CN109971066A - Infrared barrier fluoro-containing composition, preparation method and applications - Google Patents
Infrared barrier fluoro-containing composition, preparation method and applications Download PDFInfo
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Abstract
The invention discloses a kind of infrared barrier fluoro-containing compositions, preparation method and applications.The present invention not only has performance ageing-resistant, corrosion-resistant, resistant to high temperature, and also there is barrier infrared ray to generate the effect of heat preservation through visible light.
Description
Technical field
The invention belongs to field of material technology more particularly to infrared barrier fluoro-containing compositions, preparation method and applications.
Background technique
Fluorine material is because it is with the property such as excellent physical mechanical, electric property, resistant to chemical etching, low friction, high temperature resistant
Can, it is widely used in industrial circle.Wherein, fluorine material may include polytetrafluoroethylene (PTFE) (PTFE), ethylene tetrafluoroethylene copolymer
(ETFE), perfluoroethylene-propylene (FEP), Kynoar (PVDF) etc..Usually above-mentioned fluorine material is passed through modified or compound answer
In building, cable, tubing or corrosion-resistant field.
Although fluorine material has above-mentioned excellent properties, energy-efficient effect is weaker.For example, the Archtectural Coatings containing ETFE
The effect of heat preservation energy-saving can not be realized through the infrared ray and ultraviolet light in sunlight.
Thus it is necessary to combine fluorine material ETFE comprehensive performance advantage and other materials composition and processing technology, one is realized
Kind has the energy-efficient fluorine material of infrared barrier.
Summary of the invention
In view of the problems of the above-mentioned prior art, the purpose of the present invention is a kind of infrared barrier fluoro-containing compositions, preparation
Method and its application.The present invention not only has a performance ageing-resistant, corrosion-resistant, resistant to high temperature, also has barrier infrared ray, through can
It is light-exposed, have the function of heat preservation.
The purpose of the invention will be achieved through the following technical solutions:
Infrared barrier fluoro-containing composition, including ethylene tetrafluoroethylene copolymer, metal oxide, dispersible carrier, dispersing agent.
It preferably, further include crystallization nucleating agent, and/or fluorine ion inhibitor.
Preferably, according to weight part ratio meter, ethylene tetrafluoroethylene copolymer: metal oxide: dispersible carrier: dispersing agent
Ratio is 100:0.1-2:3-10:0.1-0.5.
Preferably, according to weight part ratio meter, ethylene tetrafluoroethylene copolymer: crystallization nucleating agent: the ratio of fluorine ion inhibitor
Value is 100:0.2-1:0.2-1.
Preferably, the content of the tetrafluoroethene in the ethylene tetrafluoroethylene copolymer is 50-60%.
Preferably, the metal oxide includes rice tin-antiomony oxide, nano indium tin oxide, nanometer caesium tungsten bronze powder, receives
One of rice multi-element doping tin oxide, zinc tin oxide or any combination thereof.
Preferably, the dispersible carrier includes ketone and/or esters.
Preferably, the ketone includes butanone, methylisobutylketone, and/or diisobutyl ketone；The esters include acrylic acid
Ethyl ester.
It preferably, further include ethyl alcohol.
Preferably, the dispersing agent includes that triethyl group hexyl phosphoric acid, lauryl sodium sulfate, methyl anyl alcohol, cellulose spread out
One of biology, polyacrylamide, silanes, titanate ester, and/or fatty acid polyethylene glycol ester or any combination thereof.
Preferably, the free radical scavenger includes 2,6- di-tert-butyl-4-methy phenol, bis- (3,5 di-t-butyl -4-
Hydroxy phenyl) thioether, four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol esters, 1,4-benzoquinone, durol
One of quinone, phenyl-N- tert-butylnitrone, and/or benzofuranone or any combination thereof.
Preferably, the crystallization nucleating agent includes talcum powder, silica, alum, titanium dioxide, mica, aliphatic carboxylic acid
One of metallic compound, sorbierite benzal derivative, and/or aromatic carboxylic acid metal's compound or any combination thereof.
Preferably, the fluorine ion inhibitor include magnesia, calcium hydroxide, calcium oxide, zinc oxide, calcium carbonate, and/or
One of antimony oxide or any combination thereof.
A kind of preparation method preparing above-mentioned composition, includes the following steps:
S1: metal oxide and dispersing agent, dispersible carrier shearing are dispersed, and form the metal that solid content reaches 30~50%
Oxide slurry；
S2: ethylene tetrafluoroethylene copolymer is dry, it is kneaded with the metal oxide paste prepared in step S1, and extract out
Dispersible carrier obtains mixture 1；
S3: mixture 1 made from step S2 is plasticized, and obtains mixture 2；
S4: by S3 be made mixture 2 squeeze out pelletizing, it is dry to get.
Preferably, the drying temperature in the step S2 is 95-105 DEG C, time 4-6h.
Preferably, it is twin-screw or single screw rod, plasticization temperature 270- that the plasticizing mode of mixture 1, which is made, in the step S2
320℃。
A kind of application according to above-mentioned infrared barrier fluoro-containing composition in film heat-insulating material.
Compared with prior art, a kind of infrared barrier fluoro-containing composition provided by the invention, preparation method and applications, reach
To have the technical effect that 1) present invention using ETFE as basis material, using the nano-metal-oxide with infrared barrier effect
As function powder, barrier infrared ray 90% is realized, while through the effect of visible light 70%；2) simultaneously because ETFE is with resistance to
Ultraviolet, intensity reaches 45MPa or more, antipollution, heatproof height (can use under 150 degree for a long time), to ensure that of the invention
High-intensitive, weatherability performance；3) nano-metal-oxide with infrared barrier passes through grinding distribution in oiliness carrier, double
Screw low-temperature high shear position realizes that low temperature high shear mixing is uniform by high-precision high voltage feeding equipment, and in Handpiece Location
It realizes two sections of suction filtrations, the oiliness carrier of nanometer infrared barrier powder is extracted out, to be formed a kind of finely dispersed fluorine-containing infrared
Barrier material.4) since fluorine material can release hydrogen fluoride in process, and hydrogen fluoride can be with nanometer infrared barrier material
It reacts and declines infrared barrier effect, it is therefore desirable to the hydrogen fluoride generated in production is controlled by fluorine ion inhibitor, from
And make infrared barrier effect promoting.5) make fluorine material rapid crystallization that crystalline size be made to become smaller by crystallization nucleating agent, increase
The light transmittance of material.
Below just in conjunction with the embodiments, the embodiment of the present invention is described in further detail, so that technical solution is more
It should be readily appreciated that, grasp.
Specific embodiment
The present invention will be described below by way of specific embodiments, but the present invention is not limited thereto.In following embodiments
The experimental method is unless otherwise specified conventional method；The reagent and material unless otherwise specified can be from business
Approach obtains, the scope of the patents that following example is not intended to limit the invention, all equivalence enforcements without departing from carried out by the present invention
Or change, it is intended to be limited solely by the scope of this patent.
The related description of infrared barrier fluoro-containing composition
Infrared barrier fluoro-containing composition may include ethylene tetrafluoroethylene copolymer, metal oxide, dispersible carrier, dispersion
Agent and free radical scavenger.
In some embodiments, infrared barrier fluoro-containing composition may include: according to weight part ratio meter ethylene tetrafluoroethylene
Copolymer: metal oxide: dispersible carrier: the ratio of dispersing agent is the composition of 100:0.1-2:3-10:0.1-0.5.Wherein,
The content of tetrafluoroethene in ethylene tetrafluoroethylene copolymer can be any percentage in 50-60%.Metal oxide can
With include but is not limited to nano antimony tin oxide, nano indium tin oxide, nanometer caesium tungsten bronze powder, nanometer multi-element doping tin oxide,
Or one of zinc tin oxide etc. or any combination thereof.Dispersible carrier may include ketone and/or esters.Ketone may include but
It is not limited to one of butanone, methylisobutylketone or diisobutyl ketone etc. or its any one combination.Esters may include but not
It is limited to ethyl acrylate.In some embodiments, dispersible carrier can also include ethyl alcohol.Dispersing agent can include but is not limited to three
Ethylhexyl phosphoric acid, lauryl sodium sulfate, methyl anyl alcohol, cellulose derivative, polyacrylamide, silanes, titanate ester,
Or one of fatty acid polyethylene glycol ester etc. or any combination thereof.
In some embodiments, infrared barrier fluoro-containing composition can also include but is not limited to crystallization nucleating agent or fluorine from
One of sub- inhibitor or any combination thereof.In some embodiments, infrared barrier fluoro-containing composition may include: according to weight
Part is measured than meter, ethylene tetrafluoroethylene copolymer: metal oxide: dispersible carrier: dispersing agent: crystallization nucleating agent: fluorine ion inhibits
The composition of the ratio 100:0.1-2:3-10:0.1-0.5:0.2-1:0.2-1 of agent.Wherein, crystallization nucleating agent may include but
Be not limited to talcum powder, silica, alum, titanium dioxide, mica, aliphatic carboxylic acid metal compound, sorbierite benzal derivative,
Or one of aromatic carboxylic acid metal's compound or any combination thereof.Fluorine ion inhibitor can include but is not limited to aoxidize
One of magnesium, calcium hydroxide, calcium oxide, zinc oxide, calcium carbonate or antimony oxide or any combination thereof.
Infrared barrier fluoro-containing composition
Infrared barrier fluoro-containing composition may include the ratio of each component shown in embodiment 1- embodiment 25.
For example, infrared barrier fluoro-containing composition may include 100 parts of ETFE, 0.5 part of metal oxide, dispersible carrier 3
Part, 0.3 part of dispersing agent, 0.2 part of crystallization nucleating agent, 0.2 part of fluorine ion inhibitor.Wherein, about ETFE, metal oxide, point
Dissipate carrier, dispersing agent, crystallization nucleating agent, fluorine ion inhibitor detail can be said with reference to infrared barrier fluoro-containing composition
Bright, details are not described herein.
The preparation method of infrared barrier fluoro-containing composition
Temperature when due to fluorine material processing is very high, there is corrosivity, process to release fluoride, wherein fluorine
Compound will lead to barrier property decline with the reactive metal oxide with the effect of nanometer infrared barrier, and the present invention is based on above-mentioned skills
Art difficult point need to research and develop a kind of reasonable material composition and technique, can just produce the material with infrared barrier function.
By taking embodiment 1 as an example, the preparation method of infrared barrier fluoro-containing composition is illustrated, step specifically includes:
S1: high speed is carried out in high speed grinding equipment with 0.3 part of dispersing agent, 3 parts of dispersible carrier by 0.5 part of metal oxide
Shearing dispersion forms the nanometer barrier powdery pulp that solid content reaches 30~50%；
S2: by 100 parts of ETFE, being placed at 100 DEG C dry 4-6h, then with the slurry for preparing in S1 in high-speed mixer
In be kneaded, and dispersible carrier is extracted out by Suction filtration device；
S3: mixture made from S2 is plasticized in twin-screw or single screw rod, and plasticization temperature is 270-320 DEG C, in equipment
0.2 part of crystallization nucleating agent, 0.2 part of fluorine ion inhibitor is added in different spouts；
S4: by S3 be made mixture squeeze out pelletizing, dry packing to get.
The preparation method of each composition shown in embodiment 2- embodiment 25, comparative example 1-2 and the preparation method of embodiment 1
Similar, details are not described herein.
It is specifically described the effect or principle of above-mentioned each component in the composition below:
1) there is metal oxide in barrier sunlight 90% wavelength to be the infrared ray of 800~2500nm, and can penetrate
The powder of the function of 70% visible light can be stably dispersed in fluorine material, the metal oxide by decentralized processing
Powder size can be controlled in 50~100nm, realizes that light transmission barriers function is more efficient.
There are a large amount of free radical particles on nano-metal-oxide surface with infrared barrier, these free radical particles can be with
Localized plasmon resonance occurs for infrared light, infrared energy is absorbed, to play infrared barrier function.Further, have infrared
The nano-metal-oxide of barrier reaches nanoscale can realization transparency less than transparent optical wavelength, it is therefore desirable to which dispersion is ground
Wear into nano-scale, it is seen that optical wavelength is in 380~780nm, the nanometer metal oxide powder size Control with infrared barrier
Technique and effect can be combined in 50~100nm.And with infrared barrier nanometer metal oxide powder need by
Dispersion can realize and forms uniform material with the homogeneous blend of ETFE, without dispersion nano material can occur to reunite to
So that particle size is significantly larger than infrared wavelength, translucency can not achieve.If cannot reach nano-scale can not realize it is red
Outer barriers function, it is to be understood that dispersing agent plays the role of dispersing nano-powder, and dispersible carrier is to allow handle by dispersing agent
Nano-powder be dispersed in and form stable solution in dispersible carrier, be easy to use；
2) fluorine ion inhibitor is used as using alkali metal oxide magnesia, calcium hydroxide, zinc oxide, antimony oxide etc.
It is reacted with the fluorine ion for cracking generation in ethylene tetrafluoroethylene copolymer, forms stable fluorine compounds, to inhibit fluorine
The evolution of ion, avoid fluorine ion with reacting for nanometer barrier powder and caused by nano-powder function forfeiture；
3) nucleus needed for crystallization nucleating agent provides accelerates polymer crystallization speed, refines grain structure, and light is inhibited to dissipate
It penetrates, improves the transparency and lustrous surface, be conducive to the rigidity for improving product, keep the dimensional stability of final products；
4) during adding, high-temperature vacuum devolatilization processing is carried out to basis material ETFE first, removes small molecule therein
Then component be blended forming formula materials with other components.
Test example infrared barrier fluoro-containing composition performance test
Method:
1, infrared barrier fluoro-containing composition is pressed on high temperature tablet press machine the thin slice of 1mm thickness；
2, the thin slice being pressed into is tested.
Test performance of the invention may include density, intensity, infrared ray rejection rate, visible light transmittance, heat-insulated total property
One of can etc. or any combination thereof.Wherein, the density can be according to GB/T 1033.1-2008 " the non-foam plastics of plastics
The measurement of density " in part 1: infusion process, liquid specific gravity bottle method and titration are measured and obtain；The intensity can be in material
It is tested after material tabletting, is measured and is obtained based on GJB 773A-2000；The infrared ray rejection rate can be according to GB/T
36403-2018 " glasses for infrared use infrared transmittivity test method " fourier transform method is measured and obtains；The visible light
Transmitance % can be obtained using conventional ultraviolet specrophotometer test；The heat-insulated overall performance=infrared ray rejection rate+can
Light-exposed transmitance.
For the infrared barrier fluoro-containing composition prepared by the embodiment 1-25, results of property such as table 2, table 4, table 6.
Thin slice is now pressed into as test in high temperature press using infrared barrier fluoro-containing composition prepared by embodiment 1-25
Object, contrast sample are the white glass of same thickness.In a closed case, top is equipped with 50W infrared lamp, and lower section is equipped with temperature
Sensor is spent, middle can be inserted into test object, be thermally shielded test.
The results show that the cabinet heating for being equally provided with white glass at 1 hour reaches 10 degree or more, and use of the invention
Infrared barrier fluoro-containing composition thin slice, heating are only 2 degree or so, and heat insulation is significant.
The ratio of the infrared barrier fluoro-containing composition of 1 comparative example of table and embodiment
2 comparative example of table is compared with the infrared barrier fluoro-containing composition performance of embodiment
Based on table 1, shown in table 2:
1) by the result of comparative example 1 and the heat-insulated overall performance of embodiment 1-13 it is found that heat-insulated total containing metal oxide
Performance is higher than the heat-insulated overall performance for containing only ETFE；
2) by the result of the heat-insulated overall performance of embodiment 1-9 it is found that ETFE: nanometer caesium tungsten bronze powder: dispersible carrier: dispersion
When the ratio of agent is embodiment 1, the heat-insulated overall performance of infrared barrier fluoro-containing composition is best；
3) by the result of embodiment 1 and the heat-insulated overall performance of embodiment 10-13 it is found that being nanometer caesium containing metal oxide
The heat-insulated overall performance of the infrared barrier fluoro-containing composition of tungsten bronze powder is best；
4) by comparative example 2, the result of embodiment 14-17 it is found that the ratio visible light transmittance containing dispersing agent is higher than not
Infrared barrier fluoro-containing composition containing dispersing agent；
Ratio of 3 crystallization nucleating agent of table in infrared barrier fluoro-containing composition
The performance of infrared barrier fluoro-containing composition of the table 4 containing crystallization nucleating agent
| Density g/cm3 | Intensity MPa | Infrared ray rejection rate % | Visible light transmittance % | Heat-insulated overall performance | |
| Embodiment 18 | 1.75 | 43 | 88 | 75 | 163 |
| Embodiment 19 | 1.75 | 43 | 90 | 72 | 162 |
| Embodiment 20 | 1.75 | 42 | 85 | 73 | 158 |
| Embodiment 21 | 1.75 | 41 | 88 | 71 | 159 |
By table 1- table 4 it is found that 1) embodiment 1 is compared with embodiment 18-21 it is found that the infrared barrier containing crystallization nucleating agent
The visible light transmittance of fluoro-containing composition is higher than the visible light transmittance without containing crystallization nucleating agent；
2) embodiment 18-21 compares it is found that ratio is the visible light-transmissive of the infrared barrier fluoro-containing composition of embodiment 18
Rate is best.
Ratio of the 5 fluorine ion inhibitor of table in infrared barrier fluoro-containing composition
The performance of infrared barrier fluoro-containing composition of the table 6 containing fluorine ion inhibitor
| Density g/cm3 | Intensity MPa | Infrared ray rejection rate % | Visible light transmittance % | Heat-insulated overall performance | |
| Embodiment 22 | 1.75 | 45 | 95 | 78 | 173 |
| Embodiment 23 | 1.75 | 46 | 92 | 75 | 167 |
| Embodiment 24 | 1.75 | 44 | 96 | 72 | 168 |
| Embodiment 25 | 1.75 | 50 | 96 | 73 | 169 |
By table 1,2 and table 5,6 it is found that 1) embodiment 1 is compared with embodiment 22-25 it is found that containing fluorine ion inhibitor
The heat-proof quality of infrared barrier fluoro-containing composition is higher than the nano-powder function without containing fluorine ion inhibitor；
2) embodiment 22-25 compare it is found that ratio be embodiment 22 infrared barrier fluoro-containing composition heat-proof quality most
It is good.
Several preferred embodiments of the invention have shown and described in above description, but as previously described, it should be understood that the present invention
Be not limited to forms disclosed herein, should not be regarded as an exclusion of other examples, and can be used for various other combinations,
Modification and environment, and the above teachings or related fields of technology or knowledge can be passed through within that scope of the inventive concept describe herein
It is modified.And changes and modifications made by those skilled in the art do not depart from the spirit and scope of the present invention, then it all should be in this hair
In the protection scope of bright appended claims.
Claims (16)
1. infrared barrier fluoro-containing composition, which is characterized in that carried including ethylene tetrafluoroethylene copolymer, metal oxide, dispersion
Body, dispersing agent.
2. composition according to claim 1, which is characterized in that further include that crystallization nucleating agent, and/or fluorine ion inhibit
Agent.
3. composition according to claim 1, which is characterized in that according to weight part ratio meter, ethylene tetrafluoroethylene copolymer:
Metal oxide: dispersible carrier: the ratio of dispersing agent is 100:0.1-2:3-10:0.1-0.5.
4. composition according to claim 2, which is characterized in that according to weight part ratio meter, ethylene tetrafluoroethylene copolymer:
Crystallization nucleating agent: the ratio of fluorine ion inhibitor is 100:0.2-1:0.2-1.
5. composition according to claim 1, which is characterized in that the tetrafluoroethene in the ethylene tetrafluoroethylene copolymer
Content be 50-60%.
6. composition according to claim 1, which is characterized in that the metal oxide includes nano antimony tin oxide, receives
One of rice indium tin oxide, nanometer caesium tungsten bronze powder, nanometer multi-element doping tin oxide, zinc tin oxide or any combination thereof.
7. composition according to claim 1, which is characterized in that the dispersible carrier includes ketone and/or esters.
8. composition according to claim 7, which is characterized in that the ketone include butanone, methylisobutylketone, and/or
Diisobutyl ketone；The esters include ethyl acrylate.
9. composition according to claim 7, which is characterized in that further include ethyl alcohol.
10. composition according to claim 1, which is characterized in that the dispersing agent includes triethyl group hexyl phosphoric acid, 12
Sodium alkyl sulfate, methyl anyl alcohol, cellulose derivative, polyacrylamide, silanes, titanate ester, and/or fatty acid polyglycol second two
One of alcohol ester or any combination thereof.
11. composition according to claim 2, which is characterized in that the crystallization nucleating agent includes talcum powder, titanium dioxide
Silicon, alum, titanium dioxide, mica, aliphatic carboxylic acid metal compound, sorbierite benzal derivative, and/or aromatic carboxylic acid metal
One of compound or any combination thereof.
12. composition according to claim 2, which is characterized in that the fluorine ion inhibitor includes magnesia, hydroxide
One of calcium, calcium oxide, zinc oxide, calcium carbonate, and/or antimony oxide or any combination thereof.
13. a kind of preparation method for preparing the composition as described in claim 1-12 any one, which is characterized in that including such as
Lower step:
S1: metal oxide and dispersing agent, dispersible carrier shearing are dispersed, and form the metal oxidation that solid content reaches 30~50%
Object slurry；
S2: ethylene tetrafluoroethylene copolymer is dry, it is kneaded with the metal oxide paste prepared in step S1, and extract dispersion out
Carrier obtains mixture 1；
S3: mixture 1 made from step S2 is plasticized, and obtains mixture 2；
S4: by S3 be made mixture 2 squeeze out pelletizing, it is dry to get.
14. preparation method according to claim 13, which is characterized in that the drying temperature in the step S2 is 95-105
DEG C, time 4-6h.
15. preparation method according to claim 13, which is characterized in that the plasticizing side of mixture 1 is made in the step S2
Formula is twin-screw or single screw rod, and plasticization temperature is 270-320 DEG C.
16. a kind of application of the infrared barrier fluoro-containing composition in film heat-insulating material described in -12 according to claim 1.
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| CN110373123A (en) * | 2019-07-30 | 2019-10-25 | 信义节能玻璃（芜湖）有限公司 | PVB glue film and preparation method thereof and laminated safety glass |
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Application publication date: 20190705 |