CN110066189A - A kind of expanded perlite-SiO2The preparation method of aeroge compound insulating material - Google Patents
A kind of expanded perlite-SiO2The preparation method of aeroge compound insulating material Download PDFInfo
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- CN110066189A CN110066189A CN201910379404.9A CN201910379404A CN110066189A CN 110066189 A CN110066189 A CN 110066189A CN 201910379404 A CN201910379404 A CN 201910379404A CN 110066189 A CN110066189 A CN 110066189A
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- expanded perlite
- aeroge
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- 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
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
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- 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
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5025—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with ceramic materials
- C04B41/5035—Silica
Abstract
The invention discloses a kind of expanded perlite-SiO2The preparation method of aeroge compound insulating material belongs to energy-saving building materials field.Using ethyl orthosilicate and methyltriethoxysilane as co-precursor, expanded perlite is carrier, the modified absorption method of modified or vacuum pressure impregnation is impregnated using normal pressure, by SiO2Aeroge is adsorbed onto expanded perlite hole, and modified by aging process, solvent displacement and surface, expanded perlite-SiO is made in constant pressure and dry2Aeroge compound insulating material.Expanded perlite-SiO of the present invention2Aeroge has many advantages, such as that thermal conductivity is low, non-ignitable, chemical stability is strong, is a kind of economic, environmental protection greening building energy saving thermal insulation material.
Description
Technical field
The invention belongs to building energy-saving heat-insulating material technical fields, are related to a kind of expanded perlite-SiO2Aeroge is compound
The preparation method of thermal insulation material.
Background technique
The building thermal insulation material in China is broadly divided into organic insulation material and inorganic heat insulation material at present.Organic insulation material
The mainly spin-off of petrochemical industry, including molded polystyrene (EPS), extruded polystyrene (XPS), polyurethane (PU) and phenol
Urea formaldehyde (PF) etc. has many advantages, such as that good heat insulating, light-weight, hydrophobicity performance is strong, obtains in China building heat preservation field
It is widely applied.
The excellent thermal insulation performance of organic insulation material, but organic insulation material has the shortcomings that a fatal-inflammability,
It burns when fiery very fast, and a large amount of poisonous and hazardous gases can be generated, can be made to the health of trapped person and rescue personnel
At harm, therefore in actual use, have very big security risk or even the country have occurred it is a lot of because of organic heat-insulating material
Fire caused by material burns, such as CCTV style center fire, 11.15 fire of Shanghai City, the terminal of the Capital Airport two is building mistake
Fire etc. causes huge economic loss and casualties.Organic insulation material also has at high cost, not ageing-resistant, deformation system
The disadvantages of number is big, stability is poor, as " green building assessment standard ", " Code for fire protection design of buildings " etc. are a series of increasingly tighter
The national compulsory thermal insulation material standard of lattice is put into effect in succession, and country has been continuously improved to building energy conservation and building fire protection requirement, limit
The application field of organic insulation material is made.
Expanded perlite has received widespread attention as main inorganic heat insulation material, with non-ignitable, stability is good, ring
The excellent performance such as guarantor, nontoxic, is with a wide range of applications.But expanded perlite is for organic insulation material,
Thermal conductivity is bigger than normal, and water absorption rate is high, and after absorbing water, thermal conductivity increased dramatically, and mechanical strength reduces.It therefore, need to be precious to expansion
Zhu Yan is modified processing.
SiO2Aeroge is a kind of novel inorganic nonmetallic nanometer material, because of its translucence and ultra-light-weight, sometimes
Also referred to as " solid-state cigarette " and " blue smoke ".SiO2Aeroge has many excellent performances, such as ultralow thermal conductivity, high-ratio surface
Product, high porosity, low-density and low-k etc., under vacuum condition, thermal conductivity can be allowed to down to 0.001W/ (mK)
It has broad application prospects in fields such as building trade, aerospace, petrochemical industries.But current SiO2Aeroge is prepared into
This is high, intensity is low, it is made to be not directly applicable building heat preservation field.
Patent " preparation method of aeroge expanded perlite " (application number: 201610020100.X) discloses a kind of airsetting
The preparation method of glue expanded perlite, for this method using waterglass as presoma, expanded perlite is carrier, utilizes sol-gel
Aeroge is filled by vacuum drying process or is wrapped in outside by method (sol-gel) and vacuum pressure impregnation full-cell process (VPI)
Expanded perlite is combined.It is presoma the method use waterglass, the later period need to be removed in solution with ion exchange column
Na+Ion and other impurities cation, increase process flow, and the aeroge performance finally prepared is poor.
Patent " a kind of Aerogel/inorganic lightweight aggregate composite thermal insulation material and preparation method thereof " (application number:
201210295764.9) disclose a kind of Aerogel/inorganic lightweight aggregate composite thermal insulation material and preparation method thereof, this method
Using waterglass as silicon source, colloidal sol is prepared using sol-gel method (sol-gel), by prepared colloidal sol using low pressure adsorbent
Technique is drawn into silicon dioxide gel in expanded perlite cavity, is then allowed to stand after gel, using supercritical drying work
Aeroge inorganic light-weight aggregate theremal-preserving heat-insulating material is made in skill.The method use supercritical drying process, this process costs
High, complex process and there is certain risk, is unfavorable for commercially producing and scale application.
Summary of the invention
In order to solve the problem above-mentioned with it is insufficient, the purpose of the present invention is to provide a kind of safe and reliable, simple process, can
Control property is strong, the expanded perlite-SiO with preferable reproducibility2Aeroge atmospheric preparation method.
The present invention is with ethyl orthosilicate (TEOS) and methyltriethoxysilane (MTES) for co-precursor, expanded pearlite
Rock (EP) is carrier, using vacuum impregnation absorption method, by SiO2Aeroge is adsorbed onto expanded perlite hole, at aging
Reason, solvent displacement and surface are modified, and expanded perlite-SiO is made in constant pressure and dry2Aeroge (AEP) compound insulating material.
Expanded perlite-SiO of the present invention2The preparation method of aeroge compound insulating material, comprising the following steps:
1)SiO2The synthesis of aeroge:
By ethyl orthosilicate, methyltriethoxysilane, ethyl alcohol, water according to molar ratio be 1:0.3:(6~16): (4~
14) it mixes, salt acid for adjusting pH value is added in mixed liquor, in a water bath heating stirring, ammonia spirit is then added, adjust pH,
Form SiO2Aeroge；
2) expanded perlite-SiO2The preparation of aeroge compound insulating material:
Using vacuum impregnation mode by SiO2Aeroge is adsorbed onto expanded perlite hole, is replaced through gel aging, solvent
It changes, surface modification, finally through constant pressure and dry, expanded perlite-SiO can be obtained2Aeroge compound insulating material.
Preferably, the aeroge is hydrophobic aerogels, and pore-size distribution is 2~20nm, and thermal coefficient is not more than
0.0212W/(m·K)。
Preferably, the expanded perlite is perforate expanded perlite, and thermal coefficient is 0.042~0.051W/ (mK)；
Particle size range is 0.5~0.9mm, 0.9~2mm and 2~4.7mm.
Preferably, in step 1), it is 2~3 that salt acid for adjusting pH value, which is added,；It is held in 20~30 DEG C of water-bath magnetic stirring apparatus
20~40min of continuous stirring；Then ammonia spirit is added, adjusting pH value is 6~8.
Preferably, in step 2), the relative degree of vacuum of the vacuum impregnation mode is -0.08MPa~0MPa, vacuum suction
Time is 5min~35min.
Preferably, in step 2), the gel ageing process are as follows: composite material is placed in ethanol solution and is carried out
Aging process, the temperature of gel aging are 50~60 DEG C, and the time of aging is 24~48h.
Preferably, in step 2), solvent replacement and surface modification technology are that normal pressure dipping is modified or vacuum pressure impregnation changes
Property.
Preferably, the solvent replacement and Process of Surface Modification are as follows: composite material is placed on three that volume ratio is 1:1:8
Solvent displacement and the modified 24~72h in surface in methylchlorosilane/dehydrated alcohol/n-hexane mixed solution, wherein in mixed solution,
It is (2~3) that trimethylchloro-silicane content, which accounts for the ethyl orthosilicate molar ratio in composite material: 1.
Preferably, in step 2), the drying be constant pressure and dry, successively 25 DEG C, 40 DEG C, 60 DEG C, 80 DEG C, 100 DEG C,
Freeze-day with constant temperature 1h, 1h, 2h, 2h, 3h, 2h, 2h are distinguished at 120 DEG C and 140 DEG C.
Expanded perlite-SiO of the present invention2Aeroge compound insulating material thermal conductivity is not more than 0.040W/ (mK), compares table
Area is not less than 85.41m2/g；Water absorption rate is not more than 13.7%；Cylindrical compress strength is not less than 187.91KPa.
The beneficial effects of the present invention are:
The present invention is quasi- to optimize it from the microcosmic point of material, with ethyl orthosilicate and methyltriethoxy silane
Alkane is co-precursor,, will using vacuum impregnation absorption method using cheap, light porous expanded perlite as carrier
SiO2Aeroge is adsorbed onto expanded perlite hole, modified by aging process, solvent displacement and surface, constant pressure and dry system
Obtain expanded perlite-SiO2Aeroge (AEP) compound insulating material.Expanded perlite-SiO2The preparation of airsetting gluing thermal insulation material
In the process, the performance characteristics of two kinds of materials are learnt from other's strong points to offset one's weaknesses, while improving material cost performance, realizes the advantage of two kinds of materials
The compression strength of aeroge not only can be improved in complementation, can also reduce the thermal conductivity of expanded perlite, is expanded perlite work
Skill, which is improved, provides a kind of new Research Thinking.
Detailed description of the invention
The drawings described herein are used to provide a further understanding of the present invention, constitutes part of this application, not
Inappropriate limitation of the present invention is constituted, in the accompanying drawings:
Fig. 1 vacuum suction time is to expanded perlite-SiO2The influence of aeroge compound insulating material thermal conductivity；
Fig. 2 (a)-(b) is expanded perlite-SiO prepared by the embodiment of the present invention 12Aeroge compound insulating material appearance
The scanning electron microscope of face structure, wherein Fig. 2 (a) is the expanded perlite outer surface structure for filling aeroge；Fig. 2 (b) is Fig. 2 (a)
Partial enlargement；
Fig. 3 (a)-(b) is expanded perlite-SiO prepared by the embodiment of the present invention 12Inside aeroge compound insulating material
The scanning electron microscope of cross-section structure, wherein Fig. 3 (a) is the expanded perlite internal structure for filling aeroge；Fig. 3 (b) is filling gas
The expanded perlite internal structure of gel；
Fig. 4 and Fig. 5 is respectively that not hydrophobic modified expanded perlite (blank control) and the present invention prepare expanded perlite-
SiO2The material object of the modified hydrophobic effect of aeroge shines comparison diagram.
Specific embodiment
Below in conjunction with attached drawing and specific embodiment, the present invention will be described in detail, herein illustrative examples of the invention
And explanation is used to explain the present invention, but not as a limitation of the invention.
Expanded perlite-SiO of the invention2The preparation method of aeroge compound insulating material, includes the following steps:
1)SiO2The synthesis of aeroge:
By ethyl orthosilicate, methyltriethoxysilane, ethyl alcohol, water according to molar ratio be 1:0.3:(6~16): (4~
14) it mixes, salt acid for adjusting pH value is added in mixed liquor to 2~3, promotes silicon source hydrolysis；In 20~30 DEG C of water-bath magnetic agitations
20~40min of heating and continuous stirring in device promotes silicon source to be fully hydrolyzed；Then ammonia spirit is added, adjusts pH to 6~8, promotes
Gel polycondensation forms SiO2Aeroge.Aeroge is hydrophobic aerogels, and pore-size distribution is 2~20nm, and thermal coefficient is not more than
0.0212W/(m·K)。
2) expanded perlite-SiO2The preparation of aeroge compound insulating material:
By SiO2Aeroge is adsorbed onto expanded perlite hole, modified by aging process, solvent displacement and surface.Its
In, expanded perlite is perforate expanded perlite, and preferable particle size is 0.5~0.9mm, 0.9~2mm and 2~4.7mm, thermally conductive system
Number is 0.042~0.051W/ (mK).
Wherein, composite material is placed in ethanol solution and carries out aging process, aging temperature is 50~60 DEG C, always
The change time is 24~48h.Aging process promotes further to be crosslinked between gel network, so that the skeleton structure for improving wet gel is strong
Degree, reduce constant pressure and dry during aeroge volume excess shrinkage and caused by structure collapses.
Solvent replacement and Process of Surface Modification are as follows: by composite material be placed on volume ratio be 1:1:8 trim,ethylchlorosilane/
Solvent displacement and the modified 24~72h in surface in dehydrated alcohol/n-hexane mixed solution, wherein trimethylchloro-silicane accounts in mixed solution
Ethyl orthosilicate molar ratio in composite material is (2~3): 1.
Solvent replacement and surface modification technology are that normal pressure dipping is modified or vacuum pressure impregnation is modified.Wherein use Vaccum Permeating
Relative degree of vacuum when stain suction type is -0.08MPa~0MPa, and the vacuum suction time is 5min~35min.
Dry is constant pressure and dry, and constant temperature is successively distinguished at 25 DEG C, 40 DEG C, 60 DEG C, 80 DEG C, 100 DEG C, 120 DEG C and 140 DEG C
Dry 1h, 1h, 2h, 2h, 3h, 2h, 2h constant pressure and dry, is finally cooled to room temperature with drying box, can obtain expanded perlite-SiO2
Aeroge compound insulating material.
The present invention is described in further details below by specific embodiment.
Embodiment 1
1) with ethyl orthosilicate (TEOS) and methyltriethoxysilane (MTES) for co-precursor, according to positive silicic acid second
Ester: methyltriethoxysilane: dehydrated alcohol: water=1:0.3:14:6 (molar ratio) is uniformly mixed, and hydrochloric acid is added dropwise, and adjusts pH value
It is 2.5, stirs 30min, promote being fully hydrolyzed for silicon source；
2) ammonium hydroxide is added dropwise in the solution into step 1) after hydrolysis, and adjustment solution ph is 7, and control gel time is 60min
Left and right is conducive to that aeroge is adsorbed onto the internal cavities of expanded perlite below；
3) aeroge is poured into and is filled in the vacuum cylinder that partial size is 2~4.7mm expanded perlite, until flooding in vacuum cylinder
Expanded perlite；
4) vacuum pump is opened, the vacuum degree for adjusting vacuum pump is -0.04MPa, pressure stabilizing 25min, subsequent vacuum cylinder pressure
It is down to normal pressure and remaining aeroge discharge will be impregnated, wait it inside the hole of expanded perlite and surface gel；
5) by the expanded perlite-SiO that is combined after gel2Aeroge compound insulating material is in 55 DEG C of ethanol solutions
Middle aging 40h；
6) by the expanded perlite-SiO after aging2Aeroge places trim,ethylchlorosilane: ethyl alcohol: n-hexane=1:1:8
Vacuum pressure impregnation 72h in (volume ratio) mixed solution, wherein trim,ethylchlorosilane: ethyl orthosilicate=2.5 (molar ratio).
7) drying process are as follows: sample is successively permanent respectively at 25 DEG C, 40 DEG C, 60 DEG C, 80 DEG C, 100 DEG C, 120 DEG C and 140 DEG C
Temperature dry 1h, 1h, 2h, 2h, 3h, 2h, 2h, are finally cooled to room temperature with drying box and obtain expanded perlite-SiO2Aeroge is multiple
Close thermal insulation material.
Expanded perlite-SiO2Aeroge compound insulating material thermal conductivity is 0.036W/ (mK), and specific surface area is
117.82m2/g；Water absorption rate is 8.5%；Cylindrical compress strength is 214.35KPa.
Fig. 1 vacuum suction time is to expanded perlite-SiO2The influence of aeroge compound insulating material thermal conductivity；
Fig. 2 (a)-(b) is expanded perlite-SiO prepared by the embodiment of the present invention 12Aeroge compound insulating material appearance
The scanning electron microscope of face structure, wherein (a) figure is the expanded perlite outer surface structure for filling aeroge, scale is 100 μm；(b)
Figure is the partial enlargement for scheming a, and scale is 50 μm；
Fig. 3 (a)-(b) is expanded perlite-SiO prepared by the embodiment of the present invention 12Inside aeroge compound insulating material
The scanning electron microscope of cross-section structure, wherein (a) figure is the expanded perlite internal structure for filling aeroge, scale is 50 μm；(b) figure
It is not filled by the expanded perlite internal structure of aeroge, scale is 100 μm；
Fig. 4 and Fig. 5 is respectively that not hydrophobic modified expanded perlite (blank control) and the present invention prepare expanded perlite-
SiO2The material object of the modified hydrophobic effect of aeroge shines comparison diagram.
Embodiment 2
1) with ethyl orthosilicate (TEOS) and methyltriethoxysilane (MTES) for co-precursor, according to TEOS:MTES:
EtOH:H2Hydrochloric acid is added dropwise in O=1:0.3:6:14 (molar ratio) mixing, and adjustment pH value is 2, stirs 40min, promotes filling for silicon source
Divide hydrolysis；
2) ammonium hydroxide is added dropwise to the solution in step 1), adjustment solution ph is 8, and the gel time for controlling colloidal sol is 60min
Left and right is conducive to that the hydrosol is adsorbed onto the internal cavities of expanded perlite below；
3) hydrosol is poured into and is filled in the vacuum cylinder that partial size is 0.9~2mm expanded perlite, until flooding in vacuum cylinder
Expanded perlite；
4) vacuum pump is opened, the vacuum degree for adjusting vacuum pump is -0.02MPa, pressure stabilizing 20min, subsequent vacuum cylinder pressure
It is down to normal pressure and remaining colloidal sol discharge will be impregnated, wait colloidal sol inside the hole of expanded perlite and surface gel；
5) be combined expanded perlite-SiO after collosol and gel2Aeroge aging 48h in 50 DEG C of ethanol solutions；
6) by the expanded perlite-SiO after aging2Aeroge places trim,ethylchlorosilane: ethyl alcohol: n-hexane=1:1:8
In (volume ratio) mixed solution vacuum pressure impregnation for 24 hours, wherein trim,ethylchlorosilane: ethyl orthosilicate=2 (molar ratio).
7) drying process are as follows: wet gel sample is successively at 25 DEG C, 40 DEG C, 60 DEG C, 80 DEG C, 100 DEG C, 120 DEG C and 140 DEG C
Freeze-day with constant temperature 1h, 1h, 2h, 2h, 3h, 2h, 2h respectively, are finally cooled to room temperature with drying box and obtain SiO2Aeroge.
Expanded perlite-SiO2Aeroge compound insulating material thermal conductivity is 0.040W/ (mK), and specific surface area is
85.41m2/g；Water absorption rate is 13.7%；Cylindrical compress strength is 187.91KPa.
Embodiment 3
1) with ethyl orthosilicate (TEOS) and methyltriethoxysilane (MTES) for co-precursor, according to TEOS:MTES:
EtOH:H2Hydrochloric acid is added dropwise in O=1:0.3:10:4 (molar ratio) mixing, and adjustment pH value is 3, stirs 20min, promotes filling for silicon source
Divide hydrolysis；
2) ammonium hydroxide is added dropwise to the solution in step 1), adjustment solution ph is 7.5, and the gel time for controlling colloidal sol is
60min or so is conducive to that the hydrosol is adsorbed onto the internal cavities of expanded perlite below；
3) hydrosol is poured into and is filled in the vacuum cylinder that partial size is 0.5~0.9mm expanded perlite, until flooding vacuum cylinder
In expanded perlite；
4) vacuum pump is opened, adjusts the vacuum degree of vacuum pump as 0MPa, pressure stabilizing 5min, subsequent vacuum cylinder pressure is down to often
Remaining colloidal sol discharge is pressed and will be impregnated, waits colloidal sol inside the hole of expanded perlite and surface gel；
5) be combined expanded perlite-SiO after collosol and gel2Aeroge aging 48h in 50 DEG C of ethanol solutions；
6) by the expanded perlite-SiO after aging2Aeroge places trim,ethylchlorosilane: ethyl alcohol: n-hexane=1:1:8
Vacuum pressure impregnation 48h in (volume ratio) mixed solution, wherein trim,ethylchlorosilane: ethyl orthosilicate=3 (molar ratio).
7) drying process are as follows: wet gel sample is successively at 25 DEG C, 40 DEG C, 60 DEG C, 80 DEG C, 100 DEG C, 120 DEG C and 140 DEG C
Freeze-day with constant temperature 1h, 1h, 2h, 2h, 3h, 2h, 2h respectively, are finally cooled to room temperature with drying box and obtain SiO2Aeroge.
Expanded perlite-SiO2Aeroge compound insulating material thermal conductivity is 0.038W/ (mK), and specific surface area is
94.72m2/g；Water absorption rate is 9.8%；Cylindrical compress strength is 196.41KPa.
Embodiment 4
1) with ethyl orthosilicate (TEOS) and methyltriethoxysilane (MTES) for co-precursor, according to TEOS:MTES:
EtOH:H2Hydrochloric acid is added dropwise in O=1:0.3:16:14 (molar ratio) mixing, and adjustment pH value is 2, stirs 35min, promotes filling for silicon source
Divide hydrolysis；
2) ammonium hydroxide is added dropwise to the solution in step 1), adjustment solution pH value is 7, and the gel time for controlling colloidal sol is 60min
Left and right is conducive to that the hydrosol is adsorbed onto the internal cavities of expanded perlite below；
3) hydrosol is poured into and is filled in the vacuum cylinder that partial size is 2~4.7mm expanded perlite, until flooding in vacuum cylinder
Expanded perlite；
4) vacuum pump is opened, the vacuum degree for adjusting vacuum pump is -0.08MPa, pressure stabilizing 35min, subsequent vacuum cylinder pressure
It is down to normal pressure and remaining colloidal sol discharge will be impregnated, wait colloidal sol inside the hole of expanded perlite and surface gel；
5) be combined expanded perlite-SiO after collosol and gel2Aging is for 24 hours in 60 DEG C of ethanol solutions for aeroge；
6) by the expanded perlite-SiO after aging2Aeroge places trim,ethylchlorosilane: ethyl alcohol: n-hexane=1:1:8
Vacuum pressure impregnation 36h in (volume ratio) mixed solution, wherein trim,ethylchlorosilane: ethyl orthosilicate=2.5 (molar ratio).
7) drying process are as follows: wet gel sample is successively at 25 DEG C, 40 DEG C, 60 DEG C, 80 DEG C, 100 DEG C, 120 DEG C and 140 DEG C
Freeze-day with constant temperature 1h, 1h, 2h, 2h, 3h, 2h, 2h respectively, are finally cooled to room temperature with drying box and obtain SiO2Aeroge.
Expanded perlite-SiO2Aeroge compound insulating material thermal conductivity is 0.039W/ (mK), and specific surface area is
85.41m2/g；Water absorption rate is 13.7%；Cylindrical compress strength is 187.91KPa.
Following table 1 illustrates the physical property of 1-4 different-grain diameter composite material of the embodiment of the present invention.
The physical property of 1 different-grain diameter composite material of table
Remarks: the expanded perlite of A:2~4.7mm；A1: the expanded perlite-SiO of 2~4.7mm2Aeroge
The expanded perlite of B:0.9~2mm；B1: the expanded perlite-SiO of 0.9~2mm2Aeroge
The expanded perlite of C:0.5~0.9mm；C1: the expanded perlite-SiO of 0.5~0.9mm2Aeroge
2 vacuum degree of table influences the performance of composite material
As can be seen from the above embodiments, the expanded perlite-SiO of the method for the present invention preparation2Aeroge complex heat-preservation material
Expect that thermal conductivity is not more than 0.040W/ (mK), specific surface area is not less than 85.41m2/g；Water absorption rate is not more than 13.7%；Cylinder pressure
Degree is not less than 187.91KPa.
The present invention is not limited to the above embodiments, on the basis of technical solution disclosed by the invention, the skill of this field
For art personnel according to disclosed technology contents, one can be made to some of which technical characteristic by not needing creative labor
A little replacements and deformation, these replacements and deformation are within the scope of the invention.
Claims (9)
1. a kind of expanded perlite-SiO2The preparation method of aeroge compound insulating material, which comprises the steps of:
1)SiO2The synthesis of aeroge:
According to molar ratio it is 1:0.3:(6~16 by ethyl orthosilicate, methyltriethoxysilane, ethyl alcohol, water): (4~14) are mixed
It closes, salt acid for adjusting pH value is added in mixed liquor, in a water bath heating stirring, ammonia spirit is then added, adjust pH, formed
SiO2Aeroge；
2) expanded perlite-SiO2The preparation of aeroge compound insulating material:
Using vacuum impregnation suction type by SiO2Aeroge is adsorbed onto expanded perlite hole, is replaced through gel aging, solvent
It changes, surface modification, finally through constant pressure and dry, expanded perlite-SiO can be obtained2Aeroge compound insulating material.
2. a kind of expanded perlite-SiO according to claim 12The preparation method of aeroge compound insulating material, it is special
Sign is that the aeroge is hydrophobic aerogels, and pore-size distribution is 2~20nm, and thermal coefficient is not more than 0.0212W/ (m
K)。
3. a kind of expanded perlite-SiO according to claim 12The preparation method of aeroge compound insulating material, it is special
Sign is that the expanded perlite is perforate expanded perlite, and thermal coefficient is 0.042~0.051W/ (mK)；Particle size range
For 0.5~0.9mm, 0.9~2mm and 2~4.7mm.
4. a kind of expanded perlite-SiO according to claim 12The preparation method of aeroge compound insulating material, it is special
Sign is, in step 1), it is 2~3 that salt acid for adjusting pH value, which is added,；20 are persistently stirred in 20~30 DEG C of water-bath magnetic stirring apparatus
~40min；Then ammonia spirit is added, adjusting pH value is 6~8.
5. a kind of expanded perlite-SiO according to claim 12The preparation method of aeroge compound insulating material, it is special
Sign is, in step 2), the solvent replacement and surface modification technology are that normal pressure dipping is modified or vacuum pressure impregnation is modified；Institute
The relative degree of vacuum for stating vacuum impregnation mode is -0.08MPa~0MPa, and the vacuum suction time is 5min~35min.
6. a kind of expanded perlite-SiO according to claim 12The preparation method of aeroge compound insulating material, it is special
Sign is, in step 2), the gel ageing process are as follows: composite material is placed in ethanol solution and is carried out at aging
Reason, gel aging temperature are 50~60 DEG C, and ageing time is 24~48h.
7. a kind of expanded perlite-SiO according to claim 12The preparation method of aeroge compound insulating material, it is special
Sign is that the solvent is replaced and Process of Surface Modification are as follows: composite material is placed on the trimethylchloro-silicane that volume ratio is 1:1:8
Solvent displacement and the modified 24~72h in surface in alkane/dehydrated alcohol/n-hexane mixed solution, wherein in mixed solution, trimethyl chlorine
It is (2~3) that silicone content, which accounts for the ethyl orthosilicate molar ratio in composite material: 1.
8. a kind of expanded perlite-SiO according to claim 12The preparation method of aeroge compound insulating material, it is special
Sign is, in step 2), the drying is constant pressure and dry, successively at 25 DEG C, 40 DEG C, 60 DEG C, 80 DEG C, 100 DEG C, 120 DEG C and 140
Freeze-day with constant temperature 1h, 1h, 2h, 2h, 3h, 2h, 2h are distinguished at DEG C.
9. expanded perlite-SiO according to claim 12The preparation method of aeroge compound insulating material, feature exist
In expanded perlite-SiO2Aeroge compound insulating material thermal conductivity is not more than 0.040W/ (mK), and specific surface area is not less than
85.41m2/g；Water absorption rate is not more than 13.7%；Cylindrical compress strength is not less than 187.91KPa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910379404.9A CN110066189A (en) | 2019-05-08 | 2019-05-08 | A kind of expanded perlite-SiO2The preparation method of aeroge compound insulating material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115368048A (en) * | 2022-09-19 | 2022-11-22 | 河南建筑材料研究设计院有限责任公司 | Modified expanded perlite and preparation method and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0852223A1 (en) * | 1996-12-04 | 1998-07-08 | European Atomic Energy Community (Euratom) | Method of sealing open-pore ceramic coatings, in particular thermal barriers |
| CN1888302A (en) * | 2006-05-22 | 2007-01-03 | 杨大祥 | Process for producing nano porous flexible felt composite material and application |
| CN101372337A (en) * | 2008-09-28 | 2009-02-25 | 厦门大学 | Method for preparing transparent silicon dioxide aerogel by co-precursor normal atmosphere drying |
| CN107759151A (en) * | 2017-10-23 | 2018-03-06 | 中国地质大学（北京） | A kind of expanded perlite SiO2The preparation method of the light heat-insulation wall material of aeroge |
-
2019
- 2019-05-08 CN CN201910379404.9A patent/CN110066189A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0852223A1 (en) * | 1996-12-04 | 1998-07-08 | European Atomic Energy Community (Euratom) | Method of sealing open-pore ceramic coatings, in particular thermal barriers |
| CN1888302A (en) * | 2006-05-22 | 2007-01-03 | 杨大祥 | Process for producing nano porous flexible felt composite material and application |
| CN101372337A (en) * | 2008-09-28 | 2009-02-25 | 厦门大学 | Method for preparing transparent silicon dioxide aerogel by co-precursor normal atmosphere drying |
| CN107759151A (en) * | 2017-10-23 | 2018-03-06 | 中国地质大学（北京） | A kind of expanded perlite SiO2The preparation method of the light heat-insulation wall material of aeroge |
Non-Patent Citations (1)
| Title |
|---|
| 梅阳: "膨胀珍珠岩SiO2气凝胶复合保温材料制备研究", 《中国优秀硕士学位论文全文数据库，工程科技I辑》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115368048A (en) * | 2022-09-19 | 2022-11-22 | 河南建筑材料研究设计院有限责任公司 | Modified expanded perlite and preparation method and application thereof |
| CN115368048B (en) * | 2022-09-19 | 2023-07-14 | 河南建筑材料研究设计院有限责任公司 | Modified expanded perlite and preparation method and application thereof |
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