CN107082431B - A kind of fast preparation method of aerosil - Google Patents
A kind of fast preparation method of aerosil Download PDFInfo
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- CN107082431B CN107082431B CN201710288017.5A CN201710288017A CN107082431B CN 107082431 B CN107082431 B CN 107082431B CN 201710288017 A CN201710288017 A CN 201710288017A CN 107082431 B CN107082431 B CN 107082431B
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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
- C01B33/157—After-treatment of gels
- C01B33/158—Purification; Drying; Dehydrating
- C01B33/1585—Dehydration into aerogels
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Abstract
The invention provides a kind of fast preparation method of aerosil, selecting positive esters of silicon acis is silicon source, add the organic monoacid catalytic hydrolysis reaction of low concentration, pass through the additional amount for rationally controlling nitrogenous silane again, drop rate and reaction time complete gel polycondensation reaction and one step of hydrophobically modified, no longer need to addition basic catalyst, and avoid a large amount of consumption in general rear hydrophobically modified method to displacement solvent, do not generate waste liquid, and greatly shorten manufacturing cycle, reduce process costs, it is easy to industrialized production, the aerosil product of preparation has excellent performance simultaneously.
Description
Technical field
The invention belongs to aerosil preparation technical field, more particularly, to a kind of aerosil
Fast preparation method.
Background technique
Aerosil has three-dimensional network shape skeleton structure, has low-density (0.03~0.2g/cm3), Gao Kong
Gap rate (85%~99%), low thermally conductive (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 aerospace, petroleum and petrochemical industry, metallurgy.
Aerosil most passed through sol-gel method and Supercritical Drying Technology system by Kistler early in 1931
Standby to obtain, this method also becomes most common method.Sol-gel method usually requires two step of soda acid 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 ammonium hydroxide, hydrogen-oxygen
Change sodium etc., for ethyl orthosilicate, methyl orthosilicate, waterglass and its allogenic material raw material, organic silicon source is made the silicon source used
Product purity is high, performance is stablized；Waterglass and its allogenic material raw material such as flyash, stalk, diatomite etc. are low in cost, but
Since the more needs of impurity carry out complicated pretreatment.After sol gel reaction, wet gel is done under supercritical fluid
It is dry, need high-temperature high-voltage reaction condition.Aeroge performance obtained by supercritical drying drying method is stablized, but cost is higher, it is certain to exist
Security risk, while equipment operating parameter is complicated, it is difficult to realize large-scale continuous production.In consideration of it, the preparation of aeroge
Higher cost becomes the main reason for restricting its extensive use.
Many scholars carry out the preparation of aeroge using constant pressure and dry technology generations in recent years for supercritical process.Due to solidifying
Glue has hydroxyl in hydrolytie polycondensation rear surface, needs to carry out surface alkylation and makes it have hydrophobic performance, therefore constant pressure and dry system
Standby technique generally includes several steps such as sol-gel, gel aging, solvent displacement, modified, cleaning, dry, processing step compared with
It is more, manufacturing cycle is longer, solvent displacement with modification procedure needs to consume a large amount of chemical reagent, waste liquid is more, can make to environment
At certain influence, additionally due to common constant pressure and dry mode is heated by outside, formation temperature gradient, often table
Face is dry and moisture is contained in inside, cause aeroge be mass produced in drying process take a long time, product homogeneity it is poor.
Summary of the invention
In view of this, the present invention is directed to propose one kind can realize gel polycondensation reaction and the completion of one step of hydrophobically modified
The shortening of process cycle, while can be avoided and generate waste liquid, two with excellent performance low in cost, easy to industrialized production
The preparation method of silica aerogel, to solve the above problems.
In order to achieve the above objectives, the technical solution of the invention is achieved in that
A kind of fast preparation method of aerosil, comprising the following steps:
(1) selecting positive esters of silicon acis is silicon source, and after the silicon source is dissolved with alcohol, the organic weak of low concentration is added into solution
Acid-catalyzed hydrolysis reacts to obtain solution A；
(2) under stirring conditions, organic nitrogen-containing silane is added dropwise into solution A, is stood after being added dropwise to complete, obtains gel A,
Wherein, the molar 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 being dried.
Further, the gel A first carries out aging 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 of alcohol, propyl alcohol.
Further, the concentration of the organic monoacid is 0.0001~0.01mol/L, the organic monoacid and the silicon source
Molar ratio be (0.8~1.2): 1, the catalytic hydrolysis reaction time be 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 of 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, hexamethyldisilazane, seven methyl, two silicon nitrogen
At least one of alkane, tetramethyl divinyl disilazane, hexamethyl cyclotrisilazane.
Further, the drying mode in the step (3) is microwave drying or microwave-baking oven combined drying；Microwave is dry
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 T2, 0h < T2≤2h。
Compared with the existing technology, a kind of fast preparation method of aerosil of the present invention has following excellent
Gesture:
(1) method that gel and the completion of one step of hydrophobically modified are formed using dehydrating condensation for the first time in the present invention, by reasonable
The additional amount, drop rate and reaction time for controlling nitrogenous silane are successively performed polycondensation reaction and hydrophobically modified.Using nitrogenous
Silane meets water and generates alkalinity NH3·H2O, the polycondensation reaction in catalyst system, while using the methyl in silane it is carried out hydrophobic
It is modified, it does not need to add basic catalyst again, while avoiding in general rear hydrophobically modified method and needing to consume a large amount of solvents
The step of carrying out solvent displacement, will not generate waste liquid while greatly shortening manufacturing cycle, reduce process costs, avoid
The environmental pollution that may cause；
(2) due to using the method that dehydrating condensation forms gel and one step of hydrophobically modified is completed, gel network can be more
Add quickly building to stablize, therefore can effectively shorten ageing time, in this embodiment it is not even necessary to aging process is carried out, in conventional method
Ageing time usually require 1 to 2 days, and the present invention then by ageing time control in 1h, further shorten preparation
Period, while also reducing energy consumption；
(3) use the organic monoacid of low concentration for hydrolyst in the present invention, the water of weak acid solution can satisfy silicon source
Hydrolysis requires, and does not need additionally to add moisture, simultaneously because concentration is lower, hydrolysis is mildly controllable, in the same of hydrolysis
When have certain polycondensation reaction；
(4) microwave drying or microwave-baking oven combined drying method are used in the present invention, avoid supercritical drying work
The high-temperature and high-pressure conditions of skill, process is more safe and reliable, at the same overcome surface existing for oven drying it is easily dry and it is internal not
The problem of easily drying, drying process takes long time, it is stable, excellent can to prepare performance by rationally controlling drying condition
Aerosil；Microwave drying is heating from inside to outside, with rate of drying is fast, low energy consumption, heating is easy to control, reaction
The features such as uniform, 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 existing risk；
(5) preparation method simple process of the present invention is controllable, manufacturing cycle can be foreshortened to 1 day or so, can
Realize large-scale continuous production；
(6) aerosil function admirable, the stabilization prepared using preparation method of the present invention, density are
40~60kg/m3, porosity reaches 97%, specific surface area and is up to 1050m2/ g, thermal coefficient are 0.010~0.018W/ (m ﹒ K)
Detailed description of the invention
Fig. 1 is the aerosil scanning electron microscope (SEM) photograph prepared using preparation method of the present invention；
Fig. 2 is the partial enlarged view of Fig. 1.
Specific embodiment
In addition to being defined, technical term used in following embodiment has and the invention one of ordinary skill in the art
The identical meanings being commonly understood by.Test reagent used in following embodiment is unless otherwise specified conventional biochemical reagent；
The experimental method is unless otherwise specified conventional method.
Below with reference to examples and drawings come the present invention will be described in detail create.
Embodiment 1
1L ethyl orthosilicate is added in 2L methanol solvate, after being mixed evenly, addition concentration is 0.005mol/L
Ethanedioic acid solution 120ml, stand 10h after mixing evenly；140ml tetramethyl-disilazane is delayed with the speed of 0.75ml/min
Slowly it is added dropwise in above-mentioned reaction system, total time for adding is 3h, and standing obtains after gel aging 0.5h, aging knot at 50 DEG C
Carrying 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；
Resulting aerosil product density is 57kg/m after tested3, specific surface area 920m2/ g, thermal coefficient
0.016W/ (m ﹒ K).
Embodiment 2
1L ethyl orthosilicate is added in 2.5L alcohol solvent, after being mixed evenly, addition concentration is 0.002mol/
The benzoic acid solution 220ml of L, stands 12h after mixing evenly；270ml hexamethyldisilazane is slow with the speed of 1ml/min
It is added dropwise in above-mentioned reaction system, total time for adding is 4.5h, and standing obtains after gel that aging 1h, aging terminate at 50 DEG C
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
Obtaining product is aerosil；
Resulting aerosil product density is 45kg/m after tested3, specific surface area 1050m2/ g, thermal coefficient
0.013W/ (m ﹒ K).
Embodiment 3
1L ethyl orthosilicate is added in 2L alcohol solvent, after being mixed evenly, addition concentration is 0.001mol/L
Glacial acetic acid solution 310ml, stand 3h after mixing evenly；By heptamethyldisilazane and hexamethyl cyclotrisilazane with 1:3's
Molar ratio is mixed into 200ml mixed liquor, which is slowly dropped into reaction system with the speed of 1ml/min, when overall reaction
Between be 3.3 hours, standing obtain gel after carry out oven drying after microwave drying 200s again under 200W power, oven drying
Condition is dry 2h at 105 DEG C, and products therefrom is aerosil；
Resulting aerosil product density is 60kg/m after tested3, specific surface area 865m2/ g, thermal coefficient
0.018W/ (m ﹒ K).
Preparation method of the present invention by rationally control the additional amount, drop rate and reaction time of nitrogenous silane come
It realizes that gel polycondensation reaction and one step of hydrophobically modified are completed, illustrates reaction process by taking hexamethyldisilazane (HMDZ) as an example:
HMDZ hydrolysis: (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 and discharges ammonia, and ammonia formation ammonium hydroxide soluble in water has catalysis to the silicon source hydrolyzed
The effect of polycondensation reaction, 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 reaction by rationally control nitrogenous silane additional amount and be added speed, can to avoid by
Enter reaction system in the ammonium hydroxide of excessive concentration and form precipitating or other by-products, controlling drop rate and reaction time makes 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 and one step of hydrophobically modified, gel network
It is basicly stable, shorten even eliminating aging process step, while carrying out solvent displacement without consuming a large amount of solvents, greatly
The silica airsetting for shortening manufacturing cycle, reducing process costs, not generating waste liquid, is easy to industrialized production, and prepare
Glue properties of product are excellent；
As shown in figures 1 and 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 reaches 97%, specific surface area and is up to 1050m2/
G, thermal coefficient is 0.010~0.018W/ (m ﹒ K), has good thermal and insulating performance.
In order to further illustrate the present invention the advantages of the preparation method, below as normal pressure well known in the prior art
Seasoning prepares aerosil, and is compared according to the method described in the present invention.
Comparative example 1
1L ethyl orthosilicate is added in 2.5L alcohol solvent, after being mixed evenly, it is 0.01mol/L's that concentration, which is added,
Hydrochloric acid solution 200ml, stands 2h after mixing evenly；0.1mol/L ammonium hydroxide 60ml is added and forms it into gel；At 60 DEG C after gel
For 24 hours, wherein aging is divided into two steps for aging in water-bath, and the first step is aging 12h in the mixed liquor of 1:4 in water and ethyl alcohol volume ratio,
Second step, the aging 12h in the mixed liquor that ethyl orthosilicate and ethyl alcohol volume ratio are 1:4；Respectively in isopropanol after aging
Mixed liquor that mixed liquor, isopropanol and the n-hexane volume ratio that solution, isopropanol and n-hexane volume ratio are 3:1 are 1:1, isopropyl
12h is replaced respectively in the mixed liquor that pure and mild n-hexane volume ratio is 1:3；Wet gel is changed using hexamethyldisilazane
Property；It is cleaned 3 times after 12h with n-hexane, each 12h；Wet gel dry 15h at 150 DEG C of baking oven, products therefrom is titanium dioxide
Silica aerogel；
Finally obtained aerogel products density 52kg/m after tested3, specific surface area 936m2/ g, thermal coefficient 0.015W/
(m ﹒ K)
Comparative example 2
1L ethyl orthosilicate is added in 2.5L alcohol solvent, after being mixed evenly, it is 0.01mol/L's that concentration, which is added,
Hydrochloric acid solution 200ml, stands 2h after mixing evenly；0.1mol/L ammonium hydroxide 60ml is added and forms it into gel；At 60 DEG C after gel
For 24 hours, wherein aging is divided into two steps for aging in water-bath, and the first step is aging 12h in the mixed liquor of 1:4 in water and ethyl alcohol volume ratio,
Second step, the aging 12h in the mixed liquor that the volume ratio of ethyl orthosilicate and ethyl alcohol is 1:4；It is in volume ratio after aging
Ethyl alcohol: hexamethyldisilazane: replacing for 24 hours in n-hexane=1:1:8 modification liquid, cleans 3 times with n-hexane after the completion, every time
12h；It is aerosil that wet gel, which is separately dried 4h, 8h, 2h products therefrom at 50 DEG C, 150 DEG C, 200 DEG C of baking oven,；
Through detecting finally obtained aerogel products density 89kg/m3, specific surface area 812m2/ g, thermal coefficient 0.021W/
(m ﹒ K)
By comparative example 1,2 it is found that atmosphere pressure desiccation prepares silica airsetting in the prior art compared with Examples 1 to 3
Glue, long preparation period, only one step of aging process just needs at least one day time, complex technical process, needs to consume big
It measures solvent and carries out solvent displacement, not only consume the time, improve production cost and also create a large amount of waste liquid, and embodiment 1
~3 other than with the obvious advantage in preparation method, additionally it is possible to guarantee that the aerosil prepared has good product
Performance, the performance for the aerosil that even better than certain known atmosphere pressure desiccations are prepared.
The foregoing is merely the preferred embodiments of the invention, are not intended to limit the invention creation, all at this
Within the spirit and principle of innovation and creation, any modification, equivalent replacement, improvement and so on should be included in the invention
Protection scope within.
Claims (8)
1. a kind of fast preparation method of aerosil, it is characterised in that: the following steps are included:
(1) selecting positive esters of silicon acis is silicon source, and after the silicon source is dissolved with alcohol, the organic monoacid that low concentration is added into solution is urged
Change hydrolysis and obtains solution A；
(2) under stirring conditions, organic nitrogen-containing silane is added dropwise into solution A, is stood after being added dropwise to complete, obtains gel A,
In, the molar 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；The organic nitrogen-containing silane is tetramethyl-disilazane, hexamethyldisilazane, seven methyl, two silicon nitrogen
At least one of alkane, tetramethyl divinyl disilazane, hexamethyl cyclotrisilazane；
(3) target product aerosil is obtained after gel A being 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 aging process before being dried, and aging temperature is 20~60 DEG C, ageing time 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 of methanol, ethyl alcohol, propyl alcohol.
4. a kind of fast preparation method of aerosil according to claim 1, it is characterised in that: described organic
The concentration of weak acid is 0.0001~0.01mol/L, and the molar ratio of the organic monoacid and the silicon source is (0.8~1.2): 1, institute
Stating the catalytic hydrolysis reaction time is 0.5~12h.
5. a kind of fast preparation method of aerosil according to claim 4, it is characterised in that: described organic
The concentration of weak acid is 0.0005~0.005mol/L, and the catalytic hydrolysis reaction time is 8~12h.
6. according to claim 1 to a kind of 5 described in any item fast preparation methods of aerosil, feature exists
In: the organic monoacid is ethanedioic acid, malonic acid, succinic acid, benzoic acid, phthalic acid, terephthalic acid (TPA), salicylic acid, cream
One of acid, citric acid, tartaric acid, malic acid, glyceric acid, stearic acid, glyoxalic acid, oxaloacetic acid.
7. according to claim 1 to a kind of 5 described in any item fast preparation methods of aerosil, feature exists
In: the dropwise addition total time of the organic nitrogen-containing silane is 3~5 hours.
8. according to claim 1 to a kind of 5 described in any item fast preparation methods of aerosil, feature exists
In: the drying mode in the step (3) is microwave drying or microwave-baking oven combined drying；Microwave drying condition is microwave function
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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| 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 |
| CN109679132B (en) * | 2019-01-02 | 2022-01-25 | 江苏泛亚微透科技股份有限公司 | Microwave-assisted production method of aerogel and methyl silsesquioxane aerogel |
| 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 |
| 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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| CN1724353A (en) * | 2005-07-15 | 2006-01-25 | 清华大学 | Process for preparing hydrophobic silicon dioxide aerogel using rice husk ash as raw material |
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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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| KR20120070948A (en) * | 2010-12-22 | 2012-07-02 | 주식회사 화인텍 | Manufacturing method of hydropobic silica aerogel powder with insulating performance |
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| CN1724353A (en) * | 2005-07-15 | 2006-01-25 | 清华大学 | Process for preparing hydrophobic silicon dioxide aerogel using rice husk ash as raw material |
| CN102951650A (en) * | 2012-08-31 | 2013-03-06 | 卢斌 | Ambient pressure drying method for rapidly preparing SiO2 aerogel |
| CN103435055A (en) * | 2013-06-29 | 2013-12-11 | 浙江工业大学 | Method for preparing low density silica aerogel under normal pressure |
| 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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