Fine desulfurizer and preparation method thereof

A technology of fine desulfurization and carrier, applied in the field of fine desulfurizer and its preparation, can solve the problems of corrosion of industrial pipelines and equipment, poisoning of catalysts, reduced product quality, etc., and achieve the effects of good mechanical strength, large specific surface area, and improved desulfurization effect.

Active Publication Date: 2015-11-11
CNOOC GAS & POWER GRP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Thiophene is an organosulfur and a heteroatom five-membered monocyclic compound that causes corrosion of industrial pipes and equipment, poisons catalysts and reduces product quality

Method used

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  • Fine desulfurizer and preparation method thereof

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preparation example Construction

[0035] Specifically, the preparation method of the refined desulfurizer of the present invention includes the following steps:

[0036] Step a: Mixing one or two of zinc nitrate, manganese nitrate and magnesium nitrate with aluminum nitrate to prepare a mixed salt solution. Specifically, distilled water can be used to prepare the above mixed salt solution. Wherein, the ratio of the amount of controlled aluminum nitrate to one or two of zinc nitrate, manganese nitrate and magnesium nitrate is greater than 2 or less than 1 / 2. The refined desulfurizer prepared by using the above ratio can effectively enrich the pores in the desulfurizer carrier. Specifically, after high-temperature roasting, a high-proportion aluminum-containing or high-proportion oxide containing zinc, manganese, magnesium, etc. is formed, which can be passed through subsequent acid Soluble and remove these oxides to enrich the pores of the carrier.

[0037] Step b: using an alkali solution as a precipitant to perf...

example 1

[0046] Example 1: Preparation of fine desulfurizer

[0047] (1) Mix 182g of aluminum nitrate and 446g of zinc nitrate and add them to 3000mL of distilled water to prepare a mixed salt solution, and then heat the mixture solution to 60°C and put it into the No. 1 constant temperature storage tank;

[0048] (2) Put 2700 mL of Na with a mass concentration of 10% 2 CO 3 The solution is heated to 60℃ and put into No. 2 constant temperature storage tank;

[0049] (3) Add the solutions in the No. 1 constant temperature storage tank and the No. 2 constant temperature storage tank co-currently to the constant temperature reactor for co-precipitation reaction, and control the reaction time to 20 minutes and the pH value during the reaction to 10.2;

[0050] (4) Filtering and washing the reaction product in step (3) to obtain a filter cake;

[0051] (5) Dry the filter cake obtained in step (4) at 100°C for 8 hours;

[0052] (6) Add 4% of graphite and an appropriate amount of distilled water to the ...

example 2

[0055] Example 2: Preparation of fine desulfurizer

[0056] (1) Mix 562g of aluminum nitrate and 148g of zinc nitrate and add them to 4500mL of distilled water to prepare a mixed salt solution, then heat the mixture solution to 65°C and put it into the No. 1 constant temperature storage tank;

[0057] (2) 3500mL of Na with a mass concentration of 10% 2 CO 3 The solution is heated to 65℃ and then put into No. 2 constant temperature storage tank;

[0058] (3) The solutions in the No. 1 constant temperature storage tank and the No. 2 constant temperature storage tank are added dropwise to the constant temperature reaction kettle for co-precipitation reaction, and the reaction time is controlled to 22 minutes and the pH value during the reaction is 9.2;

[0059] (4) Filtering and washing the reaction product in step (3) to obtain a filter cake;

[0060] (5) Dry the filter cake obtained in step (4) at 120°C for 8 hours;

[0061] (6) Add 4% of graphite and an appropriate amount of distilled wa...

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Abstract

The invention discloses a fine desulfurizer and a preparation method thereof. The fine desulfurizer comprises a carrier and an active component, wherein the carrier is composite oxide formed through reacting one or two of zinc, manganese and magnesium with aluminum; the active component is cupric oxide; the preparation method of the fine desulfurizer includes the following steps: mixing one or two of zinc nitrate, manganous nitrate and magnesium nitrate with aluminium nitrate to prepare a mixed salt solution; carrying out coprecipitation through reacting aqueous alkali as a precipitant with the mixed salt solution; washing, drying and calcinating the precipitate obtained in the previous step to obtain a calcination sample; placing the calcination sample in acid liquor for acid dipping treatment to obtain the carrier; placing the carrier into a copper nitrate solution for dipping treatment, then drying and carrying out pyrolysis to obtain the fine desulfurizer. The fine desulfurizer can effectively eliminate thiofuran which is difficult to remove through conventional methods; the carrier of the fine desulfurizer is subjected to acid dipping treatment, so that the fine desulfurizer is large in specific surface, high in mechanical strength, good in stability and high in desulfuration effect and breakthrough sulfur capacity.

Description

Technical field [0001] The present invention relates to the technical field of desulfurizers, and more specifically, to a method suitable for the removal of trace amounts of sulfur (including thiophene, mercaptans, carbon disulfide, etc.) in raw materials for coke oven gas to synthesize natural gas or coal to synthesize natural gas. And inorganic sulfur) fine desulfurizer and its preparation method. Background technique [0002] With the widespread application of coal-based synthesis gas methanation processes such as coal-to-natural gas and coke oven gas-to-natural gas, in order to extend the service life of nickel-based methanation catalysts, the depth of sulfur removal in methanation feed gas has been paid more and more attention. The general requirement is to reduce the sulfur content of the feed gas entering the nickel-based methanation catalyst bed to the ppb level. [0003] The sulfur in the synthesis gas obtained from coal gasification and coking by-product coke oven gas ex...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C10K1/00C10K1/20
Inventor 唐令力刘玉成宋鹏飞何洋邢云郑珩王秀林张新波侯建国刘毅高振曾凌云
Owner CNOOC GAS & POWER GRP
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