CN109987611A - A kind of preparation method of aeroge - Google Patents
A kind of preparation method of aeroge Download PDFInfo
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- CN109987611A CN109987611A CN201711486990.4A CN201711486990A CN109987611A CN 109987611 A CN109987611 A CN 109987611A CN 201711486990 A CN201711486990 A CN 201711486990A CN 109987611 A CN109987611 A CN 109987611A
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- aeroge
- microgravity
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- gel
- acid
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
- C01B33/157—After-treatment of gels
- C01B33/158—Purification; Drying; Dehydrating
- C01B33/1585—Dehydration into aerogels
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/16—Preparation of silica xerogels
- C01B33/163—Preparation of silica xerogels by hydrolysis of organosilicon compounds, e.g. ethyl orthosilicate
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/32—Thermal properties
Abstract
The invention discloses a kind of preparation methods of aeroge, which is characterized in that including colloidal sol step, gel step, microgravity centrifugal drying step.The present invention proposes to can be omitted the solvent swap step of gelinite, centrifugal drying processing is carried out to wet gel in microgravity environment, simplify aeroge drying process, it avoids the liquid in aeroge drying process in gel from generating huge capillary force and destroys aeroge nanoporous skeleton, improve aeroge microstructure, improve macro property, shortens the production cycle, widen application field, wide market.
Description
Technical field
The present invention relates to a kind of preparation methods of aeroge, belong to novel inorganic nano-porous materials field.
Technical background
The preparation process of aeroge mainly includes the preparation of wet gel and two processes of drying of wet gel, drying process pair
The performance of aeroge is most important.Liquid in wet gel nano aperture forms meniscus during to external migration, generates
Inside tensile stress, this tensile stress are related with the diameter of capillary.As the aeroge of inorganic non-crystalline material, it is difficult to ensure that capillary
Pipe absolute uniform, therefore the drying process of wet gel can cause to distort to gel skeleton, even result in skeleton and collapse.Common
For drying process there are some technical problems, constant pressure and dry is using low surface tension liquid to reduce capillary force, but cannot be disappeared
It removes；Volume change can occur for the phase transformation of liquid in freezing dry process, generate expansion or shrinkage stress to gel skeleton, may break
Bad gel skeleton；Although supercritical drying can completely eliminate capillary force, the production cycle is longer.
Microgravity environment refers to that under gravity the apparent weight of system is much smaller than the environment of its actual weight.Ground
Ball surface is 1G gravity environment, and space is in acceleration caused by vacuum state, gravity or other external force and is no more than 10-5~
10-4G, synthetic material is prepared under this environment can eliminate and settle lamination problem caused by gravity, improve phase interface problem etc..
Summary of the invention
It is an object of the invention to propose a kind of preparation method of aeroge.The study found that leading in the sol-gel stage
Addition low surface tension solvent is crossed, using the synergistic effect generated between solvent, the surface tension of mixed liquor can be reduced, in turn
Reduce the capillary force in drying process in gelinite.One aspect of the present invention reduces the capillary of mixed solution using the synergistic effect
On the other hand Guan Li utilizes microgravity environment, can further improve the mixed solvent and skeleton in wet gel nanometer hole on framework
Phase interface characteristic, can lead to mixed solvent can hardly soak gel skeleton, i.e., can no longer occur hair between solvent and skeleton
Tubule force phenomenon.Further under the action of following temperature field or centrifugal force field, mixed solvent can be made in no capillary force or micro-
It is removed from gelinite nanometer hole on framework under weak capillary force action, to complete the drying process of wet gel.The present invention is broken through
Ground environment prepares the bottleneck problem of aeroge, obtains that microstructure is controllable, aerogel material of macro property exceptional.
A kind of preparation method of aeroge, which comprises the following steps:
(1) organosilan, deionized water, organic solvent and acid catalyst are mixed colloidal sol step, obtain colloidal sol；
(2) base catalyst is added in gel step in the colloidal sol of step (1), and stirring, gel obtains gelinite；
(3) microgravity centrifugal drying step, under microgravity environment, the gelinite that step (2) is obtained carries out centrifugal drying, obtains
To aeroge；
The organosilan, deionized water, organic solvent, low surface tension solvent, acid catalyst, base catalyst molar ratio be
1:0.05~5:0.5~8:0~1:0.0025~0.5:0.0025~0.5.
Further, the step (3) is microgravity heat-drying step, specially under microgravity environment, by step
(2) the gelinite heat drying obtained, obtains aeroge.
Further, the microgravity environment is in freely falling body microgravity simulation system, parabolic flight microgravity mould
Intend system, water floats container microgravity simulation system, any in suspension type microgravity simulation system, gas suspension microgravity simulation system
It is realized in system.
Further, the microgravity environment is realized in spacecraft.
Further, the revolving speed of the centrifugal drying is 100~10000r/min.
Further, the organosilan is methyl orthosilicate, ethyl orthosilicate, methyltrimethoxysilane, methyl three
Ethoxysilane, dimethyldimethoxysil,ne, dimethyl diethoxysilane, ethyl trimethoxy silane, three ethoxy of ethyl
The mixture of one or more of base silane.
Further, the organic solvent be one of methanol, ethyl alcohol, isopropanol, the tert-butyl alcohol, ethylene glycol, glycerol or
It is a variety of.
Further, the low surface tension solvent is one of n-hexane, acetone, pentane, normal heptane or a variety of.
Further, the acid catalyst is one of hydrochloric acid, sulfuric acid, acetic acid, oxalic acid, nitric acid, hydrofluoric acid.
Further, the base catalyst is one of sodium hydroxide, potassium hydroxide, ammonium hydroxide etc..
It further, further include Aging Step and/or solvent swap step after the step (2) and before step (3)
And/or modification procedure.
Further, the heat drying is one of microwave heating, heat source contact heating.
The thermal coefficient of the aeroge as made from any of the above-described preparation method can be less than 0.01W/ (mK).
The visible light transmittance of the aeroge as made from any of the above-described preparation method can be greater than 95%.
Present invention firstly provides in microgravity environment realize to wet gel carry out centrifugal drying processing prepare aeroge, letter
Change aeroge drying process, avoids the liquid in aeroge drying process in gel from generating huge capillary force destruction aeroge and receive
Rice stephanoporate framework, improves aeroge microstructure, improves macro property, shortens the production cycle, widens application field, market prospects
It is wide.
Specific embodiment
In order to make the foregoing objectives, features and advantages of the present invention clearer and more comprehensible, below to specific reality of the invention
The mode of applying is described in detail.In the following description, numerous specific details are set forth in order to facilitate a full understanding of the present invention.But
The invention can be embodied in many other ways as described herein, and those skilled in the art can be without prejudice to this hair
Similar improvement is done in the case where bright intension, therefore the present invention is not limited to the specific embodiments disclosed below.
A kind of preparation method of aeroge, which comprises the following steps:
(1) organosilan, deionized water, organic solvent and acid catalyst are mixed colloidal sol step, obtain colloidal sol；
(2) base catalyst is added in gel step in the colloidal sol of step (1), and stirring, gel obtains gelinite；
(3) microgravity centrifugal drying step, under microgravity environment, the gelinite that step (2) is obtained carries out centrifugal drying, obtains
To aeroge；
The organosilan, deionized water, organic solvent, low surface tension solvent, acid catalyst, base catalyst molar ratio be
1:0.05~5:0.5~8:0~1:0.0025~0.5:0.0025~0.5.
The study found that liquid and nanoscale capillary wall in microgravity environment in the nano-pore of three-dimensional network gelinite
Contact angle close to 90 °, i.e., almost without wetting effect between liquid and gel skeleton, therefore, liquid is transported in gel skeleton
The process of moving can be omitted gelinite solvent swap step almost without frictional resistance under microgravity environment, because solvent is (special
Not low surface tension solvent) in microgravity environment and gel skeleton is without wetting effect, i.e. capillary force levels off to 0, because
This microgravity environment, which prepares aeroge, can greatly simplify preparation process；Centrifugal drying is produced using centrifuge rotor high speed rotation
Raw powerful centrifugal force acts on gelinite, and gelinite is fixed on centrifuge, i.e., gel skeleton is on centrifugation radius
Resultant force is zero, and the solvent in gel generates outside centrifugal force, therefore can significantly improve in wet gel liquid in three dimensional network
Migration rate in network gelinite, in the case where liquid and capillary wall point contact, quick unstressed separation avoids capillary
The generation of power protects gel three-dimensional network skeleton not to be destroyed, and drying efficiency is high, and process is short, and application prospect is huge.
Further, the step (3) is microgravity heat-drying step, specially under microgravity environment, by step
(2) the gelinite heat drying obtained, obtains aeroge.
In the present embodiment, the microgravity environment is in freely falling body microgravity simulation system, parabolic flight microgravity
Simulation system, water float container microgravity simulation system, suspension type microgravity simulation system, appoint in gas suspension microgravity simulation system
It is realized in one system.
In this way, microgravity environment is the simulation space environment under the conditions of earth, the simulation of freely falling body microgravity tower microgravity
System is by executing the movement of falling object in microgravity tower, to generate a kind of method of microgravity test environment, advantage
Be space microgravity environment simulation precision it is higher, it is safe and reliable, reusable, and the microgravity of three-dimensional space can be carried out
Experiment；
Parabolic flight microgravity simulation system is the method that microgravity environment is created using parabola maneuvering flight, and advantage is
The simulation precision of space microgravity environment is higher, and zero gravity airplane is reusable, can carry out the microgravity experiment of three-dimensional space；
It is by the buoyancy of water come the gravity of balancing mechanical arm itself that water, which floats container microgravity simulation system, floating by precisely adjusting
The buoyancy of power device makes upward water buoyancy and downward gravitational equilibrium suffered by object, generates the floating state of stochastic equilibrium, advantage
For the microgravity test that three-dimensional space may be implemented, and test period is unrestricted；
Suspension type microgravity simulation system is that aircraft self gravity is balanced by the vertical tension of hang spring, due to its structure phase
It to simple, and is easily achieved, therefore using extensively, principle is and to be offset using counterweight winged by rope mechanism and pulley blocks
The gravity of row device itself uses the gravity of hang spring system balance aircraft straight down, utilizes hang spring, pulley, guide rail, truss
Deng, and make hang spring pulling force be consistently equal to hang the gravity of aircraft using the control method of servo-actuated identical tension；
The method that gas suspension microgravity simulation system mainly passes through gas suspension lifts aircraft on smooth platform, that is, holds in the palm
Lifting force and gravity offset a kind of method to realize microgravity simulation, principle be by plane thrust air-bearing, will be by air pump
Gas after air chest divides is sprayed through plane thrust air-bearing, using gas pressure, floats test objective by air film
Aircraft, and the lubrication gas pressure by changing throttle orifice, offset self weight and the effect of load force always, make plane thrust axis
It is in the state of suspension, the frictional force and adhesion strength that at this moment axis is subject to are almost 0, so being supported on axial rotation on axis and axis
Completely freely, move freely aircraft on entire smooth platform, air bearing resistance can reach within 0.2N, and precision is very
Height, its advantage is that construction period is short, at low cost, precision is high, it is easy to accomplish and maintenance.By the size for designing plate thrust bearing
It can be realized up to several tons of aircraft microgravity simulation test, and experimental period is unrestricted, be by replacing interface unit
Recycling can be achieved, reliability and robustness are high, and it is adaptable, the structure of aircraft is not limited too much.
In the present embodiment, the microgravity environment is realized in spacecraft.
In this way, spacecraft includes the space in the space environment such as satellite, space station, carrier rocket, spaceship
Or aircraft.
In the present embodiment, the revolving speed of the centrifugal drying is 100~10000r/min.
In this way, the study found that too big revolving speed is not needed in microgravity environment can be by the solvent in gelinite
" getting rid of " comes out, and significantly improves efficiency, shortens process cycle.
In the present embodiment, the organosilan is methyl orthosilicate, ethyl orthosilicate, methyltrimethoxysilane, methyl
Triethoxysilane, dimethyldimethoxysil,ne, dimethyl diethoxysilane, ethyl trimethoxy silane, three second of ethyl
The mixture of one or more of oxysilane.
In the present embodiment, the organic solvent is one of methanol, ethyl alcohol, isopropanol, the tert-butyl alcohol, ethylene glycol, glycerol
Or it is a variety of.
In the present embodiment, the low surface tension solvent is one of n-hexane, acetone, pentane, normal heptane or more
Kind.
In the present embodiment, the acid catalyst is one of hydrochloric acid, sulfuric acid, acetic acid, oxalic acid, nitric acid, hydrofluoric acid.
In the present embodiment, the base catalyst is one of sodium hydroxide, potassium hydroxide, ammonium hydroxide etc..
It further include Aging Step and/or solvent displacement step in the present embodiment, after the step (2) and before step (3)
Rapid and/or modification procedure.In this way, the three-dimensional network frame strength of aeroge can be improved in Aging Step, change aperture；Solvent is set
Changing step can be improved drying efficiency；Modification procedure can be with directed change aeroge surface functional group, such as makes aeroge surface
With hydrophobic property.
In the present embodiment, the heat drying is one of microwave heating, heat source contact heating.In this way, in microgravity
Under the action of environment and temperature field, controlled by temperature, so that gelinite internal liquid slowly gasifies and outside diffusion mobility,
In the case where there is no capillary force, transformation of the liquid-solid boundary to gas-solid interface is completed, and then complete gelinite drying process.
The thermal coefficient of the aeroge as made from any of the above-described preparation method can be less than 0.01W/ (mK).
The visible light transmittance of the aeroge as made from any of the above-described preparation method can be greater than 95%.
Present invention firstly provides handling in microgravity environment wet gel centrifugal drying, simplify aeroge drying process,
It avoids the liquid in aeroge drying process in gel from generating huge capillary force and destroys aeroge nanoporous skeleton, improve gas
Gel microstructure improves macro property, shortens the production cycle, widens application field, wide market.
With specific embodiment, the present invention will be further described below, but protection scope is not limited by the following examples.
Embodiment 1:
(1) preparation of silica solution: being 1:0.05 by ethyl orthosilicate, deionized water, ethyl alcohol, n-hexane, hydrochloric acid in molar ratio:
0.5:1:2.5 × 10-3It is mixed, obtains silica solution；
(2) preparation of gel: it is 2.5 × 10 that molar ratio is added in the silica solution of step (1)-3Ammonium hydroxide, stirring, poured
Casting is into mold, gel；
(3) microgravity centrifugal drying: in freely falling body microgravity simulation system, step (2) is obtained using centrifugation apparatus
Wet gel centrifugal treating 50min, centrifugal rotational speed 100r/min obtain aeroge.
Embodiment 2:
(1) preparation of silica solution: being that 1:5:8:0.5 mixing is stirred by ethyl orthosilicate, deionized water, ethyl alcohol, hydrochloric acid in molar ratio
It mixes, obtains silica solution；
(2) ammonium hydroxide that molar ratio is 0.5, stirring, gel is added to the silica solution of step (1) in the preparation of gel；
(3) microgravity centrifugal drying: in parabolic flight microgravity simulation system, using Resistant heating equipment to step
(2) the wet gel contact heating processing 30min obtained, wire temperature is 100 DEG C, obtains aeroge.
Embodiment 3:
(1) preparation of silica solution: being 1:8:4:5 × 10 by ethyl orthosilicate, ethyl alcohol, deionized water, hydrochloric acid in molar ratio-3It is mixed
Close stirring；
(2) preparation of gel: it is 3 × 10 that molar ratio is continuously added into the silica solution of step (1)-3Ammonium hydroxide, stirring, gel；
(3) it microgravity centrifugal drying: floats in container microgravity simulation system in water, step (2) is obtained using centrifugation apparatus
Wet gel centrifugal treating 40min, centrifugal rotational speed 8000r/min obtain aeroge.
Embodiment 4:
(1) under gravity environment, the preparation of silica solution: being 1:6 by ethyl orthosilicate, ethyl alcohol, deionized water, hydrochloric acid in molar ratio:
4:4 × 10-3It is mixed；
(2) under gravity environment, the preparation of gel: it is 3 × 10 that molar ratio, which is added,-3Ammonium hydroxide be configured to silica solution, cast to
In mold, gel；
(3) microgravity centrifugal drying: in suspension type microgravity simulation system, step (2) is obtained using centrifugation apparatus wet
Gel centrifugal handles 10min, and centrifugal rotational speed 10000r/min obtains aeroge.
Embodiment 5:
(1) preparation of silica solution: being 1:6:4:5 × 10 by ethyl orthosilicate, ethyl alcohol, deionized water, hydrochloric acid in molar ratio-3It is mixed
Close stirring；
(2) preparation of gel: it is 3 × 10 that molar ratio is added into the silica solution of step (1)-3Ammonium hydroxide, gel；
(3) microgravity centrifugal drying: in gas suspension microgravity simulation system, step (2) is obtained using microwave equipment wet
Gel microwave heats 20min, and the temperature for controlling gelinite is 110 DEG C or so, obtains aeroge.
Following table is the performance parameter of the aeroge of embodiment 1-5:
Claims (10)
1. a kind of preparation method of aeroge, which comprises the following steps:
(1) organosilan, deionized water, organic solvent, low surface tension solvent and acid catalyst are mixed and are stirred by colloidal sol step
It mixes, obtains colloidal sol；
(2) base catalyst is added in gel step in the colloidal sol of step (1), and stirring, gel obtains gelinite；
(3) microgravity centrifugal drying step, under microgravity environment, the gelinite that step (2) is obtained carries out centrifugal drying, obtains
To aeroge；
The organosilan, deionized water, organic solvent, low surface tension solvent, acid catalyst, base catalyst molar ratio be
1:0.05~5:0.5~8:0~1:0.0025~0.5:0.0025~0.5.
2. a kind of preparation method of aeroge according to claim 1, which is characterized in that the step (3) is microgravity
Heat-drying step, specially under microgravity environment, the gelinite heat drying that step (2) is obtained obtains aeroge.
3. a kind of preparation method of aeroge according to claim 1, which is characterized in that the microgravity environment is certainly
Container microgravity simulation system is floated by falling bodies microgravity simulation system, parabolic flight microgravity simulation system, water, suspention declines
It is realized in any system in gravity simulation system, gas suspension microgravity simulation system.
4. a kind of preparation method of aeroge according to claim 1, which is characterized in that the microgravity environment is in sky
Between realize in aircraft.
5. a kind of preparation method of aeroge according to claim 1, which is characterized in that the revolving speed of the centrifugal drying is
100~10000r/min.
6. a kind of preparation method of aeroge according to claim 1, which is characterized in that the organosilan is positive silicic acid
Methyl esters, ethyl orthosilicate, methyltrimethoxysilane, methyltriethoxysilane, dimethyldimethoxysil,ne, dimethyl two
The mixture of one or more of Ethoxysilane, ethyl trimethoxy silane, ethyl triethoxysilane.
7. a kind of preparation method of aeroge according to claim 1, which is characterized in that the organic solvent be methanol,
One of ethyl alcohol, isopropanol, the tert-butyl alcohol, ethylene glycol, glycerol are a variety of.
8. a kind of preparation method of aeroge according to claim 1, which is characterized in that the low surface tension solvent is
One of n-hexane, acetone, pentane, normal heptane are a variety of.
9. a kind of preparation method of aeroge according to claim 1, which is characterized in that the acid catalyst be hydrochloric acid,
One of sulfuric acid, acetic acid, oxalic acid, nitric acid, hydrofluoric acid.
10. a kind of preparation method of aeroge according to claim 1, which is characterized in that the base catalyst is hydrogen-oxygen
Change one of sodium, potassium hydroxide, ammonium hydroxide etc.；A kind of preparation method of aeroge according to claim 1, feature exist
In after the step (2) and step (3) further includes before Aging Step and/or solvent swap step and/or modification procedure；
The preparation method of a kind of aeroge according to claim 2, which is characterized in that the heat drying is microwave heating, heat
One of source contact heating.
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| CN110586012A (en) * | 2019-09-18 | 2019-12-20 | 中国科学院上海硅酸盐研究所 | Aerospace aerogel preparation device |
| CN110713789A (en) * | 2019-09-24 | 2020-01-21 | 佛山市南海区里水镇经济促进局 | Adsorptive porous coating material and preparation method and application thereof |
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Application publication date: 20190709 |