CN106745004A - A kind of quick method for preparing hydrophobic silica aerogel of low cost - Google Patents
A kind of quick method for preparing hydrophobic silica aerogel of low cost Download PDFInfo
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- CN106745004A CN106745004A CN201710045567.4A CN201710045567A CN106745004A CN 106745004 A CN106745004 A CN 106745004A CN 201710045567 A CN201710045567 A CN 201710045567A CN 106745004 A CN106745004 A CN 106745004A
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- C01B33/113—Silicon oxides; Hydrates thereof
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- 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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- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
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- C01B33/166—Preparation of silica xerogels by acidification of silicate in the presence of an inert organic phase
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Abstract
The invention discloses a kind of quick method for preparing hydrophobic silica aerogel of low cost, comprise the following steps：S1, silicon source, water and surfactant are uniformly mixed so as to obtain precursor solution；To acid catalyst is added in precursor solution, pH=3 4 is adjusted, then hydrolysis obtains colloidal sol；Base catalyst is added dropwise in S2, the colloidal sol obtained to S1, is stirred continuously during dropwise addition, adjust pH=6 7, stand gel, aging, constant pressure and dry obtains hydrophobic silica aerogel.Low cost of the present invention, with short production cycle without exchange of solvent, free from environmental pollution, obtained hydrophobic silica aerogel has good heat insulation property, hydrophobicity and pliability.
Description
Technical field
Quickly hydrophobic titanium dioxide is prepared the present invention relates to aerosil technical field, more particularly to a kind of low cost
The method of silica aerogel.
Background technology
Aerosil is a kind of light nanoporous material, with high porosity, bigger serface, low-density and
Low thermal conductivity, these features make silica aerogel material in terms of calorifics, acoustics, optics, microelectronics, particle detection all
There is very wide application potential.The subject matter that current aerosil is present is preparation cost too high, is traditionally prepared
Aerosil need to use supercritical drying process, but supercritical drying needs to use autoclave, complex process, into
Originally, high energy consumption, and have certain danger, therefore constant pressure and dry technique is increasingly becoming everybody focus of attention.
Early in eighties of last century nineties, Deshpande, Douglas of University of New Mexico of the U.S. et al. are first with organic
Silicon source is presoma, by molten gel glue, is successfully prepared two in condition of normal pressure using the modified method in exchange of solvent, surface
Silica aerogel, subsequent domestic and foreign scholars are numerous and confused based on this, and aerosil is prepared to normal pressure have been carried out largely
Research, and delivered substantial amounts of article and patent.But traditional constant pressure and dry technique can only obtain aerogel powder not
Can directly apply, and long preparation period present in technique (aging, exchange of solvent, surface modified etc. step need a couple of days) and
The shortcomings of organic solvent consumption big (multiple exchange of solvent).In order to solve these problems, some researchers attempt being prepared in colloidal sol
During introduce the siloxanes containing hydrophobic grouping, saved preparation time so as to save surface modification step.Such as patent
CN103833041A discloses a kind of method that constant pressure and dry prepares flexible silica aerogel block, and the method is containing
The silicon source of machine group is presoma, and pliability is prepared using soda acid two-step catalysis sol-gel process and normal pressure classification dry technology
Aeroge.Patent CN102765725A also discloses that a kind of method that low cost prepares hydrophobic silicon dioxide aerogel, the party
Method is raw material with the siloxanes with alkyl, and wet gel is prepared using sol-gel, then prepares dioxy with the method for constant pressure and dry
SiClx aeroge.Although surface modification step can be saved with the siloxanes technique of hydrophobic grouping, constant pressure and dry need into
The substantial amounts of exchange of solvent of row avoids drying contraction come the water replaced in wet gel, so considerably increases preparation cost and time.
So how low cost and quickly prepare the problem that hydrophobic silica aerogel is current urgent need to resolve.
The content of the invention
Based on the technical problem that background technology is present, the present invention proposes a kind of low cost and quickly prepares hydrophobic silica
The method of aeroge, low cost of the present invention is with short production cycle without exchange of solvent, free from environmental pollution, obtained hydrophobic titanium dioxide
Silica aerogel has good heat insulation property, hydrophobicity and pliability.
The present invention proposes a kind of quick method for preparing hydrophobic silica aerogel of low cost, comprises the following steps：
S1, silicon source, water and surfactant are uniformly mixed so as to obtain precursor solution；To adding acid catalysis in precursor solution
Agent, adjusts pH=3-4, and then hydrolysis obtains colloidal sol；
Base catalyst is added dropwise in S2, the colloidal sol obtained to S1, is stirred continuously during dropwise addition, adjust pH=6-7, stand solidifying
Glue, aging, constant pressure and dry obtains hydrophobic silica aerogel.
Preferably, in S1, silicon source, water and surfactant are uniformly mixed so as to obtain precursor solution；To in precursor solution
Acid catalyst is added, pH=3-4 is adjusted, it is 35-55 DEG C then to adjust temperature, and hydrolysis 0.5-1h obtains colloidal sol.
Preferably, in S1, silicon source be silicon source containing hydrophobic grouping with mixture, the silicon source containing hydrophobic grouping of hydrophilic silicon source in
One kind.
Preferably, silicon source containing hydrophobic grouping is MTMS, MTES or ethyl trimethoxy
Base silane.
Preferably, hydrophilic silicon source is tetraethyl orthosilicate, methyl silicate, Ludox or inorganic silicon source.
Preferably, inorganic silicon source is waterglass or sodium metasilicate.
Preferably, in silicon source containing hydrophobic grouping and the mixture of hydrophilic silicon source, the molar content containing hydrophobic grouping silicon source is big
In 50%.
Preferably, in S1, surfactant is mixture, the fluorine carbon of fluorocarbon surfactant and hc-surfactant
One kind in surfactant.
Preferentially, fluorocarbon surfactant is anion fluorocarbon surfactant, cation fluorine carbon surface active agent, both sexes
Ion fluorocarbon surfactant or non-ion fluorin carbon surface active agent.
Preferably, fluorocarbon surfactant is Du PontDu PontDu PontDu PontDu PontDu PontDu PontDu PontDu PontDu PontDu PontOr Du Pont
Preferably, hc-surfactant is anion hc-surfactant, cation hc-surfactant or non-
Ion hc-surfactant.
Preferably, hc-surfactant be neopelex, hexadecyltrimethylammonium chloride, span80 or
OP-10。
Preferably, in S1, acid catalyst is that aqueous hydrochloric acid solution, aqueous sulfuric acid, aqueous solution of nitric acid or hydrofluoric acid are water-soluble
Liquid.
Preferably, in S1, acid catalyst is aqueous hydrochloric acid solution.
Preferably, in S1, silicon source is 1 with the volume ratio of water：1-6.
Preferably, in S1, silicon source can be 1 with the volume ratio of water：1.1、1：1.2、1：1.3、1：1.4、1：1.5、1：
1.6、1：1.7、1：1.8、1：1.9、1：2、1：2.1、1：2.2、1：2.3、1：2.4、1：2.5、1：2.6、1：2.7、1：2.8、1：
2.9、1：3、1：3.1、1：3.2、1：3.3、1：3.4、1：3.5、1：3.6、1：3.7、1：3.8、1：3.9、1：4、1：4.1、1：
4.2、1：4.3、1：4.4、1：4.5、1：4.6、1：4.7、1：4.8、1：4.9、1：5、1：5.1、1：5.2、1：5.3、1：5.4、1：
5.5、1：5.6、1：5.7、1：5.8 or 1：5.9.
Preferably, in S1, surfactant and precursor solution volume ratio are 0.01-1：100.
Preferably, in S1, surfactant and precursor solution volume ratio can be 0.05：100、0.1：100、
0.15：100、0.2：100、0.25：100、0.3：100、0.35：100、0.4：100、0.45：100、0.5：100、0.55：100、
0.6：100、0.65：100、0.7：100、0.75：100、0.8：100、0.85：100、0.9：100 or 0.95：100.
Preferably, in S2, standing gel time is 5-10min.
Preferably, in S2, it can be 5.5,6,6.5,7,7.5,8,8.5,9 or 9.5min to stand gel time.
Preferably, in S2, aging temperature is 35-55 DEG C, and ageing time is 1-2h.
Preferably, in S2, aging temperature can for 36,37,38,39,40,41,42,43,44,45,46,47,48,
49th, 50,51,52,53 or 54 DEG C, ageing time can be 1.1,1.2,1.3,1.4,1.5,1.6,1.7,1.8 or 1.9h.
Preferably, in S2, constant pressure and dry is that normal pressure is classified drying, is concretely comprised the following steps：60-70 DEG C is warming up to, 1- is dried
3h, is then warming up to 110-130 DEG C, dries 1-3h, then is warming up to 140-160 DEG C, dries 3-5h.
Preferably, in S2, constant pressure and dry is that normal pressure is classified drying, is concretely comprised the following steps：60 DEG C are warming up to, 2h is dried, connect
And be warming up to 120 DEG C, dry 2h, then be warming up to 150 DEG C, dry 4h.
Preferably, in S2, base catalyst is sodium hydrate aqueous solution, potassium hydroxide aqueous solution or ammonia spirit.
Above-mentioned water is deionized water.
Above-mentioned " waterglass " is the aqueous solution of sodium metasilicate.
Above-mentioned acid catalyst, base catalyst, its concentration is not specified, and its concentration is determined according to concrete operations.
Because silicon source containing hydrophobic grouping can not be miscible with water, cause to disperse uneven in a solvent, the present invention is by screening
Adding suitable surfactant can be such that silicon source containing hydrophobic grouping is dispersed in water, be formed after hydrolyzing in acid condition
Colloidal sol, it is cost-effective without using organic solvent, it is to avoid environmental pollution；In addition to the colloidal sol formed by silicon source containing hydrophobic grouping
In base catalyst is directly added dropwise, it may appear that be separated and form precipitation, the present invention can by screening the suitable surfactant of addition
So as to form gel in water by the colloidal sol that silicon source containing hydrophobic grouping is formed and occur without precipitation；The present invention is used and carries hydrophobic group
The silicon source of group saves surface modification technology, cost-effective, shortening preparation time；Replace alcoholic solvent by solvent of water, save into
This, it is to avoid pollution environment；Suitable surfactant is added in aqueous solvent can both promote silicon source dispersed with water, again can be with
The surface tension of presoma is reduced, so that the Pore Solution in gel has very low surface tension, it is not necessary to which solvent is replaced, consumption
Take the plenty of time, directly can obtain hydrophobic silica aerogel by constant pressure and dry, greatly shorten preparation time, reduces cost；
The hydrophobic silica aerogel for preparing has good heat insulation property, hydrophobicity and pliability.
Brief description of the drawings
Fig. 1 is the pictorial diagram of the prepared hydrophobic silica aerogel of the present invention.
Fig. 2 is the microcosmic scanning electron microscope (SEM) photograph of the prepared hydrophobic silica aerogel of the present invention.
Specific embodiment
Below, technical scheme is described in detail by specific embodiment.
Embodiment 1
A kind of quick method for preparing hydrophobic silica aerogel of low cost, comprises the following steps：
S1, silicon source, water and surfactant are uniformly mixed so as to obtain precursor solution；To adding acid catalysis in precursor solution
Agent, adjusts pH=3.5, and then hydrolysis obtains colloidal sol；
Base catalyst is added dropwise in S2, the colloidal sol obtained to S1, is stirred continuously during dropwise addition, adjust pH=6.5, stand solidifying
Glue, aging, constant pressure and dry obtains hydrophobic silica aerogel.
Embodiment 2
A kind of quick method for preparing hydrophobic silica aerogel of low cost, comprises the following steps：
S1, by MTMS, water and Du PontIt is uniformly mixed so as to obtain precursor solution；To presoma
It is the aqueous hydrochloric acid solution of 0.1mol/L that concentration is added in solution, adjusts pH=3, and it is 45 DEG C then to adjust temperature, and hydrolysis 0.5h is obtained
To colloidal sol, wherein, MTMS is 1 with the volume ratio of water：4, Du PontWith precursor solution body
Product is than being 0.5：100；
It is the ammonia spirit of 0.5mol/L that concentration is added dropwise in S2, the colloidal sol obtained to S1, is stirred continuously during dropwise addition, is adjusted
Section pH=6.5, stands gel 10min, is warming up to 45 DEG C, and aging 2h is warming up to 60 DEG C, dries 2h, is then warming up to 120 DEG C,
Dry 2h, then be warming up to 150 DEG C, dry 4h and obtain hydrophobic silica aerogel.
Hydrophobic silica aerogel obtained in embodiment 2 is observed, as a result reference picture 1-2：
Reference picture 1, Fig. 1 is the pictorial diagram of the prepared hydrophobic silica aerogel of the present invention；
Reference picture 2, Fig. 2 is the microcosmic scanning electron microscope (SEM) photograph of the prepared hydrophobic silica aerogel of the present invention.
Embodiment 3
A kind of quick method for preparing hydrophobic silica aerogel of low cost, comprises the following steps：
S1, by silicon source, water and Du PontIt is uniformly mixed so as to obtain precursor solution；It is dense to being added in precursor solution
The aqueous hydrochloric acid solution for 0.1mol/L is spent, pH=3 is adjusted, it is 45 DEG C then to adjust temperature, and hydrolysis 0.5h obtains colloidal sol, wherein,
Silicon source is 1 with the volume ratio of water：3, silicon source is the mixture that MTMS and tetraethyl orthosilicate are constituted, wherein, first
The molar content of base trimethoxy silane is 60%, Du PontIt is 0.5 with precursor solution volume ratio：100；
It is the ammonia spirit of 0.5mol/L that concentration is added dropwise in S2, the colloidal sol obtained to S1, is stirred continuously during dropwise addition, is adjusted
Section pH=6.5, stands gel 5min, is warming up to 45 DEG C, and aging 2h is warming up to 60 DEG C, dries 2h, is then warming up to 120 DEG C, does
Dry 2h, then it is warming up to 150 DEG C, dry 4h and obtain hydrophobic silica aerogel.
Embodiment 4
A kind of quick method for preparing hydrophobic silica aerogel of low cost, comprises the following steps：
S1, ethyl trimethoxy silane, water and surfactant are uniformly mixed so as to obtain precursor solution；To in precursor solution
Aqueous sulfuric acid is added, pH=4 is adjusted, it is 35 DEG C then to adjust temperature, and hydrolysis 1h obtains colloidal sol, wherein, ethyl trimethoxy
Silane is 1 with the volume ratio of water：1, surfactant and precursor solution volume ratio are 1：100, surfactant is Du PontWith the mixture of neopelex；
Sodium hydrate aqueous solution is added dropwise in S2, the colloidal sol obtained to S1, is stirred continuously during dropwise addition, adjust pH=6, it is quiet
Gel 9min is put, 35 DEG C are warming up to, aging 1.5h is warming up to 65 DEG C, dries 3h, is then warming up to 110 DEG C, dries 3h, then rise
Temperature dries 5h and obtains hydrophobic silica aerogel to 140 DEG C.
Embodiment 5
A kind of quick method for preparing hydrophobic silica aerogel of low cost, comprises the following steps：
S1, silicon source, water and surfactant are uniformly mixed so as to obtain precursor solution；To being added in precursor solution, nitric acid is water-soluble
Liquid, adjusts pH=3.2, and it is 55 DEG C then to adjust temperature, and hydrolysis 0.6h obtains colloidal sol, wherein, silicon source is 1 with the volume ratio of water：
6, silicon source is the mixture of MTES and Ludox, wherein, the molar content of MTES is
51%, surfactant and precursor solution volume ratio are 0.01：100, surfactant is Du PontWith
The mixture of span80；
Potassium hydroxide aqueous solution is added dropwise in S2, the colloidal sol obtained to S1, is stirred continuously during dropwise addition, adjust pH=7, it is quiet
Gel 7min is put, 55 DEG C are warming up to, aging 1h is warming up to 70 DEG C, dries 1h, is then warming up to 130 DEG C, dries 1h, then heat up
To 160 DEG C, dry 3h and obtain hydrophobic silica aerogel.
Embodiment 6
A kind of quick method for preparing hydrophobic silica aerogel of low cost, comprises the following steps：
S1, silicon source, water and surfactant are uniformly mixed so as to obtain precursor solution；To addition hydrofluoric acid water in precursor solution
Solution, adjusts pH=3.8, and it is 40 DEG C then to adjust temperature, and hydrolysis 0.8h obtains colloidal sol, wherein, silicon source is with the volume ratio of water
1：2, silicon source is the mixture of ethyl trimethoxy silane and sodium metasilicate, wherein, the molar content of ethyl trimethoxy silane is
80%, surfactant and precursor solution volume ratio are 0.7：100, surfactant is Du PontWith
The mixture of op-10；
Ammonia spirit is added dropwise in S2, the colloidal sol obtained to S1, is stirred continuously during dropwise addition, adjust pH=6.8, stand solidifying
Glue 8min, is warming up to 50 DEG C, and aging 1.3h is warming up to 62 DEG C, dries 2.5h, is then warming up to 125 DEG C, dries 1.5h, then rise
Temperature dries 4.5h and obtains hydrophobic silica aerogel to 145 DEG C.
Test example 1
Embodiment 1-6 is counted, and performance test is carried out to obtained hydrophobic silica aerogel, as a result such as
Under：
As can be seen from the above table, short preparation period of the present invention, can quickly prepare hydrophobic silica aerogel, prepare
Hydrophobic silica aerogel density it is low, heat insulation property is good, and hydrophobicity is good.
The above, the only present invention preferably specific embodiment, but protection scope of the present invention is not limited thereto,
Any one skilled in the art the invention discloses technical scope in, technology according to the present invention scheme and its
Inventive concept is subject to equivalent or change, should all be included within the scope of the present invention.
Claims (10)
1. a kind of method that low cost quickly prepares hydrophobic silica aerogel, it is characterised in that comprise the following steps：
S1, silicon source, water and surfactant are uniformly mixed so as to obtain precursor solution；To acid catalyst is added in precursor solution, adjust
Section pH=3-4, then hydrolysis obtains colloidal sol；
Base catalyst is added dropwise in S2, the colloidal sol obtained to S1, is stirred continuously during dropwise addition, adjust pH=6-7, stand gel,
Aging, constant pressure and dry obtains hydrophobic silica aerogel.
2. the method that low cost quickly prepares hydrophobic silica aerogel according to claim 1, it is characterised in that in S1
In, silicon source, water and surfactant are uniformly mixed so as to obtain precursor solution；To acid catalyst is added in precursor solution, pH is adjusted
=3-4, it is 35-55 DEG C then to adjust temperature, and hydrolysis 0.5-1h obtains colloidal sol.
3. the method that low cost according to claim 1 or claim 2 quickly prepares hydrophobic silica aerogel, it is characterised in that
In S1, silicon source be silicon source containing hydrophobic grouping with mixture, the silicon source containing hydrophobic grouping of hydrophilic silicon source in one kind；Preferably,
Silicon source containing hydrophobic grouping is MTMS, MTES or ethyl trimethoxy silane；Preferably, parent
Water silicon source is tetraethyl orthosilicate, methyl silicate, Ludox or inorganic silicon source；Preferably, inorganic silicon source is waterglass or silicic acid
Sodium；Preferably, in silicon source containing hydrophobic grouping and the mixture of hydrophilic silicon source, the molar content containing hydrophobic grouping silicon source is more than
50%.
4. the method that the low cost according to claim any one of 1-3 quickly prepares hydrophobic silica aerogel, its feature
It is that in S1, surfactant is mixture, the fluorocarbon surfactant of fluorocarbon surfactant and hc-surfactant
In one kind；Preferentially, fluorocarbon surfactant is anion fluorocarbon surfactant, cation fluorine carbon surface active agent, two
Property ion fluorocarbon surfactant or non-ion fluorin carbon surface active agent；Preferably, fluorocarbon surfactant is Du PontDu PontDu PontDu PontDu PontDu PontDu PontDu PontDu PontDu PontDu PontOr Du PontIt is preferred that
Ground, hc-surfactant is anion hc-surfactant, cation hc-surfactant or the hydrocarbon surface of nonionic
Activating agent；Preferably, hc-surfactant be neopelex, hexadecyltrimethylammonium chloride, span80 or
OP-10。
5. the method that the low cost according to claim any one of 1-4 quickly prepares hydrophobic silica aerogel, its feature
It is that in S1, acid catalyst is aqueous hydrochloric acid solution, aqueous sulfuric acid, aqueous solution of nitric acid or hydrofluoric acid aqueous solution；Preferably,
In S1, acid catalyst is aqueous hydrochloric acid solution.
6. the method that the low cost according to claim any one of 1-5 quickly prepares hydrophobic silica aerogel, its feature
It is that in S1, silicon source is 1 with the volume ratio of water：1-6；Preferably, in S1, surfactant and precursor solution volume
Than being 0.01-1：100.
7. the method that the low cost according to claim any one of 1-6 quickly prepares hydrophobic silica aerogel, its feature
It is that in S2, standing gel time is 5-10min.
8. the method that the low cost according to claim any one of 1-7 quickly prepares hydrophobic silica aerogel, its feature
It is that in S2, aging temperature is 35-55 DEG C, and ageing time is 1-2h.
9. the method that the low cost according to claim any one of 1-8 quickly prepares hydrophobic silica aerogel, its feature
It is that in S2, constant pressure and dry is that normal pressure is classified drying, is concretely comprised the following steps：60-70 DEG C is warming up to, 1-3h is dried, then heated up
To 110-130 DEG C, 1-3h is dried, then be warming up to 140-160 DEG C, dry 3-5h.
10. the method that the low cost according to claim any one of 1-9 quickly prepares hydrophobic silica aerogel, its feature
It is that in S2, base catalyst is sodium hydrate aqueous solution, potassium hydroxide aqueous solution or ammonia spirit.
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