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Regeneration method for cobalt-manganese catalyst in p-xylene oxidation mother liquor

A p-xylene and catalyst technology, which is applied in the field of chemical engineering, can solve the problems of complex operation and flow of the regeneration method, high process requirements, and the inability to apply mass production of TA production, etc., achieving remarkable regeneration effect, simple process, and optimized regeneration process conditions Effect

Inactive Publication Date: 2014-02-12
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The recovery method of the cobalt-manganese catalyst in the p-xylene oxidation mother liquor involved in the above-mentioned patent has already been applicable to the recovery of cobalt and manganese catalysts in the mass production of TA. Mass production TA production

Method used

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  • Regeneration method for cobalt-manganese catalyst in p-xylene oxidation mother liquor

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Effect test

Embodiment 1

[0045] Take 200g of catalyst slurry, analyze the content of soluble / insoluble Co and Mn, put it into the reaction kettle, heat it to 200°C under the protection of nitrogen, according to the space velocity of 1000h -1 A mixed gas of air and nitrogen (O in the mixed gas 2 / N 2 =5:100) Keep the pressure inside the reactor at 2.0MPa and react for 30 minutes to decompose and regenerate the recovered catalyst. After the reaction, analyze the soluble / insoluble Co and Mn content in the regenerated catalyst, and calculate the precipitation of insoluble Co and Mn in the recovered catalyst slurry The decomposition rate of Co precipitation is 33.36%, and the decomposition rate of Mn precipitation is 39.24%.

Embodiment 2

[0047] Take 200g of catalyst slurry, analyze the content of soluble / insoluble Co and Mn, put it into the reaction kettle, add 0.6g of acetaldehyde, heat to 200°C under the protection of nitrogen, according to the space velocity of 800h -1 A mixed gas of air and nitrogen (O in the mixed gas 2 / N 2 =5:100) Keep the pressure inside the reactor at 2.0MPa and react for 30 minutes to decompose and regenerate the recovered catalyst. After the reaction, analyze the soluble / insoluble Co and Mn content in the regenerated catalyst, and calculate the precipitation of insoluble Co and Mn in the recovered catalyst slurry The decomposition rate of Co precipitation is 67.77%, and the decomposition rate of Mn precipitation is 83.51%.

Embodiment 3

[0049] Take 200g of catalyst slurry, analyze the content of soluble / insoluble Co and Mn, put it into the reaction kettle, add 0.2g of acetaldehyde, heat to 180°C under the protection of nitrogen, according to the space velocity of 1000h -1 A mixed gas of air and nitrogen (O in the mixed gas 2 / N 2 =1:100) Keep the pressure inside the reactor at 2.5MPa and react for 70 minutes to decompose and regenerate the recovered catalyst. After the reaction, analyze the soluble / insoluble Co and Mn content in the regenerated catalyst, and calculate the precipitation of insoluble Co and Mn in the recovered catalyst slurry The decomposition rate of Co precipitation is 89.58%, and the decomposition rate of Mn precipitation is 95.34%.

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Abstract

The invention relates to a regeneration method for a cobalt-manganese catalyst in p-xylene oxidation mother liquor. The regeneration method includes adding an oxalic acid solution and a sodium hydroxide solution which are used as precipitating agents into the p-xylene oxidation mother liquor; filtering to obtain slurry; adding the slurry into a reactor; adding acetaldehyde the weight of which accounts for 0.1-1% of the total weight of the slurry; heating to 150-220 DEG C; and feeding a gas mixture of air and nitrogen to maintain the pressure of the reactor to be 1.5-2.5 MPa and reacting for 30-90 min. According to the regeneration method, the acetaldehyde is added into the slurry, and therefore the cobalt-manganese catalyst in the p-xylene oxidation mother liquor is decomposed and regenerated at a low temperature. Regeneration technology conditions are optimized. The technology is simple and the regeneration effect is significant. The activity and stability of the regenerated catalyst can be recovered to the level of a new catalyst, and can be used again for TA preparation by oxidation of PX.

Description

technical field [0001] The invention belongs to the technical field of chemical engineering, and in particular relates to a method for regenerating a cobalt-manganese catalyst in a p-xylene oxidation mother liquor. Background technique [0002] Terephthalic Acid (TA for short) is a very important organic chemical raw material widely used in polyester and other chemical production. TA is obtained by oxidation reaction with p-xylene (PX) as raw material, cobalt acetate and manganese acetate as catalyst, and HBr as auxiliary agent under certain reaction pressure and reaction temperature. Recycling PX oxidation Co, Mn catalyst regeneration and reapplying PX oxidation to produce TA has important economic and social benefits. [0003] GB 1413829 invented a method for recovering and regenerating metal catalysts from TA residues. Stir and extract the TA residue at 80-85°C with water (the weight ratio of water to residue is 5:1) overnight, cool and filter to separate the insoluble ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/40B01J31/04B01J38/14B01J38/64B01J38/62
Inventor 沈品德李超武文良丁家海周晓峰王建平周志伟郭向前
Owner CHINA PETROLEUM & CHEM CORP