CN104458488A - Analysis method of EVA hot melt adhesive - Google Patents

Analysis method of EVA hot melt adhesive Download PDF

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Publication number
CN104458488A
CN104458488A CN201410774045.4A CN201410774045A CN104458488A CN 104458488 A CN104458488 A CN 104458488A CN 201410774045 A CN201410774045 A CN 201410774045A CN 104458488 A CN104458488 A CN 104458488A
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China
Prior art keywords
eva
melt adhesive
content
testing sample
analytical approach
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CN201410774045.4A
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Chinese (zh)
Inventor
贾梦虹
裴丽娟
吴杰
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Shanghai Microspectrum Chemical Technology Service Co Ltd
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Shanghai Microspectrum Chemical Technology Service Co Ltd
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Priority to CN201410774045.4A priority Critical patent/CN104458488A/en
Publication of CN104458488A publication Critical patent/CN104458488A/en
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  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)

Abstract

The invention relates to an analysis method of content of EVA in an EVA hot melt adhesive. The analysis method comprises the following steps: providing the EVA hot melt adhesive which is composed of PE and EVA to obtain a first sample to be tested; analyzing the first sample to be tested by use of TGA, thereby obtaining the first VA content; dissolving the first sample to be tested in chloroform, separating PE and EVA, calculating the quantity of the dissolved substance and the soluble substance, and drying the soluble substance to obtain a second sample to be tested; analyzing the sample to be tested by use of TGA to obtain the second VA content; calculating the content of the EVA in the PE/EVA system based on the first VA content and the second VA content.

Description

The analytical approach of EVA hot-melt adhesive
Technical field
The present invention relates to analysis field, be specifically related to microgram spectral analysis technology, particularly the analytical approach of EVA hot-melt adhesive.
Background technology
EVA hot-melt adhesive be a kind of do not need solvent, not water content, 100% the polymkeric substance of solid meltability, be solid at normal temperatures, heating and melting becomes to a certain extent and can flow and have the liquid adhesive of certain viscosity, is light brown translucent body or this white after its melting.
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.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 EVA hot-melt adhesive, comprises the following steps:
There is provided EVA hot-melt adhesive, 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 43%.
Described first testing sample 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, may be ooze effect owing to exceeding simultaneously, when EVA content lower than 43% 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
The analytical approach of EVA content in EVA hot-melt adhesive, comprises the following steps:
There is provided EVA hot-melt adhesive, 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 43%.
Described first testing sample 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 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 PE/EVA is separated and adopts apparatus,Soxhlet's to be separated.
For the co-mixing system containing pigment or filler, method of the present invention is suitable for too.
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 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).
 
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.
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 EVA hot-melt adhesive is cut into the flake parcel of 1mm*1mm with filter paper, record mixture weight m 0.
The filter paper being enclosed with the first testing sample is placed in 100ml beaker, add chloroform to 80ml, make chloroform submergence first testing 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 heating plate dries and weigh, 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 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.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:
Get 0.1gPE/EVA blend and send survey TGA, residue EVA hot-melt adhesive is cut into the flake parcel of 1mm*1mm with filter paper, record mixture weight m 0.
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 heating plate dries and weigh, 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 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.
 
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 43%, 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:
In order to reduce error during de-process of acetic acid, choose the terminal of the weightless peak of VA in the first differential curve of TGA data and the PE weightlessness temperature corresponding to peak-to-peak minimum point as de-process of acetic acid.
    
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 43% 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)

  1. The analytical approach of 1.EVA hot melt adhesive, comprises the following steps:
    There is provided EVA hot-melt adhesive, 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. 2. the analytical approach of EVA hot-melt adhesive according to claim 1, is characterized in that, in described PE/EVA, the content of EVA is lower than 43%.
  3. 3. the analytical approach of EVA hot-melt adhesive according to claim 1, is characterized in that, described first testing sample also comprises pigment and/or filler.
  4. 4. the analytical approach of EVA hot-melt adhesive according to claim 1, is characterized in that, described filler is one or more in silicon dioxide, titania, calcium carbonate.
  5. 5. the analytical approach of EVA hot-melt adhesive according to claim 1, is characterized in that, described pigment is inorganic pigment.
  6. 6. the analytical approach of EVA hot-melt adhesive 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. 7. the analytical approach of EVA hot-melt adhesive 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 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.
  8. 8. the analytical approach of EVA hot-melt adhesive according to claim 1, is characterized in that, described PE, EVA are separated and adopt apparatus,Soxhlet's to be separated.
CN201410774045.4A 2014-12-16 2014-12-16 Analysis method of EVA hot melt adhesive Pending CN104458488A (en)

Priority Applications (1)

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Citations (3)

* Cited by examiner, † Cited by third party
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
CN102967524A (en) * 2012-12-04 2013-03-13 韩华新能源（启东）有限公司 Ethylene vinyl acetate (EVA) crosslinking degree testing method

Patent Citations (3)

* Cited by examiner, † Cited by third party
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
CN102967524A (en) * 2012-12-04 2013-03-13 韩华新能源（启东）有限公司 Ethylene vinyl acetate (EVA) crosslinking degree testing method

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
刘光耀等: "增强热收缩制品表面基材改性PE的热稳定性", 《现代塑料加工应用》 *
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》 *
詹达利: "《热塑性聚合物》", 31 July 2008 *

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