CN103207177B - Test method for content of crosslinking agent in EVA - Google Patents
Test method for content of crosslinking agent in EVA Download PDFInfo
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- CN103207177B CN103207177B CN201210012147.3A CN201210012147A CN103207177B CN 103207177 B CN103207177 B CN 103207177B CN 201210012147 A CN201210012147 A CN 201210012147A CN 103207177 B CN103207177 B CN 103207177B
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Abstract
The invention provides a test method for content of a crosslinking agent in EVA. The test method comprises the following steps of dissolving the EVA; suction filtering and collecting a filter solution; rotary evaporating the filter solution collected by the above step until the filter solution is dried; adding potassium iodide, isopropanol and acetic acid to a flask containing an extract extracted by the above step and a clean flask respectively, adding a magnetic stirrer to each flask; putting the flasks in water bath; reacting under the magnetic stirring to obtain a sample and a blank sample; titrating the above sample and the blank sample with sodium thiosulfate to colorless; and calculating the content of peroxy bonds in the crosslinking agent. The test method for the content of the crosslinking agent in the EVA can not only extract the crosslinking agent from the EVA but also analyze the content of the crosslinking agent. At the same time, the test method is simple in process and has relatively low test cost and strong pertinency and practicality.
Description
Technical field
The present invention relates to the technical field of measurement and test of photovoltaic encapsulation EVA, particularly relate to a kind of method of testing of EVA content of crosslinking agent.
Background technology
EVA is the widely used encapsulating material of crystal silicon solar energy battery.EVA has excellent pliability, resistance to impact, elasticity, optical transparence, low temperature flexing, stickability, environmental stress crack resistance, weatherability, chemical-resistant, heat sealability and electrical property etc.
But in existing industry, the evaluation of EVA cross-linking system is generally only adopted to the method for test degree of crosslinking, and the overall evaluation of degree of crosslinking just to EVA cross-linking system, to some problem EVA or assembly, only test the degree of crosslinking of EVA, and deep anatomy is not carried out to EVA cross-linking system, be difficult to find question classification., very easily decompose because crosslinking chemical is heated, and molecular characterization is not strong meanwhile, thus is difficult to test its content by chromatographic process, thus in existing industry, do not test the method for content of crosslinking agent so far.
In view of this, the method for testing that a kind of EVA content of crosslinking agent is provided is necessary, to solve the problem.
Summary of the invention
The object of the present invention is to provide a kind of method of testing all in fields such as developing material, failure analysis, resisting ageing for long time researchs with the EVA content of crosslinking agent of very strong using value.
For achieving the above object, the method for testing of a kind of EVA content of crosslinking agent of the present invention, it comprises the following steps:
S10, EVA to be dissolved;
S20, suction filtration, and collect filtrate;
S30, by step S20 collect filtrate rotary evaporation do;
S40, add potassium iodide, isopropyl alcohol, acetic acid respectively in two extract extracted containing S30 in steps and clean flasks, add magnetic stir bar, put into the reaction of water-bath magnetic agitation, obtain sample and blank sample;
S50, respectively said sample and blank sample are titrated to colourless with sodium thiosulfate;
The volume of sodium thiosulfate, the concentration of the sodium thiosulfate of demarcation and the weight of EVA that S60, the volume of sodium thiosulfate utilizing titration sample to consume, the blank sample of titration consume are to calculate the content of crosslinking chemical peroxide bridge.
As a further improvement on the present invention, described step S10 specifically comprises:
S101, uncrosslinked EVA tetrahydrofuran to be dissolved;
S102, in the lysate of step S101, add absolute ethyl alcohol, and carry out stirring and producing precipitation.
As a further improvement on the present invention, described step S10 is specially: soaked by the EVA absolute ethyl alcohol after crosslinked, and add magnetic stir bar, and 40 DEG C of lower magnetic forces stir 40-50 hour.
As a further improvement on the present invention, described step S101 was specially: get EVA and join in conical flask, add tetrahydrofuran, and add magnetic stir bar, 35 DEG C to 45 DEG C lower magnetic force stirring and dissolving 25 ~ 35 minutes.
As a further improvement on the present invention, described step S101 is specifically 40 DEG C of lower magnetic force stirring and dissolving 30 minutes.
As a further improvement on the present invention, described step S20 is specially: use bottle,suction vacuum filtration, and rinses conical flask and filter residue at least three times with absolute ethyl alcohol, collects whole filtrate.
As a further improvement on the present invention, described step S30 is specially: filtrate be poured in flask, rotary evaporation at 40 DEG C to 55 DEG C.
As a further improvement on the present invention, described step S30 comprises further: filtrate rotary evaporation be concentrated into 1/10th or less time, whole concentrate is poured into and compares in another little clean flask of above-mentioned flask volume, continue rotary evaporated to dryness.
As a further improvement on the present invention, described step S30 carries out rotary evaporation at 50 DEG C.
As a further improvement on the present invention, described step S40 is magnetic agitation reaction 3-40 minute in the water-bath of 65 DEG C to 90 DEG C specifically, obtains sample and blank sample.
As a further improvement on the present invention, described two flasks are that magnetic agitation reacts 15 minutes in the water-bath of 70 DEG C.
As a further improvement on the present invention, the concentration of the sodium thiosulfate of described step S50 employing is 0.005mol/L.
Compared with prior art, advantage of the present invention is: the method for testing of EVA content of crosslinking agent of the present invention, can not only extract crosslinking chemical from EVA, can also do content analysis to it; Meanwhile, this method of testing process is simple and direct, testing cost is lower, specific aim and practicality stronger.
Accompanying drawing explanation
Fig. 1 is the process flow diagram of the method for testing of EVA content of crosslinking agent of the present invention.
Fig. 2 is the particular flow sheet of step S10 shown in Fig. 1.
Embodiment
In order to make the object, technical solutions and advantages of the present invention clearly, describe the present invention below in conjunction with the drawings and specific embodiments.
As shown in Figure 1, the method for testing of EVA content of crosslinking agent of the present invention, comprises the following steps:
S10, EVA to be dissolved;
S20, suction filtration, and collect filtrate;
S30, by step S20 collect filtrate rotary evaporation do;
S40, add potassium iodide, isopropyl alcohol, acetic acid respectively in two extract extracted containing S30 in steps and clean flasks, add magnetic stir bar, put into the reaction of water-bath magnetic agitation, obtain sample and blank sample;
S50, respectively said sample and blank sample are titrated to colourless with sodium thiosulfate;
The volume of sodium thiosulfate, the concentration of the sodium thiosulfate of demarcation and the weight of EVA that S60, the volume of sodium thiosulfate utilizing titration sample to consume, the blank sample of titration consume are to calculate the content of crosslinking chemical peroxide bridge.
In present embodiment, calculate the expression formula of crosslinking chemical peroxide bridge content=
, the wherein volume of sodium thiosulfate that consumes for titration sample of V1, the volume of the sodium thiosulfate that V0 consumes for the blank sample of titration, c is the concentration of the sodium thiosulfate demarcated, and m is the weight of EVA.
The method of testing of EVA content of crosslinking agent of the present invention can be applicable to uncrosslinked EVA, also can be applicable to the EVA after being cross-linked.
As shown in Figure 2, for uncrosslinked EVA, described step S10 specifically comprises:
S101, uncrosslinked EVA tetrahydrofuran to be dissolved;
S102, in the lysate of step S101, add absolute ethyl alcohol, and carry out stirring and producing precipitation.
Wherein, described step S101 was specially: get EVA and join in conical flask, add tetrahydrofuran, and add magnetic stir bar, 35 DEG C to 45 DEG C lower magnetic force stirring and dissolving 25 ~ 35 minutes.Further, described step S101 is specifically 40 DEG C of lower magnetic force stirring and dissolving 30 minutes.In present embodiment, to get EVA 2g, then described step S101 is specially: get EVA 2g, cut little after join in 250ml conical flask, add 30ml tetrahydrofuran, and add magnetic stir bar, 40 DEG C of lower magnetic force stirring and dissolving 30 minutes.
Described step S102 is specially: in conical flask, pour 150ml absolute ethyl alcohol into, rapid stirring 5 minutes, and then produces precipitation.
For the EVA after crosslinked, described step S10 is: soaked by the EVA absolute ethyl alcohol after crosslinked, and add magnetic stir bar, and 40 DEG C of lower magnetic forces stir 40-50 hour.Wherein, described step S10 is specially: get EVA 2g, is cut into 1mm × 5mm size, joins in 250ml flask, adds 150ml absolute ethyl alcohol, and adds magnetic stir bar, stirs 48 hours at 40 DEG C of lower magnetic forces.
As shown in Figure 1, described step S20 is specially: use bottle,suction vacuum filtration, and rinses conical flask and filter residue at least three times with absolute ethyl alcohol, collects whole filtrate.
Described step S30 is specially: filtrate be poured in flask, rotary evaporation at 40 DEG C to 55 DEG C.Described step S30 comprises further: filtrate rotary evaporation be concentrated into 1/10th or less time, whole concentrate is poured into and compares in another little clean flask of above-mentioned flask volume, continue rotary evaporated to dryness.Wherein, described step S30 carries out rotary evaporation at 50 DEG C.In present embodiment, described step S30 is specially: filtrate be poured in 500ml flask, rotary evaporation at 50 DEG C, when filtrate rotary evaporation is concentrated into 15ml, is poured into by whole concentrate in another clean 50ml flask, continues rotary evaporated to dryness.
Described step S40 is specially: respectively to containing extract with clean two flasks in add 0.1-1g potassium iodide, 5-50ml isopropyl alcohol, 0.1-10ml acetic acid, adds magnetic stir bar, put into the water-bath magnetic agitation reaction 3-40 minute of 65 DEG C to 90 DEG C, obtain sample and blank sample.Wherein, described two flasks are that magnetic agitation reacts 15 minutes in the water-bath of 70 DEG C.In present embodiment, described step S40 is specially: respectively to containing extract with clean two 50ml flasks in add 0.4g potassium iodide, 10ml isopropyl alcohol, 1ml acetic acid, add magnetic stir bar, the water-bath magnetic agitation putting into 70 DEG C reacts 15 minutes, obtains sample and blank sample.
The concentration of the sodium thiosulfate that described step S50 adopts is 0.005mol/L.Wherein, the preparation steps of the sodium thiosulfate of described 0.005mol/L is: 1.24g thiosulfuric acid sodium crystal and 0.2g powdered sodium carbonate are joined in the brown volumetric flask of 1000ml, rocks evenly.
In described step S60, the demarcating steps of hypo solution is specially: get potassium dichromate and dry 1 hour at 120 DEG C, in desiccator after cooling, take 0.01g and put into 100ml Erlenmeyer flask, and add 0.4g potassium iodide, 5ml distilled water, the sulfuric acid solution of 2ml 20%, jiggles dissolving, places after 20 minutes in dark cabinet, light color is titrated to sodium thiosulfate, add starch indicator 3, shake up rear continuation titration, make it become bright green from blueness.
The concentration computing formula of the hypo solution demarcated in described step S60 is: the concentration c of hypo solution=
, wherein, m is the weight of potassium dichromate, the volume of the sodium thiosulfate that V consumes for titration.
The method of testing of EVA content of crosslinking agent of the present invention, can not only extract crosslinking chemical, and do content analysis from uncrosslinked EVA; Crosslinking chemical can also be extracted from the EVA after crosslinked, and do content analysis, be the much progress in existing industry; Meanwhile, the method for testing of EVA content of crosslinking agent of the present invention all has very strong using value in fields such as developing material, failure analysis, resisting ageing for long time researchs.
In sum, the method for testing of EVA content of crosslinking agent of the present invention, not only process simple and direct, only need several conventional chemical reagent and vessel, and testing cost is lower, require also lower to tester, slightly doing training can operate, meanwhile, specific aim, practicality are stronger.
Above embodiment is only in order to illustrate technical scheme of the present invention and unrestricted, although with reference to preferred embodiment to invention has been detailed description, those of ordinary skill in the art is to be understood that, can modify to technical scheme of the present invention or equivalent replacement, and not depart from the spirit and scope of technical solution of the present invention.
Claims (12)
1. a method of testing for EVA content of crosslinking agent, described EVA crosslinking chemical is used for photovoltaic encapsulation, and it is characterized in that, the method for testing of described EVA content of crosslinking agent comprises the following steps:
S10, EVA to be dissolved;
S20, suction filtration, and collect filtrate;
S30, by step S20 collect filtrate rotary evaporation do;
S40, add potassium iodide, isopropyl alcohol, acetic acid respectively in two extract extracted containing S30 in steps and clean flasks, add magnetic stir bar, put into the reaction of water-bath magnetic agitation, obtain sample and blank sample;
S50, respectively said sample and blank sample are titrated to colourless with sodium thiosulfate;
The volume of sodium thiosulfate, the concentration of the sodium thiosulfate of demarcation and the weight of EVA that S60, the volume of sodium thiosulfate utilizing titration sample to consume, the blank sample of titration consume are to calculate the content of crosslinking chemical peroxide bridge.
2. the method for testing of EVA content of crosslinking agent according to claim 1, is characterized in that: described step S10 specifically comprises:
S101, uncrosslinked EVA tetrahydrofuran to be dissolved;
S102, in the lysate of step S101, add absolute ethyl alcohol, and carry out stirring and producing precipitation.
3. the method for testing of EVA content of crosslinking agent according to claim 1, is characterized in that: described step S10 is specially: soaked by the EVA absolute ethyl alcohol after crosslinked, and add magnetic stir bar, and 40 DEG C of lower magnetic forces stir 40-50 hour.
4. the method for testing of EVA content of crosslinking agent according to claim 2, it is characterized in that: described step S101 is specially: get EVA and join in conical flask, add tetrahydrofuran, and add magnetic stir bar, 35 DEG C to 45 DEG C lower magnetic force stirring and dissolving 25 ~ 35 minutes.
5. the method for testing of EVA content of crosslinking agent according to claim 4, is characterized in that: described step S101 is specifically 40 DEG C of lower magnetic force stirring and dissolving 30 minutes.
6. the method for testing of the EVA content of crosslinking agent according to claim 3 or 4, is characterized in that: described step S20 is specially: use bottle,suction vacuum filtration, and rinses conical flask and filter residue at least three times with absolute ethyl alcohol, collects whole filtrate.
7. the method for testing of EVA content of crosslinking agent according to claim 6, is characterized in that: described step S30 is specially: filtrate be poured in flask, rotary evaporation at 40 DEG C to 55 DEG C.
8. the method for testing of EVA content of crosslinking agent according to claim 7, it is characterized in that: described step S30 comprises further: filtrate rotary evaporation be concentrated into 1/10th or less time, whole concentrate is poured into and compares in another little clean flask of above-mentioned flask volume, continue rotary evaporated to dryness.
9. the method for testing of EVA content of crosslinking agent according to claim 7, is characterized in that: described step S30 carries out rotary evaporation at 50 DEG C.
10. the method for testing of EVA content of crosslinking agent according to claim 7, is characterized in that: described step S40 is magnetic agitation reaction 3-40 minute in the water-bath of 65 DEG C to 90 DEG C specifically, obtains sample and blank sample.
The method of testing of 11. EVA content of crosslinking agent according to claim 10, is characterized in that: described two flasks are that magnetic agitation reacts 15 minutes in the water-bath of 70 DEG C.
The method of testing of 12. EVA content of crosslinking agent according to claim 10, is characterized in that: the concentration of the sodium thiosulfate that described step S50 adopts is 0.005mol/L.
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| CN104458487A (en) * | 2014-12-16 | 2015-03-25 | 上海微谱化工技术服务有限公司 | Analysis method of wire and cable |
| CN104390876A (en) * | 2014-12-16 | 2015-03-04 | 上海微谱化工技术服务有限公司 | Analysis method for PE pipe |
| CN104406883A (en) * | 2014-12-16 | 2015-03-11 | 上海微谱化工技术服务有限公司 | Analysis method of PE and EVA blending system |
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| CN102004102A (en) * | 2010-11-10 | 2011-04-06 | 湖北富邦化工科技有限公司 | Method for measuring content of fatty amine in oily anticaking agent |
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Address after: 215000 Suzhou high tech Industrial Development Zone, Jiangsu Province, Lu Lu, No. 199, No. Co-patentee after: Changshu Canadian Solar Inc. Patentee after: Artes sunshine Power Group Co. Ltd. Address before: 215000 Suzhou high tech Industrial Development Zone, Jiangsu Province, Lu Lu, No. 199, No. Co-patentee before: Changshu Canadian Solar Inc. Patentee before: Canadian (China) Investment Co., Ltd. |
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Address after: No. 199, deer mountain road, Suzhou high tech Zone, Jiangsu Province Patentee after: Atlas sunshine Power Group Co.,Ltd. Patentee after: Changshu Artes Sunshine Power Technology Co.,Ltd. Address before: 215000 No. 199 Lu Shan Road, Suzhou hi tech Industrial Development Zone, Suzhou, Jiangsu Patentee before: CSI SOLAR POWER GROUP Co.,Ltd. Patentee before: Changshu Artes Sunshine Power Technology Co.,Ltd. |