CN104502221A - Method for analyzing functional greenhouse film - Google Patents
Method for analyzing functional greenhouse film Download PDFInfo
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- CN104502221A CN104502221A CN201410773574.2A CN201410773574A CN104502221A CN 104502221 A CN104502221 A CN 104502221A CN 201410773574 A CN201410773574 A CN 201410773574A CN 104502221 A CN104502221 A CN 104502221A
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Abstract
The invention relates to a method for analyzing a functional greenhouse film. The method comprises the following steps: providing a functional greenhouse film comprising PE and EVA to obtain a first to-be-detected sample; analyzing the first to-be-detected sample by virtue of TGA to obtain a first VA content; dissolving the first to-be-detected sample with chloroform, separating PE from EVA, calculating to obtain the mass of a dissolved substance and a soluble substance and drying the soluble substance to obtain a second to-be-detected sample; analyzing the second to-be-detected sample by virtue of TGA to obtain a second VA content; and calculating the first VA content and the second VA content to obtain the content of EVA in a PEEVA system.
Description
Technical field
The present invention relates to analysis field, be specifically related to microgram spectral analysis technology, particularly the analytical approach of EVA in functional greenhouse film.
Background technology
PE is the main material producing functional greenhouse film, functional greenhouse film needs to have higher weather-proof, resistance to droplet and heat-insulating property, but because tygon does not have polarity, even if add a certain amount of antifogging agent, its antifogging property also can only maintain about 2 months, and adds the canopy film that a certain amount of EVA resin makes, and not only has higher transmittance, and antifogging property is also greatly improved, generally can more than 4 months.
In prior art, ethene EVA co-mixing system is good flexibility and a little elasticity just, and wherein the ratio of PE is higher, and tack is poorer, and general being used as produces film.By regulating two kinds of chemical substance ratios, make it meet different application needs, wherein the content of EVA medium vinyl acetate is higher, and its transparency, pliability and toughness can improve relatively.So the determination of EVA content in co-mixing system just seems extremely important.
PE/EVA system is mainly the mechanical blending system of PE and EVA, PE and the EVA key distinction is that PE is formed by the addition polymerization of ethene, the Polymer be formed by connecting by-CH2-the unit repeated, EVA then forms for ethene and vinyl acetate random copolymerization, and ratio is variable between two kinds of components, therefore, by conventional method as infrared, nuclear-magnetism all cannot carry out quantitatively composition each in PE/EVA system.
Summary of the invention
In order to solve the problems of the technologies described above, an object of the present invention is the analytical approach providing a kind of functional greenhouse film, comprises the following steps:
There is provided functional greenhouse film, obtain the first testing sample, described first testing sample is made up of PE, EVA;
Use TGA to analyze the first testing sample, obtain a VA content;
PE, EVA in first testing sample is separated, after oven dry, obtains the second testing sample;
Use TGA to analyze the second testing sample, obtain the 2nd VA content;
The content of EVA in PEEVA system is obtained by a VA content, the 2nd VA cubage.
In described PE/EVA, the content of EVA is lower than 55%.
Described functional greenhouse film also comprises pigment and/or filler.
Described filler is one or more in silicon dioxide, titania, calcium carbonate.
Described pigment is inorganic pigment.
Described leachable is through repeatedly chloroform and is dissolved to after double leachable is less than 0.005g and obtains.
PE/EVA separating step comprises:
The filter paper being enclosed with the first testing sample is placed in beaker, add chloroform, make chloroform submergence first testing sample, and be placed on heating plate and heat, by chloroformic solution residue in another clean beaker, and be placed in by the first testing sample heating plate dries and weigh, and record is equipped with the mass change value m of the beaker of leachable
1, subsequent operation is with above-mentioned, and each leachable is transferred in same beaker, records each mass change value m
n, until when double leachable quality is all less than or equal to 0.005g, think that PE/EVA system has been separated completely.
Use method of the present invention can obtain EVA content in PE/EVA effectively and accurately, quantitative deviation all lower than 9%, and the quantitative deviation of conventional separation methods to have height to have low.Visible method of the present invention is more general.
Existing EVA major part VA content distribution is wider, the content of the VA of major part business EVA product is all average content, ooze effect owing to exceeding simultaneously, when EVA content lower than 55% time, all EVA in PE/EVA can not dissolve by chloroform, but EVA can dissolve with identical VA content distribution by chloroform.Adopt the method be separated, quantitative deviation is greater than 25% substantially, adopts method of the present invention, and quantitative deviation is less than 9%.
Embodiment
Leachable of the present invention refers to that chloroform dissolves remaining material after canopy film, and solvend refers to the chloroformic solution obtained after chloroform dissolves canopy film.
The analytical approach of functional greenhouse film, comprises the following steps:
There is provided functional greenhouse film, obtain the first testing sample, described first testing sample is made up of PE, EVA;
Use TGA to analyze the first testing sample, obtain a VA content;
PE, EVA in first testing sample is separated, after oven dry, obtains the second testing sample;
Use TGA to analyze the second testing sample, obtain the 2nd VA content;
The content of EVA in PEEVA system is obtained by a VA content, the 2nd VA cubage.
In described PE/EVA, the content of EVA is lower than 55%.
Described functional greenhouse film also comprises pigment and/or filler.
Described filler is one or more in silicon dioxide, titania, calcium carbonate.
Described pigment is inorganic pigment.
Described solvend is through repeatedly chloroform and is dissolved to after double leachable is less than 0.005g and obtains.
Described PE/EVA is separated and adopts apparatus,Soxhlet's to be separated.
The separated and dissolved of PE/EVA co-mixing system:
PE/EVA separating step comprises:
The filter paper being enclosed with the first testing sample is placed in beaker, add chloroform, make chloroform submergence first testing sample, and be placed on heating plate and heat, by chloroformic solution residue in another clean beaker, and be placed in by the first testing sample heating plate dries and weigh, and record is equipped with the mass change value m of the beaker of leachable
1, subsequent operation is with above-mentioned, and each leachable is transferred in same beaker, records each mass change value m
n, until when double leachable quality is all less than or equal to 0.005g, think that PE/EVA system has been separated completely.
According to the different dissolubilities of PE and EVA in chloroform, use chloroform to be separated PE/EVA co-mixing system, concrete operations are as follows:
Get 0.1gPE/EVA blend and send survey TGA, residue canopy film is cut into the flake parcel of 1mm*1mm with filter paper, record mixture weight m0.
The filter paper being enclosed with sample is placed in 100ml beaker, add chloroform to 80ml, make chloroform submergence sample, and be placed on 150 degrees Centigrade plates and heat, be transferred in another clean beaker when chloroformic solution in beaker remains about 30ml, and be placed in equally and heating plate dried heavy, and record is equipped with the mass change value m of the beaker of leachable
1, namely first time leachable quality, subsequent operation is with above-mentioned, and each leachable is transferred in same beaker, records the m of each quality cotton
n, until when double leachable quality is all less than or equal to 0.005g, think that PE/EVA system has been separated completely.Survey TGA is sent by finally obtaining solvend sampling.
The separated and dissolved of PE/EVA co-mixing system also can adopt apparatus,Soxhlet's 5-10 hour to be separated.
According to the decomposition feature of EVA, it is the process of de-acetic acid at 370 degrees centigrade, and remember that former mixed system send the survey de-process of acetic acid weight-loss ratio that TGA obtains to be W1, final solvend send the survey de-process of acetic acid weight-loss ratio that TGA obtains to be W2, then, the mass ratio wt(EVA of EVA in PE/EVA) be:
For the co-mixing system containing pigment or filler, method of the present invention is suitable for too.
Specific embodiment:
Raw material sources:
HDPE, LDPE, LLDPE come from Iranian petrochemical complex.
EVA18-3(VA content 18%), EVA14J4(VA content 14%), EVA18J3(VA content 18%), EVA6J2(VA content 6%), EVA4F2(VA content 4.7%), EVA12J4(VA content 12%), EVA9F2(VA content 9%, actual content 7.6%), EVA K3212(VA content 21%) come from Yanshan Petrochemical.
EVA250(VA content 28%), EVA560(VA content 15%) come from E.I.Du Pont Company.
In order to verify the general applicability of the co-mixing system that the inventive method forms for the EVA of variety classes and different VA content, get after beaker weighs PE and EVA according to the scheme of form below, add 60ml toluene heating for dissolving, stir and toluene evaporate to dryness is obtained PE/EVA co-mixing system.
Get 0.1gPE/EVA blend and send survey TGA, residue canopy film is cut into the flake parcel of 1mm*1mm with filter paper, record mixture weight m0.
The filter paper being enclosed with sample is placed in 100ml beaker, add chloroform to 80ml, make chloroform submergence sample, and be placed on 150 degrees Centigrade plates and heat, be transferred in another clean beaker when chloroformic solution in beaker remains about 30ml, and be placed in equally and heating plate dried heavy, and record is equipped with the mass change value m of the beaker of leachable
1, namely first time leachable quality, subsequent operation is with above-mentioned, and each leachable is transferred in same beaker, records the m of each quality cotton
n, until when double leachable quality is all less than or equal to 0.005g, think that PE/EVA system has been separated completely.
Visible, adopting leachable to carry out calculating the quantitative deviation of the mass percent of EVA in PE/EVA system has very large amplitude, does not have versatility.Especially, when EVA content is lower than 55%, its quantitative deviation is larger.
By finally obtain solvend sampling and former state send survey TGA.Remember that former mixed system send the survey de-process of acetic acid weight-loss ratio that TGA obtains to be W1, final solvend send the survey de-process of acetic acid weight-loss ratio that TGA obtains to be W2, then, and and the mass ratio wt(EVA of EVA in PE/EVA) be:
The data obtained see the following form:
Use method of the present invention can obtain EVA content in PE/EVA effectively and accurately, quantitative deviation all lower than 9%, and the quantitative deviation of conventional separation methods to have height to have low.Visible method of the present invention is more general.
In existing most of EVA, VA content distribution is wider, the content of the VA of major part business EVA product is all average content, simultaneously present inventor has found that the quantitative deviation of conventional separation methods larger reason of floating there occurs to exceed to ooze effect, when EVA content lower than 55% time, all EVA in PE/EVA can not dissolve by chloroform, but ooze effect because exceed, EVA can dissolve with identical VA content distribution by chloroform.Adopt the method be separated, quantitative deviation is greater than 25% substantially, adopts method of the present invention, and quantitative deviation is less than 9%.
Claims (8)
1. the analytical approach of functional greenhouse film, comprises the following steps:
There is provided functional greenhouse film, obtain the first testing sample, described first testing sample is made up of PE, EVA;
Use TGA to analyze the first testing sample, obtain a VA content;
PE, EVA in first testing sample is separated, after oven dry, obtains the second testing sample;
Use TGA to analyze the second testing sample, obtain the 2nd VA content;
The content of EVA in PEEVA system is obtained by a VA content, the 2nd VA cubage.
2. the analytical approach of functional greenhouse film according to claim 1, is characterized in that, in described PE/EVA, the content of EVA is lower than 55%.
3. the analytical approach of functional greenhouse film according to claim 1, is characterized in that, described functional greenhouse film also comprises pigment and/or filler.
4. the analytical approach of functional greenhouse film according to claim 1, is characterized in that, described filler is one or more in silicon dioxide, titania, calcium carbonate.
5. the analytical approach of functional greenhouse film according to claim 1, is characterized in that, described pigment is inorganic pigment.
6. the analytical approach of functional greenhouse film according to claim 1, is characterized in that, described solvend is through repeatedly chloroform and is dissolved to after double leachable is less than 0.005g and obtains.
7. the analytical approach of functional greenhouse film according to claim 1, is characterized in that, described PE/EVA is separated and adopts apparatus,Soxhlet's to be separated.
8. the analytical approach of functional greenhouse film according to claim 1, is characterized in that, the step that described PE/EVA is separated comprises:
The filter paper being enclosed with the first testing sample is placed in beaker, add chloroform, make chloroform submergence first testing sample, and be placed on heating plate and heat, by chloroformic solution residue in another clean beaker, and be placed in by the first testing sample heating plate dries and weigh, and record is equipped with the mass change value m of the beaker of leachable
1, subsequent operation is with above-mentioned, and each leachable is transferred in same beaker, records each mass change value m
n, until when double leachable quality is all less than or equal to 0.005g, think that PE/EVA system has been separated completely.
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| CN201410773574.2A CN104502221A (en) | 2014-12-16 | 2014-12-16 | Method for analyzing functional greenhouse film |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| KR20180138019A (en) * | 2017-06-20 | 2018-12-28 | 주식회사 엘지화학 | Control system and method for ethylene vinyl acetate copolymerization process |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| KR20180138019A (en) * | 2017-06-20 | 2018-12-28 | 주식회사 엘지화학 | Control system and method for ethylene vinyl acetate copolymerization process |
| KR102153474B1 (en) * | 2017-06-20 | 2020-09-08 | 주식회사 엘지화학 | Control system and method for ethylene vinyl acetate copolymerization process |
| US10995171B2 (en) | 2017-06-20 | 2021-05-04 | Lg Chem, Ltd. | System for controlling ethylene vinyl acetate copolymerization process and method of controlling the same |
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Application publication date: 20150408 |