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Method for determining the content of hydrocarbons and oxygen-containing compounds in Fischer-Tropsch synthetic oil

A technology for Fischer-Tropsch synthesis of oils and compounds, applied in the field of analysis and detection, can solve the problems of high carrier gas requirements, low detector utilization, poor performance, etc., to reduce the number of components, reduce mutual interference, and prolong service life. Effect

Pending Publication Date: 2020-06-19
YANKUANG ENERGY R&D CO LTD
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

One-dimensional chromatography uses a high-efficiency capillary column to separate the various components in the oil, and then uses peak area normalization for quantification. However, due to the complex composition of Fischer-Tropsch synthetic oil, the output of hydrocarbons and oxygenates There is a large amount of overlapping peaks, and ordinary gas chromatography is not good at separating them
Multidimensional chromatography is to connect two or more chromatographic columns through valves, which can get better separation effect, but it is often only suitable for the accurate quantification of a certain part of the compound. Representative methods such as SH / T 0663 are only suitable for testing gasoline. Some oxygenated compounds below C6 have higher accuracy; SH / T 0741 is only effective for testing hydrocarbons below C12 in gasoline, and they cannot solve the mutual interference problem between some oxygenated compounds and aromatic compounds , and cannot meet the test requirements for the content of hydrocarbons and oxygenates in Fischer-Tropsch synthetic oil
[0004] CN102079987A, CN104749298B, and CN106947515B all disclose methods for separating different types of compounds in crude oil or heavy oil by solid phase extraction, and the oil is separated into various hydrocarbons such as alkanes and aromatics and colloidal parts, but all mainly focus on the hydrocarbons therein. No further analysis of the oxygenates in the colloids was carried out, and none of these analytical methods were applicable to Fischer-Tropsch synthetic oils with large differences in composition
However, the oxygen selective ionization detector does not have a qualitative function, and cannot distinguish the carbon number and type of oxygen-containing compounds at all. All compounds need to be qualified by standard samples
Also, when the number of oxygenates is high, it is not possible to tell whether a single chromatographic peak represents a pure substance
In these respects, its performance is far inferior to that of mass spectrometers
In addition, the oxygen selective ionization detector includes a high-temperature cracking device, which is very expensive, has high requirements on the carrier gas, and has a very high failure rate, and the maintenance and repair costs in the later period are very high.
The use of this detector is still low today

Method used

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  • Method for determining the content of hydrocarbons and oxygen-containing compounds in Fischer-Tropsch synthetic oil
  • Method for determining the content of hydrocarbons and oxygen-containing compounds in Fischer-Tropsch synthetic oil
  • Method for determining the content of hydrocarbons and oxygen-containing compounds in Fischer-Tropsch synthetic oil

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Experimental program
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Effect test

Embodiment 1

[0074] Establishment of compound qualitative database:

[0075] 1) carry out the analysis of gas chromatography-mass spectrometry to hydrocarbon and oxygenated compound standard substance, determine their retention time;

[0076] 2) Select a plurality of common samples of Fischer-Tropsch synthetic oil, split them into hydrocarbon part and oxygen-containing compound part by solid phase extraction method, conduct gas chromatography-mass spectrometry analysis respectively, and determine the compounds corresponding to each retention time by mass spectrometry;

[0077] 3) For hydrocarbons and oxygenated compounds, take normal alkanes and 2-n-ketones as reference components respectively, calculate the retention index of each compound, and correspond the retention index to the compound one by one to obtain the qualitative database of hydrocarbon compounds and the qualitative database of oxygenated compounds, some of the results are shown in Table 1 and Table 2.

[0078]Table 1 Parti...

Embodiment 2

[0090] Determination of hydrocarbon and oxygenate content in Fischer-Tropsch synthetic light oil:

[0091] 1) Collect the Fischer-Tropsch synthetic oil obtained from the Fischer-Tropsch synthesis unit, cut the Fischer-Tropsch synthetic oil through a real boiling point device, and collect light oil with a boiling point less than 250°C;

[0092] 2) After the silica gel was activated at a constant temperature at 150°C for 5 hours, it was taken out, packed into a solid phase extraction column to obtain a stationary phase, and the packing height was 40mm, and then the silica gel was wetted with n-hexane;

[0093] 3) Accurately weigh 2g of light oil, transfer it to a solid-phase extraction column, add 1mL of n-hexane to rinse to make the light oil adsorb on the stationary phase, and mix with 35mL of n-hexane and 20mL of dichloromethane-ethanol respectively Solution (volume ratio: 9:1) washes the stationary phase to ensure that the washing speed is basically controlled at 3.0mL / min; ...

Embodiment 3

[0103] Determination of hydrocarbon and oxygenate content in Fischer-Tropsch synthetic heavy oil:

[0104] 1) Collect the Fischer-Tropsch synthetic oil obtained from the Fischer-Tropsch synthesis unit, cut the Fischer-Tropsch synthetic oil through a real boiling point device, and collect heavy oil with a boiling point greater than 250°C;

[0105] 2) After the silica gel was activated at a constant temperature at 150°C for 5 hours, it was taken out, packed into a solid phase extraction column to obtain a stationary phase, and the packing height was 40mm, and then the silica gel was wetted with n-hexane;

[0106] 3) Accurately weigh 2g of heavy oil, transfer it to a solid-phase extraction column, add 1mL of n-hexane to rinse to make the light oil adsorb on the stationary phase, and mix with 35mL of n-hexane and 20mL of dichloromethane-ethanol respectively Solution (volume ratio: 9:1) washes the stationary phase to ensure that the washing speed is basically controlled at 3.0mL / mi...

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Abstract

The invention relates to a method for determining the content of hydrocarbons and oxygen-containing compounds in Fischer-Tropsch synthetic oil. The method comprises the following steps: separating theFischer-Tropsch synthetic oil through a solid-phase extraction method to obtain a hydrocarbon mixed component and an oxygen-containing compound mixed component; carrying out gas chromatography-massspectrometry analysis, determining a reference component in an obtained spectrogram, calculating a retention index of each peak, determining hydrocarbons or oxygen-containing compounds corresponding to each peak according to the retention indexes and a compound qualitative database, and obtaining the content of each hydrocarbon or oxygen-containing compound according to the peak area. Compared with the prior art, according to the invention, the method has the advantages that rapid separation of hydrocarbons and oxygen-containing compounds in the Fischer-Tropsch synthetic oil is realized through a solid phase extraction method, mutual interference of hydrocarbons and oxygen-containing compounds in the Fischer-Tropsch synthetic oil in retention time is effectively eliminated through GC-MS, and rapid qualitative and quantitative analysis of each component is realized in combination with qualitative advantages of GC-MS and a simple data processing algorithm.

Description

technical field [0001] The invention belongs to the technical field of analysis and detection, and relates to a method for determining the content of hydrocarbons and oxygen-containing compounds in Fischer-Tropsch synthetic oil, in particular to a method for determining the content of hydrocarbons and oxygen-containing compounds in Fischer-Tropsch synthetic oil, which is simple, fast and less disturbing. Method for compound content. Background technique [0002] The research on Fischer-Tropsch synthesis has a history of nearly a hundred years. In recent years, due to the increase of proven reserves of coal and natural gas and the adjustment of energy industry structure in various countries, Fischer-Tropsch synthesis has become one of the research hotspots in the field of energy substitution at home and abroad. Fischer-Tropsch synthetic oil is one of the main products of the Fischer-Tropsch synthesis process. Its main components include alkanes, olefins, naphthenes, aromatics...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88G01N30/06G01N30/12G01N30/34B01D15/10B01D15/42C10G55/02
CPCG01N30/88G01N30/06G01N30/12G01N30/34B01D15/10B01D15/424C10G55/02G01N2030/884G01N2030/8854G01N2030/062G01N2030/126
Inventor 孙启文孙燕
Owner YANKUANG ENERGY R&D CO LTD
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