Preparation method of vulcanization type catalyst

A catalyst and vulcanization technology, which is applied in the direction of physical/chemical process catalysts, chemical instruments and methods, chemical/physical processes, etc., can solve the problems affecting the airtightness of the device and corrosion of the device, so as to improve the degree of sulfidation, simple production process, Effects that are easy to store

Active Publication Date: 2013-05-15
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the catalyst prepared by this method, the active metal does not exist in a sulfide state, and there is no problem of self-heating. However, during the start-up process of the catalyst, the active metal sulfides prematurely, releasing hydrogen sulfide gas, which affects the airtightness of the device.
In addition, the catalyst still retains some water after low-temperature drying. During the activation process of the catalyst, too much water vapor in the circulating hydrogen will corrode the device.

Method used

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  • Preparation method of vulcanization type catalyst

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preparation example Construction

[0023] 1. Preparation of catalyst carrier: Prepare the catalyst carrier by conventional methods, and select the carrier type according to the number of acid sites required by the catalyst, such as silica-alumina, silica with additives, alumina or molecular sieve with additives, etc. The carrier powder is mixed with binder, pore-enlarging agent and extrusion aid, extruded on an extruder, dried and calcined to make a catalyst carrier. Catalyst carrier preparation method is content well known to those skilled in the art;

[0024] 2. Preparation of sulfurized catalyst

[0025] a) Step-by-step impregnation method: Prepare solutions containing Mo or W sulfide precursors and solutions containing Ni or Co inorganic salts respectively, and impregnate the carrier in two steps. The first step is impregnated with a solution containing Mo or W sulfide precursors After the catalyst is supported, it is dried at 20°C to 200°C for 1 to 10 hours, and the second step is to impregnate the dried ...

Embodiment 1

[0028] Embodiment 1 Preparation of sulfurized catalyst A

[0029] Weigh pseudo-boehmite (produced by Shandong Alumina Plant, 73% by weight on a dry basis) 900g, 19g of scallop powder, 32g of citric acid, 48ml of nitric acid (30% by weight), silica gel (containing two by weight) Silica 30%) 159ml, deionized water 250ml, mixed evenly, extruded on extruder into 1.2mm clover strips, dried and calcined at 600°C for 3 hours to obtain the required catalyst carrier 1.

[0030] Take a solution containing ammonium thiomolybdate and nickel nitrate (containing 30g / 100ml of molybdenum oxide and 24g / 100ml of nickel oxide) to impregnate carrier 1 and treat it at 210°C for 3 hours under a vacuum of -0.08MPa to obtain catalyst A. Hydrogen curve see figure 1 .

[0031]

Embodiment 2

[0032] Embodiment 2 Preparation of sulfurized catalyst B

[0033] Take the ammonium thiomolybdate solution (containing 30 g / 100ml of molybdenum oxide) to impregnate the carrier 1 and then dry it at 180°C for 3 hours, take the solution containing nickel nitrate (containing 10g / 100ml of nickel oxide) to spray the obtained catalyst precursor, at 180 ℃ for 3 hours, and then treated at 230 ℃ for 1 hour under a vacuum of -0.09MPa to obtain catalyst B. The hydrogen sulfide curve is shown in figure 1 .

[0034]

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Abstract

The invention discloses a preparation method of a vulcanization type catalyst. The method comprises: adopting a dipping solution containing a sulfide precursor of active metal Mo or W and an inorganic salt of Ni or Co to dip a needed catalyst carrier, and then conducting after-treatment under certain vacuum degree and temperature, thus obtaining the vulcanization type catalyst. The method can control vulcanization of the catalyst under an appropriate temperature in a startup activation process, thus avoiding untimely vulcanization of the active metal, release of a hydrogen sulfide gas and the consequent influence on equipment air tightness. Meanwhile, in the after-treatment process, redundant water in catalyst pores are removed to prevent excess water in recycle hydrogen from influencing the catalyst activity during activation and corroding equipment. The catalyst prepared by the method provided in the invention is applicable to preparation of a petroleum fraction hydrogenation catalyst.

Description

technical field [0001] The invention relates to a method for preparing a sulfurized catalyst, in particular to a method for preparing a sulfurized hydrogenation catalyst using a solution containing a metal sulfide precursor. Background technique [0002] Conventional hydrogenation catalysts are in an oxidized state, but the active substances are in a sulfurized state in actual use, so they need to be sulfurized in the reactor before use. This not only increases the production cost, but also the vulcanization process is likely to cause pollution to people and the environment, so researchers at home and abroad are actively seeking solutions. The current research mainly focuses on two aspects: one is presulfurization outside the device, and the other is the direct preparation of sulfurized catalysts. External presulfurization refers to the introduction of vulcanizing agent into the pores of the oxidized catalyst by sublimation, melting or impregnation, and then the catalyst is...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/051B01J27/049C10G45/08
Inventor 徐黎明高玉兰
Owner CHINA PETROLEUM & CHEM CORP
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