SU1657227A1 - Method of producing petroleum product hydrofining catalyst - Google Patents

Abstract

The invention relates to catalytic chemistry, in particular the preparation of a catalyst for hydrotreating petroleum that can be used in petrochemistry. The goal is to increase the hydrogenating and hydrodesulfurizing activity of the catalyst. It is prepared by precipitating aluminum hydroxide, first peptizing with nitric acid, and then with an aqueous solution of ammonium metavanadate. After evaporation of the solution, the molybdenum compound is introduced, extruded (molded), dried, calcined and impregnated with a nickel or cobalt nitrate solution, followed by drying and calcining. The resulting catalyst provides a degree of desulfurization at 390 and 410 ° C to 88 and 90.5%, respectively, as well as a degree of hydrogenation of aromatic hydrocarbons at 390 ° C, 57.1% against 86.4 and 93% without hydrogenation of aromatic hydrocarbons, contained in diesel fuel (fractions 214-350 ° C). 1 tab. J

Description

The invention relates to a method for producing catalysts for refining and petrochemicals, and can be used in the manufacture of catalysts for hydrotreating petroleum.

The aim of the invention is to obtain a catalyst with increased hydrogenating and hydrodesulfurizing activity by using nitric acid for peptization as an inorganic acid and the introduction of a molybdenum compound at a certain stage after evaporation.

Example 1.500 g of aluminum hydroxide of continuous precipitation with a moisture content of 80% by weight, with continuous stirring, 4.5 ml of concentrated nitric acid with a density of 1.34 g / cm and then 6 ml of an aqueous solution of ammonium metavanadate containing 0.575 g of ammonium metavanadate. The peltized mass is evaporated in a water bath for 30 min with stirring, and a solution containing 14.80 g of ammonium paramolybdate in 75 ml of distilled water is poured.

ABOUT

ate |

H)

Che

stirring, evaporated in a water bath to a moisture content of 70% and molded by extrusion in the form of cylindrical particles with a diameter of 2 mm and a length of 4 mm. The formed particles are dried in air for 12 hours, dried for 2 hours at 100 ° C and 2 hours at 120 ° C, g Groking at 550 ° C for 2 hours. 100 g of calcined alumina containing 0.5 wt.% VfcOs and 10 wt.% Mooz. placed in 145 ml of an aqueous solution which contains 27.00 g of nickel nitrate. The impregnation of the carrier is carried out at 60-70 ° C for 1 hour. The excess impregnating solution is separated by decantation. The catalyst is dried for 2 hours at 80 ° C, 2 hours at 100 ° C, 2 hours at 120 ° C, 2 hours at 140 ° C, 6 hours at 160 ° C and 2 hours at 180 ° C. then calcined at 550 ° C for 2 hours.

The composition of the catalyst, wt.%: Mooz Yu; N10 3; V205 0.5; A12Oz 86.5.

Example 2. 500 g of aluminum hydroxide with continuous precipitation with a moisture content of 80% by weight are peptized with continuous stirring with 4.5 ml of concentrated nitric acid with a density of 1.34 g / cm3, and then 48 ml of an aqueous solution of ammonium metavanadate containing 4.76 g of metavanadate ammonium. The peptized mass is evaporated in a water bath for 30 minutes with stirring, and a solution containing 18.97 g of ammonium paramolybdate in 96 ml of distilled water is poured. The mass with stirring is evaporated in a water bath to a moisture content of 70% and molded by extrusion in the form of cylindrical particles with a diameter of 2 mm and a length of 4 ml. Molded particles are subjected to heat treatment as in example 1.

100 g of calcined alumina containing 3.0 wt.% V20s and 12 wt.% MoO3 are placed in a 145 ml aqueous solution that contains 38.45 g of nickel nitrate. The impregnation, drying and calcination of the catalyst are carried out analogously to example 1. The composition of the catalyst. Wt.%: MoOz 12; NI04; V20s3; A120381

Example 500 g of aluminum hydroxide continuous precipitation with a moisture content of 80% by weight is peptized with continuous stirring with 4.5 ml of concentrated nitric acid with a density of 1.34 g / cm3, and then 90 ml of an aqueous solution of ammonium metavanadate containing 8.81 g of ammonium metavanadate. The peptized mass is evaporated in a water bath for 30 minutes with stirring, and a solution containing 26.96 g of ammonium paramolybdate in 126 ml of distilled water is poured. The mass with stirring is evaporated in a water bath to a moisture content of 70 wt.% And molded by extrusion in the form of cylindrical particles.

with a diameter of 2 mm and a length of 4 mm. The formed particles are subjected to heat treatment as in Example 1.

100 g of calcined alumina containing 5.0 wt.% V20s and 16 wt.% MoO3 are placed in 145 ml of an aqueous solution which contains 63.98 g of nickel nitrate. Impregnation, drying and calcination of the catalyst are carried out analogously to example 1.

Catalyst composition, wt.%: MoOZ 16, N10 6; V20s 5; A120Z 73.

EXAMPLE 4,100 g of calcined alumina, prepared as in Example 1 and containing 0.5% by weight V20s m 100% by weight MoO3, are placed in 145 ml of an aqueous solution which contains 27.00 g of cobalt nitrate, Impregnation, drying and calcination of the catalyst are carried out analogously to example 1.

The composition of the catalyst, wt.%: MoOz 10; Soo 3; V20s 0.5; A1203 86.5.

PRI me R 5. 100 g of calcined alumina, prepared analogously to example 2 and containing 3.0 wt.% V20s and 12 mas,% MoO3, are placed in 145 ml of an aqueous solution, which contains 38.45 g of cobalt nitrate. Impregnation, drying and calcination of the catalyst are carried out analogously to example 1.

The composition of the catalyst, wt.%: MoOz 12; CoO 4; V2053; A120381

Example 6. 100 g of calcined alumina, prepared analogously to example 3 and containing 5.0 wt.% V20s and 16 May. % Mooz, placed in 145 ml of an aqueous solution containing 63.98 g of cobalt nitrate. Impregnation, drying and calcination of the catalyst are carried out analogously to example 1.

The composition of the catalyst, wt.%: MoOz 16; So: V2055: A 20z73.

A comparative characteristic of the hydrodesulfurizing and hydrogenating activity of a known industrial catalyst, GB - 168S and catalysts synthesized according to examples 1-6, is presented in the table. Testing of catalysts is carried out on a laboratory flow unit for hydrotreatment of diesel fuel of fraction 214–350 ° C, with a sulfur content of 2.29 wt.%. The pressure is 3.5 MPa, the ratio of hydrogen to raw materials is 400: 1. volumetric feed rate of 2.5 h 1.

Thus, the proposed method allows to obtain a catalyst, about which the enhanced hydrogenating and hydro-desulfurizing activity is enhanced.

Claims (1)

The invention The method of preparation of the catalyst for the hydrotreatment of petroleum drain. involving the precipitation of aluminum hydroxide, peltiation first with an inorganic acid, and then with an aqueous solution of ammonium metavanadate, evaporation, introduction of a molybdenum compound, extrusion molding, drying, calcining, impregnation of the resulting carrier with a solution of nitrate and calcination, which is different. In order to obtain a catalyst with hydrogenating and hydrodesulfurizing activity, inorganic acid is used as inorganic acid and the introduction of the compound nickel or cobalt, followed by drying of the deden is carried out after evaporation. and calcination, characterized in that. In order to obtain a catalyst with enhanced hydrogenating and hydrodesulfurizing activity, nitric acid is used as an inorganic acid and the introduction of the compound molyb Data obtained in the process of hydrotreatment of light gas oil. ten