CN110511425A - A kind of soft silicone aeroge and preparation method thereof - Google Patents
A kind of soft silicone aeroge and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/28—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2383/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2383/04—Polysiloxanes
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Abstract
A kind of soft silicone aeroge, density are 0.05~0.25gcm‑3, pore-size distribution is 50~2000nm, and compression modulus is 0.02~0.15MPa, and bending angle is more than 180 °.Preparation step is as follows: alkyltrialkoxysilaneand, dialkyl dialkoxy silicane, trialkyl alkoxy silane, cetyl trimethylammonium bromide, deionized water is miscible with molar ratio 1:0.1~0.6:0.05~0.1:0.01~0.05:10~30；It adds ammonium hydroxide and adjusts solution ph 9-10 formation gel, by gained gel in 40-90 DEG C of aging 4-24h；Gel after aging is impregnated with deionized water, removes unreacted substance；Soaked gel progress constant pressure and dry is obtained into polysiloxanes aeroge.The aeroge has preferable compression rebound degree, curvature.
Description
Technical field
The invention belongs to aeroge porous material preparation field more particularly to a kind of soft silicone aeroge and its systems
Preparation Method.
Background technique
Aerosil is a kind of new material with three-D nano-porous structure, have low-density (0.003~
0.8g·cm-3), high porosity (80~99.8%), high-specific surface area (200~1000m2·g-1), lower thermal conductivity (~
0.02W·m-1K-1) etc. properties, have in application fields such as aerospace, chemical industry, energy saving building, military affairs, communication, electronics, metallurgy
Very wide prospect.However aerosil is not used widely, this is primarily due to silica airsetting
The three-dimensional net structure that glue network structure is cross-linked to form by simple rigid Si-O-Si key, this structure are held under external force
Easy fracture is broken, and structure collapses lead to poor mechanical property.
United States Patent (USP) US7078359 B2, US8214980 B2 and Chinese patent CN1803602A, CN101318659A,
CN101671030A, CN101973752A improve the brittleness of aerosil using fiber as reinforced phase.But it is fine
Dimension diameter is more much bigger than aeroge aperture, and the network structure resulted in is uneven, and composite material haves the defects that certain.Separately
Outside, the compatibility of reinforced phase fibrous material and aeroge matrix also will affect the comprehensive performance of material.U.S. Meador et al. is adopted
With enhancing by polymer SiO2Aeroge, using polymer in SiO2Particle surface forms clad to improve the mechanical property of aeroge
Can, first in SiO2The upper special functional group's such as amino of gel surface modification, by immersing the gel of modification after exchange of solvent
Into the solvent of certain organic monomers, then causes polymerization and supercritical drying obtains the SiO of enhancing by polymer2Aeroge, such as
Polyureas enhances SiO2Aeroge, epoxy enhance SiO2Aeroge, polystyrene enhance SiO2Aeroge etc..But this method preparation
The big (> 0.4gcm of aeroge density-3), therefore solid phase conduction of heat is stronger, the higher (> 0.04Wm of thermal conductivity-1·k-1),
Aeroge lacks flexibility.
In addition, the preparation of aeroge generallys use supercritical drying, the high requirements on the equipment.Constant pressure and dry is simplest dry
Drying method, but aerogel structure collapsing of the constant pressure and dry because leading to preparation there are capillary force.To overcome constant pressure and dry to exist
This disadvantage, usually between constant pressure and dry hydrophobically modified is carried out to the surface of gel and with the organic solvent of low surface tension
It is replaced.But the problems such as modified method process replaced with solvent in this surface is cumbersome, low efficiency, big solvent-oil ratio.
Therefore, there is still a need for a kind of simple process, high-efficient production method prepare the airsetting glue material of excellent combination property
Material, pushes the scale application of aeroge.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of soft silicone aeroge, there is flexibility well,
With lesser density, network structure is relatively uniform.
In order to solve the above technical problems, technical solution provided by the invention is a kind of soft silicone aeroge, it is special
Sign is that the density of the aeroge is 0.05~0.25gcm-3, pore-size distribution is 50~2000nm, compression modulus 0.02
~0.15MPa, bending angle are more than 180 °.
The contact angle of the aeroge is 150~178 °.
The aeroge can absorb the organic liquid of 6-30 times of sole mass, and recycles organic liquid by fashion of extrusion,
It can be recycled more than 100 times.
The present invention also provides a kind of preparation methods for preparing soft silicone aeroge comprising following specific steps:
(1) by alkyltrialkoxysilaneand, dialkyl dialkoxy silicane, trialkyl alkoxy silane, cetyl three
Methyl bromide ammonium, deionized water are mixed with molar ratio 1:0.1~0.6:0.05~0.1:0.01~0.05:10~30 proportion
It is molten to obtain clear solution；
(2) ammonium hydroxide is added in clear solution and adjusts solution ph 9-10 formation gel, gained gel is old at 40-90 DEG C
Change 4-24h；
(3) gel after aging is impregnated with deionized water, removes unreacted substance；
(4) soaked gel progress constant pressure and dry is obtained into polysiloxanes aeroge.
Deionized water impregnates gel in the step (3), impregnates 4-8h every time, impregnates 3-5 times.
Drying temperature is 60~120 DEG C in the step (4), drying time 24-48h.
Alkyltrialkoxysilaneand described in step (1) is methyltrimethoxysilane, methyltriethoxysilane, second
Base trimethoxy silane, ethyl triethoxysilane, propyl trimethoxy silicane, propyl-triethoxysilicane, vinyl front three
Oxysilane, vinyltriethoxysilane, octyl trimethoxy silane, octyltri-ethoxysilane, cetyl trimethoxy
Base silane, hexadecyl, dodecyltrimethoxysilane, dodecyl triethoxysilane, octadecane
At least one of base trimethoxy silane, octadecyltriethoxy silane.
Dialkyl dialkoxy silicane described in step (1) is dimethyldimethoxysil,ne, dimethyl diethoxy
Silane, methylvinyldimethoxysilane, methyl vinyl diethoxysilane, aminomethyl phenyl dimethoxysilane, methyl
Diethylamino phenyl oxysilane, second, isobutyl dimethoxy silane, diisobutyl diethoxy silane, octyl methyl dimethoxy silicon
Alkane, octyl methyl diethoxy silane, Cyclohexyl Methyl Dimethoxysilane, in cyclohexyl methyl diethoxy silane at least
It is a kind of.
Trialkylsilane described in step (1) is trimethylmethoxysilane, trimethylethoxysilane, trimethyl chlorine
At least one of silane, trimethyl phenoxysilane.
The invention has the benefit that
1. the crosslink density of aeroge can be greatly lowered to improve the flexible of aeroge in preparation method of the invention
Property；Aerogel material skeleton structure contains a large amount of non-hydrolytic alkyl groups simultaneously, since alkyl group is in mistake close to each other
Repulsion can be generated in journey can also assign aeroge excellent flexibility.
2. preparation method of the invention can directly assign aeroge hydrophobicity, does not need to carry out exchange of solvent and surface changes
Property step, preparation efficiency increase substantially；Aeroge has macroporous structure simultaneously, and the capillary of normal pressure generation can be greatly lowered
Guan Li, to obtain the complete block aeroge of low-density under constant pressure and dry.
Detailed description of the invention
Fig. 1 is the microscopic appearance figure of polysiloxanes aeroge prepared by embodiment 1.
Fig. 2 is the compression rebound figure of polysiloxanes aeroge prepared by embodiment 2.
Fig. 3 is the bending figure of polysiloxanes aeroge prepared by embodiment 3.
Specific embodiment
For the above-mentioned technical solution for soft silicone aeroge and preparation method thereof, now had for embodiment
Body explanation.
The preparation method for preparing soft silicone aeroge of the invention comprising following specific steps:
(1) by alkyltrialkoxysilaneand, dialkyl dialkoxy silicane, trialkyl alkoxy silane, cetyl three
Methyl bromide ammonium, deionized water are mixed with molar ratio 1:0.1~0.6:0.05~0.1:0.01~0.05:10~30 proportion
It is molten to obtain clear solution；
(2) ammonium hydroxide is added in clear solution and adjusts solution ph 9-10 formation gel, gained gel is old at 40-90 DEG C
Change 4-24h；
(3) gel after aging is impregnated with deionized water, removes unreacted substance；
(4) soaked gel progress constant pressure and dry is obtained into polysiloxanes aeroge.
Deionized water impregnates gel in the step (3), impregnates 4-8h every time, impregnates 3-5 times.
Drying temperature is 60~120 DEG C in the step (4), drying time 24-48h.
Alkyltrialkoxysilaneand described in step (1) is methyltrimethoxysilane, methyltriethoxysilane, second
Base trimethoxy silane, ethyl triethoxysilane, propyl trimethoxy silicane, propyl-triethoxysilicane, vinyl front three
Oxysilane, vinyltriethoxysilane, octyl trimethoxy silane, octyltri-ethoxysilane, cetyl trimethoxy
Base silane, hexadecyl, dodecyltrimethoxysilane, dodecyl triethoxysilane, octadecane
At least one of base trimethoxy silane, octadecyltriethoxy silane.
Dialkyl dialkoxy silicane described in step (1) is dimethyldimethoxysil,ne, dimethyl diethoxy
Silane, methylvinyldimethoxysilane, methyl vinyl diethoxysilane, aminomethyl phenyl dimethoxysilane, methyl
Diethylamino phenyl oxysilane, second, isobutyl dimethoxy silane, diisobutyl diethoxy silane, octyl methyl dimethoxy silicon
Alkane, octyl methyl diethoxy silane, Cyclohexyl Methyl Dimethoxysilane, in cyclohexyl methyl diethoxy silane at least
It is a kind of.
Trialkylsilane described in step (1) is trimethylmethoxysilane, trimethylethoxysilane, trimethyl chlorine
At least one of silane, trimethyl phenoxysilane.
The soft silicone aeroge prepared by above-mentioned preparation method, the density of the aeroge is 0.05~
0.25g·cm-3, pore-size distribution is 50~2000nm, and compression modulus is 0.02~0.15MPa, and bending angle is more than 180 °.It is described
The contact angle of aeroge is 150~178 °.The aeroge can absorb the organic liquid of 6-30 times of sole mass, and passes through extruding
Mode recycles organic liquid, can be recycled more than 100 times.
Compound of the present invention is commercially available.
Embodiment 1
By methyltrimethoxysilane, dimethyldimethoxysil,ne, trimethylmethoxysilane, cetyl trimethyl
Ammonium bromide, which is dissolved in deionized water, obtains clear solution, wherein methyltrimethoxysilane, dimethyldimethoxysil,ne, front three
Methoxylsilane, cetyl trimethylammonium bromide molar ratio be 1:0.1:0.05:0.01:30；In the above solution plus
Enter ammonium hydroxide adjust solution ph be 9 formed gels, by gel 40 DEG C of agings for 24 hours；The good gel of aging is soaked with deionized water
Bubble impregnates 4h every time, impregnates 5 times, removes unreacted substance；Soaked gel is directly placed into progress normal pressure in baking oven to do
Dry, drying temperature is 60 DEG C, and drying time 48h obtains polysiloxanes aeroge.
The pore-size distribution for preparing polysiloxanes aeroge is 500~2000nm, density 0.05gcm-3, flexibility is good,
It is compressible, 240 °, compression modulus 0.02MPa can be bent, contact angle is 178 °；Sole mass 15- can be absorbed in the aeroge
30 times of organic liquid, and organic liquid is recycled by fashion of extrusion, it can be recycled 150 times.
Embodiment 2
By methyltrimethoxysilane, dimethyldimethoxysil,ne, trimethylmethoxysilane, cetyl trimethyl
Ammonium bromide, which is dissolved in deionized water, obtains clear solution, wherein methyltrimethoxysilane, dimethyldimethoxysil,ne, front three
Methoxylsilane, cetyl trimethylammonium bromide molar ratio be 1:0.6:0.1:0.05:10；It is added in the above solution
Ammonium hydroxide adjust solution ph be 10 formed gels, by gel 40 DEG C of agings for 24 hours；The good gel of aging is soaked with deionized water
Bubble impregnates 8h every time, impregnates 3 times, removes unreacted substance；Soaked gel is directly placed into progress normal pressure in baking oven to do
Dry, drying temperature is 120 DEG C, and drying time 48h obtains polysiloxanes aeroge.
The pore-size distribution for preparing polysiloxanes aeroge is 50~500nm, density 0.25gcm-3, flexibility is good, can
Compression can be bent 180 °, compression modulus 0.15MPa, and contact angle is 150 °；The aeroge can be absorbed 6-14 times of sole mass
Organic liquid, and by fashion of extrusion recycle organic liquid, can be recycled 300 times.
Embodiment 3
By ethyl trimethoxy silane, dimethyl diethoxysilane, trimethylethoxysilane, cetyl trimethyl
Ammonium bromide, which is dissolved in deionized water, obtains clear solution, wherein ethyl trimethoxy silane, dimethyl diethoxysilane, front three
Methoxylsilane, cetyl trimethylammonium bromide molar ratio be 1:0.2:0.06:0.03:20；In the above solution plus
Entering ammonium hydroxide to adjust solution ph is 9 formation gels, by gel in 90 DEG C of aging 4h；The good gel of aging is soaked with deionized water
Bubble impregnates 6h every time, impregnates 4 times, removes unreacted substance；Soaked gel is directly placed into progress normal pressure in baking oven to do
Dry, drying temperature is 80 DEG C, and drying time 36h obtains polysiloxanes aeroge.
It prepares polysiloxanes aeroge aperture and is distributed as 150~2000nm, density 0.12gcm-3, flexibility is good, can
Compression can be bent 360 °, compression modulus 0.08MPa, and contact angle is 168 °；Sole mass 10-25 can be absorbed in the aeroge
Organic liquid again, and organic liquid is recycled by fashion of extrusion, it can be recycled 200 times.
Embodiment 4
By vinyltriethoxysilane, methylvinyldimethoxysilane, trimethylethoxysilane, cetyl
Trimethylammonium bromide, which is dissolved in deionized water, obtains clear solution, wherein vinyltriethoxysilane, methyl ethylene diformazan
Oxysilane, trimethylethoxysilane, cetyl trimethylammonium bromide molar ratio be 1:0.3:0.07:0.04:15；In
It is 9 formation gels that ammonium hydroxide is added in above-mentioned solution and adjusts solution ph, by gel in 40 DEG C of aging 20h；By the good gel of aging
It is impregnated with deionized water, impregnates 5h every time, impregnated 5 times, remove unreacted substance；Soaked gel is directly placed into baking oven
Middle carry out constant pressure and dry, drying temperature are 100 DEG C, and drying time 30h obtains polysiloxanes aeroge.
It prepares polysiloxanes aeroge aperture and is distributed as 100~1500nm, density 0.18gcm-3, flexibility is good, can
Compression can be bent 270 °, compression modulus 0.11MPa, and contact angle is 158 °；The aeroge can be absorbed 8-20 times of sole mass
Organic liquid, and by fashion of extrusion recycle organic liquid, can be recycled 200 times.
Embodiment 5
By octyl trimethoxy silane, dimethyl diethoxysilane, trim,ethylchlorosilane, cetyl trimethyl bromination
Ammonium, which is dissolved in deionized water, obtains clear solution, wherein octyl trimethoxy silane, dimethyl diethoxysilane, trimethyl chlorine
Silane, cetyl trimethylammonium bromide molar ratio are 1:0.5:0.08:0.04:12；Ammonium hydroxide is added in the above solution to adjust
Solution ph be 10 formed gels, by gel 40 DEG C of agings for 24 hours；The good gel of aging is impregnated with deionized water, is soaked every time
4h is steeped, impregnates 5 times, removes unreacted substance；Soaked gel is directly placed into baking oven and carries out constant pressure and dry, dry temperature
Degree is 110 DEG C, and drying time 25h obtains polysiloxanes aeroge.
It prepares polysiloxanes aeroge aperture and is distributed as 60~800nm, density 0.21gcm-3, flexibility is good, can press
Contracting can be bent 200 °, compression modulus 0.13MPa, and contact angle is 170 °；The aeroge can be absorbed 7-16 times of sole mass
Organic liquid, and organic liquid is recycled by fashion of extrusion, it can be recycled 230 times.
Embodiment 6
By hexadecyl trimethoxy silane, diisobutyl diethoxy silane, trimethyl phenoxysilane, cetyl
Trimethylammonium bromide, which is dissolved in deionized water, obtains clear solution, wherein hexadecyl trimethoxy silane, diisobutyl diethyl
Oxysilane, trimethyl phenoxysilane, cetyl trimethylammonium bromide molar ratio are 1:0.5:0.08:0.04:12；Upper
State in solution be added ammonium hydroxide adjust solution ph be 10 formed gels, by gel 40 DEG C of agings for 24 hours；The good gel of aging is used
Deionized water is impregnated, and impregnates 4h every time, is impregnated 5 times, is removed unreacted substance；Soaked gel is directly placed into baking oven
Constant pressure and dry is carried out, drying temperature is 110 DEG C, and drying time 25h obtains polysiloxanes aeroge.
It prepares polysiloxanes aeroge aperture and is distributed as 60~900nm, density 0.20gcm-3, flexibility is good, can press
Contracting can be bent 180 °, compression modulus 0.14MPa, and contact angle is 170 °；The aeroge can be absorbed 7-16 times of sole mass
Organic liquid, and organic liquid is recycled by fashion of extrusion, it can be recycled 210 times.
As shown in Figure 1, the aeroge network structure of preparation is relatively uniform；As shown in Figure 2, the compression and back of the aeroge of preparation
Bullet degree is fine；From the figure 3, it may be seen that the aeroge of preparation has good curvature.In conclusion the poly- silicon of flexibility prepared by the present invention
Oxygen alkane aeroge network structure is more uniform, has preferable compression rebound degree, curvature.
Claims (9)
1. a kind of soft silicone aeroge, it is characterised in that the density of the aeroge is 0.05~0.25gcm-3, hole
Diameter is distributed as 50~2000nm, and compression modulus is 0.02~0.15MPa, and bending angle is more than 180 °.
2. soft silicone aeroge according to claim 1, it is characterised in that the contact angle of the aeroge is 150
~178 °.
3. soft silicone aeroge according to claim 1, it is characterised in that the aeroge can absorb itself matter
The organic liquid of 6-30 times of amount, and organic liquid is recycled by fashion of extrusion, it can be recycled more than 100 times.
4. the preparation method of any soft silicone aeroge of claim 1 or 3, it is characterised in that including following specific
Step:
(1) by alkyltrialkoxysilaneand, dialkyl dialkoxy silicane, trialkyl alkoxy silane, cetyl trimethyl
Ammonium bromide, deionized water carry out miscible obtain with molar ratio 1:0.1~0.6:0.05~0.1:0.01~0.05:10~30 proportion
To clear solution；
(2) ammonium hydroxide is added in clear solution and adjusts solution ph 9-10 formation gel, by gained gel in 40-90 DEG C of aging 4-
24h；
(3) gel after aging is impregnated with deionized water, removes unreacted substance；
(4) soaked gel progress constant pressure and dry is obtained into polysiloxanes aeroge.
5. the preparation method of soft silicone aeroge described in claim 3, it is characterised in that deionization in the step (3)
Water logging foaming gel impregnates 4-8h every time, impregnates 3-5 times.
6. the preparation method of soft silicone aeroge described in claim 3, it is characterised in that dry temperature in the step (4)
Degree is 60~120 DEG C, drying time 24-48h.
7. the preparation method of soft silicone aeroge described in claim 3, it is characterised in that alkyl described in step (1)
Trialkoxy silane is methyltrimethoxysilane, methyltriethoxysilane, ethyl trimethoxy silane, ethyl triethoxy
Silane, propyl trimethoxy silicane, propyl-triethoxysilicane, vinyltrimethoxysilane, vinyl triethoxyl silicon
Alkane, octyl trimethoxy silane, octyltri-ethoxysilane, hexadecyl trimethoxy silane, cetyl triethoxysilicane
Alkane, dodecyltrimethoxysilane, dodecyl triethoxysilane, octadecyl trimethoxysilane, octadecyl three
At least one of Ethoxysilane.
8. the preparation method of soft silicone aeroge described in claim 3, it is characterised in that dioxane described in step (1)
Base dialkoxy silicane be dimethyldimethoxysil,ne, dimethyl diethoxysilane, methylvinyldimethoxysilane,
Methyl vinyl diethoxysilane, aminomethyl phenyl dimethoxysilane, aminomethyl phenyl diethoxy silane, diisobutyl diformazan
Oxysilane, diisobutyl diethoxy silane, octyl methyl dimethoxysilane, octyl methyl diethoxy silane, hexamethylene
At least one of ylmethyl dimethoxysilane, cyclohexyl methyl diethoxy silane.
9. the preparation method of soft silicone aeroge described in claim 3, it is characterised in that three alkane described in step (1)
Base silane be trimethylmethoxysilane, trimethylethoxysilane, trim,ethylchlorosilane, in trimethyl phenoxysilane extremely
Few one kind.
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| CN111732753A (en) * | 2020-06-04 | 2020-10-02 | 淮阴工学院 | Flexible polysiloxane aerogel and rapid preparation method thereof |
| CN111807368A (en) * | 2020-06-04 | 2020-10-23 | 淮阴工学院 | Preparation method of high-temperature-resistant ultralow-density silicon carbide nanotube aerogel |
| CN112708277A (en) * | 2020-12-23 | 2021-04-27 | 北京化工大学 | High-strength flexible polysiloxane aerogel and preparation method thereof |
| CN112897534A (en) * | 2021-01-27 | 2021-06-04 | 西南大学 | Phenyl-reinforced flexible silica aerogel, and preparation method and application thereof |
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| CN112897534A (en) * | 2021-01-27 | 2021-06-04 | 西南大学 | Phenyl-reinforced flexible silica aerogel, and preparation method and application thereof |
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