The catalyst for hydroconversion hydrocarbons, method thereof and method of hydroconversion hydrocarbons

 

(57) Abstract:

The catalyst for use in hydroconversion processes comprises platinum supported on a carrier dioxide flint - aluminum trioxide, which was obtained from amorphous material dioxide flint - trioxide aluminum, having a pore volume of at least 1.0 ml/g, was impregnated with platinum by using a process, which consists in bringing into contact of the medium with a salt of platinum in the presence of fluid in the acidic conditions of the environment. The method of obtaining this catalyst comprises receiving the media from the amorphous dioxide flint - trioxide aluminum, having a pore volume of at least 1.0 ml/g and impregnation prepared in such media, bringing the carrier into contact with the platinum salt in the presence of fluid in the acidic conditions of the environment. The catalyst has a General application in hydroconversion processes, but shows high activity and selectivity in obtaining oils with hydroconversion of hydrocarbons obtained by the Fischer-Tropsch process. 4 S. p. 11 C.p. f-crystals.

The invention relates to a catalyst that is used in hydroconversion processes, mainly the catalyst for use in obtaining Godunov, produced through the Fischer-Tropsch process.

The preparation of hydrocarbons from a gaseous mixture comprising carbon monoxide and hydrogen, by bringing the above-mentioned mixture in contact with a suitable catalyst at elevated temperatures and pressures, the process is well known in the art as the Fischer-Tropsch process.

Recently, great attention has been paid to the processes of obtaining gasoil fuels. These processes include two stages: the first stage in which the hydrocarbons with high temperature limits of the boil-off is prepared from a mixture of carbon monoxide and hydrogen using the Fischer-Tropsch process, and a second stage in which the hydrocarbons obtained by the method, is subjected to hydroconversion, leading to the formation of essential oils.

For the present description, the term "gas oil" should be understood as a hydrocarbon or mixture of hydrocarbons having a boiling temperature, or temperature limits boiling, largely responsible kerosene and gas oil fractions obtained in the course of traditional distillation of crude oil under atmospheric pressure. In a typical distillation process of crude oil consistently highlighted CL is 220oC, one or more of the kerosene fraction with their boiling temperature from 140 to 300oC and one or more gas oil fraction with their boiling temperature of 180 to 370oC.

So, the published patent application UK N 2 007 289 (GB-A-2-077 289) and published applications for Europatent N 0 127 220 and N 147 873 (EP-A-0 127 220 and EP-A-0 147 873) reveal the process of obtaining oils, in which a mixture of carbon monoxide and hydrogen into a first stage in carbohydrates with a high temperature beyond the boiling using the Fischer-Tropsch process, and these hydrocarbons are then subjected to catalytic hydroconversion. In the descriptions of these patent applications revealed a number of possible compositions of catalysts for use in hydroconversion stage process, with preference being given in each case, the catalyst comprising as a catalytically active component, a metal of Group VIII in a suitable carrier. Particular preference is given to catalysts containing platinum. As disclosed in GB-A-2 289 077, suitable carriers are amorphous oxides of elements of groups II, III and IV of the Periodic system of elements, such as silicon dioxide, aluminum trioxide, magnesium oxide, zirconium dioxide as well as CIS Zirconia and zeolite materials such as mordenite and faujasite. Believe that the aluminum trioxide and silicon dioxide trioxide aluminum are the preferred materials carriers.

In the descriptions of all applications GB-A-2 289 077, EP-A-0 127 220 and EP-A-0 147 873, in particular in the example below we use hydroconversion stage of obtaining gas oil platinum/silicon dioxide trioxide aluminum catalyst, comprising of 0.82 wt.h platinum per 100 wt.h media, and the media consists of 14.6 wt. trioxide aluminum and 85,4 wt. silicon dioxide.

In processes where it is necessary to produce oils with high yields of hydrocarbons with a high temperature beyond the boiling obtained by the Fischer-Tropsch process required hydroconversion catalyst, which has both a high level of internal activity in combination with high selectivity towards gasoline.

Platinum/silicon dioxide trioxide aluminum catalysts known in the art as catalysts used in the process of hydroconversion various hydrocarbon products. For example, in UK patent No. 1 617 451 (GB 1 451 617) disclosed is a method of obtaining medical oils, in which the second temperature and pressure with a catalyst, comprising one or more noble metals of group VIII on a carrier, which contains 13 15 wt. trioxide aluminum, and the rest is silicon dioxide. The catalysts which in particular are cited as example in GB 1 617 451 include platinum, deposited on a silicon dioxide trioxide aluminum carriers having a surface area in the range of 110 to 518 m2/g and a pore volume in the range from 0.34 to 0.87 ml/g Catalyst was obtained by impregnation of the material of the carrier with an aqueous solution chloroplatinic acid.

It is now established that the mentioned catalysts described and shown as an example in GB 1 617 451, suitable for use in the process of hydroconversion hydrocarbons with high temperature limits boiling, obtained by the Fischer-Tropsch process, as a means of obtaining oils.

However, it was unexpectedly discovered a novel composition of catalyst which is active as a catalyst hydroconversion. In particular, they had found a new composition of the catalysts, which when used in hydroconversion of hydrocarbons obtained by the Fischer-Tropsch process, the most profitable shows simultaneously as visokio the present invention provides for the creation of a catalyst, comprising platinum deposited on a silica - aluminum trioxide medium; this medium was obtained from amorphous material is silicon dioxide trioxide aluminum, having a pore volume at mere,0 ml/g, and the carrier was impregnated with platinum by using a method comprising bringing into contact of the medium with a salt of platinum in the presence of fluid in the acidic conditions of the environment.

The new catalyst can be used in hydroconversion processes. The term "'ve got a hydro conversion" is used here in its broadest sense as a symbol of transformation processes occurring in the presence of hydrogen and covering a range of stiffness modes, for example, hydrocracking to mild hydrogenation processes.

A carrier for a catalyst according to the invention is an amorphous silicon dioxide trioxide aluminum. The term "amorphous" refers to the absence of a crystal structure determined by x-ray diffraction in material media, although some of the local order can be present. Amorphous silicon dioxide trioxide aluminum, suitable for use in obtaining catalyst, commercially available. Otherwise, the silicon dioxide is blowing drying and firing the obtained material, as described in GB 1 617 451.

The catalyst may include any amorphous silica - aluminum trioxide. Preferably, the amorphous silica - aluminum trioxide contained trioxide in a quantity lying in the range from 5 to 30 wt. more preferably from 10 to 20 wt. and particularly preferably from 12 to 15 wt.

To achieve a high degree of selectivity of the catalyst gas oil, it is important that the pore volume of the amorphous starting material of the silicon dioxide trioxide aluminum was at least 1.0 ml/g For this description all values of pore volume, expressed with respect to the catalyst according to the invention relate to the pore volume, measured by a method comprising the water absorption pores of the material, often referred to as the method of initial moisture; however, the pore volume is usually referred to as pore volume (H2O).

A typical method of determining pore size (H2O) catalyst or material media includes the following operations: drying the material at a temperature of approximately 500oC; weighing the dried material; immersing the material in water for a period of approximately 15 minutes; removing material from the water; removing water from the surface of the material using centrif the decayed material and the weight of water-soaked material.

Preferably, the pore volume of the amorphous material is silicon dioxide - aluminum trioxide were in the range of 1.0 to 2.0 ml/g, more preferably from 1.0 to 1.5 ml/g

In addition to silicon dioxide trioxide aluminum carrier may also contain one or more binders. Suitable binder materials include inorganic oxides. Can be used as the amorphous and crystalline binder material. Examples of binder materials include silicon dioxide, aluminum trioxide, clay, magnesium oxide, titanium dioxide, zirconium dioxide and mixtures thereof. Preferred binder materials are silicon dioxide and trioxide aluminum, and aluminum trioxide is particularly preferred. Binder material, if it is included in the catalyst composition, preferably in an amount of 5 to 50 wt. more preferably from 15 to 30 wt. with respect to the total weight of the carrier.

The catalyst according to the invention includes platinum as a catalytically active component. Preferably, platinum is present in a quantity lying in the range from 0.05 to 5.0 wt. more preferably from 0.1 to 2.0 wt. especially predpochtitel the using the impregnation process, in which the carrier is in contact with the platinum salt in the presence of fluid in the acidic conditions of the environment. It is advisable that the PH of the acidic environment was not above 4.0, more preferably not more than 3.0.

It is most convenient to choose platinum and liquid so that the salt was soluble in the liquid, and the media to bring into contact with a solution of platinum salt. Suitable liquids for use in the impregnation may be organic, such as alcohols and ethers, and inorganic, for example, water. Water is the most convenient and particularly preferred for use.

You can use any suitable salt of platinum, and preference is given to salts, soluble in the selected fluid. Suitable salts include both organic and inorganic salts. Examples of suitable salts include dibromide platinum dichloride, platinum, trichloride platinum, platinum tetrachloride, dichlorocarbanilide platinum, tetraploid platinum and platinum sulfate.

The preferred catalyst is a catalyst prepared by impregnation using a solution of acid salts of platinum, and the platinum salt is simultaneously the source of platinum and provides the necessary conditions of acidity. Site acid, hexahydroxybenzene acid, platinum monohydrochloride acid and platinum (III) sulphuric acid. Especially preferred for use as the acid salt of platinum hexachloroplatinic acid.

If the acid salt of platinum is not used in the impregnation of the support, the impregnation is carried out in the presence of additional acid. More preferably, as an acidic salt of platinum and additional acid is present in the impregnation process of the media. Suitable for use in the impregnation acids include both organic and inorganic acids, such as mono - and dicarboxylic acid, hydrochloric acid, sulfuric acid and nitric acid. Especially preferred is nitric acid. The most preferred catalyst is obtained by impregnation of the support using a combination hexachloroplatinic acid and nitric acid.

If the catalyst according to the invention obtained by the impregnation in the presence of acid salts of platinum and additional acid, it is advisable that additional acid is present in excess amount of acid salts of platinum, and the molar ratio of acidic salts of platinum predpochtitel the peculiarity is that, the invention provides for the development of the method of preparation of the catalyst, as described above; the method comprising the preparation of a carrier made of amorphous silicon dioxide trioxide aluminum, having a pore volume of at least 1.0 ml/g, and the impregnation thus obtained carrier platinum by bringing into contact of the carrier and platinum salts in the presence of fluid in the acidic conditions of the environment.

The media can be obtained from amorphous silicon dioxide trioxide aluminum by methods known to experts in this field of technology. The preferred method of receiving media includes the preparation of a paste of a mixture of amorphous silicon dioxide trioxide aluminum and a suitable acid, extruding the mixture and drying the obtained extrudates.

The mixture for extrusion should preferably have a solids content ranging from 20 to 60 wt.

Liquid for introduction into the composition of the mixture can be any suitable fluid known in the art. Examples of suitable liquids include water, alcohols such as methanol, ethanol and propanol; ketones such as acetone and aldehydes such as acrolein and aromatic liquids such as tolua extrudate, in the mixture it is advisable to include peptization. Suitable baptistery this acidic compounds, for example, inorganic acid such as aqueous solutions of hydrogen fluoride, hydrogen bromide, hydrogen chloride, nitric acid, nitrous acid and perchloric acid. Preferably, peptization was organic acid, for example, mono - or dicarboxylic acid. For the preferred organic acids include acetic acid, propionic acid and butane acid. Acetic acid is the most preferred peptizing.

The number of patinator included in the mixture should be sufficient to completely particiapate trioxide aluminum present in the material of the carrier, and can easily be determined using the pH of the mixture. During grinding the pH of the mixture should preferably be in the range from 1 to 6, most preferably from 4 to 6.

In order to improve the rheological properties of the mixture, prior to extrusion, it is advisable to include one or more additive to improve the rheological properties and/or accelerators extrusion. Suitable additives for inclusion in the mixture of fatty amines, Quaternary ammonium compounds, aliphatic monocarboxylic cycloturbine aromatic compounds, acyclic monocarboxylic acids, fatty acids, sulfonated aromatic compounds, sulfates of alcohols, sulfates, ethers, alcohols, sulfated fats and oils, salt, phosphonic acid, polyoxyethylene the bonds alkylamines, polyoxyethylene alkylamide, polyacrylamides, polyhydric alcohols, acetylene glycols. Preferred for use supplements are sold under the trademarks "Nalko and Superfloc".

It is advisable to additives for improving the rheological properties/accelerators extrusion, was present in the mixture in a total quantity ranging from 1 to 20 wt. more preferably from 2 to 10 wt. with respect to the total weight of the mixture.

In principle, the components of the mixture can be mixed in any order, and the mixture was subjected to grinding. It is preferable to mix the silicon dioxide trioxide aluminum and binder, if present, and then to ground mixture. After that add fluid, if present, peptization and the resulting mixture is subjected to further grinding. Finally, add any of improving the rheological properties of the additive/accelerators extrusion that you want to include, and the resulting mixture is subjected to grinding for the last time.

Typically, a mixture of PR is to mix the chopping device. The rate of supply of energy in the mixture is typically from 0.05 to 50 W/min/kg, preferably from 0.5 to 10 W/min/kg, the grinding Process can be carried out in a wide temperature range, preferably from 15 to 50oC. the energy input into the mixture during the grinding process there is an increase in the temperature of the mixture during grinding. The grinding process is conveniently carried out at ambient pressure. You can use the device available for sale.

After the grinding process is complete, the mixture is extruded. The extrusion can be carried out using any known commercially available extruder. In particular, you can use the extruder worm type for forcing the mixture through the capillaries in a suitable intermediate plate to obtain extrudates necessary forms. Strands, formed after extrusion can be cut into pieces of the required length.

The extrudates may be of any suitable form known in this technical field, for example, cylindrical, hollow cylindrical, multi-leaf or twisted multi-leaf. The preferred form of the catalyst particles according to the invention is cylindrical. Typically, the extrudates are nomi who may be at elevated temperature, preferably up to 800oC, more preferably up to 300oC. the drying Period is typically up to 5 h, preferably from 30 minutes to 3 hours

The extrudates after drying, it is advisable to be fired. The firing is carried out at elevated temperature, preferably up to 1000oC, more preferably from 200 to 1000oC, most preferably from 300 to 800oC. Calcination of the catalyst is carried out, as a rule, during the period of time up to 5 h, preferably 30 min to 4 h

After preparation, the medium is subjected to impregnation process in which the carrier is applied platinum. The impregnation is performed by bringing the carrier into contact with the platinum salt in the presence of fluid in the acidic conditions as described above. The carrier can be brought into contact with a platinum salt immersion in the liquid in which the salt is suspended, or more preferably dissolved.

The preferred method of impregnation for use in the method according to the invention, the method of impregnation of the pore volume, when the carrier is in contact with a platinum salt solution, and the solution is present in sufficient amount to substantially zapolnitel solution.

After impregnation the catalyst is advisable to undergo drying and firing. Drying conditions in the kiln, such as described above.

The catalyst according to the invention is active as a catalyst hydroconversion and can be used in such processes as the hydroisomerization of alkanes and hydrocracking. However, as noted, the catalyst is particularly active in selective hydroconversion hydrocarbons with a high temperature beyond the boiling to obtain a gas oil, mainly in hydroconversion products with high temperature limits boiling, obtained by the Fischer-Tropsch process.

In the Fischer-Tropsch process, the gaseous mixture comprising carbon monoxide and hydrogen in contact with a suitable catalyst at elevated temperature and pressure, giving the hydrocarbons. Preferably, the used catalyst includes a metal from the iron group of group VIII of the Periodic system of elements as catalytically active component, optionally in combination with one or more promoters. The most suitable catalyst for the Fischer-Tropsch process comprises cobalt as the catalytically active component, silicon dioxide, titanium dioxide, zirconium dioxide or mixtures thereof.

The hydrocarbon products of the Fischer-Tropsch process with a high temperature beyond the boiling can then be brought into contact with the catalyst in accordance with the invention in the presence of hydrogen and subjecting them to catalytic hydroconversion obtaining the necessary oils. Typical conditions the way for the implementation stage of hydroconversion: temperature from 175 to 400oC, preferably from 250 to 375oC; hourly space velocity of gaseous hydrogen from 100 to 10000 Mol l/l/h, preferably from 500 to 5000 Mol l/l/h; the partial pressure of hydrogen of from 10 to 250 bar, preferably from 25 to 150 bar, a space velocity from 0.1 to 5 kg/l/h, preferably from 0.25 to 2 kg/l/h; the ratio of hydrogen to oil of from 100 to 5000 Mall/kg, preferably from 250 to 2500 Mall/kg

Typical processes that can be applied to the catalyst in accordance with the present invention, are disclosed in GB-A-2 289 077, EP-A-0 127 220 and EP-A-0 147 873.

The invention is described below using the following illustrative example.

Example.

1) preparation of the catalyst. A mixture comprising amorphous silicon dioxide trioxide aluminum (from "gray "Criterion catalyst To. 554,8 g) were placed in a grinding device and milled for 10 minutes was Added acetic acid (10 wt. an aqueous solution of 200.0 g) and water (2190,3 g), the mixture was milled for 10 minutes then added polyacrylamide ("Superfloc And 1839", 2 wt. aqueous solution; 40,0 g) and the grinding was continued for another 10 minutes Finally added polyelectrolyte ("Nalko", 4 wt. aqueous solution; 80,0 g) and the mixture was milled in the last 5 minutes

The resulting mixture was extrudible using the extruder of 2.25 "bonnet", through the cylindrical intermediate plate, receiving cylindrical extrudates with a diameter of 1.7 mm, the resulting extrudates were dried at a temperature of 120oC for 2 h and then annealed at a temperature of 600oC for 2 h

Prepared an aqueous solution containing hexachloroplatinic acid (H2PtCl6, of 2.45 wt.) and nitric acid (7,66 wt.), having a pH below 1. Cylindrical particles of the carrier was impregnated with this aqueous solution, by the method of impregnation of the pores with obtaining the result of the content of platinum on the carrier 0,8 wt. Impregnated therefore, the carrier particles were annealed at a temperature of 500oC for 1 h to obtain the finished catalyst.

2) the Process of the Fischer-Tropsch synthesis. Using Cinta cobalt (18.3 wt. present in the form of cobalt oxide), Zirconia (8.5 wt. present in the form of zirconium oxide) and silica was loaded into the reactor with a fixed catalyst bed. The catalyst is brought into contact with a mixture of carbon monoxide and hydrogen with a molar ratio of carbon monoxide to hydrogen 1,1, served with hourly volumetric velocity of the gas from 1120 to 1130 Mol/l/h at a pressure of 36 bar and a temperature of from 210 to 225oC. was obtained with a high-boiling paraffin, from which was selected fraction with temperature limits boiling 370+oC.

3) the Receipt of gas oil. The catalyst obtained in Ref. 1, used to obtain the oils've got a hydro conversion fraction 370 +oC high-boiling paraffin obtained by the Fischer-Tropsch process for POS. 2 in the text above. Used testing technique was following.

A sample of the catalyst obtained in Ref. 1 was placed in a reactor with a fixed bed. The catalyst is brought into contact with 370 +oC the fraction of high-boiling paraffin and hydrogen with an hourly flow rate of hydrogen gas of 1000 Moll/l/h and time the volume-weighted velocity paraffin 1.25 kg/l/h and at a pressure of 30 bar. The temperature was set at 340oC for the Oia reactor eluent, having a temperature within a boiling range from 220 to 370oC. When the conversion of 60 wt. the catalyst showed selectivity to gas oil 50 wt.

d) alkane Hydroisomerization. The catalyst obtained in Ref. 1, was tested as a catalyst hydroisomerization alkanes, taking as a typical testing ISO-C7compounds from n-heptane. The test method was as follows: a sample of the catalyst obtained in Ref. 1, was loaded into the reactor. The catalyst is brought into contact with the supplied mixture containing n-heptane and hydrogen in a molar ratio of hydrogen to n-heptane 4:0, time when the volume-weighted rate of 1.0 kg/l/h, at a pressure of 30 bar and a temperature of 340oC. Was registered conversion of n-heptane in the number of 54.3 wt. c selectivity to ISO-C7connections 93,0 wt.

1. The catalyst for hydroconversion hydrocarbons containing platinum supported on a carrier of silica-alumina, characterized in that the medium is obtained from amorphous silica-alumina having a pore volume of at least 1.0 mg/g, and impregnated with a solution of platinum salt in the acidic conditions of the environment.

2. The catalyst p. 1, wherein the amorphous oxide credit is isator on PP.1 and 2, characterized in that the amorphous silica alumina has a pore volume of 1.0 to 2.0 mg/g, preferably 1.0 to 1.5 mg/g

4. The catalyst PP.1 to 3, characterized in that the binder material medium contains a material selected from the group comprising silicon dioxide, aluminum oxide, clay, titanium dioxide, zirconium dioxide or a mixture thereof, preferably alumina.

5. The catalyst p. 4, characterized in that the medium contains a binder in an amount of 5 to 50 wt. preferably 15 to 30 wt. in relation to the mass media.

6. The catalyst PP.1 to 5, characterized in that it contains platinum in the amount of 0.5 to 5 wt. preferably 0.2 to 1 wt.

7. The preparation method of catalyst for hydroconversion hydrocarbons, comprising receiving the media from the amorphous silica-alumina, the carrier impregnated with platinum compound and heat treatment, characterized in that the carrier is produced from amorphous silica-alumina having a pore volume of at least 1.0 mg/g, and the impregnated carrier carried by contact with a solution of platinum salt in the acidic conditions of the environment.

8. The method according to p. 7, characterized in that the contacting noisome, dicarboxylic acid, hydrochloric acid, nitric acid, preferably nitric acid.

9. The method according to PP.7 and 8, characterized in that the contacting is carried out at the pH of the medium is not more than 4.0, preferably not more than 3.0.

10. The method according to p. 7, characterized in that as a platinum salt using salt selected from the group comprising hexachloroplatinum acid, tetracyanoplatinate acid, hexahydroxybenzene acid, salt monohydrochloride acid, preferably hexachloroplatinum acid.

11. The method according to p. 7, wherein the receiving medium is carried out by grinding a mixture containing amorphous silicon dioxide, aluminum oxide and liquid, extruding the mixture and drying the obtained extrudates.

12. The method according to p. 7, characterized in that the mixture contains peptizer, preferably acetic acid.

13. The method according to PP.7 to 12, characterized in that the pH of the mixture before extrusion from 1 to 6, preferably from 4 to 6.

14. The method according to PP.7, 10 to 13, characterized in that the carrier before the impregnated calcined at a temperature up to 1000oC, preferably from 200 to 1000oS, more preferably from 300 to 800oC.

15. How hydroconversion l from silicon dioxide and aluminum oxide, in the presence of hydrogen, wherein the used catalyst, a carrier which is obtained from the amorphous silica-alumina having a pore volume of at least 1.0 mg/g, and the carrier is impregnated with a solution of platinum salt in the acidic conditions of the environment.

 

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