CN109870559A - A kind of discrimination method of ABS plastic reworked material - Google Patents
A kind of discrimination method of ABS plastic reworked material Download PDFInfo
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Abstract
The invention discloses a kind of discrimination method of ABS plastic reworked material, include the following steps: that (1) takes sample, determines the sample for ABS 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 ABS plastic reworked material in sample there are three types of method, then determine in sample containing ABS plastic reworked material.The discrimination method of ABS 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 discrimination method of ABS plastic reworked material.
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, conventional means can not determine whether this blending resin is in reworked material.Currently, not being directed to both at home and abroad
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 the finished product for adding reworked material, both require 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.Material Properties 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 ABS plastic is provided it is an object of the invention to overcome in place of above-mentioned the deficiencies in the prior art again
The discrimination method of raw material.
To achieve the above object, the technical solution used in the present invention are as follows: a kind of discrimination method of ABS plastic reworked material,
Include the following steps:
(1) sample is taken, determines the sample for ABS 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 completely dissolved in chloroformic solution and particulate matter is obvious,
Then contain ABS plastic reworked material in sample, wherein the solvent is chloroformic solution, acetone or methyl ethyl ketone；
When being identified using infrared spectroscopy (IR) analysis method, compared with the ABS plastic raw material infrared spectrum of standard, if sample
The infrared spectrum of product has obvious miscellaneous peak, then contains ABS plastic reworked material in sample；
When being identified using headspace gas chromatography (HS-GC) analysis method, if the appearance time of sample chromatogram figure is in 14min
Afterwards and the number at peak is greater than 15, then contains ABS plastic reworked material in sample；
When being identified using electron microscope analysis (SEM-EDS) method, if sample surfaces have scratch and pollution in electron microscope analysis, or
The element in element ratio ABS plastic raw material energy spectrum analysis in sample energy spectrum analysis is more, then regenerates in sample containing ABS plastic
Material；
When being identified using element distribution analysis method, if element species are greater than 15 kinds in sample, moulded in sample containing ABS
Expect reworked material；
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 ABS plastic
Reworked material then determines to contain ABS plastic reworked material in sample.
Preferably, in the step (1), if whether it is ABS plastic that sample is uncertain, sample is taken to carry out examination of infrared spectrum
Analysis, whether confirmatory sample is ABS 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, the step (2) dissolubility analysis in, sample is placed in chloroformic solution, using ultrasonic dissolution 8~
12h contains ABS plastic reworked material if sample cannot be completely dissolved and particulate matter is obvious in sample.Selecting chloroformic solution is
Because chloroform under the conditions described above dissolves ABS raw material.
Preferably, in the dissolubility analysis of the step (2), sample is placed in acetone, using extraction device, is heated to
60-80 DEG C, 0.5-1.5h is dissolved, if sample cannot be completely dissolved and particulate matter is obvious, is regenerated in sample containing ABS plastic
Material.
Preferably, in the dissolubility analysis of the step (2), sample is placed in methyl ethyl ketone, extraction device, heating are used
To 80-90 DEG C, 0.5-1.5h is dissolved, if sample cannot be completely dissolved and particulate matter is obvious, in sample again containing ABS plastic
Raw material.
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.Sample is placed in solvent, can be preferably dissolved in solution using primary resin, and again
Raw material in removal process because may introduce impurity or generate the characteristic of some carbonization insoluble matters by repeatedly processing to reflect
Whether reworked material is not contained.
Preferably, in the step (2), 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 is a kind of joint operation technology, and principle is by the volatile component in liquid or solid sample
Gas chromatograph is introduced directly into be separated and identified.The application of headspace gas chromatography is often in order to exempt redundant and complicated
Pretreatment process, and avoid organic solvent from bringing impurity effect analysis etc. into, therefore Headspace-Gas Chromatography is simple real with it
With the advantages of in environmental monitoring, drug organic residual solvent monitoring, food, forensic science, petrochemical industry, packaging material, painting
The fields such as material and wine-making industry analysis are widely used.As identification former material due to the high sensitivity of its test method
Material, modified materials, the important means of reworked material.
Preferably, in the step (2), 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 impurity element, reworked material can be identified with this
Presence.
Preferably, in the step (2), 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
The starting material solution of same volume is not taken and is dripped to test sample solution in KBr tabletting, and examination of infrared spectrum is carried out after drying, is obtained
To the infrared spectrum of test sample and the infrared spectrum of raw material, will be carried 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 ABS plastic reworked material discrimination method of the present invention；
Fig. 2 is the infrared spectrum of sample in the embodiment of the present invention 1；
Fig. 3 is the headspace gas chromatography figure of sample in the embodiment of the present invention 1；
Fig. 4 is that sample is dissolved in the solution after chloroformic solution in the embodiment of the present invention 2；
Fig. 5 is the electron microscope analysis figure of ABS plastic raw material；
Fig. 6 is the electron microscope analysis figure of sample to be tested in the embodiment of the present invention 1.
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 ABS plastic reworked material discrimination method of the present invention, existing ABS plastic unknown sample, sentences
Breaking, whether it contains ABS reworked material, and analysis method is as follows:
(1) infrared spectrum analysis: will dissolve the solution after unknown ABS sample, take 5ul drop in KBr tabletting, 70 DEG C of bakings
0.5h is toasted in case, tests its infrared spectrum, is compared with the ABS raw material infrared spectrum of standard, as shown in Fig. 2, can by Fig. 2
See, compared with the ABS infrared spectrum of standard, the infrared spectrum of sample has uncommon miscellaneous peak, therefore, it is determined that the sample contains ABS
Recycled plastics polymers.
(2) head space gas chromatography: weighing the sample of 1.2g in ml headspace bottle, and it is laggard that 4h is heated under the conditions of 120 DEG C
Enter and analyzed into gas-chromatography, then in 50 DEG C of stable 3min, is then warming up to 200 DEG C with the rate of 12K/min, finally exists
Stablize 4min at 200 DEG C of final temperature, the headspace gas chromatography figure of sample is as shown in figure 3, from attached drawing 3 as can be seen that the sample
Total peak number is greater than 15, and the still appearance after 14min, therefore, it is determined that the sample contains ABS plastic reworked material.
(3) 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 table 1ABS sample
| Element term | As a result unit | As a result |
| Na | ppm | 42.3 |
| Pb | ppm | 7 |
| Cr | ppm | 4.5 |
| Fe | ppm | 312.1 |
| Sn | ppm | 14.3 |
| Ti | ppm | 31.1 |
| Ba | ppm | 8.2 |
| Mg | ppm | 29 |
| K | ppm | 44.6 |
| Sb | ppm | 22 |
| Pe | ppm | 70.4 |
| Se | ppm | 39.3 |
| Al | ppm | 47.1 |
| Ca | ppm | 214.8 |
| Ni | ppm | 18.5 |
| Cu | ppm | 2.4 |
| Mn | ppm | 2.6 |
| Zn | ppm | 9.7 |
| Si | ppm | 1148.2 |
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
ABS plastic reworked material.
To sum up:, can be in conjunction with the identification result of infrared spectrum analysis, head space gas chromatography and element distribution analysis
It qualitatively judges this unknown ABS sample and contains ABS plastic reworked material.
Embodiment 2
A kind of embodiment of ABS plastic reworked material discrimination method of the present invention, existing ABS plastic unknown sample, sentences
Breaking, whether it contains ABS reworked material, and analysis method is as follows:
(1) dissolubility is analyzed: sample being placed in solution at room temperature using chloroformic solution, ultrasonic 10h dissolution is passed through
After the ultrasonic dissolution of 10h, solution is still more muddy, as shown in Fig. 4, ABS plastic reworked material is contained in judgement sample；
(2) infrared spectrum analysis: will dissolve the solution after unknown ABS sample, take 5ul drop in KBr tabletting, 70 DEG C of bakings
0.5h is toasted in case, tests infrared spectrum, compares with the ABS raw material spectrogram of standard, there are many miscellaneous peaks, confirms this for ABS sample
Product contain ABS plastic reworked material；
(3) electron microscope analysis (testing using SEM-EDS): after sample to be carried out to lossless pre-treatment, it is placed in electron microscopic sample
It is observed on workbench, the surface condition of sample Electronic Speculum observation is as shown in Fig. 6, compared with raw material (attached drawing 5), sample 6
Surface it is variant；
Selected characteristic position carries out energy spectrum analysis, energy spectrum analysis discovery, the EDAX results of raw material sample such as table 2
Shown, the EDAX results of unknown sample are as shown in table 3:
The EDAX results of 2 raw material sample of table
The EDAX results of 3 sample to be tested of table
From table 2, table 3 as can be seen that compared with raw material sample, in sample to be tested EDAX results element species compared with
It is more, determine that sample to be tested may contain ABS plastic reworked material.
To sum up: in conjunction with dissolubility analysis, infrared spectrum analysis, electron microscope analysis identification result, this can be qualitatively judged not
Know that sample contains ABS plastic reworked material.
Embodiment 3
The present embodiment verifies the judging standard of head space gas chromatography, and setting 5 do not contain the ABS of reworked material
Sample, respectively sample 1~5；5 samples containing reworked material, respectively sample 6~10 are set；Head space is carried out respectively
Gas chromatographic analysis: weighing 1.2g in ml headspace bottle to each sample respectively, enters gas phase after heating 4h under the conditions of 120 DEG C
It is analyzed in chromatography, then in 50 DEG C of stable 3min, then 200 DEG C is warming up to the rate of 12K/min, finally in final temperature
Stablize 4min at 200 DEG C, data are as shown in table 4:
4 1~No. 10 sample headspace gas chromatographic analysis data of table
From table 4, it can be seen that No. 1-No. 5 without containing reworked material ABS sample appearance time all before 14min, and
Peak number amount is all not more than 15；The appearance time of No. 6-No. 10 ABS samples containing reworked material is mostly after 14min, and peak number amount
Greater than 15.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 (8)
1. a kind of discrimination method of ABS plastic reworked material, which comprises the steps of:
(1) sample is taken, determines the sample for ABS 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 dissolved in a solvent and particulate matter is obvious, in sample
Contain ABS plastic reworked material, wherein the solvent is chloroformic solution, acetone or methyl ethyl ketone；
When being identified using infrared spectrum analysis, compared with the ABS plastic raw material infrared spectrum of standard, if sample is infrared
Spectrogram has obvious miscellaneous peak, then contains ABS 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 the number at peak
Greater than 15, then contain ABS plastic reworked material in sample；
When being identified using electron microscope analysis method, if sample surfaces have the element ratio in scratch and pollution or sample energy spectrum analysis
Element in ABS plastic raw material energy spectrum analysis is more, then contains ABS plastic reworked material in sample；
When being identified using element distribution analysis method, if element species are greater than 15 kinds in sample, in sample again containing ABS plastic
Raw material；
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 containing ABS plastic regenerate
Material then determines to contain ABS plastic reworked material in sample.
2. the discrimination method of ABS plastic reworked material as described in claim 1, which is characterized in that in the step (1), if sample
Whether it is ABS plastic that product are uncertain, takes sample to carry out infrared spectrum analysis, whether confirmatory sample is ABS plastic.
3. the discrimination method of ABS plastic reworked material as described in claim 1, which is characterized in that the dissolubility of the step (2)
In analysis, sample is placed in chloroformic solution, using 8~12h of ultrasonic dissolution, if sample cannot be completely dissolved and particulate matter is bright
It is aobvious, then contain ABS plastic reworked material in sample.
4. the discrimination method of ABS plastic reworked material as described in claim 1, which is characterized in that the dissolubility of the step (2)
In analysis, sample is placed in acetone, using extraction device, 60-80 DEG C is heated to, 0.5-1.5h is dissolved, if sample cannot be complete
Fully dissolved and particulate matter is obvious then contains ABS plastic reworked material in sample.
5. the discrimination method of ABS plastic reworked material as described in claim 1, which is characterized in that the dissolubility of the step (2)
In analysis, sample is placed in methyl ethyl ketone, using extraction device, 80-90 DEG C is heated to, 0.5-1.5h is dissolved, if sample cannot
It is completely dissolved and particulate matter is obvious, then contain ABS plastic reworked material in sample.
6. the discrimination method of ABS plastic reworked material as described in claim 1, which is characterized in that described in the step (2)
The condition of 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 40
DEG C -60 DEG C of stable 2.5min-5min, are then warming up to 180 DEG C -220 DEG C with the rate of 10K/min-12K/min, finally most
Stablize 3min-5min under finishing temperature.
7. the discrimination method of ABS plastic reworked material as described in claim 1, which is characterized in that described in the step (2)
Elemental redistribution is analyzed using ICP-OES test.
8. the discrimination method of ABS plastic reworked material as described in claim 1, which is characterized in that in the step (2), use
When infrared spectrum analysis identifies, the method for infrared spectrum analysis are as follows: take the raw material of phase homogenous quantities with to test sample, be dissolved in phase
In the solvent of same volume, obtains starting material solution and to test sample solution, take the starting material solution of same volume respectively and to test sample
Solution is dripped in KBr tabletting, and examination of infrared spectrum is carried out after drying, obtains the INFRARED SPECTRUM of the infrared spectrum and raw material to test sample
Figure, will compare to the infrared spectrum of test sample and the infrared spectrum of raw material, obtains to whether contain reworked material in test sample.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111257270A (en) * | 2020-02-27 | 2020-06-09 | 宁波海关技术中心 | Method for detecting composition content of each monomer unit in regenerated ABS (acrylonitrile butadiene styrene) plastic |
| CN114764099A (en) * | 2021-05-07 | 2022-07-19 | 上海睿聚环保科技有限公司 | Evaluation system for evaluating quality of regenerated plastic at multiple angles |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111257270A (en) * | 2020-02-27 | 2020-06-09 | 宁波海关技术中心 | Method for detecting composition content of each monomer unit in regenerated ABS (acrylonitrile butadiene styrene) plastic |
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Application publication date: 20190611 |