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Solid phase extraction and enrichment method of nitrogen-containing compounds in diesel fuel

A nitrogen compound and solid-phase extraction column technology, which is applied in the petroleum industry, refined hydrocarbon oil, instruments, etc., can solve the problems of separation crossover between components, large amount of solvent consumption, long time, etc., and achieve small separation crossover and solvent consumption Less, the effect of improving the separation efficiency

Active Publication Date: 2016-07-20
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of the present invention is to provide a method for separating and enriching nitrogen-containing compounds in diesel oil samples using solid-phase extraction technology, in order to solve the problem of serious separation and crossover between components, long time and solvent Problems such as large amount

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  • Solid phase extraction and enrichment method of nitrogen-containing compounds in diesel fuel
  • Solid phase extraction and enrichment method of nitrogen-containing compounds in diesel fuel

Examples

Experimental program
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Effect test

Embodiment 1

[0035] Pack 3.5g of silica gel-acidic alumina stationary phase with 10wt% acidic alumina content in the solid phase extraction column, wet with 2mL of the first eluent (the volume ratio of n-pentane to dichloromethane is 1:1) .

[0036] Use a pipette gun to take 2mL of Qingyang Petrochemical catalytic cracked diesel oil into the upper part of the solid phase extraction column and be completely absorbed by the stationary phase. Rinse the solid-phase extraction column with 8 mL of the first eluent to obtain saturated hydrocarbons and aromatic hydrocarbons, which are designated as component 1. Rinse the solid-phase extraction column with 10 mL of the second eluent (the volume ratio of dichloromethane and ethanol is 90:10) to obtain nitrogen-containing compounds, which are designated as component 2. Rinse the solid-phase extraction column with 10 mL of ethanol to obtain heavy components such as colloids, which are recorded as component 3. Solvents in saturated hydrocarbons, arom...

Embodiment 2

[0046] 4.0 g of silica gel-alumina stationary phase with an alumina content of 20 wt % was filled in the solid phase extraction column, and wetted with 2 mL of the first eluent.

[0047] Use a pipette gun to take 1.5mL Karamay Petrochemical catalytic cracked diesel oil into the upper part of the solid phase extraction column and be completely absorbed by the stationary phase. Rinse the solid-phase extraction column with 8 mL of the first eluent to obtain saturated hydrocarbons and aromatic hydrocarbons, which are designated as component 1. Rinse the solid-phase extraction column with 10 mL of the second eluent to obtain a nitrogen-containing compound, which is recorded as component 2. Rinse the solid-phase extraction column with 10 mL of ethanol to obtain heavy components such as colloids, which are recorded as component 3. Solvents in saturated hydrocarbons, aromatics and nitrogen-containing compounds were removed by rotary evaporator and nitrogen purge.

[0048] GC-NCD was...

Embodiment 3

[0056] 4.0 g of silica gel-alumina stationary phase with an alumina content of 40 wt % was filled in the solid phase extraction column, and wetted with 2 mL of the first eluent.

[0057] Use a pipette gun to take 2mL of Changqing Petrochemical catalytic cracked diesel oil into the upper part of the solid phase extraction column and be completely absorbed by the stationary phase. Rinse the solid-phase extraction column with 8 mL of the first eluent to obtain saturated hydrocarbons and aromatic hydrocarbons, which are designated as component 1. Rinse the solid-phase extraction column with 10 mL of the second eluent to obtain a nitrogen-containing compound, which is recorded as component 2. Solvents in saturated hydrocarbons, aromatics and nitrogen-containing compounds were removed by rotary evaporator and nitrogen purge. Enrichment of nitrogen-containing compounds in Qingyang Petrochemical Catalytic Cracking Diesel Oil can be completed in only 20 minutes by adopting the inventi...

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Abstract

The present invention relates to a solid phase extraction and enrichment method of nitrogen-containing compounds in diesel fuel. Diesel fuel is divided into non-nitrogenous components (saturated hydrocarbons, aromatic hydrocarbons, and sulfur-containing compounds) and nitrogen-containing compounds. The method comprises the specific steps of: wetting a solid phase extraction column with a first eluent before addition of a diesel fuel sample; then adding diesel fuel sample from an upper layer of the solid phase extraction column to completely adsorb the sample on the solid phase, rinsing the solid phase extraction column with the first eluent, and extracting saturated hydrocarbons and aromatic hydrocarbons; and continuing to rinse the solid phase extraction column with a second eluent, and extracting the nitrogen-containing compounds. The solid-phase extraction can quick enrich nitrogen-containing compounds in the diesel fuel sample, and solves the problems of nitrogen compounds in diesel fuel serious component cross, long time and a large amount of solvent in a traditional method for diesel oil separation.

Description

technical field [0001] The invention relates to a method for solid-phase extraction and enrichment of nitrogenous compounds in diesel oil. Background technique [0002] Nitrogen compounds in diesel have the following hazards: During the storage of diesel, nitrogen compounds are easily oxidized to form colloids and sediments, which affect the stability of diesel; nitrogen compounds in diesel will cause changes in the color of diesel; nitrogen compounds in diesel are burning Nitrogen oxides are produced during the process, which can easily cause poisoning of motor vehicle exhaust conversion catalysts, and nitrogen oxides are also the main pollutants emitted by motor vehicles. Therefore, reducing the nitrogen content in diesel is very critical. According to the needs of the development of diesel denitrogenation technology, it is of great significance to establish qualitative and quantitative methods for various nitrogen-containing compounds in diesel fractions to provide basic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C10G25/00G01N30/14
Inventor 史得军王春燕林骏马晨菲赫丽娜杨晓彦霍明辰汪艳薛慧峰肖占敏
Owner PETROCHINA CO LTD
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