CN107188524A - One-step method constant pressure and dry quickly prepares TiO2The method of doping silicon dioxide aerogel powder - Google Patents
One-step method constant pressure and dry quickly prepares TiO2The method of doping silicon dioxide aerogel powder Download PDFInfo
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Abstract
The present invention discloses one-step method constant pressure and dry and quickly prepares TiO2The method of doping silicon dioxide aerogel powder, it includes：Water glass solution is added and mixed in the acid solution quickly stirred, when the pH value of mixed solution reaches 4 ~ 5, then TiO is added2Ultrasonic disperse after powder and drying control chemical additive, mechanical agitation, standing forms gel；It is gel aging, broken, polar solvent is separately added into gel particle and non-polar solven carries out exchange of solvent, progress surface modification in non-polar solven and silane coupler mixed liquor is then placed in, TiO is dried to obtain using normal pressure classification2Doping silicon dioxide aerogel powder.The step sol-gel method with acid as catalytic of the present invention compares soda acid two-step catalysis method, eliminates the ion exchange process of complexity, time saving and energy saving, and reduces cost, is SiO2The large-scale production of aeroge is provided convenience condition, and improves its thermostability energy.
Description
Technical field
The present invention relates to technical field prepared by aerogel powder, more particularly to a kind of one-step method constant pressure and dry is quickly prepared
TiO2The method of doping silicon dioxide aerogel powder.
Background technology
Silica (SiO2) aeroge is a kind of low-density, lower thermal conductivity, low-k, low-refraction, Gao Bibiao
The nanoporous new material of area, high porosity (80~99.8%), these features make aerosil in thermal insulating material
The field such as material, efficient high energy electrode, acoustic impedance coupling material, gas absorption and UF membrane, catalyst carrier, sound insulation has very wide
Wealthy application potential.The thermal conductivity factor of aerosil at normal temperatures as little as 0.02W/ (mK), but when environment temperature liter
Height, infrared radiation heat transfer aggravates during more than 500 DEG C, and this is due to that pure silicon aeroge has through acting on, so spoke to infrared ray
Penetrating thermal conductivity factor can sharply increase, so as to limit its application in high temperature environments.
In terms of preparation method, aerosil generally uses soda acid two-step catalysis method, but there is production
The drawbacks of cost is higher and manufacturing cycle is longer, is unfavorable for industrialized production.If saved using a step acid catalysis preparation method
The process of ion exchange, can not only shorten manufacturing cycle, and be adapted to large-scale industrial production.
Chinese patent CN102602943A refer to the side that one-step method quickly prepares high-performance nano silicon dioxide aerogel
Method, can shorten manufacturing cycle, but this method need to use supercritical drying, the complex process of supercritical drying, cost, energy consumption
Height, and have certain danger.
Chinese patent CN101288835A refer to a kind of TiO2-SiO2Composite aerogel and preparation method thereof.The invention is adopted
With raw material TiCl cheap and easy to get4And industrial waterglass, the Ti/Si mol ratios of composite aerogel are 1:10~10:1, using normal
Drying process is pressed dry, is suitable for large-scale industrial production and application.Wherein ion exchange is taken for industrial waterglass, and ion
Exchange process operation is complex, is unfavorable for industrialization.
The content of the invention
TiO is quickly prepared it is an object of the invention to provide a kind of one-step method constant pressure and dry2Doping silicon dioxide airsetting rubber powder
The method of body, this method be based on a step acid-catalyzed sol-gel technology, using cheap industrial waterglass as silicon source, using acid solution as
Catalyst, adulterate TiO in gel process2Powder, is modified through aging and surface after wet gel is obtained, drying is classified in normal pressure
Under obtain TiO2Doping silicon dioxide aerogel powder.
The technical solution adopted by the present invention is：
One-step method constant pressure and dry quickly prepares TiO2The method of doping silicon dioxide aerogel powder, it includes following step
Suddenly：
(1) water glass solution is added and mixed in the acid solution quickly stirred, when the pH value of mixed solution reaches 4
When~5, then TiO is added2Ultrasonic disperse after powder and drying control chemical additive, mechanical agitation, standing forms gel；
(2) by after gel aging, then crushed, obtain gel particle；
(3) polar solvent is added into gel particle, untill submerging gel particle, is entered in 40~60 DEG C of water baths
Row exchange of solvent, is swapped out the water in gel；
(4) gel for obtaining step (3) is added in non-polar solven, untill submerging gel particle, at 40~60 DEG C
Exchange of solvent is carried out in water bath, to be swapped out the polar solvent added in step (3)；
(5) gel particle after step (4) exchange of solvent is put into non-polar solven and silane coupler mixed liquor,
Surface is carried out in 40~60 DEG C of water baths and is modified 12~24h；
(6) after the solvent in wet gel is poured out, TiO is dried to obtain using normal pressure classification2Doping silicon dioxide aeroge
Powder.
Water glass solution in further scheme, the step (1) is to add waterglass to stir in deionized water
The volume ratio of gained, wherein waterglass and deionized water is 1：1-6；The waterglass is the industrial waterglass that modulus is 2-3.5；
The acid solution is one kind in hydrochloric acid, sulfuric acid, oxalic acid or acetic acid；
The volume ratio of the water glass solution and acid solution is 1：(0.04~0.5).
Further scheme, the TiO2Powder is from the rutile-type that particle diameter is 0.1~3 μm, and its addition is to account for mixing
1~20wt% of solution quality；
The drying control chemical additive is formamide or DMA, its mole with the waterglass
Than for 0.1~2:1.
Churned mechanically speed in further scheme, the step (1) is 200~700r/min, ultrasonic disperse when
Between be 1~5min.
Polar solvent in further scheme, the step (3) be one kind in methanol, ethanol, isopropanol or acetone or
It is a variety of.
Exchange of solvent in further scheme, the step (3) and step (4) be every 4~8h once, exchange 2~3 times.
Further scheme, the non-polar solven of the step (4) is one kind or many in n-hexane, hexamethylene, normal heptane
Kind.
Silane coupler in further scheme, the step (5) is trim,ethylchlorosilane (TMCS), the silicon nitrogen of hexamethyl two
One or more in alkane (HMDZ), HMDO (HMDSO) or APTES；The silane
The ratio of the amount of the material of coupling agent and Si atoms is (0.3~0.85)：1.
Normal pressure classification in further scheme, the step (6) dry refer to wet gel is first dried 4 at 40~60 DEG C~
After 8 hours, then drying 4~8 hours at 80~120 DEG C.
Further scheme, the gel aging, exchange of solvent and Process of Surface Modification are carried out in constant temperature water bath, temperature
Degree control is at 40~60 DEG C.
TiO is quickly prepared the invention discloses a kind of one-step method constant pressure and dry2The side of doping silicon dioxide aerogel powder
Method, the present invention is silicon source from cheap industrial waterglass, using acid solution as catalyst, by adding particle diameter in 0.1~3 μ m
Interior rutile TiO2Powder as infrared light screening agent to improve its heat endurance, through aging and surface after wet gel is obtained
It is modified, obtain TiO in the case where normal pressure classification is dried2Doping silicon dioxide aerogel powder.
The invention has the advantages that：
(1) present invention uses a step sol-gel method with acid as catalytic, doped rutile type TiO2Powder, under constant pressure and dry
To silicon dioxide aerogel powder, the apparent density of powder is 0.05~0.12g/cm3, porosity 95% or so, pore-size distribution
Uniformly, ESEM (SEM) figure illustrates the three-dimensional net structure of aeroge, N2Prepared by adsorption/desorption isothermal curve chart is bright
Aerosil is typical mesoporous nano material.
(2) a step acid-catalyzed sol-gel method of the invention compares soda acid two-step catalysis method, and the ion for eliminating complexity is handed over
Process is changed, it is time saving and energy saving, and cost is reduced, it is SiO2The large-scale production of aeroge is provided convenience condition.While with
Cheap industrial waterglass is silicon source, and cost is greatly reduced.
(3) this hair Hymecromone overdoping rutile TiO2Powder, can be effectively reduced infrared transmittivity, improve its heat steady
Performance, strengthens application in high temperature environments.
(4) the invention provides a kind of quick preparation TiO2The method of doping silicon dioxide aerogel powder, is greatly shortened
Manufacturing cycle, terminates whole preparation time and is no more than 3 days from starting to be prepared into dry.Preparation flow letter of the present invention
It is single, it is easy to operate.
(5) drying mode involved in the present invention is constant pressure and dry, compared to supercritical drying, and reaction temperature is not high, bar
Part is gentle, security is higher, energy-conserving and environment-protective, is adapted to industrialized production.
Brief description of the drawings
Fig. 1 is preparation flow figure of the invention；
Fig. 2 is TiO prepared by the embodiment of the present invention 12The SEM figures of doping SiO2 aeroges；
Fig. 3 is TiO prepared by the embodiment of the present invention 12The TEM figures of doping SiO2 aeroges；
Fig. 4 is TiO prepared by the embodiment of the present invention 22The N of doping SiO2 aeroges2Adsorption/desorption isothermal curve figure.
Embodiment
Following embodiments are further illustrating to be used as the elaboration to the technology of the present invention content to present invention.
Embodiment 1
One-step method constant pressure and dry quickly prepares TiO2The method of doping silicon dioxide aerogel powder, it comprises the following steps
(as shown in Figure 1)：
(1) by waterglass (modulus 3.5) and deionized water by volume 1：3 are mixed and stirred for obtaining water glass solution；
(2) water intaking glass solution 120ml is added in the concentrated hydrochloric acid quickly stirred, controls the speed added first quick and back slow,
When the pH of mixed solution reaches 5, the rutile TiO for accounting for mixed solution 1wt% is added in quick stirring2Powder, is added
1ml formamides.Mechanical agitation 5min, ultrasonic disperse 3min, makes TiO2Powder is dispersed in colloidal sol, and soilless sticking occurs.
(3) after normal temperature gel in 45 DEG C of constant temperature water baths aging 4h, the wet gel after aging is crushed；
(4) 100g wet gel particle is weighed, then 45 are placed in ethanol and n-hexane submergence wet gel particle respectively
Exchange of solvent is carried out in DEG C constant temperature water bath, ethanol and n-hexane respectively exchange 2 times, 8h exchanged every time, excess of solvent is thereafter let out.
(5) surface modification, 45 DEG C of water are carried out in the n-hexane mixed liquor for adding 200ml HMDOs and 100ml
Bath heating, stirs 12h, carries out suction filtration after the completion of being modified, obtains silica wet gel；
(6) silica wet gel is placed in drying at being dried 6 hours, 100 DEG C at 60 DEG C and is then switched off drying within 8 hours
Case, as drying box is cooled to room temperature, you can obtain TiO2Doping silicon dioxide aerogel powder.Its Specifeca tion speeification is referred to
Table 1.The density of wherein aeroge is determined by tap density meter, the porosity of aeroge be by formula porosity=
(1-ρ/ρs(ρ is the density of aeroge, ρ to) × 100%sFor the skeletal density of aeroge, 2.2g/cm is taken3) calculate, heat conduction system
Number is determined by thermal conductivity factor instrument, and hydrophobic angle is determined by contact angle tester.
Table 1
| TiO2Doping | 5wt% |
| Density (g/cm3) | 0.0838 |
| Porosity | 96.2% |
| Thermal conductivity factor (W/ (mK)) | 0.0224 |
| Hydrophobicity | It is hydrophobic, 136 ° of contact angle |
It is illustrated in figure 2 the TiO of the preparation of the embodiment of the present invention 12Adulterate SiO2The SEM figures of aeroge；Fig. 3 is real for the present invention
Apply the TiO of the preparation of example 12Adulterate SiO2The TEM figures of aeroge；Illustrating the TiO2 of doping does not influence the structure of aeroge, aeroge
It is still three-dimensional net structure.
Embodiment 2
(1) by waterglass (modulus 3.5) and deionized water by volume 1:1 is mixed and stirred for obtaining water glass solution；
(2) water intaking glass solution 180ml is added in the concentrated hydrochloric acid quickly stirred, controls the speed added first quick and back slow,
When the pH of mixed solution reaches 5, the rutile TiO for accounting for mixed solution 5wt% is added in quick stirring2Powder (0.95g), then
Add 2ml formamides.Mechanical agitation 5min, ultrasonic disperse 3min, makes TiO2Powder is dispersed in colloidal sol, and soilless sticking goes out
It is existing.
(3) after normal temperature gel in 45 DEG C of constant temperature water baths aging 4h, the wet gel after aging is crushed；
(4) 100g wet gel particle is weighed, respectively with ethanol and n-hexane submergence wet gel particle, 45 DEG C of perseverances are placed in
Exchange of solvent is carried out in warm water bath, ethanol and n-hexane respectively exchange 3 times, 6h exchanged every time, excess of solvent is thereafter let out.
(5) n-hexane for adding 200ml HMDOs and 100ml carries out surface modification, and 45 DEG C of heating water baths are stirred
12h is mixed, suction filtration is carried out after the completion of being modified, obtains silica wet gel；
(6) silica wet gel is placed at 60 DEG C and dried 8 hours, dried 6 hours at 120 DEG C, be then switched off doing
Dry case, as drying box is cooled to room temperature, you can obtain TiO2Doping silicon dioxide aerogel powder.Its Specifeca tion speeification is detailed
It is shown in Table 2.
Table 2
| TiO2Doping | 5wt% |
| Density (g/cm3) | 0.069 |
| Porosity | 96.9% |
| Thermal conductivity factor (W/ (mK)) | 0.0207 |
| Hydrophobicity | It is hydrophobic, 144 ° of contact angle |
As shown in figure 4, the TiO prepared for the embodiment of the present invention 22The N of doping SiO2 aeroges2Adsorption/desorption isothermal curve
Figure, shows that aerosil prepared by the present invention is typical mesoporous nano material.
Embodiment 3
(1) by waterglass (modulus 3.5) and deionized water by volume 1:5 are mixed and stirred for obtaining water glass solution；
(2) water intaking glass solution 180ml is added in the concentrated hydrochloric acid quickly stirred, controls the speed added first quick and back slow,
When the pH of mixed solution reaches 5, the rutile TiO for accounting for mixed solution 10wt% is added in quick stirring2Powder (1.9g), plus
Enter 2ml formamides.Mechanical agitation 5min, ultrasonic disperse 5min, makes TiO2Powder is dispersed in colloidal sol, and soilless sticking occurs.
(3) after normal temperature gel in 45 DEG C of constant temperature water baths aging 4h.Wet gel after aging is crushed；
(4) 100g wet gel particle is weighed, respectively with ethanol and n-hexane submergence wet gel particle, 45 DEG C of perseverances are placed in
Exchange of solvent is carried out in warm water bath, ethanol and n-hexane respectively exchange 2 times, 6h exchanged every time, excess of solvent is thereafter let out.
(5) n-hexane for adding 200ml trim,ethylchlorosilanes and 100ml carries out surface modification, 60 DEG C of heating water baths, stirring
12h, it is modified to complete to carry out suction filtration, obtain silica wet gel；
(6) silica wet gel is placed at 60 DEG C and dried 6 hours, dried 6 hours at 120 DEG C, be then switched off doing
Dry case, as drying box is cooled to room temperature, you can obtain TiO2Doping silicon dioxide aerogel powder.Its Specifeca tion speeification is detailed
It is shown in Table 3.
Table 3
| TiO2Doping | 10wt% |
| Density (g/cm3) | 0.062 |
| Porosity | 97.2% |
| Thermal conductivity factor (W/ (mK)) | 0.0206 |
| Hydrophobicity | It is hydrophobic, 153 ° of contact angle |
Embodiment 4
(1) by waterglass (modulus 3.5) and deionized water by volume 1:6 are mixed and stirred for obtaining water glass solution；
(2) water intaking glass solution 210ml is added in the concentrated hydrochloric acid quickly stirred, controls the speed added first quick and back slow,
When the pH of mixed solution reaches 4, added in quick stirring with the rutile TiO for accounting for mixed solution 20%wt2Powder, is added
2.5mlN, dinethylformamide.Mechanical agitation 5min, ultrasonic disperse 1min, makes TiO2Powder is dispersed in colloidal sol, nothing
Reunite and occur.
(3) after normal temperature gel in 60 DEG C of constant temperature water baths aging 4h, the wet gel after aging is crushed；
(4) 100g wet gel particle is weighed, respectively with isopropanol and hexamethylene submergence wet gel particle, 60 DEG C are placed in
Exchange of solvent is carried out in constant temperature water bath, isopropanol and hexamethylene respectively exchange 3 times, 8h exchanged every time, excess of solvent is thereafter let out.
(5) 200ml3- aminopropyltriethoxywerene werenes are added and 100ml hexamethylenes carry out surface modification, 40 DEG C of water-baths
Heating, stirs 24h, carries out suction filtration after the completion of being modified, obtains silica wet gel；
(6) silica wet gel is placed at being dried 4 hours, 80 DEG C at 40 DEG C and dried 8 hours, it is then switched off drying
Case, as drying box is cooled to room temperature, you can obtain TiO2Doping silicon dioxide aerogel powder.Its Specifeca tion speeification is referred to
Table 4.
Table 4
| TiO2Doping | 5wt% |
| Density (g/cm3) | 0.052 |
| Porosity | 97.6% |
| Thermal conductivity factor (W/ (mK)) | 0.0208 |
| Hydrophobicity | It is hydrophobic, 140 ° of contact angle |
Although illustrative embodiment of the invention is described above, in order to the technology of the art
Personnel understand the present invention, it should be apparent that the invention is not restricted to the scope of embodiment, to the common skill of the art
For art personnel, as long as various change is in the spirit and scope of the present invention that appended claim is limited and is determined, these
Change is it will be apparent that all utilize the innovation and creation of present inventive concept in the row of protection.
Claims (10)
1. one-step method constant pressure and dry quickly prepares TiO2The method of doping silicon dioxide aerogel powder, it is characterised in that：Including with
Lower step：
（1）Water glass solution is added and mixed in the acid solution quickly stirred, when the pH value of mixed solution reaches 4 ~ 5
When, then add TiO2Ultrasonic disperse after powder and drying control chemical additive, mechanical agitation, standing forms gel；
（2）After gel aging, then crushed, obtain gel particle；
（3）Polar solvent is added into gel particle, untill submerging gel particle, is carried out in 40 ~ 60 DEG C of water baths molten
Agent is exchanged, and is swapped out the water in gel；
（4）By step（3）Obtained gel is added in non-polar solven, untill submerging gel particle, in 40 ~ 60 DEG C of water-bath rings
Exchange of solvent is carried out in border, to be swapped out step（3）In plus polar solvent；
（5）Will be through step（4）Gel particle after exchange of solvent is put into non-polar solven and silane coupler mixed liquor, 40
Surface is carried out in ~ 60 DEG C of water baths and is modified 12 ~ 24h；
（6）After solvent in wet gel is poured out, TiO is dried to obtain using normal pressure classification2Doping silicon dioxide aerogel powder.
2. according to the method described in claim 1, it is characterised in that：The step（1）In water glass solution be by waterglass
The gained that stirred in deionized water is added, the wherein volume ratio of waterglass and deionized water is 1：1-6；The waterglass is mould
Number is 2-3.5 industrial waterglass；
The acid solution is one kind in hydrochloric acid, sulfuric acid, oxalic acid or acetic acid；
The volume ratio of the water glass solution and acid solution is 1：（0.04~0.5）.
3. according to the method described in claim 1, it is characterised in that：The TiO2Powder is from the rutile that particle diameter is 0.1 ~ 3 μm
Type, its addition is the 1 ~ 20wt% for accounting for mixed solution quality；
The drying control chemical additive is formamide or DMA, and the mol ratio of itself and the waterglass is
0.1~2:1。
4. according to the method described in claim 1, it is characterised in that：The step（1）In churned mechanically speed for 200 ~
700r/min, the time of ultrasonic disperse is 1 ~ 5min.
5. according to the method described in claim 1, it is characterised in that：The step（3）In polar solvent be methanol, ethanol,
One or more in isopropanol or acetone.
6. according to the method described in claim 1, it is characterised in that：The step（3）And step（4）In exchange of solvent be every
4 ~ 8h once, is exchanged 2 ~ 3 times.
7. according to the method described in claim 1, it is characterised in that：The step（4）Non-polar solven be n-hexane, hexamethylene
One or more in alkane, normal heptane.
8. according to the method described in claim 1, it is characterised in that：The step（5）In silane coupler be trimethyl chlorine
Silane（TMCS）, HMDS（HMDZ）, HMDO（HMDSO）Or APTES
In one or more；The silane coupler and the ratio of the amount of the material of Si atoms are（0.3~0.85）：1.
9. according to the method described in claim 1, it is characterised in that：The step（6）In normal pressure classification dry that refer to will be wet solidifying
After glue elder generation is dried 4 ~ 8 hours at 40 ~ 60 DEG C, then drying 4 ~ 8 hours at 80 ~ 120 DEG C.
10. according to the method described in claim 1, it is characterised in that：The gel aging, exchange of solvent and Process of Surface Modification
Carried out in constant temperature water bath, temperature control is at 40 ~ 60 DEG C.
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| CN114751417A (en) * | 2022-04-13 | 2022-07-15 | 中国科学技术大学先进技术研究院 | Preparation method of silicon dioxide aerogel powder |
| CN114751417B (en) * | 2022-04-13 | 2023-07-04 | 中国科学技术大学先进技术研究院 | Preparation method of silica aerogel powder |
| CN116495774A (en) * | 2023-06-28 | 2023-07-28 | 希纳高科(江苏)有限公司 | Silicon aerogel and preparation method thereof |
| CN116495774B (en) * | 2023-06-28 | 2023-08-25 | 希纳高科(江苏)有限公司 | Silicon aerogel and preparation method thereof |
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