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Method for comprehensive recovery of valuable elements in aluminum-based petroleum refining catalysts by using reducing gas

A technology of valuable elements and catalysts, applied in the field of comprehensive recovery of valuable elements, can solve problems such as complicated separation process

Active Publication Date: 2020-07-07
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Aiming at the defect that the valuable element separation process is complicated in the existing petroleum refining waste catalyst recovery technology, the present invention provides a method for pretreating the petroleum refining waste catalyst by using reducing gas reduction to achieve efficient separation and recovery of valuable elements. The thermal reduction pretreatment makes the difference in the properties of the compounds corresponding to the valuable metal elements in the spent catalyst, so as to realize the step-by-step and efficient separation of the valuable elements, and at the same time realize the comprehensive recovery of the valuable elements

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] (1) Reduction roasting process

[0032] Extraction of spent petroleum hydrodesulfurization catalyst Ni-Mo / γ-Al 2 o 3 After being oxidized and roasted at 550°C, it contains the following elements: Al28.1%, Ni 12.3%, V 6.1%, Mo 4.7%, add sodium carbonate according to 1.2 times the theoretical demand, mix and grind until the abrasives all pass through the 200 molybdenum mesh sieve . Put the grinding material in a heating furnace, exhaust the air, and then pass in carbon monoxide at a flow rate of 100mL / min, heat to 950°C at a heating rate of 5°C / min, keep it warm for 180min, then cool to room temperature and take it out.

[0033] (2) Step-by-step extraction process of valuable elements

[0034] Add the reduction product to 2mol / L sodium hydroxide solution, stir and leach in a water bath at 80°C for 60 minutes, filter while hot to obtain a sodium aluminate solution, the leaching rate of aluminum can reach 99.1%, and metal ions such as molybdenum and vanadium in the sodiu...

Embodiment 2

[0036] (1) Reduction roasting process

[0037] Extraction of spent petroleum hydrodesulfurization catalyst Ni-Mo / γ-Al 2 o 3 After oxidizing and roasting at 650°C, it contains the following elements Al27.1%, Ni 12.1%, V 5.8%, Mo 4.6%, add sodium carbonate according to 1.3 times the theoretical demand, mix and grind until the grinding materials pass through the 200 molybdenum mesh sieve. Put the grinding material in the heating furnace, after the air is exhausted, hydrogen gas is introduced at a flow rate of 100mL / min, heated to 1050°C at a heating rate of 5°C / min, kept for 100 min, cooled to room temperature and taken out.

[0038] (2) Step-by-step extraction process of valuable elements

[0039] Add the reduction product to 1mol / L sodium hydroxide solution, stir and leach in a water bath at 70°C for 40 minutes, and filter while hot to obtain a sodium aluminate solution. The leaching rate of aluminum can reach 99.3%, and molybdenum and molybdenum can hardly be detected in the...

Embodiment 3

[0041] (1) Reduction roasting process

[0042] Extraction of spent petroleum hydrodesulfurization catalyst Ni-Mo / γ-Al 2 o 3 After being oxidized and roasted at 500°C, it contains the following elements: Al28.1%, Ni 12.3%, V 6.1%, Mo 4.7%, add sodium carbonate according to 2.0 times the theoretical demand, mix and grind until the abrasives all pass through the 200 molybdenum mesh sieve . Put the grinding material in a heating furnace under the protection of nitrogen, put the grinding material in the heating furnace, after the air is exhausted, feed methane at a flow rate of 100mL / min, heat it to 950 °C at a heating rate of 10 °C / min, and keep it warm. After 90min, cool to room temperature and take out.

[0043] (2) Step-by-step extraction process of valuable elements

[0044] Add the reduction product into deionized water, stir and leaching in a water bath at 80°C for 120 minutes, and filter while hot to obtain a sodium aluminate solution. The leaching rate of aluminum can ...

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Abstract

The invention discloses a method for realizing comprehensive recovery of valuable elements in an aluminum-based petroleum refining catalyst by utilizing reducing gas. The method comprises the following steps that spent catalyst is preatreated by adopting a reduction heat treatment process, and the three kinds of valuable metal elements in the spent catalyst generate an aluminum salt capable of being dissolved in water, metal elementary substance nickel cobalt with magnetism and acid solubility, and acid-resistant and alkali-resistant rare metal low-valence oxide, a simple substance or a carbide correspondingly, so that the property difference of the valuable elements compound to be recycled is expanded; the aluminum oxide is extracted by using an aqueous solution or an alkali solution, thenickel and cobalt are extracted through magnetic separation or acid solution leaching, and the rare metals are enriched and recycled in the leaching residues. The method has the advantages that the process is simple and reasonable, the used reducing agent is economic and environment-friendly, efficient separation and comprehensive recovery of the valuable elements in the spent catalyst can be realized at the same time, and the economic benefits are remarkable and the like.

Description

technical field [0001] The invention relates to a method for realizing comprehensive recovery of valuable elements in aluminum-based petroleum refining catalysts by using reducing gas, and belongs to the technical field of nonferrous metallurgy. Background technique [0002] Petrochemical industry is a catalyst-centered industrial sector, and about 90% of petroleum refining reactions need catalysts to proceed. During the use of the catalyst, the catalyst will be deactivated due to carbon deposition, heavy metal poisoning, and sintering of the active phase. When these deactivated catalysts cannot be economically regenerated, they become spent catalysts. Spent catalysts usually contain organic matter such as carbon deposits and residual oil, as well as sulfur, heavy metal elements nickel, cobalt, rare metal elements tungsten, molybdenum, vanadium, and carrier alumina. Without harmless disposal, unstable toxic and harmful substances in spent catalysts can easily diffuse into ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C22B1/02C22B7/00C22B21/00C22B23/00C22B34/36C22B34/34C22B34/22
CPCC22B1/02C22B7/001C22B7/007C22B7/008C22B21/0007C22B21/003C22B23/0415C22B23/0446C22B34/225C22B34/345C22B34/365Y02P10/20
Inventor 徐盛明王文强韩宇张磊李震
Owner TSINGHUA UNIV
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