CN105295506B - A kind of improvement St*ber methods prepare TiO2/SiO2The method of aerogel microball - Google Patents
A kind of improvement St*ber methods prepare TiO2/SiO2The method of aerogel microball Download PDFInfo
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Abstract
The present invention relates to a kind of improvementMethod prepares TiO2/SiO2The method of aerogel microball, including：(1) preparing titanium dioxide suspension；(2) methyl orthosilicate or the mixed sols of ethyl orthosilicate and alcohol are prepared；(3) mixed solution of ammonium hydroxide and ethyl alcohol is prepared；(4) mixed sols is made to be reacted with mixed solution；(5) into step (4) acquired solution, the reaction was continued for addition silicon fluoride self assembly liquid；(6) by step (5) acquired solution eccentric cleaning drying to get.Method provided by the invention carries out mild condition under normal pressure, and reaction temperature is not high to equipment requirement no more than 80 DEG C, can reduce production cost, improves production security.The TiO prepared using the method for the present invention2/SiO2Aerogel microball grain size is in 200~750nm, and surface is smooth, and monodispersity is preferable, aeroge integrality is good, no fragmentation or crackle, has the advantages that good transparency, hydrophobic, infrared heat reflectivity is good, thermal conductivity is low etc., it has broad application prospects in building fields such as coating, coiled materials.
Description
Technical field
The present invention relates to nanoporous SiO2A kind of gel rubber material technical field, and in particular to improvementIt is prepared by method
TiO2/SiO2The method of aerogel microball.
Background technology
SiO2Aeroge is a kind of novel super heat-insulating material to grow up in recent years.It is a kind of light porous amorphous
Solid-state material, the typical sizes of network structure Hole are 1~100nm, and porosity is then up to 80%-99.8%, specific surface
Product is even as high as 200m2/ g~1000m2/ g, and density can be down to 1kg/m3~400kg/m3, thermal conductivity factor can be down to
0.005W/ (mK) left and right.SiO2Why aeroge has above-mentioned excellent performance, and one is exactly to make the reason of critically important
By controlling technological parameter during standby so that SiO2The hole diameter of aeroge is less than air in 50nm or so, hole diameter
The mean free path of molecule so that air molecule movement is separated by hole wall, and material at this time is in the state of near vacuum.Due to
Its high specific surface area, air gaseous heat conduction and solid gel skeleton solid-state heat transfer are in the complicated path of this bending
Almost it is isolated, so that this material has the thermal conductivity factor less than air, it can be as low as 0.005W/ (mk) below.
It is used as a kind of inorganic material, SiO simultaneously2The density of aeroge is low, and water proof fire retardant is environmentally protective, is being built if applied
Exterior insulation field will have broad prospects.However, as SiO2The unique space random network structure of aeroge and low close
The design feature of degree high porosity makes its intensity difference, strong adsorption force, and water preventing ability is poor, and molding difficulty is big, so SiO2Compound gas
The progress of gel is slow.
Preparation SiO common at present2The method of aeroge has supercritical methanol technology and normal temperature and pressure method.The two of supercritical methanol technology preparation
Silica aerogel performance is more excellent, but device systems complex and expensive and need to work at high temperature under high pressure, dangerous higher.And
Gel can be shunk existing normal temperature and pressure method in the drying process, make its easily broken or cracked.In addition the prior art is made
The SiO obtained2Properties of aerogels is relatively simple, although its heat-proof quality is preferably applied on Material Field such as coating and coiled material
Shi Buneng meets multi-functional demand.In south China climate moistening rainwater more regions, wall often by rain drop erosion, contains
The exterior coating and coiled material service life for having aerosil are not grown, and can be extended if a kind of coating of super hydrophobic is developed
Its service life.In addition, being continuously increased with China's building energy consumption, energy-saving problem is increasingly valued by the people, especially
When being that summer temperature is high, the operating of air-conditioning can consume big energy.It develops a kind of absorption that can reduce solar heat, reduce room
Interior temperature reduces the research hotspot that the external wall infrared-reflection heat-insulation coating that air-conditioning uses is energy-saving building materials.
Invention content
It is of the existing technology it is an object of the invention to solve the problems, such as, a kind of improvement is providedMethod prepares TiO2/
The method of SiO2 aerogel microballs, technical scheme is as follows：
A kind of improvementMethod prepares TiO2/SiO2The method of aerogel microball, includes the following steps：(1) two are prepared
Titanium oxide suspension；(2) using methyl orthosilicate or ethyl orthosilicate and alcoholic solvent, tio_2 suspension, formamide, distillation
Water prepares mixed sols；(3) mixed solution of ammonium hydroxide and absolute ethyl alcohol is prepared；(4) under water bath with thermostatic control and stirring condition, by institute
It states mixed sols and adds in mixed solution several times and react；(5) silicon fluoride self assembly is periodically added dropwise into step (4) acquired solution
The reaction was continued for liquid；(6) step (5) acquired solution eccentric cleaning is dried.
Preferably, calgon and ultrasonic disperse processing, titanium dioxide used are also added into step (1) described suspension
Titanium is rutile-type powder, and titanium dioxide mass fraction is 3%-6% in suspension.
Preferably, the preparation of step (2) described mixed sols is included methyl orthosilicate or ethyl orthosilicate and titanium dioxide
Titanium suspension, alcoholic solvent, distilled water are stirred, and add in HNO3Solution adjusts pH value to 3-4, adds formamide ultrasound point
It dissipates, wherein methyl orthosilicate or ethyl orthosilicate and the molar ratio of distilled water, alcoholic solvent, formamide, nitric acid is 1：1：6-8：
0.6-0.8：10-4-10-3, TiO in mixed sols2:With SiO2Molar ratio be 1:10.
It is furthermore preferred that the alcoholic solvent is methanol, ethyl alcohol, one kind in butanol or combination.
Preferably, the volume ratio of step (3) absolute ethyl alcohol and ammonium hydroxide is 1:4-6.
Preferably, step (4) the water bath with thermostatic control temperature is 43 DEG C, and the mixed sols is added to isometric points for 4 times
In mixed solution, the reaction time is for 24 hours.
Preferably, step (5) the silicon fluoride self assembly liquid is under nitrogen protection, silicon fluoride to be added in isopropanol solvent
In stir evenly and with nitre acid for adjusting pH value to obtained by 1.8-2.5.
It is furthermore preferred that the silicon fluoride is 3,3,3- trifluoro propyl methyl dimethoxysilanes and ten difluoro heptyl propyl three
Methoxy silane mixture.
Preferably, the addition of step (5) silicon fluoride self assembly liquid in step 4 acquired solution volume ratio be 1:5, it is added dropwise
Bath temperature is adjusted after the completion to 65 DEG C, is continued constant temperature constant speed and is stirred to react 12h.
Step (6) the eccentric cleaning drying includes reaction product using alcohol and dimethylbenzene under the rotating speed of 4000rpm
Eccentric cleaning 4 times respectively is then placed in the dry 20-30h of 75 DEG C of constant temperature in vacuum drying chamber.
Improvement provided by the inventionMethod prepares TiO2/SiO2The method of aerogel microball overcomes supercritical methanol technology and deposits
Equipment it is complicated, production cost is high, dangerous high and non-pressure process is difficult to obtain complete S iO2It is the shortcomings that aeroge, all anti-
Mild condition should be carried out under normal pressure, and reaction temperature is no more than 100 DEG C, to the of less demanding of equipment, thus can reduce and be produced into
This, improves production security.The TiO prepared using the method for the present invention2/SiO2Aerogel microball grain size is on 200~750nm, surface
Smooth, monodispersity is preferable；Macroscopically aeroge integrality is good, no fragmentation or crackle, has good transparency, hydrophobic, infrared heat
The advantages such as reflectivity is good, thermal conductivity is low.The aeroge has broad application prospects in building fields such as coating, coiled materials.
Specific embodiment
In order to which those skilled in the art is made to fully understand technical scheme of the present invention and advantageous effect, with reference to embodiment
It illustrates.
Embodiment one
(1) preparing titanium dioxide suspension.It measures 100ml distilled water to be put into beaker, adds in six inclined phosphorus of 0.45-0.50g
Sour sodium (dispersant) adds the rutile titania powder that a certain amount of grain size is 50nm-100nm after stirring and dissolving, will
Beaker is put into ultrasonic disperse 30-50min in the ultrasonic cell disruptor of 540w, obtains the titanium dioxide that mass fraction is 3%
Suspension.
The effects that localized hyperthermia, high pressure, strong shock wave and microjet that ultrasound generates, it is micro- greatly to weaken nanometer
The nanoaction of intergranular is effectively prevented nanoparticle and reunites and be allowed to fully dispersed.Select luminous reflectanc, refraction index
Stronger rutile TiO2Adulterate SiO2Aeroge can reduce the infrared extinction coefficient of material to a certain extent, increase
TiO2/SiO2The infrared heat reflectivity of aeroge.
(2) mixed sols is prepared using methyl orthosilicate, tio_2 suspension, absolute ethyl alcohol, formamide, distilled water.
After methyl orthosilicate, tio_2 suspension, absolute ethyl alcohol, distilled water are uniformly mixed, HNO is used3Solution adjusts pH to 3-
4, it is subsequently added into drying control agent formamide and ultrasonic disperse is up to mixed sols.Methyl orthosilicate, distilled water, nothing in the colloidal sol
Water-ethanol, formamide, HNO3Molar ratio be 1:1：6-8:0.6-0.8:10-4-10-3.TiO in mixed sols obtained2:With
SiO2Molar ratio be 1:10.
Addition formamide can make the aperture increases of gel network, and the alcohol that aperture increases are conducive in methyl orthosilicate is molten
In liquid soaking process, methyl orthosilicate molecule enters each position in gel duct, reacts with-the OH of gel surface,
Generate ≡ Si-O-Si (OC2H5)2The structure of-O-Si ≡, and play the role of supporting duct.For different alcoholic solvents, methanol
In reaction rate it is most fast, the reaction rate of butanol is most slow.It can also be used in mixed way using two two or three kinds of alcohol, when methanol and fourth
The ratio of alcohol mixture is 1：When 3 (volume ratio), more consistent particle can be obtained.
(3) mixed solution of ammonium hydroxide and absolute ethyl alcohol is prepared.2~6ml ammonium hydroxide is taken to be placed in three-necked flask, adds in anhydrous second
Alcohol is uniformly mixed, and wherein absolute ethyl alcohol and ammonium hydroxide volume ratio are 1: 4-6.
(4) under water bath with thermostatic control and stirring condition, the mixed sols is added in mixed solution several times and is reacted.43
Under the conditions of DEG C water bath with thermostatic control, mixed sols point prepared by step (2) is added in three-necked flask for 4 times, is stirred to react for 24 hours.It is mixed
It is equal with liquor capacity in three-necked flask to close colloidal sol addition volume.It is added to avoid tradition several timesMethod adds in
Solution local concentration is excessively high during TMOS, so that being nucleated in solution uniform.
(5) silicon fluoride self assembly liquid is periodically added dropwise into step (4) solution the reaction was continued.It under nitrogen protection will be a certain amount of
Silicon fluoride (FAS) add in isopropanol solvent in stir evenly, add in salpeter solution adjust pH to 1.8-2.5, continue stir 12h
Obtain the silicon fluoride self assembly liquid of water white transparency.The silicon fluoride is 3,3,3- trifluoro propyls methyl dimethoxysilane and ten difluoros
Heptyl propyl trimethoxy silicane mixture.It measures a certain amount of silicon fluoride self assembly liquid to be added in separatory funnel, periodically by it
It is all added drop-wise in three-necked flask, adjusts bath temperature to 65 DEG C, constant temperature, constant speed is kept to be stirred to react 12h.Silicon fluoride self assembly
The addition of liquid is 1 with step (4) acquired solution volume ratio:5.
Silicon fluoride can make SiO2Aeroge connects 3-O- (CH3)3Form a hydrophobic umbrella-shaped structure, this hydrophobic umbrella
Shape structure can mutual long, rectangular bag form hydrophobic membrane, and fluorine-containing point with water resistance of one layer of orientation is formed on aeroge surface
Sublayer.TiO with this structure2/SiO2It is not easy to adsorb moisture content again after aerogel microball drying, there is super hydrophobic
Energy.
(6) step (5) acquired solution eccentric cleaning is dried.Reaction product in three-necked flask is taken out, 4000rpm's
Distinguish eccentric cleaning 4 times with alcohol and dimethylbenzene under rotating speed, lower sediment thing is placed in 75 DEG C of dryings of constant temperature in vacuum drying chamber
20-30h to get.
Embodiment 2-12 keeps the whole individual parameters of other parameter invariable tone such as following table with reference to embodiment one：
TiO prepared by 1-12 of the embodiment of the present invention2/SiO2Aerogel microball grain size is in 200-750nm, the microsphere particle table
The smooth monodispersity in face is good, and for hydrophobic angle up to 150 °, thermal conductivity is low.The aeroge integrality is good, no fragmentation or crackle, transparency
Good, infrared transmittivity is relative to pure SiO2The infrared transmittivity of aeroge reduces more than 50%.
In order to verify the TiO of the invention prepared2/SiO2The actual use performance of aerogel microball, we have been done about coating
The experiment of equilibrium temperature.The TiO that the embodiment 1-4 of identical weight is taken to prepare respectively2/SiO2Aerogel microball, by formula as below
(mass fraction) is prepared into modified acrylic coating material and VAE coating：10%~15% TiO2/SiO2Aerogel microball, 10%
Calcium sulfate crystal whiskers, 5% hollow glass microbead, 0.1%~5% other auxiliary agents, surplus for modified acroleic acid filming emulsion or
VAE filming emulsions.It is ultraphobic aqueous good that the modified acrylic coating material and VAE coating have, and infrared heat reflectivity is good and lower thermal conductivity
The characteristics of.Experiment is found, adds TiO prepared by embodiment 32/SiO2Modified acrylic coating material's equilibrium temperature of aerogel microball by
90 DEG C drop to 84.9 DEG C, TiO prepared by addition embodiment 12/SiO2The VAE coating equilibrium temperature of aerogel microball is by 90 DEG C
86.7 DEG C are dropped to, two kinds of coating are respectively provided with preferable infrared heat reflection performance.
Claims (9)
1. a kind of improvementMethod prepares TiO2/SiO2The method of aerogel microball, which is characterized in that include the following steps：
(1) preparing titanium dioxide suspension；(2) using methyl orthosilicate or ethyl orthosilicate and alcoholic solvent, tio_2 suspension, first
Amide, distilled water prepare mixed sols；(3) mixed solution of ammonium hydroxide and absolute ethyl alcohol is prepared；(4) in water bath with thermostatic control and stirring bar
Under part, the mixed sols is added in mixed solution several times and is reacted；(5) fluorine is periodically added dropwise into step (4) acquired solution
The reaction was continued for silane self assembly liquid；(6) step (5) acquired solution eccentric cleaning is dried；Wherein step (2) described mixed sols
Preparation include methyl orthosilicate or ethyl orthosilicate are stirred with tio_2 suspension, alcoholic solvent, distilled water, addition
HNO3Solution adjusts pH value to 3-4, adds formamide ultrasonic disperse, wherein methyl orthosilicate or ethyl orthosilicate and distillation
Water, alcoholic solvent, formamide, nitric acid molar ratio be 1:1:6-8:0.6-0.8:10-4-10-3, TiO in mixed sols2:With SiO2
Molar ratio be 1:10.
2. according to the method described in claim 1, it is characterized in that：Hexa metaphosphoric acid is also added into step (1) described suspension
Sodium simultaneously carries out ultrasonic disperse processing, and titanium dioxide used is rutile-type powder, and titanium dioxide mass fraction is in suspension
3%-6%.
3. according to the method described in claim 1, it is characterized in that：The alcoholic solvent for methanol, ethyl alcohol, one kind in butanol or
Combination.
4. according to the method described in claim 1, it is characterized in that：The volume ratio of step (3) absolute ethyl alcohol and ammonium hydroxide is
1:4-6。
5. according to the method described in claim 1, it is characterized in that：Step (4) the water bath with thermostatic control temperature is 43 DEG C, described mixed
Conjunction colloidal sol, which divides 4 times, to be added in isometric mixed solution, and the reaction time is for 24 hours.
6. according to the method described in claim 1, it is characterized in that：Step (5) the silicon fluoride self assembly liquid is protected in nitrogen
Under shield, silicon fluoride is added in isopropanol solvent and is stirred evenly and obtained by nitre acid for adjusting pH value to 1.8-2.5.
7. according to the method described in claim 6, it is characterized in that：The silicon fluoride is 3,3,3- trifluoro propyl methyl dimethoxy oxygen
Base silane and ten difluoro heptyl propyl trimethoxy silicane mixtures.
8. according to the method described in claim 1, it is characterized in that：The addition and step of step (5) silicon fluoride self assembly liquid
(4) acquired solution volume ratio is 1:5, bath temperature is adjusted after being added dropwise to complete to 65 DEG C, continues constant temperature constant speed and is stirred to react 12h.
9. according to the method described in claim 1, it is characterized in that：Step (6) the eccentric cleaning drying includes that production will be reacted
Object distinguishes eccentric cleaning 4 times under the rotating speed of 4000rpm with alcohol and dimethylbenzene, is then placed in 75 DEG C of constant temperature in vacuum drying chamber
Dry 20-30h.
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| CN106084897A (en) * | 2016-06-16 | 2016-11-09 | 常熟市屹浩食品包装材料科技有限公司 | It is applied to surfactant modifying nano material and preparation method thereof |
| CN106423000A (en) * | 2016-09-28 | 2017-02-22 | 武汉纺织大学 | Preparation method for core-shell TiO2-SiO2 microsphere self-assembled structural color film |
| CN107128934B (en) * | 2017-06-28 | 2019-04-30 | 武汉理工大学 | Light hollow aeroge ball forming method and its mold used |
| CN109337467B (en) * | 2018-09-30 | 2021-01-12 | 沈阳顺风新材料有限公司 | Water-based heat-insulating reflective coating and preparation method thereof |
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| CN114988417B (en) * | 2022-07-15 | 2024-01-12 | 中国科学院苏州纳米技术与纳米仿生研究所 | Super-white silicon oxide aerogel, preparation method and application thereof |
| CN116376406B (en) * | 2023-06-05 | 2024-02-09 | 西南石油大学 | TiO (titanium dioxide) 2 /H-SiO 2 EP superhydrophobic composite coating, preparation method and application thereof |
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