Petroleum fraction hydrofining catalyst preparation

FIELD: petrochemical process catalysts.

SUBSTANCE: invention provides catalyst for hydrofining of petroleum fractions, which catalyst shows elevated strength and stability upon regeneration. This is achieved supplementing alumina-based carrier with texturing additives selected from alumina and gibbsite thermochemical activation product in amount 5 to 30 wt %. Alumina additive is used with particle size not larger than 15 μm and gibbsite thermochemical activation product with that not larger than 45 μm. As binding agent in catalyst, nitric acid is used at molar ratio to alumina (0.01-0.03):1 and/or aluminum nitrate/ aluminum metal reaction product in amounts 1 to 5% based on alumina. Prior to be impregnated, catalyst is steamed at elevated temperature and impregnation is carried out from aqueous solution of nickel-cobalt-molybdenum-containing complex at pH 1-3.

EFFECT: improved performance characteristics of catalyst.

2 cl, 3 tbl, 10 ex

 

The invention relates to methods for producing catalyst for hydrofining petroleum fractions, and in particular to methods of preparation of the catalyst for hydrofining heavy and secondary oil fractions for the purpose of eco-friendly fuels.

One of the reserves to increase the yield of distillate products during the refining is to engage in it products secondary origin, contain a significant amount of unsaturated hydrocarbons, mechanical and other impurities. For processing such materials require catalysts with enhanced life mechanical strength necessary for carrying out multiple regenerations.

Known catalysts that perform a supporting role in the catalytic systems with enhanced durability (Oil and Gas Journal, 1993, V.93, no. 40, p.35-36). The disadvantage of these catalysts is relatively rapid deactivation of catalytic systems when they are used in the Hydrotreating process of medium and heavy petroleum fractions with a high content of unsaturated hydrocarbons and solids and insufficient durability for multiple regenerations.

Known carriers and catalysts, whose mechanical strength is achieved through the figure of the cross-section is three, the quatrefoil, five-, sestito ecna star (EN 2142339 C1, EN 2052288 C1). The production of media of this type is suitable for small-scale or pilot batches.

Closest to the proposed solution to the technical essence and the achieved effect is a method of obtaining alumina catalyst of training materials for the hydrofining of petroleum fractions (EN 2142339 C1), which consists in the impregnation of the support is aluminum oxide, calcined at temperatures below 800°C, aqueous solutions of salts of active ingredients, followed by drying and calcining. The catalyst in this way is used as a protective layer composed of catalytic systems.

The disadvantage of this method (EN 2142339 C1) is to obtain a catalyst with a low level of desulfurization in the processing of heavy petroleum fractions, resulting in the basal layer of the catalyst of the catalytic system comes raw materials with high content of toxogenic components, which leads to its rapid coking.

Furthermore, the method of preparation of the catalyst according to the prototype includes annealing the media at very high temperatures, which is almost impossible for catalyst production.

The aim of the invention is to obtain a solid catalyst with high activity in reactions hydrofining in the processing of heavy petroleum fractions and raw materials, with the unsaturated compound containing a series of.

This objective is achieved in that in the method of producing a catalyst for hydrofining petroleum fractions, including the production of alumina carrier with subsequent impregnation with an aqueous solution of active ingredients in the composition of the carrier injected texturemode additives, carrier before impregnation process steam at elevated temperature and impregnation of lead from aqueous solution of Nickel or cobaltmolybdenum complex at pH=1-3. As texturebrush additives in the carrier injected or alumina with a particle size of not more than 15 μm, in amounts of 5-30 wt.%, or the product of thermochemical activation of gibbsite with a particle size of not more than 45 μm in the amount of 5-30 wt.%, or alumina and the product of thermochemical activation of gibbsite in the total amount of 10-30 wt.%. For unit mass of nitric acid in the ratio of (0.01 to 0.03 mol HNO3):1.0 mol Al2O3and/or the product of the interaction of nitrate and aluminum metal in the amount of 1-5% in terms of Al2O3. The media treated water vapor content of his 40-100% at a temperature of 650-750°C for 2-6 hours. Nickel - or cobaltmolybdenum complex is obtained by introducing an aqueous solution of Nickel (or cobalt and molybdenum or nitric, or phosphoric acid, or hydrogen peroxide, or with whom the combination.

Distinctive features of the present invention is to obtain alumina carrier by adding a hydroxide of eumenia pseudoboehmite patterns texturebrush additives: alumina or product thermochemical activation of gibbsite, PTHA, the introduction of a coupling agent, treatment of the carrier with water vapor at elevated temperatures and the introduction of the active component by impregnation from an aqueous solution of Ni or Co-molybdenum complex at pH 1-3.

Use as a carrier of aluminum oxide with additives of alumina and/ or product thermochemical activation of gibbsite, PDA, as well as the technology of preparation of media, including the introduction of nitric acid in the ratio of (0.01 to 0.03 mol HNO3):1.0 mol Al2About3and/or product of the interaction of nitrate and aluminum metal in the amount of 1-5% in terms of Al2O3the treatment with water vapor, impregnation with an aqueous solution of the complex of active components results in broad porous, strong and active catalyst. High strength provides, first, protecting the catalyst from mechanical damage during operation (transportation, loading, regeneration), that allows to use it for full loading of the reactor, and as a protective layer, and, secondly, it increases the number of regenerations; Shir is the cue pores significantly reduce the formation of cocaethlyene in the processing of raw materials with high content of unsaturated hydrocarbons (including strongly flavored raw materials). The combination of these characteristics allows using the proposed catalyst for the hydrotreatment of the feedstock containing unsaturated compound, over a long period of time with high bulk velocity without loss of activity and increase in pressure drop in the reactor, as well as conduct repeated regeneration.

In known methods for producing catalysts for Hydrotreating processes of oil fractions the application of the described technology is unknown. Therefore, this solution meets the criteria of "novelty" and "significant difference".

The proposed method is illustrated by the following examples.

A list of the materials used.

1. Aluminum hydroxide pseudoboehmite patterns ("cake") with a loss on ignition at 550°SPT=70,08% wt.

2. The alumina containing α-Al2About3up to 92% wt.

3. Product thermochemical activation PDA) three-hydrate of aluminum oxide in the form of gibbsite containing up to 90 wt.%. amalfitano Al2O3.

4. Nitric acid 57%.

5. Nitrate aluminum Al(NO3)3·N2O.

6. Nitrate Nickel Ni(NO3)2·6H2O.

7. Nitric acid With cobalt(NO3)2·6N2O.

8. Ammonium molybdate - pair-(NH4)6Mo7O24·4H2O.

9 Orthophosphoric acid, H 3PO4.

10. Aluminum metal.

11. Hydrogen peroxide 30%.

12. Chemically demineralized water.

Example 1

Stage 1. The preparation of a carrier.

To do this, 1000 g of aluminum hydroxide was heated in a bath to 60°and was kept for 15 minutes. Further added 6 ml of 28% nitric acid: 1 mol Al2O30.01 mol HNO3. Under continuous stirring, the mass is brought to a homogeneous plastic state, sformovat on filiere with a hole diameter of 5 mm, provasoli on the air for 12 hours, dried at 80-120°C for 4 hours, progulivali in air at a temperature of 750°C for 8 hours, treated with water vapor at 750°C for 6 hours.

Stage 2. The preparation of the impregnating solution.

Active components (oxides of Ni or Co and Mo) was introduced by impregnation of the carrier with an aqueous solution of their salts. The volume of solution equal to the pore volume of the carrier (water absorption) +≈10%.

For impregnating 100 g of the carrier having a water absorption of 52.2%, the volume of solution should be ≈60,0 ml. current contents of Moo3is 12-14% wt.; NiO(CoO) - 4÷5% wt.

Solution A. 26 ml of water was heated to a temperature of 60°introduced 19 g of ammonium molybdate, brought before the dissolution, was added to 4.0 ml of hydrogen peroxide (30%), with stirring, was added 1.7 ml of orthophosphoric acid (85%).

Solution B. Separately ol is prepared solution of Nickel nitrate introduction in 4 ml of water 20 g of Nickel nitrate. Solution B was introduced into the solution And mixed. The total amount of impregnating solution was diluted to 60 ml, was mixed. the pH of the solution is 1.8.

The Century solution Separately prepared solution of cobalt nitrate introduction in 4 ml of water 20 g of cobalt nitrate. The solution was introduced into the solution And mixed. The total amount of impregnating solution was diluted to 60 ml, was mixed. the pH of the solution is 2.5.

The solution Was 26 ml of water was heated to a temperature of 60°introduced 19 g of ammonium molybdate, brought before the dissolution, was added to 4.0 ml of hydrogen peroxide (30%).

The solution D. Separately prepared solution of Nickel nitrate introduction in 4 ml of water 20 g of Nickel nitrate was added 4 ml of hydrogen peroxide (30%), mixed and added 1.7 ml of nitric acid (57%). The solution is introduced into the solution G was mixed. The total amount of impregnating solution was diluted to 60 ml, was mixed. the pH of the solution is 1.0.

The solution that is 26 ml of water was heated to a temperature of 60°introduced 19 g of ammonium molybdate, brought before the dissolution, was added to 4.0 ml of hydrogen peroxide (30%), mixed them up and added 2 ml of nitric acid (57%). Solution E was introduced a solution of cobalt nitrate (20 g of cobalt nitrate was dissolved in 4 ml of water)were mixed. The total amount of impregnating solution was diluted to 60 ml, was mixed. The PH of the solution is 1.0.

Stage 3. Cooking can produce the RA.

100.0 g of the carrier prepared according to examples 1-10 table 1, pour a solution of 60 ml, prepared according to examples 1-10 table 2, maintained at a temperature of 40-50°C for 30-40 min while stirring the grains to their homogeneous impregnation, then in a thin layer stand in the air for 12 hours, dried at a temperature of 120°C for 4 hours and calcined at a temperature of 500°C for 10 hours.

The composition of the catalysts and their properties are given in table 2.

Example 2.

Stage 1. The preparation of a carrier.

For this 900 g of aluminum hydroxide was heated in a bath to 60°and was kept for 15 minutes. Further added 30 g (10%) alumina brand CSO with a particle size of 15 μm, was mixed and kept at 60°With, then added 5 ml of 28% nitric acid: 1 mol Al2O30.01 mol HNO3. Under continuous stirring, the mass is brought to a homogeneous plastic state, sformovat on filiere with a hole diameter of 5 mm, provasoli on the air for 12 hours, dried at 80-120°C for 4 hours, progulivali in air at a temperature of 750°C for 8 hours, treated with water vapor at 750°C for 6 hours.

Stage 2. The preparation of the impregnating solution.

Active components (oxides of Ni or Co and Mo) was introduced by impregnation of the carrier with an aqueous solution of their salts. The volume of solution equal what took place to the pore volume of the carrier (water absorption) +≈ 10%.

For impregnating 100 g of the carrier having a water absorption 54.6%of the volume of solution should be ≈60,0 ml. current contents of Moo3is 12-14% wt.; NiO(CoO) - 4÷5% wt.

The method of preparation of the solutions described in example 1, step 2.

Stage 3. The preparation of the catalyst.

100.0 g of the carrier prepared according to examples 1-10 table 1, flooded by 60.0 ml of the solution prepared according to the conditions of example 1, stage 2, held at a temperature of 40-50°C for 30-40 min while stirring the grains to their homogeneous impregnation, then in a thin layer stand in the air for 12 hours, dried at a temperature of 120°C for 4 hours and probalily at a temperature of 500°C for 10 hours.

The composition of the catalysts and their properties are given in table 2.

Example 3

Stage 1(a). Preparation of binder.

In examples 3, 6, 8, 9 as a binder was used, the product of the interaction of aluminum nitrate and aluminum metal (chip). For this purpose, 150 g of aluminum nitrate was dissolved in 500 ml of water and added to 50 g of aluminum shavings. The mixture was heated for 8 hours to a pH of 6-7 hot mass. The reaction formed a gelatinous mass, the content of Al2O3to 98.4 g/l, pH of which after cooling is equal to 5 and used as a binder.

Stage 1. The preparation of a carrier.

For this 950 is GOA was heated in a bath to 60° C and kept for 15 minutes. Further added 15 g (5%) alumina brand CSO, mixed, stood at 60°C for 15 minutes, then added 5 ml of nitric acid (28%) and 150 ml (15 g/l Al2O3) binder, obtained as described above (stage 1A). Under continuous stirring, the mass is brought to a homogeneous plastic state, sformovat on filiere with a hole diameter of 5 mm, was pravalivai 12 hours, dried at 120°C for 4 hours, progulivali at 750°C for 8 hours, treated with 100%steam at 750°C for 6 hours.

Stage 2. The preparation of the impregnating solution.

Active components (oxides of Ni or Co and Mo) was introduced by impregnation of the carrier with an aqueous solution of their salts. The volume of solution equal to the pore volume of the carrier (water absorption) +≈10%.

For impregnating 100 g of the carrier having a water absorption of 50%, the volume of solution should be ≈60,0 ml. current contents of Moo3is 12-14% wt.; NiO(CoO) - 4÷5% wt.

The formulation of the solutions described in example 1, step 2.

Stage 3. The preparation of the catalyst.

100.0 g of the carrier prepared according to examples 1-10 table 1, pour 60 ml of the solution prepared according to the conditions of example 1, stage 2, is maintained at a temperature of 40-50°C for 30-40 min while stirring the grains to their homogeneous impregnation, then in a thin layer withstand newsdude 12 hours, dried at a temperature of 120°C for 4 hours and calcined at a temperature of 500°C for 10 hours.

Technology of preparation of sample No. 4 is similar to model No. 2, change the percentage and particle size texturise supplements.

Example 5.

Stage 1. The preparation of a carrier.

For this 900 g of aluminum hydroxide was heated in a bath to 60°and was kept for 15 minutes. Further added 60 g (30%) product THA gibbsite with a particle size of 25 μm, were mixed and kept at 60°With, then added 15 ml of 28% nitric acid: 1 mol Al2About30.03 mol HNO3. Under continuous stirring, the mass is brought to a homogeneous plastic state, sformovat on filiere with a hole diameter of 5 mm, provasoli on the air for 12 hours, dried at 80-120°C for 4 hours, progulivali in air at a temperature of 750°C for 8 hours, treated with water vapor at 750°C for 6 hours.

Stage 2.

Active components (oxides of Ni or Co and Mo) was introduced by impregnation of the carrier with an aqueous solution of their salts. The volume of solution equal to the pore volume of the carrier (water absorption) +≈10%.

For impregnating 100 g of the carrier having a water absorption of 50%, the volume of solution should be ≈60,0 ml. current contents of Moo3is 12-14% wt.; NiO(CoO) - 4÷5% wt.

Recipe solutions are given in PR is as 1, stage 2.

Stage 3. The preparation of the catalyst.

100.0 g of the carrier prepared according to examples 1-10 table 1, pour 60 ml of the solution prepared according to the conditions of example 1, stage 2, is maintained at a temperature of 40-50°C for 30-40 min while stirring the grains to their homogeneous impregnation, then in a thin layer stand in the air for 12 hours, dried at a temperature of 120°C for 4 hours and calcined at a temperature of 500°C for 10 hours.

The composition of the catalysts and their properties are given in table 2.

Technology sample preparation media No. 4, 7, 10 similar technologies for sample No. 2, and No. 6, 8, 9 similar to sample No. 3 in table 1. However varied the particle size, the ratio texturebrush additives, the ratio of binder agents, steam treatment conditions.

Conditions of preparation of the media with the introduction of texturebrush additives, a binder agent and a steam treatment and their properties are shown in table 1.

For samples 1-10 (table 1) and 1-10 (table 3) were determined by the mechanical strength of the division, water absorption, bulk density, and conducted tests on catalytic activity.

The mechanical strength of the division was determined by procedure PC-2-1 .0.

When carrying out catalytic tests in the quality of raw material used mixed diesel fraction 180-360°With sulphur 0,99% wt.

And the tests were carried out on pilot plant with a total volume of the reactor 50 cm 3at the following process parameters: temperature - 360°S, the pressure at the inlet to the reactor 3,5 MPa volumetric feed rate 3 h-1.

The catalytic activity of the catalyst was evaluated by the residual sulfur content in the hydrogenation product.

The results are shown in table. 1 and table. 2.

It is seen that the samples of the catalysts made in accordance with the formula of the invention (using texturebrush additives, manufacturing technology), are far superior in strength and catalytic activity of the selected prototype.

The stability of the catalysts for the regeneration of the proposed method was evaluated by the change in strength after processing 100%steam at a temperature of 600°C for 2, 4, 6 hours. From the results shown in the table. 3, it is seen that the strength loss during steam treatment of the proposed catalysts insignificant, in contrast to the prototype.

Table 3
The strength of the catalyst after steam treatment.
CatalystThe strength factor, kg/mm
Before steamingAfter steaming 2 the Asa After steaming for 4 hoursAfter steaming for 6 hours
No. 2the 3.82,82,62,5
No. 66,05,35,14,8
No. 103,72,62,62,5
The prototype S2,62,42,11,6

1. A method of producing a catalyst for hydrofining petroleum fractions, including the production of alumina carrier with subsequent impregnation with an aqueous solution of active ingredients, characterized in that the carrier is injected texturemode additives, prior to impregnation of the carrier is treated with water vapor at an elevated temperature, the impregnation of lead from aqueous solution of Nickel/cobaltmolybdenum complex at pH 1÷3, at the same time as texturise additives in the carrier injected alumina with a particle size of not more than 15 μm, in an amount of 5÷30 wt.%, or the product of thermochemical activation of gibbsite with a particle size of not more than 45 μm in an amount of 5÷30 wt.%, or alumina and the product of thermochemical activation of gibbsite in the total quantity 5÷30 wt.%; upon receipt alumina media for unit weight, nitric acid volnam ratio [0,01÷ 0,03]:1,0 Al2About3and/or the product of the interaction of nitrate and aluminum metal in an amount 1,0÷5.0% in terms of Al2About3.

2. The method according to claim 1, characterized in that the medium is treated with water vapor content of his 40÷100% at a temperature of 650-750°C for 2÷6 o'clock



 

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