Method and device for extracting sulfate by directional crystallization of desulfurization tail liquid through liquid phase catalysis method

A liquid-phase catalysis and directional crystallization technology, applied in the field of environmental engineering, can solve the problems of high sulfuric acid production cost and daily operating cost, difficult to handle, increase the operating cost of coking enterprises, etc., and achieve the effect of crystallizing regulation and cleaning cycle.

Pending Publication Date: 2022-08-02
KUNMING UNIV OF SCI & TECH
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  • Description
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Problems solved by technology

However, the secondary salt produced by this kind of desulfurization method has caused a large burden to coking enterprises. Although energy companies often use salt extraction and acid production methods to balance the secondary salt produced, it is difficult to create value for the crude salt produced by salt extraction. , and the cost of sulfuric acid production and daily operation costs are high, so in recent years, many domestic energy companies have tried to find a more ideal process to get rid of the current desulfurization dilemma
[0003] In the desulfurization process of liquid-phase catalytic oxidation method, the absorbed sulfur will be removed in the form of sulfur paste and auxiliary salts. In the auxiliary salts, there are not only fully oxidized sulfate, but also incompletely oxidized bisulfate, thiocyanate and sulfur. Sulfates, etc., reduce the purity of sulfur, but the purity is not high, it is difficult to handle, and the side salt needs to be cleaned regularly, which increases the operating cost of coking enterprises
Sulfate has high economic value, and in view of the difficulties brought about by the current energy gas desulfurization salty waste liquid, the research focus of the existing liquid-phase catalytic oxidation desulfurization technology should be on the selective oxidation of impurity ions and high-purity sulfate directional crystallization, but there are no related research papers and patents

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  • Method and device for extracting sulfate by directional crystallization of desulfurization tail liquid through liquid phase catalysis method

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Experimental program
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Embodiment 1

[0014] The volume ratio of water and oxygen at the inlet of the semi-wet ozone generator 6 is controlled to be 0.05, the pulse discharge frequency of the device is 150kHz, the voltage is 25kV, the distance between the high voltage electrode and the ground electrode is 30mm, and the water mist oxygen mixture is passed between the two discharge electrodes. The speed is 40m / s. The generated ozone gas is passed into the strong oxidation regeneration device 1 equipped with the HPF method desulfurization tail liquid, and the gas flow rate is controlled to be 180 mL / min. The liquid pump 8 is pumped into the crystallizing tank 2, anhydrous methanol is added (the volume ratio of anhydrous methanol and the solution in the crystallizing tank is 0.6), the pH is adjusted to 4.0, the reaction temperature of the system is 60 ° C, and the stirring speed is 100 rpm. After 5 minutes of reaction , pass part of the crystallization and liquid into the crystallization tank 3, after the crystals are...

Embodiment 2

[0016] The volume ratio of water and oxygen at the inlet of the semi-wet ozone generator is controlled to be 0.08, the pulse discharge frequency of the device is 200 kHz, the voltage is 45 kV, and the distance between the high-voltage electrode and the ground electrode is 30 mm. The speed is 50m / s. The generated ozone gas is passed into the strong oxidation regeneration device 1 equipped with the ADA method desulfurization tail liquid, and the control gas flow is 230 mL / min. The liquid pump 8 is pumped into the crystallizing tank 2, acetone is added (the volume ratio of acetone to the solution in the crystallizing tank is 0.8), the pH is adjusted to 6.5, the reaction temperature of the system is 50 ° C, and the stirring speed is 230 rpm. The liquid is passed into the crystallization tank 3. After the crystals are fully grown and precipitated in the crystallization tank 3, the crystals enter the crystal mud storage tank for preliminary liquid-solid separation and then pass into...

Embodiment 3

[0018] The volume ratio of water and oxygen at the inlet of the semi-wet ozone generator is controlled to be 0.1, the pulse discharge frequency of the device is 300 kHz, the voltage is 65 kV, and the distance between the high-voltage electrode and the ground electrode is 30 mm. The speed is 60m / s. The generated gas is passed into the strong oxidation regeneration device 1 equipped with the complex iron method desulfurization tail liquid, and the control gas flow rate is 430mL / min. 8 Pump into the crystallizing tank 2, add acetone (the volume ratio of acetone to the solution in the crystallizing tank is 0.8), adjust the pH to 8.0, the reaction temperature of the system is 30 ° C, and the stirring speed is 400 rpm. into the crystallizing tank 3, after the crystals in the crystallizing tank 3 are fully grown and precipitated, the crystals enter the crystal mud storage tank for preliminary liquid-solid separation, and then pass into the filter device for further filtration to obta...

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Abstract

The invention discloses a method for extracting sulfate by directional crystallization of liquid-phase catalytic desulfurization tail liquid, which comprises the following steps: O3 is introduced into a strong oxidation regeneration device filled with the liquid-phase catalytic desulfurization tail liquid, the liquid-phase catalytic desulfurization tail liquid is fully oxidized, O3 reacts with S2O3 < 2-> in the tail liquid to generate. OH, and the. OH reacts with S2O3 < 2-> in the tail liquid to generate. The method comprises the following steps: oxidizing sulfur salt in tail liquid and generated sulfur into SO4 < 2->, regenerating a desulfurization catalyst in the liquid-phase catalytic desulfurization tail liquid, introducing the oxidized liquid into a crystallizing tank, adding a solventing-out agent, separating out sulfate crystals under stirring at the pH value of 2.0-9.5 and the temperature of 20-150 DEG C, and carrying out solid-liquid separation to obtain high-purity sulfate crystals, according to the method disclosed by the invention, the sulfur paste is fully oxidized into SO4 < 2-> by virtue of the strong oxidizing property of the active oxidizing substance, the influence of the sulfur paste on the oxidation regeneration process of the desulfurization tail liquid is reduced, the liquid-phase catalytic desulfurization catalyst is effectively regenerated, high-purity ammonium sulfate by-salt can be directionally extracted, and the by-product value of the liquid-phase catalytic desulfurization method is improved.

Description

technical field [0001] The invention belongs to the field of environmental engineering, and in particular relates to a method and a device for directional crystallization of liquid-phase catalytic desulfurization tail liquid to extract sulfate. Background technique [0002] At present, more than ten related desulfurization processes have been used in the actual production of industrial desulfurization. The traditional liquid-phase catalytic oxidation desulfurization technologies include HPF method, ADA method, tannin extract method, PDS catalytic desulfurization method, etc., but the desulfurization effect is unstable. , and H 2 Disadvantages such as incomplete removal of reducing sulfide gas such as S. In addition, since the 1990s, the most widely used HPF method has been used by more than half of domestic energy companies, and it is a relatively mature desulfurization method. However, the secondary salts produced by such desulfurization methods have caused a great burden...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D53/86B01D53/96C01B17/96C01C1/24B01D53/50
CPCB01D53/96B01D53/8609C01B17/96C01C1/24C01P2006/80Y02P20/584
Inventor 瞿广飞赵晨阳李军燕李应丽保德山李志顺成吴丰辉潘科衡
Owner KUNMING UNIV OF SCI & TECH
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