The method of producing catalyst

 

(57) Abstract:

The invention relates to the production of catalysts for oil refining, in particular hydrofining catalysts. The aim of the proposed method is to increase the degree of impregnation of the catalyst at low concentrations of the impregnating solution, providing stability and reducing the cost of catalyst. The essence of the proposed method is that the solution paramolybdate ammonium and nitrate cobalt processed by a permanent magnetic field before the impregnation of the carrier. At the intersection of the magnetic field of the fluid flow is increased activity of the metal cations in solution and the wetting ability of the solution. This leads to facilitate the penetration of the applied metals in the particles of the medium and, consequently, the increase in the concentration of deposited metal. This goal is achieved by exposure to the treatment solution of the permanent magnetic field of 80-120 kA/m at a flow rate through the generator magnetic field of 0.5-1.5 m/s the present invention allows to increase the degree of impregnation of the carrier 7-15 Rel. % at constant concentrations of the impregnating solutions, refers to the production of catalysts for oil refining, in particular the production of catalysts for hydrodesulphurization unit of crude oil.

Known technology for producing catalysts for hydrodesulphurization unit, comprising the sequential impregnation of a pre-formed solid acid carrier solution of ammonium complex salt of molybdenum or tungsten and a solution of salt of cobalt or Nickel with an intermediate (between impregnation and final heat treatment, which consists in drying and calcination of the catalyst precursor [H. R. Gaisano, I. I., Zadka, S. L. Munde, A. N. The elders. Simplification of impregnation upon receipt of Hydrotreating catalysts. Chemistry and technology of fuels and oils. 1991, No. 1, S. 26]. We studied the influence of several parameters impregnation of the carrier on the number of deposited active metal on the catalyst and, consequently, on its gidroobesserivaniya activity.

The disadvantage of this method is the inability to obtain a stable solution, providing a high level of catalyst activity without special additives-stabilizers.

Known method of preparing catalysts for hydrodesulphurization unit of crude oil by successive impregnation at pH=3-4 pre formuvannia. The impregnation is carried out with intermediate drying. Upon completion of the impregnation, the catalyst precursor is subjected to heat treatment, which consists in drying and calcination [RF Patent N 2052288, 01 J 35/02]. Applying a known method to obtain a catalyst with a certain limited amount of deposited material under specified conditions.

The disadvantage of this method is the need to increase the concentration of the impregnating solution to obtain a catalyst with a high content of deposited active metal. This leads to reduced stability of the solutions, reducing the efficiency of the impregnation, the increase in the cost of the catalyst.

The aim of the proposed method is to increase the degree of impregnation of the catalyst at low concentrations of the impregnating solution, ensuring its stability, reducing the cost of the catalyst.

The essence of the proposed method is that the solution paramolybdate ammonium and nitrate cobalt processed by a permanent magnetic field before the impregnation of the carrier. At the intersection of the magnetic field of the fluid flow is increased activity of the metal cations in solution, and also wetting is therefore the increase in the concentration of deposited metal.

The proposed method is as follows.

Pre-prepared solution of paramolybdate ammonium concentration 80-160 g/l) direct from the bottom up in magnitudea device electromagnetic execution core [Application N 98104229/25 (004435) C 02 F 1/48]. Moreover, the device is located vertically or obliquely, to avoid the formation of air pockets. The flow of the impregnating solution perpendicularly intersects a constant magnetic field with a linear speed of 0.5 - 1.5 m/s field strength in the gap of the device is chosen in the range from 80 to 120 kA/m and set by changing the DC power in the power supply device (the specified interval is selected based on preliminary studies). Treated with a solution of paramolybdate ammonium at pH=3-4, the temperature of 70-80oC impregnated pre-formed shape aluminium oxide particles with a cross-section in the form of revolucio hexagonal star with a radius of from 2.0 to 3.5 mm, the resulting catalyst precursor is dried at a temperature of 105-120oC for 4-5 hours. Then the impregnation is conducted with a solution of cobalt nitrate (concentration of 40-60 g/l), which clicks drying the catalyst precursor at 105-120oC for 4-5 hours and calcination at 400 to 500oC for 1.5-2 hours. The amount deposited on the catalyst metal was determined by XRF.

Preparation of the impregnating solutions.

The first impregnation solution in 1 l of water was dissolved 120 g paramolybdate ammonium, the resulting solution was allowed to cross magnitudea device with a linear velocity of 1.0 m/s is the magnetic field strength was 110 kA/m

The second impregnating solution in 1 l of water was dissolved 50 g of cobalt nitrate, the resulting solution was treated in the same way in a magnetic field. Processing the magnetic field of the solutions produced immediately before the impregnation.

Example.

100 g of pre-formed shaped particles of aluminum oxide with a cross-section in the form of revolucio hexagonal star with a radius of 3.5 mm was impregnated treated in a magnetic field solution paramolybdate ammonium (62 ml, concentration of 120 g/l) at pH=3.5 and a temperature of 80oC, dried at 120oC for 4 hours, then soaked pre-treated in a magnetic field with a solution of nitrate of cobalt (58 ml concentration of 50 mg/l), was dried at a temperature of 120oC for 4 s catalysts, the composition of which is given in the table.

Thus, the proposed method comprising the acid impregnation of the carrier with a solution-treated in a constant magnetic field, allows to increase the degree of impregnation of the carrier of the active metals in the 7-15% (relative) at a constant concentration of impregnating solution, temperature, time of impregnation, drying and final heat treatment.

1. The method of producing catalyst hydrodesulphurization unit of crude oil, including sequential impregnation of the solid acid carrier, formed in the form of discrete particles, solutions paramolybdate ammonium and nitrate cobalt at pH = 3 to 4, intermediate drying and final heat treatment of the catalyst precursor, which consists in drying and calcining, characterized in that solutions of paramolybdate ammonium and nitrate cobalt before impregnation is exposed to a constant magnetic field of 80 - 120 kA/m

2. The method according to p. 1, characterized in that the concentration of the solution of paramolybdate ammonium is 80 - 140 g/l, and nitrate of cobalt 40 - 60 g/L.

 

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FIELD: production of hydrorefining catalyst.

SUBSTANCE: the invention presents a method of production of hydrorefining catalysts, that provides for preparation of non-calcined catalyst for hydrorefining of hydrocarbonaceous raw materials polluted with low-purity heteroatoms. The method includes: combining of a porous carrying agent with one or several catalytically active metals chosen from group VI and group III of the Periodic table of elements by impregnation, joint molding or joint sedimentation with formation of a predecessor of the catalyst containing volatile compounds, decrease of the share of the volatile compounds in the predecessor of the catalyst during one or several stages, where at least one stage of decrease of the shares of the volatile compounds is carried out in presence of at least one compound containing sulfur; where before the indicated at least one integrated stage of decrease of the share of volatile compounds - sulfurization the indicated predecessor of the catalyst is not brought up to the temperatures of calcination and the share of the volatile compounds in it makes more than 0.5 %. Also is offered a not-calcined catalyst and a method of catalytic hydrorefining. The invention ensures production of a catalyst of excellent activity and stability at hydrorefining using lower temperatures, less number of stages and without calcination.

EFFECT: the invention ensures production of a catalyst of excellent activity and stability at hydrorefining using lower temperatures, less number of stages and without calcination.

10 cl, 8 ex, 4 dwg

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