CN111103364A - PET content detection method - Google Patents
PET content detection method Download PDFInfo
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- CN111103364A CN111103364A CN201910365642.4A CN201910365642A CN111103364A CN 111103364 A CN111103364 A CN 111103364A CN 201910365642 A CN201910365642 A CN 201910365642A CN 111103364 A CN111103364 A CN 111103364A
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
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Abstract
The invention relates to the field of chemical fiber recycling, in particular to a method for detecting PET content, which comprises the steps of solution preparation, sample preparation, alkaline hydrolysis sample preparation, liquid chromatography detection of PET content and analysis of PET content. Carrying out alcoholysis on the polyester foam by using an alkaline hydrolysis sample, then obtaining a raw material monomer, and carrying out liquid chromatography calibration on sodium phthalate generated by detecting alcoholysis reaction, thereby realizing accurate detection of PET content. The method is simple and convenient to operate, has high detection accuracy, can realize rapid analysis of high-impurity-content samples, and has wide application prospect for polyester regeneration, particularly textile regeneration.
Description
[ technical field ] A method for producing a semiconductor device
The invention relates to the field of polyester chemical raw materials, in particular to a method for detecting PET content.
[ background of the invention ]
China is a large country for producing textiles and clothes, the accumulated stock of waste textiles is nearly hundred million tons, the total amount of fiber processing in China is about 5000 million tons, more than 2000 million tons of waste textiles are generated, the comprehensive utilization amount of the waste textiles is about 300 million tons, the comprehensive utilization rate is only about 15%, and most of old clothes are finally buried or burned as garbage.
The accumulated production of waste textiles in China reaches 1.4 hundred million tons, and the annual consumption of the textiles is increased by more than 12%. According to statistics, the amount of waste textiles produced in China reaches 2000 million tons every year. The production amount of the waste chemical fiber textiles reaches 2 hundred million tons in the case of thirteen five ends. The waste textiles occupy very large resources whether being buried or treated, and are easy to cause secondary pollution. The polyester fiber (PET) is a textile raw material with the largest production and content internationally at present due to high yield and capacity, so the polyester fiber (PET) has very important social significance for recycling the PET.
At present, polyester recycling chemical recycling is adopted, all textiles are reduced to prepare a polymerized monomer, and the prepared raw materials are used for polyester polymerization, so that the product quality is high, but the production cost is high; in the process of recycling polyester by domestic production enterprises at present, an important process is to process textile into foam after washing, and then put the foam into an alcoholysis reaction kettle for reaction, but because the content of PET in the polyester foam is difficult to detect, the uniformity of the input raw materials during the alcoholysis reaction is poor, the error of alcoholysis products is large, the material consumption is large, and the production cost and the ecological environmental protection pressure of the enterprises are large. Therefore, the chemical recovery method of the polyester foam needs to accurately detect the content of PET in the polyester foam so as to obtain an effective raw material ratio, and no effective detection method exists at home and abroad at present.
[ summary of the invention ]
The invention aims to provide a method for detecting the content of PET.
The purpose of the invention is realized by the following technical scheme: a method for detecting the content of PET comprises the following steps:
(I) solution preparation
(1) Preparation of internal standard solution
Weighing 5 g of benzoic acid, putting the benzoic acid into a 500mL graduated beaker, diluting the benzoic acid with N, N-Dimethylformamide (DMF), and carrying out constant volume to prepare an internal standard solution with the benzoic acid concentration of 10 g/L.
(2) Preparation of acetonitrile solution
The measuring cylinder measures 500mL of acetonitrile, and pure water is used for constant volume until the acetonitrile solution with the volume concentration of 25 percent is prepared.
(3) Preparation of eluent
A eluent was prepared by adding 2ml of a trifluoroacetic acid solution to the acetonitrile solution prepared in the above (2).
(II) sampling of samples
A sampler with an inner diameter of 4.0cm-4.5cm and a stainless steel tube with the length of 90cm is adopted to randomly sample in the polyester foam material, and the sampling rate is 30-40%. And (4) taking one sample every time, packaging the sample by using a self-sealing bag, and preparing the sample.
(III) preparation of alkaline hydrolysis sample
(1) Weigh 5.00. + -. 0.001 g of the sample of polyester foam obtained in step (II) into a conical beaker.
(2) Then 3 + -0.01 g of sodium hydroxide and 100 + -0.1 g of ethylene glycol ester are added and the mixture is placed in a stirrer.
(3) A designated cooling pipe is arranged on the conical flask and then placed on a magnetic stirrer, cooling water is conducted,
the stirrer temperature was set at a predetermined temperature, the temperature was raised, and stirring was started at a controlled rotation speed of 200 rpm. Heating is started to control the surface temperature of the stirrer to 350 ℃, and when the foam material is not dissolved yet and cannot be stirred, the stirring is started after the foam material is dissolved to a certain degree. The alkali decomposition reaction was carried out for 70 minutes. After completion of the alkaline hydrolysis, heating was stopped, stirring was carried out, a jack was inserted between the conical flask and the hot plate, and cooling was started.
(4) After cooling, the flask was transferred to a 500ml graduated flask and aligned with the marked line.
(5) A volume pipettor was used to collect 20ml of the sample and place it into a 50ml graduated beaker, 10ml of internal standard solution was added and diluted to the mark with purified water.
(6) About 1 gram was then collected and placed in a spiral tube and diluted with about 50ml acetonitrile to prepare an alkaline hydrolysis sample.
(IV) liquid chromatography detection of PET content
(1) And opening the liquid chromatogram, confirming the residual amount of the eluent, turning on a computer power supply, and simultaneously turning on a detection system of the liquid chromatograph.
(2) And in the measuring process, selecting a schedule parameter setting picture for display, and inputting the cup number, the sample name, the method data name and the times of the sample. And after the input is finished, closing the set picture, putting the sample, starting click measurement, and selecting to execute analysis to start analysis. And obtaining a liquid phase data map after the measurement is finished. Firstly, preparing a sample as an internal standard solution to obtain a characteristic peak area IS of the internal standard solution, and then replacing the sample with a polyester foam sample to obtain a detected PET area.
(3) And (4) shutdown operation, namely selecting to close the measurement interface and clicking to open the measurement interface to finish the shutdown operation of the liquid chromatogram.
(V) analysis of PET content
The invention has the positive effects that:
(1) the polyester foam material contains other various fiber materials, so that the content determined by PET in polyester needs to be determined in the polyester regeneration recycling process, but no effective method can be used for analyzing the polyester foam material containing mixed components at present, so that the effective analysis of the polyester is difficult to perform in the chemical recycling process, and the method effectively monitors substances by adopting a liquid chromatography method, so that the accurate detection of the content of PET in fiber textile materials such as the polyester foam material and the like is realized;
(2) the method for alkaline hydrolysis by adopting the glycol ester and the sodium hydroxide can avoid the influence of other impurity-containing components on the alkaline hydrolysis of the polyester, avoid the influence of other fiber materials on the polyester components, and improve the effectiveness and the accuracy of the detection structure.
(3) The method adopts a liquid chromatography method, is simple and convenient to detect, has low operation feasibility and investment, and is suitable for most of regenerated polyester production enterprises.
[ description of the drawings ]
FIG. 1 is a schematic flow chart of a method for detecting PET content according to the present invention.
[ detailed description ] embodiments
The following provides a specific embodiment of the method for detecting PET content according to the present invention.
Example 1
The purpose of the invention is realized by the following technical scheme: a method for detecting the content of PET comprises the following steps:
(I) solution preparation
(1) Preparation of internal standard solution
Weighing 5 g of benzoic acid, putting the benzoic acid into a 500mL graduated beaker, diluting the benzoic acid with N, N-Dimethylformamide (DMF), and carrying out constant volume to prepare an internal standard solution with the benzoic acid concentration of 10 g/L.
(2) Preparation of acetonitrile solution
The measuring cylinder measures 500mL of acetonitrile, and pure water is used for constant volume until the acetonitrile solution with the volume concentration of 25 percent is prepared.
(3) Preparation of eluent
A eluent was prepared by adding 2ml of a trifluoroacetic acid solution to the acetonitrile solution prepared in the above (2).
(II) sampling of samples
A sampler with the inner diameter of 4.0cm-4.5cm and the length of a stainless steel pipe of 90cm is adopted to randomly sample in the polyester foam material, and the sampling rate is 40 percent. And (4) taking one sample every time, packaging the sample by using a self-sealing bag, and preparing the sample. Samples No. 1, 2 and 3 are sampled, and four samples are taken for each sample.
(III) preparation of alkaline hydrolysis sample
(1) A sample of the polyester foam obtained in step (II) was weighed in an amount of 5.001 g and placed in a conical beaker.
(2) Then 3.01 g of sodium hydroxide and 100.1 g of ethylene glycol ester were added and the mixture was placed in a stirrer.
(3) A designated cooling pipe is arranged on the conical flask and then placed on a magnetic stirrer, cooling water is conducted,
the stirrer temperature was set at a predetermined temperature, the temperature was raised, and stirring was started at a controlled rotation speed of 200 rpm. Heating is started to control the surface temperature of the stirrer to 350 ℃, and when the foam material is not dissolved yet and cannot be stirred, the stirring is started after the foam material is dissolved to a certain degree. The alkali decomposition reaction was carried out for 70 minutes. After completion of the alkaline hydrolysis, heating was stopped, stirring was carried out, a jack was inserted between the conical flask and the hot plate, and cooling was started.
(4) After cooling, the flask was transferred to a 500ml graduated flask and aligned with the marked line.
(5) A volume pipettor was used to collect 20ml of the sample and place it into a 50ml graduated beaker, 10ml of internal standard solution was added and diluted to the mark with purified water.
(6) About 1 gram was then collected and placed in a spiral tube and diluted with about 50ml acetonitrile to prepare an alkaline hydrolysis sample.
(IV) liquid chromatography detection of PET content
(1) And opening the liquid chromatogram, confirming the residual amount of the eluent, turning on a computer power supply, and simultaneously turning on a detection system of the liquid chromatograph.
(2) And in the measuring process, selecting a schedule parameter setting picture for display, and inputting the cup number, the sample name, the method data name and the times of the sample. And after the input is finished, closing the set picture, putting the sample, starting click measurement, and selecting to execute analysis to start analysis. And obtaining a liquid phase data map after the measurement is finished. Firstly, preparing a sample as an internal standard solution to obtain a characteristic peak area IS of the internal standard solution, and then replacing the sample with a polyester foam sample to obtain a detected PET area.
(3) And (4) shutdown operation, namely selecting to close the measurement interface and clicking to open the measurement interface to finish the shutdown operation of the liquid chromatogram.
(V) analysis of PET content
| First measurement | Second measurement | Third measurement | The fourth measurement | Average content | Standard deviation of the mean | |
| 1# | 97.60％ | 93.26％ | 96.59％ | 93.7％ | 95.29％ | 1.8％ |
| 2# | 91.83％ | 91.34％ | 89.79％ | 92.59％ | 91.39％ | 1.0％ |
| 3# | 95.22％ | 94.20％ | 94.70％ | 93.93％ | 94.51％ | 0.5％ |
The foregoing is considered as illustrative only of the preferred embodiments of the invention, and is for the purpose of promoting an understanding of the principles and concepts of the invention, and is not to be construed as limiting the scope of the invention. It should be understood that various modifications, combinations and adaptations may be made without departing from the spirit of the invention and are intended to be included within the scope of the claims.
Claims (1)
1. A method for detecting PET content is characterized by comprising the following steps:
(I) solution preparation
(1) Preparation of internal standard solution
Weighing 5 g of benzoic acid, putting the benzoic acid into a 500mL graduated beaker, diluting the benzoic acid with N, N-Dimethylformamide (DMF), and performing constant volume to prepare an internal standard solution with the benzoic acid concentration of 10 g/L;
(2) preparation of acetonitrile solution
Measuring 500mL of acetonitrile by using a measuring cylinder, and fixing the volume by using pure water until an acetonitrile solution with the acetonitrile volume concentration of 25% is prepared;
(3) preparation of eluent
Adding 2ml of trifluoroacetic acid solution into the acetonitrile solution obtained in the step (2) to prepare a eluent;
(II) sampling of samples
Randomly sampling in the polyester foam by using a sampler with an inner diameter of 4.0cm-4.5cm and a stainless steel tube with the length of 90cm, wherein the sampling rate is 30-40%; taking one sample every time, packaging the sample by using a self-sealing bag, and preparing to obtain a sample;
(III) preparation of alkaline hydrolysis sample
(1) Weighing 5.00 +/-0.001 g of the polyester foam sample obtained in the step (II) and putting the polyester foam sample into a conical beaker;
(2) then adding 3 plus or minus 0.01 g of sodium hydroxide and 100 plus or minus 0.1 g of glycol ester, and putting into a stirrer;
(3) installing a specified cooling pipe on the conical flask, then placing the conical flask on a magnetic stirrer, conducting cooling water, setting the temperature of the stirrer according to the specified temperature, starting to heat, starting stirring at the same time, and controlling the rotating speed to be 200 revolutions per minute; heating to control the surface temperature of the stirrer to 350 ℃, and when the foam material is not dissolved and cannot be stirred, stirring after the foam material is dissolved to a certain degree; carrying out alkali decomposition reaction for 70 minutes; after the alkaline hydrolysis is finished, stopping heating and stirring, inserting a jack between the conical flask and the hot plate, and starting cooling;
(4) after cooling, transferring the mixture into a 500ml graduated flask, and aligning the flask with a marked line;
(5) collecting 20ml by using a positive displacement pipettor, putting the collected 20ml into a 50ml graduated beaker, adding 10ml of internal standard solution, and diluting the standard solution to a marked line by using pure water;
(6) then collecting about 1 g of the mixture, putting the mixture into a spiral tube, and diluting the mixture by using about 50ml of acetonitrile solution to prepare an alkaline hydrolysis sample;
(IV) liquid chromatography detection of PET content
(1) Opening the liquid chromatogram, confirming the residual amount of the eluent, turning on the power supply of a computer, and simultaneously turning on a detection system of the liquid chromatograph;
(2) and in the measuring process, selecting a schedule parameter setting picture for display, and inputting the cup number, the sample name, the method data name and the times of the sample. After the input is finished, closing the set picture, putting a sample, starting to click to measure, and selecting to execute analysis to start analysis; and obtaining a liquid phase data map after the measurement is finished. Firstly, preparing a sample as an internal standard solution to obtain a characteristic peak area IS of the internal standard solution, and then replacing the sample with a polyester foam sample to obtain a detected PET area;
(3) the shutdown operation is carried out, wherein the shutdown operation of the liquid chromatogram is completed by selecting to close and clicking to open on a measurement interface;
(V) analysis of PET content
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910365642.4A CN111103364A (en) | 2019-05-02 | 2019-05-02 | PET content detection method |
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| CN201910365642.4A CN111103364A (en) | 2019-05-02 | 2019-05-02 | PET content detection method |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1143090A (en) * | 1995-05-08 | 1997-02-19 | 国际壳牌研究有限公司 | Method for recirculating mixed polymer containing poly terephthalic acid glycol ester |
| CN104730170A (en) * | 2015-04-09 | 2015-06-24 | 潍坊沃尔特科技有限公司 | Method for detecting m-benzene dimethyl isophthalate-5-sodium sulfonate purity by liquid chromatography |
| CN105561629A (en) * | 2015-12-24 | 2016-05-11 | 上海微谱化工技术服务有限公司 | Separation and analysis detection methods of diphenyl silanediol in PET (polyethylene glycol terephthalate) fiber |
-
2019
- 2019-05-02 CN CN201910365642.4A patent/CN111103364A/en not_active Withdrawn
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1143090A (en) * | 1995-05-08 | 1997-02-19 | 国际壳牌研究有限公司 | Method for recirculating mixed polymer containing poly terephthalic acid glycol ester |
| CN104730170A (en) * | 2015-04-09 | 2015-06-24 | 潍坊沃尔特科技有限公司 | Method for detecting m-benzene dimethyl isophthalate-5-sodium sulfonate purity by liquid chromatography |
| CN105561629A (en) * | 2015-12-24 | 2016-05-11 | 上海微谱化工技术服务有限公司 | Separation and analysis detection methods of diphenyl silanediol in PET (polyethylene glycol terephthalate) fiber |
Non-Patent Citations (2)
| Title |
|---|
| LEI WANG ET AL.: "A Simple Method for Quantifying Polycarbonate and Polyethylene Terephthalate Microplastics in Environmental Samples by Liquid Chromatography−Tandem Mass Spectrometry", 《ENVIRONMENTAL SCIENCE AND TECHNOLOGY LETTERS》 * |
| 杨勇等: "反相高效液相色谱法分析超临界甲醇解聚聚对苯二甲酸乙二醇醋的产物", 《分析化学研究报告》 * |
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Address after: Building 7, No.5, Haitang Road, Yuecheng District, Shaoxing City, Zhejiang Province Applicant after: ZHEJIANG JIAREN NEW MATERIALS Co.,Ltd. Address before: 312071 Zhejiang city of Shaoxing Province on economic and Technological Development Zone Paojiang Road No. 5 Applicant before: ZHEJIANG JIAREN NEW MATERIALS Co.,Ltd. |
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Application publication date: 20200505 |