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A kind of method that prepares high-efficiency anthraquinone hydrogenation catalyst by FCC waste catalyst

A technology for hydrogenation catalysts and spent catalysts, which is applied in the direction of catalyst activation/preparation, molecular sieve catalysts, chemical instruments and methods, etc. It can solve the problems of complex process waste catalysts, low utilization of silicon and aluminum elements, and incomplete removal of heavy metals. Achieve the effects of high recycling rate of anthraquinone, low cost and good texture properties

Inactive Publication Date: 2020-08-11
WUHAN UNIV OF TECH
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Problems solved by technology

Chinese patent document CN101219396A proposes a method for revitalizing and regenerating spent FCC catalysts. This method adopts organic acid and inorganic acid synergistic treatment to remove heavy metals in FCC spent catalysts and greatly improves the reactivity of FCC spent catalysts. However, heavy metals are removed. Defects of incomplete and revived catalysts with low activity
Chinese patent literature CN1704350A proposes a method for preparing polyaluminosilicate by FCC waste catalyst, the method first leaches the FCC waste catalyst with sulfuric acid and then leaches the filter residue with NaOH, and then mixes the two leaching solutions under certain conditions for a period of reaction Polymerized aluminum silicate has been prepared for a long time, but this method has the disadvantages of complex process and low utilization rate of unactivated spent catalyst silicon and aluminum elements
Chinese patent literature CN104261424 proposes a method for preparing 4A zeolite from FCC waste catalyst and kaolin, which adds water and one or more of kaolin, FCC waste catalyst, dispersant, pore-enlarging agent, auxiliary agent, and binder Stir evenly to make slurry and shape. The shaped material is roasted at 700-1000°C for a period of time, and then heated in water at a certain temperature for a period of time to filter and dry to obtain 4A zeolite. This method has the defects of high activation temperature and high energy consumption.
Basaldella et al. (Basaldella EI, Sa′nchez RMT, Conconi MS. Conversion of exhausted fluid cracking catalysts into zeolites by alkaline fusion. Appl. Clay. Sci. 2009, 42:611–614) proposed a method for the preparation of NaA from spent FCC catalysts. The method of zeolite, the method first mixes the spent FCC catalyst with a certain quality of sodium carbonate, and then roasts at 800°C for a certain period of time, then adds a certain amount of sodium metaaluminate solution to the roasted material, and further hydrothermally reacts, filters, and dries to produce To obtain NaA zeolite, this method has the disadvantages of needing to add some chemical reagents, high activation temperature, and large energy consumption

Method used

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  • A kind of method that prepares high-efficiency anthraquinone hydrogenation catalyst by FCC waste catalyst
  • A kind of method that prepares high-efficiency anthraquinone hydrogenation catalyst by FCC waste catalyst
  • A kind of method that prepares high-efficiency anthraquinone hydrogenation catalyst by FCC waste catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Weigh 3g of spent FCC catalyst and place it in a crucible, add 4.25g of solid NaOH and 2.1ml of deionized water, and bake at 400°C for 2h. Fully grind the roasted material through a 200-mesh sieve, add 52.55ml of deionized water to it, first stir and age at 60°C at 180r / min for 1h, after aging, raise the temperature to 90°C, and stir at 180r / min After crystallization for 4 hours, the mixture was filtered, and the filter cake was washed with deionized water until pH≤11, and dried at 105° C. for 2 hours to obtain 4A zeolite. The calcium ion exchange capacity of the resulting 4A zeolite is 305mgCaCO 3 / g-dry basis, the specific surface area is 9.9m2 / g, and the pore volume is 0.032cm 3 / g, the average pore diameter is 10.5nm.

[0038] Take 1.0g of the above 4A zeolite, mix 0.0050g of PdCl 2 The powder is dissolved in hydrochloric acid with a mass concentration of 0.003wt% and pH=3 to obtain H 2 PdCl 4 solution, the amount of hydrochloric acid is required to be equal to...

Embodiment 2

[0040]Weigh 3g of spent FCC catalyst and place it in a crucible, add 3.84g of solid NaOH and 1.8ml of deionized water, and bake at 400°C for 2h. Fully grind the calcined material through a 200-mesh sieve, add 47.54ml of deionized water to it, stir and age at 60°C and 180r / min for 1h, after aging, raise the temperature to 90°C, Stir and crystallize for 4 hours, filter the mixture, wash the filter cake with deionized water until pH≤11, and further dry at 105° C. for 2 hours to obtain zeolite 4A. The calcium ion exchange capacity of the resulting 4A zeolite is 288mg CaCO 3 / g-dry basis, the specific surface area is 10.8m 2 / g, the pore volume is 0.032cm 3 / g, the average pore diameter is 10.3nm.

[0041] The loading process is the same as in Example 1.

[0042] The highest hydrogenation efficiency of the obtained catalyst in the self-made slurry bed is 9.82g / L working solution, and the anthraquinone recycling rate is 100.0%.

Embodiment 3

[0044] Weigh 3g of spent FCC catalyst and place it in a crucible, add 3.84g of solid NaOH and 1.8ml of deionized water, and bake at 400°C for 2h. Fully grind the roasted material through a 200-mesh sieve, add 43.22ml of deionized water to it, stir and age at 60°C and 180r / min for 2 hours, after the aging is over, raise the temperature to 90°C, Stir and crystallize for 3 hours, filter the mixture, wash the filter cake with deionized water until pH≤11, and dry at 105° C. for 2 hours to obtain 4A zeolite. The calcium ion exchange capacity of the resulting 4A zeolite is 285mg CaCO 3 / g-dry basis, the specific surface area is 15.3m 2 / g, the pore volume is 0.041cm 3 / g, the average pore diameter is 9.4nm.

[0045] The loading process is the same as in Example 1.

[0046] The highest hydrogenation efficiency of the obtained catalyst measured in a self-made slurry bed is 9.53g / L working fluid, and the anthraquinone recycling rate is 94.0%.

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Abstract

The invention relates to a method for preparing an efficient anthraquinone hydrogenation catalyst by using an FCC dead catalyst. The preparation method comprises the following steps that the FCC deadcatalyst, NaOH and a small amount of water are mixed uniformly and roasted at a certain temperature for some time; the roasted material is ground fully and screened; a certain amount of deionized water is added into the roasted material, and stirring and ageing are carried out for some time with the temperature rising to a certain temperature; after the ageing, stirring and crystallization are carried out for some time with the temperature rising to a certain temperature; after filter, washing and drying, a filter cake, namely, 4A zeolite is obtained; the 4A zeolite is subjected to equivalent-volume impregnation by using an H2PdC14 solution and excessive impregnation by using an NaOH solution, washed, dried and roasted to obtain the catalyst. According to the preparation method, the FCC dead catalyst is taken as a raw material, and the zeolite with high purity is prepared at the lower activation temperature and has the advantages of catalyst activity, high recycling recovery rate of anthraquinone and the like when taken as the barrier of the anthraquinone hydrogenation catalyst.

Description

technical field [0001] The invention relates to a method for preparing a high-efficiency anthraquinone hydrogenation catalyst from an FCC waste catalyst. Background technique [0002] Fluid Catalytic Cracking (FCC) is an important part of modern petroleum refining process. The FCC process is to crack heavy raw materials under the action of a certain temperature and catalyst, and is the main method of lightening heavy oil. During the use of FCC catalyst, due to the catalyst being polluted by heavy metals, the activity of the catalyst is reduced, resulting in the deterioration of the reaction selectivity of the catalyst. Therefore, it is necessary to periodically unload a part of the catalyst to ensure the activity and selectivity of the catalyst in the device. The unloaded part is called For FCC spent catalyst. In 2015, the output of waste refining catalysts in my country exceeded 200kt, of which the spent catalysts produced by FCC units accounted for the vast majority. FCC...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/70B01J29/74B01J35/10B01J37/02C01B15/023
CPCB01J29/7003B01J29/7407B01J35/1009B01J35/1014B01J35/1038B01J35/1061B01J37/024B01J2229/18B01J2229/38C01B15/023Y02P20/584
Inventor 蔡卫权仇家凯汝绪阳杨志超蔡智君
Owner WUHAN UNIV OF TECH
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