Journal of Sol-Gel Science and Technology

https://doi.org/10.1007/s10971-022-05741-z

ORIGINAL PAPER: NANO-STRUCTURED MATERIALS (PARTICLES, FIBERS,

COLLOIDS, COMPOSITES, ETC.)

Recyclable thermo-insulating panels made by reversible gelling of

dispersed silica aerogel microparticles
Kun Zhang1 Tailing Li1 Zengzi Wang1 Zhizhi Sheng1 Xuetong Zhang
● ● ● ●
1,2

Received: 16 May 2021 / Accepted: 8 February 2022

© The Author(s), under exclusive licence to Springer Science+Business Media, LLC, part of Springer Nature 2022

Abstract
Hydrophobic silica aerogel composite materials are considered as one of the most promising thermal insulation materials in
energy-saving buildings. With the increasing negative effect on the environment of construction waste, it is necessary to
develop an effectively recyclable thermal aerogel material for the building industry. In this work, we firstly employed a
reversible gelling of hydrophobic silica aerogel microparticles dispersed with methyl cellulose surfactant (MCS) to prepare
recyclable thermo-insulating panels (RTIP). The RTIP, with low bulk density (<0.05 g/m3) and thermal conductivity
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(0.027 W/(mK) at 20 °C), has a splintering mass loss of the composite material as low as 1% after 2 h continuous high-
frequency oscillation, which was attributed to the rigid support of gelatinized MCS layers. Through mechanical mixing to re-
dissolving in water, the reproducible RTIP can be obtained by the same gelling and drying process, with fairly stable
hydrophobicity and thermal conductivity after 10 cycles. The strategy demonstrated here provides a new paradigm for
developing environmentally-friendly materials for thermal-insulating buildings.

Graphical abstract

Keywords Surface wetting Composites Recyclable Thermal insulation

● ● ●

Supplementary information The online version contains

supplementary material available at https://doi.org/10.1007/s10971-
022-05741-z.

* Xuetong Zhang
[email protected]
2
Division of Surgery and Interventional Science, University
1
Suzhou Institute of Nano-Tech and Nano-Bionics, Chinese College London, London NW3 2PF, UK
Academy of Sciences, Suzhou 215123, P.R. China
 Journal of Sol-Gel Science and Technology

Highlights
● A simple strategy was developed to prepare a highly uniform and stable hydrophobic silica aerogel aqueous solution.
● Recyclable thermo-insulating panels exhibits high porosity, good mechanical strength, and low thermal conductivity
(0.027 W/(mK) at 20 °C).
● Recyclable thermo-insulating panels shows no obvious change in mechanical properties and thermal conductivity after
five recyclable cycles.

1 Introduction microparticles because of the presence of adhesive and glass

fiber. Aerogel particles are used for processing various heat
Energy is the most essential requirement for social devel- insulation coatings, foaming boards, and other composite
opment and human survival, but with the unprecedented materials. However, the porous structure of the composite
growth of worldwide energy consumption, serious energy materials easily collapses after secondary drying, because the
crisis and environmental pollution problems have been trig- internal pores of silica aerogel are easily filled with organic
gered [1]. According to a survey by the International Energy solvents arising from the wet process. In addition, these
Agency (IEA), nearly 40% of global energy consumption aerogel composite materials can hardly be reused, which will
and 30% of total carbon dioxide emissions were caused by inevitably cause serious waste and limit their use in practical
building energy consumption [2]. Therefore, reducing applications. Therefore, it is urgent to exploit a convenient
building energy consumption and improving building energy recyclable silica aerogel thermal insulation material.
utilization are important breakthroughs for most countries to The hydrophobic silica aerogel can prevent the water phase
achieve carbon neutrality before 2060. To achieve this target, from entering the mesopores of the aerogel and can retain the
some new concepts of building energy-saving structural porous structure of the aerogel itself. Meanwhile, it can avoid
systems such as passive energy-saving houses [3] and zero- the loss of thermal insulation performance, thus extending the
emission buildings [4] were proposed recently. High- service life of the aerogel [18–21]. However, the dispersion of
performance thermal insulation materials, including mineral superhydrophobic solid microparticles in the water phase is a
wools, polyurethane foam, expanded polystyrene, cellulose, formidable task in the composite material preparation process.
aerogels, etc. [5], can effectively reduce the heat loss from The conventional methods include [12, 22–25]: 1. Hydro-
indoor to the external environment, which is an important philic modification of the particle surface to reduce the
part of constructing new energy-saving buildings. interfacial tension with water. 2. Addition of surfactants to the
Among these materials, aerogels possess unique nano- solvent or compatibilized micelles to achieve good dispersion.
scale porous structure and ultra-high porosity [6], and a 3. Use of high-speed dispersion, ball milling, ultrasonic, and
lower density and smaller construction thickness can be other powerful dispersion methods in cooperation with sur-
realized with the same thermal insulation performance when factants or surface treatment to make dispersions. For this
aerogels have been used in the construction of buildings. purpose, surface chemical modification will affect the
The silica aerogel is one of the most widely studied aerogels hydrophobic properties of the material and reduce the thermal
due to its mature production technology. The colloidal silica insulation performance and service life of the resulting pro-
nanoparticles are connected by Si-O-Si bonds to form a ducts, while it is more feasible to disperse the hydrophobic
continuous and irregular network structure with nano ske- silica aerogel microparticles by utilizing an efficient surfactant
leton porosity that is filled with air medium [7, 8]. The combined with mechanical stirring.
unique nano-porous network structure endows it with many Herein, recyclable silica aerogel composite thermal-
excellent properties, such as high specific surface area insulation panels (RTIP) were fabricated using hydro-
(500–1200 m2/g), high porosity (80–99.8%), extremely low phobized silica aerogel microparticles via wetting and
density (~0.003 g/cm3), and high thermal insulation (ca. dispersion using methyl cellulose surfactant (MCS).
0.015 W/mK) with tunable surface chemistry [8–10]. Firstly, a uniform and stable aqueous dispersion of silica
Generally, silica aerogel thermal insulation materials can aerogel without affecting the microstructure and perfor-
be divided into aerogel felt, aerogel particle, and aerogel plate mance was prepared from a mixture of a small amount of
[11–16]. The aerogel felt can be produced by mixing various MCS with the massive hydrophobic silica aerogel
types of glass fiber felt with silica sol, but the production microparticles. Secondly, the creamy-white dispersion
process is cumbersome and time-consuming, and its was gelatinized at low temperature and dried at high
mechanical properties are poor [17]. The thermal conductivity temperatures to obtain RTIP thermal insulation material.
and density of the rigid aerogel plate insulation material The microstructure of mesoporous RTIP was character-
obtained by adding organic adhesive or short glass fiber to ized by scanning electron microscopy (SEM) and nitrogen
silica aerogel is usually higher than that of aerogel physisorption via the Brunauer–Emmett–Teller (BET)
Journal of Sol-Gel Science and Technology

method. The thermal insulation performance and ensure that there were no bubbles in the dispersion sys-
mechanical property of RTIP with different mass ratios tem. Then the silica aerogel dispersion was transferred to
between silica aerogel and MCS were investigated. The a customized mold, with continuous shaking to ensure
recyclable property of RTIP was proved based on the filling, and left in an oven at 80 °C for gelation for 1 h.
morphology, contact angle (CA), and thermal con- Then the temperature was quickly raised to 120 °C for
ductivity characterization of the reproduced RTIP. drying over 12 h. When cooled to room temperature, the
silica aerogel composite thermal insulation panel were
obtained.
2 Experimental section
2.4 Characterization
2.1 Materials
The microtopography of samples was characterized by a
Tetraethoxysilane (TEOS, AR), hexane (AR) and hydro- cold field emission scanning electron microscope (SEM,
chloric acid (36–38 wt%) were purchased from Sinopharm Hitachi S-4800) at an acceleration voltage of 10–20 kV.
Chemical Reagent Co., Ltd. Methyl cellulose surfactant The stability of the aerogel dispersion was characterized
(MCS, 7000–10000 mPa·s, 2 wt.% in water at 20 °C) was through visible light transmittance of the lower mixed
purchased from TCI Chemicals Co., Ltd. Trimethyl- liquid after centrifuging at 3000 r/min for 10 minutes.
chlorosilane (TMCS, 98%) was purchased from Nanjing Contact angle values were determined using an optical
Habo Medical Technology Co., Ltd. All chemicals were contact angle measuring instrument (OCA 15 EC, Data
used as received without further purification. physics Instruments GmbH, Germany). The mean dia-
meter of synthesized silica particles was measured by a
2.2 Synthesis of hydrophobic silica aerogel wet particle size analyzer (HELOES BR, SYMPATEC
microparticles GmbH, Germany) The pore structure and size distribu-
tion of samples were evaluated by the BJH method
TEOS, ethanol, and diluted hydrochloric acid (0.01 M) (ASAP 2020, Micromeritics, USA). A rheometer (Haake
aqueous solution with a molar ratio of TEOS: ethanol: RS6000, Thermo Fisher Scientific, USA) was operated in
HCl = 1:4:1.2 were mixed at room temperature for 30 min a small amplitude oscillatory mode to determine gel
and refluxed at 130 °C for 8 h to obtain colorless silica temperature. Thermogravimetric analysis (TGA) was
precursor. The obtained precursor was uniformly mixed performed on a TG 209F1 Libra analyzer (NETZSCH)
with an equal volume of ethanol, and an appropriate amount under nitrogen atmosphere. The heating rate was set to
of ammonia was added to adjust pH and stirred for 2 min to 10 °C/min in the range of 25 to 900 °C. The specific
form an alcogel. After aging at 80 °C for 2 h, the alcogel surface area of samples was measured at 77 K by the
was pulverized with a colloid mill (JML-50, 2880 r/min). Brunauer–Emmett-Teller (BET) method based on the
The ground wet gel was transferred to an equal volume of amount of N2 adsorbed in the relative pressure range
TMCS/hexane modification solution, and phase separation from 0.05 < P/P0 < 0.3. Fourier transform infrared (FTIR)
occurred after hydrophobic reaction for 1 h at 50 °C. The spectroscopy (Nicolet 670iN10, USA) was employed in
modified organogel was taken out from the top layer of the the range of 400–4000 cm−1 for checking the bonding
mixed solution and washed for three times with hexane. between the silica and MCS species. Thermal con-
Finally, the modified organogel was dried at 150 °C for ductivity data at different temperatures (20–70 °C) of the
2 hours at ambient pressure to obtain hydrophobic silica sample (25 cm × 25 cm) were collected by a thermal
aerogel microparticles. conductivity measuring instrument (HFM 436/3/1E,
NETZSCH, Germany). The compression performance of
2.3 Fabrication of recyclable silica aerogel composite materials was evaluated by a universal mate-
composite thermal insulation panels (RTIP) rial testing machine (Instron 3365, USA). The thermal
insulation and cold insulation performance were char-
The appropriate amount of hydrophobic silica aerogel acterized using ceramic sheets heated by a high-precision
microparticles were mixed with a specified volume of DC stabilized power supply (2280S-60-3, Keithley,
MCS (1 wt. %) water solution under high-speed USA) as the thermal source and a cold table for liquid
mechanical stirring until no obvious particles could be nitrogen refrigeration as the cold source. The surface
found. The obtained slurry was stirred for 15 min at a temperature of the sample, thermal or cold source, and
stirring speed of 3000 r/min and ground by a colloid the environment were measured by a data logger (Key-
machine for 30 min to further improve the uniformity of sight34970A, KEYSIGHT, USA) with a K-type ther-
the dispersion, and then ultrasonicated for 30 min to mocouple. Data were recorded every 5 s.
 Journal of Sol-Gel Science and Technology

Fig. 1 a Schematic illustration

of silica aerogel surface
wettability change. b The
transmittance of centrifugal
hydrophobic silica aerogel
dispersion prepared by mixing
MCS with different
concentrations (inset picture:1%
mass ratio of MCS)

3 Results and discussion chains can meet the above requirements, and a uniform and
stable hydrophobic silica aerogel water-soluble dispersion
3.1 Preparation of RTIP can be successfully prepared. The transmittance of cen-
trifugal dispersions prepared by mixing with different
The hydrophobic silica aerogel microparticles (see digital concentrations of MCS was employed to characterize the
photograph Figure S1a) were synthesized according to our stability of the dispersions, as shown in Fig. 1b. It can be
previous work [26–28]. The water contact angle of silica seen from the transmittance results that as the mass ratio of
aerogel microparticles was nearly 150° (Figure S1b), MCS increased to 0.75%, the stability of the aerogel dis-
showing a superhydrophobic characteristic due to the sur- persion gradually improved, with the transmittance of cen-
face modification by TMCS. To evaluate the particle trifuged dispersion being below 10%. However, the
dimensions, laser particle size analyzer measurements were transmittance increased slightly when the concentration is
performed for ethanol suspension, revealing hydrodynamic greater than 1%, which may be due to the entanglement
diameters of 19 ± 2 μm (Figure S2). Therefore, the wetting between the excessive dispersant and the molecular chains
behavior of water on the aerogel surface must be modified adsorbed on the surface, leading to particle aggregation, and
to achieve stable dispersions with water. According to reduced stability of the dispersion. Therefore, for a disper-
Young’s equation [29, 30], the wetting process involves a sion with a 3% silica aerogel mass concentration, the opti-
three-phase interface: mal addition amount of MCS is 1%.
Cellulose-based hydrogel is a typical physical hydrogel,
σ sg ¼ σ sl þ σ lg cos θ ð1Þ
with most of the macromolecules in the MCS solution
σ sl  σ sg existing as randomly curled isolated molecular chains. When
cos θ ¼ ð2Þ the temperature is increased beyond the gel temperature, it
σ lg
begins to reconstitute the original solid-state structure due to
where σsg is solid surface tension, σsl is solid-liquid the dehydration between MCS molecular chains. In order to
interfacial tension, σlg is liquid surface tension, and θ is determine the gel temperature of the dispersion, the rheolo-
solid-liquid contact angle. Based on Eq. (2), a suitable gical measurement was performed on the MCS aqueous
surfactant can reduce the solid-liquid interfacial tension σlg solution [31]. At first, the linear viscoelastic zone of the MCS
without changing the σsg, thereby reducing the contact angle aqueous solution should be confirmed. As shown in Figure
as shown in the schematic of Fig. 1a. S3a, the storage modulus (G′) and loss modulus (G″) are
The surfactant candidate in this work needs to meet the unchanged in the range of 0.02 to 0.3 Pa, so the temperature-
following three criteria: 1. The hydrophilic and hydrophobic dependent oscillatory rheology data was collected at a shear
properties of the ends of the hydrophilic and hydrophobic stress of 0.1 Pa with the temperature changing from 30 °C to
chains need to be significantly different to satisfy the wet- 80 °C. It can be observed from the temperature-dependent
ting effect of the silica aerogel surface. 2. It must maintain oscillatory rheology curve (Figure S3b) that G′ increased
the stability of the dispersion system through steric hin- more rapidly than G″ when the temperature increased beyond
drance effects, hydrogen bonds, etc. 3. It can be gelatinized 65 °C, indicating that the MCS solution showed elastic
at low temperatures and can return to the solution-state after behavior and a gel was formed at this point. Consequently,
cooling. Considering the above factors, the high molecular thermally reversible gelation of MCS aqueous solutions of
weight MCS with distinct hydrophilic and hydrophobic macromolecules has been identified as the formation of a
Journal of Sol-Gel Science and Technology

Fig. 2 Design schematic of recyclable thermo-insulating panels

three-dimensional cross-linked network structure, which does The SEM images of RTIP with different aerogel con-
not involve the making or breaking of any new covalent centrations (0%, 65%, 70%, 80%, 90%, and 100%) are
bonds. Due to water being the main component, the gel presented in Fig. 3; the 0% and 100% represent pure MCS
temperature of the hydrophobic silica aerogel dispersion is foam and silica aerogel, respectively. It was clearly
set higher than this temperature but below 100 °C; therefore, demonstrated that a large amount of silica aerogel particles
the final gel temperature was chosen at 80 °C. was attached to the assembled layer structure of the sample
The MCS gel that formed at 80 °C for one hour was quickly with 65% aerogel concentration. It can be seen from the
frozen in liquid nitrogen to maintain the gel structure, and then SEM images that the abundance of silica aerogel micro-
freeze-dried to obtain MCS foam. The photograph and SEM particles gradually increased as the concentration of silica
images of MCS foam in Figure S4a, b shows that the milky aerogel was increased from 65% to 90%, as expected. When
white MCS foam was constructed of nanosheets stacked on top the content of aerogel increases to 90%, it is difficult to
of each other, and the length and width of the nanosheets can observe the layer structure formed by MCS. Instead of a
reach hundreds of microns. It is demonstrated that MCS is a large amount of aerogel microparticles, it is shown that the
satisfactory cross-linking agent to prepare the RTIP. microparticles are arranged in a lamellar pattern, indicating
From the perspective of raw materials, the interaction that the stratified structure of MCS foam has good adhesion
between point-to-point contact of silica particles leads to to the silica aerogel particles.
friable properties of silica aerogel, and it is necessary to add
a certain proportion of binder for practical use. The for- 3.2 Physical and chemical properties
mation of MCS macromolecule-quasi-cross-linkages in the
gel network is attributed to the secondary valance force as The porous structures of the different silica aerogel con-
the solvating power of the medium decreases. Through the centration composite RTIP are also confirmed by nitrogen
hydrophobization of the methoxy group, the MCS aerogel is adsorption-desorption measurement. The pore diameter
physically cross-linked to form a three-dimensional lamellar distribution plots are shown in Fig. 4a. These data indicate
structure [32, 33]. According to the microstructure of MCS that the mesopores of pure silica aerogel microparticles are
foam, the large-scale nanosheets are assembled by mainly mainly distributed around 25 nm, while the pore size dis-
surface-to-surface stacking or edge-to-edge lapping, which tributions of the aerogel composite samples are similar to
leads to an irreversible deformation under external force. As silica aerogel microparticles. The samples are mainly
illustrated in Fig. 2, combining the point-to-point contact mesoporous (10–40 nm) with some micropores (<2 nm) and
between the aerogel microparticles and the surface-to- macropores (>50 nm). This indicates that the aerogel com-
surface stacking in the MCS foam can transform a single posite material inherits the pore structure characteristics of
point-point contact into multiple point-surface contacts. aerogel microparticles. The nitrogen adsorption-desorption
Here, silica aerogel microparticles not only play a rigid isotherms of samples presented in Fig. 4b could be ascribed
support role between the filled MCS layers, but also to type IV based on the IUPAC classification, and the
improve the toughness of the aerogel itself, exhibiting good typical hysteresis loop of type H1 can be observed in all the
formability and excellent properties. data, revealing the homogeneous mesoporous structure of
 Journal of Sol-Gel Science and Technology

Fig. 3 a–f SEM images of silica

aerogel composites with
different aerogel concentrations:
0%, 65%, 70%, 80%, 90%, and
100%, respectively

all samples. In addition, the calculated specific surface area decrease of MCS foam (0.02 g/cm3) concentration, but
data is also shown in the inset in Fig. 4b. It can be seen that remains much lower than that of commercially available
as the aerogel content increases, the specific surface area of aerogel felt (200 kg/m3). The hydrophobic property of the
the sample gradually increases. aerogel composite material was also determined by CA test
The physical properties of RTIP, including thermal sta- as shown in Fig. 4e. These data indicate that the hydrophilic
bility, material density, and hydrophobicity, are shown in MCS foam (CA: 44°) was gradually transformed into a
Fig. 4c–e. The thermal stability of the insulation material is hydrophobic composite material (CA: 149°) after combin-
the critical basis for the selection of auxiliary insulation ing with 95% mass ratio of superhydrophobic silica
application scenarios. From the TG curve (Fig. 4c) of RTIP aerogels.
with different MCS content, it can be found that the sig- FT-IR analysis was performed to identify variations in
nificant mass loss occurred at 220 °C, so it is suitable for the the chemical environment of the silica aerogels after for-
application of thermal insulation in medium and low- mation of the MCS composites. The characteristic peaks of
temperature scenarios. The lower density of the thermal MCS appear at 3440 cm−1, 2925 cm−1, and 1074 cm−1 as
insulation material can bring about higher thermal insula- shown in the black line in Fig. 4f. The peak at 1100 cm−1 in
tion performance per unit mass. In Fig. 4d, the density of the spectrum of the aerogel (red line) is assigned to the
the silica aerogel composite materials increased with the stretching vibration of Si-O-Si. The characteristic peaks of
Journal of Sol-Gel Science and Technology

Fig. 4 Physical and chemical properties characterization of RTIP. a (e) CA tests of different silica aerogel concentration. f FT-IR spectra of
Pore size distributions, (b) nitrogen adsorption-desorption isotherms, MCS, silica aerogel, and RTIP
and BET data (inset graph), (c) TG curves, (d) materials density, and

the Si-C bonds are visible at 840 cm−1, which are intro- the components of RTIP were assembled by physical
duced by using TMCS as the modifier during the hydro- stacking instead of chemical bonding between them.
phobic modification process, while the peak at 2960 cm−1 is
attributed to the characteristic C–H stretching mode of 3.3 Mechanical strength of RTIP
surface methyl groups (-O-Si(CH3)3), which reflects the
molecular structure of a typical hydrophobic silica aerogel Good mechanical properties are crucial for thermal insula-
[34, 35]. From the infrared spectrum of RTIP in Fig. 4f, it is tion materials [36–40]. The compressive stress-strain curves
evident that all the characteristic peaks are from MCS and of the different silica aerogels composite thermal insulation
silica aerogel, and no new peaks appear. This suggests that materials are shown in Fig. 5a. The compressive stress of
 Journal of Sol-Gel Science and Technology

Fig. 5 Mechanical strength characterization of RTIP. a Compressive silica aerogel concentration composite materials; Stress-strain curves
stress-strain curves for different silica aerogel concentrations; (b) of 90% silica aerogel concentration composite materials under (c)
Oscillation mass loss comparison of commercial aerogel felt and 90% different maximum strains and (d) cycled 20 times under 30% strain

the material increases with increasing silica aerogel content almost overlap after 20 compression cycles, indicating that
from 65% to 95%. Specifically, when the aerogel content is the aerogel composite material has good compression
less than 70%, the material has good plasticity. As the performance.
aerogel content increases to 95%, the compressive strength
is significantly increased to 1.3 MPa, but brittle fracture will 3.4 Thermal insulation performance of RTIP
occur when the strain is 60%. Therefore, when the aerogel
content is between 75% and 95%, the material has both To evaluate the thermal insulation performance, three com-
higher toughness and higher strength. In addition, an mon thermal insulation materials were chosen as a reference
oscillation test using a fast disperser was employed to to show the advantages of RTIP. As shown in Fig. 6a, it can
characterize the stability of the silica aerogel composite be observed that the thermal conductivity of RTIP at 20 °C is
material in comparison to a commercially available silica as low as 0.027 W/mK and is lower than the other materials in
aerogel felt. The results (Fig. 5b) show that the mass loss the temperature range of 20–70 °C. Further, the thermal
(1%) of composite material is significantly smaller than that insulation performance in the actual use of RTIP was
of ordinary aerogel felt (>5%) after oscillating for two demonstrated in Fig. 6b. As a contrast, silica aerogel felt and
hours, indicating that silica aerogel composite material has RTIP were placed on the ceramic heating plate, and the sur-
higher stability. The compression cycle curves of the 90 % face temperature variation curve of the samples were obtained
aerogel composite material within the 5–40% strain range through heating and cooling the ceramic plate. It is found that
are presented in Fig. 5c; it is found that the sample shows a the surface temperature of RTIP is lower than the silica
continuous rebound trend and a high recovery capacity. aerogel felt during the entire heating and cooling process.
Figure 5d shows the loop performance test for the same Combined with the thermal infrared image of Fig. 6d, it is
sample under 30% deformation; the stress-strain curves obvious that the RTIP exhibits a superior thermal insulating
Journal of Sol-Gel Science and Technology

Fig. 6 a The thermal conductivity comparison of RTIP with other insulation materials at different temperatures. Temperature curve comparison of
(b) thermal and (c) cold insulation of RTIP and silica aerogel felt. d Thermal infrared image during thermal insulation test

property. Similarly, the cold insulation performance of RTIP the binding ability of the hydrophilic and hydrophobic
is also demonstrated in Fig. 6c. After placing the sample on a segments in water without additional crosslinking agents. It
cold plate at −170 °C for 50 minutes, the surface temperature can be found from the infrared spectrum of the RTIP (Fig.
of RTIP is nearly 50 °C higher than that of aerogel felt, 4f) that there are no new peaks or peak shifts before and
demonstrating that it also has better cold insulation properties. after compounding, indicating that the aerogel micro-
particles and MCS molecules form a simple physical mix-
3.5 Recycling of RTIP ture without chemical reaction, Hence, the aerogel
composite material can be simply mechanically stirred and
Degradable or recyclable thermal insulation materials can then dispersed in aqueous solution. By comparing the SEM
greatly alleviate the increasing negative effect of building images and the CA characterization before and after
materials on the environment [41–46]. The recycling of regeneration, it is shown that the recycled material retains
RTIP thermal insulation materials is presented in Fig. 7. At its micromorphology and hydrophobicity. The thermal
first, the RTIP was mixed with an appropriate amount of conductivity at 25 °C after ten recyclable cycles, as given in
water under vigorous stirring. The MCS component was Fig. 7d, does not exceed 0.030 W/mK, indicating that the
quickly dissolved and the material structure of RTIP was RTIP is an excellent environmentally-friendly thermal
collapsed. A layered solution was subsequently obtained, insulation material.
comprised of a top layer of aerogel microparticles and a
lower layer of MCS solution. It was continually
mechanically-agitated to form a silica aerogel dispersion 4 Conclusions
and followed by the drying process to regenerate a com-
posite material. Here, it is worth mentioning that the MCS In this work, based on the use of hydrophobic silica aerogel
gel process is a reversible gel process based on changes in microparticles with excellent thermal insulation
 Journal of Sol-Gel Science and Technology

Fig. 7 Recycling characterization of RTIP thermal insulation materials. a Recycling process, (b) SEM and (c) contact angle test change after
recycling, (d) the thermal conductivity (25 °C) stability after multiple recycling steps

Acknowledgements We gratefully acknowledge the support from the

performance and mature production technology, low-den-
National Key Research and Development Program of China
sity, low thermal conductivity, high mechanical perfor- (2016YFA0203301, 2020YFB1505703), the National Natural Science
mance, and highly hydrophobic recyclable aerogel Foundation of China (52173052), and the Royal Society Newton
composite thermal insulation panels were fabricated by a Advanced Fellowship (NA170184).
simple method. The MCS was firstly used as a dispersant
for superhydrophobic silica aerogel particles to prepare a Compliance with ethical standards
uniform and stable aerogel dispersion, due to the reversible
Conflict of interest The authors declare no competing interests.
temperature response of MCS aqueous solution. Simple
heat-treating and drying processes were subsequently used
Publisher’s note Springer Nature remains neutral with regard to
to transform the silica aerogel dispersions into recyclable jurisdictional claims in published maps and institutional affiliations.
silica aerogel composite panels (RTIP). The SEM and BET
characterization show that the RTIP has a uniform meso- References
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