CN107382265A - A kind of modified aerogels heat-insulating heat-preserving material and preparation method thereof - Google Patents
A kind of modified aerogels heat-insulating heat-preserving material and preparation method thereof Download PDFInfo
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- CN107382265A CN107382265A CN201710615722.1A CN201710615722A CN107382265A CN 107382265 A CN107382265 A CN 107382265A CN 201710615722 A CN201710615722 A CN 201710615722A CN 107382265 A CN107382265 A CN 107382265A
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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
- C04B30/00—Compositions for artificial stone, not containing binders
- C04B30/02—Compositions for artificial stone, not containing binders containing fibrous materials
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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
- 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
- C04B2111/27—Water resistance, i.e. waterproof or water-repellent materials
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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
- 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
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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
- 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
Abstract
Mixed the invention discloses a kind of modified aerogels heat-insulating heat-preserving material and preparation method thereof, including by 40 50 parts of 10 20 parts of tetraethyl orthosilicate, 12 15 parts of butyl titanate and ethanol；The 20min of magnetic agitation 10；25 35 parts of 8 10 parts of ammoniacal liquor and water, static 16 24h, you can obtain the TiO is added dropwise2‑SiO2Colloidal sol；By TiO2‑SiO210 15 parts of colloidal sol, 8 12 parts of nanofiber, nano titanium dioxide powder mixings, in 60 70 DEG C of 30 40min of stirring of temperature；8 10 parts of methyl benzilate, 8 10 parts of dicyclohexyl phthalate, 12 15 parts of ethylenediamine tetra-acetic acid are added, impregnates 2 4h at 50 60 DEG C of temperature；Subsequent warming while stirring continues to stir 20 30min to 80 100 DEG C, and drying is that can obtain the modified aerogels heat-insulating heat-preserving material after cooling.
Description
Technical field
The invention belongs to heat-insulating heat-preserving material field, more particularly to a kind of modified aerogels heat-insulating heat-preserving material and its preparation
Method.
Background technology
China is in industrialization and urbanization Rapid development stage, and economic fast development will certainly cause China to build
Energy consumption consumption is in rapid growth period.Between past few years, the annual new building area in China increases substantially, and turns into maximum in the world
Construction market.If with reference to current building energy consumption situation, 1.2 trillion kW.h of consumption and 4.1 hundred million t are marked into coal every year, approached
3 times of current national building energy consumption.The energy consumption of building materials has accounted for the 35% of national energy consumption.Therefore, building energy conservation turns into state
The Vital Strategic Problems of family.In the existing heat-insulating heat-preserving material in China, the insulation material for meeting national A levels (non-ignitable) standard mainly has
Expanded perlite thermal-nsulation coating, adhesive powder-polystyrene granule thermal insulation mortar and rock wool etc., wherein, pearlite insulation coating and adhesive polystyrene
Granule thermal insulation slurry heat-insulating property is bad, although and rock wool heat-insulating property is fine, be constrained to mineral reserve abundance and exploitation amount,
It is not produced on a large scale.
SiO2Aeroge is exactly typical super insulating material, under normal temperature and pressure, SiO2The overall thermal conductivity factor of aeroge can
As little as 0.015W/ (m.K) below, SiO2Aeroge is a kind of ultra-fine SiO by nanometer scale2Particle phase mutually assembles composition nanometer
Porous network, and a kind of unbodied high dispersive solid-state material full of gaseous state decentralized medium in hole, it has macroscopical spy concurrently
Property and make it have ultralow thermal conductivity factor the characteristics of nano effect, turn into most typical meaning, study most deep, heat-insulating property
One of most excellent super insulating material.However, traditional pure SiO2But poor mechanical property, the easy moisture absorption, brittle be present in aeroge
The deficiencies of splitting, it is impossible to directly apply.
The content of the invention
For drawbacks described above, it is an object of the invention to provide a kind of modified aerogels heat-insulating heat-preserving material and its preparation side
Method, by TiO2-SiO2Colloidal sol is modified, and strengthens the mechanical properties such as its intensity, toughness, it is possessed nonflammable, heat conduction system
The features such as number is low, hydrophobic effect is good.
A kind of preparation method of modified aerogels heat-insulating heat-preserving material, is comprised the following steps：
(1) tetraethyl orthosilicate 10-20 parts, butyl titanate 12-15 parts and the mixing of ethanol 40-50 parts；Magnetic agitation 10-
20min；Ammoniacal liquor 8-10 parts and water 25-35 parts, static 16-24h, you can obtain the TiO is added dropwise2-SiO2Colloidal sol；
(2) TiO that will be prepared in step (1)2-SiO2Colloidal sol, nanofiber 8-12 parts, nano titanium dioxide powder
10-15 parts mix, in 60-70 DEG C of stirring 30-40min of temperature；
(3) methyl benzilate 8-10 parts, dicyclohexyl phthalate 8-10 parts, second two are added into step (2)
Amine tetraacethyl 12-15 parts, impregnate 2-4h at 50-60 DEG C of temperature；
(4) then warming while stirring to 80-100 DEG C, continue stir 20-30min, after cooling drying i.e. can obtain it is described
Modified aerogels heat-insulating heat-preserving material.
Preferably, step (4) includes needing to add methyl benzilate 8-10 parts, adjacent benzene again after drying after cooling down
Dioctyl phthalate dicyclohexyl maleate 8-10 parts, ethylenediamine tetra-acetic acid 12-15 parts, rise temperature react 1- while stirring to 100-120 DEG C
3h, reaction cooling, dry.
Preferably, 45 parts of 16 parts of step (1) tetraethyl orthosilicate, 13 parts of butyl titanate and ethanol mixing；Magnetic agitation
16min；28 parts of 9 parts of ammoniacal liquor and water, static 20h is added dropwise.
Preferably, 13 parts of 10 parts of nanofiber described in step (2), nano titanium dioxide powder mixings, in temperature
65 DEG C of stirring 35min.
Preferably, 9 parts of methyl benzilate described in step (3), 10 parts of dicyclohexyl phthalate, ethylenediamine tetraacetic
15 parts of acetic acid, impregnate 3h at 55 DEG C of temperature.
Preferably, warming while stirring to 90 DEG C, continues to stir 25min in step (4).
Preferably, added again described in step (4) 8 parts of methyl benzilate, 8 parts of dicyclohexyl phthalate,
12 parts of ethylenediamine tetra-acetic acid, rise temperature react 1.5h while stirring to 115 DEG C.
Preferably, the heat-insulated guarantor of modified aerogels being prepared according to the preparation method of modified aerogels heat-insulating heat-preserving material
Adiabator.
Compared with prior art, its advantage is the present invention：
A kind of preparation method of modified aerogels heat-insulating heat-preserving material of the present invention, prepares TiO2-SiO2Colloidal sol, with
Aeroge is merely with SiO in the prior art2Compare, structural strength is strengthened；By adding nanofiber, nanometer titanium dioxide
Titanium valve, micron matter composite construction is formed, improve intensity and toughness；By adding methyl benzilate, the ring of phthalic acid two
The materials such as own ester, hydrophilic radical is substituted with inertia group, makes its surface-hydrophobicized, while prevented because absorbing water to the heat-insulated effect of material
The influence of fruit.
Embodiment
The present invention is further illustrated with reference to embodiments.
Embodiment 1
(1) 50 parts of 10 parts of tetraethyl orthosilicate, 15 parts of butyl titanate and ethanol mixing；Magnetic agitation 10min；Ammoniacal liquor 10 is added dropwise
25 parts of part and water, static 16h, you can obtain the TiO2-SiO2Colloidal sol；
(2) TiO that will be prepared in step (1)2-SiO2Colloidal sol, 8 parts of nanofiber, 15 parts of nano titanium dioxide powder
Mix, 30min is stirred in temperature 60 C；
(3) 8 parts of methyl benzilate, 10 parts of dicyclohexyl phthalate, ethylenediamine tetrem are added into step (2)
12 parts of acid, impregnates 2h under temperature 60 C；
(4) then warming while stirring to 80 DEG C, continues to stir 20min, and drying is that can obtain the modified gas after cooling
Gel heat-insulation insulation material.
Embodiment 2
(1) 40 parts of 20 parts of tetraethyl orthosilicate, 12 parts of butyl titanate and ethanol mixing；Magnetic agitation 20min；Ammoniacal liquor 8 is added dropwise
35 parts of part and water, static 24h, you can obtain the TiO2-SiO2Colloidal sol；
(2) TiO that will be prepared in step (1)2-SiO2Colloidal sol, 12 parts of nanofiber, nano titanium dioxide powder 10
Part is mixed, and 40min is stirred in temperature 70 C；
(3) 10 parts of methyl benzilate, 8 parts of dicyclohexyl phthalate, ethylenediamine tetrem are added into step (2)
15 parts of acid, impregnates 4h under temperature 50 C；
(4) then warming while stirring to 100 DEG C, continues to stir 30min, and drying is that can obtain the modified gas after cooling
Gel heat-insulation insulation material.
Embodiment 3
(1) 45 parts of 13 parts of tetraethyl orthosilicate, 14 parts of butyl titanate and ethanol mixing；Magnetic agitation 15min；Ammoniacal liquor 9 is added dropwise
30 parts of part and water, static 18h, you can obtain the TiO2-SiO2Colloidal sol；
(2) TiO that will be prepared in step (1)2-SiO2Colloidal sol, 10 parts of nanofiber, nano titanium dioxide powder 11
Part mixes, in 65 DEG C of stirring 40min of temperature；
(3) 9 parts of methyl benzilate, 8 parts of dicyclohexyl phthalate, ethylenediamine tetrem are added into step (2)
14 parts of acid, impregnates 2.5h under temperature 50 C；
(4) then warming while stirring to 90 DEG C, continues to stir 26min, dried after cooling；Diphenylglycollic acid is added again
8 parts of methyl esters, 10 parts of dicyclohexyl phthalate, 14 parts of ethylenediamine tetra-acetic acid, rise temperature are reacted while stirring to 105 DEG C
1.5h, it is that can obtain the modified aerogels heat-insulating heat-preserving material that reaction, which is cooled down, dried,.
Embodiment 4
(1) 50 parts of 18 parts of tetraethyl orthosilicate, 13 parts of butyl titanate and ethanol mixing；Magnetic agitation 20min；Ammoniacal liquor 8 is added dropwise
28 parts of part and water, static 20h, you can obtain the TiO2-SiO2Colloidal sol；
(2) TiO that will be prepared in step (1)2-SiO2Colloidal sol, 12 parts of nanofiber, nano titanium dioxide powder 14
Part mixes, in 68 DEG C of stirring 30min of temperature；
(3) 8 parts of methyl benzilate, 10 parts of dicyclohexyl phthalate, ethylenediamine tetrem are added into step (2)
12 parts of acid, impregnate 3h at 58 DEG C of temperature；
(4) then warming while stirring to 85 DEG C, continues to stir 24min, dried after cooling；Diphenylglycollic acid is added again
10 parts of methyl esters, 8 parts of dicyclohexyl phthalate, 12 parts of ethylenediamine tetra-acetic acid, rise temperature are reacted while stirring to 115 DEG C
3h, it is that can obtain the modified aerogels heat-insulating heat-preserving material that reaction, which is cooled down, dried,.
Embodiment 5
(1) 45 parts of 16 parts of tetraethyl orthosilicate, 13 parts of butyl titanate and ethanol mixing；Magnetic agitation 16min；Ammoniacal liquor 9 is added dropwise
28 parts of part and water, static 20h, you can obtain the TiO2-SiO2Colloidal sol；
(2) TiO that will be prepared in step (1)2-SiO2Colloidal sol, 10 parts of nanofiber, nano titanium dioxide powder 13
Part mixes, in 65 DEG C of stirring 35min of temperature；
(3) 9 parts of methyl benzilate, 10 parts of dicyclohexyl phthalate, ethylenediamine tetrem are added into step (2)
15 parts of acid, impregnate 3h at 55 DEG C of temperature；
(4) then warming while stirring to 90 DEG C, continues to stir 25min, dried after cooling；Diphenylglycollic acid is added again
8 parts of methyl esters, 8 parts of dicyclohexyl phthalate, 12 parts of ethylenediamine tetra-acetic acid, rise temperature are reacted while stirring to 115 DEG C
1.5h, it is that can obtain the modified aerogels heat-insulating heat-preserving material that reaction, which is cooled down, dried,.
Correlated performance test, in detail knot are carried out to the modified aerogels heat-insulating heat-preserving material obtained by above-mentioned each embodiment
Fruit see the table below：
| Experiment | Thermal conductivity factor (W/ (mk)) | Compression strength (MPa) | Hydrophobicity (contact angle °) |
| Embodiment 1 | 0.020 | 1.24 | 126 |
| Embodiment 2 | 0.018 | 1.20 | 128 |
| Embodiment 3 | 0.015 | 1.48 | 145 |
| Embodiment 4 | 0.013 | 1.42 | 148 |
| Embodiment 5 | 0.011 | 1.5 | 150 |
The invention is not restricted to embodiment here, those skilled in the art do not depart from the present invention according to the announcement of the present invention
The improvement and modification that category is made all should be within protection scope of the present invention.
Claims (8)
1. a kind of preparation method of modified aerogels heat-insulating heat-preserving material, it is characterised in that comprise the following steps：
(1) tetraethyl orthosilicate 10-20 parts, butyl titanate 12-15 parts and the mixing of ethanol 40-50 parts；Magnetic agitation 10-20min；Drop
Ammonification water 8-10 parts and water 25-35 parts, static 16-24h, you can obtain the TiO2-SiO2 colloidal sols；
(2) by the TiO2-SiO2 colloidal sols being prepared in step (1), nanofiber 8-12 parts, nano titanium dioxide powder 10-
15 parts of mixings, in 60-70 DEG C of stirring 30-40min of temperature；
(3) methyl benzilate 8-10 parts, dicyclohexyl phthalate 8-10 parts, ethylenediamine tetraacetic are added into step (2)
Acetic acid 12-15 parts, impregnate 2-4h at 50-60 DEG C of temperature；
(4) then warming while stirring to 80-100 DEG C, continues to stir 20-30min, and drying is that can obtain the modification after cooling
Aerogel thermal insulation material.
A kind of 2. preparation method of modified aerogels heat-insulating heat-preserving material according to claim 1, it is characterised in that step
(4) include needing to add methyl benzilate 8-10 parts, dicyclohexyl phthalate 8-10 again after drying after cooling down
Part, ethylenediamine tetra-acetic acid 12-15 parts, rise temperature are reacted 1-3h, reaction cooling, dried while stirring to 100-120 DEG C.
A kind of 3. preparation method of modified aerogels heat-insulating heat-preserving material according to claim 1, it is characterised in that step
(1) 45 parts of 16 parts of the tetraethyl orthosilicate, 13 parts of butyl titanate and ethanol mixing；Magnetic agitation 16min；Be added dropwise 9 parts of ammoniacal liquor and
28 parts of water, static 20h.
A kind of 4. preparation method of modified aerogels heat-insulating heat-preserving material according to claim 1, it is characterised in that step
(2) 13 parts of nanofiber 10 described in part, nano titanium dioxide powder mixings, in 65 DEG C of stirring 35min of temperature.
A kind of 5. preparation method of modified aerogels heat-insulating heat-preserving material according to claim 1, it is characterised in that step
(3) methyl benzilate 9 described in part, 10 parts of dicyclohexyl phthalate, 15 parts of ethylenediamine tetra-acetic acid, in 55 DEG C of temperature
Lower dipping 3h.
A kind of 6. preparation method of modified aerogels heat-insulating heat-preserving material according to claim 1, it is characterised in that step
(4) warming while stirring continues to stir 25min to 90 DEG C in.
A kind of 7. preparation method of modified aerogels heat-insulating heat-preserving material according to claim 2, it is characterised in that step
(4) 8 parts of methyl benzilate, 8 parts of dicyclohexyl phthalate, 12 parts of ethylenediamine tetra-acetic acid are added described in again, is risen
High-temperature reacts 1.5h while stirring to 115 DEG C.
8. it is prepared into according to a kind of preparation method of modified aerogels heat-insulating heat-preserving material described in any one of claim 1-7
The modified aerogels heat-insulating heat-preserving material arrived.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108585762A (en) * | 2018-05-30 | 2018-09-28 | 巩义市泛锐熠辉复合材料有限公司 | The preparation method of heat-insulation and heat-preservation aerosil felt |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108585762A (en) * | 2018-05-30 | 2018-09-28 | 巩义市泛锐熠辉复合材料有限公司 | The preparation method of heat-insulation and heat-preservation aerosil felt |
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