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Comprehensive utilization method of waste FCCU catalyst

A technology of catalyst and mixed liquid, which is applied in the field of comprehensive utilization of waste FCCU catalysts, can solve the problems of long process route, dripping, complicated operation, etc., and achieve the effects of low operation complexity, avoiding the risk of poisoning, and short process route

Inactive Publication Date: 2018-09-04
崔延强
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reaction raw materials involved in this recovery technology are highly toxic. Due to the risk of poisoning the staff, serious leakage and leakage at the filtration site, there are more process equipment, longer process routes, more complicated operations, and higher energy consumption. , and the residual waste is not less than 15%, and these residual wastes are theoretically hazardous wastes

Method used

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  • Comprehensive utilization method of waste FCCU catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Mix 500ml of concentrated sulfuric acid and 700g of FCCU catalyst in a reaction kettle, heat to 80°C and stir for 2 hours, then cool down to 60°C, add 15ml of hydrogen peroxide and 10ml of oxalic acid at the same time, mix and stir for 30 minutes, add 20g of sodium bicarbonate and stir for 30 minutes, stir Keep the reaction temperature at 95°C during the process, filter, evaporate the filtrate at 10KPa and 165°C to evaporate about 85% of concentrated sulfuric acid, the concentration of concentrated sulfuric acid obtained at this time is ≮76%, and the content of lanthanum and cerium rare earth elements in the concentrated filtrate is ≥17%. Fe, Cu, S, Pb, As total≯3.5%. The filter residue is washed with water and then dried to obtain a mixed powder of alumina and silicon dioxide with a metal content (excluding Al) ≤ 0.5%.

Embodiment 2

[0028] Mix 500ml of concentrated sulfuric acid and 700g of FCCU catalyst in a reaction kettle, heat to 80°C and stir for 3 hours, then add 15ml of hydrogen peroxide and 10g of oxalic acid at the same time, mix and stir for 60 minutes, add 20g of sodium bicarbonate and stir for 60 minutes, keep the reaction during stirring Filter at 95°C, evaporate about 85% of concentrated sulfuric acid from the filtrate at 10KPa and 165°C, the concentration of concentrated sulfuric acid obtained at this time is ≮83%, and the content of lanthanum and cerium rare earth elements in the concentrated filtrate is ≥21%, Fe, Cu, The total of S, Pb, and As is ≯5%. The filter residue is washed with water and then dried to obtain aluminum trioxide and silicon dioxide powders with a metal content (excluding Al) ≤ 0.1%.

Embodiment 3

[0030] Mix 500ml of concentrated sulfuric acid and 700g of FCCU catalyst in a reaction kettle, heat to 120°C and stir for 2 hours, then cool down to 80°C, add 15ml of hydrogen peroxide and 10ml of oxalic acid at the same time, mix and stir for 30 minutes, add 20g of sodium bicarbonate and stir for 30 minutes, During the stirring process, keep the reaction temperature at 95°C, filter, evaporate the filtrate at 10KPa, 165°C, about 85% of concentrated sulfuric acid, the concentration of concentrated sulfuric acid obtained at this time is ≮81%, and the content of lanthanum and cerium rare earth elements in the concentrated filtrate is ≥19% , Fe, Cu, S, Pb, As total≯2%. The filter residue is washed with water and then dried to obtain alumina and silicon dioxide powders with a metal content of ≤0.5%.

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Abstract

The invention discloses a comprehensive utilization method of waste FCCU catalyst. The comprehensive utilization method of waste FCCU catalyst comprises following steps: waste FCCU catalyst is introduced into a reaction vessel, concentrated sulfuric acid with a mass concentration of 98% is added for immersion, hydrogen peroxide and oxalic acid are added for mixing and stirring, and sodium bicarbonate is added, so that the pores on catalyst microspheres are cut through by micro pulse generated in neutralization reaction process of sodium bicarbonate with concentrated sulfuric acid; after reaction, filtering is carried out; an obtained filtrate is delivered through an evaporator for recovery of about 80% sulfuric acid in the filtrate, the left sulfuric acid is stored in the evaporator for mixing with reaction liquid obtained in a next time of reaction, a plurality of evaporative concentration is carried out so as to obtain an acid solution rich in lanthanum and cerium, wherein the concentration of the acid solution is 25%; an obtained filter residue is subjected to water washing acid removing and drying collecting so as to obtain aluminium trioxide and silica powder, an obtained water washing liquid is subjected to evaporative concentration and cooling, and is recycled as water used in water washing acid removing, and a part of the water washing liquid is discharged into a sewagetreatment station for treatment and recycling. The raw materials adopted in the comprehensive utilization method posses no direct toxicity, operation complexity is low, energy consumption is low, recovery rate is high, after waste FCCU catalyst recycling, residual refuse accounts for 0.5% or lower.

Description

technical field [0001] The invention belongs to the technical field of recycling waste chemical raw materials, and in particular relates to a method for comprehensive utilization of waste FCCU catalysts. Background technique [0002] For spent FCCU catalysts, at present, most refineries adopt a continuous process of discharging mixed catalysts while adding new catalysts, and the discharged mixed catalysts still become waste. If the spent FCCU catalyst is directly discharged outside, it will not only waste resources, but also have a great impact on the environment. [0003] The main principle of the existing waste FCCU catalyst recovery technology is to react toxic raw materials such as sulfuric acid, HCL, hydrogen peroxide, ammonia, and alkali in the reactor, and then filter through the plate and frame filter press. . The reaction raw materials involved in this recovery technology are highly toxic. Due to the risk of poisoning the staff, serious leakage and leakage at the ...

Claims

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Application Information

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IPC IPC(8): C01F17/00C01F7/02C01B33/12B09B3/00
CPCC01B33/124C01F7/02C01F17/282B09B3/80Y02P20/584
Inventor 崔延强
Owner 崔延强
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