CN106395835A - Preparation method of silicon dioxide block aerogel taking sodium silicate as silicon source - Google Patents
Preparation method of silicon dioxide block aerogel taking sodium silicate as silicon source Download PDFInfo
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- C01—INORGANIC CHEMISTRY
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- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
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Abstract
The invention relates to a preparation method of silicon dioxide block aerogel taking sodium silicate as a silicon source. According to the method, after acid gel is added, trimethylchlorosilane/absolute ethyl alcohol is utilized for modifying, and the silicon dioxide block aerogel is formed through acid catalysis after drying. The preparation method is simple in technology, does not need deionization exchange, is wild in reaction conditions, and can prepare the silicon dioxide block aerogel at normal pressure, and moreover, the silicon dioxide block aerogel is good in block forming and hydrophobicity and high in adsorption efficiency, and is suitable for industrial promotion and application.
Description
Technical field
The invention belongs to adsorbing material studying technological domain is and in particular to a kind of titanium dioxide silico briquette with sodium silicate as silicon source
The preparation method of bromhidrosis gel.
Background technology
Aeroge (aerogels) is typically referred to mutually be assembled with nanometer scale ultramicro powder and is constituted nanoporous network knot
Structure, and it is full of the lightweight nano solid material of gaseous state disperse medium in network hole, its density can as little as 0.03cm3/ g, leads
Hot coefficient can as little as 0.02W/m.K, porosity may be up to 99%, specific surface area up to 500~1000m2/ g, thus be that one kind exists
There is the star of good application prospect in the fields such as aviation, heat-insulating, acoustical delay, integrated circuit, environmental-protection adsorption and catalysis
Material.The formation mechanism of aeroge is to make the gel dehydration that early stage is formed ensure gel not again in dry run simultaneously
Can subside, thus admitting air into the position substituting water in former gel in gel network.At present both at home and abroad many with methyl silicate,
The silicon alkoxides such as tetraethyl orthosilicate are silicon source, prepare SiO with supercritical drying process2Aeroge, its preparation process is complicated, consumption
Can be time-consuming, cost intensive and silicon alkoxide raw material have certain toxicity, and the drying of supercritical High Temperature High Pressure there is also larger danger
Property, thus limiting its large-scale production and application.And not hydrophobically modified aeroge SiO2Aeroge is due to strongly hydrophilic
Understand avalanche when contacting aqueous solution and lose nano-porous structure.Therefore, from more cheap material, more economical preparation skill
Art, it is carried out with hydrophobically modified is SiO in recent years2The focus of aeroge preparation research.
Waterglass is silicon materials that are more cheap and being easy to get, and part research prepares SiO with waterglass silicon source, constant pressure and dry2
Aeroge achieves certain breakthrough.Constant pressure and dry technique typically need to generate through gel, water in aging, organic solvent displacement gel
Point, the step such as hydrophobically modified ultimately generate hydrophobic type aeroge.But at present some preparation technologies such as A.Parvathy Rao,
Poonam M.Shewale A, Sharad D.Bhagat, Fei Shi, Wang Lijiu, Liu Guangwu (201210114691.9) etc. use
Ion exchange resin is by the Na in waterglass+It is replaced into H+Thus obtaining silicic acid, and A.Parvathy Rao, Poonam
The silicic acid gel of the Process Production of M.Shewale A etc. has certain temperature requirement in ageing process, also early stage is generated
Gel be broken under granule fluidized state with organic solvent displacement gel in moisture, drying make will at different temperatures the stage do
Dry, process is extremely loaded down with trivial details, and preparation was not only time-consuming but also uneconomical;Although the technique of Sharad D.Bhagat, Fei Shi does not subsequently have that
Complicated, but there is also the uneconomic problem of ion-exchange process;Also there is research (Shen Jun) not adopt ion exchange, pass through respectively
HF mono- step catalysis-aging-modified and HNO3SiO has been prepared in-NaOH two-step catalysis-aging-modification2Aeroge, but blockiness relatively
Difference, HNO3- NaOH two-step catalysis method product even powder, affects its application.
Content of the invention
It is an object of the invention to provide one kind prepares link and simplifying, can preparing block two of good performance at ambient pressure
The method of silica aerogel.
To achieve these goals, the technical solution adopted in the present invention is to comprise the steps of:
(1) preparation of sodium silicate solution
Sodium silicate granule is added in ultra-pure water and dissolves, prepared mass fraction is 20% sodium silicate solution;
(2) acid adding gel
The mol ratio of ethylene glycol and acetamide, sodium silicate and ethylene glycol and acetamide is added in sodium silicate solution:1:0.9
~1.1:1.9~2.1, then in solution, acid adding is 7~8 to pH while stirring, treats that solution, by clarifying change mist formation white states, stops
Only stirring and acid adding, stands 8~10 minutes, and when inclination 45° angle liquid level does not flow, that is, plastic completes, and obtains wet gel, will be wet
Gel stands aging 24~30h;
(3) substitution
Wet gel after will be aging is washed with deionized removal alkali metal ion, is dipped to wet gel in dehydrated alcohol
In water replaced by dehydrated alcohol completely, then with volume ratio be 1:5~6 trim,ethylchlorosilane/dehydrated alcohol is carried out to gel
Surface modification at least 24 hours, with absolute ethanol washing, obtains modified gel;
(4) it is dried
The modified gel of step (3) is put into be respectively put in air dry oven or vacuum drying oven and be dried, in air blast
With 60 DEG C, 70 DEG C, 80 DEG C of classification dryings, each drying 24~30h in drying baker, entered with 80~85 DEG C of temperature in vacuum drying oven
Row drying, prepared silicon dioxide block aeroge.
Further, above-mentioned steps (2) can be to add ethylene glycol and acetamide, sodium silicate and second in sodium silicate solution
Glycol and the mol ratio of acetamide:1:0.9~1.1:1.9~2.1, then be hydrogenated with while stirring in solution fluoric acid, sulphuric acid or
Acetic acid is 7~8 to pH, treats that solution, by clarifying change mist formation white states, stops stirring and acid adding, stands 8~10 minutes, wait
When 45° angle liquid level does not flow, that is, plastic completes, and obtains wet gel, and wet gel is stood aging 24~30h.
Further, above-mentioned steps (2) can also be:Ethylene glycol and acetamide, sodium silicate is added in sodium silicate solution
Mol ratio with ethylene glycol and acetamide:1:0.9~1.1:1.9~2.1, then salt adding acid while stirring is 7 to pH in solution
~8, treat that solution, by clarifying change mist formation white states, stops stirring and acid adding, stands 8~10 minutes, 45° angle liquid level to be tilted is not
During flowing, that is, plastic completes, and obtains wet gel, and wet gel is stood aging 24~30h;
Corresponding to step (4) is:The modified gel of step (3) is put into and is respectively put into air dry oven or vacuum drying oven
Middle drying, with 60 DEG C, 70 DEG C, 80 DEG C of classification dryings in air dry oven, each 24h is dried, in vacuum drying oven with 80~
85 DEG C of temperature are dried, and use the NaOH of 0.5mol/L to soak 2~3h afterwards, 80~85 DEG C of constant pressure and dries are processed, prepared dioxy
SiClx block aeroge.
The preparation method of the silicon dioxide block aeroge with sodium silicate as silicon source of the present invention, it is after acid adding gel
Modified using trim,ethylchlorosilane (TMCS)/dehydrated alcohol, silicon dioxide Monolithic aerogel is obtained with acid catalysiss after drying, this
Invention Simplified flowsheet, exchanges without deionization, and reaction condition is gentle, can prepare under normal pressure, and gained silicon dioxide is block
Aeroge bulk forming, hydrophobicity is good, adsorption efficiency is high, is suitable to industrial application.
Brief description
Fig. 1 is the structure of the aerosil prepared by the present invention.
Fig. 2 and 3 is the hydrophobic effect of the aerosil prepared by the present invention.
Fig. 4 is SiO before and after post processing2Aeroge XRD spectrum.
Fig. 5 is the infrared spectrum of aerosil.
Fig. 6 is SiO2The impact to absorption for the aeroge difference dosage.
Fig. 7 is the SiO that different acids are not prepared2Aeroge absorption property contrasts.
Specific embodiment
In conjunction with drawings and Examples, technical scheme is further described.
Embodiment 1
The preparation method of the silicon dioxide block aeroge with sodium silicate as silicon source for the present embodiment is realized by following steps:
(1) preparation of sodium silicate solution
Sodium silicate granule is added in ultra-pure water and dissolves, prepared mass fraction is 20% sodium silicate solution;
(2) acid adding gel
Add ethylene glycol and acetamide in sodium silicate solution, make the mol ratio of sodium silicate and ethylene glycol and acetamide:1:
1:2, then in solution while stirring plus sulphuric acid to pH be 7, treat solution by clarify become mist formation white states, stop stirring and plus
Acid, stands 10 minutes, and when inclination 45° angle liquid level does not flow, that is, plastic completes, and obtains wet gel, wet gel is stood aging
24h;
(3) substitution
Wet gel after will be aging is washed with deionized removal alkali metal ion, is dipped to wet gel in dehydrated alcohol
In water replaced by dehydrated alcohol completely, then with volume ratio be 1:5 trim,ethylchlorosilane/dehydrated alcohol carries out surface to gel
Modified 24 hours, with absolute ethanol washing, obtain modified gel;
(4) it is dried
The modified gel of step (3) is put into be respectively put in air dry oven and be dried, in 60 DEG C, 70 DEG C, 80 DEG C of classifications
Be dried, each 24h is dried, prepared silicon dioxide block aeroge, taken pictures with camera, as shown in figure 1, be in block.
Embodiment 2
The preparation method of the silicon dioxide block aeroge with sodium silicate as silicon source for the present embodiment is realized by following steps:
(1) preparation of sodium silicate solution
Sodium silicate granule is added in ultra-pure water and dissolves, prepared mass fraction is 20% sodium silicate solution;
(2) acid adding gel
The mol ratio of ethylene glycol and acetamide, sodium silicate and ethylene glycol and acetamide is added in sodium silicate solution:1:
0.9:2.1, then in solution while stirring plus acetic acid to pH be 8, treat solution by clarify become mist formation white states, stop stirring and
Acid adding, stands 8 minutes, and when inclination 45° angle liquid level does not flow, that is, plastic completes, and obtains wet gel, wet gel is stood aging
30h;
(3) substitution
Wet gel after will be aging is washed with deionized removal alkali metal ion, is dipped to wet gel in dehydrated alcohol
In water replaced by dehydrated alcohol completely, then with volume ratio be 1:6 trim,ethylchlorosilane/dehydrated alcohol carries out surface to gel
Modification at least 24 hours, with absolute ethanol washing, obtains modified gel;
(4) it is dried
The modified gel of step (3) is put into 80~85 DEG C of dryings in vacuum drying oven, prepared silicon dioxide block airsetting
Glue.
Embodiment 3
The preparation method of the silicon dioxide block aeroge with sodium silicate as silicon source for the present embodiment is realized by following steps:
(1) preparation of sodium silicate solution
Sodium silicate granule is added in ultra-pure water and dissolves, prepared mass fraction is 20% sodium silicate solution;
(2) acid adding gel
Add ethylene glycol and acetamide in sodium silicate solution, make the mol ratio of sodium silicate and ethylene glycol and acetamide:1:
1.1:1.9, then be hydrogenated with while stirring in solution fluoric acid to pH be 7, treat solution by clarify become mist formation white states, stop stirring
And acid adding, stand 10 minutes, when inclination 45° angle liquid level does not flow, that is, plastic completes, and obtains wet gel, and wet gel is stood
Aging 28h;
(3) substitution
Wet gel after will be aging is washed with deionized removal alkali metal ion, is dipped to wet gel in dehydrated alcohol
In water replaced by dehydrated alcohol completely, then with volume ratio be 1:6 trim,ethylchlorosilane/dehydrated alcohol carries out surface to gel
Modified 24 hours, with absolute ethanol washing, obtain modified gel;
(4) it is dried
The modified gel of step (3) is put into be respectively put in air dry oven and be dried, in 60 DEG C, 70 DEG C, 80 DEG C of classifications
Be dried, each 30h is dried, prepared silicon dioxide block aeroge.
Embodiment 4
The preparation method of the silicon dioxide block aeroge with sodium silicate as silicon source for the present embodiment is realized by following steps:
(1) preparation of sodium silicate solution
Sodium silicate granule is added in ultra-pure water and dissolves, prepared mass fraction is 20% sodium silicate solution;
(2) acid adding gel
The mol ratio of ethylene glycol and acetamide, sodium silicate and ethylene glycol and acetamide is added in sodium silicate solution:1:
1.1:2, then in solution while stirring salt adding acid to pH be 7, treat solution by clarify become mist formation white states, stop stirring and plus
Acid, stands 8 minutes, and when inclination 45° angle liquid level does not flow, that is, plastic completes, and obtains wet gel, wet gel is stood aging
24h;
(3) substitution
Wet gel after will be aging is washed with deionized removal alkali metal ion, is dipped to wet gel in dehydrated alcohol
In water replaced by dehydrated alcohol completely, then with volume ratio be 1:5~6 trim,ethylchlorosilane/dehydrated alcohol is carried out to gel
Surface modification at least 24 hours, with absolute ethanol washing, obtains modified gel;
(4) it is dried
The modified gel of step (3) is put into 80~85 DEG C of temperature in vacuum drying oven be dried, use 0.5mol/ afterwards
The NaOH of L soaks 3h, 85 DEG C of constant pressure and dries are processed, prepared silicon dioxide block aeroge.
Drying condition in above-described embodiment 4 can also be classified drying using air dry oven, uses 0.5mol/L afterwards again
NaOH soak, 80 DEG C of constant pressure and dries, be not limited only to the drying mode of above-described embodiment.
In order to verify the technique effect of the present invention, inventor passes through taking the aerosil of embodiment 1 preparation as a example
Hereinafter experiment illustrates, specially:
(1) aerosil and its hydrophobic performance
Aerosil obtained by the embodiment of the present invention 1 is placed in water tumbler, and surface sprinkling thereon, see
Examine its hydrophobicity, and take pictures result as shown in Figures 2 and 3 with camera.
The block figure it is seen that aerosil is creamy white, floats on water surface, and its density is after measured
0.08~0.10kg/m3;From figure 3, it can be seen that water droplet is in relatively regular spheroid on aeroge surface, aeroge hydrophobicity is described
Well.
(2) X-ray diffraction (XRD)
Observe the embodiment of the present invention 1 gained aerosil using X-ray diffractometer, result is as shown in Figure 4.
Fig. 4 is that aeroge X-ray diffraction (XRD) result prepared can be seen that with silicic acid and sodium salt acid normal pressure preparation
The SiO obtaining2XRD spectrum have a disperse broad peak between 20 degree to 30 degree, meanwhile, at 32,46,57,68,76 degree
There is strong peak in left and right, its appearance angle is corresponding with silicic acid crystal again.The SiO of this explanation preparation2Aeroge is typical no fixed
Also exist compared with multi-silicate crystal in type (amorphous) structure, and sample.And the sample through NaOH post processing, the peak value of disperse broad peak
It is remarkably reinforced, the peak value of silicic acid crystal almost disappears, show having reached in the base not destroying raw sample framing structure of post processing
Silicic acid is converted on plinth by the effect of silicon dioxide.
(3) FTIR spectrum (FIIR)
Fig. 5 is the FTIR spectrum (FIIR) of aerosil it can be seen that in 850cm-1Nearby occur in that
Peak, illustrates aerosil after surface modification, and aeroge skeleton surface has connected silicon methyl;In 1088cm-1,
461cm-1The peak nearby occurring represents antisymmetric stretching vibration and the bending vibration of Si-O-Si respectively, in 960cm-1Nearby exist
Peak represent Si-OH stretching vibration peak substantially inconspicuous, this explanation aerosil through trim,ethylchlorosilane surface
After hydrophobically modified, silicone hydroxyl is considerably less, has reached the effect of hydrophobically modified.
(4) adsorption effect
A certain amount of silicon dioxide block aeroge is added in the C.I. 13020. solution that 100mL concentration is 100mg/L, every
0.5h measures C.I. 13020. concentration until C.I. 13020. concentration no longer changes, and to check its adsorption effect, result is as shown in Figures 6 and 7.
By Fig. 6 and 7 as can be seen that 0.4g/L adsorbent amount under decolouring 4h after C.I. 13020. percent of decolourization up to 85% with
On, thus can illustrate that the present invention can reach little adsorption effect in the case that consumption is few.
Above-mentioned experiment simply illustrates taking the product of embodiment 1 as a example, and other embodiment products obtained therefroms all can obtain
To close experimental result, gained silicon dioxide block aeroge of the present invention is in block shape, and consumption is few and by preferably hydrophobic
Property and adsorption effect.
Claims (3)
1. a kind of preparation method of the silicon dioxide block aeroge with sodium silicate as silicon source is it is characterised in that by following steps group
Become:
(1) preparation of sodium silicate solution
Sodium silicate granule is added in ultra-pure water and dissolves, prepared mass fraction is 20% sodium silicate solution;
(2) acid adding gel
The mol ratio of ethylene glycol and acetamide, sodium silicate and ethylene glycol and acetamide is added in sodium silicate solution:1:0.9~
1.1:1.9~2.1, then in solution, acid adding is 7~8 to pH while stirring, treats that solution, by clarifying change mist formation white states, stops
Stirring and acid adding, stand 8~10 minutes, and when inclination 45° angle liquid level does not flow, that is, plastic completes, and obtains wet gel, will be wet solidifying
Glue stands aging 24~30h;
(3) substitution
Wet gel after will be aging is washed with deionized removal alkali metal ion, is dipped in wet gel in dehydrated alcohol
Water is replaced by dehydrated alcohol completely, then is 1 with volume ratio:5~6 trim,ethylchlorosilane/dehydrated alcohol carries out surface to gel
Modification at least 24 hours, with absolute ethanol washing, obtains modified gel;
(4) it is dried
The modified gel of step (3) is put in air dry oven or vacuum drying oven and is dried, air dry oven is used 60
DEG C, 70 DEG C, 80 DEG C classification dryings, each drying 24~30h, be dried with 80~85 DEG C of temperature in vacuum drying oven, be obtained
Silicon dioxide block aeroge.
2. the preparation method of the silicon dioxide block aeroge with sodium silicate as silicon source according to claim 1, its feature
It is:Described step (2) is to add ethylene glycol and acetamide in sodium silicate solution, the rubbing of sodium silicate and ethylene glycol and acetamide
You compare:1:0.9~1.1:1.9~2.1, then be hydrogenated with while stirring in solution fluoric acid, sulphuric acid or acetic acid to pH be 7~8, treat
Solution, by clarifying change mist formation white states, stops stirring and acid adding, stands 8~10 minutes, 45° angle liquid level to be tilted does not flow
When, that is, plastic completes, and obtains wet gel, and wet gel is stood aging 24~30h.
3. the preparation method of the silicon dioxide block aeroge with sodium silicate as silicon source according to claim 1, its feature
It is:Described step (2) is to add ethylene glycol and acetamide in sodium silicate solution, the rubbing of sodium silicate and ethylene glycol and acetamide
You compare:1:0.9~1.1:1.9~2.1, then in solution, salt adding acid while stirring is 7~8 to pH, treats that solution is become by clarification
Mist white states, stop stirring and acid adding, stand 8~10 minutes, and when inclination 45° angle liquid level does not flow, that is, plastic completes, and obtains
To wet gel, wet gel is stood aging 24~30h;
Described step (4) is:The modified gel of step (3) is put in air dry oven or vacuum drying oven and is dried, rousing
In wind drying baker with 60 DEG C, 70 DEG C, 80 DEG C classification dryings, each 24h is dried, carried out with 80~85 DEG C of temperature in vacuum drying oven
It is dried, use the NaOH of 0.5mol/L to soak 2~3h afterwards, 80~85 DEG C of constant pressure and dries are processed, prepared silicon dioxide block airsetting
Glue.
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Cited By (6)
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CN107934972A (en) * | 2017-12-07 | 2018-04-20 | 西安科技大学 | It is a kind of using gangue as block aerosil of silicon source and its preparation method and application |
CN109133070A (en) * | 2018-08-28 | 2019-01-04 | 浙江工业大学 | A method of hydrophobic silica aerogel is prepared by the supper-fast normal pressure of raw material of waterglass |
CN109650396A (en) * | 2019-01-28 | 2019-04-19 | 安徽科昂纳米科技有限公司 | A kind of preparation method of aerosil and aerosil obtained |
CN110329175A (en) * | 2019-05-23 | 2019-10-15 | 连云港冠泰汽车配件有限公司 | A kind of passive acoustic material of passenger car crew module NVH |
CN115432710A (en) * | 2022-09-16 | 2022-12-06 | 西安科技大学 | Preparation method of ultra-low density silicon dioxide aerogel block |
CN115432710B (en) * | 2022-09-16 | 2024-07-16 | 西安科技大学 | Preparation method of ultralow-density silica aerogel block |
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107934972A (en) * | 2017-12-07 | 2018-04-20 | 西安科技大学 | It is a kind of using gangue as block aerosil of silicon source and its preparation method and application |
CN109133070A (en) * | 2018-08-28 | 2019-01-04 | 浙江工业大学 | A method of hydrophobic silica aerogel is prepared by the supper-fast normal pressure of raw material of waterglass |
CN109650396A (en) * | 2019-01-28 | 2019-04-19 | 安徽科昂纳米科技有限公司 | A kind of preparation method of aerosil and aerosil obtained |
CN110329175A (en) * | 2019-05-23 | 2019-10-15 | 连云港冠泰汽车配件有限公司 | A kind of passive acoustic material of passenger car crew module NVH |
CN115432710A (en) * | 2022-09-16 | 2022-12-06 | 西安科技大学 | Preparation method of ultra-low density silicon dioxide aerogel block |
CN115432710B (en) * | 2022-09-16 | 2024-07-16 | 西安科技大学 | Preparation method of ultralow-density silica aerogel block |
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