Zinc oxide based normal-temperature deep desulfurizing agent as well as preparation method and application thereof

A deep desulfurization, zinc oxide-based technology, applied in chemical instruments and methods, refining with metal oxides, separation methods, etc., can solve the problems of increased energy consumption and operating costs, insufficient low-temperature activity of desulfurizers, and insufficient desulfurization accuracy. Achieve the effect of reducing energy consumption, mild operating conditions and improving utilization

Active Publication Date: 2017-05-24
SHANGHAI RES INST OF CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] To sum up, although after years of research, the desulfurization performance of zinc oxide-based desulfurizers has been greatly improved, but the current technology of zinc oxide-based desulfurizers still has the following deficiencies: 1) The sulfur capacity of the desulfurizer needs to be improved. Further improvement, especially the sulfur capacity at room temperature is generally lower than 15%; 2) The desulfurization precision is not enough, it is difficult to remove hydrogen sulfide to below 0.03ppm; 3) The low-temperature activity of the desulfurizer is insufficient, so it is necessary to achieve good desulfurization effect and high sulfur capacity It often needs to be carried out at a higher temperature, which increases energy consumption and operating costs; 4) It is still necessary to find a simpler preparation method for desulfurization agent, improve the utilization rate of active components, and reduce costs

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] A preparation method of zinc oxide-based normal temperature deep composite desulfurizer, adopting the following steps:

[0035](1) Zinc nitrate, aluminum nitrate and manganese nitrate are dissolved in water, and the concentration is prepared into respectively the salt solution of 0.1mol / L and then mixed, fully stirred until uniform, and mixed metal salt solution is obtained; wherein, zinc nitrate and aluminum nitrate And the mol ratio of manganese nitrate is 100:15:5; Preparation concentration is the sodium carbonate solution of 0.1mol / L simultaneously;

[0036] (2) Add sodium carbonate solution to the above mixed salt solution, the molar ratio of the mixed salt to the sodium carbonate is 1:1.5, react at 70°C for 1 h to obtain a precursor slurry; Fully stir the body slurry and age at a temperature of 80°C for 4 hours;

[0037] (3) Centrifuge the precursor slurry, collect the precipitate, wash the precipitate with deionized water, dry at 90°C for 6 hours, and then roast...

Embodiment 2

[0040] A preparation method of zinc oxide-based normal temperature deep composite desulfurizer, adopting the following steps:

[0041] (1) Dissolve zinc acetate, aluminum nitrate and nickel nitrate in water, and mix them into salt solutions with a concentration of 0.05mol / L respectively, and mix them thoroughly until they are evenly mixed to obtain a mixed metal salt solution; wherein, zinc acetate and aluminum nitrate And the molar ratio of nickel nitrate is 100:1:20; Prepare the ammonium carbonate solution that concentration is 0.05mol / L simultaneously;

[0042] (2) Add ammonium carbonate solution to the above mixed salt solution, the molar ratio of the mixed salt to the ammonium carbonate is 1:2, react at 20°C for 2 hours to obtain a precursor slurry; then the obtained precursor Fully stir the body slurry, and age at a temperature of 90°C for 2 hours;

[0043] (3) Centrifuge the precursor slurry, collect the precipitate, wash the precipitate with deionized water, dry at 80...

Embodiment 3

[0046] A preparation method of zinc oxide-based normal temperature deep composite desulfurizer, adopting the following steps:

[0047] (1) Zinc chloride, aluminum nitrate and cobalt nitrate are dissolved in water, are mixed respectively after being prepared into the salt solution that concentration is 3mol / L, fully stir until uniform, obtain mixed metal salt solution; Wherein, zinc chloride and nitric acid The molar ratio of aluminum and cobalt nitrate is 100:25:15; the ammonium bicarbonate solution whose concentration is 3mol / L is prepared simultaneously;

[0048] (2) Add ammonium bicarbonate solution to the above mixed salt solution, the molar ratio of the mixed salt to the ammonium bicarbonate is 1:4, react at 60°C for 2h under stirring to obtain a precursor slurry; then the obtained The precursor slurry was fully stirred and aged at 80°C for 4 hours;

[0049] (3) Centrifuge the precursor slurry, collect the precipitate, wash the precipitate with deionized water, dry at 12...

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Abstract

The invention relates to a zinc oxide based normal-temperature deep desulfurizing agent as well as a preparation method and application thereof. During preparation, a mixed solution of a zinc salt, an aluminum salt and an aid metallic salt is subjected to a one-step coprecipitation reaction to form a compound precipitate; the compound precipitate is subjected to aging, drying and roasting to obtain the zinc oxide based normal-temperature deep compound desulfurizing agent. The prepared zinc oxide based normal-temperature deep desulfurizing agent is used for the normal-temperature deep removal of H2S in various gaseous and liquid materials in the field of petroleum and coal chemical industries; that is, the fixed-bed operation is adopted; in conditions that a reaction temperature is 20 to 60 DEG C and operation pressure is 0.1MPa to 5MPa, the volume space velocity of liquid is controlled to be 1h<-1> to 12h<-1> or a gas-phase space velocity is controlled to be 1,000h<-1> to 30,000h<-1>; the H2s of which the content is 1ppm to 1,000ppm in a to-be-treated material is removed until the content is not more than 0.03ppm. Compared with the prior art, the desulfurizing agent prepared by the preparation method has breakthrough sulfur capacity, which reaches 26.1 percent, at a normal temperature and desulfurization precision which reaches 0.03ppm or below; the preparation method is simple, and can be used for large-scale industrialized production.

Description

technical field [0001] The invention belongs to the technical field of energy and chemical materials, and relates to a zinc oxide-based deep desulfurizer at normal temperature and its preparation method and application, in particular to a method for desulfurizing hydrogen sulfide in various gaseous and liquid materials at normal temperature in the field of petroleum and coal chemical industry. Zinc oxide-based desulfurizer for deep removal and its preparation method and application. Background technique [0002] Hydrogen sulfide (H 2 S) widely exists in petroleum and coal chemical products such as olefins, liquefied petroleum gas, natural gas, and synthetic gas. During the transportation and storage of these chemical raw materials, H 2 S will corrode equipment and pipes. Especially in the process of its subsequent deep processing and utilization, a very small amount of H 2 The presence of S will lead to catalyst poisoning. Therefore, in the industrial production process...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D53/52B01D53/82C10L3/10C10K1/32C10K1/20C10G29/16C01B3/56B01J20/08B01J20/06B01J20/30C07C7/148C07C11/06C07C11/04
CPCB01D53/52B01D53/82B01D2253/104B01D2253/1124B01D2257/304B01J20/041B01J20/06B01J20/08B01J2220/42B01J2220/4806C01B3/56C07C7/148C10G29/16C10K1/20C10K1/32C10L3/103C07C11/06C07C11/04
Inventor 张磊叶丽萍陈孙维罗勇李建龙
Owner SHANGHAI RES INST OF CHEM IND
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