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A method for oxidative desulfurization of oil-complex iron emulsion

A technology for oxidative desulfurization and iron complexation, applied in chemical instruments and methods, separation methods, and sulfur preparation/purification, etc., can solve the problems of tower blockage and foaming that are not completely solved, and achieve no secondary pollution, source Wide range of effects to improve reaction efficiency

Active Publication Date: 2016-05-18
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method does not completely solve the problems of tower plugging and foaming that have always existed

Method used

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  • A method for oxidative desulfurization of oil-complex iron emulsion

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preparation example Construction

[0043] The preparation method of oil-in-water type oil-complex iron emulsion is as follows:

[0044]Based on the quality of the oil-complexed iron emulsion, add 30wt% catalytically cracked diesel oil to the reactor, and add 2wt% emulsifier, wherein the emulsifier type is a composite emulsifier of Span80 and AEO-3 (mass ratio is 48: 52), keep the temperature at 30°C for 5 minutes, then stir at a stirring speed of 300-500r / min, add 68wt% complex iron aqueous solution dropwise, and stir at 30°C for 30 minutes to prepare the oil-in-water oil-complex iron emulsion .

[0045] The present invention is achieved in such a way:

[0046] Contains H 2 S gas 1 enters absorber 2 to contact with oil-complexed iron emulsion, H 2 S is oxidized by complex iron to sulfur, and sulfur dissolves in the surrounding oil phase, releasing H 2 The purified gas 3 of S is discharged from the top of the absorber 2. After the oil-complexed iron emulsion is absorbed and saturated, the oil-complexed iron ...

Embodiment 1

[0050] Removal of H 2 The reaction conditions at S are as follows: In the absorber: the temperature is 50°C, the reaction pressure is 0.5MPa, and the 2 The volume ratio of the hourly flow rate of S gas to the oil-complex iron emulsion is 6:1; in the solid-liquid separator: the temperature for cooling and separating sulfur is 10°C.

[0051] Composition of hydrogen sulfide-containing gas (volume): hydrogen sulfide content is 0.62%, SO 2 COS is 0.01%, and COS is 0.01%. The oil-complexed iron emulsion includes: catalytic diesel oil with a distillation range of 240~260°C, and the Fe ion concentration is 0.06mol / L. Oxidative desulfurization of oil-complexed iron emulsion to purify H in gas 2 S concentration is 10mg / m 3 , the purity of recovered sulfur is 98.5%, demulsification and oil-water separation are carried out every 2 hours, and the absorber is switched at the same time.

Embodiment 2

[0053] Removal of H 2 The reaction conditions at S are as follows: In the absorber: the temperature is 60°C, the reaction pressure is 1MPa, and the 2 The volume ratio of the hourly flow rate of S gas to the oil-complex iron emulsion is 3:1; in the solid-liquid separator: the temperature for cooling and separating sulfur is 5°C.

[0054] Composition of hydrogen sulfide-containing gas (volume): hydrogen sulfide content is 0.18%, SO 2 COS is 0.1%, and COS is 0.03%. The oil-complexed iron emulsion includes: catalytic diesel oil with a distillation range of 260~280°C, and the concentration of Fe ions is 0.08mol / L. After oxidative desulfurization of the desulfurization liquid, the H in the gas is purified 2 S concentration is 6mg / m 3 , the purity of the recovered sulfur is 99.5%, demulsification and oil-water separation are carried out every 3 hours, and the absorber is switched at the same time.

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Abstract

The invention discloses an oxidative desulfurization method of an oil-iron complex emulsion, which comprises the following steps: hydrogen sulfide-containing gas is introduced in an absorber and then is contacted with the oil-iron complex emulsion, sulphur is generated through a hydrogen sulfide reaction, sulphur is dissolved in an oil phase, purified gas is discharged from top of the absorber, demulsification treatment is carried out on the oil-iron complex emulsion containing sulphur, and then oil and water is separated, and sulphur is recovered from oil phase; wherein the oil-iron complex emulsion is the oil-in-water emulsion. The method has the characteristics of fast absorption speed, high desulphurization efficiency and easy operation, and has wide application prospect of hydrogen sulfide degasification and sulphur recovery / utilization in petroleum refining and coal chemical industry.

Description

technical field [0001] The invention relates to an oxidative desulfurization method, in particular to an oil-complexed iron emulsion oxidative desulfurization and sulfur recovery method. Background technique [0002] Alkali (Na 2 CO 3 or K 2 CO 3 ) in aqueous solution absorbs sulfide, H 2 S gas reacts with alkali to form HS - , through the reduction of high-valence Fe ions to low-valence Fe ions, the HS - converted to sulfur. During the regeneration process, the complex iron solution in the low-valence state is contacted with air and oxidized into a high-valence complex iron solution to restore the oxidation performance, and the solution circulates to absorb hydrogen sulfide gas. The reaction mechanism of complex iron oxidative desulfurization is as follows: where g represents the gaseous state, l represents the liquid state; [0003] h 2 S(g)→H 2 S(l); [0004] h 2 S(l)+(OH - )→(HS - )+H 2 O; [0005] HS - +OH - →2S 2- +H 2 O; [0006] 2Fe 3+ +2S 2- →...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D53/78B01D53/52C01B17/04
CPCY02P20/10
Inventor 刘淑鹤方向晨王学海陈玉香杨爱霞程明珠
Owner CHINA PETROLEUM & CHEM CORP
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