CN103102552A - Phase-changed heat insulation polyolefin foam material and preparation method thereof - Google Patents
Phase-changed heat insulation polyolefin foam material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a phase-changed heat insulation polyolefin foam material and a preparation method thereof. The phase-changed heat insulation polyolefin foam material is prepared by carrying out the operations including mixing, melt extrusion, preheating and foaming on raw materials including phase-changed microcapsules, polyolefin resin, a foaming agent, a cross-linking agent, a blowing promoter, a color masterbatch, an antiager and a processing aid. When the temperature is reduced, the phase of the phase-changed material can be changed, heat is released, and thus, the environment temperature is regulated. Meanwhile, a microcapsule technology is adopted, the phase-changed material is used as a capsule core material to be wrapped inside a capsule wall, and thus, the loss of the phase-changed capsule core material from a porous foam material is reduced, and the continuity of a heat insulation effect is improved.
Description
Technical field
The present invention relates to a kind of lagging material and preparation method thereof, refer in particular to a kind of phase-transition heat-preserving polyolefin foam and preparation method thereof.
Background technology
The polyolefins plastic applications is in extensive range, has good physics, chemistry and mechanical property, and its toughness, flexibility and shock-absorbing capacity are good, and has electrical isolation, the character such as heat insulation, is widely used in the fields such as packing, chemical industry, building.The polyolefins porous plastics is widely used, and is also one of porous plastics that successfully makes the earliest.As far back as nineteen forty-one, du pont company just utilizes the nitrogen method successfully to prepare the LDPE porous plastics.Through the development of decades, foamed polyolefine plastic is full-fledged, has realized variation in kind and application facet.Along with deepening continuously and the progress of foaming technique of theoretical investigation, porous plastics is having significant progress aspect output and quality.The characteristic low due to its density, that heat-insulating property is good is widely used as lagging material in fields such as building, vehicles.
Phase change material refers to that phase-changing energy storage material is a kind of novel green energy conservation material, phase change material by solid-state become liquid state or become solid-state process by liquid state be called phase transition process, not only form changes in phase transition process, also can absorb or discharge a large amount of latent heat.The application of phase change material has improved energy utilization rate, has reduced energy consumption.By add phase change material in foam materials, can play better heat insulation effect.But due to and phase change material has when the phase transformation liquid generation can affect the foaming effect of foam materials, simultaneously because foam materials is vesicular structure, liquid phase-change is easily revealed, and makes heat insulation effect weaken gradually.
Microcapsulary is that a kind of film forming material that utilizes is wrapped in solid, liquid or gaseous matter in capsule, and forming a diameter is the technology of the small container of micron order or millimeter meter.Microcapsule have protection something which is in the bag matter avoid revealing, extend the material storage time, with effects such as special material isolation, be widely used in a plurality of fields such as biological medicine, food, coating.
For the research of polyolefin foam, mainly concentrate on it and use the aspect with the preparation method at present.A kind of expanded polyolefin preparation method of high fondant-strength diaxial orientation is disclosed as CN101243122B; CN101263187B discloses a kind of soft polyolefin foams formula and preparation method with high heat resistance; CN1282693C discloses a kind of wide aperture polyolefin foam for absorbing sound, being incubated etc.And for phase change material and microcapsulary are applied in polyolefin foam simultaneously, the research that improves heat-insulating property yet there are no report.
Summary of the invention
For overcoming the weak point of existing cellular insulant, the invention provides a kind of phase-transition heat-preserving polyolefin foam that utilizes phase change material and microcapsulary exploitation and preparation method thereof, with the demand of satisfying the market to lagging material.
The present invention adopts following technical proposals to realize:
A kind of phase-transition heat-preserving polyolefin foam, take phase-change microcapsule, polyolefin resin, whipping agent, linking agent, frothing aid, colour batch, antiaging agent and processing aid as raw material, through mix, melt extrude, preheating, foaming and get, each component is counted by weight:
70～90 parts of polyolefin resines
1～10 part of phase-change microcapsule
3～20 parts of whipping agents
0.1～5 part of linking agent
0～1.5 part of frothing aid
0～15 part of colour batch
0～5 part of processing aid
Described phase-change microcapsule is prepared from by the component of following weight part:
30～80 parts of cyst materials
10～65 parts of phase transformation core materials
0.1～15 part of emulsifying agent
Described cyst material is one or more the mixture in carbamide resin, vibrin, melamine formaldehyde resin, urea-carbamide multipolymer, polymethacrylate, gelatin, Precondensed UreaFormaldehyde Resin, poly-polyprotonic acid, gelatin-Arabic gum, aminoresin, epoxy resin, melmac, urethane, cyclodextrin, styrene-maleic anhydride copolymer.
Described phase transformation core materials is one or more the mixture in paraffin, aliphatic hydrocarbon, lipid acid, fatty acid ester, polyvalent alcohol, hydrated inorganic salt.
Described emulsifying agent is one or more the mixture in Sodium dodecylbenzene sulfonate, polyoxyethylene sorbitan fatty acid ester, sorbitan fatty acid esters, acrylic homopolymer, acrylic copolymer, maleic anhydride class homopolymer, maleic anhydride analog copolymer, tween.
Described whipping agent is one or more the mixture in N-nitroso compound, azo-compound, hydrazide kind compound.
Described linking agent is one or more the mixture in peroxide cross-linking agent, silane crosslinker, quinones linking agent, polyol crosslink agent, polyamine linking agent.
Described frothing aid is one or more the mixture in stearic acid, oxalic acid, Whitfield's ointment, phthalic acid, Zinic stearas, barium stearate, lead stearate, zinc oxide, barium oxide, plumbous oxide.
Described processing aid is one or more the mixture in uv-absorbing agent, photostabilizer, oxidation inhibitor, softening agent, dispersion agent, lubricant.
The preparation method of a kind of phase-transition heat-preserving polyolefin foam of the present invention is:
After being prepared into phase-change microcapsule by single or multiple lift wall building method, then by mix, melt extrude, preheating, foaming make the phase-transition heat-preserving polyolefin foam.Its concrete operation is:
Step 1: the preparation of phase-change microcapsule
(1) phase transformation core materials, emulsifying agent are emulsified into emulsion according to a certain percentage under high-speed emulsifying machine, high-speed emulsifying machine rotating speed 1000～12000 turns/min, emulsification times 1～60min;
(2) adopt in-situ compositing, individual layer wall building method or multilayer wall building method that phase transformation core materials emulsion is wrapped in and be prepared into phase-change microcapsule in cyst material, 50～120 ℃ of temperature of reaction, pH value is 1～6, time 1～24h;
Step 2: the preparation of phase-transition heat-preserving polyolefin foam
(1) polyolefin base resin, phase-change microcapsule, whipping agent, linking agent, frothing aid, colour batch and processing aid thereof are added kneader in proportion, mediate 110 ℃～190 ℃ of temperature, kneading time 15～120min;
(2) material that mixes is added the forcing machine hopper, melt extrude by screw extrusion press.Wherein the extruder screw length-to-diameter ratio is greater than 28, and screw speed 30～70r/min melt extrudes 110 ℃～150 ℃ of temperature, the thickness 0.1～5mm of the master slice of extruding;
(3) master slice is carried out preheating through preheating oven, 90 ℃～180 ℃ of preheating temperatures, warm up time 0.5～15min;
(4) master slice is foamed through foaming furnace, 170 ℃～210 ℃ of blowing temperatures, foamed time 0.5～5min.
The present invention compared with prior art has following beneficial effect:
Phase change material is applied to polyolefine insulating foam material, and when temperature reduced, phase change material can undergo phase transition, release of heat, thereby adjusting ambient temperature.Simultaneously the present invention has adopted microcapsulary, and phase change material is wrapped in cyst wall inside as core materials, when making phase transformation occur, presents liquid phase transformation core materials and can not run off from the foam materials of porous, has improved the persistence of heat insulation effect.
Embodiment
Below by embodiment, the present invention will be further described.
Embodiment 1:The preparation of phase-change microcapsule
(1) n-tetradecane 40kg, Sodium dodecylbenzene sulfonate 2kg are mixed, be emulsified into emulsion under high-speed emulsifying machine, high-speed emulsifying machine rotating speed 1000r/min, emulsification times 5min;
(2) add carbamide performed polymer 20kg in emulsion, stir, by second acid for adjusting pH value 3.5, react 0.5h under 70 ℃, stirring velocity 500 r/min;
(3) be warming up to 90 ℃, continue reaction 1h, stirring velocity 500 r/min.
Behind step (1), (2), can prepare take n-tetradecane as capsule-core, take the phase-change microcapsule of melamine formaldehyde resin as the individual layer cyst wall; By step (1)～(3) can prepare take n-tetradecane as capsule-core, take the phase-change microcapsule of melamine formaldehyde resin as the multilayer cyst wall.
Embodiment 2:The preparation of phase-change microcapsule
(1) paraffin 10kg, tween emulsifier 6kg are mixed, be emulsified into emulsion under high-speed emulsifying machine, high-speed emulsifying machine rotating speed 3000r/min, emulsification times 5min;
(2) add urea aldehyde performed polymer 60kg in emulsion, stir, place 2h, continue during this period to stir stirring velocity 2500 r/min.；
(3) add urea formaldehyde resin curing agent ammonium chloride 1kg, stir, regulating pH value with acetic acid is 2～3, reacts 1h under 80 ℃, stirring velocity 2500 r/min;
(4) be warming up to 90 ℃, continue reaction 1h, stirring velocity 2500 r/min.
Can prepare take paraffin as capsule-core by step (1)～(3), take the phase-change microcapsule of urea-formaldehyde resin as the individual layer cyst wall; Can prepare take the phase-change microcapsule of urea-formaldehyde resin as the multilayer cyst wall by step (1)～(4).
Embodiment 3:The preparation of phase-change microcapsule
(1) get gelatin 10kg, Sudan Gum-arabic 25kg is prepared into respectively 15% the aqueous solution, is warming up to 55 ℃;
(2) get Octadecane 30kg, sorbitan fatty acid esters 5kg mixes, and is emulsified into emulsion under high-speed emulsifying machine, high-speed emulsifying machine rotating speed 1000r/min, emulsification times 5min;
(3) gelatin solution adds, and adjusting the pH value with citric acid is 4.0, stirs, and keeps 55 ℃ of system temperatures constant, reaction 2h;
(4) the Sudan Gum-arabic liquation that configures is added, adjusting the pH value with citric acid is 3.5, stirs, and keeps 55 ℃ of system temperatures constant, reaction 5h.
Can prepare take Octadecane as capsule-core by step (1)～(3), take the phase-change microcapsule of gelatin as the individual layer cyst wall; Can prepare take the phase-change microcapsule of gelatin-Arabic gum as the multilayer cyst wall by step (1)～(4).
Embodiment 4:The preparation of phase-transition heat-preserving polyolefin foam
(1) with phase-change microcapsule 5kg, the Cellmic C 121 8kg, dicumyl peroxide 0.5kg, the zinc oxide 0.2kg that prepare in polyethylene 70kg, embodiment 1, uv-absorbing agent 0.01kg, photostabilizer 0.01kg, oxidation inhibitor 0.01kg, dispersion agent 0.02kg, dropping in proportion kneader mediates, mediate 140 ℃ of temperature, time 20min;
(2) material is added the forcing machine hopper, and melt extrude through screw extrusion press.Wherein the forcing machine length-to-diameter ratio 40, and screw speed 40r/min, the design temperature of each section of forcing machine are 115 ℃, and 120 ℃, 130 ℃, 130 ℃, 130 ℃, 125 ℃, the master slice thickness 2mm that extrudes;
(3) master slice after extruding is the preheating oven of 90 ℃, 120 ℃, 160 ℃ through excess temperature successively, is respectively 2min, 1min, 1min warm up time, makes the linking agent in master slice full cross-linked, and make master slice inner with the outside temperature trend evenly;
(4) be the foaming furnace of 200 ℃ through excess temperature through the master slice after preheating, the time is 0.5min.
Prepared phase-transition heat-preserving polyolefine material expansion ratio is 20 times, and transformation temperature is 5.3 ℃.
Embodiment 5:The preparation of phase-transition heat-preserving polyolefin foam
(1) with phase-change microcapsule 3.5kg, the Cellmic C 121 10kg, dicumyl peroxide 1kg, the zinc oxide 0.2kg that prepare in polyethylene 60kg, ethylene-vinyl acetate copolymer 15kg, embodiment 2, uv-absorbing agent 0.01kg, photostabilizer 0.01kg, oxidation inhibitor 0.01kg, dispersion agent 0.02kg, dropping in proportion kneader mediates, mediate 135 ℃ of temperature, time 15min;
(2) material is added the forcing machine hopper, and melt extrude through screw extrusion press.Wherein the forcing machine length-to-diameter ratio 40, and screw speed 40r/min, the design temperature of each section of forcing machine are 110 ℃, and 120 ℃, 130 ℃, 130 ℃, 125 ℃, 120 ℃, the master slice thickness 2mm that extrudes;
(3) master slice after extruding is the preheating oven of 90 ℃, 110 ℃, 130 ℃ through excess temperature successively, is respectively 2min, 5min, 5min warm up time, makes the linking agent in master slice full cross-linked, and make master slice inner with the outside temperature trend evenly;
(4) be the foaming furnace of 180 ℃ through excess temperature through the master slice after preheating, the time is 0.5min.
Prepared phase-transition heat-preserving polyolefine material expansion ratio is 20 times, and transformation temperature is 13.1 ℃.
Embodiment 6:The preparation of phase-transition heat-preserving polyolefin foam
(1) with phase-change microcapsule 10kg, Cellmic C 121 15kg, the dicumyl peroxide 1.5kg of preparation in polyethylene 80kg, octene-ethylene copolymer 5kg, embodiment 3, drop in proportion kneader and mediate, mediate 115 ℃ of temperature, time 15min;
(2) material is added the forcing machine hopper, and melt extrude through screw extrusion press.Wherein the forcing machine length-to-diameter ratio 40, and screw speed 40r/min, the design temperature of each section of forcing machine are 110 ℃, and 115 ℃, 125 ℃, 125 ℃, 120 ℃, 120 ℃, the master slice thickness 2mm that extrudes;
(3) master slice after extruding is the preheating oven of 90 ℃, 110 ℃, 120 ℃ through excess temperature successively, is respectively 2min, 2min, 1min warm up time, makes the linking agent in master slice full cross-linked, and make master slice inner with the outside temperature trend evenly;
(4) be the foaming furnace of 210 ℃ through excess temperature through the master slice after preheating, the time is 0.2min.
Prepared phase-transition heat-preserving polyolefine material expansion ratio is 30 times, and transformation temperature is 30.5 ℃.
Claims (4)
1. phase-transition heat-preserving polyolefin foam, it is characterized in that: make as raw material take phase-change microcapsule, polyolefin resin, whipping agent, linking agent, frothing aid, colour batch, antiaging agent and processing aid, each component is counted by weight:
70～90 parts of polyolefin resines
1～10 part of phase-change microcapsule
3～20 parts of whipping agents
0.1～5 part of linking agent
0.1～1.5 part of frothing aid
0～15 part of colour batch
0～5 part of processing aid.
2. a kind of phase-transition heat-preserving polyolefin foam according to claim 1 is characterized in that described phase-change microcapsule is prepared from by the component of following weight part:
30～80 parts of cyst materials
10～65 parts of phase transformation core materials
0.1～15 part of emulsifying agent
Described cyst material is one or more the mixture in carbamide resin, vibrin, melamine formaldehyde resin, urea-carbamide multipolymer, polymethacrylate, gelatin, Precondensed UreaFormaldehyde Resin, poly-polyprotonic acid, gelatin-Arabic gum, aminoresin, epoxy resin, melmac, urethane, cyclodextrin, styrene-maleic anhydride copolymer; Described phase transformation core materials is one or more the mixture in paraffin, aliphatic hydrocarbon, lipid acid, fatty acid ester, polyvalent alcohol, hydrated inorganic salt; Described emulsifying agent is one or more the mixture in Sodium dodecylbenzene sulfonate, polyoxyethylene sorbitan fatty acid ester, sorbitan fatty acid esters, acrylic homopolymer, acrylic copolymer, maleic anhydride class homopolymer, maleic anhydride analog copolymer, tween.
3. a kind of phase-transition heat-preserving polyolefin foam according to claim 1 is characterized in that: described whipping agent is one or more the mixture in N-nitroso compound, azo-compound, hydrazide kind compound; Described linking agent is one or more the mixture in peroxide cross-linking agent, silane crosslinker, quinones linking agent, polyol crosslink agent, polyamine linking agent; Described frothing aid is one or more the mixture in stearic acid, oxalic acid, Whitfield's ointment, phthalic acid, Zinic stearas, barium stearate, lead stearate, zinc oxide, barium oxide, plumbous oxide; Described processing aid is one or more the mixture in uv-absorbing agent, photostabilizer, oxidation inhibitor, softening agent, dispersion agent, lubricant.
4. its preparation method of according to claim 1,2 or 3 described a kind of phase-transition heat-preserving polyolefin foams, it is characterized in that: after being prepared into phase-change microcapsule by single or multiple lift wall building method, again by mix, melt extrude, preheating, foaming make the phase-transition heat-preserving polyolefin foam, its concrete steps are as follows:
Step 1: the preparation of phase-change microcapsule
1) phase transformation core materials, emulsifying agent are emulsified into emulsion according to a certain percentage under high-speed emulsifying machine, high-speed emulsifying machine rotating speed 1000～12000 turns/min, emulsification times 1～60min;
2) adopt in-situ compositing, individual layer wall building method or multilayer wall building method that phase transformation core materials emulsion is wrapped in and be prepared into phase-change microcapsule in cyst material, 50～120 ℃ of temperature of reaction, pH value are 1～6, time 1～24h;
Step 2: the preparation of phase-transition heat-preserving polyolefin foam
1) polyolefin base resin, phase-change microcapsule, whipping agent, linking agent, frothing aid, colour batch and processing aid are added kneader in proportion, mediate 110 ℃～190 ℃ of temperature, kneading time 15～120min;
2) material that mixes is added the forcing machine hopper, melt extrude by screw extrusion press, wherein the extruder screw length-to-diameter ratio is greater than 28, and screw speed 30～70r/min melt extrudes 110 ℃～150 ℃ of temperature, the thickness 0.1～5mm of the master slice of extruding;
3) master slice is carried out preheating through preheating oven, 90 ℃～180 ℃ of preheating temperatures, warm up time 0.5～15min;
4) master slice is foamed through foaming furnace, 170 ℃～210 ℃ of blowing temperatures, foamed time 0.5～5min.
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Application publication date: 20130515 |