CN104927688B - The compound preparation method for turning light packaging adhesive film material of EVA/ vulcanized lead quantum dots - Google Patents
The compound preparation method for turning light packaging adhesive film material of EVA/ vulcanized lead quantum dots Download PDFInfo
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- CN104927688B CN104927688B CN201510300308.2A CN201510300308A CN104927688B CN 104927688 B CN104927688 B CN 104927688B CN 201510300308 A CN201510300308 A CN 201510300308A CN 104927688 B CN104927688 B CN 104927688B
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
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Abstract
The invention discloses a kind of compound preparation methods for turning light packaging adhesive film material of EVA/ vulcanized lead quantum dot；The material is combined by vulcanized lead quantum dot and EVA packaging adhesive films；The vulcanized lead quantum dot is the PbS nanoparticle that scale is 1~20nm；First vulcanized lead quantum dot under ultrasound condition is surface-treated, then with EVA, crosslinking agent, UV light stabilizing agent, antioxidant, plasticizer etc. melt again compound, preparation has the function of the EVA/ vulcanized lead quantum dot composite package adhesive film materials for turning light.Emit visible ray since the material can absorb ultraviolet light, utilization of the solar cell module to ultraviolet light can be improved, so as to be expected to improve efficiency, meanwhile, there is the longer service life than rare-earth light-converting material.
Description
Technical field
The invention belongs to solar cell field of optical functional material, and in particular to a kind of compound turn of EVA/ vulcanized lead quantum dot
The preparation method of light packaging adhesive film material.
Background technology
Solar energy is a kind of inexhaustible, nexhaustible green regenerative energy sources, and pollution is not generated yet to environment, because
This, in the case that in fossil energy sources, increasingly exhausted and environmental pollution is on the rise, is gradually favored be subject to people.The profit of solar energy
The forms such as utilize with mainly having photo-thermal, Photochemical convertion and photovoltaic generation.Wherein photovoltaic generation is turned luminous energy by opto-electronic conversion
Electric energy is changed to, energy transmission facilitates, and irreplaceable excellent all with other two ways in storage and versatility etc.
Gesture.With the development of photovoltaic power generation technology, photoelectric conversion efficiency of the solar battery is continuously improved, production cost constantly declines, and indicates
Solar energy power generating will play an important role in human society future development.
At present, solar battery sheet due to material intensity itself it is relatively low, in actual use, it is impossible to be directly exposed to
, it is necessary to carry out protectiveness encapsulation to it in air, solar cell module is prepared into.General encapsulating material is largely determined
Determine performance and the service life of solar cell module, therefore the requirement to packaging adhesive film is very stringent, at present, mainly using light transmittance
Solar battery sheet is packaged by the packaging adhesive film high, adhesive property is good, ageing-resistant performance is excellent.
Since ethylene-vinyl acetate copolymer (EVA) has, high transparency, high resiliency, melting temperature be low, fluidity of molten
The features such as good and bond vitrified, and it is cheap, and nearly 80% commercialized solar cell is used as encapsulation using EVA
Material.The energy for being only limitted to some visible light that the silica-based solar cell of the EVA encapsulation of commercialization can generally utilize, it is most of
Ultraviolet light be not all fully utilized.Therefore, preferably to improve battery efficiency using solar energy, will have the function of to turn the dilute of light
Native organic coordination compound with EVA is compound has some research work (such as to improve battery efficiency：Chinese patent CN104152065A；
CN103709946A；CN103254495A etc.), and also obtained that there is the EVA encapsulating films for turning light, but since rare earth has
The short life of machine complex limits its application.
The content of the invention
It is compound to provide a kind of new EVA/ vulcanized lead quantum dots for the deficiency that it is an object of the invention to be directed in the prior art
Turn the preparation method of light packaging adhesive film material；The present invention's is simple for process, easy to produce, and manufactured composite material has fluorescence spy
Property, the new functions of EVA are imparted, and are effectively improved utilization of the solar cell to ultraviolet light.
For purpose as realization, the present invention is proposed to add in the vulcanized lead quantum dot of surface treatment in EVA, added in simultaneously
Crosslinking agent, UV light stabilizing agent, antioxidant and plasticizer, its melting mixing is uniform, and being made has the function of the EVA/ sulphur for turning light
Change lead quantum dot composite package adhesive film material.
The purpose of the present invention is what is be achieved through the following technical solutions：
The present invention relates to a kind of compound preparation method for turning light packaging adhesive film material of EVA/ vulcanized lead quantum dot, including as follows
Step：
It is prepared by the vulcanized lead quantum dot of surface treatment：In a solvent, addition vulcanized lead quantum dot and coupling agent, ultrasound 10~
180 minutes, the vulcanized lead quantum dot suspending liquid A being surface-treated；
It is prepared by EVA/ vulcanized lead quantum dot composite packages adhesive film material：In parts by weight, by 100 parts of ethyl vinyl acetate second
Enoate copolymer, 0.2~5 part of crosslinking agent, 0.3~5 part of UV light stabilizing agent, 0.1~3 part of antioxidant, 0.1~15 part of plasticising
Agent and 1~20 part of vulcanized lead quantum dot suspending liquid A, be uniformly mixed, under the conditions of 80~130 DEG C melt it is compound, i.e.,
Obtain the EVA/ vulcanized lead quantum dot composite package adhesive film material.
As optimal technical scheme, the vulcanized lead quantum dot is nano-particle vulcanized lead of the diameter in 1~20nm.Due to
Inorganic matter wants transparent and is necessarily less than 1/10th of light wave in the polymer, i.e., less than 40nm, but after vulcanized lead is more than 20nm
There is no fluorescence that cannot reach requirement, and less than 1nm, then there are three aspects：One is difficult to synthesize, second is that after synthesis very
Easily reunite, three be less than the light sent after 1nm be not the present invention it is required；In addition, vulcanized lead lateral size of dots is that statistics is flat
As a result, the diameter of current vulcanized lead quantum dot is not homogeneous, the present invention vulcanizes using 1~20nm nano-particles
Lead.
As optimal technical scheme, the mass ratio of the vulcanized lead quantum dot and coupling agent is 100: (1~10)；The idol
Join the mixture that agent is selected from one or more of silane coupling agent, titanate coupling agent, aluminate coupling agent.Coupling agent should
Play the role of connecting vulcanized lead quantum dot and polymer, it is few at low cost, but do not work very little, too many price, simultaneously
The particle of vulcanized lead can also increased, influences transparency, therefore the mass ratio of preferred vulcanized lead quantum dot and coupling agent in the present invention
For 100: (1~10).
As optimal technical scheme, the solvent is selected from ethyl alcohol, acetone, hexane, hexamethylene, toluene and tetrahydrofuran；Institute
The quality for stating solvent is 5~20 times of vulcanized lead quantum point mass.More volatile solvent is selected first, meanwhile, in order to vulcanize
Lead is preferably scattered in polymer solvent cannot be very little, otherwise can not disperse in polymerization；Therefore, the matter of preferred solvent of the present invention
It measures as 5~20 times of vulcanized lead quantum point mass.
As optimal technical scheme, the mass content of vinylacetate is 24 in the ethylene-vinyl acetate copolymer
~40%.EVA is commercialization, if 24%, advantages of good crystallization and it is opaque, so selection is more than 24%, but higher than 40%
It hardly results in.Because copolymer VA contents are difficult to obtain more than 40%, meanwhile, also make encapsulating film low strength, thus select 24
~40%.
As optimal technical scheme, the crosslinking agent is selected from two alkane of peroxidating, cyclohexanone peroxide, peroxidating diisopropyl
Benzene, methyl ethyl ketone peroxide, benzoyl peroxide, 2,2- azos double (2- methyl-props amidine) hydrochloride, dicetyl peroxydicarbonate diisopropyls
Ester, peroxidating two acyl, tert-butyl peroxy acetate, the different monooctyl ester tert-butyl ester of peroxidating, one kind in peroxidized t-butyl perbenzoate or
Several mixtures.
As optimal technical scheme, the UV light stabilizing agent is selected from 2,4-DihydroxyBenzophenone, 2- hydroxyl -4- methoxies
Base benzophenone, 2-hydroxy-4-n-octoxybenzophenone, 2- (2 '-hydroxyl -5 '-aminomethyl phenyl) benzotriazole, 2- (2 '-hydroxyls
Base -3 ', 5 '-diamyl phenyl) benzotriazole, 2- (2 '-hydroxyl -5 '-t-octyl phenyl) benzotriazole, 2- phenyl benzo miaows
Azoles -5- sulfonic acid, succinic acid and (4- hydroxyls -2,2, the polymer of 6,6- tetramethyl -1- piperidine alcohols), it is double (2,2,6,6- tetramethyls -
4- piperidyls) sebacate, double (- 4 hydroxybenzyl phosphate mono ethyl ester of 3,5- di-t-butyl) nickel, poly- { [6- (1,1,3,3- tetramethyls
Base butyl) one or more of mixture.
As optimal technical scheme, the antioxidant is selected from N, N '-bis- [3- (3,5- di-tert-butyl-hydroxy phenyl) third
Acyl] hydrazine, dilauryl thiodipropionate, pentaerythrite diphosphite two (2,4- di-tert-butyl phenyl) ester, double (2,2,6,6- tetra-
Methyl -4- piperidyls) sebacate, 2,2 '-methylene bis (4- methyl-6-tert-butylphenols), 2,6- di-t-butyl -4- methylbenzenes
Phenol, three (2,4- di-tert-butyl-phenyl) phosphite esters, four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythrites
The mixture of one or more of ester, 4,4 '-(β, β '-two propoxy phenyl of dihydroxy) -2,2- propane.
As optimal technical scheme, the plasticizer is one or more of Chinese wax oil, stearic acid, citric acid ester type
Mixture.
As optimal technical scheme, the melting is complex as the one or more in extrusion, mixing, injection or mill.
Just vulcanized lead can only show to turn photosensitiveness in specific dimensions scope, meanwhile, in order to meet wanting for solar cell
Blood orange light should be able to be converted uv light by asking, and is prepared Nano lead sulfide at present and had not been reported for conversion film.In addition, sulphur
It is undesirable to change the interaction of lead and polymer, the present invention is passed through by each component and its dosage, the reasonable selection of preparation process
Coupling agent and ultrasound realize the good nano-dispersed of vulcanized lead, obtain transparent encapsulating film.
The present invention is found through experiments that, ultraviolet light irradiate repeatedly 1000 it is small when more than, encapsulating film, which still has, turns photosensitiveness.And show
Have in technology using rare earth organic complex as in the scheme of light conversion agent, rare earth organic complex due to being organic matter ligand,
Thus ultraviolet light can decompose ligand, the optical property that turns of rare earth is quenched, when ultraviolet light 700 is small repeatedly after do not have turn
Photosensitiveness, this is the common sense of rare earth compounding this field.Also, rare earth luminous narrow range is 612nm, and vulcanized lead quantum dot light emitting
Scope width is 400~600nm.As it can be seen that this invention also solves the rare earth organic complexes and EVA composite membranes that have the function of to turn light
Existing short life, the problems such as efficiency is not good enough.
Compared with prior art, the device have the advantages that being：The EVA/ vulcanized lead obtained for having the function of to turn light
Quantum dot composite package adhesive film material, while there is the transparency, excellent turns photosensitiveness and permanent service life, ultraviolet light 1000
Hour or more still have turn optical property.
Description of the drawings
Upon reading the detailed description of non-limiting embodiments with reference to the following drawings, other feature of the invention,
Objects and advantages will become more apparent upon：
Fig. 1 is the transmitting light turn with the EVA/ vulcanized lead quantum dot composite package adhesive film materials of light of embodiment 2
Spectrum, as shown in Figure 1, the light emitting region of packaging adhesive film is 400~600nm；
Fig. 2 be embodiment 3 have the function of to turn the EVA/ vulcanized lead quantum dot composite package adhesive film materials of light it is ultraviolet-can
See spectrogram, as seen from Figure 2, packaging adhesive film is in light transmittance >=74% of visible ray；
Fig. 3 is the packaging adhesive film photo of embodiment 4, from the figure 3, it may be seen that packaging adhesive film is transparent.
Specific embodiment
Technical scheme is further described below by way of specific embodiment.Following embodiment is to this hair
It bright further explanation rather than limits the scope of the invention.
Embodiment 1
By weight, in 100 parts of acetone, 5 parts of vulcanized lead quantum dot, 0.05 part of silane coupling agent, ultrasound 10 are added in
Minute, it is spare as vulcanized lead quantum dot suspending liquid A.
By 100 parts of EVA (VA contents be 24%wt), 0.2 part of two alkane of peroxidating, 0.3 part of 2,4-DihydroxyBenzophenone,
1 part of N, N '-bis- [3- (3,5- di-tert-butyl-hydroxy phenyl) propionyl] hydrazine, 2 parts of dilauryl thiodipropionates, 0.1 part of Chinese wax
Oil and 20 parts of above-mentioned suspending liquid As, are put into high-speed mixer and are uniformly mixed, and are then uniformly mixed in 80 DEG C of open mills to get tool
There are the EVA/ vulcanized lead quantum dot composite package adhesive film materials for turning light function, it is seen that optical range light transmittance >=70% turns optical range
For 400-600nm.
Embodiment 2
In 100 parts of tetrahydrofurans, 20 parts of vulcanized lead quantum dot, 2 parts of titanate coupling agent are added in, ultrasound 120 minutes is made
It is spare for vulcanized lead quantum dot suspending liquid A.
By 100 parts of EVA (VA contents be 28%wt), 0.5 part of benzoyl peroxide, the different monooctyl ester tert-butyl ester of 2 parts of peroxidating,
0.3 part of double (2,2,6,6- tetramethyl -4- piperidyls) sebacate, 2.5 parts of 2-PHENYLBENZIMIDAZOLE-5-SULFONIC ACIDs, 1 part of Ji Wusi
Alcohol diphosphite two (2,4- di-tert-butyl phenyl) ester, 0.5 part 2,2 '-methylene bis (4- methyl-6-tert-butylphenols), 10 parts of lemons
Lemon acid esters and 10 parts of above-mentioned suspending liquid As, are put into high-speed mixer and are uniformly mixed, and are then uniformly mixed in 100 DEG C of mixers, i.e.,
There must be the EVA/ vulcanized lead quantum dot composite package adhesive film materials for turning light, it is seen that optical range light transmittance >=73%；Fig. 1 is
The emission spectrum turn with the EVA/ vulcanized lead quantum dot composite package adhesive film materials of light of embodiment 2, what which referred to
It is free intensity, as shown in Figure 1, the light emitting region of packaging adhesive film is 400~600nm.
Embodiment 3
In 100 parts of hexamethylenes, 10 parts of vulcanized lead quantum dot, 0.5 part of aluminate coupling agent are added in, ultrasound 180 minutes is made
It is spare for vulcanized lead quantum dot suspending liquid A.
By 100 parts of EVA (VA contents be 40%), 5 parts of cumyl peroxides, 5 parts of 2- (2 '-hydroxyl -3 ', 5 '-diamyl
Phenyl) benzotriazole, 0.1 part of 2,6- di-tert-butyl-4-methy phenol, 15 parts of stearic acid and 1 part of above-mentioned suspending liquid A, it is put into height
Fast mixer is uniformly mixed, and is then uniformly mixed have the function of to turn the EVA/ vulcanized lead quantum of light in 130 DEG C of extruders
Point composite package adhesive film material turns optical range as 400-600nm；Fig. 2 has the function of to turn the EVA/ vulcanized lead of light for embodiment 3
The UV-visible spectrum of quantum dot composite package adhesive film material, as seen from Figure 2, packaging adhesive film is in the light transmission of visible ray
Rate >=74%.
Embodiment 4
In 100 parts of toluene, 15 parts of addition vulcanized lead quantum dot, 0.2 part of titanate coupling agent, 0.4 part of silane coupling agent,
Ultrasound 100 minutes, it is spare as vulcanized lead quantum dot suspending liquid A.
By 100 parts of EVA (VA contents are 33%), 1 part of 2,2- azo double (2- methyl-props amidine) hydrochloride, 0.2 part of peroxidating
T-butyl perbenzoate, 0.3 part of 2-hydroxy-4-n-octoxybenzophenone, 1.2 parts of double (- 4 hydroxybenzyl phosphorus of 3,5- di-t-butyl
Sour mono ethyl ester) nickel, 0.2 part of double (2,2,6,6- tetramethyl -4- piperidyls) sebacate, 0.6 part 4,4 '-(β, β '-dihydroxy two
Propoxy phenyl) -2,2- propane, 1 part of citrate, 2 parts of stearic acid and 15 parts of above-mentioned suspending liquid As, it is put into high-speed mixer mixing
Uniformly, after then being mixed in 90 DEG C of open mills, then 120 ° of film forming vulcanize to get the EVA/ turn with light in injection molding machine
Lead quantum dot composite package adhesive film material, it is seen that optical range light transmittance >=73% turns optical range as 400-600nm.Fig. 3 is implementation
The packaging adhesive film photo of example 4, from the figure 3, it may be seen that packaging adhesive film is transparent.
Although present disclosure is discussed in detail by above preferred embodiment, but it should be appreciated that above-mentioned
Description is not considered as limitation of the present invention.After those skilled in the art have read the above, for the present invention's
A variety of modifications and substitutions all will be apparent.Therefore, protection scope of the present invention should be limited to the appended claims.
Claims (6)
1. a kind of compound preparation method for turning light packaging adhesive film material of EVA/ vulcanized lead quantum dot, which is characterized in that including as follows
Step：
It is prepared by the vulcanized lead quantum dot of surface treatment：In a solvent, vulcanized lead quantum dot and coupling agent, ultrasound 10~180 are added in
Minute, the vulcanized lead quantum dot suspending liquid A being surface-treated；
EVA/ vulcanized lead quantum dots are compound to turn light packaging adhesive film material preparation：In parts by weight, by 100 parts of ethyl vinyl acetate second
Enoate copolymer, 0.2~5 part of crosslinking agent, 0.3~5 part of UV light stabilizing agent, 0.1~3 part of antioxidant, 0.1~15 part of plasticising
Agent and 1~20 part of vulcanized lead quantum dot suspending liquid A, be uniformly mixed, under the conditions of 80~130 DEG C melt it is compound, i.e.,
The EVA/ vulcanized lead quantum dot is compound turns light packaging adhesive film material；
The vulcanized lead quantum dot is nano-particle vulcanized lead of the diameter in 1~20nm；The vulcanized lead quantum dot and coupling agent
Mass ratio be 100:(1~10)；The coupling agent is in silane coupling agent, titanate coupling agent, aluminate coupling agent
One or more of mixtures；
The UV light stabilizing agent is selected from 2,4 dihydroxyl benzophenone, ESCALOL 567,2- hydroxyls -4-
Oxy-octyl benzophenone, 2- (2'- hydroxyl -5'- aminomethyl phenyls) benzotriazole, 2- (2 '-hydroxyl -3 ', 5 '-diamyl phenyl)
Benzotriazole, 2- (2'- hydroxyl -5'- t-octyls phenyl) benzotriazole, 2-PHENYLBENZIMIDAZOLE-5-SULFONIC ACID, succinic acid and (4-
Hydroxyl -2,2,6,6- tetramethyl -1- piperidine alcohols) polymer, bis(2,2,6,6-tetramethyl-4-piperidyl)sebacate,
The mixture of one or more of double (hydroxybenzyl phosphate of 3,5-di-t-butyl-4 mono ethyl ester) nickel；
The plasticizer is the mixture of one or more of Chinese wax oil, stearic acid, citric acid ester type.
2. the compound preparation method for turning light packaging adhesive film material of EVA/ vulcanized lead quantum dot according to claim 1, special
Sign is that the solvent is selected from ethyl alcohol, acetone, hexane, hexamethylene, toluene and tetrahydrofuran；The quality of the solvent is vulcanization
5~20 times of lead quantum point mass.
3. the compound preparation method for turning light packaging adhesive film material of EVA/ vulcanized lead quantum dot according to claim 1, special
Sign is that the mass content of vinylacetate is 24~40% in the ethylene-vinyl acetate copolymer.
4. the compound preparation method for turning light packaging adhesive film material of EVA/ vulcanized lead quantum dot according to claim 1, special
Sign is that the crosslinking agent is selected from two alkane of peroxidating, cyclohexanone peroxide, cumyl peroxide, methyl ethyl ketone peroxide, 2,
2- azos double (2- methyl-props amidine) hydrochloride, di-isopropyl peroxydicarbonate, peroxidating two acyl, tert-butyl peroxy acetate, mistakes
Aoxidize the mixture of one or more of the different monooctyl ester tert-butyl ester, peroxidized t-butyl perbenzoate.
5. the compound preparation method for turning light packaging adhesive film material of EVA/ vulcanized lead quantum dot according to claim 1, special
Sign is that the antioxidant is selected from N, N'- double [3- (3,5- di-tert-butyl-hydroxy phenyl) propionyl] hydrazine, thio-2 acids two
Lauryl, pentaerythrite diphosphite two (2,4- di-tert-butyls phenyl) ester, double (2,2,6,6- tetramethyl -4- piperidyls) last of the ten Heavenly stems two
Acid esters, 2,2'- methylene bis (4- methyl-6-tert-butylphenols), 2,6 di tert butyl 4 methyl phenol, three (2,4- di-t-butyls
Phenyl) phosphite ester, four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol esters, 4,4'- (β, β '-dihydroxy
Two propoxy phenyls) one or more of -2,2- propane mixture.
6. the compound preparation method for turning light packaging adhesive film material of EVA/ vulcanized lead quantum dot according to claim 1, special
Sign is that the melting is complex as the one or more in extrusion, mixing, injection or mill.
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| TW201805404A (en) * | 2016-03-24 | 2018-02-16 | ３Ｍ新設資產公司 | Quantum dot compositions and quantum dot articles |
| CN106833406A (en) * | 2017-02-22 | 2017-06-13 | 杭州福斯特光伏材料股份有限公司 | A kind of high refractive index nano inorganic matter hydridization photovoltaic encapsulation material |
| CN109747018A (en) * | 2017-11-02 | 2019-05-14 | 中国科学院金属研究所 | A kind of shinyleaf yellowhorn fruit shell antibacterial bacteriostatic artificial composite plank and its manufacturing method |
| CN109929557A (en) * | 2017-12-15 | 2019-06-25 | Tcl集团股份有限公司 | A kind of composite membrane and the preparation method and application thereof |
| CN108034391B (en) * | 2017-12-27 | 2020-01-07 | 厦门大学 | Solar cell EVA packaging adhesive film material with light conversion function and preparation method thereof |
| CN109161349B (en) * | 2018-07-12 | 2021-02-05 | 杭州福斯特应用材料股份有限公司 | High-light-transmittance photovoltaic packaging material adopting nucleation anti-reflection agent |
| CN111363483A (en) * | 2018-12-24 | 2020-07-03 | 中国科学院上海高等研究院 | Composite material adhesive film, photovoltaic module structure and preparation method |
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| CN102226064B (en) * | 2011-04-29 | 2013-03-13 | 浙江大学 | Ethylene-vinyl acetate adhesive film containing quantum dots as well as preparation method and application thereof |
| CN102891203A (en) * | 2012-10-06 | 2013-01-23 | 保定天威薄膜光伏有限公司 | Fluorescence conversion white packaging material and solar cell adopting same |
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