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Recovery method for waste CO sulfur tolerant shift catalyst

A technology for sulfur-resistant conversion and recovery methods, which is applied in chemical recovery, chemical instruments and methods, inorganic chemistry, etc., and can solve problems such as poor control of zinc content

Active Publication Date: 2015-02-18
河北瑞克新能源科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the recovery process, zinc is used to replace cobalt twice. Since the amount of zinc required for the replacement is not easy to control, impurity zinc is easily introduced into the replaced cobalt.

Method used

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  • Recovery method for waste CO sulfur tolerant shift catalyst

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] A spent CO sulfur-tolerant shift catalyst, after fluorescence analysis, its composition is mass percent (%): Co (calculated as CoO): 4.1%, Mo (calculated as MoO 3 Total): 11.3%, K 2 O: 3.4%, S (as SO 2 Total): 15.55%, Fe 2 o 3 : 0.15%, Al 2 o 3 : 65.5%. The spent catalyst was pulverized to below 60 mesh, and 100 g of the pulverized spent catalyst was taken, calcined at 600° C. for 1 h, and weighed 85.5 g after calcined. Add 140 g of potassium carbonate to the spent catalyst after primary roasting, and roast at 350° C. for 1.5 h. After cooling, leaching with 50°C distilled water for 4h. Filter to obtain the filter residue and filtrate 1. Add 1 mol / L nitric acid to the filter residue, stir and react at 50°C for 2 hours, and control the pH of the reaction solution to 1-2. After the reaction, the waste residue was removed by filtration to obtain filtrate 2. Regulate the pH value of the filtrate 2 with 15% potassium carbonate solution, adjust the pH to be about 4, ...

Embodiment 2

[0023] A spent CO sulfur-tolerant shift catalyst, after fluorescence analysis, its composition is mass percentage (%): Co (calculated as CoO): 3.8%, Mo (calculated as MoO 3 Total): 9.5%, K 2 O: 2.6%, S (as SO 2 Total): 13.52%, Fe 2 o 3 : 0.08%, Al 2 o 3 : 70.5%. The spent catalyst was crushed to below 100 mesh, and 100 g of the crushed spent catalyst was taken, calcined at 500° C. for 3 h, and weighed 84.6 g after calcined. Add 165 g of potassium carbonate to the spent catalyst after primary roasting, and roast at 450° C. for 3 hours. After cooling, leaching with 70°C distilled water for 6h. Filter to obtain the filter residue and filtrate 1. Add 2 mol / L nitric acid to the filter residue, stir and react at 50°C for 2 hours, and control the pH of the reaction solution to 1-2. After the reaction, the waste residue was removed by filtration to obtain filtrate 2. Regulate the pH value of filtrate 2 with mass percentage concentration 25% potassium carbonate solution, adju...

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Abstract

The invention discloses a method for recovering waste CO sulfur-tolerant shift catalysts, in particular to a method for recycling metal oxides in cobalt and molybdenum-based waste CO sulfur-tolerant shift catalysts, and belongs to the technical field of catalysts. In the recovery method, the spent CO sulfur-tolerant shift catalyst is pulverized, roasted once, roasted twice with alkali, and then leached with hot water. After the obtained filter residue is dissolved with acid, the pH value of the solution is adjusted in steps of alkali to remove Fe(OH)3 and separate Al(OH)3 respectively to obtain a mixed solution containing cobalt nitrate and potassium nitrate. The mixed solution can be directly used to prepare a new CO sulfur-tolerant shift catalyst. The filtrate obtained by soaking in hot water is used to adjust the pH value step by step with acid, and finally molybdic acid and potassium nitrate can be obtained. The recovery method can fully separate and recover the metals in the waste CO sulfur-tolerant shift catalyst, the recovery rate of cobalt can reach more than 85%, and the recovery rate of molybdenum can reach more than 90%.

Description

technical field [0001] The invention relates to a recovery method of a waste CO sulfur-tolerant shift catalyst, in particular to a method for recycling metal oxides in cobalt and molybdenum-based waste CO sulfur-tolerant shift catalysts, and belongs to the technical field of catalysts. Background technique [0002] CO sulfur-tolerant shift catalysts are widely used in the fertilizer industry and petroleum industry due to their excellent sulfur tolerance and low-temperature activity. With the development of industry, the amount of CO shift catalyst is increasing. The active components of the CO sulfur-tolerant shift catalyst are cobalt and molybdenum, and the carrier is aluminum oxide, which may contain potassium as an additive. According to incomplete statistics, more than 3,000 tons of waste CO sulfur-tolerant shift catalysts are replaced every year in my country's chemical fertilizer industry. If such a large amount of waste CO sulfur-tolerant shift catalysts is not prop...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01F7/34C01G39/00C01G51/00C01D9/04
CPCY02P20/584
Inventor 周焕文黄燕
Owner 河北瑞克新能源科技有限公司