CN107055556A - 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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- CN107055556A CN107055556A CN201710170065.4A CN201710170065A CN107055556A CN 107055556 A CN107055556 A CN 107055556A CN 201710170065 A CN201710170065 A CN 201710170065A CN 107055556 A CN107055556 A CN 107055556A
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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
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- C01B33/1585—Dehydration into aerogels
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Abstract
The invention discloses a kind of preparation method of hydrophilic silicon dioxide aerogel microball, specifically, the preparation method 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 aqueous phase；3) plus after alkali wash；4) dry.The preparation method is environment-friendly, simple to operate, with low cost；The hydrophilic silicon dioxide aerogel microball that this method is obtained has the silica shell of 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, the hydrophilic silicon dioxide aerogel microball has preferable dispersive property, high applied to the adhesive force in coating with matrix.
Description
Technical field
The present invention relates to material technology technical field, and in particular to a kind of hydrophilic silicon dioxide aerogel microball and its preparation
Method.
Background technology
Aeroge is to be currently known the minimum material of thermal conductivity, has higher application potential in heat-barrier material field.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, overcritical, subcritical and constant pressure and dry method is generally passed through
Solvent is extracted from the nano-pore of gel rubber material and is made.The bore hole size of aeroge is general below 50 nanometers, less than normal temperature
Collision probability under normal pressure between the mean free path (70 nanometers) of air molecule, 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 is 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 Stanford University doctor Kistler 1931 by sol-gel process 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 cannot also realize large-scale application mostly also in the starting stage.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) alcosol of silicon is obtained in alcoholic solvent reclaimed water solution, then by adjusting pH to neutrality, obtain
Wet gel, that is, so-called sol-gel process.Second step, is also a most important step, is exactly the selection of dry technology, is led to
Often there are supercritical drying and constant pressure and dry.The general principle of supercritical drying is the temperature in regulation container in high-pressure bottle
Make the critical point that it exceedes dried medium with pressure, the air liquid interface so existed before this will be disappeared, 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 in the drying process of glue skeleton and cave in, the performance comparision of aeroge because obtained from is excellent.But supercritical drying
Device systems it is complicated, it is expensive, it is often necessary to work at high temperature under high pressure, it is dangerous high, while production cost is also difficult to
Reduction.CO for example 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, and pressure is 9-13MPa.Recent year
Outer researcher is directed to constant pressure and dry and prepares aerogel material, makes reaction condition gentle, reduces the risk and cost of production,
Realize the industrialized production of aeroge.But the preparation technology of sol-gel process is constrained to, constant pressure and dry is needed duct repeatedly
Interior solvent is replaced as the solvent (such as n-hexane, hexamethylene) of low surface tension, in addition it is also necessary to carry out inner surfaces of pores hydrophobic
Change processing (general to use hydrophobic modified dose of trim,ethylchlorosilane etc.), could so reduce the capillary force in duct, it is ensured that
In the drying process, aeroge skeleton does not shrink or caved in as far as possible.Such as patent CN101503195, CN102020285A and
CN103043673A individually discloses the process that constant pressure and dry prepares aeroge, but production cycle length (a couple of days to several weeks), molten
Agent usage amount is big, operates miscellaneous, large-scale production and application difficult to realize.
The technological problemses that later stage drying faces are removed, the aeroge form of preparation can also limit it in itself further to be made
With.The aerosil produced at present is largely bulk, and matter is crisp frangible, and difficult forming realizes aeroge if desired
With the high efficiency composition of other materials, it is necessary to using crushing or Monolithic aerogel is broken to irregular shape powder by milling apparatus,
On the one hand the process crushed may destroy the loose structure of aeroge, another aspect irregular shape silicon dioxide aerogel powder
In actual applications, poor fluidity, filling are uneven, while hole is easily filled by other materials, have a strong impact on it heat-insulated
The application of aspect.Thus, there is researcher to start exploration and prepare micron-size spherical aerosil.Such as United States Patent (USP)
US2006/0084707A1 discloses a kind of method, i.e., silicon dioxide gel is sprayed at a high speed by atomising device and be furnished with 400-
In the oil phase of 3000 revs/min of stirrings, after ammonification hydrogel, oil phase and washes clean are removed.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
Agent and the stabilization of cosurfactant, the alcosol of silica is dispersed in non-polar organic-dielectric, obtains non-equal
Phase emulsion, then rapidly joins the organic solvent for washing residual after ammoniacal liquor gel, solid-liquor separation off by template of the emulsion, with super
Critical or extremal stability obtains silica aerosil microballoon.Because being related to exhibiting high surface activating agent and nonpolar organic molten
The use of agent, later-period purification process is complicated, and industrialization production is still restricted.
The content of the invention
In order to 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 present invention uses following technical scheme：
A kind of preparation method of hydrophilic silicon dioxide aerogel microball, comprises the following steps：
1) siloxanes performed polymer is synthesized：The hydrophilic compounds of tetraalkoxysilane, hydroxyl are added into the first solvent with 100-
1000 revs/min of speed is stirred to transparent, adds dilute acid soln, after reaction completely, is removed solvent, is obtained 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, monose or polysaccharide；
2) self assembly：By step 1) siloxanes performed polymer be added to the water carry out self assembly, obtain white " milky " liquid；
3) wash：To step 2) emulsion in add alkali regulation pH to 9-11, stirring, standing obtain white precipitate, mistake
Water is filtered out, and is washed with water until pH is 6-8；
4) dry：By step 3) white precipitate in 40-90 DEG C of constant pressure and dry, produce silica aerosil microballoon.
Preferably, step 1) in, the alkoxy of the tetraalkoxysilane is in methoxyl group, ethyoxyl and isopropoxy
One or more.
Preferably, step 1) in, first solvent is methanol, ethanol, isopropanol, butanol, propylene glycol monomethyl ether, acetone
Or butanone.
Preferably, step 1) in, the polyalcohols molecular weight is 200-10000, and the polyalcohols is polyethylene glycol or poly- second
Enol.
Preferably, step 1) in, first solvent is ethanol, and the hydrophilic compounds of the hydroxyl are PEG1000,
Tetraalkoxysilane, ethanol, PEG1000 weight ratio are 100:(25-100)：(1-10).
Preferably, step 1) in, first solvent is ethanol, and the hydrophilic compounds of the hydroxyl are PVA500,
Tetraalkoxysilane, ethanol, PVA500 weight ratio are 100:(25-100)：(1-10).
Preferably, step 1) in, it is that vacuum distillation or constant-pressure and high-temperature distill to remove the method for solvent.
Preferably, step 2) in, the addition of water is 1-100 times of tetraalkoxysilane weight.
Preferably, step 3) in, the alkali is sodium hydroxide, potassium hydroxide or ammoniacal liquor.
Second object of the present invention is to provide hydrophilic silicon oxides aeroge prepared by a kind of utilization above method
Microballoon.
Compared with prior art, the beneficial effects of the present invention are：
1) preparation method that provides of the present invention is whole water phase reaction, using the siloxanes performed polymer of synthesis in water from group
Dress behavior, without adding other surfaces activating agent or organic solvent, it is possible to additionally incorporate alkali gelation rate soon, without ageing, at the later stage
Reason is simple, without carrying out solvent displacement with low surface tension solvent, it is not required that carry out hydrophobically modified to aeroge duct, directly
Constant pressure and dry, will not make loose structure occur destruction or cave in.Therefore it is with short production cycle, drying can be obtained in 24 hours
Silica aerosil microballoon, greatly reduces production cost, make it possible large-scale production and application；
2) the hydrophilic silicon dioxide aerogel microball that this method is obtained has obviously double-layer structure, i.e., outside relatively to cause
The continuous skeleton of close shell and internal high porosity, is shaped as spherical, and Microsphere Size is controllable in micrometer range, can basis
Different application adjusts size.Mechanical strength is high, and bearing capacity is strong, can be answered without crushing, grinding with other materials
Close without destroying its loose structure, do not interfere with its thermal and insulating performance.
3) aerogel microball that this method is obtained, surface hydrophilic can be well dispersed in aqueous matrix, such as aqueous
In coating, there is a stronger interaction with matrix, will not reunite after drying, dry linting.In addition, in hydrophobic matrices, because
There is abundant hydroxyl on aeroge surface, its surface can be modified with hydrophobic modifier and (not interfere with aeroge inner hydrophilic
Property), it is had more preferable compatibility with hydrophobic substrates.
Brief description of the drawings
Fig. 1 is the structural representation for the hydrophilic silicon dioxide aerogel microball that embodiment 1 is obtained.
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；
Dispersion liquid of the silica aerosil microballoon in water obtained by Fig. 4 embodiment of the present invention 1；
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.
Embodiment
Below, with reference to accompanying drawing and embodiment, the present invention is described further：
In specific examples below, such as non-specified otherwise, the reagent used can pass through commercially available mode or routine test
Means are obtained.
The present invention provides a kind of preparation method of hydrophilic silicon dioxide aerogel microball, comprises the following steps：
1) siloxanes performed polymer is synthesized：The hydrophilic compounds of tetraalkoxysilane, hydroxyl are added into the first solvent with 100-
1000 revs/min of speed is stirred to transparent, adds dilute acid soln, after reaction completely, is removed solvent, is obtained 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, monose 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 mean molecule quantity is 200-10000, and mean molecule quantity is 200-
10000 polyvinyl alcohol, monose and polysaccharide etc.；Tetraalkoxysilane/the ethanol/hydroxyl hydrophilic compounds mass ratio is
100/25-100/1-10；The stirring is one kind in magnetic agitation or mechanical agitation, and mixing speed is 100-1000 revs/min
Clock；Acid is one kind in hydrochloric acid, nitric acid, sulfuric acid, acetic acid or oxalic acid；The mode of solvent is removed to steam for vacuum distillation, constant-pressure and high-temperature
Evaporate, one kind in rotary evaporation and thin film evaporation, preferably vacuum distillation；
2) self assembly：By step 1) siloxanes performed polymer be added to the water carry out self assembly, obtain white " milky " liquid；Water is excellent
Elect deionized water as；
3) wash：To step 2) emulsion in add alkali regulation pH to 9-11, stirring, standing obtain 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 ammoniacal liquor one kind；
4) dry：By step 3) white precipitate in 40-90 DEG C of constant pressure and dry, produce 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 is obtained
The structural representation of silica aerogel microballoon is as shown in figure 1, it includes the silica shell with smaller hole and is wrapped in described
The silicon dioxide skeleton with larger pore structure in silica shell.The aerogel microball size is 0.1-100 microns, institute
The thickness for stating silica shell is 5-50 nanometers, and the pore size being distributed 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, comprises the following steps:
(1) 278.32 grams of tetraethyl orthosilicates, 150 grams of ethanol, 10 grams of polyethylene glycol (mean molecule quantity 1000) are mixed equal
It is even to transparent；15 grams of concentrated hydrochloric acids (mass concentration is 37%) and 20 grams of water are well mixed, is then slowly dropped into, waits to be added dropwise to complete
Afterwards, be warming up to 60 degree, continue stirring reaction 2 hours, decompression flash distillation falls the ethanol in system, obtain with certain viscosity,
Flowable, transparent siloxanes performed polymer；
(2) 50 grams of above-mentioned siloxanes performed polymers are added in 100 grams of distilled water for (500 revs/min) under high velocity agitation, treated
It is added dropwise to complete, pH to 10 is adjusted with ammoniacal liquor, continue stirring reaction 2 hours, obtains white emulsion；
(3) above-mentioned emulsion is stood and obtains white precipitate in 1 hour, be removed by filtration aqueous phase, and rinsed twice and arrive with water
PH is put into 80 DEG C of baking oven close to neutrality, by gained solid and heated 5 hours, that is, obtains dry silica aerosil microballoon.
The aerogel microball scanning electron microscope (SEM) photograph of gained is as shown in Figure 2, infrared absorption spectra is as shown in figure 3, its size is in 1-2
Microns, spherical complete, even size distribution does not find substantially to rupture and cave in after drying.The aerogel microball of gained
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
The difference of embodiment 2 and embodiment 1 is, tetraethyl orthosilicate in step (1) is replaced with into positive silicic acid four
Methyl esters, 203.5 grams are reduced to by amount, and polyethylene glycol (mean molecule quantity 1000) is replaced with into polyvinyl alcohol (mean molecule quantity
500) amount, is reduced to 5 grams, reaction temperature is brought up to 80 DEG C.
Finally give the transmission electron microscope picture of aerosil as shown in figure 5, its size range be 5-10 micron, inside
Porosity is high, after drying, and does not find that loose structure is damaged in high vacuum conditions.
Embodiment 3
The difference of embodiment 3 and embodiment 1 is, the amount of concentrated hydrochloric acid in step (1) is increased into 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 of stirring reaction is increased to 5 hours.
Aerosil its 1g stacking volume is finally given as shown in fig. 6, its size range is at 20-50 microns,
Density is 0.05g/cm3, specific surface area is 800m2/g。
Embodiment 4
The difference of embodiment 4 and embodiment 1 is, tetraethyl orthosilicate in step (1) is replaced with into positive silicic acid four
Methyl esters, is reduced to 203.5 grams by amount, ethanol is replaced with into methanol, and amount is reduced into 105 grams, by polyethylene glycol (mean molecule quantity
1000) glucose (molecular formula is replaced with：C6H12O6), amount is increased to 15.0 grams, concentrated hydrochloric acid is replaced with into concentrated nitric acid, and (quality is dense
Spend 65%), amount to be reduced into 8.5 grams.
The aerosil size finally given is at 10-20 microns, and density is 0.15g/cm3, specific surface area is
650m2/g。
It will be apparent to those skilled in the art that technical scheme that can be as described above and design, make other various
It is corresponding to change and deformation, and all these change and deformation should all belong to the protection domain of the claims in the present invention
Within.
Claims (10)
1. a kind of preparation method of hydrophilic silicon dioxide aerogel microball, it is characterised in that comprise the following steps：
1) siloxanes performed polymer is synthesized：The hydrophilic compounds of tetraalkoxysilane, hydroxyl are added into the first solvent with 100-1000
Rev/min speed stir to transparent, add dilute acid soln, after reaction completely, remove solvent, obtain siloxanes performed polymer；Institute
State hydrionic concentration in dilute acid solnThe 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, monose or polysaccharide；
2) self assembly：By step 1) siloxanes performed polymer be added to the water carry out self assembly, obtain white " milky " liquid；
3) wash：To step 2) emulsion in add alkali regulation pH to 9-11, stirring, standing obtains white precipitate, crosses and filter out
Water is removed, and is washed with water until pH is 6-8；
4) dry：By step 3) white precipitate in 40-90 DEG C of constant pressure and dry, produce silica aerosil microballoon.
2. according to the method described in claim 1, it is characterised in that step 1), the alkoxy of the tetraalkoxysilane is
It is more than one or both of methoxyl group, ethyoxyl and isopropoxy.
3. according to the method described in claim 1, it is characterised in that step 1), first solvent is methanol, ethanol, different
Propyl alcohol, butanol, propylene glycol monomethyl ether, acetone or butanone.
4. according to the method described in claim 1, it is characterised in that step 1), the polyalcohols molecular weight is 200-10000,
The polyalcohols is polyethylene glycol or polyvinyl alcohol.
5. according to the method described in claim 1, it is characterised in that step 1), first solvent is ethanol, described to contain hydroxyl
The hydrophilic compounds of base are PEG1000, and tetraalkoxysilane, ethanol, PEG1000 weight ratio are 100:(25-100)：(1-
10)。
6. according to the method described in claim 1, it is characterised in that step 1), first solvent is ethanol, described to contain hydroxyl
The hydrophilic compounds of base are PVA500, and tetraalkoxysilane, ethanol, PVA500 weight ratio are 100:(25-100)：(1-10).
7. according to the method described in claim 1, it is characterised in that step 1), the method for solvent is removed for distillation or is depressurized
Distillation.
8. according to the method described in claim 1, it is characterised in that step 2), the addition of water is tetraalkoxysilane weight
1-100 times of amount.
9. according to the method described in claim 1, it is characterised in that step 3), the alkali be sodium hydroxide, potassium hydroxide or
Ammoniacal liquor.
10. hydrophilic silicon oxides aerogel microball prepared by a kind of method described in utilization claim any one of 1-9.
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