CN113960189A - Detection method of bio-based degradable material poly (butylene adipate)/terephthalate) - Google Patents
Detection method of bio-based degradable material poly (butylene adipate)/terephthalate) Download PDFInfo
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Abstract
The invention belongs to the field of analysis and detection, and relates to a detection method of a bio-based degradation material polybutylene adipate/terephthalate (PBAT), which adopts a thermal cracking gas-mass spectrometry method to perform qualitative and/or quantitative analysis on the polybutylene adipate/terephthalate (PBAT). The method provided by the invention can be used for qualitatively and quantitatively detecting the content of PBAT in the degradable plastic product without carrying out complicated, harsh and long-time pretreatment processes. The method is simple, convenient, rapid and accurate, and is suitable for qualitative, quantitative and rapid screening and detection of the PBAT cracking component of the degradable material. The detection method is simple and easy to operate, and accurate in result.
Description
Technical Field
The invention belongs to the field of analysis and detection, and particularly relates to a quick detection method of a bio-based degradation material poly (butylene adipate terephthalate) (PBAT).
Background
The information in this background section is only for enhancement of understanding of the general background of the invention and is not necessarily to be construed as an admission or any form of suggestion that this information forms the prior art that is already known to a person of ordinary skill in the art.
The poly (butylene adipate/terephthalate) (PBAT) belongs to thermoplastic biodegradable plastics, is a copolymer of butylene adipate and butylene terephthalate, has the characteristics of both PBA and PBT, and has better ductility and elongation at break as well as better heat resistance and impact performance; in addition, the biodegradable plastic has excellent biodegradability, and is one of the best degradable materials which are very active in the research of the current biodegradable plastics and are applied to the market.
In GB/T32366-. The existing PBAT detection means only stay in infrared spectrum, terminal carboxyl content, intrinsic viscosity, molecular weight and distribution thereof, mechanical property and contact angle, and the means can not realize qualitative and quantitative detection of PBAT.
The pyrolysis gas chromatography-mass spectrometry combines the pyrolysis technology and the gas chromatography-mass spectrometry technology to realize on-line analysis, and has the characteristics of simple equipment, convenient analysis operation, high sensitivity and separation efficiency, high analysis speed and large information amount. Under the set cracking condition, the high molecules are rapidly heated and are rapidly cracked into volatile small molecules, the volatile small molecules enter a chromatographic column under the action of carrier gas for separation and analysis, the volatile small molecules are detected by a detector, and then the cracking chromatogram of the substances is obtained through an online workstation connected with a mass spectrometer, so that the relationship among the composition, the structure and the physical properties of the high molecular substances can be qualitatively and quantitatively researched. There are researches summarizing 163 standard cracking chromatograms and thermograms of representative synthetic and natural macromolecules, and giving corresponding mass spectrograms for characteristic cracking products of each substance, and the structures of the characteristic cracking products can be conveniently confirmed through direct comparison with the mass spectrograms, thereby deducing the compositions and structures of complex polymer systems (such as copolymers and multi-component blends). The method is currently applied to the component analysis of high polymer polymers such as chlorinated paraffin, polyester fiber, molded silicone rubber, biomass and the like.
However, the inventor finds that: the existing thermal cracking gas chromatography-mass spectrometry technology adopts solid sample injection, can only determine the quality of PBAT and other polymers, and cannot determine the quantity.
Disclosure of Invention
In order to overcome the problems, the invention provides a method for rapidly detecting poly (butylene adipate terephthalate) (PBAT) serving as a bio-based degradation material. The method is simple, convenient, rapid and accurate, and is suitable for qualitative and quantitative rapid screening and detection of the PBAT cracking component of the degradable material. The detection method is simple and easy to operate, and accurate in result.
In order to achieve the technical purpose, the invention adopts the following technical scheme:
in a first aspect of the present invention, a method for rapidly detecting poly (butylene adipate/terephthalate) as a bio-based degradable material is provided, which comprises:
the method adopts a thermal cracking gas-mass combination method to carry out qualitative or quantitative analysis on the degradable biological product containing the poly-adipic acid/butylene terephthalate.
The method is used for detecting the components and the content of the fully biodegradable material PBAT of the fully biodegradable plastic and the product based on the pyrolysis gas chromatography-mass spectrometry technology, and mainly comprises the steps of carrying out pyrolysis temperature on the fully biodegradable material PBAT, carrying out gas quality test parameters, screening standard substances, determining characteristic fragments and checking multi-component detection interference factors.
Research and development find that: the thermal cracking gas chromatography-mass spectrometry technology has the main problems in qualitative and quantitative identification of a bio-based degradation material PBAT, namely selection of characteristic substances, how to effectively separate the characteristic substances in the PBAT, and avoiding/reducing influence of interfering substances, so that the method is the key point for realizing accurate determination and quantification. Therefore, on the basis of long-term system research, the invention finds out through a large number of experiments: by matching the pretreatment process and the cracking process, two characteristic substances of 1, 6-dioxacyclododecane-7, 12-dione (a polymer of adipic acid and butanediol) and benzoic acid in the PBAT can be thermally cracked out from the PBAT and used as the basis of qualitative analysis, and the peak area of the 1, 6-dioxacyclododecane-7, 12-dione (a polymer of adipic acid and butanediol) is quantitatively analyzed to avoid interference and achieve better qualitative and quantitative analysis effects.
Furthermore, in the quantitative analysis process of the poly (butylene adipate/terephthalate), the peak area of 1, 6-dioxacyclododecane-7, 12-dione is taken as the quantitative basis.
Further, the specific conditions of the gas chromatography-mass spectrometry combination are that the temperature is kept at 40-45 ℃ for 2-3 min, then the temperature is increased to 280-290 ℃ at 20-25 ℃/min, and the temperature is kept for 5-6 min; the sample inlet temperature is 280-290 ℃, the split ratio is 20: 1-1.5, and the auxiliary heating area is 300-310 ℃; preferably, the temperature is kept for 2min at 40 ℃, and then is raised to 280 ℃ at 20 ℃/min and kept for 5 min; the sample inlet temperature is 280 ℃, the split ratio is 20:1, and the auxiliary heating zone is 300 ℃.
Further, the specific conditions of thermal cracking are: keeping the temperature at 50-55 ℃ for 1-1.2 s, then increasing the temperature to 350-355 ℃ at 20-22 ℃/ms, keeping the temperature for 8-10 s, keeping the temperature of a transmission line at 300-305 ℃, and keeping the temperature of a valve box at 300-305 ℃; preferably, 50 ℃ is maintained for 1s, then 20 ℃/ms is increased to 350 ℃, the temperature is maintained for 8s, the temperature of the transmission line is 300 ℃, and the temperature of the valve box is 300 ℃.
Further, the preparation method of the PBAT standard solution comprises the following steps: the PBAT standard solution is prepared by using dichloromethane as a solvent, and preferably, the concentration of the PBAT standard solution is 1000 mg/L.
Further, the preparation method of the sample solution comprises the following steps: and crushing the sample, drying to constant weight, and dissolving in a dichloromethane solution for later use.
Furthermore, the standard solution, the sample solution and the blank solution are filtered before being analyzed by a thermal cracking gas chromatograph-mass spectrometer.
Further, the sample injection amount of the sample is 2-3 muL.
In a second aspect of the present invention, a rapid detection system for poly (butylene adipate/terephthalate) as a bio-based degradable material is provided, which comprises: a thermal cracking-gas chromatography-mass spectrometer, a weighing device, a crushing device and an ultrasonic generator.
In a third aspect of the invention, the application of the combined use of thermal cracking gas in the detection of bio-based degradation materials is provided.
In the present invention, "PBAT" means: poly (butylene adipate/terephthalate).
The invention has the beneficial effects that:
(1) the method provided by the invention can be used for qualitatively and quantitatively detecting the content of PBAT in the degradable plastic product without carrying out complicated, harsh and long-time pretreatment processes.
(2) The PBAT cracking characteristic product 1, 6-dioxacyclododecane-7, 12-diketone has a good linear relation in the range of 10 mg/L-250 mg/L, the recovery rate is 92.8% -101.8% under the three addition levels of 10mg/L, 50mg/L and 250mg/L, the relative standard deviation is within 11%, and the robustness meets the requirement.
(3) The method is simple, convenient, rapid and accurate, and is suitable for qualitative and quantitative rapid screening and detection of the PBAT cracking component of the degradable material. The detection method is simple and easy to operate, and accurate in result.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate exemplary embodiments of the invention and together with the description serve to explain the invention and not to limit the invention.
FIG. 1 is a chromatogram of 1, 6-dioxacyclododecane-7, 12-dione, which is a characteristic peak of a PBAT cleavage product in example 1 of the present invention;
FIG. 2 is a mass spectrum of 1, 6-dioxacyclododecane-7, 12-dione in example 1 of the present invention;
FIG. 3 is a graph showing the working curve of a PBAT standard solution in example 1 of the present invention (external standard method).
Detailed Description
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
A method for rapidly detecting a biodegradable material poly (butylene adipate)/terephthalate) comprises the following steps:
the present invention is described in further detail below with reference to specific examples, which are intended to be illustrative of the invention and not limiting.
In the following examples, specific information of the instruments used is: a thermal cracking-gas chromatography (Py-GC-MS, Agilent, USA), an electronic balance (Sidolisi scientific instruments Beijing, Inc., precision 0.1 mg), a high-speed universal pulverizer (Tester instruments, Inc., Tianjin), and an ultrasonic generator.
The specific information of the reagents used is: poly (butylene adipate terephthalate) (PBAT, CAS: 55231-08-8), purity ≥ 99%, available from Michael reagents, Inc.; dichloromethane, pure in chromatography, purchased from national pharmaceutical group, ltd; the laboratory water is first-grade water specified in GB/T6682, and is prepared by self.
Example 1: quantitative/qualitative detection of samples
The invention adopts a certain production enterprise to provide 4 types of biodegradable plastic products containing PBAT, namely: I. biodegradable plastic films, biodegradable lunch boxes II, biodegradable shopping bags II and biodegradable express packaging films IV respectively represent the most widely used and most representative degradable materials, 3 batches of samples are selected for each type, and the specific information is shown in the following table 1.
TABLE 1 Experimental sample information
1) Preparation of PBAT Standard solution
Because the solubility of PBAT in dichloromethane solvent is better, the invention adopts dichloromethane as solvent to prepare PBAT standard solution (1000 mg/L), 0, 0.1, 1 and 10mL of standard mother liquor are respectively absorbed into a 100mL volumetric flask, and the volume is determined by using dichloromethane and then the machine is used for detection.
2) Preparation of sample solutions
Crushing the sample to the diameter of less than or equal to 0.3cm, drying at 105 ℃ to constant weight, weighing 0.1-0.3 g of the sample, accurately weighing the sample to 0.1mg, adding 100mL of dichloromethane solution into a glass volumetric flask, dissolving to constant volume, filtering, and loading on a machine for later use. Meanwhile, a blank test is carried out by taking a dichloromethane solution as a blank test solution.
3) Detection by thermal cracking-gas chromatography
After filtering the prepared PBAT series concentration standard solution, sample test solution and blank test solution, taking 2 mu L for Py-GC-MS detection, wherein the instrument conditions are shown in Table 2.
TABLE 2 thermal cracking/gas mass apparatus model and parameter information
4) Quantitative/qualitative result analysis
FIGS. 1 and 2 show chromatogram and mass spectrum of PBAT cleavage feature product 1, 6-dioxacyclododecane-7, 12-dione, respectively, and 10.10min chromatogram peak is 1, 6-dioxacyclododecane-7, 12-dione. The PBAT solutions with 5 concentrations are selected for determination, a standard working curve (figure 3) is drawn, and the linear equation, the correlation coefficient, the detection limit and the quantitative limit of the standard curve are shown in tables 3 and 4.
TABLE 3 Linear Range versus Standard Curve
TABLE 4 detection limit, quantitation limit test results
As can be seen from Table 3, the standard calibration curve of each plasticizer has good linear correlation coefficient which is greater than 0.995, linear range of 10-500 mg/L and wide linear range, and provides a basis for the accuracy of subsequent measurement data.
Further analysis shows that the PBAT generally adopts Adipic Acid (AA), terephthalic acid (PTA) and 1, 4-Butanediol (BDO) as raw materials, tetra-n-butyl titanate and antimony trioxide as composite catalysts, and adopts a direct melt polymerization method to prepare poly (adipic acid)/butylene terephthalate (PBAT). In order to research a qualitative and quantitative method for PBAT high-molecular degradation polymers, the method is obtained by reversely deducing a PBAT synthesis process, wherein a PBAT cracking product mainly comprises Adipic Acid (AA), terephthalic acid (PTA) and 1, 4-Butanediol (BDO) monomer or an esterification product at a certain cracking temperature, the cracking product is explored from the cracking temperature of 700 ℃ to 350 ℃, and 1, 6-dioxacyclododecane-7, 12-diketone (a polymer of adipic acid and butanediol) and benzoic acid appear in the cracking product at the cracking temperature of 350 ℃, so that the cracking temperature of 350 ℃ is determined. The PBAT is characterized by two characteristic peaks of 1, 6-dioxacyclododecane-7, 12-dione and benzoic acid, when the PBAT is quantified, the cracked product of the polybutylene terephthalate (PBT) is considered to contain the benzoic acid, when the sample contains the PBT, positive deviation can occur by using the benzoic acid for quantification, so the PBAT quantification only considers the peak area of the 1, 6-dioxacyclododecane-7, 12-dione, and the peak shape is standard without interfering with the front and the back peaks.
Example 2: accuracy and precision experiment of method
The test solutions were prepared and tested as in example 1.
The blank simulated liquid (dichloromethane solution) was subjected to the recovery rate and relative standard deviation test, and the results of the method recovery rate and precision test are shown in table 5.
TABLE 5 accuracy and precision test
Example 3: comparison of thermal cracking gas chromatography-mass spectrometry technique and nuclear magnetic resonance (hydrogen spectroscopy) method
The test solutions were prepared and tested as in example 1.
In order to verify the reliability of the method, the invention respectively adopts the nuclear magnetic resonance method and the thermal cracking gas chromatography-mass spectrometry technology to select a certain biodegradable shopping bag (marked as PBAT + CaCO)3) The results of 3 batches of the product were tested and are shown in table 6, and it can be seen from the test results that the relative deviation of the two test methods at the level of 20% of PBAT content is within 10%.
TABLE 6 comparison of results of different test methods
Example 4: detection of class 4 typical biodegradable plastic articles containing PBAT
The test solutions were prepared and tested as in example 1.
4 types of typical biodegradable plastic products containing PBAT are selected, the PBAT content of each type of the plastic products in 3 batches is detected, and the results are shown in Table 7.
TABLE 74 content of typical biodegradable plastic articles containing PBAT
The PBAT content of the four typical biodegradable plastic products except the biodegradable lunch box is in the range of a standard curve, and the PBAT content is detected on a computer after the sample is diluted by ten times, so that the data parallelism is better, and the relative deviation is within 0.2-3.5 percent.
Therefore, the method provided by the invention can be used for qualitatively and quantitatively detecting the content of PBAT in the degradable plastic product without carrying out complicated, harsh and long-time pretreatment processes. The PBAT cracking characteristic product 1, 6-dioxacyclododecane-7, 12-diketone has a good linear relation in the range of 10 mg/L-250 mg/L, the recovery rate under the three addition levels of 10mg/L, 50mg/L and 250mg/L is 92.8-101.8%, the relative standard deviation is within 11%, and the robustness meets the requirement. The detection method is simple and easy to operate, and accurate in result.
It should be noted that the above-mentioned embodiments are only preferred embodiments of the present invention, and the present invention is not limited thereto, and although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications and equivalents can be made in the technical solutions described in the foregoing embodiments, or equivalents thereof.
Claims (10)
1. A detection method of a bio-based degradable material poly (butylene adipate)/terephthalate) is characterized by comprising the following steps:
carrying out qualitative or quantitative analysis on the degradable biological product containing poly (adipic acid)/butylene terephthalate by adopting a thermal cracking gas-mass combination method;
in the quantitative analysis process of the degradable biological product containing poly-adipic acid/butylene terephthalate, the peak area of 1, 6-dioxacyclododecane-7, 12-diketone is taken as the quantitative basis.
2. The method for detecting poly (butylene adipate/terephthalate), a biodegradable material, according to claim 1, wherein said qualitative or quantitative analysis comprises: and (3) carrying out combined detection of thermal cracking treatment and gas chromatography-mass spectrometry.
3. The method for detecting the poly (butylene adipate)/terephthalate) as the bio-based degradable material according to claim 2, wherein the specific conditions of the gas chromatography-mass spectrometry are that the temperature is kept at 40-45 ℃ for 2-3 min, then the temperature is increased to 280-290 ℃ at 20-25 ℃/min, and the temperature is kept for 5-6 min; the sample inlet temperature is 280-290 ℃, the split ratio is 20: 1-1.5, and the auxiliary heating area is 300-310 ℃.
4. The method for detecting poly (butylene adipate/terephthalate) as a biodegradable material according to claim 2, wherein the thermal cracking treatment is performed under the following specific conditions: keeping the temperature at 50-55 ℃ for 1-1.2 s, then raising the temperature to 350-355 ℃ at 20-22 ℃/ms, keeping the temperature for 8-10 s, keeping the temperature of a transmission line at 300-305 ℃, and keeping the temperature of a valve box at 300-305 ℃.
5. The method for detecting the biodegradable material poly (butylene adipate/terephthalate) as claimed in claim 2, wherein in the GC-MS detection, methylene chloride is used as a solvent to prepare a poly (butylene adipate/terephthalate) standard solution.
6. The method for detecting the polybutylene adipate/terephthalate as the biodegradable material according to claim 5, wherein the concentration of the polybutylene adipate/terephthalate standard solution is 800-1200 mg/L.
7. The method for detecting the poly (butylene adipate)/terephthalate) as the bio-based degradable material according to claim 2, wherein in the gas chromatography-mass spectrometry detection, the preparation method of the sample solution comprises the following steps: the degradable biological product containing poly-adipic acid/butylene terephthalate is crushed, dried to constant weight and dissolved in dichloromethane solution for standby.
8. The method for detecting poly (butylene adipate/terephthalate) as claimed in claim 2, wherein the standard solution, the sample solution and the blank solution are filtered before being analyzed by the thermal cracking gas chromatograph-mass spectrometer in the gas chromatography-mass spectrometer.
9. The method for detecting the poly (butylene adipate)/terephthalate) as the bio-based degradable material according to claim 2, wherein the sample introduction amount of the sample is 2-3 μ L in the gas chromatography-mass spectrometry detection.
10. The method for detecting the poly (butylene adipate/terephthalate) as the bio-based degradable material of claim 1, wherein the poly (butylene adipate/terephthalate) containing degradable biological product is a biodegradable mulching film, a biodegradable lunch box, a biodegradable shopping bag or a biodegradable express packaging film.
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