Method for preparing Y-type molecular sieve from FCC waste catalyst by microwave heating

Abstract

The invention relates to a method for preparing a Y-type molecular sieve from an FCC waste catalyst by microwave heating, and belongs to the technical field of secondary resource comprehensive recovery and utilization. The method comprises the following steps: first, removing toxic metals, namely, vanadium, nickel and iron, from the FCC waste catalyst by soaking for 10 to 60 minutes at 50 to 120 DEG C by a chemical method, wherein a molecular sieve framework structure must be remained simultaneously; taking metal-removed reactivated FCC waste catalyst as an aluminium source, performing seed crystal growth for 10 to 60 minutes at the microwave power of 400 to 1,600 W at 80 to 140 DEG C in the situation of externally adding a silicon source, a sodium source, water and a guiding agent, cooling to 60 to 120 DEG C, crystallizing for 0.5 to 3 hours at the microwave power of 400 to 1,600 W, and drying to obtain the Y-type molecular sieve. According to the method, the problem of massive discharging of the FCC waste catalyst can be solved, high-efficiency and quick utilization of the FCC waste catalyst can also be realized, and the problem about the aluminium source required in a preparation process is also solved.

Description

technical field

[0001] The invention relates to a method for preparing Y-type molecular sieves from FCC waste catalysts by microwave heating, and belongs to the technical field of comprehensive recovery and utilization of secondary resources. Background technique

[0002] FCC catalyst is the most widely used catalyst in the petroleum refining process, which has the characteristics of high catalytic activity, good selectivity, stability and strong anti-toxicity. With the increasingly heavy and inferior crude oil and the continuous recycling of FCC catalysts, the metals deposited on the FCC catalysts will gradually increase, resulting in a decrease in activity and heavy oil conversion capacity, and the formation of spent catalysts. At present, the global FCC waste catalyst emissions are 150,000 to 170,000 tons per year, and it is estimated that the annual increase of FCC waste catalysts is about 5%.

[0003] The main component of spent FCC catalysts is molecular sieve, which ...

Examples

Embodiment 1

[0025] This microwave heating prepares the method for Y-type molecular sieve from FCC waste catalyst, and its concrete steps are as follows:

[0026] Step 1. First, mix the spent FCC catalyst with the leaching mother liquor (5wt% HCl solution) at a liquid-solid ratio of 6:1mL / g, and then leaching for 30 minutes at a temperature of 80°C to obtain vanadium, nickel, and iron poisoning metals. The leaching solution (the leaching rates of Fe, V, and Ni are 44%, 46%, and 33%, respectively, and the Al loss rate is 10%) and the spent FCC catalyst with basically complete molecular sieve structure after demetallization and revival; the molecular sieve structure after demetallization and revival The basically complete SEM image of FCC spent catalyst is shown in Fig. figure 1 shown;

[0027] Step 2. Use the spent FCC catalyst with basically complete molecular sieve structure obtained in step 1 as the aluminum source, and add 6.5 kilograms of silicon source (silica sol) and 2.1 kilograms ...

Embodiment 2

[0030] This microwave heating prepares the method for Y-type molecular sieve from FCC waste catalyst, and its concrete steps are as follows:

[0031]Step 1. First, mix the spent FCC catalyst with the leaching mother liquor (3wt% HCl solution) at a liquid-solid ratio of 10:1mL / g, and then leaching for 30 minutes at a temperature of 80°C to obtain vanadium, nickel, and iron poisoning metals. Leaching solution (the leaching rates of Fe, V, and Ni are 42%, 40%, and 28%, respectively, and the loss rate of Al is 12%) and the spent FCC catalyst with basically complete molecular sieve structure after demetallization and resurrection;

[0032] Step 2. Use the spent FCC catalyst with basically complete molecular sieve structure obtained in step 1 as the aluminum source, and add 6.8 kilograms of silicon source (silica sol) and 2.0 kilograms of sodium source (sodium source is sodium hydroxide), 12.0 kg of water and 2.8 kg of directing agent (the molecular formula of the directing agent is...

Embodiment 3

[0035] This microwave heating prepares the method for Y-type molecular sieve from FCC waste catalyst, and its concrete steps are as follows:

[0036] Step 1. First, mix the spent FCC catalyst with the leaching mother liquor (concentration: 1wt% oxalic acid solution) at a liquid-solid ratio of 15:1mL / g, and then leaching for 50 minutes at a temperature of 50°C to obtain vanadium, nickel, and iron poisoning metals. The leaching solution (the leaching rates of Fe, V, and Ni are 63%, 58%, and 32%, respectively, and the loss rate of Al is 3%) and the spent FCC catalyst with basically complete molecular sieve structure after demetallization and resurrection;

[0037] Step 2. Use the spent FCC catalyst with basically complete molecular sieve structure obtained in step 1 as the aluminum source, and add 6.7 kilograms of silicon source (silica sol) and 1.9 kilograms of sodium source (sodium source is sodium hydroxide), 11.9 kg of water and 3.0 kg of directing agent (the molecular formul...

technical field

[0001] The invention relates to a method for preparing Y-type molecular sieves from FCC waste catalysts by microwave heating, and belongs to the technical field of comprehensive recovery and utilization of secondary resources. Background technique

[0002] FCC catalyst is the most widely used catalyst in the petroleum refining process, which has the characteristics of high catalytic activity, good selectivity, stability and strong anti-toxicity. With the increasingly heavy and inferior crude oil and the continuous recycling of FCC catalysts, the metals deposited on the FCC catalysts will gradually increase, resulting in a decrease in activity and heavy oil conversion capacity, and the formation of spent catalysts. At present, the global FCC waste catalyst emissions are 150,000 to 170,000 tons per year, and it is estimated that the annual increase of FCC waste catalysts is about 5%.

[0003] The main component of spent FCC catalysts is molecular sieve, which ...

Examples

Embodiment 1

[0025] This microwave heating prepares the method for Y-type molecular sieve from FCC waste catalyst, and its concrete steps are as follows:

[0026] Step 1. First, mix the spent FCC catalyst with the leaching mother liquor (5wt% HCl solution) at a liquid-solid ratio of 6:1mL / g, and then leaching for 30 minutes at a temperature of 80°C to obtain vanadium, nickel, and iron poisoning metals. The leaching solution (the leaching rates of Fe, V, and Ni are 44%, 46%, and 33%, respectively, and the Al loss rate is 10%) and the spent FCC catalyst with basically complete molecular sieve structure after demetallization and revival; the molecular sieve structure after demetallization and revival The basically complete SEM image of FCC spent catalyst is shown in Fig. figure 1 shown;

[0027] Step 2. Use the spent FCC catalyst with basically complete molecular sieve structure obtained in step 1 as the aluminum source, and add 6.5 kilograms of silicon source (silica sol) and 2.1 kilograms ...

Embodiment 2

[0030] This microwave heating prepares the method for Y-type molecular sieve from FCC waste catalyst, and its concrete steps are as follows:

[0031]Step 1. First, mix the spent FCC catalyst with the leaching mother liquor (3wt% HCl solution) at a liquid-solid ratio of 10:1mL / g, and then leaching for 30 minutes at a temperature of 80°C to obtain vanadium, nickel, and iron poisoning metals. Leaching solution (the leaching rates of Fe, V, and Ni are 42%, 40%, and 28%, respectively, and the loss rate of Al is 12%) and the spent FCC catalyst with basically complete molecular sieve structure after demetallization and resurrection;

[0032] Step 2. Use the spent FCC catalyst with basically complete molecular sieve structure obtained in step 1 as the aluminum source, and add 6.8 kilograms of silicon source (silica sol) and 2.0 kilograms of sodium source (sodium source is sodium hydroxide), 12.0 kg of water and 2.8 kg of directing agent (the molecular formula of the directing agent is...

Embodiment 3

[0035] This microwave heating prepares the method for Y-type molecular sieve from FCC waste catalyst, and its concrete steps are as follows:

[0036] Step 1. First, mix the spent FCC catalyst with the leaching mother liquor (concentration: 1wt% oxalic acid solution) at a liquid-solid ratio of 15:1mL / g, and then leaching for 50 minutes at a temperature of 50°C to obtain vanadium, nickel, and iron poisoning metals. The leaching solution (the leaching rates of Fe, V, and Ni are 63%, 58%, and 32%, respectively, and the loss rate of Al is 3%) and the spent FCC catalyst with basically complete molecular sieve structure after demetallization and resurrection;

[0037] Step 2. Use the spent FCC catalyst with basically complete molecular sieve structure obtained in step 1 as the aluminum source, and add 6.7 kilograms of silicon source (silica sol) and 1.9 kilograms of sodium source (sodium source is sodium hydroxide), 11.9 kg of water and 3.0 kg of directing agent (the molecular formul...

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