CN102967524A - Ethylene vinyl acetate (EVA) crosslinking degree testing method - Google Patents
Ethylene vinyl acetate (EVA) crosslinking degree testing method Download PDFInfo
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- CN102967524A CN102967524A CN2012105099809A CN201210509980A CN102967524A CN 102967524 A CN102967524 A CN 102967524A CN 2012105099809 A CN2012105099809 A CN 2012105099809A CN 201210509980 A CN201210509980 A CN 201210509980A CN 102967524 A CN102967524 A CN 102967524A
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Abstract
The invention discloses an ethylene vinyl acetate (EVA) crosslinking degree testing method, which comprises the following steps: cutting EVA subjected to laminating, crosslinking and curing into fragments; performing liquid nitrogen refrigeration treatment on the EVA fragments, so that the EVA is subjected to vitrification; milling the EVA subjected to vitrification into particles; filling the milled EVA in a screening bag with the particle size of 120-200 meshes for screening; extracting and stirring the weighed screening bag and the EVA in a solvent at the medium/low-temperature of 120-140 DEG C; drying the screening bag filled with EVA in a drying box at the temperature of 140 DEG C after extraction is finished; weighing the dried EVA and the screening bag together; and obtaining the crosslinking degree of the EVA according to a formula that the crosslinking degree is equal to the weight difference before and after the extraction of the screening bag filled with the EVA dividing the weight before extraction of the screening bag filled with the EVA. The method is convenient to operate and accurate.
Description
Technical field
The present invention relates to a kind of EVA degree of crosslinking measuring technology, belong to the photovoltaic field.
Background technology
The EVA degree of crosslinking is the important indicator of EVA performance.Understand according to the applicant, in the at present domestic and international photovoltaic industry, for the test of EVA degree of crosslinking, the basic technology that adopts extraction and DSC.DSC is the english abbreviation of differential scanning calorimetry, and the DSC measuring accuracy is higher, but equipment investment is relatively large, and specimen quantity is few, is difficult to satisfy suitability for industrialized production to the demand of test.Abstraction technique mainly is to adopt toluene and dimethylbenzene as solvent, under 140 ℃ the EVA sample behind the lamination crosslinking curing is being extracted, and does not have crosslinked EVA strand in the extraction sample.Existing EVA degree of crosslinking measuring technology, first the EVA behind the lamination crosslinking curing to be cut into little EVA fragment, then by being generally the long-time extraction of 140 ℃ of high temperature and 5 hours, again oven dry, at last by the degree of crosslinking formula: degree of crosslinking=fill the front total amount of screening bag extraction front and back weight difference/extraction of EVA, calculate degree of crosslinking.Yet, this method, because EVA itself has elasticity, the EVA sample size after the shearing is bigger than normal, the size that 2*2mm is arranged usually is unfavorable for the migration extraction of uncrosslinked EVA strand, simultaneously, under long-time high temperature, secondary cross-linking occurs in EVA easily, can cause the measurement result distortion like this.
Summary of the invention
The object of the present invention is to provide a kind of convenience, EVA degree of crosslinking method of testing accurately.
Technical solution of the present invention is:
A kind of EVA degree of crosslinking method of testing is characterized in that: comprise the steps:
(1) EVA behind the lamination crosslinking curing is cut into fragment;
(2) the EVA fragment is carried out the liquid nitrogen frozen processing and make the EVA vitrifacation;
(3) vitrified EVA is milled become particle;
(4) 120～200 purposes screening bag of packing into of the EVA after will milling screens;
(5) the screening bag after the weighing is placed 120 ℃～140 ℃ extractions of solvent low temperature together with EVA, and stir;
(6) the screening bag that fills EVA after extraction is finished places 140 ℃ of dryings of drying box;
(7) EVA that drying is finished carries out weighing together with the screening bag, according to the EVA weight before remaining EVA weight after degree of crosslinking=extraction/extraction, obtains the degree of crosslinking of EVA.
Described stirring is to adopt electric stirrer with shaft to stir or adopt constant temperature blender with magnetic force to stir.The extraction solvent for use is dimethylbenzene.
EVA after the present invention is crosslinked to lamination forms the EVA fragment through shearing, through having realized vitrified transformation after the liquid nitrogen frozen processing, make to have flexible EVA and present fragility, the EVA fragment is milled again, it is little to obtain particle diameter, the particle that specific surface area is high, then 120～200 purposes of packing into screening bag screens, and again by the uncrosslinked EVA of stirring technique low-temperature extraction, thereby has shortened the traditional extraction time of EVA, reduce extraction temperature, improved the accuracy of testing efficiency and test result.
Conventional EVA degree of crosslinking measuring technology, EVA after crosslinked to lamination cuts into fragment, then directly under 140 ℃ of high temperature, carry out nothing and stir extraction, can cause the EVA chip size bigger than normal, uncrosslinked EVA strand migration distance is partially long, be difficult for being extracted out, high temperature causes EVA again crosslinked easily, so that the resultant error of measuring is bigger than normal.Because the present invention adopts ripe liquid nitrogen frozen technology, so that have flexible EVA embrittlement originally, namely realized the EVA vitrifacation, be easy to mill, make EVA become fine particle is achieved by milling, effectively shorten the migration distance of uncrosslinked EVA strand, increased the contact area of EVA extraction solvent.Simultaneously, because EVA degree of crosslinking measuring technology, in extraction process, used stirring technique, can form liquid turbulence like this, accelerate the migration rate of uncrosslinked EVA strand, therefore can farthest improve the speed of EVA degree of crosslinking, can reduce accordingly the temperature of extraction solvent, reduce to greatest extent the secondary cross-linking of EVA and the deviation of test result.
The present invention is with general industrialized conventional EVA degree of crosslinking p-wire can be well compatible at present, can directly utilize existing conventional equipment, avoided the with high investment of equipment aspect, be conducive to EVA degree of crosslinking measuring technology industrialization popularization and application, improve the test rate of EVA degree of crosslinking and the accuracy of data.By cooled with liquid nitrogen EVA, obtain vitrified EVA, be convenient to mill; To vitrified EVA, milling obtains fine particle; Relatively conventional EVA degree of crosslinking measuring technology, adopt stirring technique in the extraction process, can form liquid turbulence like this, accelerate the migration rate of uncrosslinked EVA strand, therefore can farthest improve the speed of EVA degree of crosslinking, the temperature of extraction solvent be can reduce accordingly, the secondary cross-linking of EVA and the deviation of test result reduced to greatest extent.
Description of drawings
The invention will be further described below in conjunction with drawings and Examples.
Fig. 1 is nitrogen cooling and the milling device synoptic diagram of EVA degree of crosslinking measuring technology.
Fig. 2 is electric stirring apparatus synoptic diagram.
Fig. 3 is the magnetic stirring apparatus synoptic diagram.
Embodiment
The measuring technology of the EVA degree of crosslinking of present embodiment (such as Fig. 1, Fig. 2, shown in Figure 3) comprises the steps:
(1) EVA after adopting scissors or cutting knife crosslinked to lamination shears, and obtains the EVA fragment;
(2) it is freezing to adopt 1 pair of EVA fragment of liquid nitrogen to carry out, and makes its vitrifacation;
(3) EVA after 2 pairs of refrigeration glass of employing milling device mills;
(4) adopt 120～200 purposes screening bag 5 rear weighings of EVA particle, screening of packing into after milling;
(5) the screening bag 5 after the weighing is placed the there-necked flask 7 that fills xylene solvent together with EVA, adopt electric heating cover 8 P-xylene solvents to be heated to 120 ℃～140 ℃, adopt thermopair 4 to measure the temperature of xylene solvent, adopt condensation reflux unit 6 P-xylene condensing refluxes, and adopt stirring apparatus P-xylene solvent to stir;
In this step, stirring has following two kinds of methods:
1, employing comes the P-xylene solvent to stir with the electric stirrer 3 of shaft.
2, employing constant temperature blender with magnetic force 10 comes P-xylene to carry out the oil bath heating and magnet rotor 9 P-xylene solvent under magneticaction stirs.
(6) the screening bag that fills EVA after extraction is finished places 140 ℃ of dryings of drying box;
(7) EVA that drying is finished carries out weighing together with the screening bag;
(8) by the degree of crosslinking formula: degree of crosslinking=extraction is the front EVA weight of remaining EVA weight/extraction afterwards, obtains the degree of crosslinking of EVA.
Basic step method among the present invention, such as EVA is sheared, with xylene solution to EVA extraction, dry together with EVA to the screening bag with drying box, to the weighing of EVA, belong to existing proven technique means, therefore in the present embodiment, the method for these steps is not described in detail.Innovative point of the present invention is to adopt cooled with liquid nitrogen EVA, obtain vitrified EVA, be convenient to mill, by to vitrified EVA, milling, it is large to obtain specific surface area, the particle of small particle diameter, can increase the contact area of solvent and EVA, reduce the migration distance of uncrosslinked EVA, adopt stirring technique in the extraction process, can form liquid turbulence like this, so that the temperature of xylene solution is more balanced, the EVA solute is more even, therefore can farthest improve the speed of EVA degree of crosslinking, can reduce accordingly the temperature of extraction solvent, reduce to greatest extent the secondary cross-linking of EVA and the deviation of test result.The present invention has outstanding characteristics and significant progressive.
In addition to the implementation, the present invention can also have other embodiments.All employings are equal to the technical scheme of replacement or equivalent transformation formation, all drop on the protection domain of requirement of the present invention.
Claims (3)
1. an EVA degree of crosslinking method of testing is characterized in that: comprise the steps:
(1) EVA behind the lamination crosslinking curing is cut into fragment;
(2) the EVA fragment is carried out the liquid nitrogen frozen processing and make the EVA vitrifacation;
(3) vitrified EVA is milled become particle;
(4) 120～200 purposes screening bag of packing into of the EVA after will milling screens;
(5) the screening bag after the weighing is placed 120 ℃～140 ℃ extractions of solvent low temperature together with EVA, and stir;
(6) the screening bag that fills EVA after extraction is finished places 140 ℃ of dryings of drying box;
(7) EVA that drying is finished carries out weighing together with the screening bag, according to the EVA weight before remaining EVA weight after degree of crosslinking=extraction/extraction, obtains the degree of crosslinking of EVA.
2. EVA degree of crosslinking method of testing according to claim 1 is characterized in that: described stirring is to adopt electric stirrer with shaft to stir or adopt constant temperature blender with magnetic force to stir.
3. EVA degree of crosslinking method of testing according to claim 1 and 2, it is characterized in that: the extraction solvent for use is dimethylbenzene.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104075958A (en) * | 2013-03-27 | 2014-10-01 | 普德光伏技术（苏州）有限公司 | Method for testing degree of crosslinking of materials of encapsulation layers of photovoltaic module |
| CN104280309A (en) * | 2013-07-02 | 2015-01-14 | 普德光伏技术（苏州）有限公司 | Measuring method for crosslinking degree of photovoltaic assembly EVA packaging material |
| CN104347447A (en) * | 2014-09-15 | 2015-02-11 | 阿特斯(中国)投资有限公司 | EVA (ethylene-vinyl acetate copolymer) cross-linking rate test method |
| CN104458488A (en) * | 2014-12-16 | 2015-03-25 | 上海微谱化工技术服务有限公司 | Analysis method of EVA hot melt adhesive |
| CN106644813A (en) * | 2016-12-26 | 2017-05-10 | 广州市白云化工实业有限公司 | Analysis method of cross-linking degree of moisture-curable polyurethane |
| CN106706458A (en) * | 2016-11-30 | 2017-05-24 | 安徽振兴光伏新能源有限公司 | Electric-jacket crosslinking degree testing method for EVA (Ethylene-Vinyl Acetate copolymer) |
| CN109142134A (en) * | 2018-07-18 | 2019-01-04 | 凯盛光伏材料有限公司 | A kind of test method of the photovoltaic module POE glue film degree of cross linking |
| CN110441181A (en) * | 2019-08-20 | 2019-11-12 | 江苏厚生新能源科技有限公司 | A kind of test method of lithium battery film material molten index |
| CN114414423A (en) * | 2021-11-25 | 2022-04-29 | 苏州腾晖光伏技术有限公司 | Method for testing crosslinking degree of white adhesive film of photovoltaic module |
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Patent Citations (3)
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104075958A (en) * | 2013-03-27 | 2014-10-01 | 普德光伏技术（苏州）有限公司 | Method for testing degree of crosslinking of materials of encapsulation layers of photovoltaic module |
| CN104280309A (en) * | 2013-07-02 | 2015-01-14 | 普德光伏技术（苏州）有限公司 | Measuring method for crosslinking degree of photovoltaic assembly EVA packaging material |
| CN104347447A (en) * | 2014-09-15 | 2015-02-11 | 阿特斯(中国)投资有限公司 | EVA (ethylene-vinyl acetate copolymer) cross-linking rate test method |
| CN104347447B (en) * | 2014-09-15 | 2017-03-08 | 阿特斯(中国)投资有限公司 | A kind of method of testing of EVA crosslinking rate |
| CN104458488A (en) * | 2014-12-16 | 2015-03-25 | 上海微谱化工技术服务有限公司 | Analysis method of EVA hot melt adhesive |
| CN106706458A (en) * | 2016-11-30 | 2017-05-24 | 安徽振兴光伏新能源有限公司 | Electric-jacket crosslinking degree testing method for EVA (Ethylene-Vinyl Acetate copolymer) |
| CN106644813A (en) * | 2016-12-26 | 2017-05-10 | 广州市白云化工实业有限公司 | Analysis method of cross-linking degree of moisture-curable polyurethane |
| CN106644813B (en) * | 2016-12-26 | 2019-08-27 | 广州市白云化工实业有限公司 | A kind of analysis method of the moisture cure urethanes degree of cross linking |
| CN109142134A (en) * | 2018-07-18 | 2019-01-04 | 凯盛光伏材料有限公司 | A kind of test method of the photovoltaic module POE glue film degree of cross linking |
| CN110441181A (en) * | 2019-08-20 | 2019-11-12 | 江苏厚生新能源科技有限公司 | A kind of test method of lithium battery film material molten index |
| CN114414423A (en) * | 2021-11-25 | 2022-04-29 | 苏州腾晖光伏技术有限公司 | Method for testing crosslinking degree of white adhesive film of photovoltaic module |
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Application publication date: 20130313 |