A catalyst for hydrotreating petroleum fractions 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 new catalyst for Hydrotreating petroleum fractions containing aluminum oxide, molybdenum oxide, Nickel oxide or cobalt, zinc oxide, fluorine and chlorine. The catalyst has the following composition, wt.%: molybdenum oxide 10 - 14; Nickel oxide or cobalt oxide 3,5; zinc oxide 0,2 - 2,0; fluorine and chlorine of 0.2 - 1.0 at a molar ratio of fluorine to chlorine 1.7 to 2.2; 0,2 - 1,0; aluminum oxide 78 is 86.6. Describes the method of its preparation. The technical result is an increase in the activity of the catalyst. 3 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 obtain a catalyst with increased activity due to the introduction of the catalyst modifier additive is ZnO and item VII A group, preferably F and Cl, taken in a specific molar ratio.

The LEVEL of TECHNOLOGY is the firmness of the active components of the oxides of molybdenum, Nickel or cobalt and phosphate anhydride /EN 2074025 C1, 27.02.97/.

The disadvantage of these catalysts is that the introduction of phosphoric acid in the aluminum hydroxide significantly reduces the mechanical strength of the catalyst, which affects its performance.

Closest to the invention to the technical essence and the achieved effect is the way [SU 1657226 A1, 23.06.91], according to which aluminumalloy catalyst, modified additives tin and fluorine, shows its highest activity in the field of high temperature Hydrotreating process, which reduces the yield of the target product and the increase in the concentration of coke on the catalyst.

The INVENTION consists in the following: the invention is directed to solving the problem of obtaining a highly active catalyst hydrodesulphurization unit as straight-run petroleum fractions and products of secondary processes.

The technical result allows us to solve the problem. This technical result is achieved by obtaining a catalyst of the following composition, wt. percent: molybdenum oxide - 10-14; Nickel oxide or cobalt oxide - 3-5; zinc oxide - 0,2-2,0; fluorine and is,2-2,0 wt.% zinc oxide in the form of zinc acetate in the weight of aluminum hydroxide, modified fluorine and chlorine, the contents of which are on calcined catalyst is 0.2 to 1.0 wt.% when the molar ratio of 1.7 to 2.2, and a method of producing a catalyst, comprising impregnating alyumomolibdyenovykh media modified from 0.2 to 1.0 wt.% fluorine and chlorine in a molar ratio of 1.7 to 2.2, joint aqueous solution of zinc acetate and nitrate or acetate of Nickel or cobalt.

The ESSENTIAL features of the present invention is a catalyst composition, the ratio of its components, and how to obtain it.

DISTINCTIVE features of this invention are the composition and ratio of catalyst components, wt.%:

Molybdenum oxide (MoO3) - 10 - 14

Nickel oxide (NiO) or cobalt oxide (CoO) - 3 - 5

Zinc oxide (ZnO) - 0,2 - 2,0

Fluorine (F) and chlorine (Cl) in sum, when the molar ratio n(F)/n(Cl) = 1,7 - 2,2 - 0,2 - 1,0

Aluminum oxide (Al2O3) - 78 - 86,6

and the method of its production, including the introduction of zinc acetate in the aluminum hydroxide-modified fluorine and chlorine in a molar ratio of 1.7 to 2.2, and a process comprising impregnation alyumomolibdyenovykh media modified with fluorine and chlorine in a molar ratio of 1.7 to 2.2, joint water retorqued in the introduction part alumnirelations or aluminoborosilicate catalyst modifiers fluorine and chlorine, taken at a specific molar ratio, and zinc oxide, and method of its introduction in the aluminum hydroxide on stage peptization of an aqueous solution of zinc acetate and impregnation stage alyumomolibdyenovykh media modified with fluorine and chlorine, joint aqueous solution of zinc acetate and nitrate or acetate of Nickel or cobalt. The presence of aluminum hydroxide fluoride and chlorine, taken with a specific molar ratio, contributes to the formation of the active phase formed of aggregated particles of molybdenum oxide, which contributes to such distribution of the zinc oxide, in which he to the maximum extent exerts its electron-donor properties. This ultimately leads to increased activity alumonickelsilicate and aluminoborosilicate catalysts in the reactions of the Hydrotreating process and reduce the process temperature to achieve a certain degree of conversion of hetero-organic compounds.

The invention is illustrated by the following examples.

Example 1. 433 g of aluminum hydroxide with a humidity of 80 wt.% foryouth, adding 0,245 ml of concentrated hydrofluoric acid with a density of 0.99 g/cm3and then when continuous paramashiva the aluminum hydroxide containing 0.2 wt.% the amount of fluorine and chlorine in a molar ratio of n(F)/n(Cl) = 1,7, with stirring, add 10 ml of an aqueous solution containing 0.45 g of zinc acetate. Mixing the modified aluminum hydroxide continued until smooth, then add in the mass of 65 ml of an aqueous solution containing 12.8 g of paramolybdate ammonium. The mass is stirred, evaporated on a water bath to a moisture content of 70 wt.%, molded by extrusion in the form of cylindrical pellets with a diameter of 2.0 to 2.3 mm Molded granules are subjected to heat treatment: drying in air for 12 h; drying for 2 h at 60oC; 2 h at 80oC and 2 h at 110oC; annealing at a temperature of 550oC for 4 h

97 g of calcined modified alyumomolibdyenovykh media containing 10.0 wt.% MoO3; 0.2 wt.% ZnO; 0.2 wt.% in the sum of F and Cl when the molar ratio n(F)/n(Cl) = 1,7, placed in 70 ml of impregnating solution containing 12.8 g of uranyl nitrate Nickel. Impregnation of the carrier is carried out at 60-70oC for 1 h

The catalyst was subjected to heat treatment: drying for 1 h at 80oC; 1 h at 100oC; 1 h at 120oC; 1 h at 140oC; 1 h at 160oC; 1 h at 180oC; annealing when the rate is 0.2 at a molar ratio of n(F)/n(Cl) = l,7; Al2O3- 86,6.

Example 2. 413 g of aluminum hydroxide with a humidity of 80 wt.% foryouth by adding 0.75 ml of concentrated hydrofluoric acid with a density of 0.99 g/cm3and then with continuous stirring peptizer of 0.74 ml of concentrated hydrochloric acid with a density of 1.18 g/cm3. In patinirovannuyu weight of aluminum hydroxide, containing by weight 0.6% the amount of fluorine and chlorine in a molar ratio of n(F)/n(Cl) = 1,7, with stirring, add 10 ml of an aqueous solution containing 1.8 g of zinc acetate. Mixing the modified aluminum hydroxide continued until smooth, then add in the mass of 65 ml of an aqueous solution containing 15,4 g paramolybdate ammonium. The mass is stirred, evaporated on a water bath, formed by extrusion in the form of cylindrical pellets subjected to heat treatment as in example 1.

96 g of calcined modified alyumomolibdyenovykh media containing 12 wt.% MoO3; 0.8 wt.% ZnO; 0.6 wt.% the amount of fluorine and chlorine in a molar ratio of n(F)/n(Cl) = 1,7, placed in 70 ml of impregnating solution containing 16 g of uranyl nitrate Nickel. Impregnation of the modified carrier, heat treatment of the obtained catalyst PMA F and Cl - 0.6 molar ratio n(F)/n(Cl) = 1,7; Al2O3- 82,6.

Example 3. 390 g of aluminum hydroxide with a humidity of 80 wt.% foryouth, adding to 1.23 ml of concentrated hydrofluoric acid with a density of 0.99 g/cm3and then with continuous stirring peptizer 1,20 ml of concentrated hydrochloric acid with a density of 1.18 g/cm3In patinirovannuyu mass of aluminum hydroxide containing 1.0 wt.% the amount of fluorine and chlorine in a molar ratio of n(F)/n(Cl) = 1,7, with stirring, add 10 ml of an aqueous solution containing 4.52 g of zinc acetate. Mixing the modified aluminum hydroxide continued until smooth, then add in the mass of 65 ml of an aqueous solution containing 17.9 g of paramolybdate ammonium. The mass is stirred, evaporated on a water bath, formed by extrusion in the form of cylindrical pellets subjected to heat treatment as in example 1.

95 g of calcined modified, alyumomolibdyenovykh media containing 14 wt. % MoO3; 2.0 wt.% ZnO; 1.0 wt.% the amount of fluorine and chlorine in a molar ratio of n(F)/n(Cl) = 1,7, placed in 70 ml of impregnating solution containing 20 g of uranyl nitrate Nickel. Impregnation of the modified carrier, heat is RA, wt.%: MoO3- 14,0; NiO - 5,0; ZnO to 1.0; the sum of F and Cl is 1.0 when the molar ratio n(F)/n(Cl) = 1,7; Al2O3- 78,0.

Example 4. 433 g of aluminum hydroxide with a humidity of 80 wt.% foryouth, adding, and 0.28 ml of concentrated hydrofluoric acid with a density of 0.99 g/cm3and then with continuous stirring peptizer of 0.21 ml of concentrated hydrochloric acid with a density of 1.18 g/cm3. In patinirovannuyu mass of aluminum hydroxide containing 0.2 wt.% the amount of fluorine and chlorine in a molar ratio of n(F)/n(Cl) = 2,2, with stirring, add 10 ml of an aqueous solution containing 0.45 g of zinc acetate. Mixing the modified aluminum hydroxide continued until smooth, then add in the mass of 65 ml of an aqueous solution containing 12.8 g of paramolybdate ammonium. The mass is stirred, evaporated on a water bath, formed by extrusion in the form of cylindrical pellets subjected to heat treatment as in example 1.

97 g of calcined modified alyumomolibdyenovykh media containing 10 wt.% MoO3; 0.3 wt.% ZnO; 0.2 wt.% the amount of fluorine and chlorine in a molar ratio of n(F)/n(Cl) = 2,2, placed in 70 ml of impregnating solution containing 12 g of uranyl nitrate of cobalt. Profit 1.

The composition of the obtained catalyst, wt.%: MoO3- 10,0; CoO - 3,0; ZnO - 0,2; the sum of F and Cl - 0.2 at a molar ratio of n(F)/n(Cl) = 2,2; Al2O3- 86,6

Example 5. 413 g of aluminum hydroxide with a humidity of 80 wt.% foryouth, adding 0,84 ml of concentrated hydrofluoric acid with a density of 0.99 g/cm3and then with continuous stirring peptizer 0.63 ml of concentrated hydrochloric acid with a density of 1.18 g/cm3. In patinirovannuyu weight of aluminum hydroxide, containing by weight 0.6% the amount of fluorine and chlorine in a molar ratio of n(F)/n(Cl) = 2,2, with stirring, add 10 ml of an aqueous solution containing 1.8 g of zinc acetate. Mixing the modified aluminum hydroxide continued until smooth, then add in the mass of 65 ml of an aqueous solution containing 15,4 g paramolybdate ammonium. The mass is stirred, evaporated on a water bath, formed by extrusion in the form of cylindrical pellets subjected to heat treatment as in example 1.

96 g of calcined modified alyumomolibdyenovykh media containing 12 wt.% MoO3; 0.8 wt.% ZnO; 0.6 wt.% the amount of fluorine and chlorine in a molar ratio of n(F)/n(Cl) = 2,2, placed in 70 ml of impregnating solution containing 16 g hexage the and carry out analogously to example 1.

The composition of the obtained catalyst, wt.%: MoO3to 12.0; CoO - 4,0; ZnO - 0,8; the sum of F and Cl - 0.6 molar ratio n(F)/n(Cl) = 2,2; Al2O3- 86,6.

Example 6. 390 g of aluminum hydroxide with a humidity of 80 wt.% foryouth, adding to 1.4 ml of concentrated hydrofluoric acid with a density of 0.99 g/cm3and then with continuous stirring peptizer of 1.05 ml of concentrated hydrochloric acid with a density of 1.18 g/cm3. In patinirovannuyu mass of aluminum hydroxide containing 1.0 wt.% the amount of fluorine and chlorine in a molar ratio of n(F)/n(Cl) = 2,2, with stirring, add 10 ml of an aqueous solution containing 4.52 g of zinc acetate. Mixing the modified aluminum hydroxide continued until smooth, then add in the mass of 65 ml of an aqueous solution containing 17.9 g of paramolybdate ammonium. The mass is stirred, evaporated on a water bath, formed by extrusion in the form of cylindrical pellets subjected to heat treatment as in example 1.

95 g of calcined modified alyumomolibdyenovykh media containing 14 wt.% MoO3; 2.0 wt.% ZnO; 1.0 wt.% the amount of fluorine and chlorine in a molar ratio of n(F)/n(Cl) = 2,2, placed in 70 ml of impregnating solution containing 20 g of g is Isadora carried out analogously to example 1.

The composition of the obtained catalyst, wt.%: MoO3- 14,0; CoO - 5,0; ZnO - 2,0; the sum of F and Cl is 1.0 when the molar ratio n(F)/n(Cl) = 2,2; Al2O3- 78,0.

Example 7. 433 g of aluminum hydroxide with a humidity of 80 wt.% foryouth, adding 0,27 ml of concentrated hydrofluoric acid with a density of 0.99 g/cm3and then with continuous stirring peptizer to 0.22 ml of concentrated hydrochloric acid with a density of 1.18 g/cm3. In patinirovannuyu mass of aluminum hydroxide containing 0.2 wt.% the amount of fluorine and chlorine in a molar ratio of n(F)/n(Cl) = 2, while stirring, 65 ml of an aqueous solution containing 12.8 g of paramolybdate ammonium. The mass is stirred, evaporated on a water bath, formed by extrusion in the form of cylindrical pellets subjected to heat treatment as in example 1.

97 g of calcined modified alyumomolibdyenovykh media containing 10 wt. % MoO3; 0.2 wt. % in the sum of F and Cl when the molar ratio (F)/n(Cl) = 2, placed in 70 ml aqueous impregnating solution containing 0.45 g of zinc acetate and 10 g of uranyl acetate Nickel. Impregnation of the modified carrier, heat treatment of the obtained catalyst is carried out analogously to example 1.

The composition SUB>O3- 86,6.

Example 8. 413 g of aluminum hydroxide with a humidity of 80 wt.% foryouth, adding 0,81 ml of concentrated hydrofluoric acid with a density of 0.99 g/cm3and then with continuous stirring peptizer of 0.66 ml of concentrated hydrochloric acid with a density of 1.18 g/cm3. In patinirovannuyu weight of aluminum hydroxide, containing by weight 0.6% the amount of fluorine and chlorine in a molar ratio of n(F)/n(Cl) = 2, while stirring, 65 ml of an aqueous solution containing 15,4 g paramolybdate ammonium. The mass is stirred, evaporated on a water bath, formed by extrusion in the form of cylindrical pellets subjected to heat treatment as in example 1.

96 g of calcined modified alyumomolibdyenovykh media containing 12 wt. % MoO3; 0.6 wt.% in the sum of F and Cl when the molar ratio (F)/n(Cl) = 2, placed in 70 ml aqueous impregnating solution containing 1.8 g of zinc acetate and 13.3 g of the acetate tetrahydrate Nickel. Impregnation of the modified carrier, heat treatment of the obtained catalyst is carried out analogously to example 1.

The composition of the obtained catalyst, wt.%: MoO3to 12.0; PIO - 4,0; ZnO - 0,8; the sum of F and Cl - 0.6 molar ratio n(F)/n(Cl) = 2; Al2O3- 82,6.< hydrofluoric acid with a density of 0.99 g/cm3and then with continuous stirring peptizer 1,10 ml of concentrated hydrochloric acid with a density of 1.18 g/cm3. In patinirovannuyu mass of aluminum hydroxide containing 1.0 wt.% the amount of fluorine and chlorine in a molar ratio of n(F)/n(Cl) = 2, while stirring, 65 ml of an aqueous solution containing 17.9 g of paramolybdate ammonium. The mass is stirred, evaporated on a water bath, formed by extrusion in the form of cylindrical pellets subjected to heat treatment as in example 1.

95 g of calcined modified alyumomolibdyenovykh media containing 14 wt. % MoO3; 1,0 wt. % in the sum of F and Cl when the molar ratio (F)/n(Cl) = 2, placed in 70 ml aqueous impregnating solution containing 4.52 g of zinc acetate and 16.7 g of the acetate tetrahydrate Nickel. Impregnation of the modified carrier, heat treatment of the obtained catalyst is carried out analogously to example 1.

The composition of the obtained catalyst, wt.%: MoO3- 14,0; NiO - 5,0; ZnO - 2,0; the sum of F and Cl is 1.0 when the molar ratio n(F)/n(Cl) = 2; Al2O3- 78,0.

Example 10. 433 g of aluminum hydroxide with a humidity of 80 wt.% foryouth, adding 0,27 ml of concentrated hydrofluoric acid with a density of 0.99 g/cm3and ZAT is. In patinirovannuyu mass of aluminum hydroxide containing 0.2 wt.% the amount of fluorine and chlorine in a molar ratio of n(F)/n(Cl) = 2, while stirring, 65 ml of an aqueous solution containing 12.8 g of paramolybdate ammonium. The mass is stirred, evaporated on a water bath, formed by extrusion in the form of cylindrical pellets subjected to heat treatment as in example 1.

97 g of calcined modified alyumomolibdyenovykh media containing 10 wt. % MoO3; of 0.21 wt.% in the sum of F and Cl when the molar ratio (F)/n(Cl) = 2, placed in 70 ml aqueous impregnating solution containing 0.45 g of zinc acetate and 10 g of acetate tetrahydrate cobalt. Impregnation of the modified carrier, heat treatment of the obtained catalyst is carried out analogously to example 1.

The composition of the obtained catalyst, wt.%: MoO3- 10,0; CoO - 3,0; ZnO - 0,2; the sum of F and Cl - 0.2 at a molar ratio of n(F)/n(Cl) = 2; Al2O3- 86,6.

Example 11. 413 g of aluminum hydroxide with a humidity of 80 wt.% foryouth, adding 0,81 ml of concentrated hydrofluoric acid with a density of 0.99 g/cm3and then with continuous stirring peptizer of 0.66 ml of concentrated hydrochloric acid with a density of 1.18 g/cm3. In peptise the while stirring, 65 ml of an aqueous solution, containing 15,4 g paramolybdate ammonium. The mass is stirred, evaporated on a water bath, formed by extrusion in the form of cylindrical pellets subjected to heat treatment as in example 1.

96 g of calcined modified alyumomolibdyenovykh media containing 12 wt. % MoO3; 0.6 wt.% in the sum of F and Cl when the molar ratio (F)/n(Cl) = 2, placed in 70 ml aqueous impregnating solution containing 1.8 g of zinc acetate and 13.3 g of the acetate tetrahydrate cobalt. Impregnation of the modified carrier, heat treatment of the obtained catalyst is carried out analogously to example 1.

The composition of the obtained catalyst, wt.%: MoO3to 12.0; CoO - 4,0; ZnO - 0,8; the sum of F and Cl - 0.6 molar ratio n(F)/n(Cl) = 2; Al2O3- 82,6.

Example 12. 390 g of aluminum hydroxide with a humidity of 80 wt.% foryouth, adding 1.35 ml of concentrated hydrofluoric acid with a density of 0.99 g/cm3and then with continuous stirring peptizer 1,10 ml of concentrated hydrochloric acid with a density of 1.18 g/cm3. In patinirovannuyu mass of aluminum hydroxide containing 1.0 wt.% the amount of fluorine and chlorine in a molar ratio of n(F)/n(Cl) = 2, while stirring, 65 ml of an aqueous solution, soderjaschiesya granules, subjected to heat treatment as in example 1.

95 g of calcined modified alyumomolibdyenovykh media containing 14 wt. % MoO3; 1.0 wt.% in the sum of F and Cl when the molar ratio (F)/n(Cl) = 2, placed in 70 ml aqueous impregnating solution containing 4.52 g of zinc acetate and 16.7 g of the acetate tetrahydrate cobalt. Impregnation of the modified carrier, heat treatment of the obtained catalyst is carried out analogously to example 1.

The composition of the obtained catalyst, wt.%: MoO3- 14,0; CoO - 5,0; ZnO - 2,0; the sum of F and Cl is 1.0 when the molar ratio n(F)/n(Cl) = 2; Al2O3- 78,0

Test the activity of the catalysts was conducted on a laboratory flow-through installation in the Hydrotreating process of straight-run diesel weighted fractional composition in mixture with oil coking and catalytic cracking gas oil. Mixed raw materials with their boiling temperature 180-400oC had the following composition, vol.%;

Straight-run diesel fuel - 80

The oil coking - 10

The catalytic cracking gas oil - 10

The total sulfur content of raw materials amounted to 1.20 wt.%.

The process temperature of 340 and 360oC; volumetric feed rate of 2.5 h-1; pressure of 3.5 MWe catalyst comparison of the selected catalyst-prototype [2] mark G-26.

From the table it follows that the proposed catalyst for Hydrotreating petroleum fractions, including secondary origin, characterized by a higher activity that allows you to achieve where there is a high degree of desulfurization of the raw materials at low process temperatures. This leads to the reduction of energy consumption and prolong the service life of the catalyst.

SOURCES OF INFORMATION

1. RF patent N 2074025. Nasirov R. K. a Method of producing catalyst for Hydrotreating petroleum fractions. Publ. 27.02.97. Bull. N 6. B 1 J 21/04.

2. Auth. mon. USSR N 1657226. Loginova, A. N., Sharygina M. A., Tomina N. N., Plaksina Centuries , Shabalina I.e., Milutin B. C., Waskow C. A., Vasiliev M. I. Kuibyshev Polytechnic Institute. Century Century Kuibyshev. Publ. 23.06.91. Bull. N 23. B 01 J 37/02, 23/88.

1. A catalyst for Hydrotreating petroleum fractions containing aluminum oxide, molybdenum oxide, Nickel oxide or cobalt, zinc oxide, fluorine and chlorine, characterized by the following ratio, wt.%:

Molybdenum oxide (MoO3) - 10 - 14

Nickel oxide (NiO) or cobalt oxide (CoO) - 3 - 5

Zinc oxide (ZnO) - 0,2 - 2,0

Fluorine (F) and chlorine (Cl) in sum, when the molar ratio n(F)/n(Cl) = 1,7 - 2,2 - 0,2 - 1,0

Aluminum oxide (Al2O3) - 78 - 86,6

introduction molybdenum compounds, molding, extrusion, drying, calcination, impregnation with an aqueous solution of active ingredients, followed by drying and calcination, wherein peptization fluorinated aluminum hydroxide carried out with hydrochloric acid, taken in such quantity that the molar ratio of F and Cl was 1.7 to 2.2, with successive introduction to patinirovannuyu weight aqueous solutions of salts of zinc acetate and paramolybdate ammonium, followed by molding, drying, calcination, impregnation with an aqueous solution of nitrate or acetate of Nickel or cobalt, drying, and calcination.

3. The method of producing catalyst under item 1, including deposition of aluminum hydroxide, fluoridation, peptization, introduction molybdenum compounds, molding, extrusion, drying, calcination, impregnation with an aqueous solution of active ingredients, followed by drying and calcination, wherein alyumomolibdyenovykh media containing 10 to 14 wt.% MoO3and 0.2 - 2.0 wt.% fluorine and chlorine in a molar ratio of 1.7 to 2.2, impregnate joint aqueous solution of zinc acetate and nitrate or acetate of Nickel or cobalt, followed by drying and calcination.

 

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