The method of pre-sulphurization of the catalyst, the catalyst obtained by this method, and a method of converting hydrocarbon material

 

(57) Abstract:

The invention relates to a method of pre-sulphurization of catalysts for conversion of hydrocarbons. Describes how pre-sulphurization of porous catalyst particles containing at least one metal or metal oxide, comprising a stage of impregnation of the catalyst with a solution containing ions of inorganic polysulfides of the General formula S(x)2- where X is an integer having a value of at least 3, to obtain a catalyst in which the introduced sulfur and in which at least part of the sulphide or sulphur introduced into the pores of the catalyst and heating the catalyst introduced with sulfur in the presence of non-oxidizing gas selected from the group consisting of nitrogen, carbon dioxide, argon, helium and mixtures thereof. Also describes the catalyst obtained by this method, and a method of converting hydrocarbon starting material in the presence of the above catalyst. 3 s and 5 C.p. f-crystals, 2 tab.

The present invention relates to a method of pre-sulfurylase or prior acarnania catalysts for conversion of hydrocarbons.

It is well known that it is often desirable to use of certain catalysts, used for cleaning and/or hydroconversion hydrocarbons, either before initial use, i.e. fresh catalysts, or after they were used again after regeneration. Catalytic conversion of hydrocarbons, such as hydrobromide, hydrocracking and catalytic processing of residual gases is usually subjected to such preliminary acarnania" (preliminary sulfatirovaniu).

The catalyst hydrobromide is any catalytic composition, which can be used to catalyze the hydrogenation of hydrocarbons, and in particular the hydrogenation of certain components of the raw materials, such as organic compounds containing sulfur, nitrogen and metals, as well as unsaturated hydrocarbons. The hydrocracking catalyst is any catalyst composition, which can be used for cracking large and complex molecules derived from oil, with the aim to obtain molecules of smaller size with concomitant addition of hydrogen to molecules. The catalyst for residual gases is any catalytic composition, which can be used to catalyze the conversion of harmful exhaust gases into less harmful products, and in particular, CT sulfur. The recovered catalyst is any catalyst composition, which contains the metal in a reduced form, such as, for example, catalytic hydrogenation of olefins. These metals usually recover with the help of a reducing agent, such as, for example, hydrogen or formic acid. Metals such recovered catalyst can be fully restored or partially restored.

Catalyst composition for hydrogenation catalysts are well known and some of them are produced by the industry. Usually the active phase of the catalyst based on at least one metal of groups VIII, VIB, IVB, IIB, IB of the Periodic table. In General, the hydrogenation catalysts contain at least one element selected from the group Pt, Pd, Ru, Ir, Rh, Os, Fe, Co, Ni, Cu, Mo, W, Ni, Hg, Hell or Au, on the carrier, such as alumina, silica, silica-alumina carrier and carbon.

Catalytic composition for hydrobromide and/or hydrocracking or processing of residual gases are well known, and some of them are produced by the industry. Catalysts based on metal oxides, which fall under this definition, including the media, which are alumina, silica, silica-alumina carrier, including zeolite. For these purposes it is possible to use catalysts containing other transition metals. In General, the catalysts containing at least one element selected from V, CR, Mn, Re, Co, Ni, Cu, Zn, Mo, W, Rh, Ru, Os, Ir, Pd, Pt, Ag, Au, Cd, Sn, Sb, Bi, Te, suitable for these purposes.

To maximize the effectiveness of these catalysts based on metal oxides convert at least partially in the sulphides of the metals. Catalysts based on metal oxides can eternity (sulfuriodine) in the reactor by contact at elevated temperatures with hydrogen sulfide or sulfur-containing oil or source material (in situ).

However, users want to be catalysts based on metal oxides containing or sulfur, or a sulfur in the form of organic sulfur compounds included in the catalyst. These pre-sulfurized catalysts can be loaded into the reactor and to bring conditions in the reactor to the reaction conditions in the presence of hydrogen, causing the sulfur or sulfur compounds to interact with hydrogen and a metal oxide, converting them into sulfides without additional is be many dangers, such as Flammability and toxicity, with which the operators of facilities are faced when using hydrogen sulfide, liquid sulfides, organic polysulfides and/or mercaptans to acarnania catalysts.

There are several ways of pre-acarnania catalysts based on metal oxides. Preliminary acarnania catalysts hydrobromide carried out by introduction of sulfur compounds in porous catalyst before hydrobromide hydrocarbon source material. For example, in U.S. patent 4530917 described by way of preliminary acarnania catalyst hydrobromide organic polysulfides. In U.S. patent 4177136 described by way of preliminary acarnania catalyst by treating the catalyst elemental sulfur. After that used hydrogen as a reducing agent to convert the elemental sulfur to hydrogen sulfide. In U.S. patent 4089930 described pre-treatment of the catalyst elemental sulfur in the presence of hydrogen. In U.S. patent 4943547 described by way of preliminary acarnania catalyst hydrobromide by sublimirovanny elemental sulfur in the pores of the catalyst, followed by heating in privorot hydrogen. Published PCT application W0 93/02793 discloses a method of pre-acarnania catalyst, when elemental sulfur is introduced into the porous catalyst and simultaneously or sequentially perform processing of the catalyst liquid olefinic hydrocarbon.

However, these pre-sulfurized ex-situ catalysts must be activated first before their contact with the hydrocarbon feedstock in a reactor for processing hydrocarbons.

Therefore, the present invention is to obtain activated pre-sulfurized or sulfatirovaniu catalyst, either fresh or regenerated without the need for separate processing by activating before the contacting of the catalyst with the hydrocarbon starting material in the reactor.

In accordance with the present invention, a method of pre sulfurylase porous catalyst particles, subject to acarnania containing at least one metal oxide, in which carry out the following:

(a) impregnorium the catalyst with a solution of inorganic polysulfides to obtain a catalyst in which the introduced sulfur and in which at MPa, in the atmosphere causes oxidation.

The present invention further discloses a pre-sulfurized catalyst, which can be obtained by the method according to the invention.

In the text of the present description, the term "inorganic polysulfide" refers to polysulfide ions of General formula(x)2-where x is an integer more than 2, i.e., x is an integer having a value of at least 3, preferably from 3 to 9, from 3 to 5, and refers to "inorganic" compounds, i.e., the inorganic is the nature of polysulfide fragment, and not the counterion, which can be organic. In the text of the present description, the term "solution of inorganic polysulfides" refers to a solution containing inorganic polysulfides. In this description, the terms "catalysts containing metal(s), oxide(s) metals, sulfide(s) of metals" include the precursors of catalysts, which are used as these catalysts. Hereinafter, the term "metal(s)" includes the metal(s) in a partially oxidized form. The term "oxide(s) of metals" includes metal oxides in a partially restored. The term "sulfide(s) of metals" vuoksenmaa terms include partially other components such as carbides, borides, nitrides, oxyhalides, alkoxides and the alcoholate.

In the present invention pre-sulfurized (sulfirovanie) catalysts containing metals or metal oxides, impregnorium solution of inorganic polysulfides for the preliminary acarnania be UserMenu-based catalyst metal or metal oxide at a temperature and for a time sufficient to enter the sulfide or sulfur into the pores of the catalyst. The catalyst is heated for subsequent application in conditions that do not cause oxidation, over a period of time sufficient to sulfide or sulfur joined to the catalyst.

Catalysts, which are here spoken of as "subject to acarnania catalysts based on metal oxide" may represent the precursors of catalysts, which are used as the true catalysts, sulfurized form, and not in the form of oxide. Because the methods of preparation of the present invention can be applied to the regenerated catalyst, which may be a metal sulfide, is not completely converted to oxide, the term "subject to acarnania catalysts on the basis of the om.

In the preferred embodiment of the invention before application of the solution of inorganic polysulfides particles or beads of a catalyst containing a metal or a metal oxide, hydronaut to equilibrium with air condition, to restore the initial esotericist.

When implementing the method according to the present invention, the porous particles of the catalyst are in contact and interact with a solution of inorganic polysulfides in conditions which cause the inclusion of sulfide or sulfur compounds in the pores of the catalyst in the process of impregnation. Catalysts, which are introduced inorganic polysulfides or sulfur compounds, will be referred to as "catalysts, which are introduced sera.

A solution of inorganic polysulfides are usually obtained by dissolving elemental sulfur in an aqueous solution of ammonium sulfide (or a derivative of ammonia, i.e., Tetramethylammonium, tetraethylammonium, and so on). Preferred polysulfides include inorganic polysulfides of the General formula S(x)2-where x is an integer more than 2, i.e., x is an integer having a value of at least 3, preferably from 3 to 9, from 3 to 5, is to>A solution of inorganic polysulfides is a red liquid, in which the dark color means long-chain polysulfide, and the lighter color means short-chain polysulfide. The thus obtained solution of inorganic polysulfides used to impregnate catalyst particles, using the method of impregnating the pore size, or by the initial wetting, so that the pores of the catalyst are filled without exceeding the volume of the catalyst. The amount of sulfur used in the method according to the invention will depend on the number present in the catalyst of the catalytic metal, which must be converted to the sulfide. For example, for a catalyst containing molybdenum, will require two moles of sulfur or monosemantic compounds in order to convert each mole of molybdenum in molybdenum disulfide, and a similar relation is valid for other metals. In the case of regenerated catalysts, the sulfur levels can be taken into account when calculating the required quantities of sulfur.

The amount of sulfur is usually present in a solution of inorganic polysulfides in the method according to the present invention is in the range is the concentration of the original solution of ammonium sulfide. A solution of inorganic polysulfides will usually have a ratio of sulfur to sulfide by weight in the range from 2:1 to 5:1, preferably in the range from 2:1 to 3:1. The amount of sulfur in the solution of inorganic polysulfides are usually such that the amount of sulphur impregnated in the catalyst particles, is typically an amount sufficient to provide a stoichiometric conversion of the metal components of the oxide in the form of sulphides, and is typically in the range from 2 to 15 wt.%, preferably from 4 to 12 wt.% from the total mass of sulfurized catalyst.

It was found that the addition of sulfur to pre acarnania in amounts up to about 50% of the stoichiometric requirements will give catalysts with adequate hydrodenitrification activity, which is an important property of the catalysts for hydrobromide and the first stage hydrocracking. Thus, the amount of sulfur for pre-acarnania used to introduce the catalyst is usually in the range from 0.2 to 1.5 times the stoichiometric amount, and preferably from 0.4 to 1.2 times the stoichiometric amount.

For catalysts for hydrobromide/hydrocare is more acarnania is usually from 1 to 15 wt.% from the mass loading of the catalyst, and preferably, the amount of sulfur for pre-acarnania should be from 4 to 12 wt. % by weight loading of the catalyst.

Phase sulfur impregnation is usually carried out at a temperature in the range from 0 to 30oWith or above 60oC. the Lower temperature limit is limited by the freezing point of a solution of inorganic polysulfides in certain conditions of impregnation, while the upper temperature limit is limited by the decomposition temperature of the solution of inorganic polysulfides to volatile compounds and elemental sulfur.

After impregnation the catalyst particles with a solution of inorganic polysulfides, the catalyst, which introduced the sulfur is subjected to heat treatment in the presence of a stream of non-oxidizing gas, such as nitrogen, carbon dioxide, argon, helium and mixtures thereof, at a temperature sufficient to bring most of the water remaining in the pores, and to bind the sulfur on the catalyst. Heat treatment of the catalyst, which introduced the sulfur, it is preferable to carry out when using the method of the ramp, during which the catalyst, which introduced the sulfur is first heated to temperate the catalyst is heated to the final temperature in the range from 120 to 400oC, preferably from 230 to 350oWith to bind the sulfur on the catalyst. After such heat treatment, the catalyst was cooled down to room temperature (to ambient temperature) and are registraciyu water saturated with gas, without causing oxidation. The catalyst is stable in the air.

Pre sulfatirovaniu or pre-sulfurized catalyst according to the present invention can then load, for example, in the reactor for hydrobromide and/or hydrocracking, or in a reactor for processing of residual gases, the reactor is heated to the working temperature (for example, temperature hydrobromide and/or hydrocracking or processing of residual gas) and then immediately perform the contact of the catalyst with a hydrocarbon source material, without prolonged activation of the catalyst with hydrogen prior to contact of the catalyst with the hydrocarbon starting material. Not tying himself to a certain theory, we assume that the phase of prolonged activated hydrogen, which were required for catalysts, advanced acarnania which produced outside the reactor, is not necessary for catalysts, advanced acarnania who was reagirovali with metal or metal oxides prior to the formation of sulfides of metals, or Vice versa, sulfur bound in the pores of the catalyst to such an extent that it does not leave the pores of the catalyst to convert the sulfide.

The method according to the present invention is applicable to acarnania used catalyst which has been regenerated with oxygen. After the usual regeneration with oxygen, the catalyst can be pre-usernet as fresh catalyst, as described above.

The method according to the invention is best suited for catalysts for hydrobromide and/or hydrocracking or processing of residual gas. These catalysts usually contain metals of group VIB and/or group VIII on a porous carrier such as alumina, silica, silica-alumina carrier and zeolites. These materials are well known and can be obtained by methods described, for example, in U.S. patent 4530911 and U.S. patent 4520128. Preferred catalysts for hydrobromide and/or hydrocracking, or processing of residual gases will contain a metal of group VIB, selected from molybdenum, tungsten and mixtures thereof, and the metal of group VIII selected from Nickel, cobalt and mixtures thereof and deposited on the alumina. Commonly used catalysts hydrobromide and/or hydrocracking, which ablaye catalysts on a carrier of aluminum oxide. Widely used catalyst for the treatment of residual gases, which shows high activity in various conditions in the reactor, is cobaltmolybdenum catalyst on aluminum oxide.

The method of pre-acarnania ex-situ according to the present invention allows faster to bring to the operating status of the conditions in the reactors for hydrobromide, hydrocracking and/or processing of residual gases, since it provides direct contact with the hydrocarbon starting material in the reactor and removes long stage activated hydrogen, which is required in the usual preliminary asemanii catalysts ex-situ.

Thus the present invention provides a method of converting hydrocarbon source material (i.e., a method of converting hydrocarbons), during which contact the source material with hydrogen at elevated temperature in the presence of pre-sulfurized catalyst of the present invention.

Conditions hydrobromide include a temperature in the range of 100oWith up to 425oC and a pressure of 40 atmospheres (4,05 MPa). The total pressure will usually be in the range from 400 to 2500 psig (skorosti supply of hydrogen will generally be in the range of from 200 to 10,000 standard cubic feet per barrel (SCF/BBL") (5663,38 DM3to 283169 DM3on 0,158987 m3). Feeding is usually done with an average hourly velocity in the range from 0.1 to 15.

The hydrocracking conditions include a temperature in the range of 200oWith up to 500oC and a pressure of 40 atmospheres (4,05 MPa). The total pressure is usually in the range from 400 to 3000 psig (2.76 to 20,68 MPa). The partial pressure of hydrogen is usually in the range from 300 to 2600 psig (2,07-17,93 MPa). The feed rate of hydrogen is usually in the range from 1000 to 10,000 standard cubic feet per barrel (SCF/BBL") (5663,38 DM3to 283169 DM3on 0,158987 m3). Feeding is usually done with an average hourly velocity in the range from 0.1 to 15. Installation for the first stage hydrocracking, which carry out a significant part of hydrobromide source material, can operate at higher temperatures than plants for hydrobromide and at higher temperatures than the setup for the second stage hydrocracking.

Hydrocarbon source material being hydrobromide or hydrocracking the method according to the present invention can have various boiling point. This includes light fractions, so zeuli, beastality, "long" and "short" remains subjected to catalytic cracking cycle oils, gas oils are subjected to thermal or catalytic cracking, synthetic crude oil, which can be obtained from tar Sands, shale oil residues from mineral processing or raw materials from biomass. Can also be used various combinations of hydrocarbons.

Reactors for treatment of residual gases typically operate at temperatures in the range of 200oWith up to 400oC and at atmospheric pressure (101.3 kPa). About 0.5-5% vol. fed into the reactor residual gases will represent a hydrogen. Standard average hourly feed rate of the residual gas through the reactor are in the range of from 500 to 10000 h-1. There are several ways in which you can activate the catalysts through which the processing gas in the reactor. To activate the catalyst, you can use the Claus plant for the source material or residual gas. Additional hydrogen, if required, you can enter by means of a gas burner, which substochiometric relation to produce hydrogen.

Further nastoya solution of inorganic polysulfides

A solution of inorganic polysulfides for use in the following examples was obtained by adding 42 grams of elemental sulfur in a vigorously stirred solution of ammonium sulfide (150 ml, 22 wt.%). Elemental sulfur immediately began to dissolve, and the resulting solution became red-orange. The mixture was stirred until then, until it all dissolved sulfur. The actual content of sulfur in the solution amounted to 30 wt.%, and the ratio of sulfur to sulfide in the solution was 3.0.

Example 1

Commercially available catalyst hydrobromide having the following properties was used for the preparation of pre-sulfurized catalysts.

Table a catalyst properties

Nickel, wt.% - 3,0

Molybdenum, wt.% - 13,0

Phosphorus, wt.% - 3,5

Media - Gamma alumina

Surface area, m2/g - 162

Pore volume of water, CC/g - 0,47

Size - 1/16 inch (1,5875 mm) three-petal

A sample of 50 g of the above catalyst was hydrational to equilibrium with air. The hydrated catalyst was then impregnable 28,0 milliliters of the above solution of inorganic polysulfides. This solution by injection of use in nitrogen purged (0.5 liters/minute) 300 mm 3N round bottom flask. The tripod, which is fixed to the flask, subjected to vibration when using the vibrator, the amplitude of vibration that is installed in such a way as to create allowany layer of beads of catalyst. Received black beads were then heated from room temperature to 121o(250oF.) for one hour. Then the catalyst was brought to a final temperature of 260o(500oF.) and held for one hour. The final sulfur level was 9.3% of the total weight of the catalyst. Conducted analysis of sulfur content in the catalyst using serouglerode analyzer SC-432 company LECO. Properties of the catalyst are given in table. 1.

Comparative example AND

The catalyst hydrobromide, commercially available and described in Example 1 were subjected to the following procedure acarnania in place.

A sample of the catalyst was ground and sieved on a sieve 14-45 mesh were loaded into the device for testing, pressure sulfiding gas (5% H2S/95% H2) which was 1 atmosphere and a flow rate of 45 liters/hour. Then the temperature was raised from room temperature to 204oWith a rate of 0.5oWith in a minute and maintained this temperature for two hours. Then is their hours, and then cooled to room temperature. After that the installation was switched on, the flow of pure hydrogen and set the desired speed and pressure, and then began feeding hydrocarbon starting material. The final sulfur level was 8.8% of the total weight of the catalyst. The sulfur content in the catalyst was determined using serouglerode analyzer SC-432 company LECO. Properties of the catalyst are given in table. 1 .

The catalyst test

Sulfurized catalyst of Example 1 was used for hydrobromide heavy gas oil is subjected to catalytic cracking in the reactor drip-flow type. A sample of the catalyst was ground and sieved through a sieve 16-45 mesh, diluted with silicon carbide and loaded into the reactor drip-flow type. The reactor was created pressure to 1100 psi (7.6 MPa) using a stream of hydrogen flowing at a speed of 45 liters per hour. Then the reactor was heated to 93oWith the heavy gas oil is subjected to catalytic cracking, was passed over the catalyst with an average hourly velocity of the fluid supply 1.5. The temperature was raised at a rate of 0.5oWith an hour to 332oC, and then maintained for six hours. After that, the samples collect points and comparison with results of Comparative example A.

Comparative example a was tested as in Example 1, except that because it was produced acarnania catalyst in situ, the catalyst was unloaded from the reactor after acarnania.

The results are shown in table.1.

As can be seen from the table. 1, the method of pre-acarnania of the present invention, in which the solution is applied inorganic polysulfides, is an effective means of introducing sulfur in the catalyst of the hydraulic control treatment (IPF Example 1).

Example 2

The catalyst hydrocracking Z-763 Ni-W/Ultrastable Y, manufactured by Zeolyst International Inc., subjected to preliminary acarnania as described below.

a 100 g sample of the above catalyst was gidratirovana to equilibrium with air. Hydrogenated catalyst was then impregnable 23.4 ml of the above solution of inorganic polysulfides, diluted to volume of water in the pores 38.6 ml. This solution drop by drop was added to the mixed layer of the catalyst, which represented the balls that are in nitrogen purged (0.5 liters/minute) 300 mm 3N round bottom flask using the injection device. The tripod on which the anchor is advised to create allowany layer of beads of catalyst. Received black beads were then heated from room temperature to 150oC for one hour. Then the catalyst was heated up to the temperature of the final artificial aging at 343oC and maintained at this temperature for one hour. After cooling to room temperature is sensitive to air, the catalyst was subjected to rehydration with water, using water-saturated stream of nitrogen so that the catalyst can be safely keep in the air while laying in the reactor. The resulting level of sulfur was of 7.48% of the total weight of the catalyst. Analysis of sulfur content in the catalyst was carried out using serouglerode analyzer SC-432 company LECO. Properties of the catalyst are given in table. 2.

Comparative example B

Commercially available hydrocracking catalyst described in Example 2, was subjected to the following procedure acarnania carried out on the spot.

A sample of catalyst was loaded into the device for testing, pressure sulfiding gas (5% H2S/95% H2) which was 350 psig (2.4 MPa) and the flow rate was set so to get the hourly gas flow rate of 1500 (e.g., to 40 ml of the catalyst the rate of potoa, and then with 150oWith up to 370oWith and maintained this temperature for six hours. Then the temperature was maintained at a level of 370oC for two hours, and then reduced to 150oC. After that, the installation was switched on, the flow of pure hydrogen and set the desired speed and pressure, and then began feeding hydrocarbon starting material. The final sulfur level was $ 5.45 per cent of the total weight of the catalyst. The sulfur content in the catalyst was determined using serouglerode analyzer SC-432 company LECO. Properties of the catalyst are given in table.2.

The catalyst test

Sulfurized catalysts according to Example 2 and Comparative example B was used for hydrocracking light gas oil, is subjected to catalytic hydrobromide in the reactor with the flow drip type. A sample of the catalyst was ground and sieved through a sieve 16-45 mesh, diluted with silicon carbide and loaded into the reactor drip type. In the reactor created a pressure of 1500 pounds per square inch (10,34 MPa) using a flow of hydrogen. Then the reactor was heated to 150 C and subjected to catalytic hydrobromide light gas oil was passed over the catalyst hourly feed rate of the liquid in 6.0. Poda is the temperature raised with the intensity of the 22oWith a day for four days and with the intensity of the 6oWith a day for five days to a temperature of 260oC. Then the temperature was set at this level to get the conversion in 1 wt.% raw materials at 190oC. the Results are shown in table.2.

As can be seen from the table.2, the retention of sulfur catalyst, acarnania which was produced by the method according to the invention, which used the solution of inorganic polysulfides (Example 2) was 96%, and it indicates that almost all sulfur remains on the catalyst after the stage of heating. In addition, the activity of the catalyst according to Example 2 in respect of hydrocracking is equal to the activity of the catalyst hydrocracking, acarnania which was produced using the conventional method of pre-acarnania on site (Comparative example B).

1. The method of pre-sulphurization of porous catalyst particles, subject to sulfonation and containing at least one metal or metal oxide, comprising a stage of impregnation of the catalyst with a solution of polysulfide to obtain a catalyst in which the introduced sulfur and in which at least part of the sulphide or sulphur introduced into the pores of the catalyst, and heating of the catalyst in the argon, helium and their mixtures, characterized in that as polysulfide solution for impregnation of the catalyst using a solution containing ions of inorganic polysulfides of the General formula S(x)2-where X is an integer having a value of at least 3.

2. The method according to p. 1, characterized in that a solution containing ions of inorganic polysulfides, obtained by dissolving elemental sulfur in an aqueous solution of ammonium sulfide or a derivative of ammonia.

3. The method according to p. 1 or 2, characterized in that the solution contains sulfur in an amount of 5 to 50 wt. % of the total mass of the solution.

4. The method according to any of the preceding paragraphs, characterized in that before impregnation, the catalyst containing at least one metal or metal oxide, hydronaut to equilibrium with the air.

5. The method according to any of the preceding paragraphs, characterized in that the impregnation is carried out at a temperature from 0 to 60oC.

6. The method according to any of the preceding paragraphs, characterized in that the heating is carried out at a temperature of from 50 to 400oC.

7. Pre-sulfated catalyst obtained by the method according to any of the preceding paragraphs. 1-6.

 

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