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Method for separating porphyrin vanadium and non-porphyrin vanadium compounds in heavy oil

A porphyrin vanadium compound and technology of porphyrin vanadium, applied in the direction of organic chemistry, test sample preparation, etc., can solve the problems of complex operation, low recovery rate, and long time consumption

Active Publication Date: 2019-04-16
CHINA PETROLEUM & CHEM CORP +1
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Problems solved by technology

However, this method has the following disadvantages: ①Complicated operation and long time-consuming; ②It can only extract porphyrin vanadium in crude oil or residual oil, but cannot separate porphyrin vanadium in asphaltenes; ③Cannot separate and obtain non-porphyrin vanadium compounds components
[0007] Mohammad et al. (Mohammad F.A, et al.Nickel and Vanadyl Porphyrins in Saudi Arabian Crude Oils [J]. Energy & Fuels, 1993, (7): 179-184.) used adsorption column chromatography to separate porphyrin vanadium in crude oil, but the The method adopts two adsorption column chromatography to purify the porphyrin vanadium, the operation is complicated, and the recovery rate of the adsorbent and elution solvent used in the experiment is very low when separating the vanadium compounds in the residual oil or asphaltenes, which is not suitable for heavy Separation of porphyrin vanadium and non-porphyrin vanadium compounds in crude oil
[0008] Qian et al. (Qian K, Mennito A S, Edwards K E, et al.Observation of vanadylporphyrins and sulfur-containing vanadyl porphyrins in a petroleum asphalteneby atmospheric pressure photonionization Fourier transform ion cyclotronresonance mass spectrometry[J].Rapid Commun.20 8 Spectrometry : 2153-2160.) Asphaltenes were treated by the principle of solubility dissolution, and porphyrin vanadium was characterized from asphaltenes. Although this method is easy to operate, it cannot separate porphyrin vanadium and non-porphyrin vanadium in asphaltenes. Vanadium compounds, not conducive to the study of non-porphyrin vanadium compounds in asphaltenes

Method used

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  • Method for separating porphyrin vanadium and non-porphyrin vanadium compounds in heavy oil

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preparation example Construction

[0022] The preparation method of the adsorbent in the present invention is as follows: calcining silica gel at 110-280° C., preferably 90-160° C., and calcining alumina at 400-700° C., and the calcining time is preferably 3-6 hours. Add required water to the calcined silica gel or the mixture of silica gel and alumina, shake vigorously for 5-30 minutes, and then let it stand for 10-30 hours.

[0023] The specific surface area of ​​the silica gel is preferably 300 to 700 meters 2 / g, the pore volume is preferably 0.3-0.8 ml / g, and the particle size is preferably 75-150 microns. The alumina is preferably γ-alumina, and its specific surface area is preferably 300-700 m 2 / g, the pore volume is preferably 0.3-0.8 ml / g, and the particle size is preferably 75-150 microns.

[0024] (1) step of the present invention is to load the heavy oil in the adsorbent. The loading method includes dissolving the heavy oil with chlorinated alkanes, adding the adsorbent to impregnate it, removing...

example 1

[0050] (1) Preparation of adsorbent

[0051] The silica gel was fired at 180°C for 5.5 hours, and the γ-alumina was fired at 500°C for 5.5 hours. Add 0.4 mL of distilled water to 40 g of the calcined mixture of silica gel and alumina with a mass ratio of 1:0.3, shake vigorously for 15 minutes, and let stand for 24 hours to obtain Adsorbent A, in which the water content is 1.0% by mass.

[0052] (2) Load Iranian vacuum residue

[0053] Dissolve 0.2021g of Iranian vacuum residue in 20mL of dichloromethane, add 3.1g of adsorbent A, stir evenly, and dry at 90°C for 1 hour after the solvent has completely volatilized naturally, so that the dichloromethane is completely volatilized to obtain the loaded Adsorbents for Iranian vacuum residues.

[0054] (3) Separation of non-porphyrin vanadium compounds and porphyrin vanadium compounds in Iranian vacuum residue

[0055] Take 20g of adsorbent A, put it into a glass adsorption column with a column length of 30 cm and an inner diameter...

example 2

[0064] (1) Preparation of adsorbent

[0065] The silica gel was baked at 150°C for 3.5 hours, and the γ-alumina was fired at 450°C for 5 hours. Add 1.0 mL of distilled water to 40 g of the calcined mixture of silica gel and alumina with a mass ratio of 1:0.15, shake vigorously for 20 minutes, and let stand for 24 hours to obtain Adsorbent B, in which the water content is 2.5% by mass.

[0066] (2) Separation of colloids in Iranian vacuum residue

[0067] Adopt RIPP10-90 method (Yang Cuiding, Gu Kanying, Wu Wenhui. Petrochemical Analysis Method (RIPP Test Method) [M]. Beijing: Science Press, 1990: 31-33) to separate the colloidal components in the Iranian vacuum residue, The specific operation steps are as follows: use n-heptane to remove asphaltenes in Iranian vacuum residue, take 40 grams of alumina with a water content of 1.0% by mass as an adsorbent, and put it into an adsorption column with a specification of 10×800mm , add 1.5 g of deasphalted oil to the adsorption colu...

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Abstract

A method for separating vanadium porphyrin and vanadium nonporphyrin compounds from heavy oil comprises the following steps: 1, loading the heavy oil to an adsorbent, wherein the adsorbent is silica gel or a silica gel and alumina mixture with the water content of 0.5-6.0 mass%; and 2, filling the upper layer of an adsorption column with the heavy oil supported adsorbent, and sequentially eluting the adsorbent with eluents with gradually increasing polarity 5 times, wherein the five eluents are a mixture containing inert hydrocarbon and aromatic hydrocarbons according to a volume ratio of 1:0.3-1.2, a mixture containing inert hydrocarbon and aromatic hydrocarbons according to a volume ratio of 1:1.5-5.0, a mixture containing inert hydrocarbon, aromatic hydrocarbons and a polar organic solvent according to a volume ratio of 0.1-0.3:1:0.1-0.3, a mixture containing aromatic hydrocarbons and a polar organic solvent according to a volume ratio of 1:0.8-3.0, and a mixture containing aromatic hydrocarbons and a polar organic solvent according to a volume ratio of 1:5.0-10.0. The method can effectively separate the vanadium porphyrin and vanadium nonporphyrin compounds from heavy oil, is simple to operate, and is convenient and fast.

Description

technical field [0001] The invention relates to a method for extracting and separating different types of compounds in heavy oil, specifically, a method for extracting and separating non-porphyrin vanadium compounds and porphyrin vanadium compounds in heavy oil. Background technique [0002] With the increasing consumption of petroleum resources, heavy oil resources have received more and more attention, but the metal vanadium compounds in heavy oil will cause great harm to the petroleum processing process, not only poisoning the catalyst in the refining process, but also generating low Melting point substances, corroding oil refining equipment and combustion equipment. Therefore, it is necessary to conduct a detailed analysis of vanadium compounds in heavy oil in order to optimize or develop a suitable heavy oil demetallization process. [0003] Currently, the characterization of the composition and distribution of vanadium compounds in heavy oil is still a difficult probl...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N1/28C07D487/22
Inventor 史延强王威刘泽龙
Owner CHINA PETROLEUM & CHEM CORP
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