CN105199472A - Preparation method of aerogel-based heat-insulation phase change coating - Google Patents
Preparation method of aerogel-based heat-insulation phase change coating Download PDFInfo
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Abstract
The invention discloses a preparation method of an aerogel-based heat-insulation phase change coating and belongs to the technical field of heat-insulation materials for buildings. An aerogel-based composite phase change material is used as a main functional filler and is compounded with a film forming emulsion, hollow glass micro-beads, fiber, a dispersing agent, a wetting agent, a film forming additive, a pigment, deionized water, a defoaming agent, a thickening agent and the like in certain proportion to prepare the high-performance aerogel-based heat-insulation phase change coating. The aerogel-based heat-insulation phase change coating has the advantages that the aerogel-based composite phase change material is used as the main functional filler to prepare the high-performance heat-insulation phase change coating, and the heat-insulation phase change coating prepared by means of the preparation method is excellent in heat-insulation performance, flame-retardant, water-proof and long in service life; the preparation method is simple in reaction process, moderate in condition, short in process and suitable for industrial production.
Description
Technical field
The present invention relates to a kind of lagging material technical field for building, particularly a kind of preparation method of airsetting matrix insulation phase-change coating.
Background technology
Along with the significantly propelling of China's process of industrialization, rapid development of economy, urbanization degree improves constantly, and energy problem has become the principal element of restriction Economic development, and save energy is very urgent.And the development of energy-conservation energy storage material, green can be realized with China, energy-conservation, the strategy of sustainable development is closely related.Along with China is to the continuous attention of save energy and protection of the environment, the energy-conservation energy storage technology of building maintenance structure is also being strengthened day by day, and especially External Walls Heating Insulation obtains significant progress, has become the energy-saving building technology that one, China is important.
Insulation phase-change coating is the important materials realizing building energy conservation energy storage, can brush on matrix during use, and easy construction, suitability are wide.Phase transformation component in insulation phase-change coating can utilize the phase transition process of material, absorb and the heat of environment is stored, and when needed by heat release out, effectively can solve between the heat energy Supply and Demand that caused by time, space or intensity and not mate and uneven contradiction.Most widely used in phase change material is solid-liquid phase change material, there is the solid-state transformation to liquid state in its phase transition process, in order to avoid the leakage of phase change material under liquid phase state, needs to prepare composite phase-change material and is shaped by phase change material.Therefore develop a kind of sizing phase-change material of good stability, and be applied to be incubated phase-change coating field, effectively can prevent the leakage because phase change material phase transformation causes.Insulation phase-change coating is applied to external thermal insulation system, greatly can reduces the cold and hot loss of building, improves the effect of energy-saving and emission-reduction.
Summary of the invention
Goal of the invention: the object of the invention is for the deficiencies in the prior art, provides a kind of excellent thermal insulation performance, fire-retardant, waterproof, anti-leak and the preparation method of the airsetting matrix of long service life insulation phase-change coating.
Technical scheme: the preparation method of a kind of Novel air gel base insulation phase-change coating of the present invention, comprises the steps:
(1) silane, organic aldehydes, dehydrated alcohol and hydrochloric acid are mixed by weight 1:0.2 ~ 1:15 ~ 30:0.06 ~ 0.6, at room temperature stir 10 ~ 30min to mix, above-mentioned solution sealing is preserved, wet gel is formed at 20 ~ 80 DEG C of insulation 6 ~ 36h, then the ethanol/water mixed solution in wet gel is removed, add organic solvent and put 20 ~ 70 DEG C of immersion 10 ~ 24h in an oven, the water in displacement wet gel; Above-mentioned steps is repeated 1 ~ 4 time, then the gel after immersion ageing is positioned in baking oven, is warming up to 60 ~ 120 DEG C with the temperature rise rate of 1 ~ 5 DEG C/min, after constant pressure and dry 24 ~ 120h, namely obtains modified Nano hole aerosil;
(2) solubility phase transformation core is dissolved in solvent, under 10 ~ 120 DEG C of conditions, stirs 1 ~ 5h, phase transformation core is dissolved completely, obtain phase transformation core homogeneous phase solution;
(3) the improved silica aerogel carrier of above-mentioned preparation is vacuumized 2 ~ 10h under 40 ~ 200 DEG C of conditions, the duct of matrix is opened completely, obtains body material;
(4) body material described in step (3) is scattered in phase transformation core homogeneous phase solution described in step (2), 2 ~ 24h is stirred at 10 ~ 120 DEG C, then loft drier is placed in, at 40 ~ 80 DEG C, dry 24 ~ 72h, obtains improved silica aerogel base composite phase-change material;
(5) by deionized water, dispersion agent, wetting agent, defoamer, film coalescence aid, pigment by mixing, then the phase transformation of improved silica airsetting matrix described in step (4) composite phase-change material, hollow glass micropearl, fiber mixing is added, then filming emulsion, defoamer are added and mix, add thickening material adjusting viscosity under agitation condition, obtain airsetting matrix insulation phase-change coating.
Preferably, described silane is one or more in 3-aminopropyl trimethoxysilane, 3-aminopropyl dimethylethoxysilane or 3-aminopropyl triethoxysilane.
Preferably, described organic aldehydes is terephthalaldehyde, 4,4
'one or more in-diphenyl-dimethanal or 2 amino-terephthalaldehyde.
Preferably, described acid is one or more in hydrochloric acid, nitric acid, formic acid or acetic acid, and concentration is 0.1molL
-1~ 0.5molL
-1.
Preferably, described is one or more in anhydrous methanol, dehydrated alcohol or normal hexane for removing the organic solvent of the ethanol/water mixed solution in wet gel.
Preferably, described phase transformation core is one or more of polyalcohols, stearic acid, crystalline hydrate salt, inorganic salts or paraffin class.
For avoiding introducing foreign ion, described solvent be preferably in water or ethanol one or both.
Preferably, described polyalcohols specifically comprises polyoxyethylene glycol, tetramethylolmethane, neopentyl glycol, Tutofusin tris, TriMethylolPropane(TMP), 2,2-dihydroxymethyls-propyl alcohol or trimethylolethane.
Preferably, described stearic acid specifically comprises stearic acid, tetradecanoic acid, palmitinic acid capric acid, lauric acid, acetic acid or pentadecylic acid.
Preferably, described crystalline hydrate salt specifically comprises Sodium carbonate decahydrate, sal glauberi, ten hydrogen phosphate dihydrate sodium, calcium chloride hexahydrate, Sodium acetate trihydrate or five water Sulfothiorine.
Preferably, described inorganic salt specifically comprise sodium-chlor, SODIUMNITRATE, sodium carbonate, sodium sulfate, saltpetre, lithium nitrate, Repone K, lithium chloride, lithium chromate or Quilonum Retard.
Preferably, when phase transformation core is inorganic salts described in step (2), dried product described in step (4) need be placed in retort furnace, at 100 ~ 500 DEG C, calcine 1 ~ 10h, furnace cooling, obtains improved silica aerogel base composite phase-change material.
Preferably, when described in step (2), phase transformation core is crystalline hydrate salt, need in step (4) body material stirred and phase transformation core mixing solutions to be put into refrigerator at-5 ~ 5 DEG C of refrigeration 1 ~ 24h, then heat drying, obtains improved silica aerogel base composite phase-change material.
Preferably, the mass ratio of filming emulsion described in step (5), improved silica aerogel base composite phase-change material, hollow glass micropearl, fiber, dispersion agent, wetting agent, film coalescence aid, pigment, deionized water, defoamer, thickening material is 100:1 ~ 40:1 ~ 40:1 ~ 40:0.1 ~ 10:0.1 ~ 10:0.5 ~ 15:0 ~ 15:10 ~ 200:0.1 ~ 3:0.1 ~ 3.
Beneficial effect: (1) is passed through aerogel base composite phase-change material as major function filler, provide the preparation method of a kind of high-performance insulation phase-change coating, insulation phase-change coating prepared by the inventive method, heat-proof quality is excellent, fire-retardant, waterproof and long service life; (2) simple with method reaction process provided by the invention, mild condition, flow process are short, are applicable to suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is the FT-IR figure of the aerosil after hydrophobically modified;
Fig. 2 is the FT-IR figure of improved silica base load P EG2000 composite phase-change material;
Fig. 3 is the DSC figure of improved silica base load P EG2000 composite phase-change material.
Embodiment
Below by accompanying drawing, technical solution of the present invention is described in detail, but protection scope of the present invention is not limited to described embodiment.
Embodiment 1:
By 3-aminopropyl trimethoxysilane, terephthalaldehyde, 0.2molL
-1hydrochloric acid soln and dehydrated alcohol with the mixed in molar ratio of 1:0.33:20:0.4, at room temperature stir 20min Homogeneous phase mixing, above-mentioned solution sealing preserved, form gels at 40 DEG C of insulation 12h.Then the gel obtained is removed unnecessary ethanol/water mixed solution, be immersed in appropriate dehydrated alcohol, continue, after 40 DEG C of insulation 24h, to remove residual chemical substance.Repetition like this 2 times.Then be warming up to 80 DEG C under the program of 1 DEG C/min at heat-up rate, after constant pressure and dry 36h, obtain modified Nano hole aerosil.
The PEG2000 of 0.5g is dissolved in 30mL dehydrated alcohol, makes it dissolve completely under agitation, at 80 DEG C, stir 3h, obtain uniform solution.The improved silica aerogel of 0.125g is vacuumized 4h under 100 DEG C of conditions, the duct of matrix is opened completely.Then the improved silica aerogel through vacuumizing process being scattered in ready PEG2000 solution, at 80 DEG C, stirring 6h hour, be then put in loft drier, dry 36h at 60 DEG C, obtaining improved silica load P EG composite phase-change material.
Deionized water, dispersion agent, wetting agent, defoamer, film coalescence aid, pigment are mixed, then improved silica load P EG composite phase-change material, hollow glass micropearl, fiber mixing is added, then filming emulsion, defoamer are added and mix, stir and add thickening material adjusting viscosity, obtaining airsetting matrix insulation phase-change coating.Wherein, the mass ratio of filming emulsion, improved silica load P EG composite phase-change material, hollow glass micropearl, fiber, dispersion agent, wetting agent, film coalescence aid, deionized water, defoamer, thickening material is 100:5:25:5:1:0.5:2:50:0.3:0.3.
Fig. 1 is the FT-IR figure of the aerosil after hydrophobically modified; Obviously Si-O, CH=N-and-CH is had in figure
3diffraction peak, provablely obtain modified Nano hole aerosil; Fig. 2 is the FT-IR figure of improved silica base load P EG2000 composite phase-change material, obviously has-CH in figure
2-and the diffraction peak of-OH, successfully introduce PEG fragment in matrix material, prove successful synthesis modification silicon dioxide base load P EG2000 composite phase-change material; Fig. 3 is the DSC figure of improved silica base load P EG2000 composite phase-change material, and by finding out in figure that the fusing point of composite phase-change material is 53.85 DEG C, potential heat value is 149.34Jg
-1, there is good thermal storage performance.
Embodiment 2:
By 3-aminopropyl dimethylethoxysilane, 4,4
'-diphenyl-dimethanal, 0.1molL
-1nitric acid, anhydrous methanol with the mixed in molar ratio of 1:0.2:30:0.06, at room temperature stir 10min Homogeneous phase mixing, above-mentioned solution sealing preserved, form gels at 80 DEG C of insulation 6h.Then the gel obtained is removed unnecessary ethanol/water mixed solution, be immersed in appropriate dehydrated alcohol, continue, after 20 DEG C of insulation 10h, to remove residual chemical substance.Repetition like this 1 time.Then be warming up to 120 DEG C under the program of 2.5 DEG C/min at heat-up rate, after constant pressure and dry 24h, obtain modified Nano hole aerosil.
The stearic acid of 0.5g is dissolved in 30mL dehydrated alcohol, makes it dissolve completely under agitation, at 10 DEG C, stir 1h, obtain uniform solution.The improved silica aerogel of 0.125g is vacuumized 2h under 40 DEG C of conditions, the duct of matrix is opened completely.Then the improved silica aerogel through vacuumizing process being scattered in ready stearic acid solution, at 10 DEG C, stirring 2h hour, be then put in loft drier, dry 24h at 40 DEG C, obtaining improved silica load stearic acid composite phase-change material.
Deionized water, dispersion agent, wetting agent, defoamer, film coalescence aid, pigment are mixed, then improved silica load stearic acid composite phase-change material, hollow glass micropearl, fiber mixing is added, then filming emulsion, defoamer are added and mix, stir and add thickening material adjusting viscosity, obtaining airsetting matrix insulation phase-change coating.Wherein, the mass ratio of filming emulsion, improved silica load stearic acid composite phase-change material, hollow glass micropearl, fiber, dispersion agent, wetting agent, film coalescence aid, pigment, deionized water, defoamer, thickening material is 100:1:40:1:0.1:10:15:1:200:0.1:0.1.
Embodiment 3:
By 3-aminopropyl triethoxysilane, 2 amino-terephthalaldehyde, 0.5molL
-1formic acid, normal hexane with the mixed in molar ratio of 1:1:15:0.6, at room temperature stir 30min Homogeneous phase mixing, above-mentioned solution sealing preserved, form gels at 20 DEG C of insulation 36h.Then the gel obtained is removed unnecessary ethanol/water mixed solution, be immersed in appropriate dehydrated alcohol, continue, after 70 DEG C of insulation 24h, to remove residual chemical substance.Repetition like this 4 times.Then be warming up to 60 DEG C under the program of 5 DEG C/min at heat-up rate, after constant pressure and dry 120h, obtain modified Nano hole aerosil.
The paraffin of 0.5g is dissolved in 30mL dehydrated alcohol, makes it dissolve completely under agitation, at 120 DEG C, stir 5h, obtain uniform solution.The improved silica aerogel of 0.125g is vacuumized 10h under 200 DEG C of conditions, the duct of matrix is opened completely.Then the improved silica aerogel through vacuumizing process being scattered in ready paraffin solution, at 120 DEG C, stirring 24h hour, be then put in loft drier, dry 72h at 80 DEG C, obtaining improved silica load paraffin composite phase change material.
By deionized water, dispersion agent, wetting agent, defoamer, film coalescence aid, pigment by mixing, then improved silica load paraffin composite phase change material, hollow glass micropearl, fiber mixing is added, then filming emulsion, defoamer are added and mix, stir and add thickening material adjusting viscosity, obtaining airsetting matrix insulation phase-change coating.Wherein, the mass ratio of filming emulsion, improved silica load paraffin composite phase change material, hollow glass micropearl, fiber, dispersion agent, wetting agent, film coalescence aid, pigment, deionized water, defoamer, thickening material is 100:40:1:40:10:0.1:0.5:15:10:3:3.
Embodiment 4:
3-aminopropyl trimethoxysilane, terephthalaldehyde, 0.2molL
-1acetic acid solution and dehydrated alcohol with the mixed in molar ratio of 1:0.33:20:0.4, at room temperature stir 20min Homogeneous phase mixing, above-mentioned solution sealing preserved, form gels at 20 DEG C of insulation 36h.Then the gel obtained is removed unnecessary ethanol/water mixed solution, be immersed in appropriate dehydrated alcohol, continue, after 40 DEG C of insulation 24h, to remove residual chemical substance.Repetition like this 2 times.Then be warming up to 80 DEG C under the program of 1 DEG C/min at heat-up rate, after constant pressure and dry 120h, obtain modified Nano hole aerosil.
8g lithium nitrate is dissolved in the deionized water of 10mL, makes it dissolve completely under agitation, at 40 DEG C, stir 3h, obtain uniform solution.The improved silica aerogel of above-mentioned for 3.5g preparation is vacuumized 4h under 100 DEG C of conditions, the duct of matrix is opened completely.Then the improved silica aerogel through vacuumizing process being scattered in ready lithium nitrate solution, at 80 DEG C, stirring 6h hour, be then put in loft drier, dry 20h at 110 DEG C.Products therefrom is placed in retort furnace, calcines 2h, furnace cooling at 310 DEG C.Obtain the aerogel carried lithium nitrate composite phase-change material of improved silica.
By deionized water, dispersion agent, wetting agent, defoamer, film coalescence aid, pigment by mixing, then the aerogel carried lithium nitrate composite phase-change material of improved silica, hollow glass micropearl, fiber mixing is added, then filming emulsion, defoamer are added and mix, stir and add thickening material adjusting viscosity, obtaining airsetting matrix insulation phase-change coating.Wherein, the mass ratio of filming emulsion, the aerogel carried lithium nitrate composite phase-change material of improved silica, hollow glass micropearl, fiber, dispersion agent, wetting agent, film coalescence aid, pigment, deionized water, defoamer, thickening material is 100:10:5:15:1:2:1:2:80:0.3:0.3.
Embodiment 5:
By 3-aminopropyl trimethoxysilane, terephthalaldehyde, 0.2molL
-1hydrochloric acid soln and dehydrated alcohol with the mixed in molar ratio of 1:0.33:20:0.4, at room temperature stir 20min Homogeneous phase mixing, above-mentioned solution sealing preserved, form gels at 40 DEG C of insulation 12h.Then the gel obtained is removed unnecessary ethanol/water mixed solution, be immersed in appropriate dehydrated alcohol, continue, after 40 DEG C of insulation 24h, to remove residual chemical substance.Repetition like this 2 times.Then be warming up to 80 DEG C under the program of 1 DEG C/min at heat-up rate, after constant pressure and dry 36h, obtain modified Nano hole aerosil.
8g Sodium carbonate decahydrate is dissolved in the deionized water of 10mL, makes it dissolve completely under agitation, at 40 DEG C, stir 3h, obtain uniform solution.The improved silica aerogel of above-mentioned for 3.5g preparation is vacuumized 4h under 100 DEG C of conditions, the duct of matrix is opened completely.Then the improved silica aerogel through vacuumizing process being scattered in ready Sodium carbonate decahydrate solution, at 80 DEG C, stirring 6h hour, be then put in loft drier, dry 20h at 110 DEG C.Products therefrom is placed in retort furnace, calcines 2h, furnace cooling at 310 DEG C.Obtain the aerogel carried lithium nitrate composite phase-change material of improved silica.
By deionized water, dispersion agent, wetting agent, defoamer, film coalescence aid, pigment by mixing, then the aerogel carried Sodium carbonate decahydrate composite phase-change material of improved silica, hollow glass micropearl, fiber mixing is added, then filming emulsion, defoamer are added and mix, stir and add thickening material adjusting viscosity, obtaining airsetting matrix insulation phase-change coating.Wherein, the mass ratio of filming emulsion, the aerogel carried Sodium carbonate decahydrate composite phase-change material of improved silica, hollow glass micropearl, fiber, dispersion agent, wetting agent, film coalescence aid, pigment, deionized water, defoamer, thickening material is 100:10:5:15:1:2:1:2:80:0.3:0.3.
As mentioned above, although represented with reference to specific preferred embodiment and described the present invention, it shall not be construed as the restriction to the present invention self.Under the spirit and scope of the present invention prerequisite not departing from claims definition, various change can be made in the form and details to it.
Claims (10)
1. a preparation method for Novel air gel base insulation phase-change coating, is characterized in that comprising the steps:
(1) silane, organic aldehydes, dehydrated alcohol and acid are mixed by weight 1:0.2 ~ 1:15 ~ 30:0.06 ~ 0.6, at room temperature stir 10 ~ 30min to mix, above-mentioned solution sealing is preserved, wet gel is formed at 20 ~ 80 DEG C of insulation 6 ~ 36h, then the ethanol/water mixed solution in wet gel is removed, add organic solvent and put 20-70 DEG C of immersion 10 ~ 24h in an oven, the water in displacement wet gel; Above-mentioned steps is repeated 1 ~ 4 time, then the gel after immersion ageing is positioned in baking oven, is warming up to 60 ~ 120 DEG C with the temperature rise rate of 1 ~ 5 DEG C/min, after constant pressure and dry 24 ~ 120h, namely obtains modified Nano hole aerosil;
(2) solubility phase transformation core is dissolved in solvent, under 10 ~ 120 DEG C of conditions, stirs 1 ~ 5h, phase transformation core is dissolved completely, obtain phase transformation core homogeneous phase solution;
(3) the improved silica aerogel carrier of above-mentioned preparation is vacuumized 2 ~ 10h under 40 ~ 200 DEG C of conditions, the duct of matrix is opened completely, obtains body material;
(4) body material described in step (3) is scattered in phase transformation core homogeneous phase solution described in step (2), 2 ~ 24h is stirred at 10 ~ 120 DEG C, then loft drier is placed in, at 40 ~ 80 DEG C, dry 24 ~ 72h, obtains improved silica aerogel base composite phase-change material;
(5) by deionized water, dispersion agent, wetting agent, defoamer, film coalescence aid, pigment by mixing, then the phase transformation of improved silica airsetting matrix described in step (4) composite phase-change material, hollow glass micropearl, fiber mixing is added, then filming emulsion, defoamer are added and mix, add thickening material adjusting viscosity under agitation condition, obtain airsetting matrix insulation phase-change coating.
2. the preparation method of improved silica aerogel base composite phase-change material according to claim 1, is characterized in that: silane described in step (1) is one or more in 3-aminopropyl trimethoxysilane, 3-aminopropyl dimethylethoxysilane or 3-aminopropyl triethoxysilane.
3. the preparation method of Novel air gel base according to claim 1 insulation phase-change coating, is characterized in that described phase transformation core is one or more of polyalcohols, stearic acid, crystalline hydrate salt, inorganic salts or paraffin class.
4. the preparation method of Novel air gel base insulation phase-change coating according to claim 2, it is characterized in that described polyalcohols is polyoxyethylene glycol, tetramethylolmethane, neopentyl glycol, Tutofusin tris, TriMethylolPropane(TMP), 2,2-dihydroxymethyls-propyl alcohol or trimethylolethane.
5. the preparation method of Novel air gel base insulation phase-change coating according to claim 2, is characterized in that described stearic acid is stearic acid, tetradecanoic acid, palmitinic acid capric acid, lauric acid, acetic acid or pentadecylic acid.
6. the preparation method of Novel air gel base insulation phase-change coating according to claim 2, is characterized in that described crystalline hydrate salt is Sodium carbonate decahydrate, sal glauberi, ten hydrogen phosphate dihydrate sodium, calcium chloride hexahydrate, Sodium acetate trihydrate or five water Sulfothiorine.
7. the preparation method of Novel air gel base insulation phase-change coating according to claim 2, is characterized in that described inorganic salt are sodium-chlor, SODIUMNITRATE, sodium carbonate, sodium sulfate, saltpetre, lithium nitrate, Repone K, lithium chloride, lithium chromate or Quilonum Retard.
8. the preparation method of Novel air gel base insulation phase-change coating according to claim 1, it is characterized in that, when described in step (2), phase transformation core is inorganic salts, dried product described in step (4) need be placed in retort furnace, 1 ~ 10h is calcined at 100 ~ 500 DEG C, furnace cooling, obtains improved silica aerogel base composite phase-change material.
9. the preparation method of Novel air gel base insulation phase-change coating according to claim 1, it is characterized in that, when described in step (2), phase transformation core is crystalline hydrate salt, need in step (4) body material stirred and phase transformation core mixing solutions to be put into refrigerator at-5 ~ 5 DEG C of refrigeration 1 ~ 24h, then heat drying, obtains improved silica aerogel base composite phase-change material.
10. the preparation method of Novel air gel base insulation phase-change coating according to claim 1, it is characterized in that, the mass ratio of filming emulsion described in step (5), improved silica aerogel base composite phase-change material, hollow glass micropearl, fiber, dispersion agent, wetting agent, film coalescence aid, pigment, deionized water, defoamer, thickening material is 100:1 ~ 40:1 ~ 40:1 ~ 40:0.1 ~ 10:0.1 ~ 10:0.5 ~ 15:0 ~ 15:10 ~ 200:0.1 ~ 3:0.1 ~ 3.
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