Method gel-chromatographic analysis of terephthalates compounds

A technology of terephthalic acid and ester compounds, applied in the direction of analyzing materials, material separation, measuring devices, etc., can solve the problem of low product solubility, and achieve the effect of easy repeatability and easy operation

Inactive Publication Date: 2004-09-15
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The mobility used in both systems is relatively low relative to the solubility of the above products, and there are many problems with sample representativeness and reproducibility

Method used

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  • Method gel-chromatographic analysis of terephthalates compounds
  • Method gel-chromatographic analysis of terephthalates compounds
  • Method gel-chromatographic analysis of terephthalates compounds

Examples

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Effect test

Embodiment 1

[0012] The mensuration of embodiment 1 diethylene glycol terephthalate (BHET)

[0013] ①Determination purpose In conjunction with the basic research of supercritical extraction of polyethylene terephthalate (PET), the purity of the chromatographic standard sample diethylene terephthalate (BHET) needs to be determined first.

[0014] ② Source of pure reagent: TCI-EP Terephthalic Acid, manufactured by Tokyo Chemical Industry Co., Ltd., the purity content is not indicated.

[0015] ③Analysis conditions

[0016] Analytical instrument: Shimadzu LC-3A high-performance liquid chromatography; detector: UVD-2 ultraviolet detector; wavelength: 254nm; chromatographic column: GPC-801, inner diameter 8.0mm, length 300mm (produced by Shimadzu Corporation of Japan)

[0017] Experimental conditions Mobile phase: tetrahydrofuran; flow rate: 0.9ml / min; column temperature: 19°C; sample concentration: 0.066g / 100ml; injection volume: 3 microliters.

[0018] Calculation method: Since the reagent ...

Embodiment 2

[0020] Embodiment 2 Determination of pure reagent-dimethyl terephthalate (DMT)

[0021] ① Determining the purpose of polyethylene terephthalate (PET), polytrimethylene terephthalate (PTT) and their polymerized plastics under supercritical extraction, the main monomer generated is terephthalate For dimethyl formate (DMT), a pure reagent must be used as a reference for the chromatographic qualification and quantification of this monomer. Before using this pure reagent, it is necessary to measure the purity of this pure sample.

[0022] ② Source of pure reagent Dimethyl terephthalate (Dimethyl terephthalate, DMT), produced by Aldrich Chem Corp Inc.

[0023] ③Analysis conditions

[0024] Analytical instrument: Shimadzu LC-3A high-performance liquid chromatography; detector: UVD-2 ultraviolet detector; wavelength: 254nm; chromatographic column: GPC-801, inner diameter 8.0mm, length 300mm (produced by Shimadzu Corporation of Japan)

[0025] Experimental conditions Mobile phase: te...

Embodiment 3

[0028] Example 3 Selection of synthetic dipropylene glycol terephthalate (BHPT)

[0029] ① Determining the purpose of polyethylene terephthalate (PTT) in supercritical depolymerization, according to the reaction mechanism, there should be by-product dipropylene glycol terephthalate (BHPT). When testing, terephthalic acid Dipropylene glycol ester (BHPT) standard reagent, however, there is no such supply in the domestic and foreign markets at present, for this reason, need self research, synthesis. The method can measure the products synthesized by the process and carry out evaluation.

[0030] ② Sample source: Sample 1 and Sample 2 are obtained by reacting polyethylene terephthalate (PET) with propylene glycol at 240°C.

[0031] ③Analysis conditions

[0032] Analytical instrument: Shimadzu LC-3A high-performance liquid chromatography; detector: UVD-2 ultraviolet detector; wavelength: 254nm; chromatographic column: GPC-801, inner diameter 8.0mm, length 300mm (manufactured by S...

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Abstract

In the method, following instruments and parameters are adopted: 'Daojin' LC-3A high performance liquid chromatograph, UVD-2 ultraviolet detector, wavelength 254nm, GPC-801 chromatographic column with inner diameter 8.0mm and length 300mm, tetrahydrofuran mobile phase, velocity of flow 0.8-0.9ml / min, column temperature 15-22 deg.C. Analysis is carried out for solution of 100 ml. in density 0.001-0.070 prepared from sample of esters compound of terephthalic acid. The invention solves qualitative analysis and quantitative analysis for dimethyl terephthalate, its esters compound, intermediate product and dimer product, possessing features of convenient operation, easy of repetition.

Description

Technical field: [0001] The invention belongs to a method for analyzing terephthalate compounds, in particular to a method for analyzing terephthalate compounds by gel chromatography. technical background: [0002] Terephthalate compounds are the main raw materials for the synthesis of polymers (polymerized terephthalates), which in turn are the main raw materials for making plastics. In modern times, with the increase of various plastics and polyester products year by year, the disposal of waste polyester products has become an increasingly serious environmental protection problem. The early studies on polyester depolymerization mainly include liquid alcohol depolymerization method and hydrolysis polymerization method, but these methods not only need to add catalyst, but also the selectivity and yield of the monomer-dimethyl terephthalate in the product are low. lower. Recently, the emergence of supercritical extraction technology has brought the research of polyester dep...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/36G01N30/74
Inventor 张昌鸣杨建丽刘振宇
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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