CN106046293A - Preparation method of active-temperature-regulation noctilucent rigid foam material - Google Patents

Preparation method of active-temperature-regulation noctilucent rigid foam material Download PDF

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Publication number
CN106046293A
CN106046293A CN201610476028.1A CN201610476028A CN106046293A CN 106046293 A CN106046293 A CN 106046293A CN 201610476028 A CN201610476028 A CN 201610476028A CN 106046293 A CN106046293 A CN 106046293A
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China
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rigid foam
temperature
regulation
noctilucent
foam material
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Inventor
胡先海
罗俊杰
付昌春
罗辉
王书升
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ANHUI SIWEI NEW BUILDING MATERIAL Co Ltd
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ANHUI SIWEI NEW BUILDING MATERIAL Co Ltd
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Priority to CN201610476028.1A priority Critical patent/CN106046293A/en
Publication of CN106046293A publication Critical patent/CN106046293A/en
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40—High-molecular-weight compounds
    • C08G18/4009—Two or more macromolecular compounds not provided for in one single group of groups C08G18/42 - C08G18/64
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    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
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    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
    • C08J9/12—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent
    • C08J9/14—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent organic
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    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
    • C08J9/12—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent
    • C08J9/14—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent organic
    • C08J9/143—Halogen containing compounds
    • C08J9/144—Halogen containing compounds containing carbon, halogen and hydrogen only
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    • C08L75/00—Compositions of polyureas or polyurethanes; Compositions of derivatives of such polymers
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    • 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
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    • C08G2110/00—Foam properties
    • C08G2110/0025—Foam properties rigid
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    • C08J2203/00—Foams characterized by the expanding agent
    • C08J2203/14—Saturated hydrocarbons, e.g. butane; Unspecified hydrocarbons
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    • C08J2203/00—Foams characterized by the expanding agent
    • C08J2203/18—Binary blends of expanding agents
    • C08J2203/182—Binary blends of expanding agents of physical blowing agents, e.g. acetone and butane
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08J2375/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
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    • C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
    • C08J2423/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
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    • C08L2203/14—Applications used for foams
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  • Manufacturing Of Micro-Capsules (AREA)
  • Luminescent Compositions (AREA)

Abstract

The invention discloses a preparation method of an active-temperature-regulation noctilucent rigid foam material. A long-afterglow rare-earth noctilucent material and a photo-thermal conversion energy-storage temperature-regulation material are utilized to prepare the polyurethane rigid foam. The preparation method comprises the following steps: proportionally weighing polyester polyol, polyether glycol, the nano long-afterglow rare-earth noctilucent material, the photo-thermal conversion energy-storage temperature-regulation material, silicone oil, a catalyst, a foaming agent and a flame retardant, uniformly mixing, and mixing with modified MDI (methylenediphenyl diisocyanate) at high speed; and when foam emits and becomes white, injecting the mixture into a mold, foaming, fixing, demolding and postcuring to obtain the active-temperature-regulation noctilucent rigid foam material. The polyurethane rigid foam material prepared by the method can store the light energy under lighting conditions, and can maintain the environmental space within a certain brightness without illumination at night. Besides, the active-temperature-regulation noctilucent rigid foam material can store the light energy into the phase transition energy, and can release the stored light energy in the form of heat when the ambient temperature is lower than a certain value, thereby achieving the goal of heating and thermal insulation to some extent.

Description

A kind of preparation method of active homoiothermic noctilucence rigid foam material
Technical field
The invention belongs to building material field, be specifically related to the preparation method of a kind of active homoiothermic noctilucence rigid foam material.
Background technology
As optimal insulation material, rigid polyurethane foam heat insulation composite board is the applicating history in existing more than 30 years in Europe, And it is widely used in various public and residential construction area.Along with implementing of national energy-saving policy and going deep into of energy-conservation sight, poly- The urethane thermal insulating composite panel that hard bubbles because of the energy conservation characteristic of its brilliance, the relatively characteristic such as high performance-price ratio and environmental protection, have the most wide Market prospect.This product has the heat-insulating property of brilliance and preferable anti-bending strength, and intensity height, surfacing, template Fashionable, in terms of insulation and fire prevention, especially reach international most advanced level, won the accreditation in market, receive user's Welcome.But this material is passive insulation material, relies primarily on relatively low heat conductivity and reach the purpose of insulation.Can not be actively Improve ambient temperature.
Long after glow luminous material is called for short long-afterglow material, and the light-storing and emitting material that is otherwise known as, Noctilucent material, it is substantially It it is a kind of embedded photoluminescent material.It is that a class absorbs energy, such as visible ray, ultraviolet light, X-ray etc., and after exciting stopping still Can continue to send the material of light, it can store energy in falling into, and is a kind of material with application prospect.People are in reality Life utilizes the characteristic that the RE luminous material over time of long afterglow is luminous, makes various light-passing plastic and be pressed into various symbol together Number, parts, articles for use (such as on and off switch, socket etc.) and the wall decoration of various families.These luminous components through light irradiate after, night Between or accidental power failure it still at continuous illumination, make people can distinguish peripheral direction, for work and life bring convenience.It addition, can To reduce the use of night illumination power supply, reach the effect of energy-saving and emission-reduction.
Summary of the invention
The technical problem to be solved is to provide the preparation method of a kind of active homoiothermic noctilucence rigid foam material.
For solving above-mentioned technical problem, the technical solution used in the present invention is as follows:
The preparation method of a kind of active homoiothermic noctilucence rigid foam material, it is characterised in that by PEPA, polyether polyols Alcohol, SrAl2O4:Eu2+,Dy3+, photothermal deformation accumulation of energy thermal control material, silicone oil, dibutyl tin laurate, Pentamethylene. and poly Ammonium phosphate (APP) is according to following mass fraction mix homogeneously:
Regulating system temperature to 25 DEG C, then high-speed stirred is mixed together with the modified MDI BASF M20S of 2 parts of quality Close, observe have bubble to send, foam injects in mould when turning white and foams, through swollen fixed, demoulding and after solidify, obtain actively homoiothermic night Light rigid foam material.
The active homoiothermic noctilucence rigid foam material that the inventive method prepares, can be as ceiling decoration, decorative material for wall surface Etc. being widely used in building materials of house fitting-up field.
Beneficial effects of the present invention:
1, luminous effect, it is possible to environmental protection and energy saving.Under conditions of need not illuminating night, it is possible to certain in maintaining environment space Brightness.
2, under illumination condition, it is possible to luminous energy is stored, and when ambient temperature is less than a certain particular value, it is possible to will storage The luminous energy deposited discharges in the form of heat, reaches certain heating and heat preservation purpose (actively heat preservation property).
Detailed description of the invention
According to following embodiment, the present invention be may be better understood.But, as it will be easily appreciated by one skilled in the art that reality Execute the content described by example and be merely to illustrate the present invention, and should be also without limitation on basis described in detail in claims Invention.
Embodiment 1:
The preparation method of a kind of active homoiothermic noctilucence rigid foam material: more than PEPA, polyether polyol, nanoscale length The RE luminous material of brightness, photothermal deformation accumulation of energy thermal control material, silicone oil, double dimethylaminoethyl ether, 1-chloro-3,3,3-trifluoro propene And fire retardant following mass fraction mix homogeneously:
Regulating system temperature to 30 DEG C, then high-speed stirred is mixed together with the modified MDI Bayer 44v20 of 1.5 parts of quality Close, observe have bubble to send, foam injects in mould when turning white and foams, through swollen fixed, demoulding and after solidify, obtain actively homoiothermic night Light rigid foam material.
Wherein, PEPA, polyether polyol molecular weight are 1300, and hydroxyl value is 400KOH/g, and degree of functionality is 5.
Wherein, the RE luminous material of nanoscale long afterglow is Zn3Ga2Ge2O10:Cr3+, material particle size is 200nm.
Wherein, the preparation of photothermal deformation accumulation of energy thermal control material comprises the steps:
1) melting mixing, shape at 120 DEG C by the phase-change material micro-capsule of 10 parts of quality and the polyethylene pelletizing of 2 parts of quality Become melt I.
2) by the polypropylene pelletizing melting mixing of the nanometer zirconium carbide powder (particle diameter 50nm) of 4 parts of quality Yu 1 part of quality, shape Become melt II.
3) being mixed according to mass ratio 2:1 with melt II by melt I, cooling granulation is also pulverized, and obtains photothermal deformation accumulation of energy and adjusts Adiabator, particle size range is 200nm.
Wherein, the preparation of described phase-change material micro-capsule, comprise the steps:
1) n-octadecane emulsion is prepared.Take 2g atactic styrene-maleic anhydride copolymer powder, 0.4g NaOH and 100mL Water joins in there-necked flask.Heating in water bath is warming up to 90 DEG C, and keeps 2h, when solution presents pale yellow transparent shape, uses 1mol/L citric acid solution regulation solution ph is to 5.Then take 40g n-octadecane to be mixed with, after n-octadecane is melted, adopt With high speed dispersor, n-octadecane solution being carried out emulsifying, rotating speed is 16000 revs/min.Maintain emulsification system temperature at 70 DEG C.
2) performed polymer is prepared.Take 4.0g tripolycyanamide and 0.5g urea powder, 9g formalin (mass fraction 37%- 40%) and 30mL water joins in 100mL there-necked flask, and with triethanolamine, system pH is adjusted to 8.5.Heating in water bath arrives 70 DEG C, after solution went clear, continue insulation 50min.
3) microcapsule is prepared.Being added drop-wise in n-octadecane emulsion by the performed polymer prepared, time for adding controls 15min.Maintain reaction temperature at 70 DEG C, response time 5h.Take out sample, washing, sucking filtration after completing, obtain the micro-glue of phase-change material Capsule.
Wherein, described fire retardant is ammonium polyphosphate (APP) and three (2,3-dibromopropyl) fulminuric acid ester (TBC) To wait mass mixing.
PEPA, polyether polyol that the present invention uses are preferably the many glycol of polyester, the many glycol of polyethers.
Embodiment 2:
The preparation method of a kind of active homoiothermic noctilucence rigid foam material: more than PEPA, polyether polyol, nanoscale length The RE luminous material of brightness, photothermal deformation accumulation of energy thermal control material, silicone oil, pentamethyl-diethylenetriamine, pentafluoropropane and methylphosphine Dimethyl phthalate (DMMP) is according to following mass fraction mix homogeneously:
System temperature is regulated to 18 DEG C, then high-speed stirred together with the modified MDI Yantai ten thousand China PM-200 of 1 part of quality Mixing, observe have bubble to send, foam injects in mould when turning white and foams, through swollen fixed, demoulding and after solidify, obtain actively homoiothermic Noctilucence rigid foam material.
Wherein, PEPA, polyether polyol molecular weight are 800, and hydroxyl value is 430KOH/g, and degree of functionality is 3.
Wherein, the RE luminous material of nanoscale long afterglow is Sr2MgSi2O7:Eu2+,Dy3+, material particle size is 500nm.
Wherein, the preparation of photothermal deformation accumulation of energy thermal control material comprises the steps:
1) melting mixing, shape at 100 DEG C by the phase-change material micro-capsule of 5 parts of quality and the polyethylene pelletizing of 1 part of quality Become melt I.
2) by the polypropylene pelletizing melting mixing of the nanometer zirconium carbide powder (particle diameter 100nm) of 4 parts of quality Yu 1 part of quality, Form melt II.
3) being mixed according to mass ratio 1:1 with melt II by melt I, cooling granulation is also pulverized, and obtains photothermal deformation accumulation of energy and adjusts Adiabator, particle size range is 500nm.
Wherein, the preparation of described phase-change material micro-capsule, comprise the steps:
1) n-octadecane emulsion is prepared.Take 4g atactic styrene-maleic anhydride copolymer powder, 0.6g NaOH and 100mL Water joins in there-necked flask.Heating in water bath is warming up to 95 DEG C, and keeps 1h, when solution presents pale yellow transparent shape, uses 1mol/L citric acid solution regulation solution ph is to 6.Then take 80g n-octadecane to be mixed with, after n-octadecane is melted, adopt With high speed dispersor, n-octadecane solution being carried out emulsifying, rotating speed is 17000 revs/min.Maintain emulsification system temperature at 60 DEG C.
2) performed polymer is prepared.Take 3.5g tripolycyanamide and 0.4g urea powder, 8g formalin (mass fraction 37%- 40%) and 30mL water joins in 100mL there-necked flask, and with triethanolamine, system pH is adjusted to 8.Heating in water bath is to 80 DEG C, after solution went clear, continue insulation 60min.
3) microcapsule is prepared.Being added drop-wise in n-octadecane emulsion by the performed polymer prepared, time for adding controls 17min.Maintain reaction temperature at 80 DEG C, response time 4h.Take out sample, washing, sucking filtration after completing, obtain the micro-glue of phase-change material Capsule.
Embodiment 3:
The preparation method of a kind of active homoiothermic noctilucence rigid foam material: more than PEPA, polyether polyol, nanoscale length The RE luminous material of brightness, photothermal deformation accumulation of energy thermal control material, silicone oil, dibutyl tin laurate, Pentamethylene. and polyphosphoric acids Ammonium (APP) is according to following mass fraction mix homogeneously:
Regulating system temperature to 25 DEG C, then high-speed stirred is mixed together with the modified MDI BASF M20S of 2 parts of quality Close, observe have bubble to send, foam injects in mould when turning white and foams, through swollen fixed, demoulding and after solidify, obtain actively homoiothermic night Light rigid foam material.
Wherein, PEPA, polyether polyol molecular weight are 1200, and hydroxyl value is 420KOH/g, and degree of functionality is 8.
Wherein, the RE luminous material of nanoscale long afterglow is SrAl2O4:Eu2+,Dy3+, material particle size is 400nm.
Wherein, the preparation of photothermal deformation accumulation of energy thermal control material comprises the steps:
1) melting mixing at 180 DEG C by the phase-change material micro-capsule of 8 parts of quality and the polyethylene pelletizing of 1.5 parts of quality, Form melt I.
2) by the polypropylene pelletizing melting mixing of the nanometer zirconium carbide powder (particle diameter 80nm) of 3 parts of quality Yu 2 parts of quality, shape Become melt II.
3) being mixed according to mass ratio 3:1 with melt II by melt I, cooling granulation is also pulverized, and obtains photothermal deformation accumulation of energy and adjusts Adiabator, particle size range is 300nm.
Wherein, the preparation of described phase-change material micro-capsule, comprise the steps:
1) n-octadecane emulsion is prepared.Take 3g atactic styrene-maleic anhydride copolymer powder, 0.8g NaOH and 100mL Water joins in there-necked flask.Heating in water bath is warming up to 80 DEG C, and keeps 1.5h, when solution presents pale yellow transparent shape, uses 1mol/L citric acid solution regulation solution ph is to 5.5.Then take 60g n-octadecane to be mixed with, after n-octadecane is melted, Using high speed dispersor that n-octadecane solution is carried out emulsifying, rotating speed is 18000 revs/min.Maintain emulsification system temperature at 80 DEG C.
2) performed polymer is prepared.Take 3.8g tripolycyanamide and 0.3g urea powder, 8.5g formalin (mass fraction 37%- 40%) and 30mL water joins in 100mL there-necked flask, and with triethanolamine, system pH is adjusted to 9.Heating in water bath is to 65 DEG C, after solution went clear, continue insulation 70min.
3) microcapsule is prepared.Being added drop-wise in n-octadecane emulsion by the performed polymer prepared, time for adding controls 13min.Maintain reaction temperature at 65 DEG C, response time 3h.Take out sample, washing, sucking filtration after completing, obtain the micro-glue of phase-change material Capsule.
Embodiment 4:
The preparation method of a kind of active homoiothermic noctilucence rigid foam material: more than PEPA, polyether polyol, nanoscale length The RE luminous material of brightness, photothermal deformation accumulation of energy thermal control material, silicone oil, organo-bismuth, Pentamethylene. and three (2,3-dibromopropyls) are different Cyanurate (TBC) is according to following mass fraction mix homogeneously:
By system temperature regulate to 20 DEG C, then step 5005 with the modified MDI Hensel of 1 part of quality together with high-speed stirred mix Close, observe have bubble to send, foam injects in mould when turning white and foams, through swollen fixed, demoulding and after solidify, obtain actively homoiothermic night Light rigid foam material.
Wherein, PEPA, polyether polyol molecular weight are 1100, and hydroxyl value is 410KOH/g, and degree of functionality is 6.
Wherein, the RE luminous material of nanoscale long afterglow is Zn3Ga2Ge2O10:Cr3+With Sr2MgSi2O7:Eu2+,Dy3+With etc. Mass mixing, material particle size is 400nm.
Wherein, the preparation of photothermal deformation accumulation of energy thermal control material comprises the steps:
1) melting mixing, shape at 150 DEG C by the phase-change material micro-capsule of 6 parts of quality and the polyethylene pelletizing of 1 part of quality Become melt I.
2) by the polypropylene pelletizing melting mixing of the nanometer zirconium carbide powder (particle diameter 60nm) of 3 parts of quality Yu 1 part of quality, shape Become melt II.
3) being mixed according to mass ratio 2:1 with melt II by melt I, cooling granulation is also pulverized, and obtains photothermal deformation accumulation of energy and adjusts Adiabator, particle size range is 400nm.
Wherein, the preparation of described phase-change material micro-capsule, comprise the steps:
1) n-octadecane emulsion is prepared.Take 2.5g atactic styrene-maleic anhydride copolymer powder, 0.5g NaOH and 100mL water joins in there-necked flask.Heating in water bath is warming up to 90 DEG C, and keeps 1.5h, when solution presents pale yellow transparent shape Time, by 1mol/L citric acid solution regulation solution ph to 5.Then take 70g n-octadecane to be mixed with, treat that n-octadecane is melted After, use high speed dispersor that n-octadecane solution is carried out emulsifying, rotating speed is 18000 revs/min.Maintain emulsification system temperature 65 ℃。
2) performed polymer is prepared.Take 3.6g tripolycyanamide and 0.3g urea powder, 9g formalin (mass fraction 37%- 40%) and 30mL water joins in 100mL there-necked flask, and with triethanolamine, system pH is adjusted to 8.Heating in water bath is to 70 DEG C, after solution went clear, continue insulation 55min.
3) microcapsule is prepared.Being added drop-wise in n-octadecane emulsion by the performed polymer prepared, time for adding controls 14min.Maintain reaction temperature at 70 DEG C, response time 3.5h.Take out sample, washing, sucking filtration after completing, obtain phase-change material micro- Capsule.
Wherein, described foaming agent is Pentamethylene. with 1-chloro-3,3,3 ,-trifluoropropene to wait mass mixing.
Embodiment 5:
The preparation method of a kind of active homoiothermic noctilucence rigid foam material: more than PEPA, polyether polyol, nanoscale length The RE luminous material of brightness, photothermal deformation accumulation of energy thermal control material, silicone oil, dimethyl cyclohexyl amine, pentafluoropropane and fire retardant Following mass fraction mix homogeneously:
Regulating system temperature to 28 DEG C, then high-speed stirred mixes together with the modified MDI Bayer 44v20 of 2 parts of quality, Inject in mould when observation has bubble to send, foam turns white and foam, through swollen fixed, demoulding and after solidify, obtain actively homoiothermic noctilucence Rigid foam material.
Wherein, PEPA, polyether polyol molecular weight are 900, and hydroxyl value is 420KOH/g, and degree of functionality is 7.
Wherein, the RE luminous material of nanoscale long afterglow is Zn3Ga2Ge2O10:Cr3+With SrAl2O4:Eu2+,Dy3+With etc. matter Amount mixing, material particle size is 300nm.
Wherein, the preparation of photothermal deformation accumulation of energy thermal control material comprises the steps:
1) melting mixing, shape at 160 DEG C by the phase-change material micro-capsule of 7 parts of quality and the polyethylene pelletizing of 2 parts of quality Become melt I.
2) by the polypropylene pelletizing melting mixing of the nanometer zirconium carbide powder (particle diameter 70nm) of 3 parts of quality Yu 2 parts of quality, shape Become melt II.
3) being mixed according to mass ratio 3:1 with melt II by melt I, cooling granulation is also pulverized, and obtains photothermal deformation accumulation of energy and adjusts Adiabator, particle size range is 300nm.
Wherein, the preparation of described phase-change material micro-capsule, comprise the steps:
1) n-octadecane emulsion is prepared.Take 3.5g atactic styrene-maleic anhydride copolymer powder, 0.7g NaOH and 100mL water joins in there-necked flask.Heating in water bath is warming up to 85 DEG C, and keeps 2h, when solution presents pale yellow transparent shape, By 1mol/L citric acid solution regulation solution ph to 6.Then take 50g n-octadecane to be mixed with, after n-octadecane is melted, Using high speed dispersor that n-octadecane solution is carried out emulsifying, rotating speed is 17000 revs/min.Maintain emulsification system temperature at 75 DEG C.
2) performed polymer is prepared.Take 3.3g tripolycyanamide and 0.4g urea powder, 8g formalin (mass fraction 37%- 40%) and 30mL water joins in 100mL there-necked flask, and with triethanolamine, system pH is adjusted to 8.5.Heating in water bath arrives 75 DEG C, after solution went clear, continue insulation 65min.
3) microcapsule is prepared.Being added drop-wise in n-octadecane emulsion by the performed polymer prepared, time for adding controls 16min.Maintain reaction temperature at 75 DEG C, response time 4.5h.Take out sample, washing, sucking filtration after completing, obtain phase-change material micro- Capsule.
Wherein, described fire retardant is ammonium polyphosphate (APP) with dimethyl methyl phosphonate (DMMP) to wait mass mixing.
Comparative example 1:
The preparation method of a kind of luminous polyurethane rigid foam material: by PEPA, polyether polyol, nanoscale long afterglow RE luminous material, silicone oil, dibutyl tin laurate, Pentamethylene. and ammonium polyphosphate (APP) are according to following mass fraction Mix homogeneously:
Regulating system temperature to 25 DEG C, then high-speed stirred is mixed together with the modified MDI BASF M20S of 2 parts of quality Close, observe have bubble to send, foam injects in mould when turning white and foams, through swollen fixed, demoulding and after solidify, obtain luminous polyurethane Rigid foam material.
Wherein, PEPA, polyether polyol molecular weight are 1200, and hydroxyl value is 420KOH/g, and degree of functionality is 8.
Wherein, the RE luminous material of nanoscale long afterglow is SrAl2O4:Eu2+,Dy3+, material particle size is 400nm.
Comparative example 2:
The preparation method of a kind of accumulation of energy heat insulating polyurethane hard foam material: by PEPA, polyether polyol, photothermal deformation Accumulation of energy thermal control material, silicone oil, pentamethyl-diethylenetriamine, pentafluoropropane and dimethyl methyl phosphonate (DMMP) are according to following matter Amount number mix homogeneously:
System temperature is regulated to 18 DEG C, then high-speed stirred together with the modified MDI Yantai ten thousand China PM-200 of 1 part of quality Mixing, observe have bubble to send, foam injects in mould when turning white and foams, through swollen fixed, demoulding and after solidify, obtain accumulation of energy insulation Polyurethane rigid foam material.
Wherein, PEPA, polyether polyol molecular weight are 800, and hydroxyl value is 430KOH/g, and degree of functionality is 3.
Wherein, the preparation of photothermal deformation accumulation of energy thermal control material comprises the steps:
1) melting mixing, shape at 100 DEG C by the phase-change material micro-capsule of 5 parts of quality and the polyethylene pelletizing of 1 part of quality Become melt I.
2) by the polypropylene pelletizing melting mixing of the nanometer zirconium carbide powder (particle diameter 100nm) of 4 parts of quality Yu 1 part of quality, Form melt II.
3) being mixed according to mass ratio 1:1 with melt II by melt I, cooling granulation is also pulverized, and obtains photothermal deformation accumulation of energy and adjusts Adiabator, particle size range is 500nm.
Wherein, the preparation of described phase-change material micro-capsule, comprise the steps:
1) n-octadecane emulsion is prepared.Take 4g atactic styrene-maleic anhydride copolymer powder, 0.6g NaOH and 100mL Water joins in there-necked flask.Heating in water bath is warming up to 95 DEG C, and keeps 1h, when solution presents pale yellow transparent shape, uses 1mol/L citric acid solution regulation solution ph is to 6.Then take 80g n-octadecane to be mixed with, after n-octadecane is melted, adopt With high speed dispersor, n-octadecane solution being carried out emulsifying, rotating speed is 17000 revs/min.Maintain emulsification system temperature at 60 DEG C.
2) performed polymer is prepared.Take 3.5g tripolycyanamide and 0.4g urea powder, 8g formalin (mass fraction 37%- 40%) and 30mL water joins in 100mL there-necked flask, and with triethanolamine, system pH is adjusted to 8.Heating in water bath is to 80 DEG C, after solution went clear, continue insulation 60min.
3) microcapsule is prepared.Being added drop-wise in n-octadecane emulsion by the performed polymer prepared, time for adding controls 17min.Maintain reaction temperature at 80 DEG C, response time 4h.Take out sample, washing, sucking filtration after completing, obtain the micro-glue of phase-change material Capsule.
Embodiment 6:
Active homoiothermic noctilucence rigid foam material character such as following table prepared by the present invention:
Test event Embodiment 1 Embodiment 2 Embodiment 3 Embodiment 4 Embodiment 5 Comparative example 1 Comparative example 2
Heat conductivity W/ (m k) 0.017 0.022 0.021 0.025 0.021 0.025 0.027
Accumulation of energy heat-insulating property DEG C/h 0.87 0.95 1.02 0.90 0.92 2.03 0.98
Persistence h 30 10 20 24 25 10 0
Twilight sunset initial luminous brightness cd/m2 1.298 1.034 1.011 1.027 1.102 1.032 0
Noctilucence performance test:
Use the afterglow property of PR-305 phosphorescence afterglow luminance test instrument test material, arrange and excite illumination 1000Lx.By The most sensitive to illumination in noctilucent coating, can not be affected by other light in test process, therefore, test is entered in dark place OK.
Under illumination condition, the accumulation of energy heat-insulating property of material measures:
Material in embodiment and comparative example is cut into the sheet material of 1m × 1m × 10mm, sheet material is surrounded a 1m × 1m The hollow cubic body of × 1m, centre arranges the cold light source that a power is 10W, and initial external environment temperature is set to 25 DEG C, then will External environment temperature is reduced to 10 DEG C, tests hollow cubic body internal temperature T after 2h.The accumulation of energy heat-insulating property of material is with in interior environment Rate of temperature fall characterize, the variations in temperature in portion in the hollow cubic body that i.e. in the unit interval, material surrounds.Rate of temperature fall is the least, Material heat-insulating property is the best.
The a series of detailed description of those listed above is only for the feasibility embodiment of the present invention specifically Bright, they also are not used to limit the scope of the invention, all equivalent implementations made without departing from skill of the present invention spirit Or change should be included within the scope of the present invention.
Although moreover, it will be appreciated that this specification is been described by according to embodiment, but the most each embodiment only wraps Containing an independent technical scheme, this narrating mode of description is only that for clarity sake those skilled in the art should Description can also be formed those skilled in the art through appropriately combined as an entirety, the technical scheme in each embodiment May be appreciated other embodiments.

Claims (1)

1. the preparation method of an actively homoiothermic noctilucence rigid foam material, it is characterised in that by PEPA, polyether polyol, SrAl2O4:Eu2+,Dy3+, photothermal deformation accumulation of energy thermal control material, silicone oil, dibutyl tin laurate, Pentamethylene. and polyphosphoric acids Ammonium (APP) is according to following mass fraction mix homogeneously:
Regulating system temperature to 25 DEG C, then high-speed stirred mixes together with the modified MDI BASF M20S of 2 parts of quality, sees Examined that bubble sends, foam injects in mould when turning white and foams, through swollen fixed, demoulding and after solidify, obtain actively homoiothermic noctilucence hard Foam material.
CN201610476028.1A 2016-06-24 2016-06-24 Preparation method of active-temperature-regulation noctilucent rigid foam material Pending CN106046293A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107513253A (en) * 2017-08-17 2017-12-26 东莞市鼎耀实业有限公司 Compound carbon fiber spectacle frame and its preparation technology
CN109180893A (en) * 2018-08-14 2019-01-11 山东科技大学 Grouting low heat value high-strength polyurethane material and preparation method thereof

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103772963A (en) * 2012-10-24 2014-05-07 中国石油化工股份有限公司 Phase-change energy-storage polyurethane foam and preparation method thereof

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103772963A (en) * 2012-10-24 2014-05-07 中国石油化工股份有限公司 Phase-change energy-storage polyurethane foam and preparation method thereof

Non-Patent Citations (5)

* Cited by examiner, † Cited by third party
Title
LI WEI等: "Preparation and characterization of microencapsulated phase change material with low remnant formaldehyde contend", 《MATERIALS CHEMISTRY AND PHYSICS》 *
NIHAL SARIER等: "Thermal characteristics of polyurethane foams incorporated with phase change materials", 《THERMOCHIMICA ACTA》 *
中国稀土学会: "《稀土科学技术学科发展报告》", 30 April 2016, 中国科学技术出版社 *
王曙中等: "《高科技纤维概论》", 30 June 2014, 北京交通大学出版社 *
由明等: "添加相变材料微胶囊的聚氨酯泡沫制备及表征", 《化工新型材料》 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107513253A (en) * 2017-08-17 2017-12-26 东莞市鼎耀实业有限公司 Compound carbon fiber spectacle frame and its preparation technology
CN109180893A (en) * 2018-08-14 2019-01-11 山东科技大学 Grouting low heat value high-strength polyurethane material and preparation method thereof
CN109180893B (en) * 2018-08-14 2020-10-09 山东科技大学 Low-calorific-value high-strength polyurethane material for coal mine grouting and preparation method thereof

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