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Method for separating heavy oils by solid phase extraction

A heavy oil and extraction technology, which is applied in ion exchange, refined hydrocarbon oil, petroleum industry, etc., can solve the problems of many steps in the separation process, poor separation efficiency, and reduced sample processing volume, and achieve high separation efficiency, avoid pollution, and large samples The effect of throughput

Active Publication Date: 2013-11-06
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The chromatographic column used in this method is longer, the separation process has many steps, and the separation speed is slow
CN1690704A discloses a method for determining the composition of VGO hydrocarbons by solid-phase extraction and mass spectrometry. The height of the solid-phase extraction column used is 40-70 mm, the internal diameter of the column is 4-9 mm, the stationary phase is silica, and the loading capacity is 1.0 mm. -2.0 grams, sample processing amount 0.1-0.3 grams, wash out saturated hydrocarbons, aromatics and colloids with n-pentane or n-hexane, dichloromethane, benzene-ethanol respectively. Compared with ASTM D2549, the separation accuracy of this method is quite ( Generally, the amount of cross-contamination between saturated hydrocarbons and aromatics does not exceed 5%), the separation and analysis time is significantly shortened, but the amount of sample processing is greatly reduced
[0005] In general, the above separation methods either have too little processing capacity to meet the sample volume requirements for subsequent reactions and evaluation experiments; or the separation efficiency is poor, and there is relatively serious cross-contamination between saturated hydrocarbons and aromatics; Ratio (stationary phase to oil sample weight ratio), solvent flushing rate and other separation operating conditions are more stringent

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] This example is used to illustrate the processing and preparation of silica gel (silicon dioxide) and silica gel samples loaded with silver ions in the present invention.

[0024] The fine-pored silica gel raw material was dried in an oven at 150°C for 4 hours to obtain activated silica gel for use, and the code is SG. Store in a desiccator for later use.

[0025] Weigh 60.9g AgNO 3 Dissolve in 400g water to make a solution; weigh 400g silica gel, add the silica gel to the prepared AgNO 3 In the solution, stir while adding, after adding the silica gel, stir for 15 minutes; impregnate the AgNO 3 The silica gel was put into an oven and dried at 150° C. for 4 hours to obtain activated silver ion-loaded silica gel, coded as ASG, with a silver nitrate loading of 13.2% by weight. Store in a desiccator away from light for later use.

Embodiment 2

[0027] This example is used to illustrate that the solid phase extraction method provided by the present invention is used to efficiently and quickly separate vacuum distillate oil and prepare saturated hydrocarbons, aromatic hydrocarbons and colloidal components therein.

[0028] Weigh 15g of Daqing vacuum distillate oil (distillation range 510-570°C) sample and dissolve it in 220mL of n-hexane; fill 100g of ASG in a solid-phase extraction column (internal diameter 28mm, the same below); install the solid-phase extraction column in On the solid-phase extraction device with vacuum system, wet stationary phase (ASG) with 100 milliliters of n-hexane; The n-hexane solution of above-mentioned oily sample is filled in the solid-phase extraction column, and the vacuum degree of control makes solution filling The rate was stabilized at 15 ml / min; after the oil sample was filled, saturated hydrocarbons were extracted by washing the stationary phase with 300 ml of n-hexane, and the vacu...

Embodiment 3

[0031] This example is used to illustrate that the solid phase extraction method provided by the present invention is used to efficiently and quickly separate vacuum distillate oil and prepare saturated hydrocarbons, aromatic hydrocarbons and colloidal components therein.

[0032] Weigh 6g of VGO (Saudi Medium Crude Vacuum Distillate, distillation range 350-540°C) sample in the sand and dissolve it in 90mL of n-hexane; fill the lower layer of the solid-phase extraction column with 50 grams of ASG, and the upper layer with 50 grams of SG; The solid-phase extraction column is installed on a solid-phase extraction device with a vacuum system, wet the stationary phase with 100 ml of n-hexane, fill the n-hexane solution of the above oil sample into the solid-phase extraction column, and control the vacuum to make the solution The filling rate of the oil sample was stabilized at 10 ml / min; after the oil sample was filled, the saturated hydrocarbon was extracted by flushing the statio...

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Abstract

A method for separating heavy oils by solid phase extraction comprises the step of the contact of the heavy oils with stationary phase, wherein the stationary phase consists of silica loaded with silver ions and alumina. In the method, solid extraction separation is used to separate the heavy oils to obtain saturated hydrocarbon, aromatic hydrocarbon, and colloid, and then the saturated hydrocarbon, the aromatic hydrocarbon and the colloid are prepared. By using the method, the separation efficiency and the handling capacity can be taken into account, and the rapid and efficient separation of the heavy oils is realized.

Description

technical field [0001] The invention relates to a method for separating heavy oil by solid phase extraction. Background technique [0002] Heavy oil is the main raw material for secondary processing (such as catalytic cracking, coking, hydrocracking, etc.) in refineries, so the level of heavy oil processing technology is an important factor affecting the economic benefits of refineries. However, the structure and composition of heavy oil are very complex. Even when the overall properties such as H / C ratio and average molecular weight are similar, their secondary processing properties are often different to a large extent. Therefore, only in-depth understanding of the chemical composition and transformation rules of heavy oil can improve the technical level of heavy oil processing. This requires the separation of heavy oil to obtain different components, and then conduct more in-depth (molecular and excimer level) analysis and reactivity research on different components. Th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C10G25/00B01D15/08B01J20/10
Inventor 宋海涛刘泽龙达志坚朱玉霞黄志青祝馨怡刘颖荣田松柏田辉平
Owner CHINA PETROLEUM & CHEM CORP
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