CN109575484A - Novel galapectite/polyvinyl alcohol composite aerogel and its preparation method and application - Google Patents
Novel galapectite/polyvinyl alcohol composite aerogel and its preparation method and application Download PDFInfo
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08J2329/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
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Abstract
The invention discloses a kind of novel galapectite/polyvinyl alcohol composite aerogels and its preparation method and application, use deionized water as solvent, borax soln is as crosslinking agent, using environmental-friendly freeze drying process of preparing same, the result shows that when PVOH:HNTs is 3:7, composite aerogel with unique three-dimensional nanoporous network structure is obtained, wherein support section of the HNTs as structural framework.Polyvinyl alcohol molecule is adhere strongly to the outer surface of fibrous HNTs.It is reduced as HNTs content increases with PVOH content, density first drops to 0.16cm3Increase after/g, thermal coefficient is exactly the opposite, and variation range is in 0.025 and 0.032Wm‑1K‑1Between.Obtain the aeroge sample of compressive strength megapascal from 0.8 to 2.5.These representative characteristics show that HNTs/PVOH composite aerogel has a wide range of applications in building heat preservation field.
Description
Technical field
The present invention relates to aeroge technical field, more particularly to novel galapectite/polyvinyl alcohol composite aerogel and its
Preparation method and application.
Background technique
Aeroge is a kind of porous material with nanostructure, has low-density, high porosity, high-specific surface area, low
The features such as thermal conductivity, this is its good candidate people as numerous areas.However, common traditional aerogel material, such as two
Silica aerogel has that low self-strength, blockiness poor, preparation flow complexity, manufacturing cycle is longer, there are solvent contaminations etc.
Defect is unable to satisfy aerogel material in practical application, the especially requirement in building heat preservation field.Therefore, it finds a kind of novel
Aeroge is very critical using a kind of low cost, pollution-free raw material and simple, environmental-friendly preparation method.Since
Mackenzie and Call is reported for the first time prepares montmorillonitic clay aeroge with freeze-drying, and clay soil clay soil silica aerogel causes more next
The concern of more researchers, due to its excellent heat-insulated, absorption property and environmental-friendly freeze drying process of preparing same.Clay
The natural material of aeroge makes it compare aerosil in practical application with relatively easy, free of contamination preparation method
In with greater advantage.The clay component of overwhelming majority clay soil clay soil silica aerogel is montmorillonite at present, however montmorillonite is micron order
Laminated clay, the pre-processing and intercalation modifying of montmorillonite can make the preparation of clay soil clay soil silica aerogel and its polymer composite aerogel
Process becomes complicated, and cost increases.In addition to this, the micron order size of montmorillonite itself determines its clay soil clay soil silica aerogel very
Hardly possible forms nanoscale porous structure, this will be such that the unique heat-proof quality of aerogel material loses significantly.
Galapectite is a kind of natural fibrous clay, has nanoscale tubular structure, by alternate oxygen-octahedron
Piece and alumina octahedral are constituted with the stoichiometric ratio of 1:1.General 0.2-1.5 μm of its length, the general 50nm of overall diameter.According to
Report before this, HNTs are be evaluated as one-dimensional (1D) nanofiller of polymer.It should be noted that due to weak between galapectite
Bridging property, it is that the aerogel material with three-dimensional porous structure impossible is independently formed by collosol and gel mode.Therefore, it needs
It introduces polymer and constructs three-dimensional porous network structure jointly as the cross-linked phase between HNTs.Polyvinyl alcohol is a kind of building
The ideal material of aeroge porous structure, due to its low cost, water-soluble and between clay strong interaction, previous
In report, polyvinyl alcohol is just frequently used for synthesizing polyethylene alcohol/montmorillonite Composite aeroge.At the same time, for being crosslinked poly- second
The crosslinking agent of enol be used to increase solution viscosity while the polymer content in less aeroge and keep mechanical performance, obtain
To high porosity, high intensity, low combustible composite aerogel.
Summary of the invention
In view of the technical drawbacks of the prior art, it is an object of the present invention to provide a kind of novel galapectites
(HNTs)/polyvinyl alcohol (PVOH) composite aerogel and its preparation method and application.
The technical solution adopted to achieve the purpose of the present invention is:
A kind of novel galapectite/polyvinyl alcohol composite aerogel of the invention, the molecular weight of the polyvinyl alcohol are
80000-90000, the density of the composite aerogel are 0.04-0.17g/cm3, thermal conductivity is 0.02-0.04W m-1K-1, compression
Modulus is 4.2-8.7MPa；
It prepares in accordance with the following methods:
Step 1, polyvinylalcohol solids are dissolved in deionized water, the magnetic agitation 4-6h under 70-90 DEG C of water bath condition,
Then ultrasonic treatment 3-10min, prepares poly-vinyl alcohol solution；
Step 2, galapectite is mixed into deionized water, with ultrasonic emulsifier ultrasound 5-15min, prepares HNTs suspension；
Step 3, the poly-vinyl alcohol solution that step 1 obtains and the HNTs suspension that step 2 obtains are mixed to get mixed liquor,
Wherein mass percent of the polyvinyl alcohol in the mixed liquor is 1wt%-9wt%, quality of the HNTs in the mixed liquor
Percentage is 9wt%-1wt%, then at the uniform velocity enters water-soluble borax saturated solution, the water solubility borax dropwise into mixed liquor
The volume ratio of saturated solution and mixed liquor is (2-3): 100, it is added dropwise with the speed of 1-2ml per minute, obtains height after being added dropwise
Viscosity mixed sols is put into freezing after obtained high viscosity mixed sols is kept 6-10h at a temperature of -20 DEG C~-30 DEG C
Dry 24-72h, the PVA/HNTs composite aerogel being crosslinked in drying machine；The PVA/HNTs composite aerogel of the crosslinking
It is using HNTs nanotube as network support structure, with the three-dimensional porous net of polyvinyl alcohol molecule cross-linked phase between HNTs nanotube
Network structure.
Preferably, in the step 3, the quality summation of polyvinyl alcohol and HNTs are in the mass fraction in the mixed liquor
For 10wt%.
Preferably, in the step 3, the mass fraction of the polyvinyl alcohol is 3wt%-7wt%, preferably 3wt%, institute
The mass fraction for stating HNTs is 7wt%-3wt%, preferably 7wt%.
A kind of preparation method of novel galapectite/polyvinyl alcohol composite aerogel of the invention, comprising the following steps:
Step 1, polyvinylalcohol solids are dissolved in deionized water, the magnetic agitation 4-6h under 70-90 DEG C of water bath condition,
Then ultrasonic treatment 3-10min, prepares poly-vinyl alcohol solution；
Step 2, galapectite is mixed into deionized water, with ultrasonic emulsifier ultrasound 5-15min, prepares HNTs suspension；
Step 3, the poly-vinyl alcohol solution that step 1 obtains and the HNTs suspension that step 2 obtains are mixed to get mixed liquor,
Wherein mass fraction of the polyvinyl alcohol in the mixed liquor is 1wt%-9wt%, quality of the HNTs in the mixed liquor point
Number is 9wt%-1wt%, water-soluble borax saturated solution (saturated solution of borax in water) mixing is then added dropwise, by institute
After obtained sticky mixture keeps 6-10h at a temperature of -20 DEG C~-30 DEG C, dry 24-72h is put into freeze drier,
The PVA/HNTs composite aerogel being crosslinked；
In the PVA/HNTs composite aerogel of the crosslinking, there are interface cohesions between HNTs and polyvinyl alcohol, jointly
It constructs using HNTs nanotube as network support structure, with polyvinyl alcohol molecule, the three-dimensional of cross-linked phase is more between HNTs nanotube
Pore network structure.
Preferably, in the step 3, the quality summation of polyvinyl alcohol and HNTs are in the mass fraction in the mixed liquor
For 10wt%.
Preferably, in the step 3, the mass fraction of the polyvinyl alcohol is 3wt%-7wt%, preferably 3wt%, institute
The mass fraction for stating HNTs is 3wt%-7wt%, preferably 7wt%.
Preferably, the density of the PVA/HNTs composite aerogel of the crosslinking is 0.04-0.17g/cm3, thermal conductivity be
0.02-0.04W m-1K-1, compression modulus 4.2-8.7MPa.
Other hand of the invention, further include water-soluble borax saturated solution in cross-linking polyvinyl alcohol, galapectite to prepare
Application in PVA/HNTs composite aerogel.
Other hand of the invention further includes the PVA/HNTs composite aerogel of the crosslinking on building thermal insulation material
Using.
Preferably, the density of the PVA/HNTs composite aerogel is 0.04-0.17g/cm3, thermal conductivity 0.02-
0.04W m-1K-1, compression modulus 4.2-8.7MPa.
Compared with prior art, the beneficial effects of the present invention are:
Novel HNTs/PVOH composite aerogel block of the invention is quickly prepared by environmental-friendly freeze-drying,
Use water as solvent, borax soln is as polyvinyl alcohol crosslinked dose.The mass ratio of HNTs and PVOH is to the more of composite aerogel
Pore structure has critically important influence, when PVOH:HNTs is 3:7, with the compound of unique three-dimensional nanoporous network structure
Aeroge is obtained, wherein support section of the HNTs as structural framework.There are very strong interfaces between HNTs and polyvinyl alcohol
In conjunction with constructing a kind of unique three-dimensional porous network structure jointly.Obtained composite aerogel has low density
(0.16cm3/ g), low (the 0.025W m of thermal coefficient-1K-1At 25 DEG C) and excellent mechanical performance, have in building heat preservation and answers very well
Use prospect.
Detailed description of the invention
Fig. 1 is the high low power SEM microscopic appearance figure of composite aerogel under different PVOH:HNTs mass ratioes.
Fig. 2 is the infrared spectrogram of HNTs, pure PVOH aeroge and HNTs/PVOH clay composite aerogel.
Fig. 3 is the thermal weight loss and DTG curve of shown PVOH/HNTs composite aerogel.
Fig. 4 is the stress-strain diagram of PVOH/HNTs composite aerogel.
Fig. 5 is thermal coefficient of the different PVOH:HNTs mass than composite aerogel.
Specific embodiment
The present invention is described in further detail below in conjunction with the drawings and specific embodiments.It should be appreciated that described herein
Specific embodiment be only used to explain the present invention, be not intended to limit the present invention.
It is technical grade that polyvinyl alcohol (PVA) (MW ≈ 95000), which is purchased from Tianjin Feng Chuan chemical reagent Science and Technology Ltd.,.Angstrom
Lip river stone is from the purchase of Zhejiang Feng Hong clay Co., Ltd (Zhejiang, China).Borax (Na2B4O7·10H2O it) obtains by Tianjin
Sky over the river Chemical Industry Science Co., Ltd.It is all used in the micropore water purification system to test obtained double deionized waters.All
Chemicals and reagent are used for without being further purified.
The structural constituent of polyvinyl alcohol and HNTs are given with the percentage of deionized water.In order to prepare containing 5wt%
The aeroge (being labeled as P5H5, wherein P represents polyvinyl alcohol, and H represents HNTs) of polyvinyl alcohol and 5wt%HNTs, the poly- second of 5g
Enol solid is dissolved in 50ml deionized water, and magnetic agitation 5h, is then ultrasonically treated 5min under 80 DEG C of water bath conditions.5g
HNTs is mixed into 50ml deionized water, prepares HNTs suspension with ultrasonic emulsifier ultrasound 10min.By HNTs suspension and polyethylene
The mixture that alcoholic solution generates is introduced into beaker 200 milliliters, and subsequent 2ml borax saturated solution, which instills, to be added.Gained is sticky
Mixture be poured on polyethylene bottle (diameter: 25mm；Highly: 45mm) and aluminum dipping form (100mm × 100mm × 25mm), in -25 DEG C of temperature
Degree is lower to keep 8h, is subsequently placed into freeze drier dry 48h.Obtained crosslinking PVA/HNTs composite aerogel, is denoted as P5H5,
It is put into drying basin and waits further characterization.
Similarly, when the addition 10g of polyvinylalcohol solids is prepared P10H0, works as polyvinyl alcohol when HNTs adds 0g
P7H3 is prepared when HNTs adds 3g in the addition 7g of solid, as the addition 3g of polyvinylalcohol solids, when HNTs adds 7g, system
It is standby to obtain P3H7.
As shown in Figure 1, the component proportion of PVOH and HNTs has a very big impact its microscopic appearance in composite aerogel.
The microscopic appearance of two samples of P10H0 and P7H3 is the uneven lamellar structure formed by ice template, is existed between lamella
Part PVOH network structure.It does not exist together between the two and is exactly that the piece interlamellar spacing of P7H3 sample is reduced, and P7H3's
HNTs nanotube is interspersed with bound form in PVOH network.Apparent change has occurred in the microscopic appearance pattern of P5H5 sample,
With the reduction of HNTs content increased with PVOH content, whole pattern changes towards uniform three dimensional porous structure.In P5H5-2
In we can see that this network structure is mainly and the main work of PVOH since the mutual overlap joint of HNTs nanotube is formed
With then becoming fixing and connecting different HNTs nanotubes, to maintain this unique network structure.From P3H7-1, we can be with
Find out, with further increasing for HNTs, network structure more uniform, with smaller szie pore structure can be obtained
?.And in P3H7-2, it can be observed similar to the structure of P5H5, the frame based on HNTs, PVOH is cross-linked phase.Value
It is noted that occur the PVOH network in similar P10H0-2 image in the gap of HNTs overlapped porous structure, it is smaller
The hole of size is obtained.
Fig. 2 shows the infrared spectrogram of HNTs, pure PVOH and HNTs/PVOH composite aerogel.3697 and 3622cm-1Place
Bimodal and 911cm-1The unimodal of place respectively indicates the l-OH group stretching vibration of HNTs surface A and bending vibration.In addition,
694cm-1、754cm-1And 1032cm-1The peak that place observes corresponds respectively to the midplane extrusion of the symmetrical stretching, extension of Si-O, Si-O-Si
And asymmetrical stretch, this is the essential characteristic peak for being all HNTs.For pure PVOH aeroge sample, by 3125cm-1- the OH at place is drawn
Stretch vibration, the C=O stretching vibration at 1668cm-1,1400cm-1- the CH at place2Bending vibration and 1092cm-1The flexible vibration of the C-O at place
The dynamic characteristic absorption band for collectively constituting PVOH spectrum.The HNTs and PVOH in the infrared spectrogram of HNTs/PVOH composite aerogel
Characteristic peak completely saved, this explanation in recombination process chemical structure of HNTs and PVOH do not broken
It is bad.
As shown in figure 3, by TGA study different PVOH and HNTs mass ratioes PVOH aeroge and PVOH/HNTs it is compound
The thermal stability of aeroge.Corresponding curve is shown in Fig. 3, and the data provided are summarized in table 4.First zero-g period be by
Caused by the desorption of water, probably between 50 to 120 DEG C, since PVOH and HNTs belongs to hydrophilic material, surface is rich in
The presence of hydroxyl group.PVOH has a biggish catabolic phase and two continuous small catabolic phases, is respectively occurring at
Between 250-330 DEG C, between 420-470 DEG C between 500-540 DEG C, this and elder generation when Td10% are decomposed in starting
The preceding data in relation to report are consistent.With the reduction of PVOH content and the increase of HNTs content, the PVOH in TG curve decomposes rank
Section is gradually changed into two sections by three sections, and residual volume increased.The initial temperature of the first pyrolysis phase of PVOH is basically unchanged, however
The initial temperature of the second pyrolysis phase of PVOH increased.It is worth noting that, the coke yield of non-clay aeroge is about
10%；The addition of clay is likely to increase coke yield in a manner of simple, additive property.What is checked in this work is all
The practical carbon yield of polyalcohol/clay soil aeroge shows the loss of clay itself lower than expection.This most probable explanation of phenomenon
It is that at high temperature, caly structure is decomposed, discharges a large amount of water of hydration, in crystal structure so as to cause expected coke is lower than
Yield.
The mechanical property and density data of 1 composite aerogel of table
| Performance | P10H0 | P7H3 | P5H5 | P3H7 |
| Modulus (MPa) | 4.2±0.32 | 6.6±0.54 | 8.7±0.37 | 5.4±0.21 |
| Density (g/cm3) | 0.162±0.005 | 0.104±0.003 | 0.043±0.003 | 0.085±0.002 |
| M/d(MPa-cm3/g) | 26 | 63 | 102 | 125 |
The mechanical property and density data of composite aerogel are as shown above, in conjunction with Fig. 4 and table 1 we can see that with
The ratio of PVOH and HNTs becomes 3:7 from 10:0, then the modulus and intensity of composite aerogel, which first increased, to be declined.Initial stage is strong
The reason of degree increases may be to be advantageous as fibrous clay to the raising of composite aerogel mechanical performance due to HNTs；It removes
Except this, with the variation of component proportion, the microstructure of composite aerogel is gradually to uniform compact three-dimensional net structure
Transformation, this is conducive to the increase of mechanical property.And then the decline of composite aerogel mechanical property may be organic in aeroge
Caused by the reduction of object POVH content, this phenomenon is consistent with previous report.The mechanical property of this kind of material is general
Depending on their density, but other factors, for example, cross-linking agents, microstructure change and polymer content change
It is also to need to be considered.
Fig. 5 is thermal coefficient of the different PVOH:HNTs mass than composite aerogel.The aerogel-like material of pure PVOH preparation
Thermal coefficient be 0.038W/mK.With the reduction of PVOH content and the increase of HNTs content, the thermal coefficient of composite aerogel
It constantly reduces, heat-proof quality gradually increases.The heat transfer of porous material is broadly divided into three parts: solid heat transfer, gas heat-transfer
And radiant heat transfer.Wherein the solid heat transfer of material is mainly related with the density of material, and the density of material is lower, and porosity is higher,
Lower solid thermal conduction will be obtained, the solid thermal that furthermore complicated nanometer three-dimensional net structure is also beneficial to reduce material passes
It leads.And gas heat transfer is transmitted by the molecular vibration of air, the mean free path of air molecule vibration is 70nm, so
Hole less than 70nm effectively can hinder air molecule to vibrate, and achieve the purpose that reduce gas heat transfer.For PVOH/HNTs
The increase of composite aerogel, HNTs can be such that the microstructure of composite aerogel changes towards uniform three-dimensional net structure, and
Along with the appearance of part nanoaperture, these each contribute to the thermal coefficient for reducing composite aerogel, enhance its insulation
Performance.
The above is only a preferred embodiment of the present invention, it is noted that for the common skill of the art
For art personnel, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications
Also it should be regarded as protection scope of the present invention.
Claims (10)
1. a kind of novel galapectite/polyvinyl alcohol composite aerogel, which is characterized in that the molecular weight of the polyvinyl alcohol is
80000-90000, the density of the composite aerogel are 0.04-0.17g/cm3, thermal conductivity is 0.02-0.04W m-1K-1, compression
Modulus is 4.2-8.7MPa；
It prepares in accordance with the following methods:
Step 1, polyvinylalcohol solids are dissolved in deionized water, the magnetic agitation 4-6h under 70-90 DEG C of water bath condition, then
It is ultrasonically treated 3-10min, prepares poly-vinyl alcohol solution；
Step 2, galapectite is mixed into deionized water, with ultrasonic emulsifier ultrasound 5-15min, prepares HNTs suspension；
Step 3, the poly-vinyl alcohol solution that step 1 obtains and the HNTs suspension that step 2 obtains are mixed to get mixed liquor, wherein
Mass percent of the polyvinyl alcohol in the mixed liquor is 1wt%-9wt%, quality percentage of the HNTs in the mixed liquor
Number is 9wt%-1wt%, then at the uniform velocity enters water-soluble borax saturated solution, the water solubility borax saturation dropwise into mixed liquor
The volume ratio of solution and mixed liquor is (2-3): 100, it is added dropwise with the speed of 1-2ml per minute, obtains high viscosity after being added dropwise
Mixed sols is put into freeze-drying after obtained high viscosity mixed sols is kept 6-10h at a temperature of -20 DEG C~-30 DEG C
Dry 24-72h, the PVA/HNTs composite aerogel being crosslinked in machine；The PVA/HNTs composite aerogel of the crosslinking be with
HNTs nanotube is network support structure, with the three-dimensional porous network knot of polyvinyl alcohol molecule cross-linked phase between HNTs nanotube
Structure.
2. a kind of novel galapectite/polyvinyl alcohol composite aerogel as described in claim 1, which is characterized in that the step 3
In, mass fraction of the quality summation of polyvinyl alcohol and HNTs in the mixed liquor is 10wt%.
3. a kind of novel galapectite/polyvinyl alcohol composite aerogel as described in claim 1, which is characterized in that the step 3
In, the mass fraction of the polyvinyl alcohol is 3wt%-7wt%, and the mass fraction of preferably 3wt%, the HNTs are 7wt%-
3wt%, preferably 7wt%.
4. a kind of preparation method of novel galapectite/polyvinyl alcohol composite aerogel, which comprises the following steps:
Step 1, polyvinylalcohol solids are dissolved in deionized water, the magnetic agitation 4-6h under 70-90 DEG C of water bath condition, then
It is ultrasonically treated 3-10min, prepares poly-vinyl alcohol solution；
Step 2, galapectite is mixed into deionized water, with ultrasonic emulsifier ultrasound 5-15min, prepares HNTs suspension；
Step 3, the poly-vinyl alcohol solution that step 1 obtains and the HNTs suspension that step 2 obtains are mixed to get mixed liquor, wherein
Mass fraction of the polyvinyl alcohol in the mixed liquor is 1wt%-9wt%, and mass fraction of the HNTs in the mixed liquor is
Then water-soluble borax saturated solution (saturated solution of borax in water) mixing is added dropwise in 9wt%-1wt%, will be acquired
Sticky mixture keep 6-10h at a temperature of -20 DEG C~-30 DEG C after, be put into freeze drier dry 24-72h, obtain
The PVA/HNTs composite aerogel of crosslinking；
In the PVA/HNTs composite aerogel of the crosslinking, there are interface cohesions between HNTs and polyvinyl alcohol, common to construct
Using HNTs nanotube as network support structure, with the three-dimensional porous net of polyvinyl alcohol molecule cross-linked phase between HNTs nanotube
Network structure.
5. a kind of preparation method of novel galapectite/polyvinyl alcohol composite aerogel as described in claim 1, feature exist
In in the step 3, the quality summation of polyvinyl alcohol and HNTs are 10wt% in the mass fraction in the mixed liquor.
6. a kind of preparation method of novel galapectite/polyvinyl alcohol composite aerogel as described in claim 1, feature exist
In in the step 3, the mass fraction of the polyvinyl alcohol is 3wt%-7wt%, preferably 3wt%, the quality of the HNTs
Score is 3wt%-7wt%, preferably 7wt%.
7. a kind of preparation method of novel galapectite/polyvinyl alcohol composite aerogel as described in claim 1, feature exist
In the density of the PVA/HNTs composite aerogel for the crosslinking that the step 3 obtains is 0.04-0.17g/cm3, thermal conductivity be
0.02-0.04W m-1K-1, compression modulus 4.2-8.7MPa.
8. water-soluble borax saturated solution is in cross-linking polyvinyl alcohol, galapectite to prepare answering in PVA/HNTs composite aerogel
With.
9. PVA/HNTs composite aerogel the answering on building thermal insulation material of the crosslinking as described in any one of claim 1-3
With.
10. application of the PVA/HNTs composite aerogel being crosslinked as claimed in claim 9 on building thermal insulation material, feature
It is, the density of the PVA/HNTs composite aerogel is 0.04-0.17g/cm3, thermal conductivity is 0.02-0.04W m-1K-1, pressure
Contracting modulus is 4.2-8.7MPa.
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| CN201710910569.5A CN109575484A (en) | 2017-09-29 | 2017-09-29 | Novel galapectite/polyvinyl alcohol composite aerogel and its preparation method and application |
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