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Preparation method of vulcanization type catalyst

A catalyst and sulfurized type technology, applied in the field of preparation of sulfurized hydrogenation catalysts, can solve problems such as affecting the air tightness of the device, and achieve the effects of increasing sulfurization degree, avoiding overheating and simple production process

Active Publication Date: 2014-09-17
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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.

Method used

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  • Preparation method of vulcanization type catalyst

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preparation example Construction

[0022] 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. The catalyst carrier preparation method is well known to those skilled in the art.

[0023] 2. Preparation of sulfurized catalyst

[0024] a) Prepare solutions containing Mo or W sulfide precursors and solutions containing Ni or Co inorganic salts respectively, and impregnate the carrier in two steps. After the first step impregnates the catalyst carrier with a solution containing Mo or W sulfide precursors, Dry at 20°C to 200°C for 1 to 10 hours. In the second step, impregnate the dried catalyst carrier with an impregnating solution containing Ni...

Embodiment 1

[0027] Embodiment 1 Preparation of sulfurized catalyst A

[0028]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.

[0029] Take a solution containing ammonium thiomolybdate and nickel nitrate (containing molybdenum oxide 30g / 100ml, nickel oxide 24g / 100ml) impregnated carrier 1 and then dried at 180°C for 3 hours, took straight-run diesel oil and sprayed the obtained catalyst precursor, at 200 ℃ for 3 hours, so that the final catalyst contains 5wt% of straight-run diesel oil to obtain catalyst A, whose hydrogen sulfide curve is shown in figure 1 .

Embodiment 2

[0030] Embodiment 2 Preparation of sulfurized catalyst B

[0031] Take ammonium thiomolybdate solution (containing molybdenum oxide 30 g / 100ml) to impregnate carrier 1 and dry at 180°C, take nickel nitrate solution (containing nickel oxide 10g / 100ml) to spray the obtained catalyst precursor, and dry at 180°C For 3 hours, get the dried sample obtained before spraying and immersing the ethanol solution containing hexadecane (wherein containing 50wt% hexadecane), and treat it for 3 hours at 180°C, so that the final catalyst contains 5wt% hexadecane, to obtain catalyst B. Its hydrogen sulfide curve is shown in figure 1 .

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Abstract

The invention discloses a preparation method of a vulcanization type catalyst. The method comprises: impregnating a needed catalyst carrier by an impregnating solution, then conducting drying so as to obtain a vulcanization type catalyst, with the impregnating solution being a solution containing a metal sulfide precursor, and then carrying out aftertreatment on the catalyst by a proper organic assistant, thus obtaining the final vulcanization type catalyst. The method provided in the invention can control vulcanization of the catalyst under an appropriate temperature in a startup activation process so as to avoid untimely vulcanization of an active metal, release of a hydrogen sulfide gas and the consequent influence on equipment air tightness. The catalyst prepared by the method provided in the invention is suitable for preparation of a petroleum fraction hydrogenation catalyst.

Description

technical field [0001] The invention relates to a preparation method of a sulfurized catalyst, in particular to a preparation method of a sulfurized hydrogenation catalyst. 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 partially presulfurized by heating treatment in the...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/34
Inventor 徐黎明高玉兰
Owner CHINA PETROLEUM & CHEM CORP
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