The preparation method of catalyst for hydrotreating petroleum fractions

 

(57) Abstract:

The inventive product - catalyst (CT) composition, %: Nickel oxide 3; molybdenum oxide 9; phosphorus oxide 1,5; alumina rest. CT is obtained by impregnation at a pH of 1.5 to 3.5 pre-calcined alumina with a solution of salts of Nickel and molybdenum in the presence of phosphoric acid, followed by drying and calcining the resulting catalyst mass. At the same time as aluminum oxide is used, the oxide obtained by heat treatment of three-hydrate of aluminum with a particle size of 0.04 to 0.1 mm in a drum rotating oven at 350 - 500°C for 15-180 min with subsequent hydration of the amorphous product at pH 5.0-5.5 and a temperature of 75-90°C, plasticization in an autoclave at 140-300°C for 3-6 h, molding, drying, and calcination. Feature: high catalytic activity. table 1.

The invention relates to the refining, in particular to methods for preparing catalysts for use in hydrogenation processes for the purpose of Hydrotreating petroleum fractions.

Known method of preparing a catalyst for Hydrotreating, which used the main bearer of soosazhdenie Cilicia aluminol and silicasol in such proportions as to get in the media, Al2O3: SiO2= (1.5 to 30): 1. The resulting carrier is dried at 100-215aboutC. Alumosilicate mixed with 5-50 wt.% (20-40 wt.%) inorganic oxide (ZrO2, But2or B2O3). The obtained dry mixture is impregnated with a solution of B-compounds and phosphates so that the phosphate content of boron was 13-35%. Further, the carrier is dried and impregnated with a solution of salts of Nickel and molybdenum. Then again dried and calcined at 700-1200aboutC. the Method can be illustrated as follows. Water glass diluted with water, acidified with hydrochloric acid, diluted with water and mixed with an aqueous solution of Al2(SO4)3. Then to the mixture was added a concentrated solution of NH4OH, diluted with water and at pH=9,4 precipitated hydrogel. It is filtered off and washed with water to remove ions of Na+, SO4-and NH4+. The hydrogel repulping in an aqueous solution of phosphoric and boric acid. Reformirovanie carried out at 70aboutWith, then the precipitate is dried at 120aboutWith, pulverized and passed through sieve 10-30 mesh. The resulting powder was impregnated with a solution containing molybdenum acid and Nickel nitrate in an aqueous solution of ammonia. The impregnated particles is Phnom weight of 0.31 g/ml (1).

The disadvantage of this method is that the preparation of a carrier - alumosilicates through aluminol and silicasol complicated by the use of dilute solutions of salts, acids, additional filtering and washing to remove sodium ions, sulfate ions and ammonium ions. Required treatment and recycling of wastewater.

There is a method of preparation of the catalyst gasoline fractions, in which the catalyst was prepared by precipitation of Al(OH)3from solutions of sodium aluminate and nitric acid (2-2,4) with the following ageing sludge (1.5-2 h), forming, drying, calcination. Then are impregnated with solutions of molybdenum ammonium and nitrate of cobalt or Nickel with subsequent drying and calcination. The precipitation of Al(OH)3lead in three stages, i.e. first periodically change the pH of the medium 7-12, then the pH of the medium is maintained at the level of 10.5-11 and further to 8.8 and 9.3 (2).

The disadvantage of this method is that during the precipitation of aluminum hydroxide formed in the lavage large number of salts that are not amenable to recycling and, therefore, was discharged into the sewer. The impregnation of the support is carried out in two stages: first, a solution of molybdenum ammonium and then nitrate cobalt (Nickel) which includes - the deposition of an aqueous solution of one or more aluminum salts in water-ethanol solution (15-50% CH3OH, C2H5OH, a mixture of CH3OH and C2H5OH) phosphorus-containing compounds (0,6-0,3 mol of phosphorus on IM/Al) in the regulation of the pH from 5.5 to 10, keeping the sediment at 20-90aboutWith over 15 min at a pH of 9-12, sediment washing, mixing the precipitate with a solution containing soluble salts of heavy metals (Mo, W, a mixture of Mo and W) and metals Ni or Co (or a mixture of Ni and Co) at pH 4 to 8 and a temperature of 20-90aboutWith, separation, drying and calcining the product at 300-900aboutFor the preparation of the catalyst. The resulting catalyst has SID>300 m2/g and 20% of the total pore volume of pores with a diameter of >150 10-1m (3). The disadvantage of this method is the complexity of technical solutions and a large number of sewage.

The closest known solution of an analogous problem to the technical essence and the achieved effect is a method of preparation of the catalyst according to the invention, in which the catalyst is prepared by impregnation of the pre-calcined alumina with a solution of salts of hydrogenating metals VIB and VIII of the group (including the salts of Mo and Ni) in the presence of P-containing acids, including H3PO3l2O3with a specific surface area 20-350 m2/, the Catalyst was dried at 25-200aboutC, then heated in an inert (N2, He, Ar, Kr, Xe or a mixture) to 200-600aboutC. the Catalyst has the following chemical composition, wt.%: Ni 0,2-10, Mo 0.2 To 20; P Is 0.2-10. The catalysts were tested in the Hydrotreating of gas oil at a temperature of 315-343aboutC, a pressure of 56 MPa, the space velocity of the raw material - 1.5 h-1. The degree of desulfurization is 92%.

The aim of the invention is to obtain a catalyst with high catalytic activity. This goal is achieved by a method of preparing a catalyst for Hydrotreating petroleum fractions by pre-impregnation of the calcined alumina with a solution of salts of Nickel and molybdenum in the presence of phosphoric acid, followed by drying and calcination, in which the aluminum oxide is used, the oxide obtained by heat treatment of three-hydrate of aluminum with a particle size of 0.04 to 0.1 mm in rotating drum furnace at 350-500aboutFor 15-180 min with subsequent hydration of the amorphous product at pH=5-5,5 and 75-90aboutWith plasticization in an autoclave at 140-300aboutC for 3-6 h and the impregnation is carried out at a pH of 1.5 to 3.5. The process of obtaining aluminum hydroxide leads to a. the Noi by the cap almost perfectly mixes with the combustion gases. Application for thermal processing of a rotating drum furnace decides the question of entering into the zone of high temperature powder hydrargillite, good contact with the coolant and increases performance up to 250-300 kg/h of the Physico-chemical nature of the process consists in simultaneously running processes disordering of the crystal structure, dehydration and dispersion due to the high heating rate of the particles of three-hydrate of aluminum. The product of the process is amalfitani aluminium oxide with qualitatively new properties, in particular, the ability to swell in acid environment with formation of precipitation of hydrated alumina having plasticity and ability to be molded into pellets.

The selected mode is selected in such a way that the resulting aluminum oxide by chemical and x-ray composition is virtually no different from the aluminum oxide produced industrially resultant deposition rates. At the same time, differs from the existing industrial technology lack of consumption of acid and alkali, sharp reductions in runoff, reducing the number of process steps. Samples of media Hydrotreating catalysts on the basis of the obtained SUP>/g) average pore 40-50 40-50 .

The inventive method differs from the known fact that aluminum oxide is used, the oxide obtained by heat treatment of three-hydrate of aluminum with a particle size of 0.04 to 0.1 mm in rotating drum furnace at 350-500aboutFor 15-180 min with subsequent hydration of the amorphous product at pH=5-5,5 and 75-90aboutWith plasticization in an autoclave at 140-300aboutC for 3-6 h, molding, drying and calcination and impregnation is carried out at pH=1.5 to 3.5.

Thus, the inventive method of preparing a catalyst for Hydrotreating petroleum fractions meets the criteria of the invention of "novelty."

In the known method (4) of the Hydrotreating catalyst is prepared by impregnation of a pre-calcined alumina with a specific surface area 20-350 m2/,

Aluminum oxide is impregnated with a solution prepared by the sequential dissolution of salts hydrogenating metals in water in the presence of phosphorus-containing compounds (H3PO3H3PO4or their mixture) with pre-vacuum medium. The catalytic composition is dried at 25-200aboutC and calcined in an inert atmosphere (N2, He, Ar, Kr, Xe or a mixture thereof), built by impregnation of alumina with a solution of salts of Nickel nitrate and molybdenum ammonium in the presence of phosphoric acid (H3PO4) was tested in the process of Hydrotreating gas oil with S=1.5% at T=343aboutWith P=56 MPa, Vc= 1.5 h-1. The residual content of sulfur compounds in the product amounted to 0.12% (calcining the catalyst in an inert environment) and 0.13% (calcination in air (degree of desulfurization respectively 92 and 91.3%).

The proposed method for the preparation of the catalyst produces a catalyst in the process of Hydrotreating of vacuum gas oil with S=1.5% at a temperature of 360aboutC, a pressure of 40 MPa, the space velocity of the raw material - 1.5 h-1clears the feedstock to a residual content of sulfur compounds 0,08-0,11 (degree of desulfurization of 93.5-95%).

Higher catalytic activity compared to the prototype associated with the use of specially prepared aluminum oxide in terms of the proposed method, which provides a carrier with a highly developed surface 250-280 m2/g with an average pore volume of 0.6-0.7 cm3/g, an average pore 40-5040-50 , bulk weight of 0.6-0.65 m2/g with a high strength factor of 2.4-2.5 kg/mm Gran. In addition, the carrier impregnated with a solution of hydrogenating metals in the presence of phosphoric acid with exorbitant pH results in lower Cameron particles of 0.04-0,056 mm serves drum in the rotary kiln at a speed of 250 kg/h At the same time in the drum serves flue gases with a temperature of 600aboutC. While rotating the drum at a speed of 5 rpm is almost perfect offset three-hydrate with the coolant. Heat treatment of three-hydrate of aluminum occurs in a rotating drum furnace having a Z-shaped nozzle, when the contact temperature 350aboutWith over 180 minutes Get x-ray amorphous aluminum oxide. Loss on ignition after thermal treatment of the powder to 4.0%. Then prepare a suspension of alumina in water at a ratio of T:W=1:4 and spend the hydration of aluminum oxide at pH=5.0 and a temperature of 75aboutC for 2 h After hydration product is placed in the autoclave and the temperature is 140aboutC and stirring for 3 h hold plasticization. After the end of the process, the suspension is diluted with demineralized water, mix thoroughly and serve to filter. 400 g of aluminum hydroxide formed into pellets, dried at 150aboutS, 6 h, calcined at 550aboutC, 4 h at the same time preparing an impregnating solution. To 100 ml of water add 2 ml of 85% phosphoric acid and dissolved 19 g of molybdenum ammonium under stirring and heated to 90aboutWith, then add 17 g of Nickel nitrate, stirred until complete dissolution solution. The catalyst was dried at 110aboutS, 6 h, calcined at 550aboutC, 4 o'clock the Finished catalyst has the following chemical composition, wt. %: NiO 3,0; MoO39,0; P2O51,5; Al2O3the rest of it.

P R I m m e R 2. The three-hydrate powder of aluminum with a particle size 0,056-0,100 mm served in a drum oven, rotating at 20 rpm is Mixed with flue gases having a temperature of 800aboutC. the Heat-treated powder of the three-hydrate of aluminium is carried out at a temperature of 500aboutC for 15 minutes Receive x-ray amorphous alumina powder with a specific surface area SID= m2/year of Loss during annealing temperature after processing alumina powder 7%, average pore volume, Vn=0.7 cm3/t, the average radius of the pores Rcf=50 Rcf= 50 . Then spend the hydration of the amorphous product at pH=5,5, temperature 90aboutWith that plasticization is carried out in an autoclave at a temperature of 300aboutWith stirring for 6 hours, the Suspension of aluminum hydroxide in water after thorough mixing serves to filter. Then 373 g of aluminum hydroxide formed into pellets, dried at a temperature of 150aboutS, 6 h, calcined at a temperature of 550about4 h, after which the impregnated Gras the date of ammonium and 12 g of Nickel nitrate in the presence of 2.5 ml of phosphoric acid at pH 3.5. The catalyst was dried and calcined as in example 1.

P R I m e R 3. Raw materials - aluminium trihydrate is mixed with flue gases, heated to 675aboutWith and contact in a rotary kiln with a speed of 12.5 rpm Trihydrate of aluminum with a particle size of 0.04 to 0.1 mm is served in the oven at a rate of 25 kg/h Heat treatment of three-hydrate of aluminium is carried out at a temperature of 425aboutWith over 97,5 minutes Get x-ray amorphous aluminum oxide with a specific surface area S=280 m2/year of Loss during annealing temperature after processing alumina powder 6.5%, an average pore volume and 0.68 cm3/g, average pore - 48 of 48 . Hydration of the amorphous product is carried out at a pH of 5.25 and a temperature of 82aboutC. Then a suspension of aluminum oxide is placed in an autoclave and spend plasticization at a temperature of 220aboutWith over 4.5 hours, the Suspension is filtered, the precipitate formed into pellets, dried and calcined. The pellets are placed in an impregnating solution with a pH of 2.5 to full absorption. Then the pellets are dried and calcined as in example 1.

P R I m e R 4 (comparative). The catalyst prepared according to example 1, except that the heat treatment of three-hydrate of aluminium is carried out in a drum rotating furnace with a particle size of 0.04 mm. While watching p is e R 5 (comparative). The catalyst prepared according to example 1, only the active alumina receive, using as feedstock a trihydrate of aluminum with a particle size of 0.1 mm. Receive the finished product with the worst quality indicators: x-ray amorphous powder with 20% of boehmite, i.e., incomplete decomposition of the original product.

P R I m e R 6 (comparative). The catalyst prepared according to example 1, except that the heat treatment of three-hydrate of aluminium is carried out at a temperature of 300aboutWith over 200 minutes Get x-ray amorphous product with 30% of boehmite.

P R I m e R 7 (comparative). The catalyst prepared according to example 1, except that the heat treatment of the original three-hydrate of aluminium is carried out at 550aboutC for 10 minutes Get x-ray amorphous product with 10% boehmite.

P R I m e R 8 (comparative). The catalyst prepared according to example 1, except that the hydration of the amorphous product at pH 4.5 and a temperature of 70aboutC.

P R I m e R 9 (comparative). The catalyst prepared according to example 1, except that the hydration of the amorphous product at pH=6.0 and a temperature of 95aboutC.

P R I m e R 10 (comparative). The catalyst prepared according to example 1, except that the plasticization of hydrated product is carried out at a temperature of 120aboutWith over 7 hours

ukta is carried out at a temperature of 320aboutC for 2 h

P R I m e R 12 (comparative). The catalyst prepared according to example 1, except that the impregnation of the granules of alumina carried out by hydrogenating a solution of salts of metals in the presence of phosphoric acid at a pH of 1.2.

P R I m e p 13 (comparative). The catalyst prepared according to example 1, except that the impregnation of the granules of alumina carried out by hydrogenating a solution of salts of metals in the presence of phosphoric acid at pH=4,0.

From the above examples (1-13) and the prototype can be seen that using the proposed method of preparation of the catalyst Hydrotreating allows to obtain a catalyst with a higher catalytic activity compared to the prototype. In the Hydrotreating of vacuum gas oil at 360aboutC, P=40 MPa, Vwith=1.5 h-1in the presence of a catalyst prepared according to examples 1-3 of the present invention, the degree of removal of sulfur compounds comprises 93.5-95%. The catalyst of the prototype at T=343aboutWith P=56 MPa, Vc=1.5 h-1the degree of sulfur removal of 91.3%.

In addition, the use of the proposed method of preparation of the catalyst Hydrotreating compared with the existing industrial technology, including the preparation of alumina way soosai what I obtain aluminum hydroxide is a very handy instrument (drum rotary kiln), with the help of which the question of entering and good contact of the powder hydrargillite with the coolant. Turning hydrargillite - cheap and affordable product in the active aluminum hydroxide carry out a quick, incomplete dehydration of hydrated alumina in a turbulent flow of the flue gases at a temperature of 350-500aboutWith in which the residual water content is 4-7%, specific surface 280-300 m3/, Hydrated alumina is sprayed into the hot gas stream. The amount of product in the gas stream is relatively high. The output of the unit 250-300 kg/h To increase catalytic activity leads impregnation in the presence of phosphate (H3PO4) acid at a pH of 1.5 to 3.5. All beyond pH lead to lower activity (12, 13) and strength (AP. 13).

Thus, the combination of the proposed methods of the prepared catalysts for Hydrotreating petroleum fractions allows you to:

to increase the catalytic activity of the catalysts;

to simplify the technology of preparation by creating almost a reagent-free and environmentally friendly technologies for the media and the introduction of the hydrogenating metals methods of impregnation in one step by creamasia furnace, which allows an almost perfect mixture of three-hydrate of aluminum with flue gases. The data given in the table. In the instant of contact receive the product quality. In the production of active alumina industrial way (deposition method) is formed of more than 3 tons per 1 ton of produced products of salts, which are not amenable to recycling and discharged into the sewer.

The PREPARATION METHOD of CATALYST FOR HYDROTREATING PETROLEUM FRACTIONS by pre-impregnation of the calcined alumina with a solution of salts of Nickel and molybdenum in the presence of phosphoric acid, followed by drying and calcining the resulting catalyst mass, characterized in that aluminum oxide is used, the oxide obtained by heat treatment of three-hydrate of aluminum with lower particle 0,04 - 0,10 mm drum in a rotating oven at 350 - 500oWith over 15 - 180 min with subsequent hydration of the amorphous product at pH 5.0 - 5.5 and 75 - 90oWith plasticization in an autoclave at 140 - 300oC for 3 - 6 h, molding, drying and calcination and impregnation is carried out at a pH of 1.5 to 3.5.

 

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6 cl, 1 tbl, 8 ex

FIELD: chemistry.

SUBSTANCE: invention is referred to the area of hydrocarbons preparation by catalytical hydrodeoxygenation of products of fast pyrolysis of a biomass and working out of the catalyst for this process. The catalyst of oxygen-organic products hydrodeoxygenation of fast pyrolysis of lignocellulose biomasses, containing either precious metal in amount of no more 5.0 wt % or containing nickel, or copper; either iron, or their combination in a non-sulphide restored shape in amount of not more than 40 wt % and transitive metals in a non-sulphide shape in amount of not more than 40 wt %, carrying agent - the rest, is described. Three variants of the catalyst preparation method, providing application of transition metals on the carrying agent by a method of impregnation of the carrying agent solutions of metal compounds are described, or simultaneous sedimentation of hydroxides or carbonates of transition metals in the presence of the stabilising carrier, or the catalyst is formed by joint alloying/decomposition of crystalline hydrate nitrates of transition metals together with stabilising components of zirconium nitrate type. The process of oxygen-organic products hydrodeoxygenation of a biomass fast pyrolysis is performed using the above described catalyst in one stage at pressure of hydrogen less than 3.0 MPa, temperature 250-320°C.

EFFECT: increase stability in processing processes of oxygen-containing organic raw materials with the low content of sulphur, and also soft conditions of process realisation.

10 cl, 12 ex, 2 tbl

FIELD: chemistry.

SUBSTANCE: invention relates to composition based on gold and reducible oxide, method of its production and its application as catalyst, in particular in carbon monoxide oxidation. Described is composition based on gold on carrier based on reducible oxide, as such composition contains titanium or iron (III) oxide, content of halogen in composition, expressed by molar ratio halogen/gold, constitutes not more than 0.05, content of gold in it constitutes not more than 1%, gold is in form of particles with size not more than 10nm, and composition is subjected to reducing processing. Described is method of composition production, which contains following stages: bringing in contact compound based on reducible titanium or iron (III) oxide and compound based on gold halogenated and, in case of necessity, compound based on silver, with formation of suspension of said compounds, pH of obtained medium being set not lower than 8; separation of solid substance from reaction medium; washing solid substance with alkaline solution; in addition method includes reducing processing after mentioned above washing stage. Described is method of carbon monoxide oxidation, method of air purification and method of cigarette smoke purification using described above composition as catalyst.

EFFECT: elaboration of catalysts, efficient at low temperatures and/or high hour volume rates.

16 cl, 12 tbl, 15 ex

FIELD: chemistry.

SUBSTANCE: invention relates to production of catalysts and can be used in chemical industry and in production of medications. Described is method of preparing modified platinum catalyst for enantioselective hydration of esters of alfa-ketacarboxylic acids which includes impregnation of hexachloroplatinic acid from solution into pores of prepared carrier, as such supersewn polystyrene is used, by water-absorbing capacity from solution tetrahydrofurane : methanol : water with ratio 4:1:1, mixture of hexachlorplatinic acid and carrier is kept during 10-15 minutes mixed, after which it is dried at 70-75°C, washed with Na2CO3 solution with further reduction of hexachlorplatinic acid, filtering, washing and drying of catalyst and modification with cinchonidine solution.

EFFECT: reduction of time of catalyst preparation, increase of catalyst activity, enentioselectivity and stability.

4 cl, 1 tbl, 3 ex

FIELD: chemistry.

SUBSTANCE: catalyst for selective hydrogenation of organic compounds contains mesoporous carbon carrier and active part - nanodispersed particles of the VIII group metals with content on the carrier in the range from 1 to 10%. The method for catalyst preparation includes the thermochemical treatment of the carrier, its impregnation with the solution containing active part, and then the metals of VIII group are reduced at first in the alkaline media at ultrasonic action with frequency 35 kHz, then with formaldehyde solution.

EFFECT: enhancing of catalyst activity.

6 cl, 5 dwg, 7 ex

FIELD: chemistry.

SUBSTANCE: method of Fischer Tropsch synthesis of hydrocarbons includes the stage of carbon monoxide and hydrogen mixture interreaction in presence of catalyst in the form of particles containing homogenous mixture of cobalt and aluminium compounds at atomic ratio cobalt/aluminium in the range from 10:1 to 2:1 which after reducing at 425°C has cobalt surface area measured with hydrogen chemosorption at 150°C at least 30 m2 per 1 g of catalyst. The catalyst preparation includes the stages: (i) of precipitation of unsoluble cobalt compound from water cobalt salt solution with excess of alkali precipitator; (ii) adding of soluble aluminium compound; (iii) aging of obtained precipitate in suspended form; (iv) extracting and drying of catalyst composition; (v) catalyst activation by its reducing with hydrogen-containing gas.

EFFECT: catalysts obtaining with high cobalt content and high cobalt surface area used for hydrogenating of unsaturated compounds in Fischer Tropsch synthesis.

15 cl, 4 ex, 10 tbl

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