CN109650397A - A kind of method and aeroge preparing aerosil using the modified siliceous material of acidic materials - Google Patents
A kind of method and aeroge preparing aerosil using the modified siliceous material of acidic materials Download PDFInfo
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- CN109650397A CN109650397A CN201910144294.8A CN201910144294A CN109650397A CN 109650397 A CN109650397 A CN 109650397A CN 201910144294 A CN201910144294 A CN 201910144294A CN 109650397 A CN109650397 A CN 109650397A
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- siliceous material
- acidic materials
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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
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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
- C01B33/166—Preparation of silica xerogels by acidification of silicate in the presence of an inert organic phase
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
A kind of method and aeroge preparing aerosil using the modified siliceous material of acidic materials, is related to aeroge preparation technical field.The method for preparing aerosil using the modified siliceous material of acidic materials, it include: that will be reacted under conditions of 35~100 DEG C in the siliceous material solution of alkalinity with silica source, it is 6.5~7.5 that acidic materials are added after being cooled to room temperature and adjust pH value, and reaction obtains presoma.Wherein, siliceous material includes silicic acid or silicate；Solvent displacement is carried out to presoma using low boiling point organic solvent to cement out the moisture in presoma, is then dried.The biggish aerosil of specific surface area can be prepared in this method simple process.
Description
Technical field
The present invention relates to aeroge preparation technical fields, and in particular to a kind of modified siliceous material of utilization acidic materials
Prepare the method and aeroge of aerosil.
Background technique
Aeroge typically refers to nanometer scale ultramicro powder and mutually assembles composition nanoporous network structure, and in network hole
The lightweight nano solid material of gaseous state decentralized medium is full of in gap.Aeroge can be applied to aviation, heat-insulating, acoustical delay,
The fields such as environmental-protection adsorption.The formation mechanism of aeroge is the gel dehydration that early period should in the drying process formed, and is protected again
Card gel does not collapse, and substitutes the position of water in former gel to admit air into gel network.
Currently, aerosil usually is prepared using methyl orthosilicate, methyl orthosilicate as silicon source in the prior art, but
It is that the aeroge performance that is prepared is poor, smaller (the about 160m of specific surface area2/ g), it is not able to satisfy the field of higher requirement
Scape.
Summary of the invention
Aerosil is prepared using the modified siliceous material of acidic materials the purpose of the present invention is to provide a kind of
Method, the aerosil of large specific surface area can be prepared in this method simple process.
Another object of the present invention is to provide a kind of aeroges, with biggish specific surface area.
The present invention solves its technical problem and adopts the following technical solutions to realize.
The present invention proposes a kind of method for preparing aerosil using the modified siliceous material of acidic materials, packet
It includes:
It will be reacted under conditions of 35~100 DEG C in the siliceous material solution of alkalinity with silica source, be cooled to room
It is 6.5~7.5 that acidic materials are added after temperature and adjust pH value, and reaction obtains presoma；Siliceous material includes silicic acid or silicate；
Solvent displacement is carried out to presoma using low boiling point organic solvent to cement out the moisture in presoma, then into
Row drying.
A kind of aeroge, by the above-mentioned side for preparing aerosil using the modified siliceous material of acidic materials
Method is made.
The beneficial effect of the embodiment of the present invention is:
Siliceous material solution is alkaline solution, and silica source dissolves instead at 35~100 DEG C of temperature and alkaline condition
Silicic acid should be formed.Acidic materials provide hydrogen ion, and hydrogen ion replaces the salt ion of siliceous material to generate silicic acid, then
To presoma.After aqueous precursor gel, solvent displacement is carried out by the moisture in presoma to presoma using low boiling point organic solvent
It cements out, is then dried and may make organic solvent volatilization to retain the porous structure in presoma, to obtain sky
The aerosil of gap rate height, large specific surface area.
Detailed description of the invention
In order to illustrate the technical solution of the embodiments of the present invention more clearly, below will be to needed in the embodiment attached
Figure is briefly described, it should be understood that the following drawings illustrates only certain embodiments of the present invention, therefore is not construed as pair
The restriction of range for those of ordinary skill in the art without creative efforts, can also be according to this
A little attached drawings obtain other relevant attached drawings.
Fig. 1 is the SEM figure of the aerosil of the embodiment of the present application 3；
Fig. 2 is the SEM figure of the aerosil of the embodiment of the present application 6；
Fig. 3 is the SEM figure of the aerosil of the embodiment of the present application 10.
Specific embodiment
It in order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below will be in the embodiment of the present invention
Technical solution be clearly and completely described.The person that is not specified actual conditions in embodiment, according to normal conditions or manufacturer builds
The condition of view carries out.Reagents or instruments used without specified manufacturer is the conventional production that can be obtained by commercially available purchase
Product.
Using the modified siliceous material of acidic materials prepared by aerosil to a kind of of the embodiment of the present invention below
Method and aeroge be specifically described.
A method of aerosil is prepared using the modified siliceous material of acidic materials, comprising:
It will be reacted under conditions of 35~100 DEG C in the siliceous material solution of alkalinity with silica source, be cooled to room
It is 6.5~7.5 that acidic materials are added after temperature and adjust pH value, and reaction obtains presoma；Wherein, siliceous material includes silicic acid or silicon
Hydrochlorate.Illustratively, silicate can be sodium metasilicate, potassium silicate, calcium silicates etc..Wherein, silicate solutions are the water of silicate
Solution, silicate are hydrolyzed in water so that solution alkaline.Wherein, silicate solution is dissolved in acid solution by silicic acid and obtains.
Solvent displacement is carried out to presoma using low boiling point organic solvent to cement out the moisture in presoma, then into
Row drying.
Siliceous material solution is alkaline solution, in some embodiments, the pH value of siliceous material solution is 10~
14.Silica source dissolves reaction at 35~100 DEG C of temperature and alkaline condition and forms silicic acid.It is added after being cooled to room temperature acid
Substance, acidic materials provide hydrogen ion, and hydrogen ion replaces the salt ion of siliceous material to generate silicic acid, then obtains forerunner
Body.After aqueous precursor gel, solvent displacement is carried out to presoma using low boiling point organic solvent and displaces the moisture in presoma
Come, be then dried and may make organic solvent volatilization to retain porous structure in presoma, thus obtain voidage it is high,
The aerosil of large specific surface area.
In the present embodiment, drying mode is microwave drying, and after microwave enters gel and is absorbed, energy is in material
Dielectric internal conversion is at thermal energy, and the heat transfer direction of microwave drying is identical as organic solvent dispersal direction, and heat can uniformly seep
Thoroughly, have rate of drying big, the effect of uniform drying.
In the present embodiment, silica source includes one of white carbon black and silicon powder or a variety of.Wherein, white carbon black
It is silica with the main component in silicon powder, and is porous structure.The granularity of white carbon black and silicon powder is nanoscale,
Dissolution reaction forms silicic acid at 35~100 DEG C of temperature and alkaline condition.In some embodiments, siliceous material solution with
The reaction temperature of silica source is 50~90 DEG C.Creative thinking and test through applicant, siliceous material solution with
Silica reacts within this temperature range, and silica source can preferably dissolve thoroughly reaction and generate silicic acid.
Further, in the present embodiment, acidic materials include organic and or inorganic acids.In other words, acid
Matter can be organic acid, or inorganic acid, or the mixture of organic acid and inorganic acid.Wherein, inorganic acid includes
Any one of hydrochloric acid, sulfuric acid, phosphoric acid and nitric acid.Organic acid includes any one of acetic acid, citric acid and benzoic acid.
In addition, in the present embodiment, low boiling point organic solvent includes appointing in ethyl alcohol, pentane, methylene chloride or methanol
It is a kind of.
The boiling point of low boiling point organic solvent is lower, also can be by low boiling point in the lower situation of temperature when being dried
Organic solvent removal, to reach better drying effect.
A kind of aeroge, by the above-mentioned side for preparing aerosil using the modified siliceous material of acidic materials
Method is made.The aeroge that this method is prepared has porous structure, after tested, has biggish specific surface area and lesser leads
Hot coefficient.
Feature and performance of the invention are described in further detail with reference to embodiments.
Embodiment 1
The silicic acid calcium solution that pH value is 11 is mixed with silicon powder, is stirred under the conditions of 90 DEG C of temperature and keeps the temperature 2 hours,
It is kept stirring during heat preservation.
It is cooled to room temperature after heat preservation, hydrochloric acid is then slowly added into reaction system, control gel process pH is 6.5, is obtained
To aerogel precursor body.Aerogel precursor body is mixed with ethyl alcohol, is cemented out the moisture in presoma using ethyl alcohol, then
It carries out microwave drying and obtains aerosil, be recycled after the cooling recycling of the ethyl alcohol being evaporated.
Embodiment 2
The silicic acid calcium solution that pH value is 14 is mixed with silicon powder, is stirred under the conditions of 80 DEG C of temperature and keeps the temperature 2 hours,
It is kept stirring during heat preservation.
It is cooled to room temperature after heat preservation, sulfuric acid is then slowly added into reaction system, control gel process pH is 7.5, is obtained
To aerogel precursor body.Aerogel precursor body is mixed with pentane, is cemented out the moisture in presoma using pentane, then
It carries out microwave drying and obtains aerosil, be recycled after the cooling recycling of the pentane being evaporated.
Embodiment 3
The sodium silicate solution that pH value is 11.3 is mixed with silicon powder, stirred under the conditions of 35 DEG C of temperature and keeps the temperature 2 is small
When, it is kept stirring during heat preservation.
It is cooled to room temperature after heat preservation, acetic acid is then slowly added into reaction system, control gel process pH is 6.8, is obtained
To aerogel precursor body.It by aerogel precursor body and methane blended, utilizes, methane cements out the moisture in presoma, so
Microwave drying is carried out afterwards and obtains aerosil, is recycled after the cooling recycling of the methane being evaporated.
Embodiment 4
The potassium silicate solution that pH value is 13 is mixed with silicon powder, is stirred under the conditions of 50 DEG C of temperature and keeps the temperature 2 hours,
It is kept stirring during heat preservation.
It being cooled to room temperature after heat preservation, citric acid is then slowly added into reaction system, control gel process pH is 7.2,
Obtain aerogel precursor body.Aerogel precursor body is mixed with pentane, is cemented out the moisture in presoma using pentane, so
Microwave drying is carried out afterwards and obtains aerosil, is recycled after the cooling recycling of the pentane being evaporated.
Embodiment 5
The silicic acid calcium solution that pH value is 12.6 is mixed with silicon powder, stirred under the conditions of 70 DEG C of temperature and keeps the temperature 2 is small
When, it is kept stirring during heat preservation.
It is cooled to room temperature after heat preservation, benzoic acid is then slowly added into reaction system, control gel process pH is 7, is obtained
To aerogel precursor body.Aerogel precursor body is mixed with methanol, is cemented out the moisture in presoma using methanol, then
It carries out microwave drying and obtains aerosil, be recycled after the cooling recycling of the methanol being evaporated.
Embodiment 6
The sodium silicate solution that pH value is 12 is mixed with silicon powder, is stirred under the conditions of 90 DEG C of temperature and keeps the temperature 2 hours,
It is kept stirring during heat preservation.
It being cooled to room temperature after heat preservation, citric acid is then slowly added into reaction system, control gel process pH is 6.5,
Obtain aerogel precursor body.Aerogel precursor body is mixed with ethyl alcohol, is cemented out the moisture in presoma using ethyl alcohol, so
Microwave drying is carried out afterwards and obtains aerosil, is recycled after the cooling recycling of the ethyl alcohol being evaporated.
Embodiment 7
The sodium silicate solution that pH value is 12 is mixed with silicon powder, is stirred under the conditions of 40 DEG C of temperature and keeps the temperature 2 hours,
It is kept stirring during heat preservation.
It being cooled to room temperature after heat preservation, citric acid is then slowly added into reaction system, control gel process pH is 6.5,
Obtain aerogel precursor body.Aerogel precursor body is mixed with ethyl alcohol, is cemented out the moisture in presoma using ethyl alcohol, so
Microwave drying is carried out afterwards and obtains aerosil, is recycled after the cooling recycling of the ethyl alcohol being evaporated.
Embodiment 8
The silicate solution that pH value is 12.2 is mixed with silicon powder, stirred under the conditions of 100 DEG C of temperature and keeps the temperature 2 is small
When, it is kept stirring during heat preservation.
It is cooled to room temperature after heat preservation, hydrochloric acid and acetic acid is then slowly added into reaction system, control gel process pH is
7.2, obtain aerogel precursor body.Aerogel precursor body is mixed with ethyl alcohol, is displaced the moisture in presoma using ethyl alcohol
Come, then carry out microwave drying and obtain aerosil, is recycled after the cooling recycling of the ethyl alcohol being evaporated.
Embodiment 9
The sodium silicate solution that pH value is 13.5 is mixed with silicon powder, stirred under the conditions of 85 DEG C of temperature and keeps the temperature 2 is small
When, it is kept stirring during heat preservation.
It is cooled to room temperature after heat preservation, acetic acid is then slowly added into reaction system, control gel process pH is 7, is obtained
Aerogel precursor body.Aerogel precursor body is mixed with pentane, is cemented out the moisture in presoma using pentane, then into
Row microwave drying obtains aerosil, is recycled after the cooling recycling of the pentane being evaporated.
Embodiment 10
The sodium silicate solution that pH value is 13.2 is mixed with white carbon black, stirred under the conditions of 65 DEG C of temperature and keeps the temperature 2 is small
When, it is kept stirring during heat preservation.
It being cooled to room temperature after heat preservation, citric acid is then slowly added into reaction system, control gel process pH is 6.7,
Obtain aerogel precursor body.Aerogel precursor body is mixed with methylene chloride, is set the moisture in presoma using methylene chloride
It swaps out and, then carry out microwave drying and obtain aerosil, recycling after the cooling recycling of the methylene chloride being evaporated makes
With.
Test example
(1) aerosil that embodiment 3,6,10 is prepared is observed under a scanning electron microscope,
SEM figure is obtained, Fig. 1-Fig. 3 is please referred to.
Interpretation of result: from figure 3, it can be seen that after solid silica source and sodium metasilicate recombine, being evenly distributed, shape
At three-dimensional structure, reticular structure is obvious.There is no the solid particle of big partial size of silicon powder, illustrates solid silica source and sodium metasilicate
Fully reacting forms three-dimensional cavernous structure body.
(2) aerosil embodiment 1-10 being prepared carries out thermal coefficient, specific surface area, porosity
Test, result are recorded in table 1.
The performance test results of the aerosil of 1 embodiment 1-10 of table
Interpretation of result: from the results shown in Table 1, the aerosil of the embodiment of the present application all has biggish
Specific surface area and lesser thermal coefficient.It is found by comparative example 6 and embodiment 7, sodium silicate solution is alkalinity, reaction
The high embodiment 6 of temperature can produce the structure of higher specific surface area.
In conclusion a kind of of the embodiment of the present invention prepares silica airsetting using the modified siliceous material of acidic materials
The method of glue, since siliceous material solution is alkaline solution, silica source is molten at 35~100 DEG C of temperature and alkaline condition
Solution reaction forms silicic acid.Acidic materials provide hydrogen ion, and hydrogen ion replaces the sodium ion of siliceous material to generate silicic acid, after
And obtain presoma.After aqueous precursor gel, carrying out solvent displacement to presoma using low boiling point organic solvent will be in presoma
Moisture cements out, and is then dried and may make organic solvent volatilization to retain the porous structure in presoma, thus
The aerosil high to voidage, thermal coefficient is small.
Embodiments described above is a part of the embodiment of the present invention, instead of all the embodiments.Reality of the invention
The detailed description for applying example is not intended to limit the range of claimed invention, but is merely representative of selected implementation of the invention
Example.Based on the embodiments of the present invention, obtained by those of ordinary skill in the art without making creative efforts
Every other embodiment, shall fall within the protection scope of the present invention.
Claims (10)
1. a kind of method for preparing aerosil using the modified siliceous material of acidic materials characterized by comprising
It will be reacted under conditions of 35~100 DEG C in the siliceous material solution of alkalinity with silica source, after being cooled to room temperature
It is 6.5~7.5 that acidic materials, which are added, and adjust pH value, and reaction obtains presoma；The siliceous material includes silicic acid or silicate；
It carries out solvent displacement to the presoma using low boiling point organic solvent to cement out the moisture in the presoma, so
After be dried.
2. the method according to claim 1 for preparing aerosil using the modified siliceous material of acidic materials,
It is characterized in that, the silica source includes one of white carbon black and silicon powder or a variety of.
3. the method according to claim 1 for preparing aerosil using the modified siliceous material of acidic materials,
It is characterized in that, the pH value of the siliceous material solution is 10~14.
4. the method according to claim 1 for preparing aerosil using the modified siliceous material of acidic materials,
It is characterized in that, the acidic materials include organic and or inorganic acids.
5. the method according to claim 4 for preparing aerosil using the modified siliceous material of acidic materials,
It is characterized in that, the inorganic acid includes any one of hydrochloric acid, sulfuric acid, phosphoric acid and nitric acid.
6. the method according to claim 4 for preparing aerosil using the modified siliceous material of acidic materials,
It is characterized in that, the organic acid includes any one of acetic acid, citric acid and benzoic acid.
7. the method according to claim 1 for preparing aerosil using the modified siliceous material of acidic materials,
It is characterized in that, the low boiling point organic solvent includes any one of ethyl alcohol, pentane, methylene chloride or methanol.
8. the method according to claim 1 for preparing aerosil using the modified siliceous material of acidic materials,
It is characterized in that, the reaction temperature of the siliceous material solution and the silica source is 50~90 DEG C.
9. the method according to claim 1 for preparing aerosil using the modified siliceous material of acidic materials,
It is characterized in that, drying mode is microwave drying.
10. a kind of aeroge, which is characterized in that it utilizes the modified silicic acid of acidic materials by claim 1-9 is described in any item
The method that substance prepares aerosil is made.
Priority Applications (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910144294.8A CN109650397A (en) | 2019-02-27 | 2019-02-27 | A kind of method and aeroge preparing aerosil using the modified siliceous material of acidic materials |
| PCT/CN2019/094908 WO2020082782A1 (en) | 2018-10-22 | 2019-07-05 | Silica aerogel preparation method and aerogel prepared using said method |
| US17/238,187 US12017921B2 (en) | 2018-10-22 | 2021-04-22 | Silica aerogel preparation method and aerogel prepared using said method |
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| CN201910144294.8A CN109650397A (en) | 2019-02-27 | 2019-02-27 | A kind of method and aeroge preparing aerosil using the modified siliceous material of acidic materials |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020082782A1 (en) * | 2018-10-22 | 2020-04-30 | 天津摩根坤德高新科技发展有限公司 | Silica aerogel preparation method and aerogel prepared using said method |
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| CN102642842A (en) * | 2012-04-25 | 2012-08-22 | 浙江纳诺科技有限公司 | Method for preparing silicon dioxide aerogel by using acidic silica sol |
| WO2018170772A1 (en) * | 2017-03-22 | 2018-09-27 | 伊科纳诺（北京）科技发展有限公司 | Method for preparing silicon dioxide aerogel at atmospheric pressure and prepared silicon dioxide aerogel |
| EP3385225A1 (en) * | 2016-09-12 | 2018-10-10 | LG Chem, Ltd. | Method for manufacturing silica aerogel and silica aerogel manufactured thereby |
| CN109320882A (en) * | 2018-11-05 | 2019-02-12 | 天津摩根坤德高新科技发展有限公司 | Silica modified PVDF aeroge, preparation method and the aerogel product including it |
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2019
- 2019-02-27 CN CN201910144294.8A patent/CN109650397A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102642842A (en) * | 2012-04-25 | 2012-08-22 | 浙江纳诺科技有限公司 | Method for preparing silicon dioxide aerogel by using acidic silica sol |
| EP3385225A1 (en) * | 2016-09-12 | 2018-10-10 | LG Chem, Ltd. | Method for manufacturing silica aerogel and silica aerogel manufactured thereby |
| WO2018170772A1 (en) * | 2017-03-22 | 2018-09-27 | 伊科纳诺（北京）科技发展有限公司 | Method for preparing silicon dioxide aerogel at atmospheric pressure and prepared silicon dioxide aerogel |
| CN109320882A (en) * | 2018-11-05 | 2019-02-12 | 天津摩根坤德高新科技发展有限公司 | Silica modified PVDF aeroge, preparation method and the aerogel product including it |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2020082782A1 (en) * | 2018-10-22 | 2020-04-30 | 天津摩根坤德高新科技发展有限公司 | Silica aerogel preparation method and aerogel prepared using said method |
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Application publication date: 20190419 |