Gasoline fraction hydrotreatment and a method for preparation thereof

FIELD: petroleum processing and catalysts.

SUBSTANCE: field of invention is production of catalysts for catalytic hydrotreatment (desulfurization) of gasoline fractions, e.g. straight-run gasoline. Herein disclosed is block-type high-porosity cellular catalyst for hydrotreatment of straight-run gasoline having porosity at least 90-93% and microporosity up to 30%, average pore size being ranging from 0.5 to 2.0 μm. Catalyst consists of α-alumina-based carrier and active catalyst portion containing sulfated zirconium dioxide and metallic palladium in concentration 0.5-0.9 wt %. Catalyst preparation method is also claimed and is as follows. Carrier is prepared from reticular polyurethane foam and impregnated with slurry containing more than 30 wt % α-alumina, after which calcined at 1300-1500°C, impregnated with water-soluble zirconium salts, dried at 100-200°C, calcined at 450-950°C, treated with 5-10% sulfuric acid, dried, calcined at 500-550°C, treated with palladium nitrate, dried, and calcined at 400-450°C, whereupon palladium oxide is reduced to metallic palladium.

EFFECT: lowered pressure and temperature of hydrotreatment process, considerably reduced process duration, lowered sulfur level in straight-run gasoline due to developed surface of catalyst, and prevented crumbling and loss of catalyst due to cellular structure and high strength.

 

The invention relates to the refining and petrochemical industries and can be used, in particular, in the production of a catalyst for catalytic hydro-desulfurization) gasoline fractions, such as gasoline.

Known allocable(Nickel)molybdenum catalyst for Hydrotreating petroleum distillates and the method of its preparation (A.S. USSR №1557742, CL 01J 37/00, 23/88), including separate precipitation of sodium aluminate acid at room temperature and the boiling, the subsequent mixing of modifications of aluminum hydroxide, hot and cold deposition in a specific mass ratio, leaching, extrusion molding, drying and calcination of the obtained extrudates of alumina, impregnated alumina ammonium solution of salts of cobalt or Nickel and molybdenum, subsequent drying and calcination of the resulting catalyst in the temperature range 50...600°C.

The disadvantages of using such a catalyst in the Hydrotreating process of petroleum distillates such as gasoline, are high pressure (3.0 MPa) and temperature (340° (C) Hydrotreating process, the duration of the Hydrotreating process (24 hours), high sulfur content in hydrogenase (straight run gasoline), equal to 1.4...2.5 mg/kg

The closest in technical the coy nature of the claimed catalyst is (a patent of the Russian Federation, No. 2232047, CL 7 01J 21/04, 23/62, 23/656, 27/13, bull. No. 19, 10.07.2004) for catalytic reforming of gasoline fractions containing platinum, chlorine and the promoter is rhenium or tin, distributed on the surface of the carrier, consisting of a composition of bulk carbonaceous oxynitride, surface oxychloride and gamma-aluminum oxide, and the method of its preparation, which includes the following stages: peptization powder pseudoboehmite of aluminum hydroxide; granulating plastic paste (or pseudosasa) a carrier; drying and calcining the granules (extrudates or beads); coating the surface of the carrier compounds active ingredients: platinum (0,3% wt.), promoter (rhenium or tin), chlorine; heat treatment of the catalyst by drying and calcination in air flow). Before testing, the catalyst is reactivated by hydrogen at a temperature of 450...500°C, pressure of 1.0 MPa, the flow of hydrogen from 66.7 l/h for 4...5 hours.

The disadvantages of the catalyst can include: exposure of extrudates destruction, the complexity of the regeneration of granules (extrudates), increased hydraulic resistance of the granular layer, etc.

The technical result, which is aimed by the invention, is to develop a catalyst and the method of its preparation, it achieves a significant reduction in the content of the series is in straight-run gasoline, reducing the length of the Hydrotreating process, reducing the pressure and temperature of the Hydrotreating process, preventing the destruction of the catalyst, increasing the service life of the catalyst.

To achieve the technical result of the proposed catalyst and its preparation method.

Catalyst - block high porous foam with a porosity of not less than 90...93%, with mikroporistogo up to 30%, an average pore size of 0.5 to 2.0 μm, consisting of a carrier-based α-aluminium oxide and the active portion of the catalyst containing sulfated Zirconia and metal palladium with a mass content of 0.5...0.9 percent.

The method of preparation of such a catalyst is as follows. Highly porous cellular carrier for catalyst made from open-celled polyurethane foam, soaking the last slip, containing more than 30% wt. α-aluminium oxide. Then dried at a temperature of 100...200°and calcined at a temperature of 1300...1500°C. a highly porous carrier contains more than 90% α-aluminium oxide. For the development of the catalyst surface on the carrier causing the active substrate of oxides of metals of group IV of the Periodic table of Mendeleev, for example zirconium dioxide. For this purpose, the carrier is impregnated with solutions of water soluble salts of zirconium, for example chloride C is ranila or nitrate Zirconia, or a mixture of tetraethoxysilane with isopropyl alcohol, then dried at a temperature of 100...200°and calcined in the temperature range 450...950°C. the Content of zirconium oxide in the catalyst is 4...10% wt.

The samples treated with a solution of 5...10% sulfuric acid, dried, calcined at a temperature of 500...550°C, treated with a solution of palladium nitrate, dried and calcined at a temperature of 400...450°, restore the palladium oxide to palladium metal with a mass content of 0.5...0.9% wt.

The method of preparation of a new catalyst and its efficiency in the use process of hydro-desulfurization) gasoline confirmed by the following examples.

Example 1

Preparation of open-celled polyurethane foam is made in the form of a cylinder with a diameter of 50 mm and a height of 50 mm, impregnated with a slurry containing more than 30% wt. α-aluminium oxide, method for cyclic compression and stretching, dried at a temperature of 100...200°and calcined at a temperature of 1300...1500°C. the Resulting highly porous carrier contains more than 90% α-aluminium oxide. The carrier impregnated with 15% NaCl Zirconia, maintained at a temperature of 950°C for one hour. The content of zirconium oxide in the catalyst is 7.5% wt.

Then the carrier with the active padlock the th Zirconia is treated with a palladium nitrate solution (5% wt.), dried at a temperature of 120°C, calcined at a temperature of 400...450°, restore the palladium oxide to palladium metal.

In a heated reactor, which is a cylindrical vessel with an inner diameter of 50 mm, made of stainless steel, pour 30 ml of gasoline with a sulfur content of 440 ppm. Block a highly porous honeycomb catalyst containing zirconium dioxide, and 0.9% wt. metal palladium by weight 23 g, with a porosity of 90-93%, mikroporistogo up to 30%, is placed in the middle part of the reactor, providing its immobility. The reactor is fixed on the rocking chair, capable of producing the number of oscillations is equal to 120-160 min-1. Keep the temperature equal to 200°With, in the reactor by the flow of the coolant in the jacket of the reactor from thermostat. The Hydrotreating gasoline is carried out at a pressure of 1 MPa for 4 to 5 minutes. From the reactor is unloaded straight-run gasoline with a sulfur content equal to 51 ppm.

The Hydrotreating gasoline is performed at a pressure of 1.5 MPa for 4 to 5 minutes. From the reactor is unloaded straight-run gasoline with a sulfur content equal to 45 ppm.

The Hydrotreating gasoline is performed at a pressure of 2.0 MPa for 4 to 5 minutes. From the reactor is unloaded straight-run gasoline with a sulfur content equal to 39 ppm.

Example 2.

Preparation of open-celled polyurethane foam technology is prepared in the form of a cylinder with a diameter of 50 mm, and a height of 50 mm, impregnated with a slurry containing more than 30% wt. α-aluminium oxide, method for cyclic compression and stretching, dried at a temperature of 100...200°and calcined at a temperature of 1300...1500°C. the Resulting highly porous carrier contains more than 90% α-aluminium oxide. Then the carrier is impregnated with 15% NaCl Zirconia, maintained at a temperature of 950°C for one hour. The content of metal oxide (Zirconia) in the catalyst is 7.5% wt.

Received the sample carrier with the active substrate is treated with a solution of 10% sulfuric acid at room temperature, using the immersion technique with subsequent swelling of the excess acid without any outside influence, dried and calcined at a temperature of 500...550°C.

Then the carrier with the active backing of sulfated Zirconia is treated with a palladium nitrate solution (5% wt.), dried at a temperature of 120°C, calcined at a temperature of 400...450°, restore the palladium oxide to palladium metal.

In a heated reactor pour 30 ml of gasoline with a sulfur content of 440 ppm. Block a highly porous honeycomb catalyst containing 0.5 wt.%. metallic palladium on the sulfated Zirconia, weight 23 g, with a porosity of 90-93%, mikroporistogo up to 30%, is placed in the middle is part of the reactor. Maintain the reaction temperature being 230°With, in the reactor by the flow of the coolant in the jacket of the reactor from thermostat. The Hydrotreating gasoline is performed at a pressure of 1.0 MPa, for 4 to 5 minutes. From the reactor is unloaded straight-run gasoline with a sulfur content of 6.7 ppm.

Example 3. Analogous to example 2.

In a heated reactor pour 30 ml of gasoline with a sulfur content of 440 ppm. Block a highly porous honeycomb catalyst containing 0.5 wt.%. metallic palladium on the sulfated Zirconia, weight 23 g, with a porosity of 90-93%, mikroporistogo up to 30%, is placed in the middle part of the reactor. Maintain the reaction temperature equal to 220°With, in the reactor by the flow of the coolant in the jacket of the reactor from thermostat. The Hydrotreating gasoline is performed at a pressure of 1.0 MPa for 4 to 5 minutes. From the reactor is unloaded straight-run gasoline. The analysis showed the absence of sulfur straight-run gasoline.

In all the examples performed after the test there was no erosion of the block highly porous honeycomb catalyst, this can be judged by transparency paged product. After a process of Hydrotreating gasoline block highly porous honeycomb catalyst is subjected to regeneration. The number of regenerations - more than 50. Block of the honeycomb catalyst has fur the systematic crushing strength, 0.5...2.0 MPa, and its hydraulic resistance in two, three times less than the hydraulic resistance of the granular layer.

The use of a block of the honeycomb catalyst in the Hydrotreating process of gasoline reduces the sulfur content in straight-run gasoline to ten ppm or less, reduces the duration of the Hydrotreating process dozens of times, reducing the process pressure is 1.5 to 2.0 times, reduces the process temperature in 1.5 times and increases the service life of the catalyst is 1.5 times or more.

The process of Hydrotreating gasoline fractions, in particular gasoline, progressing only when sharing sulfated Zirconia and metal palladium.

Liquid-phase Hydrotreating gasoline fractions, in particular gasoline, carried out in a reactor with a reaction zone filled with highly porous block of the honeycomb catalyst. Block highly porous cellular material (α-Al2About3) with a porosity of not less than 90...93%, mikroporistogo up to 30%, is used as the catalyst carrier has a high Aero - and hydroponically, has a higher coefficient of external mass transfer compared to extrudates.

1. A catalyst for Hydrotreating gasoline fractions containing noble metal distributed on the surface but is of Italia, includes aluminum oxide, characterized in that it comprises a modular porous media with porosity of not less than 90...93%, with mikroporistogo up to 30%, manufactured on the basis of α-aluminium oxide and supported on a carrier of the active part of the catalyst containing sulfated Zirconia and metal palladium with a mass content of 0.5...0.9 percent.

2. The method of preparation of the catalyst according to claim 1, which includes stages of cooking, drying in the temperature range 100...200°and annealing the substrate, applying to the surface of the carrier of the active component in the form of a noble metal, drying and calcination of the catalyst and recovery of its hydrogen, characterized in that the carrier is made from open-celled polyurethane foam, impregnated with a slurry containing more than 30% of the mass α-aluminium oxide, calcined at a temperature of 1300...1500°C impregnate the carrier with water soluble salts of zirconium, dried at a temperature of 100...200°C, calcined at temperatures up to 950°With handle 5...10%sulfuric acid, dried, calcined at a temperature of 500...550°C, is treated with a palladium nitrate solution, dried, calcined at a temperature of 400...450°C, followed by reduction of palladium oxide to palladium metal.



 

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