CN107082431A - A kind of fast preparation method of aerosil - Google Patents
A kind of fast preparation method of aerosil Download PDFInfo
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- CN107082431A CN107082431A CN201710288017.5A CN201710288017A CN107082431A CN 107082431 A CN107082431 A CN 107082431A CN 201710288017 A CN201710288017 A CN 201710288017A CN 107082431 A CN107082431 A CN 107082431A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- 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
- C01B33/157—After-treatment of gels
- C01B33/158—Purification; Drying; Dehydrating
- C01B33/1585—Dehydration into aerogels
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/10—Solid density
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
- C01P2006/17—Pore diameter distribution
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/32—Thermal properties
Abstract
The invention provides a kind of fast preparation method of aerosil, it is silicon source from positive silicic acid fat, add the organic monoacid catalytic hydrolysis reaction of low concentration, again by rationally controlling the addition of nitrogenous silane, drop rate and reaction time complete gel polycondensation reaction and the step of hydrophobically modified one, without adding base catalyst again, and avoid a large amount of consumption in general rear hydrophobically modified method to replacing solvent, do not produce waste liquid, and greatly shorten manufacturing cycle, reduce process costs, it is easy to industrialized production, the aerosil product prepared simultaneously has excellent performance.
Description
Technical field
The invention belongs to aerosil preparing technical field, more particularly, to a kind of aerosil
Fast preparation method.
Background technology
Aerosil has three-dimensional network shape skeleton structure, with low-density (0.03~0.2g/cm3), Gao Kong
Gap rate (85%~99%), low heat conduction (0.01~0.03Wm-1·K-1), high-specific surface area (600~1200m2/ g) etc. it is many
Excellent properties, are usually used in the fields such as Aero-Space, petroleum and petrochemical industry, metallurgy.
Aerosil most passed through sol-gel process and Supercritical Drying Technology system early in 1931 by Kistler
Standby to obtain, this method also turns into current most common method.Sol-gel process usually requires the step of soda acid two and is catalyzed silicon source respectively
Hydrolysis, polycondensation two-step reaction.The acid of use is generally the organic acids such as hydrochloric acid, and the base catalyst of use is generally ammoniacal liquor, hydrogen-oxygen
Change sodium etc., the silicon source used is tetraethyl orthosilicate, methyl silicate, waterglass and its allogenic material raw material, and organic silicon source is made
Product purity is high, performance is stable；Waterglass and its allogenic material raw material such as flyash, stalk, diatomite etc. are with low cost, but
Need to carry out complicated pretreatment because impurity is more.After sol gel reaction, wet gel is done under supercritical fluid
It is dry, it is necessary to high-temperature high-voltage reaction condition.Aeroge performance is stable obtained by supercritical drying drying method, but cost is higher, exist certain
Potential safety hazard, while equipment operational factor is complicated, it is difficult to realize large-scale continuous production.In consideration of it, the preparation of aeroge
Cost is higher, as its wide variety of main cause of restriction.
Many scholars carry out the preparation of aeroge using constant pressure and dry technology generations for supercritical process in recent years.Due to solidifying
Glue surface after hydrolytie polycondensation carries hydroxyl, it is necessary to which carrying out surface alkylation makes it have hydrophobic performance, therefore constant pressure and dry system
Standby technique generally includes sol-gel, gel aging, solvent displacement, modified, cleaning, several steps such as dries, processing step compared with
Many, manufacturing cycle is longer, and solvent displacement needs to consume substantial amounts of chemical reagent with modification procedure, and waste liquid is more, and environment can be made
Into certain influence, additionally due to common constant pressure and dry mode is heated by outside, thermograde is formed, often table
Face is dried and moisture is contained in inside, causes time-consuming longer, the product homogeneity of drying process in aeroge large-scale production poor.
The content of the invention
In view of this, the present invention is directed to propose one kind can complete gel polycondensation reaction and the step of hydrophobically modified one, realize
The shortening of process cycle, while can avoid producing waste liquid, two with premium properties that are with low cost, being easy to industrialized production
The preparation method of silica aerogel, to solve the above problems.
To reach above-mentioned purpose, what the technical scheme of the invention was realized in：
A kind of fast preparation method of aerosil, comprises the following steps：
(1) it is silicon source from positive silicic acid fat, after the silicon source alcohol is dissolved, the organic weak of low concentration is added into solution
Acid-catalyzed hydrolysis reaction obtains solution A；
(2) under conditions of stirring, organic nitrogen-containing silane is added dropwise into solution A, is stood after being added dropwise to complete, obtains gel A,
Wherein, the mol ratio of the organic nitrogen-containing silane and the silicon source is (0.2~0.5):1, the dropwise addition of the organic nitrogen-containing silane
Total time is 2~7 hours；
(3) target product aerosil is obtained after gel A is dried.
Further, the gel A first carries out burin-in process before being dried, and the aging temperature is 20~60 DEG C,
Ageing time is T1, 0h ＜ T1≤1h。
Further, the volume ratio of the alcoholic solvent and the silicon source is (2~3):1, the alcoholic solvent is methanol, second
One kind in alcohol, propyl alcohol.
Further, the concentration of the organic monoacid is 0.0001~0.01mol/L, the organic monoacid and the silicon source
Mol ratio be (0.8~1.2):1, the catalytic hydrolysis reaction time is 0.5~12h.
Further, the concentration of the organic monoacid is 0.0005~0.005mol/L, the catalytic hydrolysis reaction time
For 8~12h.
Further, the organic monoacid be ethanedioic acid, malonic acid, succinic acid, benzoic acid, phthalic acid, to benzene two
One kind in formic acid, salicylic acid, lactic acid, citric acid, tartaric acid, malic acid, glyceric acid, stearic acid, glyoxalic acid, oxaloacetic acid.
Further, the dropwise addition total time of the organic nitrogen-containing silane is 3~5 hours.
Further, the organic nitrogen-containing silane is tetramethyl-disilazane, HMDS, the silicon nitrogen of seven methyl two
At least one of alkane, tetramethyl divinyl disilazane, the silazane of pregnancy basic ring three.
Further, the drying mode in the step (3) is microwave drying or microwave-baking oven combined drying；Microwave is done
Dry condition is that microwave power is 200~800W, and the microwave time is 20~600s；The condition of oven drying is that drying temperature is
100~150 DEG C, drying time is T2, 0h ＜ T2≤2h。
Relative to prior art, a kind of fast preparation method of aerosil of the present invention has following excellent
Gesture：
(1) method completed first using dehydrating condensation formation gel with the step of hydrophobically modified one in the present invention, by reasonable
Controlling the addition, drop rate and reaction time of nitrogenous silane is successively performed polycondensation reaction and hydrophobically modified.Using nitrogenous
Silane meets water generation alkalescence NH3·H2Polycondensation reaction in O, catalyst system and catalyzing, while being carried out using the methyl in silane to it hydrophobic
It is modified, it is not necessary to base catalyst to be added again, while avoid needs to consume a large amount of solvents in general rear hydrophobically modified method
The step of carrying out solvent displacement, waste liquid will not be produced while greatly shortening manufacturing cycle, reduce process costs, it is to avoid
The environmental pollution that is likely to result in；
(2) method completed as a result of dehydrating condensation formation gel with the step of hydrophobically modified one, gel network can be more
Plus stabilization is quickly built, therefore can effectively shorten ageing time, in this embodiment it is not even necessary to carry out in burin-in process, conventional method
Ageing time usually require 1 to 2 days, and the present invention then by ageing time control in 1h, further shorten preparation
Cycle, while also reducing energy consumption；
(3) organic monoacid of low concentration is used for hydrolyst in the present invention, the water of weak acid solution can meet silicon source
Hydrolysis is required, it is not necessary to additionally add moisture, simultaneously because concentration is relatively low, hydrolysis is gently controllable, in the same of hydrolysis
When have certain polycondensation reaction；
(4) in the present invention using microwave drying or microwave-baking oven combined drying method, it is to avoid supercritical drying work
The high-temperature and high-pressure conditions of skill, process is more safe and reliable, at the same overcome oven drying presence the easy drying in surface and it is internal not
Easily dry, the problem of drying process takes long, by rationally controlling drying condition, performance can be prepared stable, excellent
Aerosil；Microwave drying is heating from inside to outside, with rate of drying is fast, energy consumption is low, heating is easy to control, reaction
Uniform the features such as, by rationally controlling drying condition, it is possible to prevente effectively from the excessive desiccation of surface of material and organic solvent quickly expand
Dissipate the risk existed；
(5) preparation method technique of the present invention is simply controllable, can foreshorten to manufacturing cycle 1 day or so, can
Realize large-scale continuous production；
(6) the aerosil function admirable prepared using preparation method of the present invention, stably, density is
40~60kg/m3, porosity reach 97%, specific surface area up to 1050m2/ g, thermal conductivity factor are 0.010~0.018W/ (m ﹒ K)
Brief description of the drawings
Fig. 1 is the aerosil scanning electron microscope (SEM) photograph prepared using preparation method of the present invention；
Fig. 2 is Fig. 1 partial enlarged drawing.
Embodiment
In addition to being defined, technical term used has and the invention one of ordinary skill in the art in following examples
The identical meanings being commonly understood by.Test reagent used, is routine biochemistry reagent unless otherwise specified in following examples；
The experimental method, is conventional method unless otherwise specified.
The invention is described in detail with reference to embodiment and accompanying drawing.
Embodiment 1
1L tetraethyl orthosilicates are added in 2L methanol solvates, after being mixed evenly, addition concentration is 0.005mol/L
Ethanedioic acid solution 120ml, stand 10h after stirring；140ml tetramethyl-disilazanes are delayed with 0.75ml/min speed
Slowly it is added dropwise in above-mentioned reaction system, total time for adding is 3h, standing obtains after gel aging 0.5h, aging knot at 50 DEG C
Carry out oven drying after beam after microwave drying 300s again under 600W power, the condition of oven drying is dry 1.5h at 120 DEG C,
Products therefrom is aerosil；
The aerosil product density of gained is 57kg/m after tested3, specific surface area 920m2/ g, thermal conductivity factor
0.016W/ (m ﹒ K).
Embodiment 2
1L tetraethyl orthosilicates are added in 2.5L alcohol solvents, after being mixed evenly, addition concentration is 0.002mol/
L benzoic acid solution 220ml, 12h is stood after stirring；270ml HMDSs is slow with 1ml/min speed
It is added dropwise in above-mentioned reaction system, total time for adding is 4.5h, standing obtains after gel the aging 1h at 50 DEG C, and aging terminates
Carry out oven drying after microwave drying 120s again under 450W power afterwards, the condition of oven drying is dry 1.5h, institute at 150 DEG C
It is aerosil to obtain product；
The aerosil product density of gained is 45kg/m after tested3, specific surface area 1050m2/ g, thermal conductivity factor
0.013W/ (m ﹒ K).
Embodiment 3
1L tetraethyl orthosilicates are added in 2L alcohol solvents, after being mixed evenly, addition concentration is 0.001mol/L
Glacial acetic acid solution 310ml, stand 3h after stirring；By heptamethyldisilazane and the silazane of pregnancy basic ring three with 1:3
Mixed in molar ratio is 200ml mixed liquors, the mixed liquor is slowly dropped into reaction system with 1ml/min speed, during overall reaction
Between be 3.3 hours, standing obtain carrying out oven drying after gel after microwave drying 200s again under 200W power, oven drying
Condition is dry 2h at 105 DEG C, and products therefrom is aerosil；
The aerosil product density of gained is 60kg/m after tested3, specific surface area 865m2/ g, thermal conductivity factor
0.018W/ (m ﹒ K).
Preparation method of the present invention by rationally control the addition, drop rate and reaction time of nitrogenous silane come
Realize that gel polycondensation reaction is completed with the step of hydrophobically modified one, illustrate course of reaction by taking HMDS (HMDZ) as an example：
HMDZ is hydrolyzed：(CH3)3SiNHSi(CH3)3+2H2O→NH3↑+2(CH3)3SiOH
Colloidal sol polycondensation reaction：
Hydrophobically modified：≡SiOH+(CH3)3SiOH→≡Si-O-Si(CH3)3+H2O
Nitrogenous silane meets water decomposition release ammonia, and ammonia formation ammoniacal liquor soluble in water has catalysis to the silicon source hydrolyzed
The effect of polycondensation reaction, so as to form gel；And the hydroxyl on the silicon oxide compound surface of polycondensation can further by methyl replace from
And complete hydrophobically modified, during the course of the reaction by rationally control nitrogenous silane addition and add speed, can avoid by
Enter reaction system formation precipitation or other accessory substances in the ammoniacal liquor of excessive concentration, control drop rate and reaction time make polycondensation
Reaction and hydrophobically modified reaction are successively performed；
Method of the preparation method of the present invention due to being completed using dehydrating polycondensation with the step of hydrophobically modified one, gel network
It is basicly stable, shorten and even eliminate burin-in process step, while need not consume a large amount of solvents carries out solvent displacement, greatly
Manufacturing cycle is shortened, process costs is reduced, waste liquid is not produced, is easy to industrialized production, and the silica airsetting prepared
Glue properties of product are excellent；
Such as Fig. 1, shown in 2, the aerosil average pore size obtained using preparation method of the present invention is existed
13nm or so, aperture is small and is evenly distributed, and density is in 40~60kg/m3, porosity reach 97%, specific surface area up to 1050m2/
G, thermal conductivity factor are 0.010~0.018W/ (m ﹒ K), with good thermal and insulating performance.
In order to further illustrate the advantage of preparation method of the present invention, below as normal pressure well known in the prior art
Seasoning prepares aerosil, with being compared according to the method described in the present invention.
Comparative example 1
1L tetraethyl orthosilicates are added in 2.5L alcohol solvents, after being mixed evenly, it is 0.01mol/L's to add concentration
Hydrochloric acid solution 200ml, 2h is stood after stirring；Add 0.1mol/L ammoniacal liquor 60ml and form it into gel；At 60 DEG C after gel
Aging 24h in water-bath, wherein aging are divided into two steps, and the first step is 1 in water and ethanol volume ratio:Aging 12h in 4 mixed liquor,
Second step, is 1 in tetraethyl orthosilicate and ethanol volume ratio:Aging 12h in 4 mixed liquor；Aging terminate after respectively in isopropanol
Solution, isopropanol and n-hexane volume ratio are 3:1 mixed liquor, isopropanol and n-hexane volume ratio is 1:1 mixed liquor, isopropyl
Alcohol and n-hexane volume ratio are 1:12h is replaced respectively in 3 mixed liquor；Wet gel is changed using HMDS
Property；Cleaned after 12h with n-hexane 3 times, each 12h；Wet gel dries 15h at 150 DEG C of baking oven, and products therefrom is titanium dioxide
Silica aerogel；
The aerogel products density 52kg/m finally given after tested3, specific surface area 936m2/ g, thermal conductivity factor 0.015W/
(m ﹒ K)
Comparative example 2
1L tetraethyl orthosilicates are added in 2.5L alcohol solvents, after being mixed evenly, it is 0.01mol/L's to add concentration
Hydrochloric acid solution 200ml, 2h is stood after stirring；Add 0.1mol/L ammoniacal liquor 60ml and form it into gel；At 60 DEG C after gel
Aging 24h in water-bath, wherein aging are divided into two steps, and the first step is 1 in water and ethanol volume ratio:Aging 12h in 4 mixed liquor,
Second step, is 1 in the volume ratio of tetraethyl orthosilicate and ethanol:Aging 12h in 4 mixed liquor；Aging is in volume ratio after terminating
Ethanol：HMDS：N-hexane=1:1:Replace 24h in 8 modification liquid, after the completion of clean 3 times with n-hexane, every time
12h；Wet gel is separately dried 4h, 8h, 2h products therefrom as aerosil at 50 DEG C, 150 DEG C, 200 DEG C of baking oven；
The aerogel products density 89kg/m finally given after testing3, specific surface area 812m2/ g, thermal conductivity factor 0.021W/
(m ﹒ K)
Comparative example 1,2 is compared with embodiment 1~3 and understood, atmosphere pressure desiccation prepares silica airsetting in the prior art
Glue, only long preparation period, one step of burin-in process are accomplished by the time of at least one day, complex technical process, it is necessary to consume big
Measure solvent and carry out solvent displacement, not only consume the time, improve production cost and also create substantial amounts of waste liquid, and embodiment 1
~3 in addition to the obvious advantage in preparation method, additionally it is possible to ensures that the aerosil prepared has good product
Performance, the performance for the aerosil that even better than some known atmosphere pressure desiccations are prepared.
The preferred embodiment of the invention is the foregoing is only, creation is not intended to limit the invention, it is all at this
Within the spirit and principle of innovation and creation, any modification, equivalent substitution and improvements made etc. should be included in the invention
Protection domain within.
Claims (9)
1. a kind of fast preparation method of aerosil, it is characterised in that：Comprise the following steps：
(1) it is silicon source from positive silicic acid fat, after the silicon source alcohol is dissolved, the organic monoacid that low concentration is added into solution is urged
Change hydrolysis and obtain solution A；
(2) under conditions of stirring, organic nitrogen-containing silane is added dropwise into solution A, is stood after being added dropwise to complete, obtains gel A, its
In, the mol ratio of the organic nitrogen-containing silane and the silicon source is (0.2~0.5):1, the dropwise addition of the organic nitrogen-containing silane is total
Time is 2~7 hours；
(3) target product aerosil is obtained after gel A is dried.
2. a kind of fast preparation method of aerosil according to claim 1, it is characterised in that：The gel
A first carries out burin-in process before being dried, and aging temperature is 20~60 DEG C, and ageing time is T1, 0h ＜ T1≤1h。
3. a kind of fast preparation method of aerosil according to claim 1, it is characterised in that：The alcohol is molten
The volume ratio of agent and the silicon source is (2~3):1, the alcoholic solvent is one kind in methanol, ethanol, propyl alcohol.
4. a kind of fast preparation method of aerosil according to claim 1, it is characterised in that：It is described organic
The concentration of weak acid is 0.0001~0.01mol/L, and the mol ratio of the organic monoacid and the silicon source is (0.8~1.2):1, institute
The catalytic hydrolysis reaction time is stated for 0.5~12h.
5. a kind of fast preparation method of aerosil according to claim 4, it is characterised in that：It is described organic
The concentration of weak acid is 0.0005~0.005mol/L, and the catalytic hydrolysis reaction time is 8~12h.
6. a kind of fast preparation method of aerosil according to any one of claim 1 to 5, its feature exists
In：The organic monoacid is ethanedioic acid, malonic acid, succinic acid, benzoic acid, phthalic acid, terephthalic acid (TPA), salicylic acid, breast
One kind in acid, citric acid, tartaric acid, malic acid, glyceric acid, stearic acid, glyoxalic acid, oxaloacetic acid.
7. a kind of fast preparation method of aerosil according to any one of claim 1 to 5, its feature exists
In：The dropwise addition total time of the organic nitrogen-containing silane is 3~5 hours.
8. a kind of fast preparation method of aerosil according to any one of claim 1 to 5, its feature exists
In：The organic nitrogen-containing silane is tetramethyl-disilazane, HMDS, heptamethyldisilazane, tetramethyl diethyl
At least one of alkenyl disilazane, the silazane of pregnancy basic ring three.
9. a kind of fast preparation method of aerosil according to any one of claim 1 to 5, its feature exists
In：Drying mode in the step (3) is microwave drying or microwave-baking oven combined drying；Microwave drying condition is, microwave work(
200~800W of rate, 20~600s of microwave time；The condition of oven drying is, 100~150 DEG C of drying temperature, and drying time is
T2, 0h ＜ T2≤2h。
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Cited By (5)
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| CN108358212A (en) * | 2018-05-25 | 2018-08-03 | 天津二八科技股份有限公司 | The preparation method and silica aerogel particles of silica aerogel particles |
| CN109679132A (en) * | 2019-01-02 | 2019-04-26 | 江苏泛亚微透科技股份有限公司 | A kind of microwave-assisted production method and methyl silsesquioxane aeroge of aeroge |
| CN110255567A (en) * | 2019-06-12 | 2019-09-20 | 中国人民解放军海军工程大学 | Lightweight heat-proof noise reduction SiO2Aerogel material and preparation method thereof |
| CN114408932A (en) * | 2022-02-18 | 2022-04-29 | 南京工业大学 | Method for preparing silica-based aerogel balls with controllable particle size by continuous liquid phase polymerization |
| CN114539809A (en) * | 2022-02-14 | 2022-05-27 | 连云港威晟硅材料有限公司 | Surface-modified silicon micropowder and preparation method thereof |
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| CN105271260A (en) * | 2014-06-11 | 2016-01-27 | 中国科学院苏州纳米技术与纳米仿生研究所 | Method for preparing hydrophobic silica aerogel through normal-pressure drying process |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108358212A (en) * | 2018-05-25 | 2018-08-03 | 天津二八科技股份有限公司 | The preparation method and silica aerogel particles of silica aerogel particles |
| CN109679132A (en) * | 2019-01-02 | 2019-04-26 | 江苏泛亚微透科技股份有限公司 | A kind of microwave-assisted production method and methyl silsesquioxane aeroge of aeroge |
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| CN110255567A (en) * | 2019-06-12 | 2019-09-20 | 中国人民解放军海军工程大学 | Lightweight heat-proof noise reduction SiO2Aerogel material and preparation method thereof |
| CN114539809A (en) * | 2022-02-14 | 2022-05-27 | 连云港威晟硅材料有限公司 | Surface-modified silicon micropowder and preparation method thereof |
| CN114408932A (en) * | 2022-02-18 | 2022-04-29 | 南京工业大学 | Method for preparing silica-based aerogel balls with controllable particle size by continuous liquid phase polymerization |
| CN114408932B (en) * | 2022-02-18 | 2023-09-26 | 南京工业大学 | Method for preparing silica-based aerogel balls with controllable particle size by continuous liquid phase polymerization |
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