A method of producing a catalyst suitable for use in the isomerization of hydrocarbons, the catalyst obtained by this method and its application

 

(57) Abstract:

The invention relates to a method for producing an activated catalyst composition in which a catalytic composition comprising a noble metal of group VIII and a compound of aluminum with hydrocarbon substituents on aluminiumoxide carrier containing up to 20 wt.% other components selected from the group comprising silicon dioxide, magnesium oxide, titanium oxide and zirconium oxide, activated by contact with hydrogen-containing gas at a temperature above 500oWith provided that at least when present in the catalytic composition, the compound of aluminum with a hydrocarbon Deputy is not a halide of aluminum compounds with hydrocarbon Deputy, you must activate the catalytic composition by contact with the halogen compound, either before or during the stage of activation. In addition, a part of the present invention is a catalyst which can be obtained by this method, and its use in such processes for the conversion of hydrocarbons, as isomerization. The technical result - the high-temperature stage activation improves the activity of the thus obtained catalyst on the I. 3 C. and 10 C.p. f-crystals, 2 tab.

The present invention relates to a method for producing an activated catalyst composition suitable for use in the isomerization of hydrocarbons, based catalytic composition containing a noble metal of group VIII and a compound of aluminum with a hydrocarbon Deputy deposited on alumina containing up to 20 wt.% the other components of the thus obtained catalyst and its use.

Isomerization catalysts containing a noble metal of group VIII and a compound of aluminum with a hydrocarbon Deputy deposited on the aluminum oxide, known from the prior art, and methods for their preparation. In the United Kingdom patent 1432639 describes a method for the isomerization catalyst of this description, in which a composition comprising a noble metal of group VIII and aluminum oxide, in contact with the halide of aluminum compounds with hydrocarbon Deputy; formed after the catalyst was directly used for the isomerization of paraffins. In the United Kingdom patent 952348 describes a method for the isomerization catalyst, in which a composition comprising a noble metal of group VIII and aluminum oxide, contentimporter below 260oC. optionally after this treatment the catalyst is activated with hydrogen at a temperature below 371oC.

However, as described in these references catalysts are unsatisfactory and there is a need for a catalyst with increased activity.

The authors found that you can improve the catalytic activity of the composition containing a noble metal of group VIII and a compound of aluminum with a hydrocarbon Deputy deposited on alumina and containing up to 20 wt. % other components, subjecting the composition to a high temperature stage of activation, whereby the composition is in contact with a hydrogen-containing gas at a temperature of 500oC or higher. In this regard, it is necessary to take into account that if the connection of the aluminum hydrocarbon Deputy is not a halide, it is necessary to activate the catalytic composition by contact with the halogen compound, either before or during the stage of activation.

A noble metal of group VIII is present in the catalyst can be selected from the group of ruthenium, palladium, osmium, iridium and platinum, and preference is given to platinum, palladium and their mixtures. Preferably, the final to the up to 1 wt.%. Optionally, the catalytic composition may also be present other metal components. Examples of other metal components, which may affect the activity, selectivity or stability of the catalyst is tin, lead, germanium, bismuth, cobalt, Nickel, indium, gallium, zinc, uranium, thallium, zirconium, and mixtures thereof.

Aluminiumoxide carrier containing up to 20 wt.% other components, preferably has the shape of particles obtained by, for example, by extrusion, tabletting, or some other known method. The shape of these particles can be different. As acceptable forms include spheres, cylinders, rings and symmetric or asymmetric polyhedra, such as trekhgrannykh and tetrahedra. Typically, these particles will have a diameter in the range from 1 to 10 mm and a length in the range from 1 to 10 mm alumina may contain up to 20 wt.% other components, such as silicon dioxide, magnesium oxide, titanium dioxide or zirconium. Preferably, more than 90% of the medium, more preferably more than 95 wt.%, and most preferably almost the entire media, consisted of aluminum oxide. Here, the term "almost all"inim component carrier will be impurities, which is inevitable. Suitable oxides include aluminum such active materials, such as gamma-alumina, ETA-alumina, theta-alumina, and mixtures thereof. Gamma-alumina is particularly preferred.

Aluminiumoxide carrier containing up to 20 wt.% other components, preferably has a surface area of 100-500 m2/g, total pore volume of 0.1-1 ml/g and average pore diameter of 2-20 nm.

Composed of metal components with the carrier can be accomplished in any way known from the prior art. For example, you can start with the preparation of carrier particles, shaping the precursor medium, for example by extrusion and Prokaeva obtained molded particles. Then the particles of the carrier can be impregnated with an impregnating solution containing a soluble salt or complex of a metal or metals which should be applied. For example, it is possible to impregnate the carrier of an impregnating solution containing chloroplatinic acid dichloride, platinum tetrachloride hydrate, platinum and other Well-known from the prior art that the addition of additional components in the impregnating solution stabilizes the solution or affects the distribution of the metal is strongly acidic impregnation solution, such as an impregnating solution containing chloroplatinic acid with addition of hydrochloric acid and nitric acid. These impregnated particles optionally can be ignited. On the other hand, it is also possible to mix the compound of the metal (or metals) that you must enter in the composition of the catalyst, with the predecessor of the carrier and then to mould the mixture, for example by extrusion, and then the calcined extrudates.

Optional metal component of group VIII present in the medium can be recovered, for example, by passing hydrogen through the composition at a temperature in the range from 100 to 600oC.

The connection of the aluminum hydrocarbon Deputy used in the method of this invention, may be a halide, in this case, it is preferable to use a compound of aluminum chloride from hydrocarbon Deputy. The aluminum halide with a hydrocarbon Deputy may be a compound of the formula AlXyRlnR2min which X represents a halogen atom, the radicals R1 and R2 may be the same or different and are selected from alkyl groups or aryl groups, having from 1 to 12 carbon atoms; y has a value of 1 or 2, m is preferably X - chlorine. The radicals R1 and R2 can be selected from, for example, methyl, ethyl, isopropyl, butyl, phenyl, cyclohexyl, and other Suitable aluminum halides from hydrocarbon Deputy include diethylaluminium, methylaluminoxane, ethylaminoethanol and sibutraminegeneric. It should be noted that the aluminum halide with a hydrocarbon Deputy may also be a mixture of halides of aluminum with hydrocarbon substituents or complex, such as alkylalkoxysilane.

When the connection of the aluminum hydrocarbon Deputy is not a halide, it can correspond to the formula A1R1R2R3, in which the radicals Rl, R2 and R3 may be the same or different and are selected from alkyl or aryl groups, having from 1 to 12 carbon atoms, such as described above. Examples of aluminum compounds with hydrocarbon substituents include triethylaluminium and isobutylmethylxanthine. It is also possible to use mixtures of different negligently aluminum compounds with hydrocarbon substituents.

Optionally, you can use a combination of one or more halides of aluminum with hydrocarbon substituents with one or more negligently the political composition is added a sufficient amount of halide or separately, or with a halide compound of aluminum with hydrocarbon substituents.

The connection of the aluminum hydrocarbon Deputy can be entered in the catalytic composition in an amount of from 0.05 to 0.20 mol of aluminum compounds with hydrocarbon substituents on the mole of the media. This compound is aluminum with a hydrocarbon Deputy can be entered in the catalytic composition by any method known from the prior art. For example, you can enter the connection of aluminum with a hydrocarbon substituent in the catalyst by contacting it with a composition containing a noble metal of group VIII, optionally in the restored form, aluminiumoxide carrier containing up to 20 wt.% the other components.

The introduction of aluminum compounds with a hydrocarbon substituent in the catalytic composition can be performed from a solution of this compound in the solvent by impregnation of the carrier, which contains a component of the noble metal of group VIII, this solution followed by removal of solvent. Preferably the boiling point of the solvent should not be too high, because then it becomes difficult to remove the high-boiling solvent from the composition. A suitable process is the development of solvent from the solution to the stage of activation. A possible alternative is the evaporation of the solvent at the stage of activation. Of course, the ease of implementation of this option depends on the nature of the solvent and other process conditions.

In the method for activating a catalytic composition in accordance with the invention, the catalytic composition comprising a noble metal of group VIII and a compound of aluminum with hydrocarbon substituents on the carrier, in contact with a hydrogen-containing gas at a temperature above 500oWith, preferably in the range from 500 to 1000oC, more preferably in the range from 500 to 800oS, most preferably from 600 to 750oC. This activation is carried out by contacting the catalyst with hydrogen-containing gas during the period from 15 minutes to 5 hours, preferably from 0.5 to 3 hours.

During the activation process using the hydrogen-containing gas, which may contain other desired components, such as nitrogen, argon or other inert gases. Preferably the hydrogen-containing gas used in the activation method of this invention contains less than 10 ppm (M. D.) water and less than 10 M. D. oxygen or oxygen-containing components.

As indicated uglevodorodnym Deputy it is necessary that the catalytic composition is contacted with a halide compound, specifically with a compound of chlorine, either before or during the activation process. For example, it is possible to first catalytic composition is contacted with a halogen-containing compound at a temperature in the range from 0 to 800oWith, preferably in the range from 50 to 250oWith, and then activate the catalyst with hydrogen at a temperature above 500oC. moreover, the activation can be performed in the presence of halogenated compounds.

An example of a suitable halogen-containing compounds, which are used either before or during the activation processing is halogenated, such as hydrogen chloride, gaseous halogen, halogenated hydrocarbons such as carbon tetrachloride, chloroform, chlorinated ethane and other hydrogen halides, in particular chloride hydrogen are generally preferred. If the stage of activation is carried out in the presence of halogen compounds, the molar ratio of compounds of halogen to hydrogen in the activating gas is preferably in the range from 0.1 to 10, more preferably in the range from 1 to 5. When the connection of the aluminum with uglevodorodno the purpose you can use or hydrogen-containing gas, which does not contain halogen compounds, or hydrogen-containing gas that contains at least one compound of a halogen. Usually when using a hydrogen-containing gas that contains a halogen compound, receive a catalyst having higher activity than using a hydrogen-containing gas that does not contain a halogen compound. You can also contact a catalytic composition comprising a compound of aluminum halide with a hydrocarbon substituent and a noble metal of group VIII, a compound of halogen up to the implementation of activation described above, but usually you get a slight advantage. The final catalyst generally contains 0.2-15 wt.% halogen, which preferably is chlorine.

The activated catalyst obtained by the method of this invention, suitable for use in many processes for the conversion of hydrocarbons. For example, it can be used for isomerization of paraffins having from 4 to 12 carbon atoms. It is also suitable for the isomerization of various mixtures of n-paraffins and mixtures of n-paraffins to aromatic hydrocarbons. The catalyst of this invention gives particularly x is ment, contains at least 50 wt.% paraffins, which can be isomerized. Raw materials may contain olefins, but preferably less than 10%, because in the presence of olefins increases the consumption of hydrogen. As is known from the prior art, the raw material is practically not contain sulfur compounds and water, since these materials have a poisoning effect on the catalyst. Usually the raw material contains up to 1 ppm of sulfur and 0.5 ppm of water.

The isomerization process may be carried out in the form of contact isomerizing raw material with the above described catalyst in a fixed bed at a temperature in the range from 80 to 330oC, preferably from 100 to 200oSince, in the presence of hydrogen. The pressure in the isomerization reactor is typically in the range from 0.1 to 6 MPa (1-60 bar), preferably from 0.2 to 4 MPa, while the feed rate of the liquid raw material (SPGS) varies from 0.5 to 40 1/h, preferably from 1 to 20 1/h, and the molar ratio between hydrogen and the feedstock is in the range of 0.005 to 10, preferably in the range from 0.01 to 5. As is known to experts in this field of technology, the desire to extend the service life of the catalyst in raw, you can enter a small number of connections, moderatoring halogen or halogenated hydrocarbon, such as carbon tetrachloride, chloroform, chloride, ethane, and chloride isopropyl etc.

In addition, the catalyst obtained by the method of this invention can be applied to the alkylation of aromatic or aliphatic hydrocarbons by contacting alkilirutego connection with an alkylating agent under suitable temperature and pressure in the presence of a catalyst. Alkylation reaction known to specialists in this field of technology and there is no need for further explanations. Other processes that can be applied to the catalyst obtained by the method of this invention are the dimerization and oligomerization of olefins.

Example 1

Contact about 1000 g of the catalyst is gamma-alumina having a purity of above 99.9%, and the total pore volume of 0.5 ml/g (determined by the method of mercury porosimetry), within 4 hours from about 2 kg of an aqueous solution containing 11.8 g chloroplatinic acid (25% platinum), 26.7 g of 37% hydrochloric acid and 39.7 g of 65% nitric acid. Then the extrudates are dried at 120oC for 16 h and calcined for 1.5 hours at 550oC. Calcined product has a platinum content of 0.29 wt.% and the chlorine content of 0.9 wt.%. Cal is ediblered, 20 wt.%, in heptane. During the addition the temperature increases from 31 to 54oWith, later it was increased to 80oC. At this temperature the reaction is continued for 1 hour. In the course of this reaction over the catalyst is passed a stream of nitrogen (100 ml/min). Then from the round-bottom flask drain the liquid, and the liquid residue is evaporated at a temperature of 130oWith in a stream of nitrogen 1300 ml/min Then the product in the round bottom flask is heated to 640oWith the current mixture of 5% hydrogen and 95% nitrogen (total flow of 2 l/min). After 1 hour activation at 640oWith using the same stream of a mixture of hydrogen with nitrogen, the product is cooled to room temperature, completing the preparation of the catalyst.

A small portion of catalyst (10 g) is transferred into the reactor for testing, except the access of air. Then increase the temperature to 146oWith and passed through the catalyst mixture of hydrocarbons and hydrogen. The molecular ratio of hydrogen/hydrocarbon is 3, the pressure of 3 MPa and a feed rate equal to 4 g of hydrocarbons per 1 g of catalyst per hour. In hydrocarbons, consisting of 42 wt.% n-pentane, 48 wt.% n-hexane and 10 wt.% cyclohexane, add 300 M. D. chlorine in carbon tetrachloride. After 3 hours of work define NUM6and these numbers isomerization is defined by the following formulas:

NUM5=So5/(ISOs5+h5and

NUM6=1002,2 DMB/(2,2 DMB+2,3 DMB+2 MP+3 MP+nab)

in which the symbols ISOs, n-C5, 2,2 DMB, 2,3 DMB, 2 MP, 3 MP, and NS represent a hydrocarbon concentration

ISOs=isopentane,

n-C5=normal pentane,

2,2 DMB=2.2-Dimethylbutane,

2,3 DMB=2,3-dimethylbutan,

2 MP=2-methylpentan,

3 MP=3-methylpentan,

NS=normal hexane.

In the above-described experiment, the number isomerization have the following meanings NUM5=56 and NU6=19. The concentration of the products of cracking (butane and lighter) is less than 0.3 wt.%.

Example 2

Extrudates of alumina (300 g) of high purity, containing of 0.28 wt. % platinum and 1.1 wt.% chlorine and having a pore volume of 0.5 ml/g, prepared according to the method similar to that described in the first part of Example 1 was transferred into a round bottom flask. Then the extrudates in the flask is treated with pure hydrogen at a flow rate of 500 ml/min at 400oC for 2 h and then cooled to room temperature in nitrogen. To the flask add 376 g of a solution of ethylaminoethanol, 20 wt. % heptane. During the addition the temperature of watertube in 1 hour. In the course of this reaction over the catalyst is passed a stream of nitrogen (100 ml/min). Then from the round-bottom flask drain the liquid, and the liquid residue is evaporated at a temperature of 130oWith in a stream of nitrogen 3000 ml/min After drying the product in a round-bottom flask heated to 675oWith the current mixture of 5% hydrogen and 95% nitrogen (total flow of 2 l/min). After 1 hour activation at 675oWith using the same stream of a mixture of hydrogen with nitrogen, the product is cooled to room temperature in pure nitrogen, completing the preparation of the catalyst according to the invention.

A small portion of the thus obtained catalyst (10 g) is transferred into the reactor for testing, except the access of air. Then raise temperature to 155oWith and passed through the catalyst mixture of hydrocarbons and hydrogen. The molecular ratio of hydrogen/hydrocarbon raw material is 0.1, the pressure of 3.1 MPa and a feed rate equal to 5 grams of hydrocarbon per 1 g of catalyst per hour. In hydrocarbonaceous feedstock comprising n-butane, add 100 M. D. carbon tetrachloride. After about 1000 minutes of operation, determine the composition of the product. The data structure used to calculate numbers isomerization NUM4using the following formula:

NUM4aluminum (300 g) of high purity, containing of 0.28 wt. % platinum and 1.1 wt.% chlorine and having a pore volume of 0.5 ml/g, prepared according to the method similar to that described in the first part of Example 1 was transferred into a round bottom flask. Then the extrudates in the flask is treated with hydrogen (100% purity) at a flow rate of 500 ml/min at 400oC for 2 h and then cooled to room temperature in nitrogen. To the flask add 380 g of the solution of ethylaminoethanol, 20 wt.%, in heptane. During the addition the temperature was increased from 28 to 50oAnd later it was increased to 85oC. the Reaction mixture was kept at this temperature continued for 1 hour. In the course of this reaction over the catalyst is passed a stream of nitrogen (100 ml/min). Then from the round-bottom flask drain the liquid, and the liquid residue is evaporated at a temperature of 130oWith in a stream of nitrogen 1300 ml/min and Then the product is cooled to room temperature. So get the comparative catalyst in accordance with the description of the patent in the UK 1432639, containing 0.26 wt.% platinum and about 8 wt.% chlorine.

In order to obtain the catalyst according to this invention, again way to obtain comparative catalyst in accordance with the description of the patent in the UK 1432639 except for the paravane at a temperature of 130oWith in a stream of nitrogen 1300 ml/min product in a round-bottom flask heated to 640oWith the current mixture of 5% hydrogen and 95% nitrogen (total flow of 2 l/min). In accordance with this invention after 1 hour activation at 640oWith using the same stream of a mixture of hydrogen with nitrogen, the product is cooled to room temperature in pure nitrogen, completing the preparation of the catalyst.

As a comparative catalyst in accordance with the United Kingdom patent 1432639 and the catalyst according to this invention have the procedure described above in Example 1. After about 1000 minutes of operation, determine the composition of the oil. The data structure used to calculate numbers isomerization NUM5and NU6. The results are given in table.1.

From table. 1 shows that the catalyst of this invention, which is different from the catalyst in accordance with the United Kingdom patent 1432639 only the fact that it is subjected to high temperature treatment in the presence of hydrogen has a much higher activity in the isomerization, as evidenced by higher values of NU5and NU6.

Example 4

Extrudates of alumina (250 g) of high purity, containing of 0.28 wt. % platinum and 1.1 wt.% x is rinoseat in a round bottom flask. Then the flask was added 280 g of the solution of triethylaluminum, 20 wt.%, in heptane. During the addition the temperature increases from 28 to 52oAnd thereafter it increases to 85oC. the Reaction mixture was kept at this temperature continued for 1 hour. In the course of this reaction over the catalyst is passed a stream of nitrogen (100 ml/min). Then from the round-bottom flask is drained liquid.

Introducing a stream of hydrogen chloride, hydrogen, and nitrogen. After 35 minutes, the flow of hydrogen chloride increase from 120 to 720 ml/min. At the same time a stream of nitrogen decreases from 1600 ml/min to zero, and the flow of hydrogen from 200 to 72 ml/min during this time the temperature is 108oC. Then the catalyst for 35 minutes, heated to 250oWith the current hydrogen chloride (720 ml/min) and hydrogen - 72 ml/min and maintained at this temperature for 2 hours. Then block the current of hydrogen chloride and increase the flow of hydrogen to 500 ml/min, the Temperature is increased to 350oC. the Catalyst was maintained under these conditions for 1 hour, after which the catalyst was cooled down to room temperature in pure nitrogen. So get the comparative catalyst in accordance with the description of the patent in the UK 952348 which provides the e catalyst in accordance with the United Kingdom patent 952348 heated in a round bottom flask up to 640oWith the current mixture of 5% hydrogen and 95% nitrogen (total flow of 2 l/min). After 1 hour activation at 640oWith using the same stream of a mixture of hydrogen with nitrogen, the product is cooled to room temperature in pure nitrogen, completing the receipt of the catalyst according to this invention.

As a comparative catalyst in accordance with the United Kingdom patent 952348 and the catalyst according to this invention, have the procedure described above in Example 1. After about 1000 minutes of operation, determine the composition of the hydrocarbon product. The data structure used to calculate numbers isomerization NUM5and NU6for both experiments. The obtained results are given in table.2.

From table. 2 shows that the catalyst of this invention, which is different from the catalyst in accordance with the United Kingdom patent 952348 only the fact that it is subjected to high temperature treatment in the presence of hydrogen has a much higher activity in the isomerization, as evidenced by higher values of NU5and NU6.

1. The method of obtaining the activated catalytic composition, comprising the following stages: a) a composition containing a noble metal VIII the silicon led, magnesium oxide, titanium oxide and zirconium oxide; (b) optionally recovering the noble metal; (C) contacting the product of stage (a) or (b) with a compound of aluminum with a hydrocarbon Deputy, characterized in that it further comprises a stage of high-temperature activation (d), where the product of stage (C) is in contact with a hydrogen-containing gas at a temperature above 500oWith, provided that if present in the catalytic composition, the compound of aluminum with a hydrocarbon Deputy is not a halide of aluminum compounds with hydrocarbon Deputy, you must activate the catalytic composition by contact with the halogen compound, either before or during the stage of activation.

2. The method according to p. 1, characterized in that the connection of the aluminum hydrocarbon Deputy, is present in the catalytic composition to be activated, represents a halide of aluminum compounds with hydrocarbon Deputy.

3. The method according to p. 2, characterized in that the halide of aluminum compounds with hydrocarbon Deputy represents the aluminum chloride from hydrocarbon Deputy.

4. The method according to p. 2 or 3, characterized in that the ha isnR2min which X represents a halogen atom, the radicals R1 and R2 may be the same or different and are selected from alkyl groups and aryl groups, having from 1 to 12 carbon atoms, y has a value of 1 or 2, n and m have a value of 0 or 1, and the sum of y, n and m equals 3.

5. The method according to p. 1, characterized in that it is present in the catalytic composition, the compound of aluminum with a hydrocarbon Deputy corresponds to the formula A1R1R2R3, in which the radicals R1, R2 and R3 may be the same or different and are selected from alkyl or aryl groups, having from 1 to 12 carbon atoms.

6. The method according to p. 5, characterized in that a catalytic composition comprising a compound of aluminum with a hydrocarbon Deputy, which is not a halide of aluminum compounds with hydrocarbon Deputy, in contact with the connection of halogen up to the implementation stage of activation.

7. The method according to any of paragraphs.2-4 or 6, characterized in that the catalytic composition activate using the hydrogen-containing gas that does not contain any halogenated compounds.

8. The method according to any of paragraphs.2-6, wherein the catalytic composition is activated with IP characterized in that that halogen-containing compound is hydrogen chloride.

10. The method according to any of paragraphs.1-9, characterized in that the catalyst composition comprises platinum as a noble metal of group VIII.

11. Activated catalytic composition containing a noble metal of group VIII and a carrier-aluminum oxide, characterized in that it is obtained according to any one of paragraphs.1-10.

12. The method of conversion of hydrocarbons by contact with the activated catalyst composition, characterized in that use activated catalytic composition under item 11.

13. The method according to p. 12, characterized in that in the method of isomerization of n-paraffin feedstock containing n-paraffins, in contact with the activated catalytic composition according to p. 11 in the presence of hydrogen.

 

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