CN104312305A - Phase transition thermal storage microcapsule paint containing tetradecyl alcohol and micron order metal powder - Google Patents

Phase transition thermal storage microcapsule paint containing tetradecyl alcohol and micron order metal powder Download PDF

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Publication number
CN104312305A
CN104312305A CN201410481853.1A CN201410481853A CN104312305A CN 104312305 A CN104312305 A CN 104312305A CN 201410481853 A CN201410481853 A CN 201410481853A CN 104312305 A CN104312305 A CN 104312305A
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microcapsule
phase
water
tetradecyl alcohol
emulsion
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李清璠
洪卫
潘圣阳
王梁元
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J13/00Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
    • B01J13/02Making microcapsules or microballoons
    • B01J13/06Making microcapsules or microballoons by phase separation
    • B01J13/14Polymerisation; cross-linking
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K13/00Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
    • C08K13/06Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/02Elements
    • C08K3/08Metals
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/34Silicon-containing compounds
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/34Silicon-containing compounds
    • C08K3/346Clay
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
    • C08K5/04Oxygen-containing compounds
    • C08K5/05Alcohols; Metal alcoholates
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
    • C08K5/04Oxygen-containing compounds
    • C08K5/05Alcohols; Metal alcoholates
    • C08K5/053Polyhydroxylic alcohols
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00Use of pretreated ingredients
    • C08K9/10Encapsulated ingredients
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D125/00Coating 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
    • C09D125/02Homopolymers or copolymers of hydrocarbons
    • C09D125/04Homopolymers or copolymers of styrene
    • C09D125/08Copolymers of styrene
    • C09D125/14Copolymers of styrene with unsaturated esters
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D5/00Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/16Antifouling paints; Underwater paints
    • C09D5/1606Antifouling paints; Underwater paints characterised by the anti-fouling agent
    • C09D5/1612Non-macromolecular compounds
    • C09D5/1625Non-macromolecular compounds organic
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/60Additives non-macromolecular
    • C09D7/61Additives non-macromolecular inorganic
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/60Additives non-macromolecular
    • C09D7/63Additives non-macromolecular organic
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/65Additives macromolecular
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/02Elements
    • C08K3/08Metals
    • C08K2003/085Copper
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2237Oxides; Hydroxides of metals of titanium
    • C08K2003/2241Titanium dioxide

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacturing Of Micro-Capsules (AREA)

Abstract

The invention belongs to the field of building paint and discloses a phase transition thermal storage microcapsule paint mixed with micron order copper powder in order to improve the thermal properties of phase change thermal storage microcapsule paint, and with self-cleaning, heat preservation and temperature control effects. The microcapsule uses tetradecyl alcohol as a capsule core, and melamine and formaldehyde as a capsule wall. During the package of the microcapsule core by the capsule wall, an appropriate amount of the micron order copper powder is added at an appropriate rate, so that the copper powder is attached to or embedded in the microcapsules to increase enthalpy of phase change by 50J / g. The employed paint is not intermiscible with the microcapsule wall and has self-cleaning efficacy.

Description

Coating containing tetradecyl alcohol and micro-sized metal powder phase-change thermal storage microcapsule
Technical field:
The present invention relates to a kind of building coating field, be that a kind of mixing adds Micron-Sized Copper Powders Coated to improve the phase-change thermal storage enteric coating of heat conductivility, there is effect of self-cleaning insulation temperature control.
Background technology:
At present there is microcapsulary, but fail good to be applied to indoor paint field, because microcapsulary immature and need to overcome the impact of coating on properties of microcapsules.Current water-borne coatings makes good, especially the building coating based on water-borne coatings accounts for about 38% in China's coating total amount, and the cyst wall of described formulation for coating material and microcapsule does not dissolve each other, effect that microcapsule have storage and discharge latent heat of phase change can be fully played, therefore fully microcapsule can be applied to water-borne coatings field ripe already.
The deficiency of the research field of current microcapsule is latent heats of phase change of raising microcapsule that cannot be good, because the hybridization of cyst wall and capsule-core, and the obstruction that cyst wall passes to capsule-core latent heat, actual transformation latent heat generally reduces 20-50J/g than calculated value, microcapsulary that the present invention adopts encapsulating phase change material tetradecyl alcohol stores and release latent heat of phase change, simultaneously by adding heat conduction effect that appropriate Micron-Sized Copper Powders Coated substantially increases microcapsule under certain rotating speed.The actual transformation latent heat of microcapsule is made to improve about 50J/g.
Summary of the invention:
The invention provides the mixture of a kind of coating and microcapsule, described coating can well and the latent heat of phase change of effective release microcapsule.Object is to solve the bottleneck that current phase-change thermal storage microcapsule institute runs into, namely latent heat of phase change is little and be difficult to be improved by the control of rotating speed and drop rate, and reason is that microcapsule organism cyst wall pair wraps up with the capsule-core as phase change material makes it be difficult to carry out good heat conduction.
The present invention adds Micron-Sized Copper Powders Coated when effect microcapsule wall parcel capsule-core with suitable speed and consumption, makes copper powder adhere to or be partially submerged into microcapsule, improves the heat conductivility of microcapsule.Through the good heat conductive of copper powder, detect through DSC, the enthalpy of phase change recorded improves 50J/g.And the form of microcapsule and encapsulation rate can not be affected.
Formulation for coating material of the present invention, can overcome microcapsule and water-borne coatings and to mix this problem, the organic components such as various auxiliary agent of coating itself may carry out dissolving each other with the composition of microcapsule thus affect the encapsulating performance of microcapsule outer wall.Formulation for coating material of the present invention does not have mutual solubility with the composition of microcapsule, and microcapsule are scattered in coating, still can play good heat conduction heat accumulation heat release effect.
The present invention is used for interior wall and has good indoor temperature control effect, in certain temperature range, (20-25 DEG C) carries out phase transformation, and the phase change material of microcapsule inside when low temperature heats up can liquefy thus heat release, otherwise, when lowering the temperature from high temperature, can solidify in this temperature field thus absorb heat.Thus reduce the vibration frequency of room temp, be close with the body sense comfort level of human body, also play effect that household is energy-conservation.
What the microcapsule in the present invention adopted is situ aggregation method, monomer in situ aggregation method and catalyzer are all positioned at the outside or inside of capsule-core, and require monomer-soluble, generation polymkeric substance soluble, polymer deposition capsule-core surface and coated formation microcapsule.Before polymerization reaction take place, capsule-core must be dispersed into particulate.Become shell material can be water-soluble or oil-soluble monomer, can be the mixture of several monomer, also can be water-soluble low molecular weight polymkeric substance or prepolymer.
The present invention is achieved through the following technical solutions:
Contain a preparation method for the phase-change microcapsule of tetradecyl alcohol and micro-sized metal powder, comprise the steps:
(1) preparation of carbamide performed polymer:
Among the round-bottomed flask trimeric cyanamide of 3-5g being poured into 250ml, the formaldehyde solution of 37% of 5-8 is mixed with the distilled water of 40-50ml and adds, by trolamine adjust ph at about 8-9, magnetic stirring apparatus keeps 100-200r/min, at 70 DEG C, heated and stirred is about 10min, carbamide performed polymer.
(2) preparation of inner phase transformation core:
The SMA (Zelan 338) of 2-3g is poured in 250ml flask, adds 0.3-0.5gNaOH, then add 50ml distilled water, mix.At 50 DEG C, under 1200r/min condition, carry out emulsification 2h.Be about 4.5 with the lemon acid for adjusting pH of 10% afterwards.
The tetradecyl alcohol of the OP-10 of 10% of 5-10g, 15-20g is poured in above mixing solutions, at the emulsified 15min of 2500r/min, obtain uniform emulsion.
(3) compound of cyst wall and capsule-core:
The emulsion that second step is worth is added question response in there-necked flask.
At water bath with thermostatic control 50 DEG C, the performed polymer the first step obtained is added drop-wise in the obtained emulsion of second step with the speed of 0.5ml/min slowly, ensure that rotating speed is 600-700r/min simultaneously, after question response carries out 1h, at another mouth of there-necked flask, add Micron-Sized Copper Powders Coated with the speed of 0.1-0.2g/min (0.15g is best), add 1h.Copper powder and performed polymer add complete after, dripping massfraction is the acetic acid of 10%, and speed is 0.4ml/min, stops when pH is 3-4.Within one minute afterwards, the speed of 1 DEG C is warmed up to 80 DEG C, and is incubated 2h.
After completion of the reaction with after petroleum ether 2-3 time, carry out suction filtration with Büchner funnel and filter flask, with clear water, 2 times are washed again to filter cake, carrying out suction filtration, naturally drying, obtaining novel microcapsules.
The described application of phase-change thermal storage microcapsule in interior wall coating, with the mass percent shared by raw material, described water paint for internal walls raw material is: emulsion 10-50%, phase-change thermal storage microcapsule 5-20%, titanium dioxide 5-20%, diatomite 3-20%, calcium carbonate 10-30%, kaolin 1-10%, film coalescence aid 1-5%, pH adjusting agent 1-5%, thickening material 0.1-1%, defoamer 0.1-1%, organosilicon moisture repellent 1-10% and water 10-40%.
Described emulsion to be volume solid content be 40% benzene emulsion.
Described titanium dioxide is rutile titanium dioxide.
Described defoamer is one or more in butanols, 1,2-PD, emulsification dimethyl silicone oil, emulsification polymethylphenyl siloxane fluid, polyoxyethylene polyoxypropylene tetramethylolmethane ether and octanol.
Described film coalescence aid is lauryl alcohol ester.
Described pH adjusting agent is AMP-95.
Described thickening material is RM-8W.
Described organosilicon moisture repellent Dow corning waterproofing agent of organosilicon.
Polish 2 hours under the condition of 3600r/min after emulsion, titanium dioxide, diatomite, calcium carbonate, kaolin, film coalescence aid, pH adjusting agent, thickening material, defoamer, organosilicon hydrophobic and water being added during preparation; Add phase-change thermal storage microcapsule, stir and can use.
Embodiment
Below in conjunction with embodiment, the present invention is further described, but the present invention is not limited to following examples.
Embodiment one
(1) among the round-bottomed flask trimeric cyanamide of 4g being poured into 250ml, the formaldehyde solution of 6.5 37% is mixed with the distilled water of 45ml and adds, be 8 by trolamine adjust ph, magnetic stirring apparatus keeps 100r/min, at 70 DEG C, heated and stirred is about 10min, carbamide performed polymer.
(2) SMA (Zelan 338) of 2.7g is poured in 250ml flask, add 0.4gNaOH, then add 50ml distilled water, mix.At 50 DEG C, under 1200r/min condition, carry out emulsification 2h.Be about 4.5 with the lemon acid for adjusting pH of 10% afterwards.The tetradecyl alcohol of the OP-10 of 10% of 8g, 16g is poured in above mixing solutions, at the emulsified 15min of 2500r/min, obtain uniform emulsion.
(3) emulsion that (2) are obtained is added question response in there-necked flask.
At water bath with thermostatic control 50 DEG C, performed polymer obtained to (1) is added drop-wise in the obtained emulsion of second step with the speed of 0.5ml/min slowly, ensure that rotating speed is 600r/min simultaneously, after question response carries out 1h, at another mouth of there-necked flask, add Micron-Sized Copper Powders Coated with the speed of 0.1g/min, add 1h.
Copper powder and performed polymer add complete after, dripping massfraction is the acetic acid of 10%, and speed is 0.4ml/min, stops when pH is 3.Within one minute afterwards, the speed of 1 DEG C is warmed up to 80 DEG C, and is incubated 2h.
After completion of the reaction with after petroleum ether 2-3 time, carry out suction filtration with Büchner funnel and filter flask, with clear water, 2 times are washed again to filter cake, carrying out suction filtration, naturally drying, obtaining novel microcapsules.
The preparation of interior wall anti-pollution coating
By percentage to the quality, emulsion 21%, titanium dioxide 5.8%, diatomite 5.8%, calcium carbonate 19.5%, kaolin 2%, film coalescence aid 1.2%, pH adjusting agent 1%, thickening material 0.5%, defoamer 1%, organosilicon moisture repellent 1.7% and water 23.8% is added heat accumulation microcapsule prepared by 16.7% the present embodiment, stir, namely obtain the coating of the phase-change microcapsule containing tetradecyl alcohol and micro-sized metal powder.
Emulsion is the benzene emulsion of volume solid content 40%, and titanium dioxide is rutile titanium dioxide, and defoamer is butanols, and film coalescence aid is lauryl alcohol ester, and pH adjusting agent is AMP-95, and thickening material is RM-8W, and organosilicon moisture repellent is Dow corning waterproofing agent of organosilicon.
Embodiment two
(1) among the round-bottomed flask trimeric cyanamide of 4.5g being poured into 250ml, the formaldehyde solution of 6.5 37% is mixed with the distilled water of 45ml and adds, by trolamine adjust ph 8.5, magnetic stirring apparatus keeps 150r/min, at 70 DEG C, Keep agitation is about 10min, obtains carbamide performed polymer.
The SMA (Zelan 338) of 3.0g is poured in 250ml flask, adds 0.45gNaOH, then add 50ml distilled water, mix.At 50 DEG C, under 1200r/min condition, carry out emulsification 2h.Be about 4.5 with the lemon acid for adjusting pH of 10% afterwards.The tetradecyl alcohol of the OP-10 of 10% of 8.5g, 16g is poured in above mixing solutions, at the emulsified 15min of 2500r/min, obtain uniform emulsion.
The emulsion that (2) are obtained adds question response in there-necked flask.
At water bath with thermostatic control 50 DEG C, performed polymer obtained to (1) is added drop-wise in the obtained emulsion of second step with the speed of 0.5ml/min slowly, rotating speed is 650r/min, after question response carries out 1h, at another mouth of there-necked flask, add Micron-Sized Copper Powders Coated with the speed of 0.15g/min, add 1h.
Copper powder and performed polymer add complete after, dripping massfraction is the acetic acid of 10%, and speed is 0.4ml/min, stops when pH is 4.Within one minute afterwards, the speed of 1 DEG C is warmed up to 80 DEG C, and is incubated 2h.
After completion of the reaction with after petroleum ether 2-3 time, carry out suction filtration with Büchner funnel and filter flask, with clear water, 2 times are washed again to filter cake, carrying out suction filtration, naturally drying, obtaining novel microcapsules.
The preparation of interior wall anti-pollution coating
By percentage to the quality, emulsion 24%, titanium dioxide 5.8%, diatomite 5.8%, calcium carbonate 19.5%, kaolin 2%, film coalescence aid 1.2%, pH adjusting agent 1%, thickening material 0.5%, defoamer 1%, organosilicon moisture repellent 2.4% and water 26.8% is added heat accumulation microcapsule prepared by 10% the present embodiment, stir, namely obtain the coating of the phase-change microcapsule containing tetradecyl alcohol and micro-sized metal powder.
Emulsion is the benzene emulsion of volume solid content 40%, and titanium dioxide is rutile titanium dioxide, and defoamer is emulsification titanium dioxide silicone oil, film coalescence aid is lauryl alcohol ester, pH adjusting agent is AMP-95, and thickening material is RM-8W, and organosilicon moisture repellent is Dow corning waterproofing agent of organosilicon.
Embodiment three
(1) among the round-bottomed flask trimeric cyanamide of 5g being poured into 250ml, be that the formaldehyde solution of 37% mixes with the distilled water of 45ml and adds by the massfraction of 7g, by trolamine adjust ph about 9, magnetic stirring apparatus keeps 200r/min, at 70 DEG C, heated and stirred is about 10min, carbamide performed polymer.
The SMA (Zelan 338) of 3.5g is poured in 250ml flask, adds 0.5gNaOH, then add 50ml distilled water, mix.At 50 DEG C, under 1200r/min condition, carry out emulsification 2h.Be about 4.5 with the lemon acid for adjusting pH of 10% afterwards.
The tetradecyl alcohol of the OP-10 of 10% of 9.0g, 16g is poured in above mixing solutions, at the emulsified 15min of 2500r/min, obtain uniform emulsion.
The emulsion that (2) are obtained adds question response in there-necked flask.
At water bath with thermostatic control 50 DEG C, performed polymer obtained to (1) is added drop-wise in the obtained emulsion of second step with the speed of 0.5ml/min slowly, ensure that rotating speed is 700r/min simultaneously, after question response carries out 1h, at another mouth of there-necked flask, add Micron-Sized Copper Powders Coated with the speed of 0.2g/min, add 1h.
Copper powder and performed polymer add complete after, dripping massfraction is the acetic acid of 10%, and speed is 0.4ml/min, stops when pH is 4.Within one minute afterwards, the speed of 1 DEG C is warmed up to 80 DEG C, and is incubated 2h.
After completion of the reaction with after petroleum ether 2-3 time, carry out suction filtration with Büchner funnel and filter flask, with clear water, 2 times are washed again to filter cake, carrying out suction filtration, naturally drying, obtaining novel microcapsules.
The preparation of interior wall anti-pollution coating
By percentage to the quality, emulsion 21%, titanium dioxide 4.8%, diatomite 5.8%, calcium carbonate 17.2%, kaolin 2%, film coalescence aid 1.2%, pH adjusting agent 1%, thickening material 0.5%, defoamer 1%, organosilicon moisture repellent 1.7% and water 23.8% is added heat accumulation microcapsule prepared by 20% the present embodiment, stir, namely obtain the coating of the phase-change microcapsule containing tetradecyl alcohol and micro-sized metal powder.
Emulsion is the benzene emulsion of volume solid content 40%, and titanium dioxide is rutile titanium dioxide, and defoamer is 1,2-propylene glycol, film coalescence aid is lauryl alcohol ester, and pH adjusting agent is AMP-95, thickening material is RM-8W, and organosilicon moisture repellent is Dow corning waterproofing agent of organosilicon.

Claims (5)

1. contain a coating for the phase-change microcapsule of tetradecyl alcohol and micro-sized metal powder, it is characterized in that, should be made up of following component and mass percentage containing tetradecyl alcohol phase-change microcapsule, its each constituent mass percentage composition sum is 100%.
Tetradecyl alcohol phase-change microcapsule: 1 ~ 50%;
Do not dissolve each other water-borne coatings composition: 1 ~ 50%;
Micro-sized metal copper powder: 1 ~ 5%.
2. by the phase-change microcapsule coating containing tetradecyl alcohol and micro-sized metal powder according to claim 1, it is characterized in that, described particle diameter is the microcapsule contained as tetradecyl alcohol phase change material of 1 ~ 4 μm.It is for containing trimeric cyanamide, formaldehyde, distilled water, trolamine, styrene-maleic anhydride copolymer, sodium hydroxide, citric acid, OP-10, tetradecyl alcohol, the prepared product in order and under certain content and under specified conditions of acetic acid.
3., by the phase-change microcapsule coating containing tetradecyl alcohol and micro-sized metal powder that right 1 requirement is described, it is characterized in that, the described water-borne coatings that do not dissolve each other is containing deionized water, titanium dioxide, diatomite, calcium carbonate, kaolin, benzene emulsion, ten diester alcohol, PH conditioning agent (AMP95), thickening material (RM-8W), defoamer, the water-borne coatings mixture of organosilicon moisture repellent.It has the water-fast performance of anti-soil, can mix with microcapsule and not dissolve each other.
4., by the phase-change microcapsule coating containing tetradecyl alcohol and micro-sized metal powder of claim 1 requirement, it is characterized in that, the particle diameter of described micro-sized metal copper powder is at 1 ~ 10 μm, and the purity of its metallic copper powder reaches 99%.
5., by the phase-change microcapsule coating methods containing tetradecyl alcohol and micro-sized metal powder according to claim 1, it is characterized in that comprising following process:
(1) preparation of carbamide performed polymer:
Among the round-bottomed flask trimeric cyanamide of 3-5g being poured into 250ml, the formaldehyde solution of 37% of 5-8 is mixed with the distilled water of 40-50ml and adds, by trolamine adjust ph at about 8-9, magnetic stirring apparatus keeps 100-200r/min, at 70 DEG C, heated and stirred is about 10min, carbamide performed polymer.
(2) preparation of inner phase transformation core:
The SMA (Zelan 338) of 2-3g is poured in 250ml flask, adds 0.3-0.5gNaOH, then add 50ml distilled water, mix.At 50 DEG C, under 1200r/min condition, carry out emulsification 2h.Be about 4.5 with the lemon acid for adjusting pH of 10% afterwards.
The tetradecyl alcohol of the OP-10 of 10% of 5-10g, 15-20g is poured in above mixing solutions, at the emulsified 15min of 2500r/min, obtain uniform emulsion.
(3) compound of cyst wall and capsule-core:
The emulsion that second step is worth is added question response in there-necked flask.
At water bath with thermostatic control 50 DEG C, the performed polymer the first step obtained is added drop-wise in the obtained emulsion of second step with the speed of 0.5ml/min slowly, ensure that rotating speed is 600-700r/min simultaneously, after question response carries out 1h, at another mouth of there-necked flask, add Micron-Sized Copper Powders Coated with the speed of 0.1-0.2g/min (0.15g is best), add 1h.
Copper powder and performed polymer add complete after, dripping massfraction is the acetic acid of 10%, and speed is 0.4ml/min, stops when pH is 3-4.Within one minute afterwards, the speed of 1 DEG C is warmed up to 80 DEG C, and is incubated 2h.
After completion of the reaction with after petroleum ether 2-3 time, carry out suction filtration with Büchner funnel and filter flask, with clear water, 2 times are washed again to filter cake, carrying out suction filtration, naturally drying, obtaining novel microcapsules.
(4) not dissolve each other the preparation of water-borne coatings
With the mass percent shared by raw material, the water paint for internal walls raw material of monologue story-telling with gestures is: emulsion 10-50%, phase-change thermal storage microcapsule 5-20%, titanium dioxide 5-20%, diatomite 3-20%, calcium carbonate 10-30%, kaolin 1-10%, film coalescence aid 1-5%, pH adjusting agent 1-5%, thickening material 0.1-1%, defoamer 0.1-1%, organosilicon moisture repellent 1-10% and water 10-40%.
The described application of phase-change thermal storage microcapsule in interior wall coating, with the mass percent shared by raw material, the water paint for internal walls raw material of monologue story-telling with gestures is: emulsion 10-50%, phase-change thermal storage microcapsule 5-20%, titanium dioxide 5-20%, diatomite 3-20%, calcium carbonate 10-30%, kaolin 1-10%, film coalescence aid 1-5%, pH adjusting agent 1-5%, thickening material 0.1-1%, defoamer 0.1-1%, organosilicon moisture repellent 1-10% and water 10-40%.
Described emulsion to be volume solid content be 40% benzene emulsion.
Described titanium dioxide is rutile titanium dioxide.
Described defoamer is one or more in butanols, 1,2-PD, emulsification dimethyl silicone oil, emulsification polymethylphenyl siloxane fluid, polyoxyethylene polyoxypropylene tetramethylolmethane ether and octanol.
Described film coalescence aid is lauryl alcohol ester.
Described pH adjusting agent is AMP-95.
Described thickening material is RM-8W.
Described organosilicon moisture repellent Dow corning waterproofing agent of organosilicon.
(5) compound of microcapsule and coating
Be 5-20% by the adding rate of microcapsule in whole coating, stir, namely obtain the coating of this phase-change microcapsule containing tetradecyl alcohol and micro-sized metal powder.
CN201410481853.1A 2014-09-19 2014-09-19 Phase transition thermal storage microcapsule paint containing tetradecyl alcohol and micron order metal powder Pending CN104312305A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105368245A (en) * 2015-12-26 2016-03-02 孝感巨核新材料科技有限公司 Phase-change interior wall coating with energy storage and temperature adjustment functions and preparation method of coating
CN107986678A (en) * 2017-11-29 2018-05-04 广西瑞航工程咨询有限公司 A kind of construction material of new temperature controllable and preparation method thereof
CN108048039A (en) * 2017-12-26 2018-05-18 桂林电子科技大学 A kind of nano zinc oxide modified microcapsules composite phase-change material and preparation method thereof
CN108130047A (en) * 2017-12-12 2018-06-08 同济大学 The preparation method of pitch low temperature thermoregulation agent based on the tetradecane/tetradecyl alchohol/cyanurotriamide modified urea resin
CN108192467A (en) * 2018-01-02 2018-06-22 邹元月 A kind of phase-change thermal storage coating and preparation method and application

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105368245A (en) * 2015-12-26 2016-03-02 孝感巨核新材料科技有限公司 Phase-change interior wall coating with energy storage and temperature adjustment functions and preparation method of coating
CN107986678A (en) * 2017-11-29 2018-05-04 广西瑞航工程咨询有限公司 A kind of construction material of new temperature controllable and preparation method thereof
CN108130047A (en) * 2017-12-12 2018-06-08 同济大学 The preparation method of pitch low temperature thermoregulation agent based on the tetradecane/tetradecyl alchohol/cyanurotriamide modified urea resin
CN108048039A (en) * 2017-12-26 2018-05-18 桂林电子科技大学 A kind of nano zinc oxide modified microcapsules composite phase-change material and preparation method thereof
CN108192467A (en) * 2018-01-02 2018-06-22 邹元月 A kind of phase-change thermal storage coating and preparation method and application

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