A catalyst for hydrotreating of crude oil and the method of its preparation

 

(57) Abstract:

The invention relates to catalytic chemistry, in particular to the preparation of catalysts for Hydrotreating of crude oil, and can be used in the refining industry. Describes a catalyst for hydrotreatment of crude oil containing oxides of molybdenum, Nickel and aluminum, characterized in that the internal surface of the catalyst to the external is (5-8)104in the following ratio, wt.%: molybdenum oxide 11-14; Nickel oxide 3-5; alumina rest to 100. Also describes the method of preparation of the above catalyst. Technical result - producing high-strength and high-activity catalyst hydrodesulphurization unit oil fractions. 2 S. p. f-crystals, 1 table.

The invention relates to catalytic chemistry, in particular to the preparation of catalysts for Hydrotreating of crude oil, and can be used in the oil industry.

The aim of the invention is to increase the mechanical strength and gidroobesserivaniya activity of Hydrotreating catalysts.

The prior art consists in the following. A method of obtaining luminosity mass of aluminum hydroxide, coming to the moulding (Petrochemistry and oil refining, 1981, No. 8, S. 26-29).

The disadvantage of these catalysts is their insufficient mechanical strength and low gidroobesserivaniya activity.

Closest to the invention to the technical essence and the achieved effect is the way [US 4880526 A, 14.11.89], whereby to prepare the catalyst for Hydrotreating carried out the deposition of an aluminum salt, aging the precipitate at 20-30oC and pH 8-12 for 15 minutes or more, washing the precipitate, mixing it with a salt of Nickel and molybdenum (or tungsten) at 25-100oC and pH 4-10 obtaining a mixture containing 1-6% Nickel and 8-40% of another metal, extruding the mixture, drying and calcination.

However, the disadvantages of this catalyst is its low mechanical crushing strength and gidroobesserivaniya activity.

The invention consists in the following. The invention is directed to solving the problem of obtaining high-strength and high-activity catalyst hydrodesulphurization unit oil fractions.

The technical result allows us to solve the problem. This technical result is achieved by obtaining the catalyst, to the in: molybdenum oxide - 11-14%, Nickel oxide 3-5 wt. % and the alumina - rest, a method of preparation of the catalyst, including the precipitation of aluminium hydroxide sulphate method, the introduction of aluminum hydroxide first, salts of molybdenum, and then Nickel at a certain temperature and continuous stirring, the processing of the received mass with a certain humidity monobasic mineral acid until the pH of the medium 4-6, forming, the crop has wilted, drying and calcination.

The essential features of the invention are a definite correlation between the internal and external surfaces of the catalyst, the ratio of its components, and how to obtain it.

Distinctive features of this invention are against the inner surface of the catalyst to the outside within (5-8) 104when the ratio of catalyst components, wt.%: molybdenum oxide - 11-14, Nickel oxide 3-5 and alumina - rest, and a method thereof, comprising the sequential introduction of active components - first, the salts of molybdenum and then Nickel salts in pre-heated to 50-80oC aluminum hydroxide with continuous mixing of the latter with intermediate heating molybdenum Gidrostroy or hcl to pH environment within 4-6.

The novelty of the present invention is to obtain alumnirelations catalyst with respect to the inner surface to the outer limits (5-8) 104and the method thereof, comprising the sequential introduction of salt molybdenum - paramolybdate ammonium and Nickel salts in the aluminum hydroxide at a temperature of last 50-80oC with intermediate stirring and heating molybdenum-containing aluminum hydroxide for 30 min and processing mass with humidity 68-70 wt.% monobasic mineral acid to pH environment within 4-6. The proposed solution allows to obtain high strength and highly active catalyst for Hydrotreating of crude oil that can significantly increase the reaction cycle of operation of the installation.

The invention is illustrated by the following examples.

Example 1. Take 500 grams of pellets of aluminum hydroxide, sulfate obtained by the method, with a humidity of 80 wt.%, placed in a porcelain Cup and stirred at 50oC to obtain a homogeneous mass. Further, under continuous stirring and heating in a lot make salt paramolybdate ammonium [(NH4)6Mo7O244H2O] mass of 13.8 g, stirred for 30 milczenia masses with moisture content of 68 wt.% and gradually add in the weight of concentrated nitric acid until the pH of the medium 4, continue to stir and maintain the temperature of the mass 50oC for 30 minutes the Mass is formed into extrudates, extrudates provalivajut, dried and calcined.

The catalyst has the following chemical composition, wt.%:

Molybdenum oxide (MoO3) - 11,0

Nickel oxide (NiO) - 3,0

Aluminum oxide (Al2O3) - 86,0

The ratio of internal and external surfaces of the catalyst is equal to 8 to 104.

The index of the strength of the catalyst - 4.2 kg/mm

Example 2. The catalyst prepared according to example 1, but keep the temperature of the mass in a porcelain Cup is 65oC handle mass with humidity of 69 wt.% nitric acid until the pH of the medium 5.

The catalyst has the following chemical composition, wt.%:

Molybdenum oxide is 12.5

Nickel oxide - 4,0

Alumina - 83,5

The ratio of internal and external surfaces is 7 to 104.

The index of the strength of the catalyst was 3.9 kg/mm

Example 3. Prepare the catalyst of example 1, but keep the temperature of the mass is equal to 80oC, humidity 70% wt. and the pH of the medium 6.

The catalyst has the following chemical composition, wt.%:

Molybdenum oxide - 14,0

Nickel oxide - 5,0

Alumina - 81,0

Example 4. Prepare the catalyst of example 1, but instead of nitric acid using hydrochloric acid.

The catalyst has the following chemical composition, wt.%:

Molybdenum oxide - 11,0

Nickel oxide - 3,0

Alumina - 86,0

The ratio of internal and external surfaces of the catalyst - 7,8 104.

The index of the strength of the catalyst - 4,0 kg/mm

The catalysts obtained in examples 1-4, and the catalyst in comparison with the prototype were tested in the Hydrotreating (laboratory setting) fractions of straight-run diesel fuel in a mixture with light gas oil catalytic cracking and delayed coking. The total sulfur content in the raw materials - 0.85 wt.%. The temperature in the Hydrotreating - 345oC, the volumetric feed rate of 2.5 h-1the pressure of 3.5 MPa and the ratio of hydrogen supply - 400 nl/l of raw materials.

The results of the tests of the catalysts shown in the table.

From the table it follows that the proposed catalyst for Hydrotreating petroleum fractions characterized by higher mechanical crushing strength and obestsenivaya activity in Hydrotreating fractions of diesel fuel.

 

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