Petroleum fraction hydrofining process

FIELD: petroleum processing.

SUBSTANCE: invention, in particular, relates to petroleum fraction hydrofining process utilizing presulfided catalysts. Hydrofining process is described involving contacting petroleum fractions with presulfided catalyst containing alumina-carried cobalt, molybdenum, phosphorus, and boron, said process being conducted at 320-340°C, pressure 3.0-5.0 MPa, volumetric feed supply rate 1.0-6.0 h-1, normalized volumetric hydrogen-containing gas-to-feed ratio (500-1000):1 in presence of catalyst sulfided outside of reactor. Sulfidizing of catalyst is accomplished with hydrogen sulfide at 80-500°C and volumetric hydrogen sulfide flow rate 0.02-6.0 h-1. Chemical composition of catalyst is the following, wt %: MoS2 8.0-17.0, Co3S2 1.5-4.0, P2O3 2.5-5.0, B2O3 0.3-1.0, La2O3 1.0-5.0, and aluminum oxide - the balance.

EFFECT: simplified process.

2 cl, 1 tbl, 3 ex

 

The invention relates to the field of oil refining, in particular to the development of techniques for Hydrotreating petroleum fractions using presulfiding catalysts.

Practice has shown that the optimal and most efficient oil hydrodesulphurization unit fractions is achieved by contacting the feedstock with solifidianism Hydrotreating catalysts. The process of sulfatirovnie and activation of the catalysts is usually carried out in a catalytic reactor or outside of it using a sulfiding agent and hydrogen. As the sulfiding agent is used, the gas mixture of hydrogen sulfide and hydrogen, the raw material mixture with username compound, elemental sulfur and other

Getting sulfurous gas needed for acarnania catalysts loaded in the Hydrotreating reactor is associated with high technological difficulties. Options include the use of various sulfur-containing compounds that are the source of formation of hydrogen sulfide, the most acceptable option is the use of elemental sulfur, which is loaded together with the catalyst. Molten sulfur at temperatures above 120°able to quickly penetrate the pores of the catalyst and cooling to remain in it. In an atmosphere of hydrogen containing gas is hydrogenation of adsorbed sulfur education ceravolo the ode, interacting with the catalyst with the formation of sulfides of the metals in the catalyst composition.

The process of sulfatirovnie carried out directly in the catalytic reactor, is associated with corrosion of process equipment, incomplete use of the working volume of the reactor, with continuous time output setup mode.

From patent No. 2102146 (IPC RU701 J 37/04, publ. 20.01.98, Bul) there is a method of Hydrotreating petroleum fractions, performed at a temperature of 250°335°C. the Composition of the used catalyst includes alumina carrier, oxides of boron, molybdenum, Nickel and phosphorus, the catalyst has an index of strength of 2.2-2.5 kg/mm diameter pellets. The implementation of the method provides a degree of desulfurization at a temperature of 335°With level 91,9%, at a temperature of 250° - 75,0%.

The disadvantages of this process lie in the coking of the catalyst, the urgent needs of the hydrogen activation 3-4 times per year in order to restore the activity of the catalyst.

Common features of known and proposed methods is the use of a catalyst containing the oxides of cobalt, molybdenum, aluminum, and modifying connections. Carrying out Hydrotreating process at a high temperature.

From analog (Rchaser, Saginova, Nagbalik, Irracial - Presulfiding is the development of catalysts for Hydrotreating, - "Chemistry and technology of fuels and oils", 1998, No. 6, S. 19-22) there is a method of Hydrotreating petroleum fractions. Known Hydrotreating process straight-run diesel fraction is carried out by contacting the feedstock with presulfiding elemental sulfur aluminoborosilicate the catalyst with a sulfur content of 10% (from the original catalyst). Sulfatirovnie catalyst is carried out at a temperature of 120-180°C, after which the catalyst was cooled in a stream of nitrogen. Activation loaded into the catalytic reactor presulfiding of the catalyst is carried out with hydrogen. The process hydrodesulphurization unit straight-run diesel fraction is carried out at the following process conditions: hydrogen pressure of 3 MPa, the volumetric feed rate to 3 h-1hydrogen: feedstock - 200 m3/m3temperature- 320, 330, 340, 350, 360°C. Straight-run diesel fraction is characterized by the following indicators: density - 843 kg/m3at 20°, fractional composition, °From: Nicholas- 179, 50% - 286, 90% - 360, KK - 367, a sulfur content of 1.2 wt.%.

The conversion of raw materials to 95% at the hydrodesulphurization unit in the presence of presulfiding catalyst reaches at a temperature of 350°C.

The disadvantages of this method are:

the complexity and duration of the manufacturing technology presulfiding elemental sulfur catalyst used in isoimage further in the process of Hydrotreating petroleum fractions,

- the need for a thorough and uniform distribution of elemental sulfur on the layer of catalyst (almost impossible) with the use of manual labor in the manufacture of the catalyst,

- uneven sulfatirovnie processed elemental sulfur catalyst and arising in connection with these issues in further applications,

- accumulation in the catalyst bed of the water and the possibility of violation of the physical integrity of the granules (cracking) and the working of the porous structure of the catalyst.

The closest (prototype) to the claimed method of Hydrotreating petroleum fractions to the technical essence and the achieved result is a method, known from the patent No. 2185242 (IPC RU7B 01 J 37/20, C 10 G 45/08, publ. 20.07.2002). The known method is carried out by contacting the feedstock with presulfiding a catalyst containing cobalt, molybdenum, phosphorus and boron deposited on the aluminum oxide, at elevated temperature and pressure. The process of activating the catalyst includes the processing of elemental sulfur loaded in layers in a quantity of 1.0 to 2.5% by weight of the catalyst, which is heated to 120-140°followed by treatment of the catalyst in hydrogen sulfide-containing gas at a temperature of 150-175°and diesel fuel at a temperature of 250-330°C.

Activation of the catalyst described SPO is abom can improve the mechanical properties of the catalyst and to increase its activity in the processing of heavy crude oil.

The disadvantages of this method are:

- sophisticated technology of activation of the catalyst;

- the use of manual labor, the distribution of elemental sulfur on the layer of catalyst;

- uneven sulfatirovaniu processed elemental sulfur catalyst;

- the need for strict maintenance of the temperature regime throughout the volume and the height of the catalyst layer.

The present invention is to expand the range of methods of Hydrotreating using presulfiding catalysts.

The technical result of the invention consists in:

- simplify the process of Hydrotreating

reducing the duration of the activation of the catalyst,

- decrease the initial temperature of the Hydrotreating process,

- better use of the working volume of the catalytic reactor,

- increase mezhregionalnogo cycle

- preventing corrosion of an industrial reactor.

The claimed technical result in the method of Hydrotreating of petroleum fractions by contacting the feedstock with presulfiding a catalyst containing cobalt, molybdenum, phosphorus and boron deposited on the aluminum oxide, at elevated temperature and pressure reach due to the fact that the process is carried out at a temperature 320-340°C, pressure - 3,0-50 MPa, space velocity of the raw materials 1,0-6,0 h-1& all (hydrogen gas): raw 500-1000 Nov./about. raw materials, in the presence of a catalyst, sulfatirovannah outside of a catalytic reactor with hydrogen sulfide at a temperature of 80-500°and the space velocity of hydrogen sulfide of 0.02 to 6.0 h-1the catalyst further includes an oxide of lanthanum in the following ratio, wt.%:

MoS28,0-of 17.0
Co3S21,5-4,0
P2O52,5-5,0
In2O30.3 to 1.0
La2O31,0-5,0
Aluminium oxidethe rest of it.

On the layer of catalyst is placed 1,0-2,0 m3the for - a protective layer consisting of corundum ring with inner diameter 5 mm

Comparative analysis of the prototype and the claimed invention shows that a common feature of known and proposed methods of Hydrotreating petroleum fractions is the contacting of the feedstock with presulfiding a catalyst containing cobalt, molybdenum, phosphorus and boron deposited on the aluminum oxide, at elevated temperature and pressure.

The difference of the proposed method against known is that the process is carried out at a temperature 320-340° With the pressure - 3.0-5.0 MPa, the space velocity of the raw materials 1,0-6,0 h-1& everything: raw 500-1000 Nov./about. raw materials, in the presence of a catalyst, sulfatirovannah outside of a catalytic reactor with hydrogen sulfide at a temperature of 80-500°and the space velocity of hydrogen sulfide of 0.02 to 6.0 h-1the catalyst further includes an oxide of lanthanum in the following ratio, wt.%:

MoS28,0-of 17.0
Co3S21,5-4,0
P2O52,5-5,0
In2About30.3 to 1.0
La2O31,0-5,0
Aluminium oxidethe rest of it.

On the layer of catalyst is placed 1,0-2,0 m3the for - a protective layer consisting of corundum ring with inner diameter 5 mm

Implementation of the proposed method allows to reduce the duration of activation of the catalyst, to reduce the initial temperature of the Hydrotreating process, better use of the working volume of the catalytic reactor, to increase the period between regenerations, to prevent corrosion of the industrial reactor.

The possibility of implementing the invention is illustrated by the following examples.

Example 1. The manufacturer was pushing the congestion.

The catalyst is prepared by mixing 38,8 kg of aluminum hydroxide bemani patterns from 0.43 kg of boric acid and 1.3 kg nitric acid solution of lanthanum carbonate. The resulting mass is stirred at a temperature of 30°C for 15 minutes. Once smooth add the 1.5 DM325%aqueous ammonia and the mass stirred at 80°C for 20 minutes. Ready weight with a dry matter content of 50% formed into pellets with a diameter of 1.7 mm Molded pellets are dried for 5 hours at a temperature of 120-200°and then calcined at a temperature of 450°C for 5 hours.

At the same time preparing an impregnating solution in a solvent (capacity) pour 25 DM3water, add 1,7 DM3orthophosphoric acid and 5.6 kg of cobalt nitrate with continuous stirring at a temperature of 40°C. To the obtained solution at pH 3.5 load 6.5 kg of paramolybdate ammonium.

Then hold impregnation of the granules of the catalyst compounds active components, which is as follows. In the capacity of the load estimated number obtained as described above catalyst, and then from the dipstick add the estimated amount of the impregnating solution (40°C, pH 3.5)containing cobalt nitrate, paramolybdate of ammonia and phosphoric acid. Saturated compounds active component is in the catalyst is dried at a temperature of 150° C and calcined at a temperature of 450°C.

Get the catalyst in the following ratio, wt.%:

Moo311,0
CoO3,0
P2O33,0
In2About30,5
La2About32,0
Aluminium oxidethe rest of it.

Example 2. Sulfatirovnie catalyst.

Prepared according to example 1, the catalyst was contacted with hydrogen sulfide at ambient pressure outside of the catalytic reactor. Temperature sulfatirovnie support 120°With the entire length of the reactor. Sulfatirovnie operate in periodic mode for 10 hours at a space velocity of hydrogen sulfide 0,05 h-1.

Get presulfiding catalyst in the following ratio, wt.%:

MoS211,2
Co3S23,2
P2O53,0
In2O30,5
La2About32,0
Aluminium oxidethe rest of it.

The catalyst with the contains of 3.9 wt.% sulfur, has an index of strength of 2.2 kg/mm diameter pellets (rate not less than 2.0 kg/mm), the bulk density of 0.7 g/cm3.

Example 3. The process for hydrotreatment of diesel fuel.

Manufactured according to example 2 presulfiding the catalyst having the above described characteristics, experience with the Hydrotreating of diesel fuel. Conditions and results of tests presulfiding of the catalyst are presented in table 1. For comparison and quality control of the data process hydrodesulphurization unit on the catalyst, prepared as described above and solifidianism elemental sulfur. The Hydrotreating process is carried out in a reactor, in which load presulfiding catalyst. On the layer of catalyst is placed 1,0-2,0 m3the for - a protective layer consisting of corundum ring with an inner diameter of 5 mm, the Assignment is for a uniform distribution of consumption of raw materials on the catalyst surface and in the pre-treatment of raw materials. Before feed predominandy catalyst loaded in the catalytic reactor, dried with nitrogen and activate the diesel fuel.

From the table it follows that 84,0-87,0%depth of removal of sulfur compounds in the presence of a catalyst, sulfatirovannah out of the catalytic reactor with a hydrogen sulfide has rolled the political activity at the level of the catalyst sulfatirovannah elemental sulfur. In the case of use in the process of sulfatirovnie sulfurous gas occurs deposition "coke" on the catalyst surface.

Implementation of the proposed method hydrodesulphurization unit oil fractions will reduce the duration of the output setup mode for 2-3 days and reduce corrosion of the process equipment.

1. The method of Hydrotreating of petroleum fractions by contacting the feedstock with presulfiding a catalyst containing cobalt, molybdenum, phosphorus and boron deposited on the aluminum oxide, at elevated temperature and pressure, wherein the process is carried out at a temperature 320-340°C, a pressure of 3.0-5.0 MPa, the space velocity of the raw materials 1,0-6,0 h-1& everything: raw 500-1000 Nov./about. raw materials in the presence of a catalyst, sulfatirovannah outside of a catalytic reactor with hydrogen sulfide at a temperature of 80-500°and the space velocity of hydrogen sulfide of 0.02 to 6.0 h-1the catalyst further includes an oxide of lanthanum in the following ratio, wt.%:

MoS28,0-of 17.0
Co3S21,5-4,0
P2About52,5-5,0
In2O30,3-1,
La2O31,0-5,0
Aluminium oxideRest

2. The method of Hydrotreating petroleum fractions according to claim 1, characterized in that the layer of catalyst is placed 1,0-2,0 m3the for - a protective layer consisting of corundum ring with inner diameter 5 mm



 

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FIELD: petroleum processing.

SUBSTANCE: invention concerns development of catalysts for use in petroleum fraction hydrofining processes. Presulfidized catalyst including alumina-supported cobalt, molybdenum, phosphorus, and boron, active components of which are converted into operational sulfide form using sulfidizing agent, in particular hydrogen sulfide, at sulfidizing temperature 80 to 500°C and hydrogen sulfide volume flow rate 0.02 to 6.00 h-1, catalyst further contains lanthanum oxide. Composition of catalyst is the following, wt %: MoS2 8.0-17.0, Co3S2 1.5-4.0, P2O5 2.5-5.0, B2O3 0.3-1.0, La2O3 1.0-5.0, and alumina - the balance.

EFFECT: simplified catalyst preparation technology without losses in catalytic and mechanical properties.

1 tbl, 3 ex

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