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Analytical method of phenolic compounds in coal direct liquefaction oil

A technology of phenolic compounds and coal liquefied oil, which is applied to the analysis of materials, material separation, and measuring devices, etc., can solve the problems of overlapping chromatographic peaks, inability to effectively separate, low volatility, etc., to expand the detection range, improve the separation effect, The effect of promoting a complete response

Active Publication Date: 2009-11-18
CCTEG CHINA COAL RES INST
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Problems solved by technology

People such as Shi Quan disclosed in Journal of Mass Spectrometry (V0120, NO.2) that when analyzing phenolic compounds in catalytic cracking diesel oil, wherein phenolic compounds only accounted for 0.2% of the total mass of diesel oil, using N, O-bis(trimethyl Silyl)-2,2,2-trifluoroacetamide (BTSFA) was used as a silicon etherification reaction reagent, and only 44 kinds of phenolic compounds including monomeric phenol, bicyclic and tricyclic compounds in catalytic diesel were qualitatively analyzed. Accurate quantitative analysis of monomeric phenols. In addition, when this method is used for tricyclic higher phenols, there are problems such as serious overlapping of chromatographic peaks and inability to effectively separate them.
[0005] Due to the complex composition of coal liquefied oil, various types, high phenolic content, strong polarity, and low volatility, and the large number of isomers in coal liquefied oil have very similar physical and chemical properties, when using existing methods to analyze phenolic compounds , if direct injection, a considerable number of phenolic homologue peaks overlap seriously, appear double-headed peaks, and cannot be effectively separated; after using derivatization reagents, although the separation effect of some phenolic isomers can be significantly improved, the molecular weight Large, low volatility, high-level phenols with three or more rings have poor separation effect. In addition, the existing methods only use the area percentage method for simple quantitative analysis in terms of quantitative analysis.

Method used

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  • Analytical method of phenolic compounds in coal direct liquefaction oil
  • Analytical method of phenolic compounds in coal direct liquefaction oil
  • Analytical method of phenolic compounds in coal direct liquefaction oil

Examples

Experimental program
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Effect test

Embodiment 1

[0034] Weigh 2 mg of 27 standard monomeric phenolic compound samples (see Table 1 below for details), dissolve them in dichloromethane, and add 12ul N, O-bis(trimethylsilyl) corresponding to each standard monomeric phenol - 2,2,2-trifluoroacetamide (BTSFA) silicon etherification reagent and 20ul pyridine, after the complete reaction, mix the standard phenol with a 25ml volumetric flask for quantification, and place it at room temperature for 12 hours before use. Take mixed phenol standard samples for chromatography-mass spectrometry and gas chromatography analysis to determine the standard retention time of various monomeric phenols. At the same time, take 5ml, 10ml, 15ml, and 20ml standard phenol solutions to establish a four-level calibration table using external standards The percentage method was used for quantitative analysis. Table 1 shows the retention time of the monomeric phenols and the retention time of the derivatives after silicon etherification.

[0035] Table 1...

Embodiment 2

[0039] Same as the chromatographic condition of embodiment 1

[0040] Weigh 100g of coal liquefied oil, add 25ml of NaOH (10%) solution, fully shake in the separatory funnel for 5 minutes, separate the lower layer of water phase after standing for stratification, and repeatedly extract the upper layer of organic layer with NaOH (10%) solution three times, After combining four lower aqueous phases, wash with H 2 SO 4 (10M) solution neutralizes the lower alkali solution and adjusts PH=1, shakes for 5 minutes, puts the layers in a separating funnel for 10 minutes, collects the upper organic layer and then adds Na 2 SO 4 After dehydration, the solution can be enriched to obtain phenolic compounds in coal liquefied oil under the condition of 40°C water bath. Take 1.0 mg of the enriched phenolic compound, add 6.0 ul of BTSFA, and add 6 ul of pyridine, use dichloromethane as solvent, prepare 5 ml of solution in a 5 ml volumetric flask, place it at room temperature for 12 hours, an...

Embodiment 3

[0048] When diphenylphosphoryl chloride (DPPC) is selected as the derivatization reagent, N, O-bis(trimethylsilyl)-2,2,2-trifluoroacetamide (BTSFA) is selected as the derivatization reagent in other conditions Conditions during the time, still can obtain the result identical with example 2.

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Abstract

The invention relates to an analytical method of phenolic compounds in coal direct liquefaction oil, which is characterized by using 10 mass % of NaOH to extract enriched phenolic compounds, then using derivatization reagent BTSFA or DPPC and active agent pyridine to carry out quantitative derivatization reaction to obtain silicone ether derivative solution, and adopting chromatography-mass spectrometry to qualitatively analyze silicone ether derivatives of each free phenol and adopting gas phase chromatography to qualitatively analyze each free phenol. The method has wide detection range, simple and convenient operation and high sensitivity. The invention can qualitatively analyze 54 types of monomer phenolic compounds and 27 types of monomer phenolic compounds, and can be widely used for enrichment and analysis of phenolic compounds in coal direct liquefaction oil.

Description

technical field [0001] The invention relates to the field of direct coal liquefaction, in particular to an analysis method for phenolic compounds in direct coal liquefaction oil. Background technique [0002] Coal direct liquefaction (hereinafter referred to as "coal liquefaction") is one of the new coal chemical technologies that can effectively alleviate my country's oil shortage, improve primary energy utilization efficiency, and reduce serious pollution caused by direct coal utilization. [0003] The content of phenolic compounds in primary crude oil obtained from coal liquefaction is as high as 20%. These phenolic compounds will not only increase the hydrogen consumption of the process and increase the cost of coal liquefied oil in the subsequent upgrading process of coal liquefied oil, but also their reaction The generated water will adversely affect the activity and life of the catalyst, and increase the severity of the subsequent hydrogenation reaction. At the same ...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/08G01N30/28G01N30/72
Inventor 毛学锋李文博朱晓苏史士东杜淑凤高振楠张晓静胡发亭朱肖曼刘敏
Owner CCTEG CHINA COAL RES INST
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