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Waste FCC (fluid catalytic cracking) catalyst reactivation method based on controlled leaching, metal passivation and effective component compensation

A technology of spent catalysts and active ingredients, applied in the direction of catalyst regeneration/reactivation, physical/chemical process catalysts, chemical instruments and methods, etc., can solve the loss of alumina and rare earth lanthanum oxide, short service time, catalyst skeleton collapse, etc. The problem is to overcome the loss of alumina, keep the acidity stable, and improve the catalytic performance.

Active Publication Date: 2019-01-18
LIANYUNGANG NORMAL COLLEGE
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Problems solved by technology

However, due to the complex process, harsh reaction conditions, environmental pollution, and high one-time speculation, this technology has not been applied.
Domestic Zheng Lianyi et al. used oxidation-acid leaching-washing-drying-activation to obtain the FCC revived catalyst, and the micropores of the catalyst obtained after treatment were restored, but the removal rate of heavy metal nickel and alum was low, and a part of the aluminum was dissolved into the strong acid solution, resulting in Catalyst Acid Reduction
Li Chunyi et al. used inorganic acids such as hydrochloric acid, nitric acid, sulfuric acid, and perchloric acid to conduct demetallization and revival research on spent FCC catalysts. The results showed that the effect of inorganic acids on nickel removal was very poor, resulting in poor activity of the revived catalyst.
The applicant adopted the method of using mixed acid controlled leaching to remove nickel and iron, retaining the acidic component of the catalyst, aluminum oxide, and reactivating the catalyst with rare earth metals. The results showed that the removal rate of Ni reached 45%, but the reaction Both alumina and rare earth lanthanum oxide are lost during the process, and the removal of nickel is not complete, resulting in a shorter service life of the revived catalyst despite an increase in activity
The domestic patent "A Method for Reviving FCC Waste Catalyst" application number (Patent No.: 200810014209.8) discloses a method for reviving spent FCC catalysts, which uses the synergistic effect of inorganic acids and organic acids to unblock the blocked catalyst micropores , the skeleton of the catalyst has been reconstructed, but the effect of leaching heavy metal nickel with hydrochloric acid is only about 30%. inactivation faster
The application number of the domestic patent "Roasting and Silicon Tetrachloride Mixed Reaction Catalytic Cracking Spent Catalyst Resurrection Method" (Patent No.: 201510178636.X) discloses the use of gas-phase silicon tetrachloride and waste FCC catalyst for gas-solid phase reaction to revive the spent catalyst. The method utilizes the decomposition of silicon tetrachloride at a certain temperature to generate chlorine gas to form nickel chloride and wash it with water to remove nickel. The effect of removing nickel is poor, and silicon tetrachloride has a toxic gas with suffocating and irritating odor, and the production environment is harsh.
[0005] Most of the above existing waste FCC catalyst revival methods use hydrochloric acid, sulfuric acid or sulfidation or chlorination to remove heavy metal nickel. Not only the removal efficiency is low, but the process is complicated. The catalyst skeleton collapsed, and a large amount of waste acid was produced at the same time, causing secondary pollution to the environment

Method used

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  • Waste FCC (fluid catalytic cracking) catalyst reactivation method based on controlled leaching, metal passivation and effective component compensation
  • Waste FCC (fluid catalytic cracking) catalyst reactivation method based on controlled leaching, metal passivation and effective component compensation
  • Waste FCC (fluid catalytic cracking) catalyst reactivation method based on controlled leaching, metal passivation and effective component compensation

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Embodiment 1

[0029] Embodiment 1: by sieving particle size greater than 30 μm waste catalyst (below the same), react with impurity-removing active agent, (in this embodiment waste FCC catalyst is recorded as former agent, and its test sample analysis data is as follows figure 1 As shown, the phase analysis is as follows figure 2 As shown, the following examples are the same), select 1% impurity removal activator and spent catalyst to control the impurity removal reaction, the liquid-solid ratio is 6:1, the reaction time is 3 hours, the process pH is controlled at ≮1, and the filter residue is deionized and washed for 2 After rinsing twice, the filter residue was impregnated in 0.03% boric acid and lanthanum nitrate (the amount of lanthanum nitrate added is based on the mass fraction of lanthanum oxide to control the loss of impurities, the same below), the immersion temperature was 45 ° C, the immersion time was 6 hours, and the Vacuum filtration, drying and dehydration at 120°C, calcinat...

Embodiment 2

[0030] Example 2: Select 2% impurity removal agent and spent catalyst to carry out controlled impurity removal reaction, the liquid-solid ratio is 6:1, the reaction time is 4 hours, the process pH is controlled at ≮1, the filter residue is deionized, washed twice, and rinsed 2 times a kilogram, the filter residue was immersed in 0.04% boric acid and lanthanum nitrate solution, the immersion temperature was 45°C, the immersion time was 7 hours, vacuum filtered, dried and dehydrated at 120°C, roasted at 750°C for 3.5 hours, and the revived catalyst sample was obtained. Denoted as sample 2. The chemical element analysis, specific surface area and pore volume of the obtained revived catalyst were determined. See Figure 4 , Figure 5 .

Embodiment 3

[0031] Example 3: Select 3% impurity removal activator and spent catalyst to carry out controlled impurity removal reaction, the liquid-solid ratio is 6:1, the reaction time is 5 hours, the process pH is controlled at ≮1, the filter residue is deionized, pulp washed twice, and rinsed After 2 times, the filter residue was immersed in 0.05% boric acid and lanthanum nitrate solution, the immersion temperature was 45°C, the immersion time was 8 hours, vacuum filtered, dried and dehydrated at 120°C, and roasted at 760°C for 4 hours, the revived catalyst sample was obtained. Denoted as sample 3. The chemical element analysis, specific surface area and pore volume of the obtained revived catalyst were determined. See Figure 4 , Figure 5 .

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Abstract

The invention discloses a waste FCC (fluid catalytic cracking) catalyst reactivation method based on controlled leaching, metal passivation and effective component compensation reaction, and relates to the technical field of solid waste recycling. The specific reactivation method comprises steps as follows: a controlled impurity removing reactivator is adopted for removing purifies and expanding pore size in a controlled leaching manner, and aluminum oxide can be effectively prevented from being corroded in a process of removing heavy metal; boric acid is utilized as a nickel passivator, catalytic activity of residual nickel is enabled to be inert, meanwhile, deposited new metal nickel can be further deactivated by the passivator in a petroleum cracking process, loss of rare earth lanthanum oxide in an impurity removing process is compensated, so that efficient reactivation of the a waste FCC catalyst is realized, and micro-activity of the reactivated catalyst is increased by 8.68% ascompared with that of a fresh catalyst. Light oil yield under adoption of the reactivated catalyst is close to that of the fresh catalyst. Therefore, the method has a remarkable catalyst reactivationeffect, produces no secondary pollution to the environment, is cleaner and easier to implement.

Description

technical field [0001] The invention designs a boric acid controlled leaching method, metal nickel passivation and effective component compensation reaction waste FCC waste catalyst revival method, and belongs to the technical field of solid waste treatment and comprehensive utilization. Background technique [0002] The FCC catalyst is obtained by beating alumina sol, pseudoboehmite, silica sol and adhesive with acid, spray drying, ion exchange, and loaded with rare earth RE 2 o 3 Ions, roasted to prepare petroleum cracking catalysts. FCC catalyst has become one of the most widely used catalysts in the petroleum industry due to its good selectivity, high activity, stability, excellent heat resistance, and good suppression, dehydrogenation, desulfurization, and carbon deposition prevention effects. However, when the FCC catalyst is used for a period of time, due to the pollution of heavy metals (nickel, alum, and iron), carbon deposition, particle size refinement, sinterin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J38/48B01J38/60B01J38/02B01J38/00
CPCB01J38/00B01J38/02B01J38/485B01J38/60
Inventor 卢国俭朱英杰邹翔
Owner LIANYUNGANG NORMAL COLLEGE
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