CN104406883A - Analysis method of PE and EVA blending system - Google Patents
Analysis method of PE and EVA blending system Download PDFInfo
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- CN104406883A CN104406883A CN201410774081.0A CN201410774081A CN104406883A CN 104406883 A CN104406883 A CN 104406883A CN 201410774081 A CN201410774081 A CN 201410774081A CN 104406883 A CN104406883 A CN 104406883A
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Abstract
The invention relates to an analysis method of a PE and EVA blending system. The method comprises the following steps: providing a PE/EVA blending polymer consisting of PE and EVA so as to obtain a first sample to be tested; analyzing the first sample to be tested by using TGA so as to obtain a first VA content; dissolving the first sample to be tested with chloroform, separating PE/EVA, and calculating so as to obtain the amount of dissolved substances and soluble substances, and obtaining a second sample to be tested after drying the soluble substances; analyzing the second sample to be tested by using TGA so as to obtain a second VA content; obtaining an EVA content in the PE and EVA system by calculating the first VA content and the second VA content.
Description
Technical field
The present invention relates to analysis field, be specifically related to microgram spectral analysis technology, particularly the analytical approach of PE, EVA co-mixing system.
Background technology
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 PE, EVA co-mixing system, comprises the following steps:
There is provided PE, EVA blend, 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;
Be separated by PE, EVA in first testing sample, solvend obtains the second testing sample after drying;
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 50%.
Described PE/EVA blend also comprises pigment and/or filler.
Described filler is one or more in silicon dioxide, titania, calcium carbonate.
Described pigment is inorganic pigment.
Described 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 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.
Described leachable is through repeatedly chloroform and is dissolved to after double leachable is less than 0.005g and obtains.
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 50% 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 PE/EVA blend, and solvend refers to the chloroformic solution obtained after chloroform dissolves PE/EVA blend.
The analytical approach of EVA content in PE, EVA blend, comprises the following steps:
There is provided PE, EVA blend, 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;
Be separated by PE, EVA in first testing sample, solvend obtains the second testing sample after drying;
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 50%.
Described PE/EVA blend 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:
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 PE/EVA blend 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.
Described 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 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 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.(for the component containing organic and/or inorganic materials, toluene can be used to dissolve and inorganic material be separated, also can not be separated, directly use method of the present invention to analyze)
Get 0.1gPE/EVA blend and send survey TGA, residue PE/EVA blend 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 50%, 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 50% 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%.
Claims (8)
- The analytical approach of 1.PE, EVA co-mixing system, comprises the following steps:The analytical approach of EVA content in PE, EVA blend, comprises the following steps:There is provided PE, EVA blend, 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;Be separated by PE, EVA in first testing sample, solvend obtains the second testing sample after drying;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 PE, EVA co-mixing system according to claim 1, is characterized in that, in described PE/EVA, the content of EVA is lower than 50%.
- 3. the analytical approach of PE, EVA co-mixing system according to claim 1, is characterized in that, described PE/EVA blend also comprises pigment and/or filler.
- 4. the analytical approach of PE, EVA co-mixing system 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 PE, EVA co-mixing system according to claim 1, is characterized in that, described pigment is inorganic pigment.
- 6. the analytical approach of PE, EVA co-mixing system 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 PE, EVA co-mixing system 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 PE, EVA co-mixing system according to claim 1, is characterized in that, described 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 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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| CN201410774081.0A CN104406883A (en) | 2014-12-16 | 2014-12-16 | Analysis method of PE and EVA blending system |
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| CN201410774081.0A CN104406883A (en) | 2014-12-16 | 2014-12-16 | Analysis method of PE and EVA blending system |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102269681A (en) * | 2011-04-30 | 2011-12-07 | 常州天合光能有限公司 | Method for measuring vinyl acetate (VA) content in ethylene vinyl acetate (EVA) |
| WO2012160279A1 (en) * | 2011-05-26 | 2012-11-29 | Arkema France | Method for characterizing an ethylene and vinyl acetate copolymer |
| CN103207177A (en) * | 2012-01-16 | 2013-07-17 | 阿特斯(中国)投资有限公司 | Test method for content of crosslinking agent in EVA |
| CN103709296A (en) * | 2013-12-30 | 2014-04-09 | 上海微谱化工技术服务有限公司 | Method for extracting pure ethylene-ethylene vinyl-acetate copolymer |
-
2014
- 2014-12-16 CN CN201410774081.0A patent/CN104406883A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102269681A (en) * | 2011-04-30 | 2011-12-07 | 常州天合光能有限公司 | Method for measuring vinyl acetate (VA) content in ethylene vinyl acetate (EVA) |
| WO2012160279A1 (en) * | 2011-05-26 | 2012-11-29 | Arkema France | Method for characterizing an ethylene and vinyl acetate copolymer |
| CN103207177A (en) * | 2012-01-16 | 2013-07-17 | 阿特斯(中国)投资有限公司 | Test method for content of crosslinking agent in EVA |
| CN103709296A (en) * | 2013-12-30 | 2014-04-09 | 上海微谱化工技术服务有限公司 | Method for extracting pure ethylene-ethylene vinyl-acetate copolymer |
Non-Patent Citations (4)
| Title |
|---|
| C. CHEN ET AL.: "Processability and Thermal Properties of Blends of High Density Polyethylene, Poly(Ethylene Terephthalate), and Ethyl Vinyl Acetate Compatibilizer", 《POLYMER ENGINEERING AND SCIENCE》 * |
| J. REYES-LABARTA ET AL.: "DSC and TGA study of the transitions involved in the thermal treatment of binary mixtures of PE and EVA copolymer with a crosslinking agent", 《POLYMER》 * |
| 史旭明 等: "醋酸乙烯酯含量测定方法及其评价", 《塑料》 * |
| 吕瑞瑞 等: "太阳能封装胶膜EVA中Va含量的测定", 《合成材料老化与应用》 * |
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Application publication date: 20150311 |