CN108793172A - A kind of preparation method of aerosil - Google Patents
A kind of preparation method of aerosil Download PDFInfo
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- CN108793172A CN108793172A CN201810592642.3A CN201810592642A CN108793172A CN 108793172 A CN108793172 A CN 108793172A CN 201810592642 A CN201810592642 A CN 201810592642A CN 108793172 A CN108793172 A CN 108793172A
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- aerosil
- acetonitrile
- mix reagent
- wet gel
- preparation
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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
Abstract
The invention discloses a kind of preparation methods of aerosil.When preparation, TEOS, MTMS and APTES are first mixed into obtain mix reagent A, acetonitrile and deionized water are mixed into obtain mix reagent B;Then the temperature of mix reagent A and B are down to 0 DEG C;Two kinds of reagents after cooling are mixed again, and aging at room temperature, obtains wet gel;Wet gel after ethyl alcohol and acetonitrile solvent exchange, is first impregnated in the acetonitrile solution of hexamethylene diisocyanate, is then transferred in acetonitrile solution, and keep the temperature 72h at 70 DEG C, then wet gel is placed in acetonitrile solution and carries out exchange of solvent successively;Last wet gel passes through CO2Supercritical drying obtains the aerosil of isocyanates enhancing.Using the method in the present invention, it can effectively solve aeroge and prepare the technical issues of needing to carry out at -77 DEG C and be unfavorable for large-scale production.
Description
Technical field
The invention belongs to aeroge preparing technical fields, and in particular to a kind of preparation method of aerosil.
Background technology
Aerosil has low-density, high voidage, high-specific surface area, lower thermal conductivity, high thermal stability etc.
Characteristic, superior property make it be widely used in fields such as high-energy physics, catalysis, energy storage and space probations.
However, since itself intrinsic brittleness, hydrophily and poor mechanical property make its application be restricted.So far it is
Only, scientists have invented a variety of methods to improve the mechanical property of aeroge.Such as using containing long flexible chain
Silicon source is covered with polymer on the skeleton of aeroge by being crosslinked, initial gel is adulterated as skeleton etc. using fiber.It is total and
Yan Zhi is needed with connecting organic matter on the skeleton of aeroge, or by be crosslinked with the functional group on aeroge surface (such as-
NH2) react to improve the mechanical property of aeroge.
It has been reported that recently and connects functional group-NH on the skeleton of aeroge2It, can be anti-with isocyanates as reaction site
It answers, as reinforcing agent.The aerosil for the amino functional reported before is by methyl orthosilicate (TMOS) and 3-
What the hydrolysis and polycondensation of aminopropyl triethoxysilane (APTES) were got, reaction needs carry out at -77 DEG C, this is unfavorable
In large-scale production.In order to which silica mechanical property can be enhanced later, so design one kind preparing ammonia in a mild condition
The aerosil of base functionalization is very significant.
Invention content
For the above-mentioned prior art, the present invention provides a kind of preparation method of aerosil, to solve aeroge
Prepare the technical issues of needing to carry out at -77 DEG C and be unfavorable for large-scale production.
In order to achieve the above object, the technical solution adopted in the present invention is:A kind of system of aerosil is provided
Preparation Method, this method gel ageing step nearby carry out at 0 DEG C, include the following steps:
(1) ethyl orthosilicate, methyltrimethoxysilane and 3- aminopropyl triethoxysilanes are mixed simultaneously at room temperature
90~100min is stirred, mix reagent A is obtained;Acetonitrile and deionized water are mixed and stirred for 40~60min at room temperature, must be mixed
Reagent B;
(2) mix reagent A and mix reagent B are placed in ice water, its temperature is made to be down to 0 DEG C;
(3) by after cooling mix reagent A and mix reagent B mix, first stir 3~10min at 0 DEG C, then old at room temperature
Change 24~30h, obtains wet gel;
(4) wet gel obtained by step (3) is first placed in ethyl alcohol and acetonitrile solution and carries out exchange of solvent, swap time is each
3 days;
(5) wet gel after exchange of solvent first impregnates in the acetonitrile solution of hexamethylene diisocyanate to 20~
For 24 hours, it is then transferred in the acetonitrile solution that volume fraction is 40%~50%, and keeps the temperature 72h at 70 DEG C, then will be wet solidifying
Glue, which is placed in acetonitrile solution, carries out exchange of solvent, and processing is finally dried, and obtains the silica airsetting of isocyanates enhancing
Glue.
Based on the above technical solution, the present invention can also be improved as follows.
Further, ethyl orthosilicate in step (1), methyltrimethoxysilane and 3- aminopropyl triethoxysilanes rub
You are than being 1:1~7:1~4, the volume ratio of acetonitrile and deionized water is 20:5~6.
Further, the mass percent of hexamethylene diisocyanate is in the acetonitrile solution of hexamethylene diisocyanate
15wt%~30wt%.
Further, in solvent exchange procedure, the volume fraction of ethanol solution and acetonitrile solution used is 50%.
Further, the mode being dried in step (5) is CO2Supercritical drying.
Further, CO2Supercritical drying carries out under conditions of T=40 DEG C, P=12MPa.
The beneficial effects of the invention are as follows:
1. prepare in the prior art the aerosil of amino functional need under conditions of less than -70 DEG C into
Row, and to reach the temperature, difficulty is larger, and needs to use special installation during the reaction, is unfavorable for large-scale work
Industry metaplasia is produced.Hydrolysis and the more slow ethyl orthosilicate of polycondensation speed (TEOS) and methyl trimethoxy oxygroup silicon are utilized in the present invention
Alkane (MTMS) is used as common presoma, substitutes methyl orthosilicate (TMOS), at mild temperature can be with 3- ammonia third (near 0 DEG C)
Ethyl triethoxy silicane alkane reacts, and generates the aerosil of amino functional, considerably reduces production difficulty, and
And can be reacted with conventional chemical reaction device, be conducive to large-scale promotion application, be convenient for industrialized production.
2. using this hair after obtaining the silica airsetting of amino functional, by the silica airsetting of amino functional
With band-CH3Isocyanates mixing reacted ,-NH2It is crosslinked with isocyanates, aeroge skeleton will be enhanced, improve gas
The mechanical property of gel.Meanwhile unhydrolyzed-CH is introduced in aeroge3, make aeroge that there is hydrophobic performance, to improve gas
The adaptive capacity to environment of gel.
Description of the drawings
Fig. 1 is the preparating mechanism figure of aerosil;
Fig. 2 is the infrared spectrum and water contact angle schematic diagram of amido modified aerosil;
Fig. 3 is amido modified SiO2The SEM of aeroge schemes;
Fig. 4 is the SiO of HDI enhancings2The SEM of aeroge schemes;
Fig. 5 is that the stress-for the aerosil that amido modified aerosil and isocyanates enhance is answered
Become figure.
Specific implementation mode
The specific implementation mode of the present invention is described in detail below in conjunction with the accompanying drawings.
The physical-property parameter of agents useful for same is as follows in the present invention:
Ethyl orthosilicate:ρ=0.934g/ml, M=208.33g/mol;
Methyltrimethoxysilane:ρ=0.955g/ml, M=136.22g/mol;
3- aminopropyl triethoxysilanes:ρ=0.946g/ml, M=221.37g/mol.
Embodiment one
Molar ratio MTMS is prepared under the conditions of 0 DEG C:TEOS:APTES=1:1:1 aerosil, including following step
Suddenly:
(1) measure respectively ethyl orthosilicate, methyltrimethoxysilane and 3- aminopropyl triethoxysilanes 11.2ml,
7.2ml, 11.7ml are placed in container a, stir 100min at room temperature, obtain mix reagent A;Acetonitrile and deionized water are measured respectively
50ml, 12.5ml are placed in container b, stir 60min at room temperature, obtain mix reagent B;
(2) container a and container b are respectively placed in ice water, until mix reagent A therein and mix reagent B temperature drop
To 0 DEG C;
(3) the mix reagent B after cooling is quickly poured into mix reagent A, 3min is stirred at 0 DEG C first, to complete gel
Change;The solution after gelation is poured into aging in preprepared mold again and for 24 hours, obtains wet gel;
(4) wet gel of gained is first placed on the acetonitrile that ethanol solution, fraction that volume fraction is 50% are 50%
Exchange of solvent is carried out in solution, replaces fresh ethanol and acetonitrile, each 3 days of swap time daily;
(5) step (4) treated wet gel will be passed through first in the acetonitrile containing 15wt% hexamethylene diisocyanates
It is impregnated for 24 hours in solution;It is then transferred in the acetonitrile solution that volume fraction is 40%, and 72h is kept the temperature at 70 DEG C;Again will
Wet gel, which is placed in acetonitrile solution, carries out exchange of solvent, and swap time is 3 days, replaces fresh acetonitrile daily;
(6) by step, (5) treated that wet gel is put into supercritical extract instrument, at T=40 DEG C, P=12MPa experiments
Under the conditions of through CO2Supercritical drying obtains aerosil finished product.
Embodiment two
Molar ratio MTMS is prepared under the conditions of 0 DEG C:TEOS:APTES=7:1:4 aerosil, including following step
Suddenly:
(1) measure respectively ethyl orthosilicate, methyltrimethoxysilane and 3- aminopropyl triethoxysilanes 11.2ml,
50.4ml, 47ml are placed in container a, stir 100min at room temperature, obtain mix reagent A;Acetonitrile and deionized water are measured respectively
50ml, 15ml are placed in container b, stir 40min at room temperature, obtain mix reagent B;
(2) container a and container b are respectively placed in ice water, until mix reagent A therein and mix reagent B temperature drop
To 0 DEG C;
(3) the mix reagent B after cooling is quickly poured into mix reagent A, 10min is stirred at 0 DEG C first, to complete gel
Change;The solution after gelation is poured into aging 30h in preprepared mold again, obtains wet gel;
(4) wet gel of gained is first placed on the acetonitrile that ethanol solution, fraction that volume fraction is 50% are 50%
Exchange of solvent is carried out in solution, replaces fresh ethanol and acetonitrile, each 3 days of swap time daily;
(5) step (4) treated wet gel will be passed through first in the acetonitrile containing 30wt% hexamethylene diisocyanates
20h is impregnated in solution;It is then transferred in the acetonitrile solution that volume fraction is 60%, and 72h is kept the temperature at 70 DEG C;Again will
Wet gel, which is placed in acetonitrile solution, carries out exchange of solvent, and swap time is 3 days, replaces fresh acetonitrile daily;
(6) wet gel after exchange of solvent is put into supercritical extract instrument, under conditions of T=40 DEG C, P=12MPa into
Row CO2Supercritical drying obtains amido modified aerosil.
Embodiment three
Molar ratio MTMS is prepared under the conditions of 0 DEG C:TEOS:APTES=4:1:1 aerosil, including following step
Suddenly:
(1) measure respectively ethyl orthosilicate, methyltrimethoxysilane and 3- aminopropyl triethoxysilanes 8.9ml,
28.8ml, 11.7ml are placed in container a, stir 95min at room temperature, obtain mix reagent A;Acetonitrile and deionized water are measured respectively
50ml, 13.5ml are placed in container b, stir 50min at room temperature, obtain mix reagent B;
(2) container a and container b are respectively placed in ice water, until mix reagent A therein and mix reagent B temperature drop
To 0 DEG C;
(3) the mix reagent B after cooling is quickly poured into mix reagent A, 8min is stirred at 0 DEG C first, to complete gel
Change;The solution after gelation is poured into aging 28h in preprepared mold again, obtains wet gel;
(4) wet gel of gained is first placed on the acetonitrile that ethanol solution, fraction that volume fraction is 50% are 50%
Exchange of solvent is carried out in solution, replaces fresh ethanol and acetonitrile, each 3 days of swap time daily;
(5) step (4) treated wet gel will be passed through first in the acetonitrile containing 25wt% hexamethylene diisocyanates
It is impregnated for 24 hours in solution;It is then transferred in the acetonitrile solution that volume fraction is 40%, and 72h is kept the temperature at 70 DEG C;Again will
Wet gel, which is placed in acetonitrile solution, carries out exchange of solvent, and swap time is 3 days, replaces fresh acetonitrile daily;
(6) by step, (5) treated that wet gel is put into supercritical extract instrument, at T=40 DEG C, P=12MPa experiments
Under the conditions of through CO2Supercritical drying obtains aerosil finished product.
Example IV
Molar ratio MTMS is prepared under the conditions of 0 DEG C:TEOS:APTES=4:1:2 aerosil, including following step
Suddenly:
(1) measure respectively ethyl orthosilicate, methyltrimethoxysilane and 3- aminopropyl triethoxysilanes 11.2ml,
28.8ml, 23.5ml are placed in container a, stir 90min at room temperature, obtain mix reagent A;Acetonitrile and deionized water are measured respectively
50ml, 12ml are placed in container b, stir 60min at room temperature, obtain mix reagent B;
(2) container a and container b are respectively placed in ice water, until mix reagent A therein and mix reagent B temperature drop
To 0 DEG C;
(3) the mix reagent B after cooling is quickly poured into mix reagent A, 10min is stirred at 0 DEG C first, to complete gel
Change;The solution after gelation is poured into aging 25h in preprepared mold again, obtains wet gel;
(4) wet gel of gained is first placed on the acetonitrile that ethanol solution, fraction that volume fraction is 50% are 50%
Exchange of solvent is carried out in solution, replaces fresh ethanol and acetonitrile, each 3 days of swap time daily;
(5) step (4) treated wet gel will be passed through first in the acetonitrile containing 20wt% hexamethylene diisocyanates
22h is impregnated in solution;It is then transferred in the acetonitrile solution that volume fraction is 40%, and 72h is kept the temperature at 70 DEG C;Again will
Wet gel, which is placed in acetonitrile solution, carries out exchange of solvent, and swap time is 3 days, replaces fresh acetonitrile daily;
(6) by step, (5) treated that wet gel is put into supercritical extract instrument, at T=40 DEG C, P=12MPa experiments
Under the conditions of through CO2Supercritical drying obtains aerosil finished product.
Interpretation of result
What Fig. 1 was provided is aeroge preparating mechanism figure, and silicon source-ethyl orthosilicate containing relative inertness is used in the present invention
(TEOS), while methyltrimethoxysilane (MTMS) methyl that is stayed in after sol-gel on aeroge skeleton improves gas
The hydrophobic performance of gel product, the ratio by regulating and controlling silicon source realizes prepares uniform amido modified SiO in a mild condition2
Aeroge, and on this basis with the crosslinked SiO2 aeroges of hexamethylene diisocyanate (HDI).
In order to investigate the combination situation of APTES and presoma, it is dried place after wet gel carries out exchange of solvent
Reason, obtains a kind of amido modified aerosil.Fig. 2 be amido modified aerosil infrared spectrum and
Water contact angle schematic diagram.It was found from the figure that 783.5cm-1Place corresponds to the asymmetric stretching vibration peak of Si-C, 691cm-1With
1570cm-1The respectively stretching vibration peak of the flexural vibrations peak of N-H and N-H shows the successful scion grafting of amino group in aeroge
Skeleton on.1035cm-1And 1131cm-1Place is the bending vibration of Si-O-Si groups, 1400cm-1And 2950cm-1Place corresponds to
The flexural vibrations peak of C-H, 765cm-1And 1265cm-1Place corresponds to the peak position of Si-C, shows there is methyl base on the skeleton of aeroge
The presence of group, it is inferred that aeroge has hydrophobic performance.It can be seen that with the change of MTMS and TEOS molar ratios, when
MTMS compares for 7 with 1 with the molar ratio of TEOS, and the peak position of Si-C and the peak position of C-H are more obvious in infrared spectrum.Illustrate with
The raising of MTMS contents, surface Si-CH in aeroge network3Quantity increase, show when the molar ratio of MTMS and TEOS be 7 when
Aeroge has better hydrophobic performance.It can be seen from the figure that when the molar ratio of MTMS and TEOS is 1, amido modified two
The contact angle of silica aerogel is 20.5 °, which is less than 90 °, illustrates that this aeroge is hydrophilic;When MTMS's and TEOS
When molar ratio is 7, the contact angle of amido modified aerosil is 155.7 °, which is more than 150 °, illustrates this gas
Gel shows super-hydrophobic characteristic.Main cause amount of MTMS in being to increase silicon source can improve airsetting after hydrolysis, polycondensation
Glue surface-CH3Content, while the content of aeroge surface-OH is also opposite reduces.Thus the hydrophobic performance of aeroge entirety obtains
To prodigious raising, stability enhancing in the environment.
Fig. 3 is amido modified SiO2The SEM of aeroge schemes, it can be seen that amido modified SiO2The net of aeroge
Network skeleton is uniform, is the network structure of pearl chain.Fig. 4 is the SiO of HDI enhancings2The SEM of aeroge schemes, it can be seen that
It is wrapped by organic polymer on the nanometer skeleton of aeroge, before crosslinking, the introducing of organic polymer makes aeroge
The contact area of secondary becomes larger, and network skeleton is thicker, and aeroge still keeps tridimensional network.
Fig. 5 is that the stress-for the aerosil that amido modified aerosil and isocyanates enhance is answered
Become figure.There it can be seen that the stress-strain curve of aeroge can be divided into three phases:The elastic deformation stage surrenders rank
Section (plastic deformation), densification stage.As can be seen from the figure the limit fracture deformation of amido modified aerosil
It is 48.9%, and the limit fracture deformation of the aeroge sample after organic matter crosslinking is respectively 70.5% and 66.2%.From stress-
Strain figure can calculate the silica gas of the amido modified aerosil of sample and the enhancing of different content organic matter
The Young's modulus of gel is respectively 5.73MPa, 51.59MPa (embodiment three) and 108.12MPa (example IV).Thus three
The specific modulus (Young's modulus/density) of sample calculates respectively 68.21,185.62 and 444.93.The organic polymer of preparation
The crosslinked SiO of object2The needs that aeroge maximum specific modulus (density/Young's modulus) is 444.93 and conventional method is reported are dry
It is prepared in ice/acetone mixing bath (- 77 DEG C), then crosslinked SiO2The specific modulus (~483.23) of aeroge is close.
Although being described in detail to the specific implementation mode of the present invention in conjunction with attached drawing, should not be construed as special to this
The restriction of the protection domain of profit.In range described by claims, those skilled in the art are without creative work
The various modifications and deformation that can make still belong to the protection domain of this patent.
Claims (6)
1. a kind of preparation method of aerosil, which is characterized in that include the following steps:
(1) ethyl orthosilicate, methyltrimethoxysilane and 3- aminopropyl triethoxysilanes are mixed and stirred at room temperature
90~100min obtains mix reagent A;Acetonitrile and deionized water are mixed and stirred for 40~60min at room temperature, obtain mix reagent
B;
(2) mix reagent A and mix reagent B are placed in ice water, its temperature is made to be down to 0 DEG C;
(3) by after cooling mix reagent A and mix reagent B mix, prior to 0 DEG C at stir 3~10min, then at old at room temperature
Change 24~30h, obtains wet gel;
(4) wet gel obtained by step (3) is first placed in ethyl alcohol and acetonitrile solution and carries out exchange of solvent, each 3 days of swap time;
(5) wet gel after exchange of solvent first impregnates in the acetonitrile solution of hexamethylene diisocyanate to 20~for 24 hours,
It is then transferred in the acetonitrile solution that volume fraction is 40%~50%, and keeps the temperature 72h at 70 DEG C, then wet gel is set
Exchange of solvent is carried out in acetonitrile solution, processing is finally dried, and obtains the aerosil of isocyanates enhancing.
2. the preparation method of aerosil according to claim 1, it is characterised in that:Positive silicic acid in step (1)
The molar ratio of ethyl ester, methyltrimethoxysilane and 3- aminopropyl triethoxysilanes is 1:1~7:1~4, acetonitrile and deionization
The volume ratio of water is 20:5~6.
3. the preparation method of aerosil according to claim 1, it is characterised in that:The hexa-methylene two is different
The mass percent of hexamethylene diisocyanate is 15wt%~30wt% in the acetonitrile solution of cyanate.
4. the preparation method of aerosil according to claim 1, it is characterised in that:In solvent exchange procedure,
The volume fraction of ethanol solution and acetonitrile solution used is 50%.
5. the preparation method of aerosil according to claim 1, it is characterised in that:In step (5) at drying
The mode of reason is CO2Supercritical drying.
6. the preparation method of aerosil according to claim 5, it is characterised in that:CO2Supercritical drying is in T
=40 DEG C, carry out under conditions of P=12MPa.
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CN110105925A (en) * | 2019-05-21 | 2019-08-09 | 温州大学 | Cetylamine/silicon dioxide composite shape-stabilized phase phase-change material preparation method |
CN111101819A (en) * | 2019-12-11 | 2020-05-05 | 石家庄铁道大学 | Preparation method of hydrophobic silica aerogel heat-insulation glass |
CN111924850A (en) * | 2020-07-08 | 2020-11-13 | 南京工业大学 | Preparation method of polymer cross-linking modified spherical silica aerogel material |
CN113912903A (en) * | 2021-10-21 | 2022-01-11 | 中建材科创新技术研究院(山东)有限公司 | Preparation method of large-size transparent silicon dioxide aerogel block |
CN114478983A (en) * | 2022-01-26 | 2022-05-13 | 王永涛 | Preparation method of pre-polymerized resin and coating composition |
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Cited By (8)
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CN111101819A (en) * | 2019-12-11 | 2020-05-05 | 石家庄铁道大学 | Preparation method of hydrophobic silica aerogel heat-insulation glass |
CN111101819B (en) * | 2019-12-11 | 2021-07-20 | 石家庄铁道大学 | Preparation method of hydrophobic silica aerogel heat-insulation glass |
CN111924850A (en) * | 2020-07-08 | 2020-11-13 | 南京工业大学 | Preparation method of polymer cross-linking modified spherical silica aerogel material |
CN113912903A (en) * | 2021-10-21 | 2022-01-11 | 中建材科创新技术研究院(山东)有限公司 | Preparation method of large-size transparent silicon dioxide aerogel block |
CN114478983A (en) * | 2022-01-26 | 2022-05-13 | 王永涛 | Preparation method of pre-polymerized resin and coating composition |
CN114478983B (en) * | 2022-01-26 | 2024-02-06 | 上海特锦供应链管理有限公司 | Preparation method of pre-polymerized resin and coating composition |
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