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Method for solid phase extraction separating of components in heavy oil

A heavy oil and extraction technology, applied in separation methods, solid adsorbent liquid separation, chemical instruments and methods, etc., can solve problems such as poor separation efficiency, low stationary phase or column efficiency, and inability to meet the analysis and processing of aromatic components

Active Publication Date: 2016-01-27
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

However, this method does not further separate the aromatic components, and cannot meet the needs of further analysis and processing of aromatic components of different polarities.
In addition, the silica gel loaded with silver ions in the stationary phase used in this method has a low adsorption strength for silver ions. When washing the colloidal components, an alumina column needs to be connected in series at the lower end of the device to avoid the silver ions being washed down. Into the separated components, but also increases the operation steps and difficulty
[0009] Generally speaking, the above-mentioned stationary phase or column efficiency is too low, the separation efficiency is too poor, and there is a serious crossover between saturated hydrocarbons, light aromatics, medium aromatics and heavy aromatics; or the processing capacity is too small to meet the requirements of preparative separation. The separation requirements of the sample; or in the case of the same separation accuracy, the processing volume each time is too small to achieve preparative-level separation of different polar components in heavy oil; or a large amount of silver ions are eluted into each component Go, affect the subsequent analysis and detection of the separated components and the evaluation of processing performance

Method used

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Examples

Experimental program
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Effect test

preparation example Construction

[0020] The preparation method of the stationary phase provided by the invention comprises the steps of immersing aluminum oxide in silver nitrate solution, stirring evenly, immersing at 20-70° C. for 0.5-5.0 hours under reduced pressure, and then drying.

[0021] The suitable concentration of the silver nitrate solution is preferably 0.2-10.0% by mass, preferably 0.5-6.0% by mass.

[0022]The pressure for impregnating alumina with silver nitrate solution is preferably 20-100 kPa, and the drying temperature after impregnation is preferably 100-200°C.

[0023] In the process of introducing silver nitrate by impregnation, the volume of the silver nitrate solution used for impregnation is 1 to 10 times, preferably 2 to 5 times, the pore volume of the carrier alumina. After impregnation, the alumina impregnated with silver salt (silver nitrate) is dried at 100-200° C., preferably 120-180° C., and the drying time is 1-30 hours, preferably 1-10 hours. The process of introducing silv...

example 1

[0045] This example is used to illustrate the pretreatment and preparation process of silica, alumina and alumina loaded with silver ions in the present invention.

[0046] The fine-pored silica gel raw material was dried in a ventilated drying oven at 150° C. for 5 hours to obtain activated silica gel, which was stored in a desiccator for future use.

[0047] The neutral alumina was calcined at 550°C for 5 hours to obtain activated alumina, which was stored in a desiccator for later use.

[0048] Dissolve 7.41 grams of silver nitrate in 160 mL of deionized water to prepare a silver nitrate solution, take 200 grams of neutral alumina, add the alumina to the silver nitrate solution, stir evenly, and immerse at 60 °C under a pressure of 50 kPa for 4 hours, then Dry the aluminum oxide impregnated with silver nitrate at 150°C for 2 hours, cool to room temperature, then impregnate and dry again with the same volume and concentration of silver nitrate aqueous solution according to t...

example 2

[0050] This example illustrates the effect of using the stationary phase provided by the invention to separate components of vacuum distillate oil.

[0051] The bottom layer of the separation column is filled with 30g of neutral alumina, the middle is filled with 110g of silver ion-loaded alumina A, and the upper layer is filled with 30g of silica gel; the lower end of the separation column is connected to a vacuum system. The total volume of the stationary phase was 150 mL.

[0052] Take 10.20g (11.19mL) sample of Tahe vacuum distillate oil (distillation range 350~540°C), dissolve it in 30mL of n-hexane, first wet the stationary phase filled in the separation column with 100mL of n-hexane, and then put the above The n-hexane solution of the oil sample was added to the separation column. Use 170mL n-hexane to wash out saturated hydrocarbon components, 255mL toluene:n-hexane volume ratio of 1:19 solvent to wash out light aromatics components, and 255mL toluene:n-hexane volume ...

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Abstract

A method for solid phase extraction separating of components in heavy oil comprises the following steps: heavy oil is diluted and added into a stationary phase, the stationary phase is washed orderly by C5-C6 alkanes to obtain saturated hydrocarbon components, the stationary phase is washed by a solvent with the volume ratio of aromatic hydrocarbon and C5-C6 alkanes of 1: 15-25 to obtain light aromatic hydrocarbon components, the stationary phase is washed by a solvent with the volume ratio of aromatic hydrocarbon and C5-C6 alkanes of 1: 3 to 5 to obtain middle aromatic hydrocarbon components, the stationary phase is washed by aromatic hydrocarbon to obtain heavy aromatic hydrocarbon components, the stationary phase is washed by a solvent with the volume ratio of aromatic hydrocarbon and monohydric alcohol of 1: 0.8 to 1.5 to obtain colloid components, the stationary phase is silver-ion-supported alumina, and supported silver ions accounts for 0.5 to 12% of the mass of alumina. According to the method, the silver-ion-supported alumina is used as the stationary phase for separating hydrocarbons with different polar components in the heavy oil, and the stationary phase is easy to be eluted compared with the supported silver ions which are large in sample processing capacity, and high in separation efficiency.

Description

technical field [0001] The invention relates to a method for separating various hydrocarbon components in heavy oil, specifically, a method for separating hydrocarbon components with different structures in heavy oil by solid phase extraction. Background technique [0002] Heavy oil is the main raw material for secondary processing processes such as catalytic cracking, hydrofining, hydrocracking and coking, and the processing level of heavy oil is an important factor affecting the economic benefits of refineries. Due to the complex structure and composition of heavy oil, even when the overall properties such as H / C ratio and average molecular weight are similar, the detailed hydrocarbon composition and carbon number distribution of heavy oil are very different. These differences will cause differences in transformation laws due to different chemical reactions. Therefore, it is necessary to select the most matching secondary processing technology based on the understanding of...

Claims

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Application Information

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IPC IPC(8): C10G25/00B01D15/42G01N1/40
Inventor 赵丽萍田松柏龙军刘泽龙宋海涛陈妍
Owner CHINA PETROLEUM & CHEM CORP
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