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Regeneration method of inactivated catalyst

A technology for deactivating catalysts and catalysts, applied in catalyst regeneration/reactivation, molecular sieve catalysts, chemical instruments and methods, etc., can solve problems such as difficult separation of macromolecular by-products, molecular sieve structure damage, and large amount of solvents. Hydrogen/dehydrogenation reactivity, improvement of dispersion, effect of avoiding aggregation

Active Publication Date: 2016-12-07
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the amount of solvent used in this method is too large, and the macromolecular by-products in the detergent are also difficult to separate.
Moreover, this method first uses an organic solvent to remove part of the easy-to-remove coke to reduce the heat released during charcoal regeneration, but ultimately still requires a high-temperature charcoal burning process, and there are still problems encountered by isomerization dewaxing catalysts during high-temperature regeneration. , especially the aggregation of metal platinum and the destruction of the molecular sieve structure

Method used

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  • Regeneration method of inactivated catalyst
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  • Regeneration method of inactivated catalyst

Examples

Experimental program
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Effect test

Embodiment 1

[0040] Preparation of the catalyst E-1 of the present invention.

[0041] Add 1450 mL of organic solvent (the volume ratio of ethanol to benzene is 2:1) into a 2000 mL flask, and treat the deactivated catalyst FD-1 after 200 mL industrial operation. The catalyst number after 2.0 hours of distillation is Ca-1.

[0042] Take 100g of Ca-1 catalyst, add 11.8g of nickel nitrate (Nickel content 3.0wt%) solution to soak to prepare a nickel-containing sample with an atomic ratio of Ni to Pt of about 3:1, and then program-controlled firing in an air atmosphere For carbon, the specific steps are to heat up to 250°C for 10 hours at a heating rate of 3°C / min, and then continue to heat up to 410°C for 3 hours at a heating rate of 3°C / min to obtain the catalyst Ea-1 of the present invention.

[0043] The catalyst Ea-1 is reduced under a hydrogen atmosphere, and the specific conditions are: the hydrogen pressure is 3.5 MPa, the reduction temperature is 430° C., and the reduction time is 6 h.

[0044...

Embodiment 2

[0047] Preparation of catalyst E-2 of the present invention.

[0048] Add 1450 mL of organic solvent (with the volume ratio of ethanol to benzene 1:1) into a 2000 mL flask to treat 200 mL of the deactivated catalyst FD-1 after industrial operation. The catalyst number after 2 hours of distillation is Ca-2.

[0049] Take 100g of Ca-2 catalyst, add 7.38g of nickel acetate (nickel content 8.0wt%) solution and soak to prepare a sample containing nickel, where the atomic ratio of Ni to Pt is about 5:1, and then proceed in an air atmosphere Program-controlled charcoal burning, the specific steps are to heat up to 240°C for 10h at a heating rate of 3°C / min, and then continue to heat up to 420°C for 3h at a heating rate of 3°C / min. The obtained catalyst number is Eb-1.

[0050] The catalyst Eb-1 is reduced in a hydrogen atmosphere, and the specific conditions are: the hydrogen pressure is 4.5 MPa, the reduction temperature is 480° C., and the reduction time is 5.0 h.

[0051] The catalyst aft...

Embodiment 3

[0054] Preparation of catalyst E-3 of the present invention.

[0055] Add 1450 mL of organic solvent (volume ratio of gasoline to kerosene is 1:1) into a 2000 mL flask, and treat 200 mL of the deactivated catalyst FD-1 after industrial operation. The catalyst number after 2.0 hours of distillation is Cb-1.

[0056] Take 100g of Cb-1 catalyst, add 35.4g of nickel sulfate (Ni content 2.0wt%) solution and soak to prepare a sample containing nickel, where the atomic ratio of Ni to Pt is about 6:1, and then proceed in an air atmosphere Program-controlled charcoal burning involves specific steps of heating up to a constant temperature of 280°C for 8 hours at a heating rate of 3°C / min, and then continuing to increase the temperature to a constant temperature of 350°C for 5 hours at a heating rate of 3°C / min to obtain the catalyst Ec-1 of the present invention.

[0057] The catalyst Ec-1 is reduced under a hydrogen atmosphere, and the specific conditions are: the hydrogen pressure is 2.5 MPa...

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Abstract

The invention discloses a regeneration method of an inactivated catalyst. The catalyst comprises a TON type molecular sieve and a group VIII precious metal component. The regeneration method comprises the following steps: processing the inactivated catalyst by using an organic solvent, loading nickel on the processed catalyst according to an atom ratio of nickel to platinum of 6:1-1:1, carrying out programmed carbon burning at a temperature being not higher than 450 DEG C under the action of an oxygen-containing gas, and reducing the processed catalyst in hydrogen atmosphere; and immersing the reduced catalyst in a chitosan-containing dilute acid solution in vacuum environment or inert atmosphere, drying the immersed catalyst, and roasting the dried catalyst to obtain the catalyst with recovered activity. The method has the advantages of effective removal of carbon deposit at a low temperature, guaranteeing of no destroy to the pore structure of the catalyst, good dispersion of precious metal, and realization of very good recovery of the performances of the regenerated catalyst.

Description

technical field [0001] The present invention relates to a regeneration method of a deactivated catalyst, more specifically, to a regeneration method of a hydroisomerization catalyst containing precious metals and TON molecular sieves, especially a regeneration method of a paraffin hydrocarbon hydroisomerization catalyst , especially suitable for the catalyst regeneration method used in the hydroisomerization dewaxing process of lubricating oil. Background technique [0002] Isomerization dewaxing technology is mainly used in the hydrogenation treatment of diesel oil, wax oil and other special oil products to achieve the purpose of reducing the content of normal paraffins and improving the quality of oil products. This technology is also of great significance for improving the low-temperature fluidity of diesel oil. Generally speaking, the wax content in straight-run diesel oil or secondary processed diesel oil is high, so its freezing point or cold filter point is unqualifi...

Claims

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Application Information

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IPC IPC(8): B01J29/90B01J29/76B01J38/52B01J38/56B01J38/60B01J38/62B01J38/02B01J38/10
Inventor 徐会青刘全杰贾立明王伟
Owner CHINA PETROLEUM & CHEM CORP
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