CN109370532A - A kind of phase-change heat-insulating coating and preparation method thereof based on phase-transition heat-storage - Google Patents
A kind of phase-change heat-insulating coating and preparation method thereof based on phase-transition heat-storage Download PDFInfo
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- CN109370532A CN109370532A CN201811251371.1A CN201811251371A CN109370532A CN 109370532 A CN109370532 A CN 109370532A CN 201811251371 A CN201811251371 A CN 201811251371A CN 109370532 A CN109370532 A CN 109370532A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/02—Materials undergoing a change of physical state when used
- C09K5/06—Materials undergoing a change of physical state when used the change of state being from liquid to solid or vice versa
- C09K5/063—Materials absorbing or liberating heat during crystallisation; Heat storage materials
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- 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
- B01J13/02—Making microcapsules or microballoons
- B01J13/06—Making microcapsules or microballoons by phase separation
- B01J13/14—Polymerisation; cross-linking
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D123/00—Coating compositions based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Coating compositions based on derivatives of such polymers
- C09D123/02—Coating compositions based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment
- C09D123/04—Homopolymers or copolymers of ethene
- C09D123/08—Copolymers of ethene
- C09D123/0846—Copolymers of ethene with unsaturated hydrocarbons containing other atoms than carbon or hydrogen atoms
- C09D123/0853—Vinylacetate
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D125/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Coating compositions based on derivatives of such polymers
- C09D125/02—Homopolymers or copolymers of hydrocarbons
- C09D125/04—Homopolymers or copolymers of styrene
- C09D125/08—Copolymers of styrene
- C09D125/14—Copolymers of styrene with unsaturated esters
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D131/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an acyloxy radical of a saturated carboxylic acid, of carbonic acid, or of a haloformic acid; Coating compositions based on derivatives of such polymers
- C09D131/02—Homopolymers or copolymers of esters of monocarboxylic acids
- C09D131/04—Homopolymers or copolymers of vinyl acetate
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/141—Feedstock
Abstract
The invention discloses a kind of paraffin/porous activated carbon-Lauxite phase-change microcapsules, which is characterized in that phase-change material is paraffin, carrier of the porous activated carbon as phase-change material, capsule skin of the Lauxite as phase-change microcapsule in the microcapsules.The invention also discloses a kind of phase-change heat-insulating coating and preparation method thereof based on phase-transition heat-storage.Thermal insulation coatings of the invention are using paraffin/porous activated carbon-micro- glue of Lauxite phase transformation as functional stuffing, it is big with latent heat of phase change, energy storage is high, the advantages that temperature adjustment ability is strong, simultaneously, paraffin is adsorbed in the hole of active carbon by using cellular porous active carbon, and the cladding of Lauxite is overlayed in the surface of active carbon, to reach the problem of preventing phase-change material paraffin from revealing, and, hole in porous activated carbon is interconnected, when phase-change material paraffin is solid-liquid conversion in this way, it can be flowed and be solidified in the hole of active carbon, reduce its impact to coating Lauxite.
Description
Technical field
The present invention relates to technical field of coatings, and in particular to a kind of phase-change heat-insulating coating and its preparation based on phase-transition heat-storage
Method.
Background technique
Architectural energy consumption occupies significant portion in social total energy consumption, and in order to solve the problems, such as architectural energy consumption, people throw sight
To phase-change material.
Phase-change material is a kind of heat function material that can absorb or discharge latent heat, phase transformation different from insulating wall material
Material application does not terminate in heat preservation under construction, it can also participate in the storage and utilization of building heat-energy, enable phase-change material
Heat-insulated, the heat insulation effect times over equivalent Conventional insulation are generated, while being reduced by the circulation of high temperature endothermic, Exotherm
The frequency of indoor air temperature fluctuation, maintains the temperature in a longer period and approaches with required temperature, increases human body and relaxes
Appropriateness, while reaching energy saving purpose, meet and currently build the trend developed to multilayer, light structures direction, imitates building energy conservation
Fruit is more significant.
And build be concentrated mainly on interior wall coating field using phase-change material at present, by that will have the phase of heat accumulation function
Become material to be filled in coating, heat is absorbed and released by phase-change material, to achieve the purpose that adjust room temperature.But
It is that existing phase-change heat-insulating coating temperature adjusting performance, heat storage performance do not reach requirement also, and phase-change material itself is there are volume change,
The problems such as being easy to appear phase-change material leakage, mutually separating, to influence the temperature adjusting performance of phase-change material.
For this purpose, (application number: 201010124626.5) disclosing a kind of composite phase change energy-storing architectural coating in Chinese patent
And preparation method thereof.The phase-change energy-storage composite material is used using expanded perlite as basis material, with ionic liquid at room temperature,
The phase-change materials such as straight chain fatty acid, alkane constitute compound phase-changing energy storage material, then newborn with styrene-acrylic emulsion, pure-acrylic emulsion, second third
The one or more of liquid mix macromolecule filming material by a certain percentage, and after being thoroughly mixed uniformly, standing can be obtained
To the building coating with phase change energy storage function.The phase-change energy-storage composite material is by using vacuum suction method by organic phase-change material
Material is absorbed into the porous structure of expanded perlite, is existed and is adsorbed defective tightness to organic phase change material, over numerous cycles
The problem of being easy leakage, to influence the thermoregulation effect of phase-change material.
Summary of the invention
In view of the above-mentioned analysis to the prior art, the present invention provides a kind of phase-change heat-insulating coating based on phase-transition heat-storage, should
Coating has many advantages, such as that latent heat of phase change is big, energy storage is high, insulating power is strong, while having volume stability using phase-change microcapsule
It is good, it is not easy to reveal, and temperature adjustment ability is strong.
In order to achieve the above object, the present invention is achieved through the following technical solutions:
A kind of paraffin/porous activated carbon-Lauxite phase-change microcapsule, phase-change material is paraffin, porous work in the microcapsules
Carrier of the property charcoal as phase-change material, capsule skin of the Lauxite as phase-change microcapsule, the enthalpy of phase change 162.7J/ of the microcapsules
G, phase transition temperature are 30.8 DEG C, and average grain diameter is 18.46 μm, and thermal coefficient is 0.235W/ (mK).
Preferably, the present invention provides the preparation sides of above-mentioned paraffin/porous activated carbon-Lauxite phase-change microcapsule
Method, comprising the following steps:
(1) porous activated carbon is placed in acetone soln, after being cleaned by ultrasonic 5min, with deionized water diafiltration, is dried in vacuo standby
With；
(2) it weighs a certain amount of paraffin and deionized water is mixed and heated, be added emulsifier after paraffin melts completely, and with height
Fast mulser emulsifies paraffin solution, is subsequently placed in three-necked flask and carries out heating water bath, and keeps the temperature at a temperature of 70 DEG C
10min obtains paraffin wax emulsions；
(3) urea liquid for taking melamine powder and mass fraction 35% and a certain amount of deionized water are to 100mL three-necked flask
In, and triethanolamine is added dropwise, system pH is adjusted to 8-9, system temperature is increased to 70 DEG C while stirring, and at 70 DEG C
5min is kept the temperature, urea resin prepolymer is obtained；
(4) paraffin wax emulsions made from step (2) are added drop-wise in the porous activated carbon in step (1), are stirred when being added dropwise, mistake
Filter, it is dry, obtain the porous activated carbon that load has paraffin；
(5) there is the porous activated carbon of paraffin to put into urea resin prepolymer the load in step (4), while stirring plus
Heat, and 1h is kept the temperature at 60 DEG C, it discharges, filters, wash, it is dry, obtain paraffin/porous activated carbon-micro- glue of Lauxite phase transformation
Capsule.
Preferably, the emulsifier is Tween-80 and neopelex is the compound of 3:1 in mass ratio.
Preferably, the phase-transition heat-preserving applies the present invention provides a kind of phase-change heat-insulating coating based on phase-transition heat-storage
Material is functional stuffing, talcum powder, titanium white by paraffin/porous activated carbon-Lauxite phase-change microcapsule described in claim 1
Powder, lotion, coalescing agent, defoaming agent, thickener, dispersing agent and deionized water are prepared as a raw material.
Preferably, the phase-change heat-insulating coating is made of raw material from the following weight: paraffin/porous activated carbon-ureaformaldehyde
20-40 parts of resin phase-change microcapsule, 60-80 parts of talcum powder, 45-65 parts of titanium dioxide, 100-150 parts of lotion, coalescing agent 1-3
Part, 0.5-1 parts of defoaming agent, 1-2 parts of thickener, 0.5-1.5 parts of dispersing agent, 180-240 parts of deionized water.
Preferably, the lotion is one of styrene-acrylic emulsion, tertiary vinegar milk liquid, ethyl vinyl acetate lotion.
Preferably, the coalescing agent is one of benzyl alcohol, alcohol ester 12；The defoaming agent is tricresyl phosphate fourth
One of ester, dimethicone；The thickener is methylcellulose, carboxymethyl cellulose, one in hydroxyethyl cellulose
Kind；The dispersing agent is one of sodium polyphosphate, calgon, sodium pyrophosphate, lauryl sodium sulfate.
Preferably, the present invention provides the preparation method of the phase-change heat-insulating coating based on phase-transition heat-storage, including following step
It is rapid:
(1) under the revolving speed of 400-500rpm, by 40-60g deionized water, the defoaming agent of 0.5-1.5g dispersing agent and 0.2-0.5g
After dispersion cup is added, mixed solution 1 is obtained after dispersing 1-3min；
(2) 45-65g titanium dioxide, 60-80g talcum powder are added into mixed solution 1, and disperses 15- at 800-1000rpm
20min；
(3) under the revolving speed of 1500-2500rpm, disperse and grind, obtain slurry；
(4) 20-40g paraffin/porous activated carbon described in claim 1-micro- glue of Lauxite phase transformation is dispersed in 120-200g
In deionized water, phase-change microcapsule slurry is obtained；
(5) slurry in step (3), the phase-change microcapsule slurry in step (4), 100-150g lotion, 0.3-0.7g are defoamed
Agent mixing, dispersion 20-30min is uniform to mixing liquid, obtains mixed solution 2；
(6) 1-3g coalescing agent, 1-2g thickener are added into mixed solution 2, disperses 10- under 350-550rpm revolving speed
20min obtains the phase-change heat-insulating coating based on phase-transition heat-storage.
Preferably, the milling time 40-60min in the step (2), 50 μm of fineness < after grinding.
Preferably, the dispersion revolving speed in the step (5) is 600-800rpm.
Compared with prior art, the present invention have it is following the utility model has the advantages that
Thermal insulation coatings of the invention, as functional stuffing, have phase using paraffin/porous activated carbon-Lauxite phase-change microcapsule
Becoming the advantages that latent heat is big, energy storage is high, temperature adjustment ability is strong, it can be ensured that phase-change heat-insulating coating has preferable heat accumulation, thermal insulation property,
Meanwhile paraffin being adsorbed in the hole of active carbon by using cellular porous active carbon, and overlay on urea in the surface of active carbon
The cladding of urea formaldehyde, to reach the problem of preventing phase-change material paraffin from revealing, also, the hole in porous activated carbon is mutually to interconnect
Logical, when such phase-change material paraffin is solid-liquid conversion, it can be flowed and be solidified in the hole of active carbon, reduce it to packet
The impact of film Lauxite；
In addition, the coated fertilizer Lauxite that the present invention uses has heating conduction, it can be by heat in extraneous and phase-change material stone
It is effectively transmitted between wax, ensure that phase-change material paraffin absorbs and releases the timeliness and validity of heat, meanwhile, it uses
Coated fertilizer Lauxite and coating system in each component have preferable compatibility, can be dispersed in coating, thus
It ensure that accumulation of heat, the thermal insulation property of phase-change heat-insulating coating.
Specific embodiment
Form by the following examples is described in further detail above content of the invention again, but should not be by this
The range for being interpreted as the above-mentioned theme of the present invention is only limitted to following embodiment, all technologies based on realization belonging to above content of the present invention
It all belongs to the scope of the present invention.
Embodiment 1
Paraffin/porous activated carbon-Lauxite phase-change microcapsule preparation method of the present embodiment, comprising the following steps:
(1) 15g porous activated carbon is placed in 20ml acetone soln, after being cleaned by ultrasonic 5min, with deionized water diafiltration, vacuum is dry
It is spare after dry；
(2) weigh 6g paraffin and 20g deionized water be mixed and heated, after paraffin melts completely be added 0.6g Tween-80 and
0.2g neopelex, and emulsified paraffin solution with high-speed emulsifying machine, it is subsequently placed in three-necked flask and carries out
Heating water bath, and 10min is kept the temperature at a temperature of 70 DEG C, obtain paraffin wax emulsions；
(3) urea liquid and 30ml deionized water for taking 10g melamine powder and 15ml mass fraction 35% are to tri- mouthfuls of 100mL
In flask, and triethanolamine is added dropwise, system pH is adjusted to 8, system temperature is increased to 70 DEG C while stirring, and in 70 DEG C
Lower heat preservation 5min, obtains urea resin prepolymer；
(4) paraffin wax emulsions made from step (2) are added drop-wise in the porous activated carbon in step (1), are stirred when being added dropwise, mistake
Filter, it is dry, obtain the porous activated carbon that load has paraffin；
(5) there is the porous activated carbon of paraffin to put into urea resin prepolymer the load in step (4), while stirring plus
Heat, and 1h is kept the temperature at 60 DEG C, it discharges, filters, wash, it is dry, obtain paraffin/porous activated carbon-micro- glue of Lauxite phase transformation
Capsule.
The preparation method of the phase-change heat-insulating coating based on phase-transition heat-storage of the present embodiment, comprising the following steps:
(1) under the revolving speed of 400rpm, after dispersion cup is added in the defoaming agent of 40g deionized water, 0.5g dispersing agent and 0.2g,
Mixed solution 1 is obtained after dispersion 1min；
(2) 45g titanium dioxide, 60g talcum powder are added into mixed solution 1, and disperses 15min at 800 rpm；
(3) under the revolving speed of 1500rpm, disperse and grind, obtain slurry；
(4) 20g paraffin/porous activated carbon-micro- glue of Lauxite phase transformation is dispersed in 120g deionized water, obtains the micro- glue of phase transformation
Capsule slurry；
(5) slurry in step (3), the phase-change microcapsule slurry in step (4), 100g lotion, 0.3g defoaming agent are mixed, point
It is uniform to mixing liquid to dissipate 20min, obtains mixed solution 2；
(6) 1g coalescing agent, 1g thickener are added into mixed solution 2, disperses 10min under 350rpm revolving speed, is based on
The phase-change heat-insulating coating of phase-transition heat-storage.
Embodiment 2
Paraffin/porous activated carbon-Lauxite phase-change microcapsule preparation method of the present embodiment, comprising the following steps:
(1) 25g porous activated carbon is placed in 30ml acetone soln, after being cleaned by ultrasonic 5min, with deionized water diafiltration, vacuum is dry
It is spare after dry；
(2) weigh 10g paraffin and 20g deionized water be mixed and heated, after paraffin melts completely be added 0.6g Tween-80 and
0.2g neopelex, and emulsified paraffin solution with high-speed emulsifying machine, it is subsequently placed in three-necked flask and carries out
Heating water bath, and 10min is kept the temperature at a temperature of 70 DEG C, obtain paraffin wax emulsions；
(3) urea liquid and 30ml deionized water for taking 15g melamine powder and 15ml mass fraction 35% are to tri- mouthfuls of 100mL
In flask, and triethanolamine is added dropwise, system pH is adjusted to 9, system temperature is increased to 70 DEG C while stirring, and in 70 DEG C
Lower heat preservation 5min, obtains urea resin prepolymer；
(4) paraffin wax emulsions made from step (2) are added drop-wise in the porous activated carbon in step (1), are stirred when being added dropwise, mistake
Filter, it is dry, obtain the porous activated carbon that load has paraffin；
(5) there is the porous activated carbon of paraffin to put into urea resin prepolymer the load in step (4), while stirring plus
Heat, and 1h is kept the temperature at 60 DEG C, it discharges, filters, wash, it is dry, obtain paraffin/porous activated carbon-micro- glue of Lauxite phase transformation
Capsule.
The preparation method of the phase-change heat-insulating coating based on phase-transition heat-storage of the present embodiment, comprising the following steps:
(1) under the revolving speed of 500rpm, after dispersion cup is added in the defoaming agent of 60g deionized water, 1.5g dispersing agent and 0.5g,
Mixed solution 1 is obtained after dispersion 3min；
(2) 65g titanium dioxide, 80g talcum powder are added into mixed solution 1, and disperses 20min at 1000rpm；
(3) under the revolving speed of 2500rpm, disperse and grind, obtain slurry；
(4) 40g paraffin/porous activated carbon-micro- glue of Lauxite phase transformation is dispersed in 200g deionized water, obtains the micro- glue of phase transformation
Capsule slurry；
(5) slurry in step (3), the phase-change microcapsule slurry in step (4), 150g lotion, 0.7g defoaming agent are mixed, point
It is uniform to mixing liquid to dissipate 30min, obtains mixed solution 2；
(6) 3g coalescing agent, 2g thickener are added into mixed solution 2, disperses 20min under 550rpm revolving speed, is based on
The phase-change heat-insulating coating of phase-transition heat-storage.
Embodiment 3
Paraffin/porous activated carbon-Lauxite phase-change microcapsule preparation method of the present embodiment, comprising the following steps:
(1) 20g porous activated carbon is placed in 25ml acetone soln, after being cleaned by ultrasonic 5min, with deionized water diafiltration, vacuum is dry
It is spare after dry；
(2) weigh 8g paraffin and 20g deionized water be mixed and heated, after paraffin melts completely be added 0.6g Tween-80 and
0.2g neopelex, and emulsified paraffin solution with high-speed emulsifying machine, it is subsequently placed in three-necked flask and carries out
Heating water bath, and 10min is kept the temperature at a temperature of 70 DEG C, obtain paraffin wax emulsions；
(3) urea liquid and 30ml deionized water for taking 13g melamine powder and 15ml mass fraction 35% are to tri- mouthfuls of 100mL
In flask, and triethanolamine is added dropwise, system pH is adjusted to 8.5, system temperature is increased to 70 DEG C while stirring, and in 70
5min is kept the temperature at DEG C, obtains urea resin prepolymer；
(4) paraffin wax emulsions made from step (2) are added drop-wise in the porous activated carbon in step (1), are stirred when being added dropwise, mistake
Filter, it is dry, obtain the porous activated carbon that load has paraffin；
(5) there is the porous activated carbon of paraffin to put into urea resin prepolymer the load in step (4), while stirring plus
Heat, and 1h is kept the temperature at 60 DEG C, it discharges, filters, wash, it is dry, obtain paraffin/porous activated carbon-micro- glue of Lauxite phase transformation
Capsule.
The preparation method of the phase-change heat-insulating coating based on phase-transition heat-storage of the present embodiment, comprising the following steps:
(1) under the revolving speed of 450rpm, after dispersion cup is added in the defoaming agent of 50g deionized water, 1g dispersing agent and 0.4g, point
Mixed solution 1 is obtained after dissipating 2min；
(2) 55g titanium dioxide, 70g talcum powder are added into mixed solution 1, and disperses 18min at 900rpm；
(3) under the revolving speed of 2000rpm, disperse and grind, obtain slurry；
(4) 30g paraffin/porous activated carbon-micro- glue of Lauxite phase transformation is dispersed in 160g deionized water, obtains the micro- glue of phase transformation
Capsule slurry；
(5) slurry in step (3), the phase-change microcapsule slurry in step (4), 1250g lotion, 0.5g defoaming agent are mixed,
It is uniform to mixing liquid to disperse 25min, obtains mixed solution 2；
(6) 2g coalescing agent, 1.5g thickener are added into mixed solution 2, disperses 15min under 450rpm revolving speed, obtains base
In the phase-change heat-insulating coating of phase-transition heat-storage.
Embodiment 4
Paraffin/porous activated carbon-Lauxite phase-change microcapsule preparation method of the present embodiment, comprising the following steps:
(1) 18g porous activated carbon is placed in 23ml acetone soln, after being cleaned by ultrasonic 5min, with deionized water diafiltration, vacuum is dry
It is spare after dry；
(2) weigh 7g paraffin and 20g deionized water be mixed and heated, after paraffin melts completely be added 0.6g Tween-80 and
0.2g neopelex, and emulsified paraffin solution with high-speed emulsifying machine, it is subsequently placed in three-necked flask and carries out
Heating water bath, and 10min is kept the temperature at a temperature of 70 DEG C, obtain paraffin wax emulsions；
(3) urea liquid and 30ml deionized water for taking 12g melamine powder and 15ml mass fraction 35% are to tri- mouthfuls of 100mL
In flask, and triethanolamine is added dropwise, system pH is adjusted to 8-9, system temperature is increased to 70 DEG C while stirring, and in 70
5min is kept the temperature at DEG C, obtains urea resin prepolymer；
(4) paraffin wax emulsions made from step (2) are added drop-wise in the porous activated carbon in step (1), are stirred when being added dropwise, mistake
Filter, it is dry, obtain the porous activated carbon that load has paraffin；
(5) there is the porous activated carbon of paraffin to put into urea resin prepolymer the load in step (4), while stirring plus
Heat, and 1h is kept the temperature at 60 DEG C, it discharges, filters, wash, it is dry, obtain paraffin/porous activated carbon-micro- glue of Lauxite phase transformation
Capsule.
The preparation method of the phase-change heat-insulating coating based on phase-transition heat-storage of the present embodiment, comprising the following steps:
(1) under the revolving speed of 400-500rpm, dispersion is added in the defoaming agent of 45g deionized water, 0.8g dispersing agent and 0.3g and is held
After device, mixed solution 1 is obtained after dispersing 1.5min；
(2) 50g titanium dioxide, 65g talcum powder are added into mixed solution 1, and disperses 16min at 850rpm；
(3) under the revolving speed of 1800rpm, disperse and grind, obtain slurry；
(4) by 25g paraffin/porous activated carbon described in claim 1-micro- glue of Lauxite phase transformation be dispersed in 120-200g go from
In sub- water, phase-change microcapsule slurry is obtained；
(5) slurry in step (3), the phase-change microcapsule slurry in step (4), 110g lotion, 0.4g defoaming agent are mixed, point
It is uniform to mixing liquid to dissipate 23min, obtains mixed solution 2；
(6) 1.5g coalescing agent, 1.3g thickener are added into mixed solution 2, disperses 13min under 400rpm revolving speed, obtains
Phase-change heat-insulating coating based on phase-transition heat-storage.
Embodiment 5
Paraffin/porous activated carbon-Lauxite phase-change microcapsule preparation method of the present embodiment, comprising the following steps:
(1) 22g porous activated carbon is placed in 28ml acetone soln, after being cleaned by ultrasonic 5min, with deionized water diafiltration, vacuum is dry
It is spare after dry；
(2) weigh 9g paraffin and 20g deionized water be mixed and heated, after paraffin melts completely be added 0.6g Tween-80 and
0.2g neopelex, and emulsified paraffin solution with high-speed emulsifying machine, it is subsequently placed in three-necked flask and carries out
Heating water bath, and 10min is kept the temperature at a temperature of 70 DEG C, obtain paraffin wax emulsions；
(3) urea liquid and 30ml deionized water for taking 14g melamine powder and 15ml mass fraction 35% are to tri- mouthfuls of 100mL
In flask, and triethanolamine is added dropwise, system pH is adjusted to 9, system temperature is increased to 70 DEG C while stirring, and in 70 DEG C
Lower heat preservation 5min, obtains urea resin prepolymer；
(4) paraffin wax emulsions made from step (2) are added drop-wise in the porous activated carbon in step (1), are stirred when being added dropwise, mistake
Filter, it is dry, obtain the porous activated carbon that load has paraffin；
(5) there is the porous activated carbon of paraffin to put into urea resin prepolymer the load in step (4), while stirring plus
Heat, and 1h is kept the temperature at 60 DEG C, it discharges, filters, wash, it is dry, obtain paraffin/porous activated carbon-micro- glue of Lauxite phase transformation
Capsule.
The preparation method of the phase-change heat-insulating coating based on phase-transition heat-storage of the present embodiment, comprising the following steps:
(1) under the revolving speed of 480rpm, after dispersion cup is added in the defoaming agent of 55g deionized water, 1.3g dispersing agent and 0.4g,
Mixed solution 1 is obtained after dispersion 2.5min；
(2) 60g titanium dioxide, 75g talcum powder are added into mixed solution 1, and disperses 18min at 950rpm；
(3) under the revolving speed of 2200rpm, disperse and grind, obtain slurry；
(4) 35g paraffin/porous activated carbon-micro- glue of Lauxite phase transformation is dispersed in 180g deionized water, obtains the micro- glue of phase transformation
Capsule slurry；
(5) slurry in step (3), the phase-change microcapsule slurry in step (4), 140g lotion, 0.6g defoaming agent are mixed, point
It is uniform to mixing liquid to dissipate 28min, obtains mixed solution 2；
(6) 2.5g coalescing agent, 1.8g thickener are added into mixed solution 2, disperses 18min under 500rpm revolving speed, obtains
Phase-change heat-insulating coating based on phase-transition heat-storage.
Test example 1
By prepared by 1-5 of the embodiment of the present invention based on the phase-change heat-insulating coating of phase-transition heat-storage according to GBT/T 9756-2009 state
Family's standard is measured coating, and specific experiment data are shown in Table 1
| Project | Unit | Index | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 |
| State in a reservoir | / | It is in uniform state after stirring without lump | It meets the requirements | It meets the requirements | It meets the requirements | It meets the requirements | It meets the requirements |
| Application property | / | It is accessible to brush two | It meets the requirements | It meets the requirements | It meets the requirements | It meets the requirements | It meets the requirements |
| Drying time (surface drying) | H | ≤2 | 1.8 | 1.7 | 1.6 | 1.7 | 1.9 |
| Appearance of film | / | Normally | Normally | Normally | Normally | Normally | Normally |
| Alkali resistance (25h) | / | It is without exception | It is without exception | It is without exception | It is without exception | It is without exception | It is without exception |
| Brushing resistance | It is secondary | ≥300 | 2100 | 2200 | 2250 | 2150 | 2000 |
| Low-temperature stability | / | It never degenerates | It never degenerates | It never degenerates | It never degenerates | It never degenerates | It never degenerates |
As shown in Table 1, the phase-change heat-insulating coating drying time prepared by various embodiments of the present invention based on phase-transition heat-storage is short, and
With good alkali resistance, abrasion resistance and low-temperature storage stability.
Test example 2
By paraffin/porous activated carbon-Lauxite phase-change microcapsule clad ratio and phase transformation prepared by 1-5 of the embodiment of the present invention
Enthalpy, and the heat preservation and insulation of the phase-change heat-insulating coating based on phase-transition heat-storage are tested, wherein
Enthalpy of phase change measurement: the enthalpy of phase change of differential scanning calorimeter (DSC) test sample, test condition are as follows: accurately weigh are used
The sample of 10mg or so, in N2Under atmosphere, 10K/min temperature rate is selected, test temperature selects -20 DEG C -100 DEG C of survey
Measure range.
Heat preservation and insulation test: 1, sample paint blade coating on tinplate 50 DEG C baking ovens dry after, is made into its recovery
To room temperature, contact type thermometric indicator is pasted on sample film；2, the thin aluminum sheet of excellent thermal conductivity is placed on to 65 DEG C of stable heat
Above source；3, after thin aluminum sheet temperature is stablized, the sample panel of test is placed on thin aluminum sheet center, while pressing stopwatch record
Heating rate.Compared with original formulation (being free of phase-change microcapsule), heat-insulation and heat-preservation is indicated with the maximum temperature difference value of same time
Energy.
Specific experimental data is shown in Table 2
| Project | Unit | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 |
| Clad ratio | % | 91.16 | 92.00 | 94.34 | 93.34 | 90.46 |
| Enthalpy of phase change | J/g | 163.8 | 165.5 | 166.8 | 167.2 | 168.3 |
| Heat preservation and insulation | ℃ | 11 | 13 | 15 | 14 | 12 |
As shown in Table 2, paraffin/porous activated carbon-Lauxite phase-change microcapsule clad ratio of the invention is higher, has preferable
Impermeable effect, and enthalpy of phase change is larger, has preferable temperature adjustment ability, and the phase-transition heat-preserving of the invention based on phase-transition heat-storage applies
Material has excellent heat preservation and insulation.
To sum up, thermal insulation coatings of the invention are filled out using paraffin/porous activated carbon-micro- glue of Lauxite phase transformation as function
Material, have many advantages, such as that latent heat of phase change is big, energy storage is high, temperature adjustment ability is strong, it can be ensured that phase-change heat-insulating coating with preferable heat accumulation,
Thermal insulation property, meanwhile, paraffin is adsorbed in the hole of active carbon by using cellular porous active carbon, and in the table of active carbon
Face overlays on the cladding of Lauxite, to reach the problem of preventing phase-change material paraffin from revealing, also, the hole in porous activated carbon
Be it is interconnected, such phase-change material paraffin be solid-liquid conversion when, can be flowed and be solidified in the hole of active carbon, reduce
Its impact to coating Lauxite；
In addition, the coated fertilizer Lauxite that the present invention uses has heating conduction, it can be by heat in extraneous and phase-change material stone
It is effectively transmitted between wax, ensure that phase-change material paraffin absorbs and releases the timeliness and validity of heat, meanwhile, it uses
Coated fertilizer Lauxite and coating system in each component have preferable compatibility, can be dispersed in coating, thus
It ensure that accumulation of heat, the thermal insulation property of phase-change heat-insulating coating.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, although referring to aforementioned reality
Applying example, invention is explained in detail, for those skilled in the art, still can be to aforementioned each implementation
Technical solution documented by example is modified or equivalent replacement of some of the technical features.It is all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of paraffin/porous activated carbon-Lauxite phase-change microcapsule, which is characterized in that phase-change material in the microcapsules
For paraffin, carrier of the porous activated carbon as phase-change material, capsule skin of the Lauxite as phase-change microcapsule, the microcapsules
Enthalpy of phase change 162.7J/g, phase transition temperature are 30.8 DEG C, and average grain diameter is 18.46 μm, and thermal coefficient is 0.235W/ (mK).
2. the preparation method of paraffin/porous activated carbon-Lauxite phase-change microcapsule according to claim 1, feature
It is, comprising the following steps:
(1) porous activated carbon is placed in acetone soln, after being cleaned by ultrasonic 5min, with deionized water diafiltration, is dried in vacuo standby
With；
(2) it weighs a certain amount of paraffin and deionized water is mixed and heated, be added emulsifier after paraffin melts completely, and with height
Fast mulser emulsifies paraffin solution, is subsequently placed in three-necked flask and carries out heating water bath, and keeps the temperature at a temperature of 70 DEG C
10min obtains paraffin wax emulsions；
(3) urea liquid for taking melamine powder and mass fraction 35% and a certain amount of deionized water are to 100mL three-necked flask
In, and triethanolamine is added dropwise, system pH is adjusted to 8-9, system temperature is increased to 70 DEG C while stirring, and at 70 DEG C
5min is kept the temperature, urea resin prepolymer is obtained；
(4) paraffin wax emulsions made from step (2) are added drop-wise in the porous activated carbon in step (1), are stirred when being added dropwise, mistake
Filter, it is dry, obtain the porous activated carbon that load has paraffin；
(5) there is the porous activated carbon of paraffin to put into urea resin prepolymer the load in step (4), while stirring plus
Heat, and 1h is kept the temperature at 60 DEG C, it discharges, filters, wash, it is dry, obtain paraffin/porous activated carbon-micro- glue of Lauxite phase transformation
Capsule.
3. the preparation method of paraffin/porous activated carbon-Lauxite phase-change microcapsule according to claim 2, feature
It is, the emulsifier is Tween-80 and neopelex is the compound of 3:1 in mass ratio.
4. a kind of phase-change heat-insulating coating based on phase-transition heat-storage, which is characterized in that the phase-change heat-insulating coating is by claim 1
Paraffin/porous activated carbon-Lauxite the phase-change microcapsule is functional stuffing, talcum powder, titanium dioxide, lotion, film forming help
Agent, defoaming agent, thickener, dispersing agent and deionized water are prepared as a raw material.
5. the phase-change heat-insulating coating according to claim 4 based on phase-transition heat-storage, which is characterized in that the phase-transition heat-preserving applies
Material is made of raw material from the following weight: paraffin/porous activated carbon -20-40 parts of Lauxite phase-change microcapsule, talcum powder 60-
80 parts, 45-65 parts of titanium dioxide, 100-150 parts of lotion, 1-3 parts of coalescing agent, 0.5-1 parts of defoaming agent, 1-2 parts of thickener, dispersion
0.5-1.5 parts of agent, 180-240 parts of deionized water.
6. the phase-change heat-insulating coating according to claim 4 based on phase-transition heat-storage, which is characterized in that the lotion is phenylpropyl alcohol
One of lotion, tertiary vinegar milk liquid, ethyl vinyl acetate lotion.
7. the phase-change heat-insulating coating according to claim 4 based on phase-transition heat-storage, which is characterized in that the coalescing agent is
One of benzyl alcohol, alcohol ester 12；The defoaming agent is one of tributyl phosphate, dimethicone；The thickener
For one of methylcellulose, carboxymethyl cellulose, hydroxyethyl cellulose；The dispersing agent is sodium polyphosphate, six inclined phosphorus
One of sour sodium, sodium pyrophosphate, lauryl sodium sulfate.
8. the preparation method of the phase-change heat-insulating coating according to claim 4 based on phase-transition heat-storage, which is characterized in that including
Following steps:
(1) under the revolving speed of 400-500rpm, by 40-60g deionized water, the defoaming agent of 0.5-1.5g dispersing agent and 0.2-0.5g
After dispersion cup is added, mixed solution 1 is obtained after dispersing 1-3min；
(2) 45-65g titanium dioxide, 60-80g talcum powder are added into mixed solution 1, and disperses 15- at 800-1000rpm
20min；
(3) under the revolving speed of 1500-2500rpm, disperse and grind, obtain slurry；
(4) 20-40g paraffin/porous activated carbon described in claim 1-micro- glue of Lauxite phase transformation is dispersed in 120-200g
In deionized water, phase-change microcapsule slurry is obtained；
(5) slurry in step (3), the phase-change microcapsule slurry in step (4), 100-150g lotion, 0.3-0.7g are defoamed
Agent mixing, dispersion 20-30min is uniform to mixing liquid, obtains mixed solution 2；
(6) 1-3g coalescing agent, 1-2g thickener are added into mixed solution 2, disperses 10- under 350-550rpm revolving speed
20min obtains the phase-change heat-insulating coating based on phase-transition heat-storage.
9. the preparation method of the phase-change heat-insulating coating according to claim 8 based on phase-transition heat-storage, which is characterized in that described
Milling time 40-60min in step (2), 50 μm of fineness < after grinding.
10. the preparation method of the phase-change heat-insulating coating according to claim 8 based on phase-transition heat-storage, which is characterized in that institute
Stating the dispersion revolving speed in step (5) is 600-800rpm.
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