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Emulsion oxidation desulfurization and sulfur recovery method

A technology for oxidative desulfurization and sulfur recovery, applied in chemical instruments and methods, separation methods, preparation/purification of sulfur, etc., can solve problems such as tower plugging and foaming that have not been completely solved, and achieve the benefits of activity, reduction of side reactions, The effect of improving reaction efficiency

Active Publication Date: 2015-04-29
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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  • Emulsion oxidation desulfurization and sulfur recovery method

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] (1) Preparation of water-in-oil type oil-complex iron emulsion: Based on the quality of the oil-complex iron emulsion, add 82.2wt% catalytically cracked diesel oil and 2wt% emulsifier to the reactor, of which the emulsifier The type is Span80 and OP-10 compound emulsifier (mass ratio is 3:1), keep the temperature at 30°C for 5 minutes, then stir at a stirring speed of 300-500r / min, and add 0.8wt% n-butanol additive dropwise at the same time and a 15wt% complex iron aqueous solution, and stirred at a constant temperature of 30°C for 30 minutes to prepare a water-in-oil type oil-complex iron emulsion.

[0051] (2) Removal of H 2 The reaction conditions at S are as follows: In the absorber: the temperature is 50°C, the reaction pressure is 0.6MPa, 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. Composition of hydrogen sulfide-cont...

Embodiment 2

[0053] (1) Same as Example 1.

[0054] (2) Removal of H 2 The reaction conditions at S are as follows: In the absorber: the temperature is 60°C, the reaction pressure is 0.3MPa, 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. 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 0.08 mol / L. After oxidative desulfurization of desulfurization liquid, H in the purified gas 2 S concentration is 9mg / m 3 , The purity of recovered sulfur is 99%, oil and water are separated every 4 hours, and the absorber is switched at the same time.

Embodiment 3

[0056] (1) Preparation of water-in-oil type oil-complex iron emulsion: Based on the quality of the oil-complex iron emulsion, add 74.5wt% catalytically cracked diesel oil to the reactor, add 3.5wt% emulsifier, and emulsify The type of agent is Tween80, Span60 and MOA-3 compound emulsifier (mass ratio is 2:1:1), and the temperature is kept at 30°C for 5 minutes, and then stirred at a stirring speed of 300-500r / min. At the same time, 2wt% of propane is added dropwise. A water-in-oil type oil-complex iron emulsion was obtained by stirring at a constant temperature of 40° C. for 25 minutes with a triol additive and 20 wt % complex iron aqueous solution.

[0057] (2) Removal of H 2 The reaction conditions at S are as follows: In the absorber: the temperature is 80°C, the reaction pressure is 0.1MPa, and the 2 The volume ratio of the hourly flow rate of S gas to the oil-complex iron emulsion is 1:2; in the solid-liquid separator: the temperature for cooling and separating sulfur is...

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Abstract

The invention discloses an emulsion oxidation desulfurization and sulfur recovery method. The method comprises the following steps: hydrogen sulfide-containing gas enters an absorber to be in contact with oil-complex iron emulsion, hydrogen sulfide reacts to generate sulfur, sulfur is dissolved in an oil phase, and purified gas is discharged from the top of the absorber; the sulfur-containing oil-complex iron emulsion is broken, oil-water separation is carried out, and sulfur is recovered from the oil phase, wherein the oil-complex iron emulsion is water-in-oil emulsion. The method has the characteristics of high absorption speed, high desulfurization efficiency, simple operation and the like, and has a wide application prospect on the aspects of petroleum refining, removal of hydrogen sulfide-containing gas in coal chemical industry and recycling of sulfur.

Description

technical field [0001] The invention relates to an oxidative desulfurization and sulfur recovery method, in particular to an oil-complexed iron emulsion oxidative desulfurization and sulfur recovery method. Background technique [0002] LO-CAT complex iron desulfurization technology is a method of wet redox removal of sulfide using iron as a catalyst. It is characterized by non-toxic absorbent and the ability to remove H 2 S is transformed into elemental sulfur, H 2 The removal rate of S can reach more than 99%. Complex iron desulfurization technology is suitable for H 2 low concentration of S or H 2 Where the S concentration is high but the gas flow rate is not large. When the output of elemental sulfur is less than 20t / d, the equipment investment and operation cost of this process have obvious advantages. 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 ...

Claims

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Application Information

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