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Separation analyzing method for nitrogen-containing compounds in heavy oil

A technology for the separation and analysis of nitrogen compounds, applied in the direction of material separation, analysis materials, measuring devices, etc., can solve the problems of inability to judge the integrity of nitrogen compounds in the separation and purification effect, and achieve the effect of large sample processing capacity and reduced solvent consumption

Inactive Publication Date: 2017-07-07
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, before using this type of analysis method, it is necessary to separate and purify the nitrogen-containing compounds in the sample. Since it is impossible to directly inject samples for analysis, it is impossible to judge the effect of separation and purification and the integrity of the information on nitrogen compounds in raw materials.
Also, this type of analytical method can only analyze nitrogen compounds in lighter oils

Method used

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  • Separation analyzing method for nitrogen-containing compounds in heavy oil
  • Separation analyzing method for nitrogen-containing compounds in heavy oil
  • Separation analyzing method for nitrogen-containing compounds in heavy oil

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] The fine-pore silica gel was dried in an oven at 120°C to obtain activated silica gel, which was placed in a desiccator and stored away from light for future use. Measure 80mL of hydrochloric acid solution and add it to 40g of the extracted silica gel, stir evenly, let it stand to dry, and the adsorbent turns slightly yellow to make acid-modified silica gel. Insert the absorbent cotton into the bottom of the Soxhlet extraction tube, put the acid-modified silica gel into the chromatographic column with a side tube, and extract with 50mL of dichloromethane for 30min until it is completely wetted and free of bubbles.

[0054] Weigh about 1g of VTB, dissolve it in 2mL of dichloromethane with ultrasonic vibration; fill 40 grams of acid-modified silica gel in a solid-phase extraction column (inner diameter of 28 mm, the same below) with side stream reflux; install the solid-phase extraction column On a solid phase extraction device with a heating and condensing system. Add 5...

Embodiment 2

[0059] This example is used to illustrate that the solid phase extraction method provided by the present invention rapidly separates colloids in Canadian oil sands bitumen vacuum residue (distillation range>524°C) (colloid separation method refers to SH / T 0509-92) and Preparation of non-alkaline components and alkaline components in colloids.

[0060] Weigh 1 gram of the colloidal component (colloid separation according to SH / T 0509-92) sample of Canadian oil sand bitumen vacuum residue (distillation range >524°C), dissolve it in 2 ml of dichloromethane with ultrasonic vibration; Pack 20 grams of acid-modified silica gel in a solid-phase extraction column (inner diameter of 28 mm, the same below) with side stream reflux; the following steps are the same as described in Example 1.

[0061] After adopting rotary evaporator to dry up the solvent in the separation product containing non-basic component and basic component, weigh, obtain non-basic component Resin-F1 and basic compo...

Embodiment 3

[0064] This example is used to illustrate the rapid separation of Liaohe vacuum residue (distillation range>500°C, referred to as LHVR) by the solid phase extraction method provided by the present invention, and to prepare the non-alkaline component (LHVR-F1 ) and alkaline components (LHVR-F2).

[0065] Weigh 1 gram of Liaohe vacuum residue sample, dissolve it in 2 milliliters of dichloromethane with ultrasonic vibration; fill 40 grams of acid-modified silica gel in a solid-phase extraction column (inner diameter 28 mm, the same below) with side stream reflux; The steps are the same as described in Example 1.

[0066] After using a rotary evaporator to evaporate to dryness the solvent in the separated product containing non-basic components and basic components, weigh them, and obtain the sample mass distribution of non-basic components LHVR-F1 and basic components LHVR-F2 as 0.6205 Grams 0.3743 grams.

[0067] Using electrospray Fourier ion cyclotron resonance high-resoluti...

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Abstract

The invention discloses a separation analyzing method for nitrogen-containing compounds in heavy oil. The separation analyzing method includes: preparing a solid phase of a solid-phase extraction chromatographic column; separating alkaline components from non-alkaline components with a solid-phase extraction chromatography; analyzing the separated components by the aid of Fourier transform ion cyclotron resonance high-resolution mass spectra. Low solid phase to oil weight ratio, less flushing solvent dosage, shorter time and less manpower are needed in the method; compared with an existing method, the separation analyzing method has the advantages of higher separation efficiency, better separation effect and higher sample throughout, the method can be used for separation to meet the requirements of sample purity for subsequent analysis and preparing the nitrogen-containing compounds in the heavy oil rapidly to provide necessary sample quantity for subsequent reaction and evaluation experiment, and meanwhile, separation effect evaluation and product composition analysis can be achieved from the molecular level by the aid of the Fourier transform ion cyclotron resonance high-resolution mass spectra.

Description

technical field [0001] The invention relates to a method for separating and analyzing nitrogenous compounds in heavy oil from the molecular level. Background technique [0002] Heavy oil is the main raw material for secondary processing in refineries (such as coking, solvent deasphalting, etc.), and it is also an important research object involved in heavy oil chemistry. Nitrogen-containing compounds in petroleum include amines, basic nitrides, non-basic nitrides, etc., which are stable to thermal structure and difficult to decompose. Therefore, about 87.5% to 92.9% of nitrogen in crude oil is enriched in residual oil. The basic nitrogen in crude oil, residue and asphaltenes accounts for about 30% of the total nitrogen. Compared with sulfur, the nitrogen content in petroleum is low, but it has an important impact on petroleum extraction, refining, and stability of petroleum products. For example, although the proportion of basic nitrogen compounds in total nitrogen compoun...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88G01N30/08
CPCG01N30/88G01N30/08
Inventor 王丽涛张艳梅刘银东赵广辉于志敏张东明毕秦岭娄立娟侯经纬张璐瑶卢竟蔓许倩崔晨曦
Owner PETROCHINA CO LTD
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