CN106769986A - The discriminating of recycling plastics and quantitative detecting method in a kind of plastic pipe - Google Patents
The discriminating of recycling plastics and quantitative detecting method in a kind of plastic pipe Download PDFInfo
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- CN106769986A CN106769986A CN201710021204.7A CN201710021204A CN106769986A CN 106769986 A CN106769986 A CN 106769986A CN 201710021204 A CN201710021204 A CN 201710021204A CN 106769986 A CN106769986 A CN 106769986A
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- 229920003023 plastic Polymers 0.000 title claims abstract description 151
- 239000004033 plastic Substances 0.000 title claims abstract description 136
- 238000004064 recycling Methods 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 29
- 239000000463 material Substances 0.000 claims abstract description 96
- 238000002844 melting Methods 0.000 claims abstract description 38
- 230000008018 melting Effects 0.000 claims abstract description 38
- 238000001514 detection method Methods 0.000 claims abstract description 16
- 238000002329 infrared spectrum Methods 0.000 claims abstract description 13
- 238000012937 correction Methods 0.000 claims abstract description 11
- 230000004907 flux Effects 0.000 claims abstract description 11
- -1 polypropylene Polymers 0.000 claims description 22
- 229920001155 polypropylene Polymers 0.000 claims description 19
- 239000004743 Polypropylene Substances 0.000 claims description 18
- 238000007906 compression Methods 0.000 claims description 14
- 230000006835 compression Effects 0.000 claims description 14
- 238000004458 analytical method Methods 0.000 claims description 9
- 238000012360 testing method Methods 0.000 claims description 9
- 238000003556 assay Methods 0.000 claims description 6
- 238000007334 copolymerization reaction Methods 0.000 claims description 6
- 238000002425 crystallisation Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 229920002554 vinyl polymer Polymers 0.000 claims description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- 210000004907 gland Anatomy 0.000 claims description 4
- 238000007789 sealing Methods 0.000 claims description 4
- 239000012530 fluid Substances 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 2
- 230000002159 abnormal effect Effects 0.000 claims 1
- 238000010276 construction Methods 0.000 abstract description 4
- 238000011161 development Methods 0.000 abstract description 4
- 239000012535 impurity Substances 0.000 abstract 1
- 230000001737 promoting effect Effects 0.000 abstract 1
- 238000001228 spectrum Methods 0.000 description 20
- 239000004698 Polyethylene Substances 0.000 description 17
- 229920000573 polyethylene Polymers 0.000 description 17
- 238000005516 engineering process Methods 0.000 description 10
- 239000000203 mixture Substances 0.000 description 7
- 239000000047 product Substances 0.000 description 6
- 238000005469 granulation Methods 0.000 description 4
- 230000003179 granulation Effects 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 230000018109 developmental process Effects 0.000 description 3
- 238000007689 inspection Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 230000008901 benefit Effects 0.000 description 2
- 150000004951 benzene Chemical class 0.000 description 2
- 239000004566 building material Substances 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 238000010348 incorporation Methods 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 239000004014 plasticizer Substances 0.000 description 2
- 238000012795 verification Methods 0.000 description 2
- 238000010792 warming Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910001018 Cast iron Inorganic materials 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000000567 combustion gas Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000004035 construction material Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000013213 extrapolation Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 230000002706 hydrostatic effect Effects 0.000 description 1
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- 230000002262 irrigation Effects 0.000 description 1
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- 230000004048 modification Effects 0.000 description 1
- 230000009972 noncorrosive effect Effects 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 238000004451 qualitative analysis Methods 0.000 description 1
- 238000011002 quantification Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3563—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/02—Investigating or analyzing materials by the use of thermal means by investigating changes of state or changes of phase; by investigating sintering
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Abstract
Discriminating and quantitative detecting method the invention provides recycling plastics in a kind of plastic pipe, comprise the following steps：(1) the primary material sample and plastic pipe sample to be measured of plastic pipe to be measured are detected respectively by infrared spectrum, judges whether to be mixed with other impurity；(2) if being free of recycling plastics in primary material sample, using formula：The content of recycling plastics is calculated, in formula,It is the main endothermic peak mean heat flux of primary material sample melted curve；
Description
Technical field
The invention belongs to construction material detection technology field, more particularly, to a kind of mirror of recycling plastics in plastic pipe
Other and quantitative detecting method.
Background technology
Plastic pipe is macromolecular material obtained in polyolefin as raw material, with material is light, corrosion-resistant, non-corrosive, no
Fouling, inner wall smooth, small flow resistance, good sanitation performance, convenient transportation, construct that convenient, labour intensity is small, construction costs is low
Advantage, be national industrial policies emphasis promote a class building material, be widely used to city water supply and sewage, building water supply and drainage,
The every field such as heating, combustion gas, agricultural drainage and irrigation, communication and Electric Wires ＆ Cables laying.Nowadays traditional cast iron, galvanized pipe have been substituted
Material, the leading products as all kinds of tubing.
In recent years, plastic pipe range of application, scale are increased rapidly, and product quality problem is also highlighted therewith, its main original
Therefore one, be exactly that some producers are ordered about in low-price competition by interests, in the production process of tubing in violation of rules and regulations, transfinite and mix by giving up
Abandon other factory's regenerated plastics of plastic processing.The quality stability that this problem can have a strong impact on plastic pipe is durable with long-term
Property, stretching yield stress, elongation at break and the hydrostatic tolerance performance of tubing are reduced, bring serious hidden to all kinds of construction projects
Suffer from, the public hazards as harm plastic pipe industry survival and development.
In existing country and professional standard, although define and do not allow containing other factory's regenerated plastics in plastic pipe, for
The incorporation of our factory's reground plasticses does not provide a kind of feasible inspection in having clearly limitation, but existing country and professional standard yet
The our factory's reground plasticses or other factory's regenerated plastics that may be mixed in tubing can be differentiated and quantitative determination by survey method.Cause
This can accurately identify modeling, it is necessary to research and develop discriminating and the quantitative detecting method of recycling plastics in a kind of plastic pipe
Whether other factory's regenerated plastics or our factory's reground plasticses and Accurate Determining incorporation are mixed in material pipe material product.
The content of the invention
In view of this, the present invention is directed to propose the discriminating of recycling plastics and quantitative detecting method in a kind of plastic pipe,
To solve the problems, such as prior art.
To reach above-mentioned purpose, the technical proposal of the invention is realized in this way：
The discriminating of recycling plastics and quantitative detecting method, comprise the following steps in a kind of plastic pipe：(1) by infrared
Spectrum detects to the primary material sample and plastic pipe sample to be measured of plastic pipe to be measured respectively, parses and judge above-mentioned two
The main component in sample is planted, and whether recycling plastics are mixed with clear and definite above two sample；
(2) if being free of recycling plastics in primary material sample, the recycling plastics in plastic pipe sample to be measured are entered
Row quantitative determination, specific method is：
A, the press sheet compression for weighing appropriate primary material and corresponding plastic pipe sample, then by press sheet compression successively
It is placed in differential scanning calorimeter, sample is pre-processed using gradient isothermal crystallization method, and according to default heating schedule
Tested, respectively obtained the melting curve of each sample；
B, read two main endotherm peak temperature T of melting curve respectively using atlas analysis softwarea, extrapolation starting temperature
Degree Ta', main endothermic peak peak area Sa；Secondary endotherm peak temperature Tb, temperature of the extrapolated onset Tb', secondary endothermic peak peak area Sb, and press
According toThe mean heat flux of main endothermic peak or secondary endothermic peak is calculated, wherein, half-peak breadth Δ T computing formula are：Δ T=T-
T′；
The content of C, the recycling plastics calculated in plastic pipe sample to be measured, computing formula is：
In formula,It is the main endothermic peak mean heat flux of primary material sample melted curve；For Pipe samples to be measured are molten
Melt the main endothermic peak mean heat flux of curve, correction coefficient K is used to correct primary material with Pipe samples because being absorbed heat caused by component difference
Variance of peak.
Further, the assay of detection method other factory's regenerated plastics suitable for polyvinyl piping materials, wherein, institute
State correction coefficientWherein, Δ T0It is the main endothermic peak half-peak breadth of primary material melting curve；ΔT1It is Pipe samples to be measured
The main endothermic peak half-peak breadth of melting curve.
Further, the assay of detection method our factory's reground plasticses suitable for polyvinyl piping materials, wherein, institute
State correction coefficientWherein, main endothermic peak mean heat fluxMain endothermic peak half-peak breadth Δ Ta0, it is secondary
Endothermic peak mean heat fluxSecondary endothermic peak half-peak breadth Δ Tb0Calculated by primary material melting curve；Main endothermic peak is average
Hot-fluidMain endothermic peak half-peak breadth Δ Ta1, secondary endothermic peak mean heat fluxSecondary endothermic peak half-peak breadth Δ Tb1By tubing
Sample melted curve is calculated.
Further, the detection method suitable for random copolymerization polypropylene pipe other factory's regenerated plastics containing measurement
It is fixed, wherein, the correction coefficientWherein, main endothermic peak mean heat fluxMain endothermic peak half
Peak width Δ Ta0, secondary endothermic peak half-peak breadth Δ Tb0Calculated by primary material melting curve；Main endothermic peak mean heat flux
Main endothermic peak half-peak breadth Δ Ta1, secondary endothermic peak half-peak breadth Δ Tb1Calculated by Pipe samples melting curve.
Further, the detection method suitable for random copolymerization polypropylene pipe our factory's reground plasticses containing measurement
It is fixed, wherein, the correction coefficientWherein, main endothermic peak mean heat fluxSecondary endothermic peak half-peak
Δ T wideb0, secondary endothermic peak mean heat fluxCalculated by primary material melting curve；Main endothermic peak mean heat flux
Secondary endothermic peak half-peak breadth Δ Tb1, secondary endothermic peak mean heat fluxCalculated by Pipe samples melting curve.
Further, it is by parsing the primary material sample of the contrast plastic pipe to be measured and treating in the step (1)
The absworption peak for surveying the infrared spectrum of plastic pipe sample judges the primary material sample and plastic pipe to be measured of plastic pipe to be measured
Whether recycling plastics are mixed with sample.
Further, the preparation method of the press sheet compression in the step (2) is to weigh primary material and corresponding tubing
Each 5mg of press sheet compression of sample, sample is placed in special aluminum sample disk, does sealing gland treatment, obtains the compressing tablet
Sample.
Further, the atlas analysis software is warm using the TA Universal Analysis2000 of TA companies of the U.S.
Analysis software.
Wherein, present invention meaning recycling plastics are specifically divided into other factory's regenerated plastics and our factory's reground plasticses：Other factory regenerates
Plastics are main, and via the other factory of cleaning and crushing, the waste plastic without particular source is processed, granulation is obtained；Our factory reground plasticses master
To be obtained via the processing of the leftover pieces in our factory's tubing production process of the same race, granulation.
Relative to prior art, the discriminating of recycling plastics and quantitative detecting method have in plastic pipe of the present invention
There is following advantage：
Whether detection method provided by the present invention mixes recycling plastics simultaneously accurately in can accurately identifying plastic pipe
The content of recycling plastics is determined, helps to set up accurate and effective plastic pipe composition qualitative and quantitative analysis method, it is complete
The kind existing plastic pipe product quality monitoring standards system of supplement, meets the active demand in building materials test field, for ensureing work
Cheng Zhiliang, promotion plastic pipe industry healthy development are significant.
Brief description of the drawings
The accompanying drawing for constituting a part of the invention is used for providing a further understanding of the present invention, schematic reality of the invention
Apply example and its illustrate, for explaining the present invention, not constitute inappropriate limitation of the present invention.In the accompanying drawings：
Fig. 1 is the infrared spectrum of the primary material described in the embodiment of the present invention 1；
Fig. 2 is the infrared spectrum of the Pipe samples described in the embodiment of the present invention 1；
Fig. 3 is the polyethylene infrared standard collection of illustrative plates provided by German Brooker Science and Technology Ltd.；
Fig. 4 is the primary material sample and the melting curve of Pipe samples described in the embodiment of the present invention 1；
Fig. 5 is the infrared spectrum of the primary material described in the embodiment of the present invention 2；
Fig. 6 is the infrared spectrum of the Pipe samples described in the embodiment of the present invention 2；
Fig. 7 is the primary material sample and the melting curve of Pipe samples described in the embodiment of the present invention 2；
Fig. 8 is the infrared spectrum of the primary material described in the embodiment of the present invention 3；
Fig. 9 is the infrared spectrum of the Pipe samples described in the embodiment of the present invention 3；
Figure 10 is the infrared standard collection of illustrative plates of atactic copolymerized polypropene provided by German Brooker Science and Technology Ltd.；
Figure 11 is the primary material sample and the melting curve of Pipe samples described in the embodiment of the present invention 3；
Figure 12 is the infrared spectrum of the primary material described in the embodiment of the present invention 4；
Figure 13 is the infrared spectrum of the Pipe samples described in the embodiment of the present invention 4；
Figure 14 is the primary material sample and the melting curve of Pipe samples described in the embodiment of the present invention 4.
Specific embodiment
It should be noted that in the case where not conflicting, the embodiment in the present invention and the feature in embodiment can phases
Mutually combination.
In the description of the invention, it is to be understood that term " " center ", " longitudinal direction ", " transverse direction ", " on ", D score,
The orientation or position relationship of the instruction such as "front", "rear", "left", "right", " vertical ", " level ", " top ", " bottom ", " interior ", " outward " are
Based on orientation shown in the drawings or position relationship, it is for only for ease of and describes the present invention and simplify to describe, rather than instruction or dark
Showing the device or element of meaning must have specific orientation, with specific azimuth configuration and operation therefore it is not intended that right
Limitation of the invention.Additionally, term " first ", " second " etc. are only used for describing purpose, and it is not intended that indicating or implying phase
To importance or the implicit quantity for indicating indicated technical characteristic.Thus, the feature for defining " first ", " second " etc. can
To express or implicitly include one or more this feature.In the description of the invention, unless otherwise indicated, " multiple "
It is meant that two or more.
In the description of the invention, it is necessary to illustrate, unless otherwise clearly defined and limited, term " installation ", " phase
Company ", " connection " should be interpreted broadly, for example, it may be being fixedly connected, or being detachably connected, or be integrally connected；Can
Being to mechanically connect, or electrically connect；Can be joined directly together, it is also possible to be indirectly connected to by intermediary, Ke Yishi
Two connections of element internal.For the ordinary skill in the art, above-mentioned term can be understood by concrete condition
Concrete meaning in the present invention.
Describe the present invention in detail below with reference to the accompanying drawings and in conjunction with the embodiments.
Signified recycling plastics in the discriminating of recycling plastics and quantitative detecting method in a kind of plastic pipe of the invention
It is specifically divided into other factory's regenerated plastics and our factory's reground plasticses：Regenerated plastics main other factory via cleaning and crushing in other factory's is without specific
The waste plastic processing in source, granulation are obtained；Our factory's reground plasticses are main via the corner in our factory's tubing production process of the same race
Material processing, granulation are obtained.
Wherein, in order to verify recycling plastics in a kind of plastic pipe of the invention discriminating and quantitative detecting method can
It is by property, its theoretical foundation and checking data list is as follows：
Because the multiple heat absorbing peak obtained after gradient isothermal crystallization method treatment sample is deposited with the segment of polymer crystallization sequence
In corresponding relation, the content of crystalline sequence segment can be quantified by calculating multiple heat absorbing peak evenly heat flow valuve.Also, again
In recycling heating process, there is the polymer side chain of low relative molecular mass to recycled plastic in polymer molecule degraded chain rupture.
Therefore, the segment of recycling plastics crystalline sequence exists significantly different with virgin plastics crystalline sequence segment.Can be by analysis
The difference of endothermic peak evenly heat flow valuve calculates the content of recycling plastics, and this is recycling plastic content in calculating plastic pipe
Theoretical foundation.
In the verification experimental verification stage, the primary material that current tubing manufacturer generally uses, and voluntarily purchase tubing city are collected
The three-level regenerated plastics sold on field.By HAAKETM PolyLabTM(you are scientific and technological for the silent winged generation of match for OS modularizations torque rheometer
Company) kneaded by different proportion, test sample is made, by reading and the meter of test sample melting curve relevant parameter
Calculate, derive above-mentioned empirical equation, and calculated value by regenerated plastics content compares with actual value, that verifies computing formula can
By property and repeatability.The collection information of primary material sample is shown in Table 1 with table 2, and result of calculation is shown in Table 3- tables 6.
The primary material sample collection information of the polyethylene of table 1
The primary material sample collection information of the atactic copolymerized polypropene of table 2 (PP-R)
Other factory's regenerated plastics cubage result in the polyethylene test sample of table 3
Our factory's reground plasticses cubage result in the polyethylene test sample of table 4
Other factory's regenerated plastics cubage result in the atactic copolymerized polypropene test sample of table 5
Our factory's reground plasticses cubage result in the atactic copolymerized polypropene test sample of table 6
By the comparing of test data it can be found that the method for present invention description can be moulded to the recycling in plastic pipe
Material carries out accurate quantification and qualification, has filled up the blank of the such detection technique in plastic pipe field.The method is comprehensively transported
Various precision detecting instruments are used, detection cycle is short, detection process controllable precise.And the method does not need manufacturer to provide again
Raw plastics, are that the formulation of follow-up relevant criterion and quality inspection organization are carried out detection work and provided convenience.The detection method will be
Ensure that the sound development of plastic pipe industry provides reliable technology monitoring means, act of unfair competition contained from source,
Prevent the product of inferior quality for architectural engineering, it is ensured that construction quality.
Embodiment 1：
(1) the primary material sample and plastic pipe sample to be measured of plastic pipe to be measured are examined respectively by infrared spectrum
Survey, parse and judge whether be mixed with recycling plastics in the main component in above two sample, and clear and definite above two sample；
From the primary material sample for preparing plastic pipe, a small amount of sample is cut, be placed in tablet press machine, pushed in 15MPa pressure
2min processed, laminates.Take out press sheet compression and be placed in FTIS (German Brooker Science and Technology Ltd.)
Decay total reflection annex on, scanned infrared collection of illustrative plates.Wave-number range is (4000~400) cm-1, measurement temperature is maintained at room temperature,
With air as background.Primary material infared spectrum is shown in Fig. 1.
For plastic pipe sample, repeat step 1, scanned infrared collection of illustrative plates.Plastic pipe sample infared spectrum is shown in Fig. 2.
By parsing primary material infared spectrum it can be found that 2914 and 2848cm-1Place's strong absworption peak is methylene-CH2-
Stretching vibration absworption peak, 1471cm-1Place's absworption peak is-CH2- deformation vibration the absworption peak, 718cm-1Place's absworption peak is-CH2- face
Interior rocking vibration is produced.These infared spectrum features are basically identical with polyethylene infrared standard collection of illustrative plates.It is understood that the original
Raw material sample main component is polyethylene, without other factory's regenerated plastics.Wherein, polyethylene infrared standard collection of illustrative plates is by German Brooker
Science and Technology Ltd. provides, and sees Fig. 3.
By parsing plastic pipe sample infared spectrum it can be found that the collection of illustrative plates is basically identical with primary material infared spectrum,
The plastic pipe sample main component is similarly polyethylene.But in 875cm-1There is obvious aromatic hydrocarbons C-H absworption peaks in place, be by
Benzene series plasticizer contained in polyethylene regenerated plastics and produce.It is understood that the Pipe samples polyethylene containing other factory is again
Raw plastics.
(2) if being free of recycling plastics in primary material sample, the recycling plastics in plastic pipe sample to be measured are entered
Row quantitative determination, specific method is：
A, the press sheet compression for weighing primary material and corresponding Pipe samples, each 5mg or so, are accurate to 0.1mg.By sample
It is placed in special aluminum sample disk, does sealing gland treatment.Then it is sequentially placed into differential scanning calorimeter, with gradient isothermal
Crystallisation prepares sample, and to be first warming up to 170 DEG C with 10 DEG C/min from room temperature, constant temperature 3min eliminates heat and goes through specific temperature program
Shi Hou, 130 DEG C are cooled to 10 DEG C/min constant speed.Then with appropriate speed, 5 DEG C is step-length, is cooled to 105 DEG C.Each stage
Constant temperature 30min~60min.Finally primary material sample is respectively obtained according to default heating schedule from 30 DEG C of constant heatingrates to 170 DEG C
The melting curve of product and Pipe samples, as shown in Figure 4.To the melting curve of primary material sample and Pipe samples through analysis, obtain
Parameters needed for quantitative determination, concrete outcome is as shown in table 7.
The primary material of table 7 and Pipe samples melting curve parameters
Thus other factory's polyethylene regenerated plastics content is 33.0% during the polyvinyl piping materials sample can be calculated.
Embodiment 2：
For the primary material sample for preparing plastic pipe, step 1, scanned infrared collection of illustrative plates in embodiment 1 are repeated.Primary material is red
Outer collection of illustrative plates is shown in Fig. 5；Pipe samples infared spectrum is shown in Fig. 6.
By parsing primary material infared spectrum it can be found that 2913 and 2847cm-1Place's strong absworption peak is methylene-CH2-
Stretching vibration absworption peak, 1471cm-1Place's absworption peak is-CH2- deformation vibration the absworption peak, 717cm-1Place's absworption peak is-CH2- face
Interior rocking vibration is produced.These infared spectrum features are basically identical with polyethylene infrared standard collection of illustrative plates.It is understood that the original
Raw material sample main component is polyethylene.Polyethylene infrared standard collection of illustrative plates is provided by German Brooker Science and Technology Ltd., sees figure
3。
By parsing Pipe samples infared spectrum it can be found that the collection of illustrative plates is basically identical with primary material infared spectrum, the pipe
Material sample main component is similarly polyethylene, and without other factory's regenerated plastics composition.
The press sheet compression of primary material and corresponding Pipe samples is weighed, step (2) in most embodiment 1 is repeated, original is obtained
The melting curve of raw material sample and Pipe samples, as shown in fig. 7, the melting curve of primary material sample and Pipe samples is through analysis,
Parameters needed for quantitative determination are obtained, concrete outcome is as shown in table 8 and table 9.
The primary material of table 8 and the main endothermic peak parameters of Pipe samples melting curve
The primary material of table 9 and Pipe samples melting curve pair endothermic peak parameters
Thus our factory's reground plasticses content is 12.9% during the polyvinyl piping materials sample can be calculated.
Embodiment 3：
For the primary material sample for preparing plastic pipe, step 1, scanned infrared collection of illustrative plates in embodiment 1 are repeated.Primary material is red
Outer collection of illustrative plates is shown in Fig. 8；Pipe samples infared spectrum is shown in Fig. 9.
By parsing primary material infared spectrum it can be found that 2950cm-1Place's absworption peak is methyl-CH3Symmetrical stretching vibration
Peak, 2912cm-1Place's absworption peak is-CH2- asymmetric stretching vibration peak, 2838cm-1Place's absworption peak is-CH2- symmetrical stretching vibration
Peak, 1455cm-1Place's absworption peak is-CH2- complete vibration peak, 1376cm-1Place's absworption peak is-CH3Flexural vibrations peak.These are infrared
TuPu method is basically identical with atactic copolymerized polypropene infrared standard collection of illustrative plates.It is understood that the primary material sample it is main into
It is divided into atactic copolymerized polypropene, without regenerated plastics or other materials composition.Atactic copolymerized polypropene infrared standard collection of illustrative plates is by moral
Brooker Science and Technology Ltd. of state provides, and sees Figure 10.
By parsing Pipe samples infared spectrum it can be found that the collection of illustrative plates is basically identical with primary material infared spectrum, the pipe
Material sample main component is similarly atactic copolymerized polypropene.But in 875cm-1There is obvious C-H absworption peaks in place, be by poly- second
Benzene series plasticizer contained in alkene regenerated plastics and produce.It is understood that the Pipe samples polyethylene containing other factory regeneration modeling
Material.
The press sheet compression of primary material and corresponding Pipe samples, each 5mg or so are weighed, 0.1mg is accurate to.Sample is put
Put in special aluminum sample disk, do sealing gland treatment.Then it is sequentially placed into differential scanning calorimeter, with gradient isothermal knot
Crystallization prepares sample, and to be first warming up to 170 DEG C with 10 DEG C/min from room temperature, constant temperature 3min eliminates thermal history to specific temperature program
Afterwards, 150 DEG C are cooled to 10 DEG C/min constant speed.Then with appropriate speed, 5 DEG C is step-length, is cooled to 95 DEG C.Each stage constant temperature
10min~20min.It is last according to default heating schedule from 30 DEG C of constant heatingrates to 170 DEG C, respectively obtain primary material sample and
The melting curve of Pipe samples, as shown in figure 11.The melting curve of primary material sample and Pipe samples obtains quantitative inspection through analysis
Parameters needed for surveying, concrete outcome is as shown in Table 10 and Table 11.
The primary material of table 10 and the main endothermic peak parameters of Pipe samples melting curve
The primary material of table 11 and Pipe samples melting curve pair endothermic peak parameters
Other factory's polyethylene regenerated plastics content is 22.7% during this can calculate the random copolymerization polypropylene pipe sample.
Embodiment 4：
For the primary material sample for preparing plastic pipe, step 1, scanned infrared collection of illustrative plates in optimal implementation one are repeated.
Primary material infared spectrum is shown in Figure 12.
For Pipe samples, repeat step 1, scanned infrared collection of illustrative plates.Pipe samples infared spectrum is shown in Figure 13.
By parsing primary material infared spectrum it can be found that 2950cm-1Place's absworption peak is methyl-CH3Symmetrical stretching vibration
Peak, 2917cm-1Place's absworption peak is-CH2- asymmetric stretching vibration peak, absworption peak is-CH at 2838cm-12- symmetrical stretching vibration
Peak, 1456cm-1Place's absworption peak is-CH2- complete vibration peak, 1376cm-1Place's absworption peak is-CH3Flexural vibrations peak.These are infrared
TuPu method is basically identical with atactic copolymerized polypropene infrared standard collection of illustrative plates.It is understood that the primary material sample it is main into
It is divided into atactic copolymerized polypropene, without regenerated plastics or other materials composition.Atactic copolymerized polypropene infrared standard collection of illustrative plates is by moral
Brooker Science and Technology Ltd. of state provides, and sees Figure 10.
By parsing Pipe samples infared spectrum it can be found that the collection of illustrative plates is basically identical with primary material infared spectrum, the pipe
Material sample main component is similarly atactic copolymerized polypropene, and without other factory's regenerated plastics composition.
The press sheet compression of primary material and corresponding Pipe samples is weighed, step 5 in optimal implementation three is repeated, obtained
The melting curve of primary material sample and Pipe samples, as shown in figure 14.
The melting curve of primary material sample and Pipe samples obtains parameters needed for quantitative determination through analysis, specific knot
Fruit is as shown in table 12 and table 13.
The primary material of table 12 and the main endothermic peak parameters of Pipe samples melting curve
The primary material of table 13 and Pipe samples melting curve pair endothermic peak parameters
Thus our factory's reground plasticses content is 16.7% during the random copolymerization polypropylene pipe sample can be calculated.
Presently preferred embodiments of the present invention is the foregoing is only, is not intended to limit the invention, it is all in essence of the invention
Within god and principle, any modification, equivalent substitution and improvements made etc. should be included within the scope of the present invention.
Claims (8)
1. the discriminating of recycling plastics and quantitative detecting method in a kind of plastic pipe, it is characterised in that comprise the following steps：
(1) the primary material sample and plastic pipe sample to be measured of plastic pipe to be measured are detected respectively by infrared spectrum, is parsed
And judge whether be mixed with recycling plastics in the main component in above two sample, and clear and definite above two sample；
(2) if being free of recycling plastics in primary material sample, the recycling plastics in plastic pipe sample to be measured are determined
Amount detects that specific method is：
, then be sequentially placed into for press sheet compression by A, the press sheet compression for weighing appropriate primary material and corresponding plastic pipe sample
In differential scanning calorimeter, sample is pre-processed using gradient isothermal crystallization method, and carried out according to default heating schedule
Test, respectively obtains the melting curve of each sample；
B, read two main endotherm peak temperature T of melting curve respectively using atlas analysis softwarea, temperature of the extrapolated onset
Ta', main endothermic peak peak area Sa；Secondary endotherm peak temperature Tb, temperature of the extrapolated onset Tb', secondary endothermic peak peak area Sb, and according toThe mean heat flux of main endothermic peak or secondary endothermic peak is calculated, wherein, half-peak breadth Δ T computing formula are：Δ T=T-T '；
The content of C, the recycling plastics calculated in plastic pipe sample to be measured, computing formula is：
In formula,It is the main endothermic peak mean heat flux of primary material sample melted curve；For Pipe samples to be measured melt song
The main endothermic peak mean heat flux of line, correction coefficient K be used to correcting primary material and Pipe samples because caused by component difference endothermic peak it is abnormal
Become.
2. the discriminating of recycling plastics and quantitative detecting method in plastic pipe according to claim 1, it is characterised in that：
The assay of detection method other factory's regenerated plastics suitable for polyvinyl piping materials, wherein, the correction coefficientWherein, Δ T0It is the main endothermic peak half-peak breadth of primary material melting curve；ΔT1It is Pipe samples melting curve master to be measured
Endothermic peak half-peak breadth.
3. the discriminating of recycling plastics and quantitative detecting method in plastic pipe according to claim 1, it is characterised in that：
The assay of detection method our factory's reground plasticses suitable for polyvinyl piping materials, wherein, the correction coefficientWherein, main endothermic peak mean heat fluxMain endothermic peak half-peak breadth Δ Ta0, secondary endothermic peak it is average
Hot-fluidSecondary endothermic peak half-peak breadth Δ Tb0Calculated by primary material melting curve；Main endothermic peak mean heat flux
Main endothermic peak half-peak breadth Δ Ta1, secondary endothermic peak mean heat fluxSecondary endothermic peak half-peak breadth Δ Tb1Melted by Pipe samples bent
Line computation draws.
4. the discriminating of recycling plastics and quantitative detecting method in plastic pipe according to claim 1, it is characterised in that：
The assay of detection method other factory's regenerated plastics suitable for random copolymerization polypropylene pipe, wherein, the correction system
NumberWherein, main endothermic peak mean heat fluxMain endothermic peak half-peak breadth Δ Ta0, secondary endothermic peak half
Peak width Δ Tb0Calculated by primary material melting curve；Main endothermic peak mean heat fluxMain endothermic peak half-peak breadth Δ Ta1、
Secondary endothermic peak half-peak breadth Δ Tb1Calculated by Pipe samples melting curve.
5. the discriminating of recycling plastics and quantitative detecting method in plastic pipe according to claim 1, it is characterised in that：
The assay of detection method our factory's reground plasticses suitable for random copolymerization polypropylene pipe, wherein, the correction system
NumberWherein, main endothermic peak mean heat fluxSecondary endothermic peak half-peak breadth Δ Tb0, secondary endothermic peak puts down
Equal hot-fluidCalculated by primary material melting curve；Main endothermic peak mean heat fluxSecondary endothermic peak half-peak breadth Δ
Tb1, secondary endothermic peak mean heat fluxCalculated by Pipe samples melting curve.
6. the discriminating of recycling plastics and quantitative detecting method in plastic pipe according to claim 1, it is characterised in that：
It is the red of primary material sample by parsing the contrast plastic pipe to be measured and plastic pipe sample to be measured in the step (1)
Whether the absworption peak of outer spectrogram judges to be mixed with recycling plastics in above two sample.
7. the discriminating of recycling plastics and quantitative detecting method in plastic pipe according to claim 1, it is characterised in that：
The preparation method of the press sheet compression in the step (2) is to weigh primary material and the press sheet compression of corresponding Pipe samples is each
5mg, sample is placed in special aluminum sample disk, does sealing gland treatment, obtains the press sheet compression.
8. the discriminating of recycling plastics and quantitative detecting method in the plastic pipe according to any one of claim 1~7, its
It is characterised by：The atlas analysis software is soft using TA Universal 2000 heat analysis of Analysis of TA companies of the U.S.
Part.
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