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1-Butyl-3-methylimidazolium ethylenediamine tetraacetate ferric catalyzed oxidation method of hydrogen sulfide

A technology of alkylimidazole EDTA iron and alkylimidazole EDTA iron liquid, which is applied in the preparation/purification of sulfur, can solve the problems of reducing the purity of sulfur products and easy scaling, and achieve rapid Efficient oxidation removal, low surface tension, avoiding the effect of by-products such as thiosulfate and sulfate

Inactive Publication Date: 2019-12-20
BEIJING INSTITUTE OF PETROCHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] Hydrogen sulfide and oxygen only generate sulfur in acidic solution, but easily generate persulfate and sulfate in alkaline solution
The by-products of these sulfur oxide salts not only reduce the purity of the product sulfur, but also are prone to fouling and must be discharged regularly (J.Mol.Catal.A-Chem., 1997, 117:289)

Method used

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  • 1-Butyl-3-methylimidazolium ethylenediamine tetraacetate ferric catalyzed oxidation method of hydrogen sulfide
  • 1-Butyl-3-methylimidazolium ethylenediamine tetraacetate ferric catalyzed oxidation method of hydrogen sulfide
  • 1-Butyl-3-methylimidazolium ethylenediamine tetraacetate ferric catalyzed oxidation method of hydrogen sulfide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] 4.8g NaOH dissolved in 100ml deionized water, 10.8g FeCl 3 ·H 2 O is dissolved in an appropriate amount of deionized water (the amount of water is measured as FeCl 3 ·H 2 O to form a clear and transparent solution) After forming a clear and transparent solution, add it to the NaOH aqueous solution, and stir slowly until a suspension is formed. Then pour the suspension into a 1000ml beaker, add tap water to 800ml, and wash 3-4 times. Filter under reduced pressure to obtain Fe(OH) 3 solid. After mixing with 10.52g of ethylenediaminetetraacetic acid and 74ml of deionized water, heat and boil until a brown transparent solution is formed, and cool to room temperature to obtain a solution of Fe-EDTA.

Embodiment 2

[0051] In the Fe-EDTA solution prepared in Example 1, add 1-butyl-3-methylimidazole hydroxide ([Bmim]OH) and stir for 10 minutes, and after rotary evaporation of water at 50°C, brown [Bmim] was obtained [Fe(EDTA)] viscous solution, the pH of the solution is 5.58, the water content is 32.5%, the EDTA content is 29.2%, and the Fe concentration is 5.67%.

[0052] Take 55mL of [Bmim][Fe(EDTA)] aqueous solution and inject it into the desulfurization reactor, at 30°C, control 99.9%O 2 The flow rate is 25mL / min, 99.9%H 2 The S flow rate is 20mL / min, and the catalytic-oxidation in the desulfurization absorption liquid is measured every hour. After 8 hours, its concentration still reaches 95% of the initial concentration (EDTA) complexing agent content. The ratio of the concentration after EDTA catalyzed-oxidation reaction to the initial concentration varies with time as figure 2 shown. Depend on figure 2 It can be seen that when the [Bmim][Fe(EDTA)] solution with a pH of 5.58 an...

Embodiment 3

[0056] In the Fe-EDTA solution prepared by the same method as in Example 1, add 1-butyl-3-methylimidazole hydroxide ([Bmim]OH) and stir for 10 minutes. After rotary evaporation of water at 50°C, brown The [Bmim][Fe(EDTA)] viscous solution has a pH of 2.64, a water content of 43.5%, a Fe concentration of 5.89%, and an EDTA content of 30.3%.

[0057] Take 47.5 mL of [Bmim][Fe(EDTA)] aqueous solution and inject it into the desulfurization reactor, at 30°C, control 99.9% O 2 The flow rate is 25mL / min, 99.9%H 2 The flow rate of S is 20mL / min, and the content of ethylenediaminetetraacetic acid (EDTA) complexing agent in the desulfurization absorption liquid is measured every hour. The ratio of the concentration after EDTA catalyzed-oxidation reaction to the initial concentration varies with time as figure 2 shown. Depend on figure 2 It can be seen that the [Bmim][Fe(EDTA)] solution with a pH of 2.64 catalyzed-oxidized hydrogen sulfide for 8 hours, and its concentration reached...

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Abstract

The invention relates to a method for performing catalytic oxidation on hydrogen sulfide through hydrophilic 1-butyl-3-methylimidazole ethylene diamine tetraacetic acid (EDTA) iron ([Bmim][Fe(EDTA)]. Compared with conventional Fe-EDTA, the [Bmim][Fe(EDTA)] has one more cation [Bmim]<+>. Due to existence of [Bmim]<+>, an aqueous solution of the [Bmim][Fe(EDTA)] has the following characteristics that 1, the surface tension is low, aggregation of newly generated sulfur is promoted, and sulfur blockage formed by floating of fine sulfur is avoided; 2, according to the [Bmim]<+> structure, hydrogen sulfide is dissolved, the hydrogen sulfide has relatively high solubility in the aqueous solution of the [Bmim][Fe(EDTA)] even if under acid conditions, and a desulfuration side reaction is avoided under the acid condition. When the hydrogen sulfide is subjected to catalytic oxidation through [Bmim][Fe(EDTA)], the degradation rate is far lower than that of Fe-EDTA, degradation byproducts of Fe-EDTA are detected through an ultraviolet spectrum, and degradation byproducts of the [Bmim][Fe(EDTA)] are not detected. The infrared spectrum proves that sulfur-oxygen byproducts are not generated in the process of performing catalytic oxidation on the hydrogen sulfide in the aqueous solution of the [Bmim][Fe(EDTA)]. The XRD (X-Ray Diffraction) proves that the catalytic oxidation product is sulfur, and the yield of the sulfur is positively correlated to iron concentration.

Description

technical field [0001] The invention relates to a liquid-phase catalytic hydrogen sulfide oxidation method using alkylimidazole ethylenediamine tetraacetate iron as a catalyst and oxygen as an oxidant. The catalytic oxidation of hydrogen sulfide by ferric alkylimidazole EDTA has the advantages of extremely low catalyst degradation rate, high sulfur yield per unit of absorption liquid, no sulfur plugging in the catalytic oxidation process, and no desulfurization side reactions. It is a kind of A new technology capable of treating various concentrations of hydrogen sulfide with high efficiency and low cost. Background technique [0002] Hydrogen sulfide (H 2 S) This poisonous acidic pollutant not only corrodes metal pipes during transportation but also forms acid rain to pollute the environment after burning. H in gaseous fuel and industrial waste gas 2 S must be purified. [0003] At present, the process with great potential for treating hydrogen sulfide is the catalysis-o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B17/05
Inventor 王建宏
Owner BEIJING INSTITUTE OF PETROCHEMICAL TECHNOLOGY
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