CN107055556B - A kind of hydrophilic silicon dioxide aerogel microball and preparation method thereof - Google Patents
A kind of hydrophilic silicon dioxide aerogel microball and preparation method thereof Download PDFInfo
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- CN107055556B CN107055556B CN201710170065.4A CN201710170065A CN107055556B CN 107055556 B CN107055556 B CN 107055556B CN 201710170065 A CN201710170065 A CN 201710170065A CN 107055556 B CN107055556 B CN 107055556B
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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 discloses a kind of preparation methods of hydrophilic silicon dioxide aerogel microball, and specifically, which includes 1) being uniformly dispersed using the hydrophilic compounds solubilizer of tetraalkoxysilane, hydroxyl, and performed polymer is obtained after acid adding；2) it is scattered in self assembly in water phase；3) it plus after alkali washs；4) dry.The preparation method is environmental-friendly, easy to operate, low in cost；Silica shell of the hydrophilic silicon dioxide aerogel microball that this method obtains with smaller hole and the silicon dioxide skeleton with larger pore structure being wrapped in the silica shell.The invention also discloses a kind of hydrophilic silicon dioxide aerogel microball, which has preferable dispersion performance, applied to high with the adhesive force of matrix in coating.
Description
Technical field
The present invention relates to material technology technical fields, and in particular to a kind of hydrophilic silicon dioxide aerogel microball and its preparation
Method.
Background technique
Aeroge is to be currently known the minimum material of thermal conductivity, in heat-barrier material field application potential with higher.Gas
Gel belongs to extremely-low density (0.003-0.6g/cm3), superhigh specific surface area (400-1500m2/ g), superelevation porosity (80-
99.8%) with ultralow thermal conductivity (0.013-0.038W/mK) material, usually pass through overcritical, subcritical and constant pressure and dry method
Solvent is extracted from the nano-pore of gel rubber material and is made.The bore hole size of aeroge is generally at 50 nanometers hereinafter, be less than room temperature
The mean free path (70 nanometers) of air molecule under normal pressure, the collision probability between air molecule is very low, is difficult to realize heat transfer,
So aerogel material is the minimum super insulating material of thermal conductivity.Meanwhile aeroge in catalyst carrier, organic solvent or has
The fields such as machine gas absorption, chromatographic isolation, cosmetic additive agent are also widely used.In recent years, with various complex techniques
Fast development, aerogel composite starts even to play the part of more and more important role in terms of the people's livelihood in national defence, industry.
Aerosil first by doctor Kistler of Stanford University 1931 by sol-gel method and
(Kistler, S.S.Nature 1931,127,741.) is made in Supercritical Drying Technology.Aerosil is ground in recent years
Study carefully the company or university for being also concentrated mainly on the states such as Germany, the U.S., France, Sweden, Japan.But to aerosil
Research is still in infancy mostly, cannot also realize large-scale application.This is primarily due to aerosil product
There are technological difficulties in preparation.The general thinking for preparing aerosil is by silica precursor (organosilicon
Alkoxide, waterglass or silicon tetrachloride) in alcoholic solvent hydrolysis obtain the alcosol of silicon, then by adjust pH to neutrality, obtain
Wet gel, that is, so-called sol-gel method.Second step and a most important step, are exactly the selection of dry technology, are led to
Often there are supercritical drying and constant pressure and dry.The basic principle of supercritical drying is to adjust the temperature in container in high-pressure bottle
It is set to be more than the critical point of dried medium with pressure, existing air liquid interface will disappear before this in this way, and surface tension is not deposited again
Dried medium will replace the alcoholic solvent in wet gel.So it is possible to prevente effectively from airsetting during supercritical drying
The contraction and collapsing of glue skeleton in the drying process, the performance of the aeroge because obtained from are more excellent.But supercritical drying
Device systems it is complicated, it is expensive, it is often necessary to work at high temperature under high pressure, risk is high, while production cost is also difficult to
It reduces.Such as the CO disclosed in patent CN103706342A2Supercritical drying pressure is 8-12MPa, in patent
The temperature of ethanol supercritical drying disclosed in CN101973558A is 250-275 DEG C, pressure 9-13MPa.It is domestic in recent years
Outer researcher is dedicated to constant pressure and dry and prepares aerogel material, keeps reaction condition mild, reduces the risk and cost of production,
Realize the industrialized production of aeroge.But it is constrained to the preparation process of sol-gel method, constant pressure and dry needs repeatedly by duct
Interior solvent is replaced as the solvent (such as n-hexane, hexamethylene) of low surface tension, it is also necessary to carry out inner surfaces of pores hydrophobic
Change processing (generally uses hydrophobic modified dose of trim,ethylchlorosilane etc.), could reduce the capillary force in duct in this way, guarantees
In the drying process, aeroge skeleton does not shrink or collapses as far as possible.Such as patent CN101503195, CN102020285A and
CN103043673A individually discloses the process that constant pressure and dry prepares aeroge, but the production cycle is long (a couple of days to several weeks), molten
Agent usage amount is big, operates tedious, large-scale production and application difficult to realize.
The later period dry technological problems faced are removed, the aeroge form of preparation itself, which also will limit it, further to be made
With.The aerosil produced at present is largely bulk, and matter is crisp frangible, difficult forming, if necessary to realize aeroge
With the high efficiency composition of other materials, need that Monolithic aerogel is broken to irregular shape powder using crushing or milling apparatus,
On the one hand the process crushed may destroy the porous structure of aeroge, another aspect irregular shape silicon dioxide aerogel powder
In practical applications, poor fluidity, filling are uneven, while hole is easy to be filled by other materials, seriously affects it heat-insulated
The application of aspect.Thus, there is researcher to start exploration and prepares micron-size spherical aerosil.Such as United States Patent (USP)
US2006/0084707A1 discloses a kind of method, i.e., silicon dioxide gel is sprayed by atomising device high speed and be furnished with 400-
In the oily phase of 3000 revs/min of stirrings, after ammoniating hydrogel, except simultaneously washes clean of deoiling mutually.Domestic Tongji University and Shanghai
The units such as silicate research institute are made that more work in this respect.Such as patent CN103964449A, CN104003406A
A kind of method for preparing silica aerosil microballoon is individually disclosed with CN1715182A, basic ideas are by surface-active
The alcosol of silica is dispersed in non-polar organic-dielectric by the stabilization of agent and cosurfactant, is obtained non-equal
Then phase emulsion rapidly joins ammonium hydroxide gel using the lotion as template, washes off remaining organic solvent after solid-liquor separation, with super
Critical or extremal stability obtains silica aerosil microballoon.Because being related to exhibiting high surface activating agent and nonpolarity being organic molten
The use of agent, later-period purification process is complicated, and industrialization production is still restricted.
Summary of the invention
For overcome the deficiencies in the prior art, an object of the present invention is to provide for a kind of parent based on aqueous phase reactions
Water silica aerosil microballoon preparation method.
In order to realize first purpose, the invention adopts the following technical scheme:
A kind of preparation method of hydrophilic silicon dioxide aerogel microball, comprising the following steps:
1) it synthesizes siloxanes performed polymer: adding the first solvent with 100- the hydrophilic compounds of tetraalkoxysilane, hydroxyl
1000 revs/min of speed is stirred to transparent, addition dilute acid soln, and after fully reacting, removing solvent obtains siloxanes pre-polymerization
Body；The C of the dilute acid solnH+=1-6mol/L；The weight ratio of the diluted acid and tetraalkoxysilane is 0.01-0.2:1；
First solvent is alcohol, ether or ketone；The hydrophilic compounds of the hydroxyl are polyalcohols, monosaccharide or polysaccharide；
2) self assembly: the siloxanes performed polymer of step 1) is added to the water carry out self assembly, obtains white " milky " liquid；
3) it washes: alkali being added into the emulsion of step 2) and adjusts pH to 9-11, stirring, standing obtains white precipitate, mistake
Water is filtered out, and is washed with water until pH is 6-8；
4) dry: by the white precipitate of step 3) in 40-90 DEG C of constant pressure and dry to get silica aerosil microballoon.
Preferably, the alkoxy of the tetraalkoxysilane is in methoxyl group, ethyoxyl and isopropoxy in step 1)
One or more.
Preferably, first solvent is methanol, ethyl alcohol, isopropanol, butanol, propylene glycol monomethyl ether, acetone in step 1)
Or butanone.
Preferably, the polyalcohols molecular weight is 200-10000 in step 1), the polyalcohols is polyethylene glycol or poly- second
Enol.
Preferably, first solvent is ethyl alcohol in step 1), the hydrophilic compounds of the hydroxyl are PEG1000,
Tetraalkoxysilane, ethyl alcohol, PEG1000 weight ratio be 100:(25-100): (1-10).
Preferably, first solvent is ethyl alcohol in step 1), the hydrophilic compounds of the hydroxyl are PVA500,
Tetraalkoxysilane, ethyl alcohol, PVA500 weight ratio be 100:(25-100): (1-10).
Preferably, removing the method for solvent in step 1) as vacuum distillation or constant-pressure and high-temperature distillation.
Preferably, the additional amount of water is 1-100 times of tetraalkoxysilane weight in step 2).
Preferably, the alkali is sodium hydroxide, potassium hydroxide or ammonium hydroxide in step 3).
Second object of the present invention is to provide a kind of hydrophilic silicon oxides aeroge prepared using the above method
Microballoon.
Compared with prior art, the beneficial effects of the present invention are:
1) preparation method provided by the invention is whole water phase reaction, using synthesis siloxanes performed polymer in water from group
Dress behavior, without adding other surfaces activating agent or organic solvent, it is fast to additionally incorporate alkali gelation rate, without ageing, at the later period
Reason is simple, without carrying out solvent displacement with low surface tension solvent, does not also need to carry out hydrophobically modified to aeroge duct, directly
Constant pressure and dry will not make porous structure occur to destroy or collapse.Therefore with short production cycle, it can be obtained in 24 hours dry
Silica aerosil microballoon greatly reduces production cost, makes it possible to be mass produced and apply；
2) the hydrophilic silicon dioxide aerogel microball that this method obtains has obviously double-layer structure, i.e., external relatively to cause
The continuous skeleton of close shell and internal high porosity, shape is spherical shape, and Microsphere Size is controllable in micron range, can basis
Different application adjusts size.Mechanical strength is high, and bearing capacity is strong, can be answered with other materials without crushing, grinding
It closes without destroying its porous structure, will not influence its thermal and insulating performance.
3) aerogel microball that this method obtains, surface hydrophilic can be well dispersed in aqueous matrix, such as aqueous
In coating, there is stronger interaction with matrix, will not reunite after dry, lose powder.In addition, in hydrophobic matrices, because
There is hydroxyl abundant on aeroge surface, (can will not influence aeroge inner hydrophilic to the modification of its surface with hydrophobic modifier
Property), so that it is had better compatibility with hydrophobic substrates.
Detailed description of the invention
Fig. 1 is the structural schematic diagram for the hydrophilic silicon dioxide aerogel microball that embodiment 1 obtains.
The scanning electron microscope (SEM) photograph of hydrophilic silicon dioxide aerogel microball obtained by Fig. 2 embodiment of the present invention 1；
The infrared absorption spectra of hydrophilic silicon dioxide aerogel microball obtained by Fig. 3 embodiment of the present invention 1；
The dispersion liquid of silica aerosil microballoon obtained by Fig. 4 embodiment of the present invention 1 in water；
The transmission electron microscope picture of hydrophilic silicon dioxide aerogel microball obtained by Fig. 5 embodiment of the present invention 2；
The stacking volume of 1 gram of hydrophilic silicon dioxide aerogel microball obtained by Fig. 6 embodiment of the present invention 3.
Specific embodiment
In the following, being described further in conjunction with attached drawing and specific embodiment to the present invention:
In following specific embodiments, such as non-specified otherwise, used reagent can pass through commercially available mode or routine test
Means obtain.
The present invention provides a kind of preparation method of hydrophilic silicon dioxide aerogel microball, comprising the following steps:
1) it synthesizes siloxanes performed polymer: adding the first solvent with 100- the hydrophilic compounds of tetraalkoxysilane, hydroxyl
1000 revs/min of speed is stirred to transparent, addition dilute acid soln, and after fully reacting, removing solvent obtains siloxanes pre-polymerization
Body；The concentration C of the dilute acid solnH+=1-6mol/L；The weight ratio of the diluted acid and tetraalkoxysilane is 0.01-0.2:1；
First solvent is alcohol, ether or ketone；The hydrophilic compounds of the hydroxyl are polyalcohols, monosaccharide or polysaccharide；
In this step, the alkoxy of tetraalkoxysilane is one or both of methoxyl group, ethyoxyl and isopropoxy
More than.The hydrophilic compounds of hydroxyl can be the polyethylene glycol that average molecular weight is 200-10000, average molecular weight 200-
10000 polyvinyl alcohol, monosaccharide and polysaccharide etc.；Tetraalkoxysilane/the ethyl alcohol/hydroxyl hydrophilic compounds mass ratio is
100/25-100/1-10；The stirring is one of magnetic agitation or mechanical stirring, and mixing speed is 100-1000 revs/min
Clock；Acid is one of hydrochloric acid, nitric acid, sulfuric acid, acetic acid or oxalic acid；The mode for removing solvent is vacuum distillation, constant-pressure and high-temperature steaming
It evaporates, one of rotary evaporation and thin film evaporation, is preferably evaporated under reduced pressure；
2) self assembly: the siloxanes performed polymer of step 1) is added to the water carry out self assembly, obtains white " milky " liquid；Water is excellent
It is selected as deionized water；
3) it washes: alkali being added into the emulsion of step 2) and adjusts pH to 9-11, stirring, standing obtains white precipitate, mistake
Water is filtered out, and is washed with water until pH is 6-8；Alkali is preferably in sodium hydroxide, potassium hydroxide or ammonium hydroxide one kind；
4) dry: by the white precipitate of step 3) in 40-90 DEG C of constant pressure and dry to get silica aerosil microballoon.
The present invention provides a kind of preparation method of hydrophilic silicon dioxide aerogel microball, the hydrophilic titanium dioxide that this method obtains
The structural schematic diagram of silica aerogel microballoon is as shown in Figure 1 comprising has the silica shell of smaller hole and is wrapped in described
The silicon dioxide skeleton with larger pore structure in silica shell.The aerogel microball is having a size of 0.1-100 microns, institute
State silica shell with a thickness of 5-50 nanometers, being distributed in pore size on shell is 2-10 nanometers, inner silica silicon
The pore size of skeleton is 2-100 nanometers.The bulk density of silica aerosil microballoon is 50-200kg/m3, and porosity is
80-99%.
Embodiment 1
A kind of preparation method of hydrophilic silicon dioxide aerogel microball, comprising the following steps:
(1) 278.32 grams of ethyl orthosilicates, 150 grams of ethyl alcohol, 10 grams of polyethylene glycol (average molecular weight 1000) are mixed equal
It is even to transparent；15 grams of concentrated hydrochloric acids (mass concentration 37%) and 20 grams of water are uniformly mixed, are then slowly dropped into, wait be added dropwise to complete
Afterwards, 60 degree are warming up to, continues to be stirred to react 2 hours, decompression flash distillation fall the ethyl alcohol in system, obtain with certain viscosity,
Flowable, transparent siloxanes performed polymer；
(2) by 50 grams of above-mentioned siloxanes performed polymers under high velocity agitation 100 grams of distilled water of (500 revs/min) additions, to
It is added dropwise to complete, adjusts pH to 10 with ammonium hydroxide, continue to be stirred to react 2 hours, obtain white emulsion；
(3) above-mentioned emulsion is stood 1 hour and obtains white precipitate, water phase is removed by filtration, and rinsed twice and arrived with water
PH is put into 80 DEG C of baking oven heating 5 hours to get dry silica aerosil microballoon is arrived close to neutrality, by obtained solid.
Resulting aerogel microball scanning electron microscope (SEM) photograph as shown in Figure 2, infrared absorption spectra as shown in figure 3, its size in 1-2
Microns, spherical complete, even size distribution do not find obviously to rupture and collapse after dry.Resulting aerogel microball
Dispersion liquid in ground water is as shown in Figure 4, it is seen that it is uniformly dispersed, and quality is fine and smooth.
Embodiment 2
Embodiment 2 difference from example 1 is that, tetraethyl orthosilicate replacement in step (1) is positive silicic acid four
Amount is reduced to 203.5 grams by methyl esters, and polyethylene glycol (average molecular weight 1000) is replaced with polyvinyl alcohol (average molecular weight
500) amount, is reduced to 5 grams, reaction temperature is increased to 80 DEG C.
Finally obtain the transmission electron microscope picture of aerosil as shown in figure 5, its size range be 5-10 micron, inside
Porosity is high, after dry, does not find porous structure breakage in high vacuum conditions.
Embodiment 3
Embodiment 3 difference from example 1 is that, the amount of concentrated hydrochloric acid in step (1) is increased to 20 grams, the amount of water
Increase to 27 grams, the amount of siloxanes performed polymer in step (2) is kept to 10 grams, the time being stirred to react is increased to 5 hours.
The stacking volume of aerosil its 1g is finally obtained as shown in fig. 6, its size range is at 20-50 microns,
Density is 0.05g/cm3, specific surface area 800m2/g。
Embodiment 4
Embodiment 4 difference from example 1 is that, tetraethyl orthosilicate replacement in step (1) is positive silicic acid four
Methyl esters, is reduced to 203.5 grams for amount, ethyl alcohol is replaced with methanol, and amount is reduced to 105 grams, by polyethylene glycol (average molecular weight
1000) glucose (molecular formula: C is replaced with6H12O6), amount is increased to 15.0 grams, concentrated hydrochloric acid is replaced with concentrated nitric acid, and (quality is dense
Degree is 65%), amount to be reduced to 8.5 grams.
Finally obtained aerosil size is at 10-20 microns, density 0.15g/cm3, specific surface area is
650m2/g。
It will be apparent to those skilled in the art that can make various other according to the above description of the technical scheme and ideas
Corresponding change and deformation, and all these changes and deformation all should belong to the protection scope of the claims in the present invention
Within.
Claims (10)
1. a kind of preparation method of hydrophilic silicon dioxide aerogel microball, which comprises the following steps:
1) it synthesizes siloxanes performed polymer: adding the first solvent with 100-1000 the hydrophilic compounds of tetraalkoxysilane, hydroxyl
Rev/min speed stir to transparent, dilute acid soln is added, after fully reacting, removes solvent, obtains siloxanes performed polymer；Institute
State hydrionic concentration in dilute acid soln=1-6mol/L；The weight ratio of the diluted acid and tetraalkoxysilane is 0.01-
0.2:1；
First solvent is alcohol, ether or ketone；The hydrophilic compounds of the hydroxyl are polyalcohols, monosaccharide or polysaccharide；
2) self assembly: the siloxanes performed polymer of step 1) is added to the water carry out self assembly, obtains white " milky " liquid；
3) it washes: alkali being added into the emulsion of step 2 and adjusts pH to 9-11, stirring, standing obtains white precipitate, crosses and filters out
Water is removed, and is washed with water until pH is 6-8；
4) dry: by the white precipitate of step 3) in 40-90 DEG C of constant pressure and dry to get silica aerosil microballoon.
2. the method according to claim 1, wherein in step 1), the alkoxy of the tetraalkoxysilane is
One or more of methoxyl group, ethyoxyl and isopropoxy.
3. the method according to claim 1, wherein in step 1), first solvent is methanol, ethyl alcohol, different
Propyl alcohol, butanol, propylene glycol monomethyl ether, acetone or butanone.
4. the polyalcohols molecular weight is 200-10000 the method according to claim 1, wherein in step 1),
The polyalcohols is polyethylene glycol or polyvinyl alcohol.
5. the method according to claim 1, wherein first solvent is ethyl alcohol, described to contain hydroxyl in step 1)
The hydrophilic compounds of base be PEG1000, tetraalkoxysilane, ethyl alcohol, PEG1000 weight ratio be 100:(25-100): (1-
10).
6. the method according to claim 1, wherein first solvent is ethyl alcohol, described to contain hydroxyl in step 1)
The hydrophilic compounds of base be PVA500, tetraalkoxysilane, ethyl alcohol, PVA500 weight ratio be 100:(25-100): (1-10).
7. the method according to claim 1, wherein removing the method for solvent in step 1) as vacuum distillation.
8. the method according to claim 1, wherein the additional amount of water is tetraalkoxysilane weight in step 2
1-100 times of amount.
9. the method according to claim 1, wherein in step 3), the alkali be sodium hydroxide, potassium hydroxide or
Ammonium hydroxide.
10. a kind of hydrophilic silicon oxides aerogel microball using the described in any item method preparations of claim 1-9.
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| CN110157315A (en) * | 2019-05-23 | 2019-08-23 | 南京珈时新材料科技有限公司 | A kind of insulating moulding coating and its application containing hollow silica microsphere |
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| US11673810B2 (en) * | 2017-10-04 | 2023-06-13 | Resonac Corporation | Aerogel and method for producing same |
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| CN102719129B (en) * | 2012-07-05 | 2013-08-21 | 河南工业大学 | Preparation method of silica aerogel aqueous heat-insulating coating |
| CN103342367B (en) * | 2013-07-09 | 2015-09-02 | 南京工业大学 | A kind of hydrophilic SiO 2the preparation method of aerogel |
| CN105347351B (en) * | 2015-12-04 | 2018-01-12 | 武汉理工大学 | A kind of emulsion method prepares TiO2/SiO2The method of aerogel microball |
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| CN110157315B (en) * | 2019-05-23 | 2021-06-04 | 南京特粒材料科技有限公司 | Heat insulation coating containing hollow silica microspheres and application thereof |
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