CN109251513A - A kind of polyurethane foamed material and its processing method of counter infrared ray radiation - Google Patents
A kind of polyurethane foamed material and its processing method of counter infrared ray radiation Download PDFInfo
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- CN109251513A CN109251513A CN201811083587.1A CN201811083587A CN109251513A CN 109251513 A CN109251513 A CN 109251513A CN 201811083587 A CN201811083587 A CN 201811083587A CN 109251513 A CN109251513 A CN 109251513A
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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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- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/08—Processes
- C08G18/0804—Manufacture of polymers containing ionic or ionogenic groups
- C08G18/0819—Manufacture of polymers containing ionic or ionogenic groups containing anionic or anionogenic groups
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- C08G18/752—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group
- C08G18/753—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group
- C08G18/755—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group and at least one isocyanate or isothiocyanate group linked to a secondary carbon atom of the cycloaliphatic ring, e.g. isophorone diisocyanate
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- C08J2203/00—Foams characterized by the expanding agent
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Abstract
The invention discloses the polyurethane foamed materials and its processing method of a kind of counter infrared ray radiation, the polyurethane foamed material crosses aerogel powder using nanometer tungsten oxide, graphene-supported titanium dioxide, dibutyltin maleate is mixed to form the thermal radiation resistance filler of infrared absorption type by the way that sulfonated carbon nano-tube modification polyurethane and good uvioresistant, the ethylene-vinyl acetate copolymer of compatibility, sorbeth polyalcohol are mixed to get premix.Wherein the preparation method of sulfonated carbon nano-tube modification polyurethane includes base polyurethane prepolymer for use as preparation, the preparation of sulfonic acid carbon nano tube, Hybrid Heating distillation.Polyurethane foam preparation method of the invention is simple, stable molding, has excellent counter infrared ray radiation, thermal and insulating performance, and will not occur after long-term expose to the sun and rain significantly to shrink and cracking, meets the requirement of solar water heater thermal insulation material.
Description
Technical field
The present invention relates to polyurethane foam technology fields, and in particular to a kind of polyurethane foamed material of counter infrared ray radiation and
Its processing method.
Background technique
Polyurethane foamed material can be divided into soft and two class of hard according to hardness, due to good mechanical strength, resistance to
The performances such as performance, caking property, elasticity, weather-proof, chemically-resistant are ground, can be used as coating, adhesive, sealant, elastomer, foam cotton
Deng.Polyurethane foamed material is generally by isocyanates, aliphatic polyester and polyether polyol in chain extender, catalyst, fire retardant
Etc. generate under the action of multiple additives.
In recent years, solar water heater is as the energy-saving green product greatly developed, to improve living environment, section
About the energy, reduction pollution make a great contribution.The polyurethane foamed material of hard is because its moulding process is simple, thermal coefficient
It is low, therefore become the first choice of solar water heater thermal insulation material.But the rigid polyurethane foam that solar water heater uses at present
The generally existing following problems of foam material: 1, polyurethane foam is easy to happen contraction after long-term rain, and laterally or longitudinally cracks, leads
It causes foam to be detached from or completely disengage with casing part, greatly reduces the heat insulation effect to water tank；2, solar water heater is long-term
Exposure outdoors, and having nearly half in solar energy is infrared energy, infra-red radiation is the main source for generating heat；?
After polyurethane foamed material absorbs a large amount of infra-red radiation heat, due to lacking good infrared absorption, optical filtering heat-blocking action,
Lead to expanded by heating, reduce thermal coefficient, heat insulation effect reduces；3, lack effective foamed time, lead to foam inner air vent
Unevenly, molding time is inadequate, there is the phenomenon that continuing expansion or shrinkage after solidification, mechanical performance is unstable.
A kind of preparation method for coating cellular polyurethane foam is disclosed in the patent of application number 201711215394.2, is led to
Coating, high-temperature digestion molding are crossed after mixing polyvinyl acetate with isocyanates, polyurethane elastomer is coated on
Except usual foam, make the characteristics such as foam has wear-resisting, shock resistance, corrosion-resistant, intensity is high, production cost is low, easy to operate.But
Be the study found that it uses as solar water heater thermal insulation material after, expanded by heating, heat preservation are easy after absorbing amount of heat
Effect can significantly reduce, and require further improvement to adapt to the requirement of solar water heater energy conservation and environmental protection development.
Summary of the invention
In order to overcome above-mentioned technical problem, the purpose of the present invention is to provide a kind of polyurethane foams of counter infrared ray radiation
Material and its processing method, by gathering mechanical performance, hydrophobic sulfonated carbon nano-tube modification corrosion-resistant, that foam performance is excellent
Urethane and good uvioresistant, the ethylene-vinyl acetate copolymer of compatibility, sorbeth polyalcohol are mixed to get premix
Material, using nanometer tungsten oxide, graphene-supported titanium dioxide cross aerogel powder, dibutyltin maleate is mixed to form infrared absorption type
Thermal radiation resistance filler, the polyurethane foam being prepared has excellent counter infrared ray radiation, thermal and insulating performance, and in length
It will not occur significantly to shrink after the exposing to the sun and rain of phase and cracking, meet the requirement of solar water heater thermal insulation material.
The purpose of the present invention can be achieved through the following technical solutions:
The present invention provides a kind of polyurethane foamed material of counter infrared ray radiation, the raw materials including following parts by weight: sulfonic acid
40-60 parts of carbon nano tube modified polyurethane, 10-25 parts of ethylene-vinyl acetate copolymer, sorbeth polyalcohol 5-12
Part, 3-6 parts of nanometer tungsten oxide, silica aerogel powder 1-3 parts graphene-supported, 0.5-1.6 parts of dibutyitin maleate,
3-12 parts of foaming agent, 1.5-4 parts of foam stabiliser；Wherein, sorbeth polyalcohol is using sorbierite as initiator, with oxidation
Propylene polymerization obtains, hydroxyl value 300-400mgKOH/g, viscosity 8000-1000mPas；
The preparation method of the sulfonated carbon nano-tube modification polyurethane the following steps are included:
1) prepared by base polyurethane prepolymer for use as: the isophorone diisocyanate of 22g being added in autoclave, nitrogen is passed through
It is 0.6MPa to kettle pressure, stirring is warming up to 78 DEG C, the poly- methyl propanediol of 6.5g is added dropwise, is stirred to react 6h, it is pre- to obtain polyurethane
Aggressiveness；
2) prepared by sulfonic acid carbon nano tube: the 49wt% of 2.6g multi-walled carbon nanotube, 10mL being added in 100mL ball grinder
Aqueous sulfuric acid, 0.23g potassium permanganate, 30mL ethyl alcohol, after ball-milling reaction 12h, deionized water washing reaction object to neutrality, very
The dry 8h of empty drying box；
3) the sulfonic acid carbon nano tube 2g for taking step 2) to prepare is dissolved in tetrahydrofuran solvent, and it is pre- to be slowly added to polyurethane
Proper amount of acetone, 85 DEG C of reaction 2.5h is added after stirring 30min in aggressiveness 5.5g, 1,2-PD -3- sodium sulfonate 0.3g, and decompression is steamed
Distillation goes acetone to obtain sulfonated carbon nano-tube modification polyurethane.
The present invention is in the screening for carrying out polyurethane foam composition, it is contemplated that although conventional polyurethane high molecule compound
With good resistant to chemical etching, weatherability, but isocyanate group in its molecule, it is long-term heated at high temperature, it is easy burning
And fatal HCN poison gas is generated, harmfulness is big.Polyurethane is modified using sulfonic acid carbon nano tube.Wherein, multi wall carbon is received
Mitron is coaxially formed by several to dozens of single-walled carbon nanotubes, and duck eye sample defect, hydrophobicity, tensile strength are covered on tube wall
Excellent, under the action of potassium permanganate strong oxidizer, with multi-walled carbon nanotube metalepsis occurs for sulfuric acid, and sulfonic group is along duck eye
Into in the pipe axis of carbon nanotube, its hydrophobicity can be improved, more preferably with the compatibility of polyurethane.Work as isophorone diisocyanate
The performed polymer and sulfonic acid carbon nano tube that ester and poly- methyl propanediol are polymerized are in dispersing agent 1,2- propylene glycol -3- sodium sulfonate
It is friendly compatible compound under effect, play good high temperature resistant, mechanical performance, compatibility.
The present invention selects nanometer tungsten oxide, graphene negative in the thermal radiation resistance aspect of performance for improving polyurethane foamed material
Carry silica aerogel powder, the collaboration of organo-tin het stabilizer dibutyitin maleate plays effect.Wherein, tungsten oxide has
The hexahedron of smoothing regulation can resolve into little particle under infra-red radiation effect, and be oxidized to WO2.9And WO2.72, specific surface
Product constantly increases, and granularity constantly reduces, and continues enduringly to play thermal radiation resistance effect.Dibutyitin maleate meeting and polyurethane
- NCO group polarizes, to keep carbon atom positively charged in polyurethane more active, it is easier to by polyalcohol hydroxyl
The attack of base reacts, and promotion polyurethane is reacted with polyalcohol, and stability, the insulation of foamed material are improved after polymerization
Property.
As a further solution of the present invention, the preparation method of the graphene-supported silica aerogel powder includes
Following steps:
1) graphene of 3-7 parts by weight graphene modification: is impregnated into the organic zirconium crosslinker of 12-23 parts by weight
In, 12h is stirred with 300r/min revolving speed, after aged overnight, 100 DEG C of dry 50min, 580 DEG C of calcining 2h grind that obtain granularity small
In 50 μm of modified graphene；
2) prepared by mixed serum: after modified graphene is mixed with deionized water according to mass ratio 1:6-8, ultrasonic 5min is obtained
To modified graphene slurries, the silica aerogel powder of modified graphene grind slurries quality 6-10% is added, saturated carbon is added dropwise
Sour hydrogen sodium solution regulation system pH value obtains mixed slurry to 7-8,55 DEG C of insulated and stirred 30min；
3) filtration drying: obtaining a filter cake after mixed slurry is filtered under diminished pressure and first-time filtrate, first-time filtrate subtract again
Press filtration obtains secondary filter cake and secondary filtrate, after one time filter cake merges with secondary filter cake, is placed in 60 DEG C of sterile drying box
To water content less than 5%, ultramicro grinding obtains graphene-supported silica aerogel powder for drying.
Graphene-supported silica aerogel powder of the invention, since graphene has nanoscale roll surface,
There is special attraction in catalytic process, select organic zirconium crosslinker to be modified it, graphene can be made to hand over
Connection forms multiple roll surface macromolecular structure, and multiple roll surface is conducive to be supported dispersion and the dimensional homogeneity of object；Change
Property graphene and deionized water slurries are made, can be dispersed in water phase, between silica aerogel powder and graphene
Hydrogen ion or hydroxide ion swap and are fixed on interlayer, not only keep good heat resistance, mechanical performance, by
Also a large amount of heat radiation can be absorbed when high temperature heat radiation, is filtered heat-insulated, and shrinking percentage < 1% is used for a long time at 650 DEG C, is mixed into poly- ammonia
Thermal radiation resistance effect can be played after ester for a long time, it is durable.
As a further solution of the present invention, the foaming agent is by ethyl acetate, 1,1,1,3,3- pentafluoropropane, 1, and 1,1,
4,4,4- hexafluorobutene is formed according to mass ratio 5:1:1 mixed preparing.
As a further solution of the present invention, the foam stabiliser is HCFC-141b, HFC-245fa, HFC-365mfc
One of or a variety of combinations.
The present invention also provides a kind of processing methods of the polyurethane foamed material of counter infrared ray radiation, comprising the following steps:
1) prepared by premix: sulfonated carbon nano-tube modification polyurethane, ethylene-vinyl acetate copolymer, sorbierite are gathered
Ethoxylated polyhydric alcohol is added sequentially in reaction kettle, and 50-60 DEG C is warming up under nitrogen protection, and insulated and stirred 40min obtains premix；
2) filler mixes: nanometer tungsten oxide, graphene-supported silica aerogel powder are added in dispersion machine,
200r/min after mixing evenly, is warming up to 60 DEG C, is slowly added dibutyltin maleate, improves revolving speed to 400r/min, continues to stir
40min is mixed, mixed fillers are obtained；
3) 10-20s, stand foaming mixing casting: is mixed in premix, mixed fillers, foaming agent, foam stabiliser
30-50min is poured into the die cavity of mold, locks mold, solidifies 25min, die sinking.
The present invention has found in the Research on processing technology to the polyurethane foamed material first by sulfonated carbon nano-tube modification
Polyurethane, ethylene-vinyl acetate copolymer, sorbeth polyalcohol mixed under oxygen-free environment can promote polyurethane with it is polynary
The reactive polymeric of alcohol forms the process of prefoam；After a variety of heat-resistant fillers, foaming agent, foam stabiliser are mixed with premix,
Stand foaming advantageously forms small uniform stomata under room temperature and gap, heat-resistant filler are mixed in stomata and gap, low temperature
It is heating and curing and promotes each ingredient compatible with open arms, apparent expansion or shrinkage phenomenon will not occur after die sinking.
As a further solution of the present invention, temperature control applies at 50-60 DEG C, and to mold when the step 3) solidifies
The pressure of 20-40kPa.
Beneficial effects of the present invention:
1, this hair invention counter infrared ray radiation polyurethane foamed material, using sulfonated carbon nano-tube modification polyurethane with
Good uvioresistant, the ethylene-vinyl acetate copolymer of compatibility, sorbeth polyalcohol are mixed to get premix, use
Nanometer tungsten oxide, graphene-supported titanium dioxide cross aerogel powder, dibutyltin maleate is mixed to form the heat resistanceheat resistant of infrared absorption type
Filler is radiated, the polyurethane foam being prepared has excellent counter infrared ray radiation, thermal and insulating performance, and preparation method is simple,
Stable molding, it is easy to industrialized production, it will not occur significantly to shrink after long-term expose to the sun and rain and cracking, meet solar energy
The requirement of water heater thermal insulation material.
2, the present invention is modified polyurethane using sulfonic acid carbon nano tube, and sulfonic group enters carbon nanotube along duck eye
Pipe axis in, its hydrophobicity can be improved, more preferably with the compatibility of polyurethane；When isophorone diisocyanate and poly- methyl-prop
The performed polymer and sulfonic acid carbon nano tube that glycol is polymerized are friendly under the action of dispersing agent 1,2-PD -3- sodium sulfonate
It is compatible compound, play good high temperature resistant, mechanical performance, compatibility.
3, in a variety of heat-resistant fillers, tungsten oxide can resolve into little particle under infra-red radiation effect, and be oxidized to WO2.9
And WO2.72, specific surface area constantly increases, and granularity constantly reduces, and continues enduringly to play thermal radiation resistance effect；Maleic acid dibutyl
Tin can polarize with polyurethane-NCO group, to keep carbon atom positively charged in polyurethane more active, promote poly-
Urethane is reacted with polyalcohol；Silica aerogel powder and graphene in graphene-supported silica aerogel powder
Between hydrogen ion or hydroxide ion swap and be fixed on interlayer, can also be absorbed when by high temperature heat radiation a large amount of
Heat radiation filters heat-insulated, and shrinking percentage < 1% is used for a long time at 650 DEG C, durable.The phase of a variety of heat-resistant fillers and polyurethane
Capacitive is good, and collaboration plays flame-proof heat-resistant, counter infrared ray radiation effect.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical scheme in the embodiment of the invention is clearly and completely described,
Obviously, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based in the present invention
Embodiment, all other embodiment obtained by those of ordinary skill in the art without making creative efforts, all
Belong to the scope of protection of the invention.
Embodiment 1
A kind of polyurethane foamed material of counter infrared ray radiation, the raw material including following parts by weight: sulfonic acid carbon nano tube changes
Property 52 parts of polyurethane, 16 parts of ethylene-vinyl acetate copolymer, 7 parts of sorbeth polyalcohol, 4 parts of nanometer tungsten oxide, graphene
2 parts of nonloaded silica aerogel powder, 0.9 part of dibutyitin maleate, 7 parts of foaming agent, foam stabiliser HCFC-141b
2.6 part.Wherein, sorbeth polyalcohol is to polymerize to obtain with propylene oxide using sorbierite as initiator, hydroxyl value 300-
400mgKOH/g, viscosity 8000-1000mPas.Wherein foaming agent is by ethyl acetate, 1,1,1,3,3- pentafluoropropane, 1,1,
1,4,4,4- hexafluorobutene is formed according to mass ratio 5:1:1 mixed preparing.
The preparation method of the sulfonated carbon nano-tube modification polyurethane the following steps are included:
1) prepared by base polyurethane prepolymer for use as: the isophorone diisocyanate of 22g being added in autoclave, nitrogen is passed through
It is 0.6MPa to kettle pressure, stirring is warming up to 78 DEG C, the poly- methyl propanediol of 6.5g is added dropwise, is stirred to react 6h, it is pre- to obtain polyurethane
Aggressiveness；
2) prepared by sulfonic acid carbon nano tube: the 49wt% of 2.6g multi-walled carbon nanotube, 10mL being added in 100mL ball grinder
Aqueous sulfuric acid, 0.23g potassium permanganate, 30mL ethyl alcohol, after ball-milling reaction 12h, deionized water washing reaction object to neutrality, very
The dry 8h of empty drying box；
3) the sulfonic acid carbon nano tube 2g for taking step 2) to prepare is dissolved in tetrahydrofuran solvent, and it is pre- to be slowly added to polyurethane
Proper amount of acetone, 85 DEG C of reaction 2.5h is added after stirring 30min in aggressiveness 5.5g, 1,2-PD -3- sodium sulfonate 0.3g, and decompression is steamed
Distillation goes acetone to obtain sulfonated carbon nano-tube modification polyurethane.
The preparation method of the graphene-supported silica aerogel powder the following steps are included:
1) graphene of 3-7 parts by weight graphene modification: is impregnated into the organic zirconium crosslinker of 12-23 parts by weight
In, 12h is stirred with 300r/min revolving speed, after aged overnight, 100 DEG C of dry 50min, 580 DEG C of calcining 2h grind that obtain granularity small
In 50 μm of modified graphene；
2) prepared by mixed serum: after modified graphene is mixed with deionized water according to mass ratio 1:6-8, ultrasonic 5min is obtained
To modified graphene slurries, the silica aerogel powder of modified graphene grind slurries quality 6-10% is added, saturated carbon is added dropwise
Sour hydrogen sodium solution regulation system pH value obtains mixed slurry to 7-8,55 DEG C of insulated and stirred 30min；
3) filtration drying: obtaining a filter cake after mixed slurry is filtered under diminished pressure and first-time filtrate, first-time filtrate subtract again
Press filtration obtains secondary filter cake and secondary filtrate, after one time filter cake merges with secondary filter cake, is placed in 60 DEG C of sterile drying box
To water content less than 5%, ultramicro grinding obtains graphene-supported silica aerogel powder for drying.
The processing method of the polyurethane foamed material of the present embodiment counter infrared ray radiation, comprising the following steps:
1) prepared by premix: sulfonated carbon nano-tube modification polyurethane, ethylene-vinyl acetate copolymer, sorbierite are gathered
Ethoxylated polyhydric alcohol is added sequentially in reaction kettle, and 58 DEG C are warming up under nitrogen protection, and insulated and stirred 40min obtains premix；
2) filler mixes: nanometer tungsten oxide, graphene-supported silica aerogel powder are added in dispersion machine,
200r/min after mixing evenly, is warming up to 60 DEG C, is slowly added dibutyltin maleate, improves revolving speed to 400r/min, continues to stir
40min is mixed, mixed fillers are obtained；
3) 15s, stand foaming mixing casting: is mixed in premix, mixed fillers, foaming agent, foam stabiliser
46min is poured into the die cavity of mold, locks mold, solidifies 25min, die sinking.
Embodiment 2
A kind of polyurethane foamed material of counter infrared ray radiation, the raw material including following parts by weight: sulfonic acid carbon nano tube changes
Property 47 parts of polyurethane, 18 parts of ethylene-vinyl acetate copolymer, 10 parts of sorbeth polyalcohol, 4 parts of nanometer tungsten oxide, graphite
1 part of alkene nonloaded silica aerogel powder, 1.3 parts of dibutyitin maleate, 5 parts of foaming agent, foam stabiliser HFC-245fa
3.2 part.Wherein, sorbeth polyalcohol is to polymerize to obtain with propylene oxide using sorbierite as initiator, hydroxyl value 300-
400mgKOH/g, viscosity 8000-1000mPas.Wherein foaming agent is by ethyl acetate, 1,1,1,3,3- pentafluoropropane, 1,1,
1,4,4,4- hexafluorobutene is formed according to mass ratio 5:1:1 mixed preparing.
The preparation method of the sulfonated carbon nano-tube modification polyurethane is same as Example 1.
The preparation method of the graphene-supported silica aerogel powder is same as Example 1.
The processing method of the polyurethane foamed material of the present embodiment counter infrared ray radiation, comprising the following steps:
1) prepared by premix: sulfonated carbon nano-tube modification polyurethane, ethylene-vinyl acetate copolymer, sorbierite are gathered
Ethoxylated polyhydric alcohol is added sequentially in reaction kettle, and 52 DEG C are warming up under nitrogen protection, and insulated and stirred 40min obtains premix；
2) filler mixes: nanometer tungsten oxide, graphene-supported silica aerogel powder are added in dispersion machine,
200r/min after mixing evenly, is warming up to 60 DEG C, is slowly added dibutyltin maleate, improves revolving speed to 400r/min, continues to stir
40min is mixed, mixed fillers are obtained；
3) 20s, stand foaming mixing casting: is mixed in premix, mixed fillers, foaming agent, foam stabiliser
40min is poured into the die cavity of mold, locks mold, solidifies 25min, die sinking.
Embodiment 3
A kind of polyurethane foamed material of counter infrared ray radiation, the raw material including following parts by weight: sulfonic acid carbon nano tube changes
Property 58 parts of polyurethane, 23 parts of ethylene-vinyl acetate copolymer, 11 parts of sorbeth polyalcohol, 5 parts of nanometer tungsten oxide, graphite
3 parts of alkene nonloaded silica aerogel powder, 1.5 parts of dibutyitin maleate, 7 parts of foaming agent, foam stabiliser HFC-
3.6 parts of 365mfc.Wherein, sorbeth polyalcohol is to polymerize to obtain with propylene oxide, hydroxyl value using sorbierite as initiator
For 300-400mgKOH/g, viscosity 8000-1000mPas.Wherein foaming agent is by ethyl acetate, five fluorine third of 1,1,1,3,3-
Alkane, 1,1,1,4,4,4- hexafluorobutene are formed according to mass ratio 5:1:1 mixed preparing.
The preparation method of the sulfonated carbon nano-tube modification polyurethane is same as Example 1.
The preparation method of the graphene-supported silica aerogel powder is same as Example 1.
The processing method of the polyurethane foamed material of the present embodiment counter infrared ray radiation, comprising the following steps:
1) prepared by premix: sulfonated carbon nano-tube modification polyurethane, ethylene-vinyl acetate copolymer, sorbierite are gathered
Ethoxylated polyhydric alcohol is added sequentially in reaction kettle, and 60 DEG C are warming up under nitrogen protection, and insulated and stirred 40min obtains premix；
2) filler mixes: nanometer tungsten oxide, graphene-supported silica aerogel powder are added in dispersion machine,
200r/min after mixing evenly, is warming up to 60 DEG C, is slowly added dibutyltin maleate, improves revolving speed to 400r/min, continues to stir
40min is mixed, mixed fillers are obtained；
3) 20s, stand foaming mixing casting: is mixed in premix, mixed fillers, foaming agent, foam stabiliser
37min is poured into the die cavity of mold, locks mold, solidifies 25min, die sinking.
Comparative example 1
This comparative example the difference from embodiment 1 is that, sulfonated carbon nano-tube modification polyurethane replaces with isophorone two
The polyurethane that isocyanates and poly- methyl propanediol generate, processing method are constant.
Comparative example 2
This comparative example the difference from embodiment 1 is that, do not add graphene-supported silica aerogel powder, process
Method is as follows:
1) prepared by premix: sulfonated carbon nano-tube modification polyurethane, ethylene-vinyl acetate copolymer, sorbierite are gathered
Ethoxylated polyhydric alcohol is added sequentially in reaction kettle, and 58 DEG C are warming up under nitrogen protection, and insulated and stirred 40min obtains premix；
2) filler mixes: nanometer tungsten oxide is added in dispersion machine, 60 DEG C is warming up to, is slowly added dibutyltin maleate,
Revolving speed is improved to 400r/min, continues to stir 40min, obtains mixed fillers；
3) 15s, stand foaming mixing casting: is mixed in premix, mixed fillers, foaming agent, foam stabiliser
46min is poured into the die cavity of mold, locks mold, solidifies 25min, die sinking.
Comparative example 3
This comparative example the difference from embodiment 1 is that, do not add nanometer tungsten oxide, processing method is as follows:
1) prepared by premix: sulfonated carbon nano-tube modification polyurethane, ethylene-vinyl acetate copolymer, sorbierite are gathered
Ethoxylated polyhydric alcohol is added sequentially in reaction kettle, and 58 DEG C are warming up under nitrogen protection, and insulated and stirred 40min obtains premix；
2) filler mixes: graphene-supported silica aerogel powder being added in dispersion machine, is warming up to 60 DEG C, slowly
Dibutyltin maleate is added, revolving speed is improved to 400r/min, continues to stir 40min, obtain mixed fillers；
3) 15s, stand foaming mixing casting: is mixed in premix, mixed fillers, foaming agent, foam stabiliser
46min is poured into the die cavity of mold, locks mold, solidifies 25min, die sinking.
Comparative example 4
The polyurethane foam that in the patent of reference application number 201711215394.2 prepared by embodiment 3.
Performance test
Referring to professional standard GB/T 26709-2011 " solar water heater rigid polyurethane foam ", to implementation
Polyurethane foam class material prepared by example, comparative example processing has carried out thermal coefficient, compressive strength, dimensional stability, water absorption rate
It measures.Counter infrared ray radiance selects operating temperature to be irradiated for 350 DEG C of LED light to polyurethane foam, and test is shone
Thermal coefficient after penetrating for 24 hours.Specific test result is shown in Table 1.
The test of 1. polyurethane foam performance of table
As can be seen from the above table, the compressive strength of the polyurethane foam of embodiment preparation, dimensional stability are better than comparative example,
Thermal coefficient is lower after manufacture 7d, 28d and variation is little, illustrates that heat preservation and insulation is excellent；It is thermally conductive after the irradiation of light source high temperature
Coefficient is lower and elevation amplitude is little, illustrates that its thermal radiation resistance is had excellent performance.Comparative example 1 does not use sulfonic acid carbon nano tube pair
Polyurethane is modified so that polyurethane can not with sorbeth polyol reaction and play good high temperature resistant, mechanicalness
Energy, compatibility, cause thermal and insulating performance, compressive strength, counter infrared ray radiance to substantially reduce.Comparative example 2 lacks graphene
Nonloaded silica aerogel powder, can not play absorbed when by high temperature heat radiation a large amount of heat radiation, filter it is heat-insulated
Effect, while bad stability, easy swelling cracking after being heated.Comparative example 3 lacks tungsten oxide, can not play persistently durable heat resistanceheat resistant
Radiation effects, heat preservation and insulation, thermal radiation resistance performance have certain reduction.
In the description of this specification, the description of reference term " one embodiment ", " example ", " specific example " etc. means
Particular features, structures, materials, or characteristics described in conjunction with this embodiment or example are contained at least one implementation of the invention
In example or example.In the present specification, schematic expression of the above terms may not refer to the same embodiment or example.
Moreover, particular features, structures, materials, or characteristics described can be in any one or more of the embodiments or examples to close
Suitable mode combines.
Above content is only citing made for the present invention and explanation, affiliated those skilled in the art are to being retouched
The specific embodiment stated does various modifications or additions or is substituted in a similar manner, and without departing from invention or surpasses
More range defined in the claims, is within the scope of protection of the invention.
Claims (6)
1. a kind of polyurethane foamed material of counter infrared ray radiation, which is characterized in that the raw material including following parts by weight: sulfonated carbon
40-60 parts of nanotube modified polyurethane, 5-12 parts of sorbeth polyalcohol, is received 10-25 parts of ethylene-vinyl acetate copolymer
3-6 parts of tungsten oxide of rice, silica aerogel powder 1-3 parts graphene-supported, 0.5-1.6 parts of dibutyitin maleate, foaming
3-12 parts of agent, 1.5-4 parts of foam stabiliser；Wherein, sorbeth polyalcohol is using sorbierite as initiator, with propylene oxide
Polymerization obtains, hydroxyl value 300-400mgKOH/g, viscosity 8000-1000mPas；
The preparation method of the sulfonated carbon nano-tube modification polyurethane the following steps are included:
1) prepared by base polyurethane prepolymer for use as: the isophorone diisocyanate of 22g being added in autoclave, is passed through nitrogen to kettle
Pressure is 0.6MPa, and stirring is warming up to 78 DEG C, the poly- methyl propanediol of 6.5g is added dropwise, is stirred to react 6h, obtains base polyurethane prepolymer for use as；
2) sulfonic acid carbon nano tube prepare: in 100mL ball grinder be added 2.6g multi-walled carbon nanotube, 10mL 49wt% sulphur
Aqueous acid, 0.23g potassium permanganate, 30mL ethyl alcohol, after ball-milling reaction 12h, deionized water washing reaction object to neutrality, vacuum is dry
The dry 8h of dry case；
3) the sulfonic acid carbon nano tube 2g for taking step 2) to prepare is dissolved in tetrahydrofuran solvent, is slowly added to base polyurethane prepolymer for use as
Proper amount of acetone, 85 DEG C of reaction 2.5h is added after stirring 30min in 5.5g, 1,2-PD -3- sodium sulfonate 0.3g, and vacuum distillation removes
Acetone is gone to obtain sulfonated carbon nano-tube modification polyurethane.
2. the polyurethane foamed material of counter infrared ray radiation according to claim 1, which is characterized in that described graphene-supported
The preparation method of silica aerogel powder the following steps are included:
1) graphene modification: the graphene of 3-7 parts by weight being impregnated into the organic zirconium crosslinker of 12-23 parts by weight, with
300r/min revolving speed stirs 12h, and after aged overnight, 100 DEG C of dry 50min, 580 DEG C of calcining 2h grind and obtain granularity less than 50 μ
The modified graphene of m；
2) prepared by mixed serum: after modified graphene is mixed with deionized water according to mass ratio 1:6-8, ultrasonic 5min is changed
Property graphene slurries, be added modified graphene grind slurries quality 6-10% silica aerogel powder, be added dropwise unsaturated carbonate hydrogen
Sodium solution regulation system pH value obtains mixed slurry to 7-8,55 DEG C of insulated and stirred 30min；
3) filtration drying: obtaining a filter cake after mixed slurry is filtered under diminished pressure and first-time filtrate, first-time filtrate depressurized again
Filter obtains secondary filter cake and secondary filtrate, after one time filter cake merges with secondary filter cake, is placed in 60 DEG C of sterile drying box and dries
To water content less than 5%, ultramicro grinding obtains graphene-supported silica aerogel powder.
3. the polyurethane foamed material of counter infrared ray radiation according to claim 1, which is characterized in that the foaming agent is by second
Acetoacetic ester, 1,1,1,3,3- pentafluoropropane, 1,1,1,4,4,4- hexafluorobutene are formed according to mass ratio 5:1:1 mixed preparing.
4. the polyurethane foamed material of counter infrared ray radiation according to claim 1, which is characterized in that the foam stabiliser
For one of HCFC-141b, HFC-245fa, HFC-365mfc or a variety of combinations.
5. a kind of processing method of the polyurethane foamed material of counter infrared ray radiation, which comprises the following steps:
1) prepared by premix: sulfonated carbon nano-tube modification polyurethane, ethylene-vinyl acetate copolymer, sorbeth is more
First alcohol is added sequentially in reaction kettle, and 50-60 DEG C is warming up under nitrogen protection, and insulated and stirred 40min obtains premix；
2) filler mixes: nanometer tungsten oxide, graphene-supported silica aerogel powder being added in dispersion machine, 200r/min
After mixing evenly, 60 DEG C are warming up to, dibutyltin maleate is slowly added, raising revolving speed to 400r/min continues to stir 40min,
Obtain mixed fillers；
3) 10-20s, stand foaming 30- mixing casting: is mixed in premix, mixed fillers, foaming agent, foam stabiliser
50min is poured into the die cavity of mold, locks mold, solidifies 25min, die sinking.
6. the processing method of the polyurethane foamed material of counter infrared ray radiation according to claim 5, which is characterized in that described
Temperature control is at 50-60 DEG C when step 3) solidifies, and applies the pressure of 20-40kPa to mold.
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| 倪敏轩: "可快速固化聚氨酯基辐射屏蔽复合材料及其关键应用组件研发", 《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110634591A (en) * | 2019-09-29 | 2019-12-31 | 新奥石墨烯技术有限公司 | Conductive paste, preparation method and application thereof, and battery |
| CN110634591B (en) * | 2019-09-29 | 2021-04-16 | 新奥石墨烯技术有限公司 | Conductive paste, preparation method and application thereof, and battery |
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