CN109870558A - A kind of discrimination method of polycarbonate plastic reworked material - Google Patents
A kind of discrimination method of polycarbonate plastic reworked material Download PDFInfo
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- CN109870558A CN109870558A CN201711264311.9A CN201711264311A CN109870558A CN 109870558 A CN109870558 A CN 109870558A CN 201711264311 A CN201711264311 A CN 201711264311A CN 109870558 A CN109870558 A CN 109870558A
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Abstract
The invention discloses a kind of discrimination method of polycarbonate plastic reworked material, include the following steps: that (1) takes sample, determines the sample for polycarbonate plastic；(2) sample is identified using at least three kinds of methods in dissolubility analysis, infrared spectrum analysis, head space gas chromatography, electron microscope analysis, element distribution analysis；According to it is above-mentioned at least three kinds of methods are identified when, at least determine to contain polycarbonate plastic reworked material in sample there are three types of method, then determine in sample containing polycarbonate plastic reworked material.The discrimination method of polycarbonate plastic reworked material of the present invention, as a result accurately, method have universality；Even when the comparision contents of reworked material are few, it can also identify whether contain reworked material using the method for the invention.
Description
Technical field
The present invention relates to a kind of discrimination method of reworked material, especially a kind of identification side of polycarbonate plastic reworked material
Method.
Background technique
Since plastics kind is numerous, and appearance character is extremely similar after product is made in it, and consumer is difficult directly to distinguish
Product is made of what material on earth, to affect the right of consumer.A few years ago, Foochow customs has successfully cracked case value together
More than 100 ten thousand dollars of the smuggling major case that the qualified product transaction for expecting that grain serves as initial configuration is reproduced using plastics recovery.It is closed in case
The technology of key is to differentiate resin raw material and reworked material.Since case-involving the appearance of a sample particle is uniform, size is regular, color one
It causes, substantially colorless difference, can not determine whether this blending resin is in reworked material by conventional means.Currently, not having both at home and abroad
For the specificity analysis method of reworked material, therefore more difficult judge whether it is regenerated granules.
Identify that the analysis task of regenerated plastics has great difficulty, reason is from these aspects: firstly, research object
It is sufficiently complex；Plastics itself are a mixtures, are made of the macromolecule and chemical assistant that are distributed with certain molecular weight；Its
Secondary, research object has high similarity；Although regenerated plastics have certain difference compared to virgin material, but their still unusual phases
Seemingly；Again, the characteristic substance of research object and concentration are uncertain；After adding reworked material in virgin material, it is different from reworked material new
The otherness substance of material is diluted.Accordingly, it is intended to identify that the finished product for adding reworked material both requires to establish highly sensitive analysis side
Method also requires to find the limit value on simultaneously Scientific Establishment statistical significance.
There are the identification method of part research original shape plastic resin and regenerated plastics resin and reworked material, SN in the country
Water in the standards such as 3095-2012, SNT 2740-2010,102175637 A of CN and patent disclosure import regenerated plastics raw material
Point, the separation of the pollutants such as initial product residue, multiphase plastics, metal, paper, glass, binder and sawdust and identification method with
And identify the method for doped portion regenerated plastics in Key works Drug packing near infrared technology.Also there are a small amount of document in foreign countries [such as
Karlsson S.Recycled Polylenfins.MaterialProperties and means for Queality
Determination [J] .Adv.Polym.Sci.2004 (169): 201-230] to the plastics and new grain of mechanical recycling and reusing
The plastics of material preparation carry out difference research.The index of differentiation is mainly that regenerated plastics have degradation oxidative phenomena, residual low molecule
Compound molecular weight (catabolite of material or host, additive, pollutant), hybrid other polymers.But in these marks
It in the discrimination method that quasi-, document and patent provide, all has the following disadvantages: the first, from the difference of packaging and appearance very
Difficulty determines new resin and regenerated plastics, more crucial problem be experienced doping person often by the preferable reworked material of quality by
Certain ratio is added in virgin material, reflects reworked material and the lesser difference of virgin material script in finished product after dilution smaller；
The second, by distinguishing original shape resin and regenerated plastics in technical indicator difference and environmentally friendly risk difference, reworked material is logical
Cross the addition and the modified technical performance for fully achieving original shape resin of auxiliary agent；Third, infrared analysis are to regeneration
The inspection fixed sum data analytic process of material are as follows: in atlas of near infrared spectra, no matter raw material or reworked material, characteristic peak frequency values phase
Together, only in peak type size, go out peak intensity and have a different, however peak type size, go out peak intensity itself and influenced to increase by operation,
To can not fundamentally distinguish raw material and reworked material.It can be seen that the above method is generally all fairly simple, rough, Zhi Nengzuo
For a kind of householder method, analyzing and identifying for reworked material can not accurately be carried out.
Currently, existing method is all less accurate for distinguishing raw material, modified materials and reworked material aspect.Chemical analysis
Method is frequently used for the analysis of small constituent content, always titled with accurate famous.Because of reworked material and raw material, modified materials component
Complexity, various structures, so the combination of several method may be needed to accurately distinguish raw material, modified materials and reworked material.
Summary of the invention
Based on this, a kind of polycarbonate modeling is provided it is an object of the invention to overcome above-mentioned the deficiencies in the prior art place
Expect the discrimination method of reworked material.
To achieve the above object, a kind of the technical solution used in the present invention are as follows: identification of polycarbonate plastic reworked material
Method includes the following steps:
(1) sample is taken, determines the sample for polycarbonate plastic；
(2) by sample using dissolubility analysis, infrared spectrum analysis, head space gas chromatography, electron microscope analysis, element point
At least three kinds of methods in cloth analysis are identified；
When being identified using dissolubility analysis method, if sample cannot be complete in o-dichlorohenzene solvent or tetrahydrofuran solvent
Fully dissolved has muddiness, then contains polycarbonate plastic reworked material in sample；
When being identified using infrared spectrum analysis, compared with the polycarbonate plastic raw material infrared spectrum of standard, if
The infrared spectrum of sample has obvious miscellaneous peak, then contains polycarbonate plastic reworked material in sample；
When being identified using head space gas chromatography method, if the appearance time of sample chromatogram figure is after 14min and peak
Number is not less than 7, then contains polycarbonate plastic reworked material in sample；
When being identified using electron microscope analysis method, if sample surfaces have scratch and pollution or sample power spectrum in electron microscope analysis
The element in element ratio polycarbonate plastic raw material energy spectrum analysis in analysis is more, then contains polycarbonate plastic again in sample
Raw material；
When identifying using element distribution analysis method, if element species are greater than 15 kinds in sample, poly- carbon is contained in sample
Acid esters recycled plastics polymers；
According to it is above-mentioned at least three kinds of methods are identified when, at least there are three types of method determine sample in contain polycarbonate
Recycled plastics polymers then determine to contain polycarbonate plastic reworked material in sample.
Preferably, in the step (1), if whether it is polycarbonate plastic that sample is uncertain, sample is taken to carry out infrared light
Test analysis is composed, whether confirmatory sample is polycarbonate plastic.
The present invention is when using the type of infrared spectrum analysis material, the method for examination of infrared spectrum are as follows: cut sample
It is wrapped up at the particle of 4mm*4mm, and with polytetrafluoroethylene film, is hot pressed under 100 DEG C -135 DEG C, the pressure of 2KN-10KN
Thin slice is put into infrared absorption instrument by thin slice, measure its 400-1-4000-1The infrared examination of wave-number range, resolution ratio 4cm-1, sweep
It retouches number 32 times.
Preferably, in the dissolubility analysis of the step (2), sample is placed in 180 DEG C -200 DEG C of o-dichlorohenzene solvent
In, 0.5~2.5h is heated, if sample cannot be completely dissolved, have muddiness, contains polycarbonate plastic reworked material in sample.
Preferably, in the dissolubility analysis of the step (2), sample is placed in 60 DEG C -80 DEG C of tetrahydrofuran solvent,
It is observed after 0.5h-1.5h, if sample cannot be completely dissolved, have muddiness, contains polycarbonate plastic reworked material in sample.
It can identify whether contain reworked material using dissolubility of the plastics in different organic solvents.Since reworked material recycles
During recycling, it is difficult to reach higher purity, can more or less there is a little impurity, lead to reworked material and raw material and modification
Dissolution sex differernce is had between material to occur.Tetrahydrofuran sample being placed in the o-dichlorohenzene solvent under high temperature or under high temperature is molten
In agent, it can be completely dissolved in solution using primary resin, and reworked material in removal process because may introduce impurity or process
Whether the characteristic that repeatedly processing generates some carbonization insoluble matters contains reworked material to identify.
Preferably, in the step (1), the condition of the head space gas chromatography are as follows: by sample at 100 DEG C -150 DEG C
Enter in gas-chromatography after lower heating 1-8h, then in 40 DEG C -60 DEG C stable 2.5min-5min, then with 10K/min-12K/min
Rate be warming up to 180 DEG C -220 DEG C, last stable 3min-5min at the final temperature.
Headspace gas chromatography (HS-GC) is a kind of joint operation technology, and principle is by waving in liquid or solid sample
Hair property component is introduced directly into gas chromatograph and is separated and identified.The application of headspace gas chromatography is often superfluous in order to exempt
Long cumbersome pretreatment process, and organic solvent is avoided to bring impurity effect analysis etc. into, thus Headspace-Gas Chromatography with
Its simple and practical advantage organic residual solvent monitoring, food, forensic science, petrochemical industry, packaging in environmental monitoring, drug
The fields such as material, coating and wine-making industry analysis are widely used.As mirror due to the high sensitivity of its test method
Other raw material, modified materials, the important means of reworked material.
Preferably, in the step (1), the Elemental redistribution is analyzed using ICP-OES test.
By sample after strong acid, oxidizing species or micro-wave digestion, the full elemental analysis function in ICP-OES is utilized
Can, elemental analysis is carried out to the sample after resolution.Often constituent content information is single in raw material, only the elements such as C, N, O, H, then
Different element informations can be usually had more in raw material than primary resin, such as has more iron, manganese, calcium impurity element, can be identified again with this
The presence of raw material.
Preferably, in the step (1), when being identified using infrared spectrum analysis, the method for infrared spectrum analysis are as follows:
It takes the raw material of phase homogenous quantities with to test sample, is dissolved in the solvent of same volume, obtain starting material solution and to test sample solution, divide
Do not take the starting material solution of same volume and to test sample solution drop in KBr tabletting, FT-IR test carried out after drying, obtain to
The infrared spectrum of test sample and the infrared spectrum of raw material will carry out pair to the infrared spectrum of the infrared spectrum of test sample and raw material
Than obtaining to whether contain reworked material in test sample.
Compared with the existing technology, the invention has the benefit that
(1) combination for using distinct methods, identifies in sample whether contain reworked material, as a result accurately, convincingness is strong；
(2) certain theoretical basis is established for reworked material identification system；
(3) using the combination of a variety of discrimination methods, method has universality；Even when the comparision contents of reworked material are few
When, it can also identify whether contain reworked material using the method for the invention.
Detailed description of the invention
Fig. 1 is a kind of flow chart of polycarbonate plastic reworked material discrimination method of the present invention；
Fig. 2 is that sample is dissolved in the solution state figure after o-dichlorohenzene solvent solution in the embodiment of the present invention 1；
Fig. 3 is the infrared spectrum of sample in the embodiment of the present invention 1；
Fig. 4 is the headspace gas chromatography figure of sample in the embodiment of the present invention 1.
Fig. 5 is that sample is dissolved in the solution state figure after tetrahydrofuran solution in the embodiment of the present invention 1；
Fig. 6 is the electron microscope analysis figure of polycarbonate plastic raw material；
Fig. 7 is the electron microscope analysis figure of sample to be tested in the embodiment of the present invention 2.
Specific embodiment
To better illustrate the object, technical solutions and advantages of the present invention, below in conjunction with the drawings and specific embodiments pair
The present invention is described further.
Embodiment 1
A kind of embodiment of polycarbonate plastic reworked material discrimination method of the present invention, an existing polycarbonate plastic is not
Know sample, judge whether it contains polycarbonate regenerated material, analysis method is as follows:
(1) dissolubility is analyzed: being used o-dichlorobenzene solution, at 190 DEG C, is heated 1.5h, sample is dissolved.By 1.5h's
After heating for dissolving, under high temperature, solution is still muddy (as shown in Figure 2), contains polycarbonate plastic reworked material in judgement sample；
(2) infrared spectrum analysis: will dissolve the solution after polycarbonate sample, take 5ul drop in KBr tabletting, and 70 DEG C
0.5h is toasted in baking oven, tests infrared spectrum, as shown in figure 3, the polycarbonate raw material spectrogram with standard compares, there is miscellaneous peak,
But principal character peak is consistent, confirms that this is polycarbonate sample, contains polycarbonate plastic reworked material；
(3) head space gas chromatography: weighing the sample of 1.2g in ml headspace bottle, and sample is heated under the conditions of 120 DEG C
It enters in headspace gas chromatography and is analyzed after 4h, then in 50 DEG C of stable 3min, be then warming up to the rate of 12K/min
200 DEG C, finally stablize 4min at 200 DEG C of final temperature, identifies the type and content of the volatile materials of sample, spectrogram is as schemed
Shown in 4, if the chromatogram appearance time of sample terminates before 14min and the number at peak is less than 7, which may be PC
Raw material；If the chromatogram appearance time of the sample terminates after 14min and the number at peak is more than or equal to 7, the material
It is likely to containing reworked material.From attached drawing 4 as can be seen that appearance time still has peak appearance when being greater than 14min, and the number at peak is greater than
7, judge that this unknown material contains polycarbonate plastic reworked material.
(4) element distribution analysis (being tested using ICP-OES): test condition: micro-wave digestion, constant volume 50ml,
Carry out full elemental analysis: the results are shown in Table 1:
The ICP-OES full elemental analysis result of 1 polycarbonate sample of table
| Element term | As a result unit | As a result |
| P | ppm | 297 |
| Pb | ppm | 7.5 |
| Cr | ppm | 3.2 |
| Ti | ppm | 40.6 |
| Mg | ppm | 35.9 |
| Sn | ppm | 67.5 |
| Ba | ppm | 8.9 |
| K | ppm | 60.4 |
| Pe | ppm | 57.7 |
| Sb | ppm | 30.7 |
| Al | ppm | 55 |
| Ca | ppm | 361.4 |
| B | ppm | 6.9 |
| Cu | ppm | 19.6 |
| Mn | ppm | 4 |
| Zn | ppm | 21.6 |
| Si | ppm | 1780.6 |
| Na | ppm | 74.4 |
It is shown from the ICP-OES test result in table 1, element species are more than 15 kinds in the sample, contain in judgement sample
Polycarbonate plastic reworked material.
To sum up: the mirror tested in conjunction with dissolubility analysis, infrared spectrum analysis, head space gas chromatography and ICP-OES
Not as a result, can qualitatively judge this unknown polycarbonate sample contains polycarbonate plastic reworked material.
Embodiment 2
A kind of embodiment of polycarbonate plastic reworked material discrimination method of the present invention, an existing polycarbonate plastic is not
Know sample, judge whether it contains polycarbonate regenerated material, analysis method is as follows:
(1) dissolubility is analyzed: sample being placed in 70 DEG C of tetrahydrofuran solvent, is observed after 1h, sample cannot be complete
Fully dissolved has muddy (as shown in Figure 5), and polycarbonate plastic reworked material is contained in judgement sample.
(2) head space gas chromatography: weighing the sample of 1.2g in ml headspace bottle, and sample is heated under the conditions of 120 DEG C
It enters in headspace gas chromatography and is analyzed after 4h, then in 50 DEG C of stable 3min, be then warming up to the rate of 12K/min
200 DEG C, finally stablize 4min at 200 DEG C of final temperature, gas-chromatography peak number and appearance time, peak area are as shown in table 2:
2 headspace gas chromatography peak number of table and appearance time, peak area
| Sample to be tested goes out peak number | Time | Peak area |
| 1 | 2.113 | 10.9 |
| 2 | 2.77 | 9 |
| 3 | 3.385 | 3 |
| 4 | 3.764 | 12.4 |
| 5 | 4.409 | 4.1 |
| 6 | 4.852 | 4.7 |
| 7 | 6.546 | 2.7 |
| 8 | 7.307 | 16.2 |
| 9 | 11.431 | 2.9 |
| 10 | 14.136 | 1.8 |
| 11 | 15.703 | 4.6 |
From table 2 it can be seen that the appearance time in sample in headspace gas chromatography spectrogram is greater than 14min, and quantity is more than 7
It is a, contain polycarbonate plastic reworked material.
(3) electron microscope analysis (SEM-EDS test): after raw material and sample are carried out lossless pre-treatment respectively, it is placed in electricity
It is observed on the workbench of mirror sample, such as attached drawing 6 (raw material), the surface no significant difference of attached drawing 7 (sample to be tested).
The characteristic portion for choosing raw material and sample to be tested respectively, carries out energy spectrum analysis, raw material energy spectrum analysis such as 3 institute of table
Show, the energy spectrum analysis of sample to be tested is as shown in table 4:
3 raw material sample energy spectrum analysis of table
The EDAX results of 4 sample to be tested of table
| Elt. | Line | Error | Atomic | Conc | Units | MDL | |
| 2-sig | % | 3-sig | |||||
| C | Ka | 6.798 | 66.881 | 57.957 | Wt.% | 0.216 | |
| O | Ka | 3.433 | 30.999 | 35.783 | Wt.% | 0.653 | |
| Al | Ka | 1.866 | 0.446 | 0.869 | Wt.% | 0.161 | |
| Si | Ka | 2.139 | 0.69 | 1.398 | Wt.% | 0.138 | |
| Ca | Ka | 1.259 | 0.216 | 0.624 | Wt.% | 0.107 | |
| Fe | Ka | 0.772 | 0.193 | 0.777 | Wt.% | 0 | |
| Ni | Ka | 0.562 | 0.128 | 0.542 | Wt.% | 0 | |
| Cu | Ka | 0.935 | 0.447 | 2.05 | Wt.% | 0 | |
| 100 | 100 | Wt.% | Total |
It is much more many than in raw material to can be seen that the element species in sample to be tested from the data in table 3, table 4, therefore sentences
Determine to contain polycarbonate plastic reworked material in sample to be tested.
To sum up: in conjunction with dissolubility analysis, head space gas chromatography, electron microscope analysis (SEM-EDS test) identification result,
This unknown sample can be qualitatively judged and contain polycarbonate plastic reworked material.
Embodiment 3
The present embodiment verifies the judging standard of head space gas chromatography, is respectively set 5 without containing reworked material
Polycarbonate sample, respectively 1~No. 5 sample；5 samples containing reworked material, respectively 6~No. 10 samples are set, point
It carry out head space gas chromatography: weighing the sample of 1.2g in ml headspace bottle, it is laggard that sample is heated to 4h under the conditions of 120 DEG C
Enter and analyzed into headspace gas chromatography, then in 50 DEG C of stable 3min, is then warming up to 200 DEG C with the rate of 12K/min, most
Stablize 4min at 200 DEG C of final temperature afterwards, data are as shown in table 5:
5 1~No. 10 sample headspace gas chromatographic analysis data of table
As can be seen from Table 5, No. 1-No. 5 without containing reworked material polycarbonate sample appearance time all 14min it
Before, and peak number amount is both less than 7；The appearance time of No. 6-No. 10 polycarbonate samples containing reworked material mostly after 14min, and
Peak number amount is greater than 7.This is consistent with the standard of perfection of head space gas chromatography in the present invention.
Finally, it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention rather than protects to the present invention
The limitation of range is protected, although the invention is described in detail with reference to the preferred embodiments, those skilled in the art should
Understand, it can be with modification or equivalent replacement of the technical solution of the present invention are made, without departing from the essence of technical solution of the present invention
And range.
Claims (7)
1. a kind of discrimination method of polycarbonate plastic reworked material, which comprises the steps of:
(1) sample is taken, determines the sample for polycarbonate plastic；
(2) by sample using dissolubility analysis, infrared spectrum analysis, head space gas chromatography, electron microscope analysis, Elemental redistribution point
At least three kinds of methods in analysis are identified；
When being identified using dissolubility analysis method, if sample cannot be completely molten in o-dichlorohenzene solvent or tetrahydrofuran solvent
It solves, have muddiness, then contain polycarbonate plastic reworked material in sample；
When being identified using infrared spectrum analysis, compared with the polycarbonate plastic raw material infrared spectrum of standard, if sample
Infrared spectrum have obvious miscellaneous peak, then in sample contain polycarbonate plastic reworked material；
When being identified using head space gas chromatography method, if the appearance time of sample chromatogram figure is after 14min and the number at peak
Not less than 7, then contain polycarbonate plastic reworked material in sample；
When being identified using electron microscope analysis method, if sample surfaces have scratch and pollution or sample energy spectrum analysis in electron microscope analysis
In element ratio polycarbonate plastic raw material energy spectrum analysis in element it is more, then in sample containing polycarbonate plastic regenerate
Material；
When identifying using element distribution analysis method, if element species are greater than 15 kinds in sample, polycarbonate is contained in sample
Recycled plastics polymers；
According to it is above-mentioned at least three kinds of methods are identified when, at least there are three types of method determine sample in contain polycarbonate plastic
Reworked material then determines to contain polycarbonate plastic reworked material in sample.
2. the discrimination method of polycarbonate plastic reworked material as described in claim 1, which is characterized in that in the step (1),
If whether it is polycarbonate plastic that sample is uncertain, sample is taken to carry out examination of infrared spectrum analysis, whether confirmatory sample is poly- carbon
Acid esters plastics.
3. the discrimination method of polycarbonate plastic reworked material as described in claim 1, which is characterized in that the step (2)
In dissolubility analysis, sample is placed in 180 DEG C -200 DEG C of o-dichlorohenzene solvent, 0.5~2.5h is heated, if sample cannot be complete
Fully dissolved has muddiness, then contains polycarbonate plastic reworked material in sample.
4. the discrimination method of polycarbonate plastic reworked material as described in claim 1, which is characterized in that the step (2)
In dissolubility analysis, sample is placed in 60 DEG C -80 DEG C of tetrahydrofuran solvent, is observed after 0.5h-1.5h, if sample is not
It can be completely dissolved, have muddiness, then contain polycarbonate plastic reworked material in sample.
5. the discrimination method of polycarbonate plastic reworked material as described in claim 1, which is characterized in that in the step (2),
The condition of the head space gas chromatography are as follows: enter in gas-chromatography after sample to be heated to 1-8h at 100 DEG C -150 DEG C, then
In 40 DEG C -60 DEG C stable 2.5min-5min, 180 DEG C -220 DEG C then are warming up to the rate of 10K/min-12K/min, finally
Stable 3min-5min at the final temperature.
6. the discrimination method of polycarbonate plastic reworked material as described in claim 1, which is characterized in that in the step (2),
The Elemental redistribution is analyzed using ICP-OES test.
7. the discrimination method of polycarbonate plastic reworked material as described in claim 1, which is characterized in that in the step (2),
When being identified using infrared spectrum analysis, the method for infrared spectrum analysis are as follows: take the raw material of phase homogenous quantities with to test sample, it is molten
In the solvent of same volume, obtain starting material solution and to test sample solution, take respectively same volume starting material solution and to
Test sample solution drop carries out infrared spectrum test in KBr tabletting after drying, obtain to test sample infrared spectrum and raw material it is red
Outer spectrogram will be compared to the infrared spectrum of test sample and the infrared spectrum of raw material, be obtained to whether contain regeneration in test sample
Material.
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| CN115616204A (en) * | 2022-12-21 | 2023-01-17 | 金发科技股份有限公司 | Method and system for identifying polyethylene terephthalate reclaimed materials |
| CN115629200A (en) * | 2022-12-21 | 2023-01-20 | 国高材高分子材料产业创新中心有限公司 | Method for identifying polyamide reclaimed material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115616204A (en) * | 2022-12-21 | 2023-01-17 | 金发科技股份有限公司 | Method and system for identifying polyethylene terephthalate reclaimed materials |
| CN115629200A (en) * | 2022-12-21 | 2023-01-20 | 国高材高分子材料产业创新中心有限公司 | Method for identifying polyamide reclaimed material |
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Application publication date: 20190611 |