 10MPa, maintains 10 hours under constant temperature and pressure state, and then sample is taken out in venting,
Obtain hydrophobic type glass mat and strengthen titanium silicon compound aerogel material.
The room temperature thermal conductivity of this material is 0.025W/ (m K), and the thermal conductivity of 400 DEG C is 0.038W/ (m K), as in figure 2 it is shown,
As can be seen from the figure material blockiness preferably.
Embodiment 3
It is 1:4.5:0.32:0.015 by volume by tetraethyl orthosilicate, dehydrated alcohol, deionized water, 1mol/L nitric acid
Uniformly mixing, blend step is with embodiment 1.
1.5h is reacted, under stirring, by SiO at 65 DEG C2:TiO2(mass ratio)=1:0.1 is by rutile titanium dioxide
Powder is added to SiO2In colloidal sol, add 1.6mol/LNH3·H2O regulation solution ph is 6.6, is stirred continuously prepared TiO2-SiO2
Complex sol；
By TiO2-SiO2Complex sol is poured in the mould of mullite fiber felt prefabricated component, treats that colloidal sol is impregnated with mullite fiber felt,
Pour out unnecessary colloidal sol, after colloidal sol composite is stood at 65 DEG C 2.5h, form gel complex material；Solidifying by obtain
Glue composite, at 70 DEG C, carries out solvent displacement with ethanol solution, replaces 3 days, with trim,ethylchlorosilane to gel
Composite carries out surface modification 3 days, to obtain hydrophobic surface, then carries out solvent displacement with ethanol solution, replaces 3
My god, it is thus achieved that there is the gel complex material of hydrophobic surface；The gel complex material CO that will obtain2Being dried of supercritical drying
Temperature is 50 DEG C, and pressure is 12MPa, maintains 11.5 hours under constant temperature and pressure state, and then sample is taken out in venting, obtains
Obtain hydrophobic type mullite fiber felt and strengthen titanium silicon compound aerogel material.
The room temperature thermal conductivity of this material is 0.028W/ (m K), and the thermal conductivity of 400 DEG C is 0.041W/ (m K), as it is shown on figure 3,
As can be seen from the figure material has good hydrophobic performance.
Embodiment 4
It is 1:5:0.32:0.015 by volume by tetraethyl orthosilicate, dehydrated alcohol, deionized water, 1.5mol/L nitric acid
Uniformly mixing, blend step is with embodiment 1.
2h is reacted, under stirring, by SiO at 70 DEG C2:TiO2(mass ratio)=1:0.15 is by rutile titanium dioxide
Powder is added to SiO2In colloidal sol, add 2mol/LNH3·H2O regulation solution ph is 7, is stirred continuously prepared TiO2-SiO2Multiple
Close colloidal sol；
By TiO2-SiO2Complex sol is poured in the mould of carbon fiber felt prefabricated component, treats that colloidal sol is impregnated with carbon fiber felt, pours out many
Remaining colloidal sol, forms gel complex material after colloidal sol composite stands at 70 DEG C 3h；The gel composite wood that will obtain
Material, at 80 DEG C, carries out solvent displacement with ethanol solution, replaces 4 days, with hexamethyl disiloxane to gel composite wood
Material carries out surface modification 4 days, to obtain hydrophobic surface, then carries out solvent displacement with ethanol solution, replaces 4 days, obtain
Must have the gel complex material of hydrophobic surface；The gel complex material Ethanol supercritical obtained is dried, is dried temperature
Degree is 275 DEG C, and pressure is 12MPa, maintains 3 hours under constant temperature and pressure state, and then sample is taken out in venting, it is thus achieved that dredge
Water type carbon fiber felt strengthens titanium silicon compound aerogel material.
The room temperature thermal conductivity of this material is 0.025W/ (m K), and the thermal conductivity of 400 DEG C is 0.04W/ (m K), as shown in Figure 4,
As can be seen from the figure material has good hydrophobic performance.
Claims (8)
1. a hydrophobic type fiber felt strengthens titanium silicon compound aerogel, it is characterised in that it is formed by following preparation of raw material:
With tetraethyl orthosilicate: dehydrated alcohol: deionized water: acid=1:3.5～5:0.32:0.015 parts by volume proportioning system
Become SiO2Colloidal sol；Use SiO again2Colloidal sol: titanium dioxide=1:0.05～0.15 proportion by weight are made hydrophobic type fiber felt and strengthened titanium
Silicon compound aerogel product.
A kind of hydrophobic type fiber felt the most according to claim 1 strengthens titanium silicon compound aerogel, it is characterised in that: described
Acid is HCl or HNO of 0.5mol/L～1.5mol/L3。
A kind of hydrophobic type fiber felt the most according to claim 1 strengthens titanium silicon compound aerogel, it is characterised in that: described
Titanium dioxide is Rutile type titanium dioxide or Detitanium-ore-type titanium dioxide.
4. the hydrophobic type fiber felt described in claim 1 strengthens a preparation method for titanium silicon compound aerogel, and its feature exists
In: preparation process is as follows:
(1) tetraethyl orthosilicate is mixed with the 2/3 of dehydrated alcohol volume, after stirring, obtain solution A；
(2) residue dehydrated alcohol is mixed with deionized water, acid, after stirring, obtain solution B；
(3) solution B is slowly added in solution A, at 50～70 DEG C, reacts 1～2h, obtain solution S iO2Colloidal sol；
(4) titanium dioxide is added to SiO2In colloidal sol, it is 6～7 with the pH of alkali regulation solution, is stirred continuously prepared titanium silicon multiple
Close colloidal sol；
(5) the titanium silicon composite sol that step (4) prepares is poured in the mould of fiber felt prefabricated component, treat that colloidal sol is impregnated with
Fiber felt, pours out unnecessary colloidal sol, forms titanium silicon composite gel material after then standing 1～3h at 50～70 DEG C；
(6) by the titanium silicon pluralgel that obtains in step (5) at 50～80 DEG C, carry out solvent with ethanol solution and put
Changing, replace 2～4 days, with surface modifier, titanium silicon composite gel material is carried out surface modification, modification 2～4 days, to obtain
Obtain hydrophobic surface, then carry out solvent displacement with ethanol solution, replace 2～4 days, to remove the unreacted table of material surface
Face modifying agent, thus obtain the titanium silicon composite gel material with hydrophobic surface；
(7) the titanium silicon composite gel material obtained in step (6) is carried out supercritical drying, it is thus achieved that hydrophobic type fiber felt increases
Strong titanium silicon compound aerogel.
A kind of hydrophobic type fiber felt the most according to claim 4 strengthens the preparation method of titanium silicon compound aerogel, its feature
It is: in described step (4), alkali is the NH of 1mol/L～2mol/L3·H2O or NaOH.
A kind of hydrophobic type fiber felt the most according to claim 4 strengthens the preparation method of titanium silicon compound aerogel, its feature
It is: fiber felt used in described step (5) is glass mat, mullite fiber felt, carbon fiber felt or basalt
Any one in fiber felt.
A kind of hydrophobic type fiber felt the most according to claim 4 strengthens the preparation method of titanium silicon compound aerogel, and it is special
Levy and be: surface modifier described in described step (6) is trim,ethylchlorosilane, hexamethyldisiloxane or hexamethyl two
In siloxanes any one.
A kind of hydrophobic type fiber felt the most according to claim 4 strengthens the preparation method of titanium silicon compound aerogel, its
It is characterised by: described in described step (7), supercritical drying mode is CO2Or in Ethanol supercritical any one, ethanol surpass
Critical dry baking temperature is 260～280 DEG C, and pressure is 10～12MPa, maintains 2～3 hours under constant temperature and pressure state,
Then sample, CO are taken out in venting2The baking temperature of supercritical drying is 40～50 DEG C, and pressure is 10～12MPa, and constant temperature is permanent
Maintaining 10～12 hours under pressure condition, then sample is taken out in venting.
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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 |
| CN108585922A (en) * | 2018-06-20 | 2018-09-28 | 响水华夏特材科技发展有限公司 | A kind of aeroge ceramic fibre heat-insulating shield and preparation method thereof |
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