[go: up one dir, main page]

CN119349588A - A kind of aerogel material and its preparation method and application - Google Patents

A kind of aerogel material and its preparation method and application Download PDF

Info

Publication number
CN119349588A
CN119349588A CN202411909278.0A CN202411909278A CN119349588A CN 119349588 A CN119349588 A CN 119349588A CN 202411909278 A CN202411909278 A CN 202411909278A CN 119349588 A CN119349588 A CN 119349588A
Authority
CN
China
Prior art keywords
aerogel
silica sol
silicon
preparing
stabilizer
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN202411909278.0A
Other languages
Chinese (zh)
Other versions
CN119349588B (en
Inventor
夏玉杰
俞晨龙
史靓辰
牛佩
王浩杰
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Xinxiang Vocational and Technical College
Original Assignee
Xinxiang Vocational and Technical College
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Xinxiang Vocational and Technical College filed Critical Xinxiang Vocational and Technical College
Priority to CN202411909278.0A priority Critical patent/CN119349588B/en
Publication of CN119349588A publication Critical patent/CN119349588A/en
Application granted granted Critical
Publication of CN119349588B publication Critical patent/CN119349588B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/113Silicon oxides; Hydrates thereof
    • C01B33/12Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/14Colloidal silica, e.g. dispersions, gels, sols
    • C01B33/157After-treatment of gels
    • C01B33/158Purification; Drying; Dehydrating
    • C01B33/1585Dehydration into aerogels
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/01Particle morphology depicted by an image
    • C01P2004/03Particle morphology depicted by an image obtained by SEM

Landscapes

  • Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Silicon Compounds (AREA)

Abstract

The invention discloses an aerogel material and a preparation method and application thereof, and belongs to the technical field of aerogel; preparing a silicon precursor, catalyzing to generate silica sol, modifying, including one-stage freezing modification and two-stage freezing modification, and drying at normal pressure to obtain the aerogel material. By introducing azodiisobutyronitrile and performing freeze modification treatment on the silica sol, the sensitivity of the waterproof and heat insulation properties to temperature changes is significantly reduced. It is worth noting that the azodiisobutyronitrile and the silica sol subjected to freezing modification can have synergistic effect, and the compounding not only further weakens the temperature dependence of the waterproof and heat insulation performances of the aerogel, but also remarkably enhances the performance of the aerogel at normal temperature, widens the suitable use temperature range of the aerogel, and improves the practical value of the aerogel.

Description

Aerogel material and preparation method and application thereof
Technical Field
The invention relates to the technical field of aerogel, in particular to an aerogel material and a preparation method and application thereof.
Background
The silicon-based aerogel is a reticular porous material and has the advantages of low density, good heat insulation performance, high hydrophobicity, high porosity and the like, but when the use temperature changes, various performances of the aerogel, especially the heat insulation performance and the hydrophobicity, can be influenced. Therefore, reducing the temperature sensitivity of the aerogel properties (especially the insulation properties and the hydrophobicity) has become a problem to be solved currently.
Based on the above, the invention designs an aerogel material, and a preparation method and application thereof, so as to solve the problems.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention provides an aerogel material, and a preparation method and application thereof.
In order to achieve the above purpose, the invention is realized by the following technical scheme:
a method of preparing an aerogel material, comprising the steps of:
step one, preparing a stabilizer;
Gradually heating azodiisobutyronitrile powder to be in a molten state, dissolving azodiisobutyronitrile in ethanol in the molten state, and stirring to obtain a stabilizer;
Preparing a silicon precursor;
Grinding industrial silicon slag with silicon dioxide as a main component into powder, pickling for 1-2h by using pickling liquor, removing aluminum oxide and alkali, and drying at 40-50 ℃ to obtain a silicon precursor;
Step three, catalyzing to generate silica sol;
adding the silicon precursor into concentrated ammonia water, stirring for 10-15min to obtain activated silicon, adding the activated silicon into a stabilizer, and catalyzing for 2-3h to generate silica sol;
step four, modification treatment;
One-stage freezing modification, namely preserving the silica sol at-5 to-2 ℃ for 25-35min, and naturally heating to normal temperature;
Two-stage freezing modification, namely preserving the silica sol subjected to the first-stage freezing modification at 8-10 ℃ below zero for 25-35min, and naturally heating to normal temperature;
And fifthly, drying at normal pressure to obtain the aerogel material.
Further, the step one specifically comprises heating azobisisobutyronitrile powder gradually to be in a molten state, dissolving azobisisobutyronitrile in ethanol in the molten state, and stirring for 20-30min at 150-200r/min to obtain the stabilizer.
Further, in the first step, the mass ratio of the azodiisobutyronitrile to the ethanol is 1.5-2:100-120.
Further, the azobisisobutyronitrile powder is heated to a temperature of 110-120 ℃.
Further, the second step is to take industrial silicon slag with silicon dioxide as main component, grind the industrial silicon slag into powder, remove alumina and alkali after pickling for 1-2h by pickling solution, and dry the powder at 40-50 ℃ to obtain the silicon precursor.
Further, the industrial silicon slag powder is sieved by a 50-70 mesh sieve.
Further, the pH of the pickling solution is 2-3.
And the third step is to add 0.5-1 part of silicon precursor into 0.2-0.5 part of strong ammonia water, stir for 10-15min at 150-200r/min to obtain activated silicon, add the activated silicon into stabilizer, catalyze for 2-3h to generate silica sol.
An aerogel material prepared according to the method for preparing an aerogel material.
The aerogel material is applied to the preparation of waterproof river sand, waterproof quartz sand, desert modifier, curing agent and waterproof agent.
Compared with the prior art, the invention has the beneficial effects that:
According to the invention, by introducing the azodiisobutyronitrile, the waterproof and heat-insulating effects of the aerogel in a high-temperature environment are obviously improved, and almost the level equivalent to that of a normal-temperature state is reached, so that the sensitivity of the waterproof and heat-insulating performance to temperature change is obviously weakened. Further, the first and second freezing modification treatments applied to the silica sol are also effective in reducing the temperature sensitivity of these properties of the aerogel. It is worth noting that according to comparative experimental data analysis, the azodiisobutyronitrile and the silica sol subjected to freezing modification can have synergistic effect, and the composition not only further weakens the temperature dependence of the waterproof and heat insulation performances of the aerogel, but also remarkably enhances the performance of the aerogel at normal temperature, widens the suitable use temperature interval of the aerogel, and improves the practical value of the aerogel.
In addition, the invention uses industrial silica slag as raw material to produce novel environment-friendly heat insulation material aerogel for building, reduces environmental pollution caused by industrial solid waste, realizes energy conservation and emission reduction, protects environment, and truly realizes green building.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below. It is evident that the drawings in the following description are only some embodiments of the present invention and that other drawings may be obtained from these drawings without inventive effort for a person of ordinary skill in the art.
FIG. 1 is a sample graph of aerogel materials made in accordance with the present invention;
FIG. 2 is a sample plot of aerogel materials produced in accordance with the present invention;
FIG. 3 is a sample plot of waterproof river sand made from aerogel materials;
FIG. 4 is a sample plot of a waterproof quartz sand made from aerogel material;
FIG. 5 is a sample graph of a desert modifier made from aerogel material;
FIG. 6 is a sample plot of a curing agent made from aerogel material;
fig. 7 is a sample graph of a waterproofing agent made from aerogel material.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more clear, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention. It will be apparent that the described embodiments are some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1 as shown in fig. 1-2, this example provides a method for preparing an aerogel material, comprising the steps of:
step one, preparing a stabilizer;
Gradually heating 2g of azodiisobutyronitrile powder to 120 ℃ to be in a molten state, dissolving the azodiisobutyronitrile in 120g of 70% ethanol in the molten state, and stirring for 30min at 200r/min to obtain a stabilizer;
Preparing a silicon precursor;
grinding industrial silicon slag with silicon dioxide as a main component into powder, sieving with a 70-mesh sieve, pickling with pickling solution with pH of 2 for 2 hours, removing aluminum oxide and alkali, and drying at 50 ℃ to obtain a silicon precursor;
Step three, catalyzing to generate silica sol;
Adding 1g of silicon precursor into 0.5g of concentrated ammonia water, stirring for 15min at 200r/min to obtain activated silicon, adding the activated silicon into a stabilizer, and catalyzing for 3h to generate silica sol;
step four, modification treatment;
One-stage freezing modification, namely preserving the silica sol at minus 5 ℃ for 35min, and naturally heating to normal temperature;
two-stage freezing modification, namely preserving the silica sol subjected to the first-stage freezing modification at the temperature of minus 10 ℃ for 35min;
step five, drying at normal pressure to obtain aerogel materials;
the method comprises the steps of sealing silica sol to be dried, then carrying out water bath heating, collecting the mass and the real-time temperature of the silica sol to be dried, determining the stirring time and the initial stirring speed during the water bath heating, adjusting the initial stirring speed according to the real-time temperature to obtain aerogel to be dried, collecting the viscosity data of the aerogel to be dried, judging whether the water bath heating is qualified, putting the aerogel to be dried into a sheet-shaped mold after judging the water bath heating is qualified, placing the aerogel to be dried into a drying chamber for normal-pressure drying, determining the initial rotating speed of a drying fan according to the arrangement density during normal-pressure drying, collecting the real-time mass data of the aerogel to be dried, and judging whether the initial rotating speed is adjusted.
The normal pressure drying method refers to a normal pressure drying method and system for silicon-based aerogel disclosed in Chinese patent CN 116929005A.
Example 2 as shown in fig. 1-2, this example provides a method for preparing an aerogel material, comprising the steps of:
step one, preparing a stabilizer;
Gradually heating 1.5g of azodiisobutyronitrile powder to 110 ℃ to be in a molten state, dissolving the azodiisobutyronitrile in the molten state in 100g of 70% ethanol, and stirring for 20min at 150r/min to obtain a stabilizer;
Preparing a silicon precursor;
grinding industrial silicon slag with silicon dioxide as a main component into powder, sieving with a 50-mesh sieve, pickling with pickling solution with pH of 3 for 1h, removing aluminum oxide and alkali, and drying at 40 ℃ to obtain a silicon precursor;
Step three, catalyzing to generate silica sol;
Adding 0.5g of silicon precursor into 0.2g of concentrated ammonia water, stirring for 10min at 150r/min to obtain activated silicon, adding the activated silicon into a stabilizer, and catalyzing for 2h to generate silica sol;
step four, modification treatment;
one-stage freezing modification, namely preserving the silica sol at minus 2 ℃ for 25min, and naturally heating to normal temperature;
Two-stage freezing modification, namely preserving the silica sol subjected to the first-stage freezing modification at the temperature of minus 8 ℃ for 25min, and naturally heating to normal temperature;
step five, drying at normal pressure to obtain aerogel materials;
the method comprises the steps of sealing silica sol to be dried, then carrying out water bath heating, collecting the mass and the real-time temperature of the silica sol to be dried, determining the stirring time and the initial stirring speed during the water bath heating, adjusting the initial stirring speed according to the real-time temperature to obtain aerogel to be dried, collecting the viscosity data of the aerogel to be dried, judging whether the water bath heating is qualified, putting the aerogel to be dried into a sheet-shaped mold after judging the water bath heating is qualified, placing the aerogel to be dried into a drying chamber for normal-pressure drying, determining the initial rotating speed of a drying fan according to the arrangement density during normal-pressure drying, collecting the real-time mass data of the aerogel to be dried, and judging whether the initial rotating speed is adjusted.
The normal pressure drying method refers to a normal pressure drying method and system for silicon-based aerogel disclosed in Chinese patent CN 116929005A.
Embodiment 3 As shown in FIGS. 1-2, the present embodiment provides a method for preparing an aerogel material, comprising the steps of:
step one, preparing a stabilizer;
Gradually heating 1.6g of azodiisobutyronitrile powder to 13 ℃ to be in a molten state, dissolving the azodiisobutyronitrile in 105g of 70% ethanol in the molten state, and stirring for 22min at 180r/min to obtain a stabilizer;
Preparing a silicon precursor;
Grinding industrial silicon slag with silicon dioxide as a main component into powder, sieving with a 70-mesh sieve, pickling with pickling solution with pH of 2.5 for 2 hours, removing aluminum oxide and alkali, and drying at 48 ℃ to obtain a silicon precursor;
Step three, catalyzing to generate silica sol;
Adding 0.8g of silicon precursor into 0.4g of concentrated ammonia water, stirring for 13min at 170r/min to obtain activated silicon, adding the activated silicon into a stabilizer, and catalyzing for 3h to generate silica sol;
step four, modification treatment;
one-stage freezing modification, namely preserving the silica sol at the temperature of minus 3 ℃ for 30min, and naturally heating to normal temperature;
Two-stage freezing modification, namely preserving the silica sol subjected to the first-stage freezing modification at the temperature of minus 10 ℃ for 30min, and naturally heating to normal temperature;
step five, drying at normal pressure to obtain aerogel materials;
the method comprises the steps of sealing silica sol to be dried, then carrying out water bath heating, collecting the mass and the real-time temperature of the silica sol to be dried, determining the stirring time and the initial stirring speed during the water bath heating, adjusting the initial stirring speed according to the real-time temperature to obtain aerogel to be dried, collecting the viscosity data of the aerogel to be dried, judging whether the water bath heating is qualified, putting the aerogel to be dried into a sheet-shaped mold after judging the water bath heating is qualified, placing the aerogel to be dried into a drying chamber for normal-pressure drying, determining the initial rotating speed of a drying fan according to the arrangement density during normal-pressure drying, collecting the real-time mass data of the aerogel to be dried, and judging whether the initial rotating speed is adjusted.
The normal pressure drying method refers to a normal pressure drying method and system for silicon-based aerogel disclosed in Chinese patent CN 116929005A.
Example 4 in some examples, as shown in fig. 3, aerogel materials prepared in example 3 were added to waterproof river sand raw materials to prepare aerogel waterproof river sand.
Example 5 in some examples, aerogel materials prepared in example 3 were added to a water-repellent silica sand raw material as shown in fig. 4 to produce aerogel water-repellent silica sand.
Example 6 in some examples, aerogel materials prepared in example 3 were added to desert modifier materials to produce aerogel desert modifiers as shown in fig. 5.
Example 7 in some examples, aerogel materials from example 3 were added to a curative feed as shown in fig. 6 to produce aerogel curatives.
Example 8 in some examples, as shown in fig. 7, aerogel materials prepared in example 3 were added to a raw material of a waterproofing agent to prepare an aerogel waterproofing agent.
Comparative example 1 differs from example 3 in that azobisisobutyronitrile is not added;
As shown in fig. 1-2, the present comparative example provides a method for preparing an aerogel material, comprising the steps of:
step one, preparing a stabilizer;
Stirring 105g of 70% ethanol at 180r/min for 22min to obtain a stabilizer;
Preparing a silicon precursor;
Grinding industrial silicon slag with silicon dioxide as a main component into powder, sieving with a 70-mesh sieve, pickling with pickling solution with pH of 2.5 for 2 hours, removing aluminum oxide and alkali, and drying at 48 ℃ to obtain a silicon precursor;
Step three, catalyzing to generate silica sol;
Adding 0.8g of silicon precursor into 0.4g of concentrated ammonia water, stirring for 13min at 170r/min to obtain activated silicon, adding the activated silicon into a stabilizer, and catalyzing for 3h to generate silica sol;
step four, modification treatment;
one-stage freezing modification, namely preserving the silica sol at the temperature of minus 3 ℃ for 30min, and naturally heating to normal temperature;
Two-stage freezing modification, namely preserving the silica sol subjected to the first-stage freezing modification at the temperature of minus 10 ℃ for 30min, and naturally heating to normal temperature;
step five, drying at normal pressure to obtain aerogel materials;
the method comprises the steps of sealing silica sol to be dried, then carrying out water bath heating, collecting the mass and the real-time temperature of the silica sol to be dried, determining the stirring time and the initial stirring speed during the water bath heating, adjusting the initial stirring speed according to the real-time temperature to obtain aerogel to be dried, collecting the viscosity data of the aerogel to be dried, judging whether the water bath heating is qualified, putting the aerogel to be dried into a sheet-shaped mold after judging the water bath heating is qualified, placing the aerogel to be dried into a drying chamber for normal-pressure drying, determining the initial rotating speed of a drying fan according to the arrangement density during normal-pressure drying, collecting the real-time mass data of the aerogel to be dried, and judging whether the initial rotating speed is adjusted.
The normal pressure drying method refers to a normal pressure drying method and system for silicon-based aerogel disclosed in Chinese patent CN 116929005A.
Comparative example 2 the difference from example 3 is that no modification treatment was performed on the silica sol;
As shown in fig. 1-2, the present comparative example provides a method for preparing an aerogel material, comprising the steps of:
step one, preparing a stabilizer;
Gradually heating 1.6g of azodiisobutyronitrile powder to 13 ℃ to be in a molten state, dissolving the azodiisobutyronitrile in 105g of 70% ethanol in the molten state, and stirring for 22min at 180r/min to obtain a stabilizer;
Preparing a silicon precursor;
Grinding industrial silicon slag with silicon dioxide as a main component into powder, sieving with a 70-mesh sieve, pickling with pickling solution with pH of 2.5 for 2 hours, removing aluminum oxide and alkali, and drying at 48 ℃ to obtain a silicon precursor;
Step three, catalyzing to generate silica sol;
Adding 0.8g of silicon precursor into 0.4g of concentrated ammonia water, stirring for 13min at 170r/min to obtain activated silicon, adding the activated silicon into a stabilizer, and catalyzing for 3h to generate silica sol;
Step four, drying at normal pressure to obtain aerogel materials;
the method comprises the steps of sealing silica sol to be dried, then carrying out water bath heating, collecting the mass and the real-time temperature of the silica sol to be dried, determining the stirring time and the initial stirring speed during the water bath heating, adjusting the initial stirring speed according to the real-time temperature to obtain aerogel to be dried, collecting the viscosity data of the aerogel to be dried, judging whether the water bath heating is qualified, putting the aerogel to be dried into a sheet-shaped mold after judging the water bath heating is qualified, placing the aerogel to be dried into a drying chamber for normal-pressure drying, determining the initial rotating speed of a drying fan according to the arrangement density during normal-pressure drying, collecting the real-time mass data of the aerogel to be dried, and judging whether the initial rotating speed is adjusted.
The normal pressure drying method refers to a normal pressure drying method and system for silicon-based aerogel disclosed in Chinese patent CN 116929005A.
Comparative example 3 differs from example 3 in that neither azobisisobutyronitrile nor silica sol was modified;
As shown in fig. 1-2, the present comparative example provides a method for preparing an aerogel material, comprising the steps of:
step one, preparing a stabilizer;
Stirring 105g of 70% ethanol at 180r/min for 22min to obtain a stabilizer;
Preparing a silicon precursor;
Grinding industrial silicon slag with silicon dioxide as a main component into powder, sieving with a 70-mesh sieve, pickling with pickling solution with pH of 2.5 for 2 hours, removing aluminum oxide and alkali, and drying at 48 ℃ to obtain a silicon precursor;
Step three, catalyzing to generate silica sol;
Adding 0.8g of silicon precursor into 0.4g of concentrated ammonia water, stirring for 13min at 170r/min to obtain activated silicon, adding the activated silicon into a stabilizer, and catalyzing for 3h to generate silica sol;
Step four, drying at normal pressure to obtain aerogel materials;
the method comprises the steps of sealing silica sol to be dried, then carrying out water bath heating, collecting the mass and the real-time temperature of the silica sol to be dried, determining the stirring time and the initial stirring speed during the water bath heating, adjusting the initial stirring speed according to the real-time temperature to obtain aerogel to be dried, collecting the viscosity data of the aerogel to be dried, judging whether the water bath heating is qualified, putting the aerogel to be dried into a sheet-shaped mold after judging the water bath heating is qualified, placing the aerogel to be dried into a drying chamber for normal-pressure drying, determining the initial rotating speed of a drying fan according to the arrangement density during normal-pressure drying, collecting the real-time mass data of the aerogel to be dried, and judging whether the initial rotating speed is adjusted.
The normal pressure drying method refers to a normal pressure drying method and system for silicon-based aerogel disclosed in Chinese patent CN 116929005A.
Experimental examples the silica-based aerogels prepared in examples 1 to 3 and comparative examples 1 to 3 were subjected to performance test, and the results are shown in the following table:
1. The method for measuring the thermal conductivity at different temperatures comprises sandwiching a measurement sample of 300×300×100mm 3 between an upper heater and a lower heater at different temperatures under a load of 0.3MPa to set the temperature difference to 20 ℃, and measuring the upper surface temperature, the lower surface temperature, etc. of the measurement sample while adjusting the temperature so as to form one-dimensional heat flow by protecting the heater. Then, the thermal resistance RS of the measurement sample is found by the following formula;
RS=N((TU-TL)/Q)-RO;
TU represents the upper surface temperature of the measured sample, TL represents the lower surface temperature of the measured sample, RO represents the contact thermal resistance of the upper and lower interfaces, Q represents the output of the heat flow meter, N is a proportionality coefficient, and is obtained in advance by using a correction sample;
thermal conductivity = d/RS.
2. Gradually cooling or heating the prepared aerogel, and observing the physical form change of the aerogel to obtain the proper use temperature (for example, the proper use temperature is below 500 ℃ when the aerogel starts to melt and deform at the temperature of above 500 ℃).
3. The water resistance at different temperatures is tested by taking samples with the size of 700 multiplied by 700mm and the thickness of 12mm, after the samples are conditioned, clamping the samples by a clamp and placing the samples on a support, and the samples face upwards during the test. The length direction of the sample is parallel to the water flow direction, 250mL of test water is quickly and stably poured into a funnel, spraying is continuously carried out for 25s-30s, immediately after the spraying is stopped, a clamp holder with the sample is taken away, the front of the sample is almost horizontal, then the clamp holder is lightly knocked against a solid hard object, the clamp holder is horizontally rotated for 180 degrees, then the clamp holder is lightly knocked again, and immediately after the knocking is finished, the front wetting degree of the sample on the clamp holder is rated according to the wetting phenomenon (grade 4: wetting at a spraying point with sporadic surface of the sample; grade 4-5: no wetting at the surface of the sample, a small amount of water drops, and grade 5: no water drops or wetting at the surface of the sample).
According to the table, the waterproof performance and the heat insulation performance of the aerogel at a high temperature are improved by adding the azodiisobutyronitrile, so that the waterproof performance and the heat insulation performance of the aerogel are almost the same as those of the aerogel at normal temperature, namely, the temperature sensitivity of the waterproof performance and the heat insulation performance of the aerogel is reduced, the waterproof performance and the heat insulation performance of the aerogel are also reduced by performing one-stage freezing modification and two-stage freezing modification on the silica sol, and in addition, the azodiisobutyronitrile is compounded with the frozen modified silica sol according to the data of the comparative example 3, and the waterproof performance and the heat insulation performance of the aerogel at normal temperature are also improved by matching the azodiisobutyronitrile and the silica sol.
The foregoing embodiments are merely for illustrating the technical solution of the present invention, but not for limiting the same, and although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those skilled in the art that modifications may be made to the technical solution described in the foregoing embodiments or equivalents may be substituted for parts of the technical features thereof, and such modifications or substitutions may be made without departing from the spirit and scope of the technical solution of the embodiments of the present invention.

Claims (10)

1. A method of preparing an aerogel material, comprising the steps of:
step one, preparing a stabilizer;
Gradually heating azodiisobutyronitrile powder to be in a molten state, dissolving azodiisobutyronitrile in ethanol in the molten state, and stirring to obtain a stabilizer;
Preparing a silicon precursor;
Grinding industrial silicon slag with silicon dioxide as a main component into powder, pickling for 1-2h by using pickling liquor, removing aluminum oxide and alkali, and drying at 40-50 ℃ to obtain a silicon precursor;
Step three, catalyzing to generate silica sol;
adding the silicon precursor into concentrated ammonia water, stirring for 10-15min to obtain activated silicon, adding the activated silicon into a stabilizer, and catalyzing for 2-3h to generate silica sol;
step four, modification treatment;
One-stage freezing modification, namely preserving the silica sol at-5 to-2 ℃ for 25-35min, and naturally heating to normal temperature;
Two-stage freezing modification, namely preserving the silica sol subjected to the first-stage freezing modification at 8-10 ℃ below zero for 25-35min, and naturally heating to normal temperature;
And fifthly, drying at normal pressure to obtain the aerogel material.
2. The method for preparing aerogel materials according to claim 1, wherein step one is to heat the azobisisobutyronitrile powder gradually to be in a molten state, dissolve the azobisisobutyronitrile in the molten state in ethanol, and stir for 20-30min at 150-200r/min to obtain the stabilizer.
3. The method of producing aerogel material according to claim 2, wherein in the first step, the mass ratio of azobisisobutyronitrile to ethanol is 1.5-2:100-120.
4. A method of preparing aerogel materials as claimed in claim 3, wherein the azobisisobutyronitrile powder is heated to a temperature of 110 to 120 ℃.
5. The method for preparing aerogel materials according to claim 4, wherein the second step comprises grinding industrial silica slag containing silica as main component into powder, pickling with pickling solution for 1-2h, removing aluminum oxide and alkali, and drying at 40-50deg.C to obtain silicon precursor.
6. The method of claim 5, wherein the industrial silica powder is sieved through a 50-70 mesh sieve.
7. The method of claim 6, wherein the pH of the pickling solution is 2-3.
8. The method for preparing aerogel material according to claim 7, wherein the third step comprises adding 0.5-1 part of silicon precursor into 0.2-0.5 part of strong ammonia water, stirring for 10-15min at 150-200r/min to obtain activated silicon, adding the activated silicon into a stabilizer, and catalyzing for 2-3h to generate silica sol.
9. An aerogel material prepared by the method of preparing an aerogel material according to any of claims 1-8.
10. Use of the aerogel material of claim 9 in the preparation of waterproof river sand, waterproof quartz sand, desert modifiers, curing agents and waterproofing agents.
CN202411909278.0A 2024-12-24 2024-12-24 Aerogel material and preparation method and application thereof Active CN119349588B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202411909278.0A CN119349588B (en) 2024-12-24 2024-12-24 Aerogel material and preparation method and application thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202411909278.0A CN119349588B (en) 2024-12-24 2024-12-24 Aerogel material and preparation method and application thereof

Publications (2)

Publication Number Publication Date
CN119349588A true CN119349588A (en) 2025-01-24
CN119349588B CN119349588B (en) 2025-05-27

Family

ID=94319210

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202411909278.0A Active CN119349588B (en) 2024-12-24 2024-12-24 Aerogel material and preparation method and application thereof

Country Status (1)

Country Link
CN (1) CN119349588B (en)

Citations (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103332696A (en) * 2013-06-24 2013-10-02 昆山蓝胜建材有限公司 Method for manufacturing water glass aerogel product by using freeze-drying method and application of product
CN106379904A (en) * 2015-08-04 2017-02-08 北京化工大学 Preparation method for high-temperature-resistant silica aerogel
CN107998996A (en) * 2017-12-06 2018-05-08 辽宁科技大学 A kind of preparation method of sial composite aerogel powder
CN110127705A (en) * 2019-05-14 2019-08-16 杭州师范大学 A kind of preparation method of graphene oxide modified flame retardant silica airgel
US20230219821A1 (en) * 2022-01-10 2023-07-13 Ford Global Technologies, Llc Conductive carbon aerogel with high silicon content for solid state battery anode applications
CN116929005A (en) * 2023-09-19 2023-10-24 新乡职业技术学院 Normal-pressure drying method and system for silicon-based aerogel
CN117088710A (en) * 2023-08-08 2023-11-21 黄山瑞盛新材料科技有限公司 Aerogel composite insulation board and preparation method thereof
CN117511219A (en) * 2024-01-05 2024-02-06 中铁建设集团有限公司 Flexible fiber reinforced nano microporous aerogel and preparation method thereof
US20240140882A1 (en) * 2021-04-05 2024-05-02 The Curators Of The University Of Missouri Amorphous and graphitic carbon aerogels from compressed xerogel powders
CN118619645A (en) * 2024-05-24 2024-09-10 新乡职业技术学院 An assembled aerogel composite insulation board
CN119100406A (en) * 2024-09-05 2024-12-10 星空男孩(杭州)科技有限公司 Modified silica aerogel powder and preparation method thereof, aerogel slurry and preparation method thereof and application thereof
CN119143140A (en) * 2024-09-13 2024-12-17 南京大毛牛环保科技有限公司 Preparation method of silicon dioxide composite heat-preservation aerogel

Patent Citations (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103332696A (en) * 2013-06-24 2013-10-02 昆山蓝胜建材有限公司 Method for manufacturing water glass aerogel product by using freeze-drying method and application of product
CN106379904A (en) * 2015-08-04 2017-02-08 北京化工大学 Preparation method for high-temperature-resistant silica aerogel
CN107998996A (en) * 2017-12-06 2018-05-08 辽宁科技大学 A kind of preparation method of sial composite aerogel powder
CN110127705A (en) * 2019-05-14 2019-08-16 杭州师范大学 A kind of preparation method of graphene oxide modified flame retardant silica airgel
US20240140882A1 (en) * 2021-04-05 2024-05-02 The Curators Of The University Of Missouri Amorphous and graphitic carbon aerogels from compressed xerogel powders
US20230219821A1 (en) * 2022-01-10 2023-07-13 Ford Global Technologies, Llc Conductive carbon aerogel with high silicon content for solid state battery anode applications
CN117088710A (en) * 2023-08-08 2023-11-21 黄山瑞盛新材料科技有限公司 Aerogel composite insulation board and preparation method thereof
CN116929005A (en) * 2023-09-19 2023-10-24 新乡职业技术学院 Normal-pressure drying method and system for silicon-based aerogel
CN117511219A (en) * 2024-01-05 2024-02-06 中铁建设集团有限公司 Flexible fiber reinforced nano microporous aerogel and preparation method thereof
CN118619645A (en) * 2024-05-24 2024-09-10 新乡职业技术学院 An assembled aerogel composite insulation board
CN119100406A (en) * 2024-09-05 2024-12-10 星空男孩(杭州)科技有限公司 Modified silica aerogel powder and preparation method thereof, aerogel slurry and preparation method thereof and application thereof
CN119143140A (en) * 2024-09-13 2024-12-17 南京大毛牛环保科技有限公司 Preparation method of silicon dioxide composite heat-preservation aerogel

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
尹正帅;刘义华;佘平江;雷宁;: "SiO_2气凝胶隔热透波复合材料的制备及其性能研究", 航天制造技术, no. 02, 25 April 2015 (2015-04-25), pages 39 - 45 *

Also Published As

Publication number Publication date
CN119349588B (en) 2025-05-27

Similar Documents

Publication Publication Date Title
CN101186475A (en) Modified vitrified microbead thermal insulation mortar and preparation method thereof
CN113149541A (en) Environment-friendly anti-freezing concrete and preparation method thereof
CN111892422B (en) Preparation method of porous sound-absorbing noise-reducing ceramic
CN106186944B (en) A method of improving cement-base composite material thermoelectricity capability
CN103044065A (en) Porous oxide ceramic heat insulating material for kilns and preparation method of porous oxide ceramic heat insulating material
CN109912833A (en) A kind of polyimide aerogel and preparation method thereof
CN119349588B (en) Aerogel material and preparation method and application thereof
CN107051339A (en) A kind of fiber reinforced SiO2Aeroge and preparation method thereof
CN111393178A (en) A kind of preparation method of SiCf@BN core-shell structure chopped fiber
CN110668802A (en) Green preparation method of light high-strength cordierite porous ceramic and filter
CN115872772B (en) Preparation method of fly ash-based ceramic membrane support
CN109678456A (en) Sound absorption ceramic material and preparation method thereof
CN104446626A (en) Preparation method of fly ash based porous thermal insulation material with low thermal conductivity
CN103553624A (en) Silicon carbide ceramic rotor material prepared through gel injection molding and preparation method thereof
CN109437946A (en) A kind of method that aqueous gel casting prepares YSZ fiber-based porous ceramic
CN110204267A (en) A kind of technique preparing cracking-resistant cement mortar using plant fiber
CN109133986A (en) Porous composite ceramics of a kind of AlN-SiC based on foaming and preparation method thereof
CN114213063A (en) Moisturizing self-curing concrete and preparation method thereof
CN106590537A (en) Solar energy drying phase change heat storage material and preparation method thereof
CN118894691A (en) A hygroscopic power generation cement-based material and preparation method thereof
CN108424168B (en) Preparation method of cement-based composite insulation board
CN111908847B (en) Anti-freezing and anti-cracking concrete and preparation method thereof
CN112142057B (en) A kind of aerogel and its preparation method based on constant temperature and humidity drying
CN118529944A (en) A method for preparing ultraviolet-proof thermal insulation glass
CN112645732A (en) Improved aerated concrete building block

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant