Preparation method of metal phosphide type hydrocracking catalyst

A metal phosphide, hydrocracking technology, applied in physical/chemical process catalysts, molecular sieve catalysts, chemical instruments and methods, etc., can solve the problems of unstable properties of heteropolyacids and insufficient catalyst stability.

Active Publication Date: 2014-08-20
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the properties of heteropolyacids are unstable, and they will gradually decompose and transform under high temperature conditions, and the stability of the catalyst is insufficient.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Using the impregnating solution of Comparative Example 1, add red phosphorus at a ratio of W to P molar ratio of 1:1 and Ni to P molar ratio of 2:1, and use an ultrasonic wave with a frequency of 18KHz and a power of 100W / L to disperse for 1 hour. Carrier T-1 was impregnated at room temperature for 2 hours. While impregnated, it was dispersed by ultrasonic waves with a frequency of 18KHz and a power of 100W / L, then dried at 120°C for 4 hours, and then reduced and activated in a hydrogen atmosphere. The reduction activation procedure is to raise from room temperature to 450°C at 5°C / min, from 450°C to 700°C at a heating rate of 2°C / min, and keep the temperature at 700°C for 2 hours to prepare the catalyst C-1 of the present invention .

[0038] Through XRD analysis (under nitrogen protection condition), it can be seen that there are tungsten phosphide (WP) and nickel phosphide (Ni phosphide) in the catalyst of the present invention. 2 The characteristic diffraction peak...

Embodiment 2

[0043] Using the impregnating solution of Comparative Example 1, add red phosphorus at the ratio of W to P molar ratio of 1:1.5 and Ni to P molar ratio of 1:1, and use ultrasonic wave with frequency of 25KHz and power of 150W / L to disperse for 5 hours. Carrier T-2 was impregnated at room temperature for 4 hours. While impregnating, it was dispersed by ultrasonic waves with a frequency of 25KHz and a power of 150W / L. Dry at ℃ for 6 hours, and then perform hydrogen activation under a hydrogen atmosphere. Firstly, increase from room temperature to 350℃ at a rate of 10℃ / min, then increase from 350℃ to 600℃ at a rate of 1℃ / min, and keep the temperature at 600℃ After 4 hours, the phosphating transition metal catalyst C-2 was prepared.

Embodiment 3

[0048] With the impregnating solution of Comparative Example 1, red phosphorus was added at the ratio of W to P molar ratio of 1:2 and Ni to P molar ratio of 1:1, and ultrasonic dispersion with a frequency of 35KHz and a power of 10W / L was used for 7 hours. Carrier T-3 was impregnated at room temperature for 4 hours, while impregnating with ultrasonic dispersion with a frequency of 35KHz and a power of 10W / L, dried at 110°C for 6 hours, and then activated in a hydrogen atmosphere. Raise from room temperature to 450°C at 8°C / min, from 450°C to 650°C at a rate of 1°C / min, and keep the temperature at 650°C for 4 hours to prepare transition metal phosphide catalyst C-3.

[0049] Table 1 Physicochemical properties of catalyst supports.

[0050] Numbering T-1 T-2 T-3 Molecular sieve, wt% 12.0 7.0 4.0 Amorphous silica-alumina, wt% 25.0 53.0 30.0 Macroporous alumina, wt% 43.0 20.0 46.0 Binder, wt% 20.0 20.0 20.0 Pore ​​volume, ml / g 0...

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Abstract

The invention describes a method for preparing a metal phosphide type hydrocracking catalyst. The method of the present invention includes the following processes: (1) preparing a catalyst carrier containing molecular sieves and inorganic refractory oxides; (2) preparing an impregnating solution containing a metal compound of Group VIB and a metal compound of Group VIII; (3) preparing in step (2) Add elemental phosphorus to the impregnating solution, perform ultrasonic dispersion, then impregnate the catalyst carrier in step (1), and then dry; (4) The material obtained in step (3) is activated with hydrogen, and after activation, hydrogenation for hydrocracking reaction is obtained. cracking catalyst. The hydrocracking catalyst prepared by the method of the invention has more outstanding performance and is especially suitable for the hydrocracking process of prolific middle distillate oil.

Description

technical field [0001] The invention relates to a method for preparing a hydrocracking catalyst. The catalyst has excellent hydrocracking performance, high activity and high selectivity for medium oil. Background technique [0002] The hydrocracking catalyst is a dual-functional catalyst with hydrogenation and cracking properties. Non-precious metal hydrocracking catalysts generally use Group VIB and Group VIII metals as hydrogenation components, and the cracking performance is mainly provided by acidic components. Crystalline zeolite and / or amorphous silica-alumina can be used. Simple use of amorphous silica-alumina, although the selectivity is high, but the activity is low, and the flexibility of operation is limited. In most hydrocracking catalysts, crystalline zeolite is used as the acidic component, or crystalline zeolite and amorphous Silica and aluminum are common acidic components. [0003] Most of the medium-oil hydrocracking catalysts currently used in industrial...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/26B01J29/78C10G47/20
Inventor 谷明镝黄薇
Owner CHINA PETROLEUM & CHEM CORP
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