High temperature steam blowing - calcining activation - acid treating regeneration failure gamma - alumina microballoon

A technology of alumina and high temperature water vapor, applied in chemical/physical process, catalyst regeneration/reactivation, physical/chemical process catalyst, etc., can solve problems such as equipment corrosion

Inactive Publication Date: 2012-08-22
谢志美 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Chinese patent 200610018373.7 reports the method of using dilute nitric acid and calcining to regenerate γ-alumina microspheres, but this method requires the application of high-concentration nitric acid to treat the invalid γ-alumina microspheres, which will cause serious corrosion to the equipment; A large amount of water is required for washing, and a large amount of waste water is generated during the production process

Method used

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  • High temperature steam blowing - calcining activation - acid treating regeneration failure gamma - alumina microballoon
  • High temperature steam blowing - calcining activation - acid treating regeneration failure gamma - alumina microballoon
  • High temperature steam blowing - calcining activation - acid treating regeneration failure gamma - alumina microballoon

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Put 100 kg of invalid γ-alumina microspheres with an average particle size of 2mm into the tower reactor, and introduce high-temperature steam at 1.1MPa and 121°C from the top inlet of the tower reactor to purge the invalid γ-alumina microspheres. Aluminum microspheres for 20 hours; after cooling, immerse the γ-alumina microspheres in an aqueous sodium nitrate solution with a mass concentration of 5% for 6 hours; place the soaked invalid γ-alumina microspheres and the solution in a pore size of less than 0.5mm Filter out moisture and fine alumina powder, put it into a low-speed centrifuge, and dry it by centrifugation at 200 rpm for 10 minutes, then place it in an air-containing atmosphere and calcinate at 750°C for 3 hours; the calcined The gamma-alumina microspheres were naturally cooled to room temperature, soaked in a nitric acid solution with a mass concentration of 1% for 3 hours, and then filtered and dried;

[0018] Bake at 400°C for 2 hours in an air atmosphere...

Embodiment 2

[0020] Put 100 kg of invalid γ-alumina microspheres with an average particle size of 2mm into the tower reactor, and feed 1.3MPa, 194°C high-temperature steam from the top inlet of the tower reactor to purge the invalid γ-alumina microspheres. Aluminum microspheres for 12 hours; after cooling, immerse the γ-alumina microspheres in an aqueous solution of sodium carbonate with a mass concentration of 5% for 3 hours; place the soaked invalid γ-alumina microspheres and the solution in a pore size less than 0.5mm Filter out moisture and fine alumina powder, put it into a low-speed centrifuge, and dry it for 5 minutes at a speed of 400 rpm, then place it in an air-containing atmosphere and calcinate at 800°C for 2 hours; the calcined The gamma-alumina microspheres were naturally cooled to room temperature, soaked in a nitric acid solution with a mass concentration of 2.5% for 2 hours, and then filtered and dried;

[0021] Place in an air atmosphere and bake at 300°C for 2.5 hours, t...

Embodiment 3

[0023] Put 100 kg of invalid γ-alumina microspheres with an average particle size of 2mm into the tower reactor, and inject high-temperature steam at 300°C from the top inlet of the tower reactor to purge the invalid γ-alumina microspheres 12 hours; after cooling, immerse the γ-alumina microspheres in an aqueous sodium hydroxide solution with a mass concentration of 2% for 2 hours; place the soaked invalid γ-alumina microspheres and the solution in a filter with a pore size of less than 0.5mm net, filter out moisture and fine alumina powder, put it into a low-speed centrifuge, and centrifuge and dry it at a speed of 500 rpm for 5 minutes, then place it in an air-containing atmosphere and calcinate at 800 ° C for 2 hours; the calcined γ - Alumina microspheres were naturally cooled to room temperature, immersed in a nitric acid solution with a mass concentration of 3.0% for 1.5 hours, filtered and dried; placed in an air atmosphere at 300° C. for 3.0 hours, and naturally cooled t...

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Abstract

The invention relates to failure gamma alumina microballoon regeneration processing technology field used for purifying and regeneration operating fluid in hydrogen peroxide production processing, provides a method for a high temperature water vapor blowing - calcining activation acid treating technology regeneration failure gamma - alumina microballoon and comprises the steps: employing high temperature water vapor to blow failure gamma alumina microballoon; then immersing gamma alumina microballoon into alkali metal compound aqueous solution, filtering, drying and calcining activation; cleaning and drying calcined gamma alumina microballoon after immersed in the dilute nitric acid solution. The regeneration failure gamma alumina employed the present invention has the characteristics of low production cost, low equipment corrosion, few three wastes in productive process and excellent regeneration gamma alumina microballoon performance.

Description

technical field [0001] The patent of the present invention relates to a method for regenerating invalid γ-alumina microspheres, in particular to a method for regenerating invalid γ-alumina microspheres used for purifying and regenerating working fluids in the hydrogen peroxide production process. Background technique [0002] Hydrogen peroxide is an important chemical raw material, and the industrial preparation of hydrogen peroxide mainly adopts the anthraquinone method. During the production of hydrogen peroxide by using 2-alkylanthraquinone such as 2-ethylanthraquinone as a raw material, hydrogenation by-product octahydroanthraquinone (OHAHQ) and oxidation by-product hydroxy anthrone such as anthracolone (OAT), anthrone and Hydroanthraquinone epoxide (THAQE). In the hydrogen peroxide production cycle, the degradation products generated by multiple cycles reduce the concentration of effective anthraquinone, which will lead to many problems such as low production efficienc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J38/02B01J38/06B01J38/64B01J38/14B01J38/60
Inventor 谢志美李加加胡舜钦
Owner 谢志美
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