The method of producing catalyst for hydrotreating heavy oil fractions

 

(57) Abstract:

Features a method of producing catalyst for Hydrotreating heavy oil fractions containing MoO3- 16-21 wt.%, NiO (CoO) - 5-7 wt.%, Al2O3- the rest, by impregnation of the carrier - aluminum oxide with a specific pore distribution, solutions of salts of molybdenum and Nickel (cobalt), drying and calcining the extrudates, characterized in that in order to obtain a catalyst with high gidroobesserivaniya activity of the impregnated extrudates are aluminum oxide obtained by molding, drying and calcining a mixture of aluminium hydroxide with fuel oil containing sulfur is not less than 1.0 wt.%, taken in an amount of 3-5% wt. by weight of aluminium hydroxide, characterized by a total pore volume of 0.4-0.6 cm3/g under the condition that the proportion of pores with a radius 10000-150000 is 20-25%, the index of tensile splitting strength of not less than 1.3 kg/mm Example: 100 g of aluminium hydroxide is mixed with 5 g of fuel oil with a sulfur content of 1.0 wt.%, peptidases solution 18% nitric acid, is formed in the form of extrudates with a diameter of 2.0 mm, dried for 5 hours at a temperature of 20oC, 6 hours at a temperature of 100oC, made red-hot at a temperature of 600oC. it Turns out the media with pore volume of 0.6 cm3321% wt. and NiO - 7 % wt. table 1.

The invention relates to the refining and petrochemical industries, in particular to methods of producing the catalyst for Hydrotreating petroleum fractions.

Known methods for producing catalysts for hydrodesulphurization unit oil fractions do not provide an effective catalyst for the implementation of the Hydrotreating process high-sulfur heavy oil fractions, characterized by the elevated temperatures of the boiling and the presence of resin-asphaltene compounds. However, the development of such processes it is necessary, in particular, for Hydrotreating of vacuum gas oil with the aim of obtaining low-sulfur raw material cracking, as well as hydrofining oil distillates.

Today, with the implementation of such processes use catalysts for Hydrotreating of middle distillate fractions, which does not allow to obtain a product with a sufficiently low sulfur content.

Known, for example, a method of obtaining alumonickelsilicate propity catalysts hydrofining petroleum fractions, obtained on the basis of aluminum oxide-modified zeolite components [1] Such catalysts are characterized by low prospectin also a way of getting alumnirelations the catalyst for Hydrotreating hydrocarbons by impregnation of the carrier, pre-treated forceremoval acid [2] This method of getting very difficult technologically, in addition, operation of the catalyst obtained by this method is accompanied by excessive corrosion of the process equipment.

The closest solution to the technical essence and the achieved result is a method of producing catalyst hydrodesulphurization unit by saturating the carrier of Y-A1203, with >75% of pores with a diameter of 30-100 and >60% of pores with a diameter of 20-60 , solutions of compounds of Nickel and molybdenum [3]

But the use of Hydrotreating of heavy oil fractions such catalyst is not possible to obtain a product of desired quality for a long time.

The purpose of the proposed invention is to develop a method of obtaining a highly efficient catalyst for Hydrotreating heavy oil fractions.

This goal is achieved by implementing a method of producing catalyst for Hydrotreating heavy oil fractions containing MoO3- 16-21% wt. NiO (CoO) 5-7% wt. Al2O3the rest, by impregnation of a carrier of aluminum oxide with a specific pore distribution, solutions of salts of molybdenum and Nickel (cobaltates moulding, drying and calcining a mixture of aluminium hydroxide with fuel oil containing sulfur is not less than 1.0 wt.%. taken in an amount of 3-5% wt. by weight of aluminium hydroxide, and characterized by a total pore volume of 0.3-0.6 cm3/g under the condition that the proportion of pores with a radius of 10000-15000 is 20-25% index of tensile splitting strength of not less than 1.3 kg/mm

A distinctive feature of the proposed method of producing catalyst for Hydrotreating petroleum fractions is that during the synthesis of the catalyst is subjected to impregnation, the extrudates of alumina obtained by molding, drying and calcining a mixture of aluminium hydroxide with fuel oil containing sulfur is not less than 1.0 wt.%. taken in an amount of 3-5% wt. by weight of aluminium hydroxide, and characterized by a total pore volume of 0.3-0.6 cm3/g under the condition that the proportion of pores with a radius of 10000-15000 is 20-25% index of tensile splitting strength of not less than 1.3 kg/mm

Introduction to cake aluminium hydroxide at the stage of forming the carrier extrudates of oil in a given amount results in media with optimal pore distribution, total pore volume and strength. During the synthesis of the carrier on the basis of aluminum oxide without the use of fuel oil to achieve optimum performance indicators has failed.

Oblimersen inactive spinel structures; the presence in the catalyst of the transport pores [4] with the pore radius 10000-15000 in a given number increases the access of raw materials to the active centers of the catalyst, which increases its activity. The excessive increase in the share of transport and then reduce the strength of the media.

The requirement sulfur content in fuel oil is determined by the necessity to create on stage calcination of the carrier optimal conditions subsequent sulfatirovnie catalyst.

Use instead of fuel oil other petroleum fractions is not possible to obtain the desired results.

In known methods for producing catalysts for Hydrotreating processes of oil fractions the application of the described technology is unknown. Therefore, this solution meets the criteria of "novelty" and "significant difference".

The proposed method is illustrated by the following examples:

Primer.

100g aluminium hydroxide is mixed with 5 g of fuel oil with a sulfur content of 1.0% by weight. peptidases solution 18% nitric acid, is formed in the form of extrudates with a diameter of 2.0 mm, dried for 5 hours at a temperature of 20oC, 6 hours at a temperature of 100oC,made red-hot at a temperature of 600oC. is Obtained but pitivat solutions paramolybdate ammonium and nitrate Nickel content Mo321% wt. and NiO 7% wt

For the obtained catalyst spend catalytic tests. When carrying out catalytic tests in the quality of raw materials used vacuum gas oil with a sulfur content of 0,84% wt. The catalytic activity of the sample was evaluated according to the degree of conversion of sulfur-containing compounds.

The results are shown in the table. The same table shows the parameters for the preparation of catalysts according to examples 2 to 7 and the results of their tests. The sequence of operations when running examples 2 to 7 is similar to example 1. All catalytic tests were carried out under the same process parameters (partial hydrogen pressure of 30 MPa, the volumetric feed rate 3 h-1temperature 360oC).

From the table it is seen that the introduction of the cake aluminium hydroxide at the stage of its forming oil with the specified sulfur content and in these quantities leads to the increase of pore volume without reducing the strength of the catalyst, and also creates an optimum distribution of the pore radii that increases the activity of the catalyst.

The method of producing catalyst for Hydrotreating heavy oil fractions, containing, by weight.

3/g under the condition that the proportion of pores with a radius of 10000 - is 20-25% index of tensile splitting strength of not less than 1.3 kg/mm

 

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FIELD: chemistry.

SUBSTANCE: invention relates to a homogeneous catalyst based on tetra-4-(4'-carboxyphenylsulphanium)-5-cobalt nitrophtalocyanine(II) of tetrasodium salt of formula .

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4 dwg, 1 tbl, 2 ex

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