CN108508115B - Identification method for regenerated terylene by physical and chemical recovery method - Google Patents
Identification method for regenerated terylene by physical and chemical recovery method Download PDFInfo
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- CN108508115B CN108508115B CN201810721996.3A CN201810721996A CN108508115B CN 108508115 B CN108508115 B CN 108508115B CN 201810721996 A CN201810721996 A CN 201810721996A CN 108508115 B CN108508115 B CN 108508115B
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The invention provides a method for identifying regenerated terylene by a physical and chemical recovery method, which comprises the following steps: 1. the sample is pretreated. Taking a sample, adding sulfolane-acetonitrile to dissolve and precipitate, oscillating at high temperature, cooling, performing centrifugal separation, and taking supernatant. 2. And (4) detecting by high performance liquid chromatography. The obtained supernatant was subjected to chromatography. 3. And (5) judging fibers. Intercepting data of the retention time period of 9.2 min-9.54 min, plotting and amplifying, displaying the difference of fibers in different processes, multiplying the peak height value by the integral of the chromatogram, wherein the difference is more obvious, and if the product is less than 1500, judging to adopt the physical-chemical recovery method regenerated polyester fiber produced by the viscosity adjusting process.
Description
Technical Field
The invention relates to an identification method of regenerated textile materials, in particular to an identification method of regenerated terylene produced by a physical chemical recovery method by adopting a viscosity adjusting process (such as solid phase tackifying, liquid phase tackifying, viscosity homogenization control and the like).
Background
Terylene, the scientific name polyethylene terephthalate fiber, is a class of polyester fibers, abbreviated by the English acronym PET fiber. It is widely applied to the textile field and is the fiber variety with the largest yield in the world at present. The primary polyester is polyethylene glycol terephthalate fiber produced by direct spinning or chip spinning after polyester is synthesized by direct esterification continuous polycondensation or intermittent polycondensation by taking purified terephthalic acid and ethylene glycol as monomers. The regenerated polyester can be divided into the following parts according to the processing method: physical recovery method and chemical recovery method. In recent years, a new physical chemical recovery method has appeared.
The physical recovery method does not damage the chemical structure of the high polymer and does not change the composition of the high polymer. The method is a regeneration circulation method of macromolecule layer which collects, classifies, purifies and dries reclaimed materials, adds necessary auxiliary agents for processing and granulation to ensure that the reclaimed materials reach the spinning raw material quality standard. The main variety is polyethylene terephthalate fiber prepared by directly melt spinning after the processes of collecting, classifying, cleaning, crushing, purifying, drying and the like of waste polyester bottles.
The chemical recovery method is a method of recovering and reusing a small molecule layer, in which a high molecular compound in a synthetic fiber is depolymerized with a chemical agent, converted into a monomer or an oligomer, and then a new chemical fiber is produced from the monomer. The method can thoroughly remove substances which cannot be removed in a physical regeneration method, such as dyes, degraded molecular chain segment structures and the like, and the quality of regenerated products can be comparable with that of primary terylene. Hydrolysis, alcoholysis, aminolysis and supercritical processes are available. The polyester degradation methods which have been realized in industrial production include hydrolysis methods of Smorgon and Oxid companies, methanol depolymerization methods of Du Pont, Eastman Kodak and Hoechst companies, ethylene glycol depolymerization methods of Goodyear, Du Pont and Hoechst companies, and a combination of ethylene glycol depolymerization and methanol ester exchange methods of Diperson. The new material company introduced by Zhejiang delight is the process of emperor company, and adopts methanol alcoholysis process, and the products are EG and dimethyl terephthalate (DMT). Since thirteen five, enterprises represented by environment-friendly GmbH of Zhejiang Green space in China adopt an ethylene glycol alcoholysis process to develop products of polyester fiber regenerated by a chemical recovery method, wherein the products are ethylene terephthalate (BHET) and oligomers thereof, and certain achievement is achieved.
The physical and chemical recovery method is an improvement and upgrade aiming at the limitation of the physical recovery method, and is characterized in that the recovered waste textile products and polyester waste are melted and then subjected to liquid-phase or solid-phase tackifying. The method mainly adopts a physical method and is assisted by a chemical method to improve the molecular weight uniformity and reduce the impurity content, effectively improves the quality of regenerated products and realizes the production of differentiated regenerated products under the condition of not increasing the production cost greatly, has very good industrial popularization value, and has important significance for improving the quality of the regenerated products and improving the regeneration utilization rate of waste textiles.
In view of the difference between the production cost, the transaction price, the technical parameters, the corresponding tax policy given by the country and the like, the method for qualitatively identifying the primary polyester and the regenerated polyester is very necessary to be established, so that the identification problem of the regenerated polyester fiber is solved from the source, and the method has very important significance for promoting export trade.
The invention relates to an identification method for physical recycling method regenerated terylene ZL201510565693.3 and an identification method for chemical recycling method regenerated terylene ZL201510843319.5 in China.
ZL201510565693.3 is a method for identifying regenerated polyester produced by a physical recovery method for recycling bottle flakes or fiber grade regenerated polyester chips obtained by melting and granulating the recycled polyester as a raw material through melt spinning; ZL201510843319.5 is an identification method for regenerated terylene by a chemical recovery method aiming at repolymerization of dimethyl terephthalate (DMT) produced by a methanol alcoholysis process, and has certain limitations. The invention relates to an identification method of regenerated terylene produced by a physical chemical recovery method by adopting a viscosity regulation process (such as solid phase tackifying, liquid phase tackifying, viscosity homogenization control and the like).
Disclosure of Invention
Aiming at the problem that an effective identification method for regenerated terylene produced by a physical chemical recovery method by adopting a viscosity regulation process (such as solid-phase tackifying, liquid-phase tackifying, viscosity homogenization control and the like) does not exist in the prior art, the identification method is provided by analyzing the essential difference of various fiber processing processes, precipitating a second sequence cyclic oligomer with a repeating unit of 2-5 and a linear oligomer with a repeating unit of 3 through a proper solvent and precipitator system, separating by using high performance liquid chromatography, and according to the difference of peak-appearing maps. The method is convenient to implement, and convenient and fast.
In order to realize the aim, the invention provides a method for identifying regenerated terylene by a physical and chemical recovery method, which comprises the following steps:
1. the sample is pretreated. Taking 5g of sample, adding sulfolane-acetonitrile prepared according to a certain volume ratio to dissolve and precipitate according to a certain bath ratio, oscillating for 30min at 180 ℃, cooling, performing centrifugal separation again, taking supernatant, refrigerating for more than 8 hours in a refrigerator, taking out, filtering, and then cooling to room temperature for high performance liquid chromatography detection.
2. And (4) detecting by high performance liquid chromatography. And carrying out chromatographic detection on the supernatant, wherein a chromatographic column is XDB C18(5 mu m), the thickness of the chromatographic column is 250mm multiplied by 4.6mm, the flow rate is 1.0mL/min, the column temperature is 30 ℃, the sample injection amount is 10.0 mu L, a detector is a diode array detector DAD, the detection wavelength is 254nm, a mobile phase 1 is methanol, and a mobile phase 2 is 10% methanol/90% water.
3. And (5) judging fibers. Intercepting high performance liquid chromatogram data of the retention time period of 9.2 min-9.54 min, multiplying the peak height value by chromatogram integral, and if the product is less than 1500, judging to adopt the physical and chemical recovery method regenerated polyester fiber produced by the viscosity adjusting process.
The invention provides a method for identifying regenerated terylene by a physical chemical recovery method, which is characterized in that in the pretreatment of a sample, the bath ratio of the sample to sulfolane-acetonitrile is 1: 25, the bath ratio of a precipitator is 80: 20, and the volume ratio of the sulfolane to the acetonitrile is 80: 20.
The invention provides a method for identifying regenerated terylene by a physical chemical recovery method, which is used for pretreating a sample, wherein the centrifugal speed for centrifugal separation is 5000r/min, and the centrifugal separation time is 5 min.
The invention provides a method for identifying regenerated terylene by a physical chemical recovery method, in the detection of high performance liquid chromatography, the gradient of a mobile phase 1 and a mobile phase 2 is as follows: at 0min, the mobile phase 1 accounts for 20%, and the mobile phase 2 accounts for 80%; at 15min, the mobile phase 1 accounts for 80%, and the mobile phase 2 accounts for 20%; at 20min, the mobile phase 1 accounts for 100%, and the mobile phase 2 accounts for 0%; at 35min, mobile phase 1 accounted for 100%, mobile phase 2 accounted for 0%.
Has the advantages that: the identification method for the regenerated terylene by the physical chemical recovery method, which is produced by adopting the viscosity regulation process (such as solid phase tackifying, liquid phase tackifying, viscosity homogenization control and the like), is convenient to implement, convenient and rapid.
Drawings
FIG. 1 is a high performance liquid chromatogram of different fibers from example 1 for residence time periods of 8.2min to 19.72min
FIG. 2 is a high performance liquid chromatogram of different fibers of example 1 for residence time periods of 9.2min to 9.54min
FIG. 3 is a high performance liquid chromatogram of different fibers in an example of residence time period of 8.2min to 19.72min
FIG. 4 is a high performance liquid chromatogram of different fibers of example 2 for residence time periods of 9.2min to 9.54min
Detailed Description
Example 1
10 samples are collected in the domestic original state, the physical recovery method regeneration and the physical chemical recovery method regeneration, and the sample number is 1# to 10#, which is shown in Table 1.
TABLE 1 sample condition table
| Numbering | Properties of fiber | Manufacturer(s) |
| 1# | Regenerating by physical and chemical recovery method, and thickening waste silk to obtain golden yellow product | |
| 2# | Primary, blue-color short fiber | Anxing |
| 3# | Virgin, extra-black short fiber | Anxing |
| 4# | Regenerating by physical and chemical recovery method, soaking with 5% of color master batch, and tackifying the soaked material to obtain black | Ningbo |
| 5# | Original, natural color full dull filament | Rainbow with water-collecting |
| 6# | Regenerating by physical and chemical recovery method, thickening bottle chip with ethylene glycol, and making black POY filament | Yizheng Zhongxing |
| 7# | Regenerating by physical and chemical recovery method, melting the waste silk after granulating, tackifying by solid phase, spinning, | ningbo Baoxin No. 2 |
| 8# | Regenerating by physical and chemical recovery method, melting the waste silk after granulating, tackifying by solid phase, spinning, | ningbo Baoxin No. 3 |
| 9# | Original, natural color short fiber | Characterization |
| 10# | Primary, large red short fiber | Anxing environmental protection |
1. Pretreating the sample
10 samples, 5g each were taken. Adding a pre-prepared sulfolane-acetonitrile dissolving and precipitating agent with the volume ratio of 80: 20 according to the bath ratio of 1: 25, shaking for 30min at the high temperature of 180 ℃, cooling, centrifuging for 5min at the centrifugal speed of 5000r/min, taking the supernatant, putting the supernatant into a refrigerator for refrigerating for more than 8 hours, taking out, filtering, and then putting the supernatant to the room temperature for high performance liquid chromatography detection.
2. High performance liquid chromatography detection
Since the test results depend on the instrument used, it is not possible to give the usual parameters of the chromatographic analysis. The following operating conditions have proven suitable for the tests. The chromatographic detection of the sample is carried out according to the following conditions:
a) a chromatographic column: XDB C18(5 μm), 250 mm. times.4.6 mm, or equivalent.
b) Flow rate: 1.0 mL/min.
c) Column temperature: at 30 ℃.
d) Sample introduction amount: 10.0. mu.L.
e) A detector: diode Array Detector (DAD).
f) Detection wavelength: 254 nm.
g) Mobile phase 1: methanol.
h) Mobile phase 2: 10% methanol/90% water.
i) The gradient is shown in table 2.
TABLE 2 gradiometer
| Time (min) | Mobile phase 1 (%) | Mobile phase 2 (%) |
| 0.00 | 20.0 | 80.0 |
| 15.00 | 80.0 | 20.0 |
| 20.00 | 100.0 | 0 |
| 35.00 | 100.0 | 0 |
3. Fiber determination
The HPLC data for the residence time period of 8.2min to 19.72min were plotted as shown in FIG. 1 below. As can be seen from the visual inspection of FIG. 1, the high performance liquid chromatography patterns of the fibers in different processes are layered and have differences in the retention time of about 9.48min, and the data of the retention time period of 9.2min to 9.54min are intercepted, plotted and amplified, and as shown in FIG. 2, the differences of 2#, 3#, 5#, 9#, 10#, 1#, 4#, 6#, 7#, and 8# appear. The peak height value is multiplied by the integral of the chromatogram, the data are shown in Table 3, and the difference is more obvious.
TABLE 3 chromatogram peak processing table for retention time periods of different fibers from 9.2min to 9.54min
If the product of the peak height value and the chromatogram integral is less than 1500, the regenerated polyester fiber is judged to be the physical and chemical recovery method produced by adopting the viscosity adjusting process. By using the method, the technicians in the field can identify five physical and chemical recovery method regenerated polyester fiber samples produced by adopting a viscosity adjusting process, namely 1#, 4#, 6#, 7# and 8 #.
Example 2
9 samples are collected in the domestic original state, the regeneration by the physical recovery method, the regeneration by the chemical recovery method and the regeneration by the physical chemical recovery method, and the sample number is 1# to 9#, see table 4.
TABLE 4 sample condition table
1. Pretreating the sample
Taking 5g of 9 samples, adding a sulfolane-acetonitrile dissolving and precipitating agent prepared in advance according to a bath ratio of 1: 25 and a volume ratio of 80: 20, oscillating for 30min at a high temperature of 180 ℃, cooling, centrifuging for 5min at a centrifugal speed of 5000r/min, taking supernatant, refrigerating for more than 8 hours in a refrigerator, taking out, filtering, and then placing to room temperature for high performance liquid chromatography detection.
2. High performance liquid chromatography detection
Since the test results depend on the instrument used, it is not possible to give the usual parameters of the chromatographic analysis. The following operating conditions have proven suitable for the tests. The chromatographic detection of the sample is carried out according to the following conditions:
a) a chromatographic column: XDB C18(5 μm), 250 mm. times.4.6 mm, or equivalent.
b) Flow rate: 1.0 mL/min.
c) Column temperature: at 30 ℃.
d) Sample introduction amount: 10.0. mu.L.
e) A detector: diode Array Detector (DAD).
f) Detection wavelength: 254 nm.
g) Mobile phase 1: methanol.
h) Mobile phase 2: 10% methanol/90% water.
i) The gradient is shown in table 5.
TABLE 5 gradiometer
| Time (min) | Mobile phase 1 (%) | Mobile phase 2 (%) |
| 0.00 | 20.0 | 80.0 |
| 15.00 | 80.0 | 20.0 |
| 20.00 | 100.0 | 0 |
| 35.00 | 100.0 | 0 |
3. Fiber determination
The HPLC data for the residence time period of 8.2min to 19.72min was plotted as shown in FIG. 3. As can be seen by visual inspection in FIG. 3, the HPLC patterns of the fibers of different processes are layered and have different values about 9.54min, and the data of the residence time period of 9.2min to 9.54min are intercepted, plotted and amplified, and as shown in FIG. 4, the differences of 2#, 5#, 1#, 3#, 4#, 6#, 7#, 8#, and 9# appear. The peak height value is multiplied by the integral of the chromatogram, the data are shown in the table 6, and the difference is more obvious.
TABLE 6 chromatogram peak processing table for retention time periods of different fibers from 9.2min to 9.54min
If the product of the peak height value and the chromatogram integral is less than 1500, the regenerated polyester fiber is judged to be the physical and chemical recovery method produced by adopting the viscosity adjusting process. By using the method, seven physical and chemical recovery method regenerated polyester fiber samples produced by adopting a viscosity adjusting process, such as 1#, 3#, 4#, 6#, 7#, 8# and 9# can be identified by the skilled person.
Claims (2)
1. A method for identifying regenerated terylene by a physical and chemical recovery method comprises the following steps:
(1) pretreating a sample: taking 5g of sample, adding the prepared sulfolane-acetonitrile dissolving precipitant, oscillating for 30min at 180 ℃, cooling, performing centrifugal separation again, taking supernatant, putting the supernatant into a refrigerator for cold storage for more than 8 hours, taking out, filtering, and then putting to room temperature for high performance liquid chromatography detection; the bath ratio of the sample to the sulfolane-acetonitrile dissolution precipitant is 1: 25, and the volume ratio of the sulfolane to the acetonitrile is 80: 20;
(2) and (3) high performance liquid chromatography detection: performing chromatographic detection on the supernatant, wherein a chromatographic column is XDB C18, the particle size is 5 microns, the particle size is 250mm multiplied by 4.6mm, the flow rate is 1.0mL/min, the column temperature is 30 ℃, the sample injection amount is 10.0 microns L, a detector is a diode array detector DAD, the detection wavelength is 254nm, a mobile phase 1 is methanol, a mobile phase 2 is 10% methanol/90% water, and the gradients of the mobile phase 1 and the mobile phase 2 are as follows: at 0min, the mobile phase 1 accounts for 20%, and the mobile phase 2 accounts for 80%; at 15min, the mobile phase 1 accounts for 80%, and the mobile phase 2 accounts for 20%; at 20min, the mobile phase 1 accounts for 100%, and the mobile phase 2 accounts for 0%; at 35min, the mobile phase 1 accounts for 100%, and the mobile phase 2 accounts for 0%;
(3) judging fibers: intercepting high performance liquid chromatogram data of the retention time period of 9.2 min-9.54 min, multiplying the peak height value by chromatogram integral, and if the product is less than 1500, judging to adopt the physical and chemical recovery method regenerated polyester fiber produced by the viscosity adjusting process.
2. The method for discriminating the regenerated terylene according to the physical chemical recovery method of claim 1, which is characterized in that: in the pretreatment of the sample, the centrifugal speed adopted by the centrifugal separation is 5000r/min, and the centrifugal separation time is 5 min.
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