CN117430372B - Dispersible aerogel particles and preparation method and application thereof - Google Patents
Dispersible aerogel particles and preparation method and application thereof Download PDFInfo
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- CN117430372B CN117430372B CN202311476357.2A CN202311476357A CN117430372B CN 117430372 B CN117430372 B CN 117430372B CN 202311476357 A CN202311476357 A CN 202311476357A CN 117430372 B CN117430372 B CN 117430372B
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- 239000004964 aerogel Substances 0.000 title claims abstract description 150
- 239000002245 particle Substances 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title abstract description 13
- 239000006185 dispersion Substances 0.000 claims abstract description 51
- 239000007788 liquid Substances 0.000 claims abstract description 33
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 30
- 239000000843 powder Substances 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 21
- 238000009413 insulation Methods 0.000 claims abstract description 20
- 239000002270 dispersing agent Substances 0.000 claims abstract description 19
- 238000001035 drying Methods 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000000080 wetting agent Substances 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- 239000012774 insulation material Substances 0.000 claims abstract description 4
- 239000004114 Ammonium polyphosphate Substances 0.000 claims description 15
- 235000019826 ammonium polyphosphate Nutrition 0.000 claims description 15
- 229920001276 ammonium polyphosphate Polymers 0.000 claims description 15
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 claims description 5
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 claims description 3
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 claims description 3
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 claims description 3
- 229920005646 polycarboxylate Polymers 0.000 claims description 3
- 229920001400 block copolymer Polymers 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 16
- 230000002209 hydrophobic effect Effects 0.000 abstract description 6
- 150000001412 amines Chemical class 0.000 abstract description 2
- 229920000137 polyphosphoric acid Polymers 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 8
- 239000008187 granular material Substances 0.000 description 8
- 239000004570 mortar (masonry) Substances 0.000 description 6
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 5
- 239000003063 flame retardant Substances 0.000 description 5
- 238000004132 cross linking Methods 0.000 description 4
- 239000000428 dust Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- 239000004721 Polyphenylene oxide Substances 0.000 description 2
- 239000004965 Silica aerogel Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 229920001577 copolymer Polymers 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 229920000570 polyether Polymers 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000000779 smoke Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 230000008719 thickening Effects 0.000 description 2
- 239000004743 Polypropylene Substances 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229920003086 cellulose ether Polymers 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000009775 high-speed stirring Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000010451 perlite Substances 0.000 description 1
- 235000019362 perlite Nutrition 0.000 description 1
- -1 polypropylene Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000003075 superhydrophobic effect Effects 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0091—Preparation of aerogels, e.g. xerogels
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
- C04B40/0046—Premixtures of ingredients characterised by their processing, e.g. sequence of mixing the ingredients when preparing the premixtures
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/20—Resistance against chemical, physical or biological attack
- C04B2111/28—Fire resistance, i.e. materials resistant to accidental fires or high temperatures
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/30—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values
- C04B2201/32—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values for the thermal conductivity, e.g. K-factors
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/50—Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Dispersion Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
The invention relates to the field of aerogel materials, in particular to dispersible aerogel particles, and a preparation method and application thereof. The method provided by the invention comprises the following steps: step 1, dissolving a dispersing agent and a wetting agent in water, and then adding aerogel powder to uniformly disperse to obtain aerogel dispersion liquid; step 2, adding a silane coupling agent into the aerogel dispersion liquid for reaction to obtain a silane coupling agent modified aerogel dispersion liquid; step 3, adding polyphosphoric acid amine into the aerogel dispersion liquid modified by the silane coupling agent for reaction to obtain a thickened paste; and step 4, granulating and drying the obtained paste to obtain dispersible aerogel particles. The aerogel particles prepared by the invention have a hydrophobic inner layer and a hydrophilic outer layer, have better dispersibility in an aqueous system, are convenient for mass addition and use, have better structural stability and better heat insulation performance, can provide a heat insulation material prepared by using the aerogel particles, have better heat insulation performance and better application prospect.
Description
Technical Field
The invention relates to the field of aerogel materials, in particular to dispersible aerogel particles, and a preparation method and application thereof.
Background
Aerogels are the least dense solids in the world, slightly less dense than air, and are also known as "frozen smoke" or "blue smoke". Since the particles in an aerogel are very small (in the order of nanometers), visible light is less scattered through it (Rayleigh scattering). In addition, since more than 80% of the aerogel is air, the aerogel has a very good heat insulation effect, and the one inch thick aerogel has the heat insulation effect equivalent to that of 20 to 30 pieces of common glass.
Because the aerogel is prepared to reduce the problem of collapse of the pore structure during drying, hydrophobic modification and drying are generally required, most of the prepared aerogel powder has good hydrophobicity, such as the Chinese patent application CN104003406A, and the super-hydrophobic aerogel powder is prepared. Hydrophobic aerogel powders are generally more difficult to uniformly disperse in systems containing water. For better dispersion, high-speed stirring or long-time dispersion is generally required, and the long-time dispersion or high-speed dispersion can cause the structure of the aerogel to be easily damaged due to poor mechanical properties of the aerogel, thereby causing the heat insulation performance to be greatly reduced, which brings inconvenience to the application of the aerogel.
In order to solve the problem that aerogel is not easy to disperse, researchers also adopt a pre-dispersing method, namely, the aerogel is pre-dispersed in water to prepare aerogel dispersion paste, and then the aerogel dispersion paste is added into a system for application, for example, in the process of preparing a coating in China patent CN115651454A, aerogel dispersion paste is added instead of directly adding aerogel. However, the aerogel is prepared into the dispersion paste for adding, the adding amount of aerogel powder in the aerogel dispersion paste is 30% at maximum, so that the problems that the preparation period is long, the preparation process is complex and the heat insulation performance of the material is not excellent due to the fact that the adding amount of the solvent is large in addition to being inconvenient to transport and use are solved.
In addition, because the aerogel is lighter in weight, in order to better disperse and improve the consistency of products prepared by using the aerogel, the aerogel is usually made into small-sized powder, such as the micron-sized powder made by the aerogel in the chinese patent application CN107265469a, but the aerogel of the small-sized powder easily generates dust when in use, is inconvenient to operate and can pose a threat to the health of experimenters, and the dispersion of the small-sized aerogel can be more difficult.
Disclosure of Invention
The invention provides dispersible aerogel particles and a preparation method and application thereof, and aims to solve the problems that aerogel powder is difficult to disperse in an aqueous system, dust is easy to generate and a large amount of aerogel powder cannot be added. The specific technical scheme is as follows:
in a first aspect of the present invention, there is provided a method for preparing dispersible aerogel particles, comprising the steps of:
Step 1, dissolving a dispersing agent and a wetting agent in water, and then adding aerogel powder to uniformly disperse to obtain aerogel dispersion liquid;
Step 2, adding a silane coupling agent into the aerogel dispersion liquid for reaction to obtain a silane coupling agent modified aerogel dispersion liquid;
Step 3, adding polyphosphoric acid amine into the aerogel dispersion liquid modified by the silane coupling agent for reaction to obtain a thickened paste;
and step 4, granulating and drying the obtained paste to obtain dispersible aerogel particles.
Specifically, the dispersing agent in the step 1 is at least one selected from polycarboxylate dispersing agents and block copolymer dispersing agents.
More specifically, the polycarboxylate dispersant in step 1 includes YCK 2280, TERSPERSE 2735;
Specifically, the wetting agent in the step 1 is at least one selected from polyether modified copolymers.
More specifically, the polyether modified copolymer specifically comprises one of YCK 2180 and TEGO Wet 270;
specifically, the aerogel in the step 1 is silicon aerogel;
More specifically, the silica aerogel may be a hydrophobic silica aerogel;
specifically, the content of dispersant, wetting agent and aerogel in the aerogel dispersion in step 1 is 1-2wt%, 0.5-1wt% and 10-30wt%, respectively.
Specifically, the silane coupling agent in the step 2 is at least one selected from methyltriethoxysilane, methyltrimethoxysilane, 3-aminopropyl trimethoxysilane and vinyltrimethoxysilane.
Specifically, the addition amount of the silane coupling agent in the step 2 is 0.5-2wt% of the addition amount of the aerogel in the step 1.
Specifically, the addition amount of the ammonium polyphosphate in the step 3 is 2-5wt% of the addition amount of the aerogel in the step 1.
Specifically, the drying temperature in the step 4 is 80-100 ℃, and the drying time is 30-60 minutes.
Specifically, the temperature of the reaction in the step 2 and the step 3 is 30-50 ℃.
In a second aspect of the invention, there is provided a dispersible aerogel particle prepared by the method of any of the above.
Specifically, the dispersible aerogel particles are regular and have a particle size of 1-3mm.
In a third aspect, the present invention provides an application of the dispersible aerogel particles in the field of thermal insulation materials.
Specifically, the heat-insulating material comprises heat-insulating mortar, heat-insulating boards and heat-insulating paint.
The preparation method comprises the steps of uniformly dispersing aerogel powder in water, and then adding a silane coupling agent for modification, so that a hydrophobic inner layer is formed on the surface of the aerogel;
then adding ammonium polyphosphate, wherein amino groups on the ammonium polyphosphate can react with hydroxyl generated by hydrolysis of a silane coupling agent to form crosslinking, and a hydrophilic layer outer layer is formed, so that aerogel particles have better dispersibility in an aqueous system; the mechanical property of the aerogel can be improved through crosslinking, the system is thickened to obtain a paste, and the formed paste can be well granulated, so that regular particles can be formed conveniently;
Meanwhile, the addition of ammonium polyphosphate introduces phosphorus-containing groups into the formed aerogel particles, so that the flame retardance of the aerogel particles can be improved, and the heat resistance of the aerogel particles can be improved.
The method has the following beneficial effects:
(1) The aerogel particles prepared by the method have a hydrophobic inner layer and a hydrophilic outer layer, have larger weight than pure aerogel powder, have better dispersibility in an aqueous system, and are convenient for mass addition and use;
(2) According to the preparation method, the silane coupling agent and the ammonium polyphosphate are crosslinked on the surface of the aerogel in the preparation process, and a pore structure is introduced, so that the prepared aerogel particles are good in structural stability and thermal insulation performance, and the thermal insulation material prepared by using the silane coupling agent and the ammonium polyphosphate is good in thermal insulation performance;
(3) The aerogel particles provided by the invention are regular large particles (1-3 mm), no dust is generated during use, the operation is convenient, the safety is high, and the consistency of the materials prepared by the aerogel particles is good due to the regular shape;
(4) The aerogel particles provided by the invention have the function of improving the mechanical property of the aerogel particles by crosslinking formed in the preparation process, and the prepared aerogel particles have better mechanical property, so that the aerogel particles can be prevented from becoming brittle after being dried or being disintegrated into powder when being dispersed in a solvent system;
(5) The aerogel particles provided by the invention have better flame retardance and heat resistance due to the introduction of the phosphorus-containing groups, and have better application prospects.
Detailed Description
The technical solutions of the present application will be clearly and completely described in conjunction with the embodiments of the present application, and it is apparent that the described embodiments are some embodiments of the present application, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the application without making any inventive effort, are intended to be within the scope of the application.
Example 1
Step 1, 2g of dispersing agent (YCK 2280) and 1g of wetting agent (YCK 2180) are taken and dissolved in 66g of water, 30g of aerogel powder is added for uniform dispersion, and aerogel dispersion liquid is obtained;
step 2, adding 0.3g of methyltriethoxysilane to react at 50 ℃ to obtain silane coupling agent modified aerogel dispersion liquid;
Step 3, adding 1g of ammonium polyphosphate into the aerogel dispersion liquid modified by the silane coupling agent to react at 40 ℃ to obtain a thickened paste;
And 4, granulating the thickened paste, extruding the aerogel paste into granules with the diameter of 1mm, and drying at 80 ℃ for 1 hour to obtain regular dispersible aerogel particles.
Example 2
Step 1, 1g of dispersing agent (TERSPERSE-2735) and 0.5g of wetting agent (YCK 2180) are taken and dissolved in 67.5g of water, 30g of aerogel powder is added for uniform dispersion, and aerogel dispersion liquid is obtained;
Step 2, adding 0.6g of 3-aminopropyl trimethoxy silane to react at 50 ℃ to obtain silane coupling agent modified aerogel dispersion;
Step 3, adding 1g of ammonium polyphosphate into the aerogel dispersion liquid modified by the silane coupling agent to react at 40 ℃ to obtain a thickened paste;
And 4, granulating the thickened paste, extruding the aerogel paste into granules with the diameter of 2mm, and drying at 80 ℃ for 1 hour to obtain regular dispersible aerogel particles.
Example 3
Step 1, dissolving 1.5g of dispersing agent (YCK 2280) and 1g of wetting agent (TEGO Wet 270) in 76.5g of water, and adding 20g of aerogel powder to uniformly disperse to obtain aerogel dispersion liquid;
step 2, adding 0.1g of methyltrimethoxysilane to react at 40 ℃ to obtain silane coupling agent modified aerogel dispersion liquid;
Step 3, adding 0.66g of ammonium polyphosphate into the aerogel dispersion liquid modified by the silane coupling agent to react at 30 ℃ to obtain a thickened paste;
And 4, granulating the thickened paste, extruding the aerogel paste into granules with the diameter of 2mm, and drying at 100 ℃ for 0.5 hour to obtain regular dispersible aerogel particles.
Example 4
Step 1, 2g of dispersing agent (TERSPERSE-2735) and 1g of wetting agent (YCK 2180) are taken and dissolved in 86g of water, and 10g of aerogel powder is added for uniform dispersion, so as to obtain aerogel dispersion liquid;
Step 2, adding 0.2g of methyltriethoxysilane to react at 30 ℃ to obtain silane coupling agent modified aerogel dispersion liquid;
Step 3, adding 0.5g of ammonium polyphosphate into the aerogel dispersion liquid modified by the silane coupling agent to react at 40 ℃ to obtain a thickened paste;
And 4, granulating the thickened paste, extruding the aerogel paste into granules with the diameter of 2mm, and drying at 80 ℃ for 1 hour to obtain regular dispersible aerogel particles.
Example 5
Step 1, 2g of dispersing agent (YCK 2280) and 1g of wetting agent (TEGO Wet 270) are taken and dissolved in 66g of water, 30g of aerogel powder is added for uniform dispersion, and aerogel dispersion liquid is obtained;
step 2, adding 0.5g of vinyl trimethoxy silane to react at 50 ℃ to obtain silane coupling agent modified aerogel dispersion liquid;
Step 3, adding 0.6g of ammonium polyphosphate into the aerogel dispersion liquid modified by the silane coupling agent to react at 40 ℃ to obtain a thickened paste;
and 4, granulating the thickened paste, extruding the aerogel paste into granules with the diameter of 3mm, and drying at 80 ℃ for 1 hour to obtain regular dispersible aerogel particles.
Comparative example 1
Step 1, 2g of dispersing agent (YCK 2280) and 1g of wetting agent (YCK 2180) are taken and dissolved in 66g of water, 30g of aerogel powder is added for uniform dispersion, and aerogel dispersion liquid is obtained;
And 2, adding 0.3g of methyltriethoxysilane to react at 50 ℃ to obtain silane coupling agent modified aerogel dispersion liquid, wherein granulation cannot be carried out, and directly drying the aerogel dispersion liquid to obtain the silane coupling agent modified aerogel material.
Comparative example 2
Step 1, 2g of dispersing agent (YCK 2280) and 1g of wetting agent (YCK 2180) are taken and dissolved in 66g of water, 30g of aerogel powder is added for uniform dispersion, and aerogel dispersion liquid is obtained;
Step 2, adding 1g of ammonium polyphosphate into the aerogel dispersion liquid to react at 40 ℃, and stirring for 3 hours to obtain thickened liquid;
And 3, granulating the thickened liquid, extruding the granules into granules with the diameter of 1mm, drying the granules at 80 ℃ for 1 hour to obtain irregular aerogel particles, and crushing the tact particles into powder.
Application example
The heat insulation mortar was obtained by mixing 6 parts of the dispersible aerogel particles or aerogel materials prepared in examples and comparative examples, 40 parts of cement, 25 parts of slag, 15 parts of perlite, 7 parts of redispersible rubber powder, 1 part of cellulose ether, 2 parts of polypropylene fiber, 0.5 part of auxiliary agent and 10 parts of water with stirring for 20 minutes.
Fire rating with reference to DIN 4102, according to the standard, the fire rating of a material can be divided into: the flame retardant performance of the A1 nonflammable material, the A2 nonflammable material, the B1 flame retardant material, the B2 flammable material and the B3 flammable material is also reduced in sequence.
Test results
| Test item | Aerogel thermal conductivity | Flame retardancy | Compressive Strength | Thermal conductivity coefficient of thermal insulation mortar |
| Example 1 | 0.017W/(m·K) | A1 | 2.96MPa | 0.032W/(m·K) |
| Example 2 | 0.021W/(m·K) | A1 | 2.61MPa | 0.037W/(m·K) |
| Example 3 | 0.019W/(m·K) | A1 | 2.68MPa | 0.039W/(m·K) |
| Example 4 | 0.020W/(m·K) | A1 | 2.73MPa | 0.038W/(m·K) |
| Example 5 | 0.022W/(m·K) | A1 | 2.81MPa | 0.041W/(m·K) |
| Comparative example 1 | 0.025W/(m·K) | A2 | 1.35MPa | 0.071W/(m·K) |
| Comparative example 2 | 0.031W/(m·K) | A1 | 1.16MPa | 0.085W/(m·K) |
As can be seen from the test results, the dispersible aerogel particles prepared by the method have smaller heat conductivity coefficient, higher flame retardant grade and higher compressive strength, which indicates that the dispersible aerogel particles prepared by the method have better heat insulation performance, flame retardant performance and mechanical performance; in addition, the dispersible aerogel particles prepared by the method have better dispersibility in an aqueous system, can avoid aerogel structural damage and heat insulation performance reduction caused by strong dispersion, and the heat insulation mortar prepared by the method has better heat insulation performance; the aerogel material prepared in comparative example 1 is good in heat insulation performance, but not good enough in flame retardant performance, and the improvement of the mechanical properties of the aerogel by the modification of the silane coupling agent is limited, so that the heat insulation mortar prepared by using the aerogel material in comparative example 1 can cause the damage of the structure of the aerogel material in the operations of mixing and the like, and the heat insulation performance is poor; in comparative example 2, only ammonium polyphosphate is added in the preparation process, thickening can be performed after long-time stirring, and besides low preparation efficiency and poor thickening effect, the prepared aerogel particles are relatively poor in heat insulation performance and poor in mechanical performance due to the fact that crosslinking cannot be well formed, and the prepared heat-insulating mortar is poor in final heat insulation performance due to the fact that the structure of the aerogel material is damaged when being used for operations such as mixing.
Claims (10)
1. A method of preparing dispersible aerogel particles comprising the steps of:
Step 1, dissolving a dispersing agent and a wetting agent in water, and then adding aerogel powder to uniformly disperse to obtain aerogel dispersion liquid;
Step 2, adding a silane coupling agent into the aerogel dispersion liquid for reaction to obtain a silane coupling agent modified aerogel dispersion liquid;
Step 3, adding ammonium polyphosphate into the aerogel dispersion liquid modified by the silane coupling agent for reaction to obtain a thickened paste;
and step 4, granulating and drying the obtained paste to obtain dispersible aerogel particles.
2. The method of preparing dispersible aerogel particles of claim 1, wherein the content of dispersant, wetting agent and aerogel in the aerogel dispersion in step 1 is 1-2wt%, 0.5-1wt% and 10-30wt%, respectively.
3. The method of preparing dispersible aerogel particles of claim 1, wherein the dispersant in step 1 is selected from at least one of polycarboxylate dispersants and block copolymer dispersants.
4. The method of preparing dispersible aerogel particles of claim 1, wherein the silane coupling agent in step 2 is selected from at least one of methyltriethoxysilane, methyltrimethoxysilane, 3-aminopropyl trimethoxysilane, and vinyltrimethoxysilane.
5. The method of preparing dispersible aerogel particles of claim 1, wherein the silane coupling agent is added in an amount of 0.5 to 2wt% of the aerogel added in step 1.
6. The method of preparing dispersible aerogel particles of claim 1, wherein the ammonium polyphosphate is added in step 3 in an amount of 2 to 5wt% of the aerogel.
7. The method of claim 1, wherein the temperature of the reaction in step 2 and step 3 is 30-50 ℃.
8. The method of preparing dispersible aerogel particles of claim 1, wherein the drying temperature in step 4 is 80-100 ℃ and the drying time is 0.5-1h.
9. A dispersible aerogel particle prepared by the method of any of claims 1 to 8, wherein the aerogel particles are regular in shape and have a particle size of 1 to 3mm.
10. Use of the dispersible aerogel particles prepared by the method of any of claims 1-8 in the field of insulation materials for thermal insulation.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311476357.2A CN117430372B (en) | 2023-11-08 | 2023-11-08 | Dispersible aerogel particles and preparation method and application thereof |
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| CN116120811A (en) * | 2023-03-14 | 2023-05-16 | 中国科学院深圳先进技术研究院 | Water-based acrylic resin composite modified aerogel heat-insulating fireproof coating and preparation method thereof |
| CN116554784A (en) * | 2022-08-16 | 2023-08-08 | 武汉中科先进材料科技有限公司 | Epoxy modified methylphenyl organic silicon aerogel heat insulation coating and preparation method thereof |
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| US11097242B2 (en) * | 2017-11-27 | 2021-08-24 | Taiwan Aerogel Technology Materials Co., Ltd. | Wet gel granule of aerogel and preparation method thereof |
| US20200339762A1 (en) * | 2019-04-29 | 2020-10-29 | Taiwan Aerogel Technology Material Co., Ltd. | Modified aerogel powder with special function group for use in plastic composite and fiber spinning and preparation method thereof |
| CN116751489B (en) * | 2023-07-28 | 2024-11-26 | 长春工业大学 | A hydrophobic modified aerogel composite epoxy resin water-insulating coating and preparation method thereof |
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| CN116554784A (en) * | 2022-08-16 | 2023-08-08 | 武汉中科先进材料科技有限公司 | Epoxy modified methylphenyl organic silicon aerogel heat insulation coating and preparation method thereof |
| CN116120811A (en) * | 2023-03-14 | 2023-05-16 | 中国科学院深圳先进技术研究院 | Water-based acrylic resin composite modified aerogel heat-insulating fireproof coating and preparation method thereof |
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