Method for recovering metallic oxide from waste aluminum base V-Mo-Ni catalyst

A technology of catalysts and oxides, applied in the direction of improving process efficiency, etc., can solve the problems of less comprehensive recycling, high solvent recovery costs, and difficulty in industrialization, and achieve good economic benefits, low recycling costs, and improve environmental conditions.

CN101457296BInactive Publication Date: 2011-04-27WUHU RENBEN ALLOY
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Publication Date
2011-04-27
Estimated Expiration
Not applicable · inactive patent

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Abstract

The invention discloses a method for recovering metal oxides from an aluminum scrap-based vanadium molybdenum nickel catalyst. The method comprises the following steps: crushing the aluminum scrap-based vanadium molybdenum nickel catalyst, evenly mixing with sodium hydroxide, calcining at high temperature of 700-1200 DEG C, maintaining a constant temperature for 3-6 hours, crushing sinter blocks, washing nickel slag with countercurrent hot water or washing aluminum hydroxide crystal with the weight ratio of liquid to solid being 5-10:1 at the temperature of 80-100 DEG C for 0.5-3 hours, acid leaching and precipitating and filtering to obtain Al(OH)3, adding ammonium salt to filtrate, filtering to obtain ammonium metavanadate, extracting molybdenum from the filtrate in which the ammonium metavanadate is filtered, recovering the nickel by acid leaching, hydrolyzing the filtrate for removing impurities from the nickel, condensing and drying to produce crystal nickel sulfate. Comprehensive recovery improves environment conditions, and creates good economic benefit; comprehensive use of secondary resources relieves the insufficient domestic resources, and protects the environment; and the recovery method has simple process and low recovery cost and is applicable to large-scale use.
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Description

technical field

[0001] The invention relates to a method for recovering metal oxides from waste aluminum-based vanadium-molybdenum-nickel catalysts. Background technique

[0002] Aluminum-based catalyst refers to a catalyst that uses alumina as a carrier and fixes active components such as noble metals or metals such as nickel, cobalt, vanadium, molybdenum, or their oxides on alumina, also known as a catalyst. In the petrochemical industry, aluminum-based molybdenum catalysts are generally used to desulfurize crude oil. During the desulfurization process, aluminum-molybdenum catalysts will absorb a large amount of impurity elements such as vanadium, nickel, phosphorus and iron from crude oil, resulting Molybdenum catalysts are poisoned and discarded as waste aluminum-based vanadium-molybdenum-nickel catalysts. According to investigations, the number of waste aluminum-based vanadium-molybdenum-nickel catalysts eliminated by the petrochemical sector due to desulfurization oper...

Examples

Embodiment 1

[0037]figure 1 It is a process flow diagram of the present invention.

[0038] 1) The waste aluminum-based vanadium-molybdenum-nickel catalyst after pulverization is fully mixed with a certain amount of sodium hydroxide, and sodium hydroxide and waste aluminum-based vanadium-molybdenum-nickel catalyst (according to Al 2 o 3 The molar ratio of ) is 2.6:1;

[0039] 2) Carry out high-temperature roasting with the mixed material in the rotary kiln, the temperature is 700 ℃, constant temperature 6 hours, the conversion rate of vanadium, molybdenum is respectively 96.3%, 97.1%, the conversion rate of aluminum is 97.5%; The main reflection equation is as follows:

[0040] Al 2 o 3 +2NaOH=2NaAlO 2 +H 2 o

[0041] V 2 o 5 +6NaOH=2Na 3 VO 4 +3H 2 o

[0042] MoO3+2NaOH=Na 2 MoO 4 +H 2 O.

[0043] 3) After the sintered block is pulverized, it is washed with hot water at 80°C in countercurrent, the liquid-solid weight ratio is 5:1, and the time is 3 hours; sodium aluminate,...

Embodiment 2

[0057] 1) The waste aluminum-based vanadium-molybdenum-nickel catalyst is fully mixed with sodium hydroxide, and the waste aluminum-based vanadium-molybdenum-nickel catalyst is mixed with sodium hydroxide (according to Al 2 o 3 ) The molar ratio is 3.4:1.

[0058] 2) The mixed materials are roasted at high temperature in a rotary kiln at a temperature of 1000° C. and kept at a constant temperature for 4.5 hours. The conversion rates of vanadium and molybdenum are 96.8% and 97.3% respectively, and the conversion rates of aluminum are 98.5%;

[0059] 3) After the sintered block is pulverized, it is washed with hot water countercurrently. The water consumption is 7.5:1 by weight ratio of liquid to solid. The temperature is 90°C for 2.5 hours.

[0060] 4) Separation by filtration and precipitation to obtain Al(OH) 3 Same as Example 1, the purity reaches more than 99.2%.

[0061] 5) Filter Al(OH) 3 The precipitated filtrate is adjusted to a pH value of 6.9, and an ammonium salt...

Embodiment 3

[0065] 1) The waste aluminum-based vanadium-molybdenum-nickel catalyst is fully mixed with sodium hydroxide, and the waste aluminum-based vanadium-molybdenum-nickel catalyst is mixed with sodium hydroxide (according to Al 2 o 3 ) The molar ratio is 4:1.

[0066] 2) The mixed waste aluminum-based vanadium-molybdenum-nickel catalyst and sodium hydroxide are roasted at a high temperature at a temperature of 1200° C. and a constant temperature of 3 hours. The conversion rates of vanadium and molybdenum are 97.6% and 98.7% respectively, and the conversion rate of aluminum is 99.5%. %.

[0067] 3) After the sintered block is pulverized, it is washed with hot water countercurrently. The amount of water is 10:1, the temperature is 100°C, and the time is 0.5 hours.

[0068] 4) Filtrate and separate the water immersion solution, and precipitate to obtain Al(OH) 3 Embodiment 1 is the same.

[0069] 5) Filter Al(OH) 3 The filtrate after precipitation is adjusted to a pH value of 7.5,...