The method of converting hydrocarbons into olefins and aromatic hydrocarbons and method for producing the catalytic composition for its implementation

 

(57) Abstract:

Usage: petrochemistry. The inventive method comprises the interaction of the hydrocarbon stream with the catalyst composition under conditions sufficient to effect the conversion of hydrocarbons to olefins and C6-C8-aromatic hydrocarbons. The catalytic composition comprises a zeolite, a binder and Bor, where the mass of boron is in the range of 0.01-10 wt.%. Also described is a method of obtaining a catalytic composition which comprises (1) mixing the zeolite with reducing the formation of coke by the amount of binding of the substance under conditions effective to obtain a mixture of zeolite-binder; (2) the interaction of the mentioned mixture of the zeolite-binder with reducing the formation of coke a number of boron compounds under conditions effective to obtain a zeolite with the introduced boron or zeolite impregnated with boron, and (3) calcining the zeolite with the introduced boron or zeolite impregnated with boron. 2 C. and 16 h.p. f-crystals, 2 tab.

The invention relates to compositions that can be used for the conversion of hydrocarbons in the C6-C8aromatic hydrocarbon and the olefin, the method of production of the composition and to FPIC is Latin.

Background of the invention

Specialists in this field it is well known that aromatic hydrocarbons and olefins, represent a class of very important industrial chemical products, which find various applications in the petrochemical industry. Specialists in this area is also well known that obtained by the catalytic cracking of hydrocarbons boiling within the gasoline fraction form the lower olefins, such as propylene, and aromatic hydrocarbons, such as benzene, toluene and xylenes (hereinafter collectively called Bq) in the presence of zeolite catalysts. The product in this way catalytic cracking process contains a large number of hydrocarbons, including not turned alkanes WITH5+; lower alkanes, such as methane, ethane and propane; lower alkenes such as ethylene and propylene; and aromatic compounds C9+ containing 9 or more carbons in the molecule. So last attempt of turning gasoline fractions into more valuable petrochemical products were aimed at improving the conversion of a gasoline fraction olefins and aromatic hydrocarbons by catalytic cracking in the presence of zeolite cuteeeee hydrocarbon in the CPD. Olefins and aromatic hydrocarbons can be useful source material for production of various organic compounds and polymers. However, the mass ratio of olefins to aromatic compounds formed by the method of transformation, usually lower than 50%. Therefore, development of a catalyst and method of converting hydrocarbons into more valuable olefins can make a significant contribution in this area and in the economy.

SUMMARY OF THE INVENTION

In accordance with the first aspect of this invention features a composition that can be used as a catalyst for the conversion of hydrocarbons or hydrocarbon mixtures in the olefin and C6-C8aromatic hydrocarbon.

The composition comprises a zeolite, a binder and Bor, where boron is present in the composition in an amount of from about 0.01 to about 10 mass percent (%).

In accordance with the second aspect of the present invention, a method for the catalytic composition. This method involves the following stages: (1) mixing the zeolite with a binder in an amount that reduces the formation of coke under conditions effective for the formation of a mixture of zeolite-linking gamestm the boron compounds under conditions effective for obtaining boron or a boron impregnated zeolite; and (3) calcining boron or a boron impregnated zeolite.

In accordance with a third aspect of the present invention, a method for converting hydrocarbon or mixture of hydrocarbons in the olefin and C6-C8aromatic hydrocarbon, which is carried out by reacting fluid containing a hydrocarbon or mixture of hydrocarbons with a catalytic composition, such as described above in the first variant implementation of the invention, under conditions effective to convert a hydrocarbon to the olefin and aromatic hydrocarbon containing 6 to 8 carbon atoms in the molecule, where the mass ratio of olefin to aromatic compound increases.

DETAILED DESCRIPTION OF THE INVENTION

The catalytic composition of the first implementation of the present invention may include or be composed of zeolite, binder, and boron. The zeolite or a mixture of zeolite-binder preferably impregnated or coated with boron. In accordance with this invention the weight of elemental boron in the composition of the invention may be from about 0.01 to about 10, preferably from about 0.05 to about what may be in the range of from about 1 to about 50, preferably from about 5 to about 40, and particularly preferably from 10 to 30 grams per 100 grams of composition. The zeolite is usually the rest of the song. The composition also differs in that it has the following physical characteristics: surface area, as determined by the BET method using nitrogen, in the range from about 300 to about 600, preferably from 350 to 500 m2/g; pore volume in the range from about 0.4 to about 0.8, preferably from about 0.5 to about 0.75, and very preferably from 0.6 to 0.75 ml/g; average diameter of pores in the range of from about 70 to about 300, preferably from about 100 to about 250, and very preferably from 125 to 200 ; and a porosity of more than about 50%.

For the method of the second variant embodiment of the invention as starting material can be used any commercially available zeolite. Examples of suitable zeolites include, but are not limited to, zeolites are described in Kirk-Othmer Encyclopedia of Chemical Technology, third edition, volume 15 (John Wiley and Sons, New York, 1991), and in W. M. Meier and D. H. Olson, "Atlas of Zeolite Structure Types", pages 138-139 (Butterworth-Heineman, Boston, Mass.,rded. 1992). The currently favored zeolites are zeolites having average pore sizes and physical characteristics described above. ZSM-5 and similar the melt (MFI), especially preferred because of the selectivity of their form.

Any binders known to the person skilled in the art are suitable for use with zeolite according to this invention. Examples of suitable bonding agents include, but are not limited to, clays, such as kaolinite, halloysite, vermiculite, chlorite, attapulgite, smectite, montmorillonite, illite, sekonic, thick, palygorskite, diatomaceous earth, and combinations of any two or more thereof; oxides of aluminum, such as, for example, aluminum oxide and alumina; silica; alumina-silica; aluminum phosphate; hydrochloride aluminum and combinations of two or more of them. Since these binders are well known to the person skilled in the art, the description of them here is not included. Preferred binding substance is currently the bentonite due to the fact that it is easily available.

The composition of this invention can be obtained by mixing the zeolite, the binder, and the boron compounds in mass percent, above, in any circumstances, be sufficient to allow the formation of such a composition.

At present, however, it is preferable that the HDMI is possible. In the first stage of the second variant of the invention, the zeolite is mixed with a binder, as described above, under conditions sufficient to obtain a mixture of zeolite-binder.

In accordance with this invention the zeolite, preferably ZSM-5, and binder are mixed by any means known to the person skilled in the art, such as stirring, blending, kneading, or extrusion, following which the mixture of zeolite-binder can be dried in air at a temperature in the range from about 20 to about 800oC for from about 0.5 to 50 hours at any pressure, which is consistent with the temperatures, preferably under atmospheric pressure. Thereafter, the dried mixture of zeolite-binder further calicivirus, if necessary, in air at a temperature in the range from about 300 to 1000oC, preferably from about 350 to about 750oAnd particularly preferably from 450 to 650oC for from about 1 to 30 hours to obtain a calcined mixture of a zeolite-binder. Before the binder is mixed with the zeolite, the zeolite can be calcined under the same conditions to remove l is t, calcined zeolite or soda mixture of zeolite-binder can be treated with a compound containing exchangeable ammonium ion, to obtain the ammonium exchanged zeolite. Regardless of calcined zeolite, or whether it contains a binder, the method of processing the second implementation is the same for each case. In the interests of brevity, the following describes only the zeolite. Examples of compounds suitable, containing ammonium, include, but are not limited to, ammonium sulfate, ammonium chloride, ammonium nitrate, ammonium bromide, ammonium fluoride, and combinations of any two or more of them. As a result of processing of the initial zeolite ions, such as, for example, ions of alkali or alkaline earth metal zeolite are replaced mainly ammonium ions. Techniques such processing is well known to the person skilled in the art, such as, for example, the initial ion exchange ions. For example, the zeolite can interact with the solution containing the salt of the target replacement ion or ions.

Typically, the zeolite is suspended in an aqueous solution of compounds containing ammonium. The concentration of the zeolite in an aqueous solution can be in the range of from about 0.01 to about 800, prepost grams per liter. The number of the desired compound containing ammonium depends on the number of initial ion (ions), which must be replaced. When getting the solution can be subjected to a temperature treatment in the range of from about 30oWith up to 200oC, preferably from about 40oWith up to 150oAnd particularly preferably from 50oWith up to 125oC for from about 1 to 100 hours, preferably from about 1 to about 50 hours, and especially preferably from 2 to 25 hours, depending on the desired degree of ion exchange. Treatment may be performed under pressure in the range from about 1 to about 10 atmospheres (ATM), preferably about 1 ATM or any pressure that is capable of maintaining the required temperature. The treated zeolite was washed with tap water for 1 to 60 minutes, followed by drying and calcining to obtain a calcined zeolite in the hydrogen form. The processes of drying and calcination is conducted essentially the same as the processes of drying and calcination as described above to obtain a calcined zeolite or a mixture of zeolite-binder.

Typically, the ammonium exchanged zeolite is hydrogen exchange rate is can exchange cations were hydrogen ions. The above ion exchange is capable of exchanging ions in the zeolite are well known to the person skilled in the art. See, for example, U.S. patent 5516956, the description of which is included here as a reference. Because the technique of ion exchange are well known, its description is not included here in the interests of brevity.

In the second variant implementation of the invention, the mixture of zeolite-binder to the desired ionic form, regardless of whether calcined or not, interacts with the boron compound under conditions known to specialists in this field, for the introduction of compounds of boron in the zeolite. Preferably the zeolite or a mixture of zeolite-binder-impregnated with a boron compound. Because the ways of introducing the boron compounds in zeolite or a mixture of zeolite-binder or impregnating such a connection zeolite or a mixture of zeolite-binder, such as, for example, impregnation method, the initial moisture, well-known specialists in this field, the description is also not included here in the interests of brevity.

In accordance with this invention any boron-containing compound, which, when it is inserted into the zeolite or a mixture of zeolite-binder or deposited on n the data of the invention. In this invention it is possible to use boron compound having the formula R3-zWz, (R)3. BWz(OR SIG)3or a combination of two or more of them, where R can be hydrogen, alkyl radical, alkenyl radical, aryl radical, arylalkyl radical, alcylaryl radical, and two or more combinations thereof, where each radical may have from 1 to 20 carbon atoms, R' can be R, RO, RS, R2N, R2P, R3Si or combinations of two or more of them, W can be halogen, NR3, NO2, SO4, PO4or two or more combinations, and z is an integer from 1 to 3. Examples of suitable boron compounds include, but are not limited to, boric acid, borane-ammonium complex, trichloride boron, boron phosphate, boron nitride, triethylborane, trimethylboron, tripropionin, trimethylboron, triethylborane, tripropellant, trimethylboroxine, triethylborane, Tripropylamine and combinations of two or more of them.

With the introduction of the boron compounds in zeolite or a mixture of zeolite-binder or impregnating compound of boron zeolite or a mixture of zeolite-binder to obtain a boron-containing zeolite or impregnated with boron of the boron-containing zeolite, the zeolite or in the range from about 300oWith up to about 1000oC, preferably from about 350oWith up to about 750oAnd especially preferably from 400oWith up to 650oWith under pressure, which is consistent with the temperature usually in the range of from about 1 to about 10 atmospheres (ATM), preferably about 1 ATM for a period of from about 1 to about 30, preferably from about 1 to 20 and particularly preferably from 1 to 15 hours, to obtain the specified composition of the invention.

The composition of the invention can be, if necessary, pre-treated regenerating agent (reducing agent) to use it in the way of hydrodealkylation. The currently favored reducing agent is a hydrogen-containing fluid which comprises molecular hydrogen (H2) in the range of from 1 to about 100, preferably from about 5 to about 100, and very preferably from 10 to 100 vol.%. Recovery can be performed at a temperature in the range from approximately 250 to 800oC for from about 0.1 to 10 hours, preferably from about 300 to about 700oC for from about 0.5 to 7 hours, and particularly preferably from 350 to 650oC for from 1 to 5 cocohut for the conversion of a hydrocarbon or hydrocarbon mixture in the mixture, enriched in olefins and C6-C8-aromatic hydrocarbons, includes the interaction of a stream of fluid comprising a hydrocarbon or hydrocarbon mixture, which can include paraffins, olefins, naphthenes, and aromatic compounds with a catalyst composition under conditions sufficient for conversion of a hydrocarbon mixture in the mixture, enriched in olefins and C6-C8-aromatic hydrocarbons, or to increase the mass relations of olefins (ethylene and propylene) to C6-C8-aromatic hydrocarbons. The catalytic composition is the same as the catalytic composition described in the first variant implementation of the invention. The term "fluid" is used here to denote a gas, liquid, steam or combinations thereof. The term "hydrocarbon" usually means, unless otherwise stated, one or more hydrocarbons having from 4 to 30 carbon atoms, preferably from about 5 to about 20 carbon atoms and particularly preferably from 5 to 16 carbon atoms in the molecule. The term "high" refers to the increased mass ratio of olefins to BTX using this catalytic composition compared to the use of zeolite, such as clucalc, but not limited to, butane, isobutane, pentane, isopentane, hexane, isohexane, cyclohexane, heptane, isoheptane, octane, isooctane, Nanan, decane, undecane, dodecane, tridecane, tetradecane, pentadecane, hexadecane, butenes, isobutene, pentene, hexene, benzene, toluene, ethylbenzene, xylenes, and combinations of any two or more of them.

Any fluid that contains hydrocarbon, as described above, can be used as raw material for the method of the present invention. Typically, the flow of fluid materials may also contain olefins, naphthenes (cycloalkanes), or some aromatic compounds. Examples of suitable, available fluid materials include, but are not limited to, gasoline fractions of a catalytic methods cracking of oil fractions, gasoline fractions of pyrolysis from thermal cracking of saturated hydrocarbons, naphtha and access to powertrain, chassis, products reformer and combinations of any two or more of them. The nature of this fluid is non-critical raw materials. Although the specific composition of the raw material is non-critical, the preferred fluid is a raw material derived from gasoline fractions, which usually contain more paraffins (alkanes) than total olefins and aromatic compounds (if present).

The interaction of flow f is in his way, periodic or semi-continuous, or continuous manner, under conditions effective for the conversion of hydrocarbons in the C6-C8-aromatic hydrocarbon. Typically, the flow of fluid, as described above, preferably in the form of vapour is injected into the aromatization reactor having a fixed catalyst bed or a moving catalyst bed, or a fluidized catalyst bed, or a combination of any two or more of them, by any means, known to specialists in this field, such as, for example, pressure means, a metered pump or similar means. Because the reactor flavoring and scenting well known to specialists in this field, the description is not given. The condition includes hourly volumetric flow rate of fluid in the range from about 0.01 to about 100, preferably from about 0.05 to about 50, and very preferably from 0.1 to 30 g raw material/g catalyst/hour. Typically, the pressure may be in the range of from about 0 to about 70,3 kg/cm2(1000 psig), preferably from about 0 to about 14,06 kg/cm2(200 psig) and very preferably from 0 to 3,515 kg/cm2(50 psig), and the temperature is from about 250 to 1000oC, preferably from 350 to 750o2-C3the fraction containing ethylene, propylene, ethane, and propane; an intermediate fraction comprising non-aromatic compounds containing more than 3 carbon atoms, and the fraction of aromatic hydrocarbons, BTX (benzene, toluene, ortho-xylene, meta-xylene and para-xylene). Usually the output stream can be divided into these main fractions by any known means, such as, for example, fractional distillation. Because separations are well known to the person skilled in the art, the description of them are omitted here. The intermediate fraction can be recycled in the above-described reactor flavoring; methane, ethane and propane can be used as a gas used as fuel or as raw material for other reactions, such as, for example, the process of thermal cracking to produce ethylene and propylene. The olefins can be selected and then divided into individual olefins by any method known to the person skilled in the art. Individual olefins can then be extracted and sold. The fraction of BTK can be further divided into individual fractions WITH6-C8-aromatic hydrocarbons. Alternatively, the fraction of BTK can be subjected to one or not is to improve the content of the most desirable aromatic hydrocarbon BTK. Suitable examples of such subsequent transformations WITH6-C8aromatic hydrocarbons are the disproportionation of toluene (to form benzene and xylenes), parallelomania benzene and xylenes (toluene formation and isomerization of meta-xylene and/or ortho-xylene to para-xylene.

After deaktivirovana catalytic composition, for example, due to the deposition of coke or poisons raw materials to such an extent that the conversion of raw materials and/or selectivity for the target relations of olefins to BTX has become unsatisfactory, the catalyst composition can be reactivated by any means known to the person skilled in the art, such as, for example, calcining in air for burning of deposited coke and other carbonaceous materials, such as oligomers or polymers, preferably at a temperature of from about 400 to about 650oC. the Optimal time periods of the calcining depend generally on the types and amounts of deactivating deposits on the catalyst composition and on the calcination temperatures. These optimal time periods can be easily identified by experts having ordinary skill in the art, and are not given here at the Institute and should not be construed to unduly limit this invention.

EXAMPLE I

This example illustrates the obtaining of the catalytic compositions of the invention.

Zeolite ZSM-5 obtained from CU Chemie Uetikon AG, Switzerland, has a product called zeochem PZ 2/50H (obtained in powder form) used in obtaining the catalytic composition of the present invention. 20 g of zeolite was thoroughly mixed with 5 g of bentonite in a beaker followed by the addition of water, sufficient to form a paste. Then the paste was extrudible at room temperature (25o(C) for further thorough mixing of the mixture of zeolite-bentonite. Thereafter, the extrudate zeolite-bentonite was dried at 125oWith in a drying Cabinet. The dried extrudate zeolite-bentonite was then subjected to calcination at 500oC for 3 hours to obtain a calcined extrudate zeolite-bentonite (reference catalyst).

Separately, 40 g of zeolite ceokat mixed with 10 g of bentonite to obtain a second soda mixture of zeolite-bentonite. After this, there was obtained a solution containing 5 g of boric acid in 100 ml of water. Part (9 g) solution was added to 10 g of the second soda mixture of zeolite-bentonite to seal the second soda mixture of zeolite-bentonite boric acid for poluchennogo moisture impregnated with boric acid, a mixture of zeolite-bentonite and education pasta dried pasta and calicivirus, as described above, to get promoted (impregnated) with boron zeolite (catalyst of the invention), which contained 0,775 wt.% boron by calcination.

In the comparative experience of the comparative catalyst was prepared by the method described above for obtaining the control catalyst, except that the zeolite powder add 5 g of boric acid simultaneously with the addition of bentonite. Obtain comparative catalyst contained 3,219 wt.% boron by calcination.

EXAMPLE II

This example illustrates the use of the catalytic composition described in example I as catalysts in the conversion of hydrocarbons to olefins and BTX.

The reactor in the form of a quartz tube (inner diameter 1 cm, length 60 cm) fill in the bottom part 20-centimeter layer of alumina, Alundum(inert aluminium oxide with a low surface area), in the middle of the tube 20-cm layer, 5 grams of one of the catalysts and in the upper part of the tube 20-centimeter layer of alumina, Alundum. The liquid raw material is gasoline fraction obtained from Phillips Petroleum Company, Bartesville, Oklahoma and containing hydrocarbons, shown is C5and C6); 1.3% of benzene; 5.4% of toluene, 8.1% of C8-aromatic hydrocarbons; 38.9% of non-aromatic compounds with boiling within the CPD and 25.9% of heavy compounds (C8+). The raw materials were introduced into the reactor at a speed of 14 ml/hour (10,44 g/h). The reaction temperature was 600oC. Leaving the reactor stream is cooled and separated into a gaseous phase and a liquid phase. Both phases were analyzed by gas chromatography at intervals of about 1 hour. Approximately 2 hours after they started feeding raw material, was again selected a sample of the effluent from the reactor stream and were analyzed by gas chromatography to determine the content of olefins and BTX. The results of the experiments after approximately 6 hours are shown in the following table II, which illustrates the formation of olefins and BTX from raw materials of table I and individual catalytic compositions obtained in example I.

The results presented in table II, demonstrate that the raw zeolite (control) formed significantly more BTC than olefins. The catalyst of the invention significantly increased the ratio of educated olefins to CPD, i.e., increased the formation of olefins. However, when using the comparative catalyst compositions, kotli unexpectedly low.

The results shown in the above examples clearly demonstrate that this invention is well adapted for carrying out the methods and achieve the above goals and advantages, as well as its inherent goals and benefits. Although specialists in this area can be made of modifications, such modifications are included in the essence of this invention as defined by the description and the claims.

1. The method of converting hydrocarbons into olefins and C6-C8aromatic hydrocarbon, through the interaction of a fluid, comprising the above-mentioned hydrocarbon, with a catalyst composition under conditions sufficient to perform this transformation, characterized in that the specified catalytic composition get through stages, including (1) mixing the zeolite ZSM-5 with a binder under conditions effective for the formation of a mixture of zeolite-binder, (2) interaction mentioned mixture of the zeolite-binder with reducing the formation of coke a number of boron compounds under conditions effective to obtain a boron or a boron impregnated zeolite; (3) calcining boron or a boron impregnated zeolite, in the above-mentioned fluid includes a gasoline fraction of the catalytic cracking of oil, the fraction of pyrolysis gasoline process of thermal cracking of saturated hydrocarbons, ligroin fraction, petroleum gas, the product of reforming, or a combination of any two or more of the above-mentioned fluids.

3. The method according to p. 1, characterized in that said hydrocarbon contains at least 4 carbon atoms.

4. The method according to p. 3, characterized in that the hydrocarbon containing 4 to 30 carbon atoms.

5. The method according to p. 4, characterized in that the hydrocarbon containing 5 to 16 carbon atoms.

6. The method according to p. 1, where the specified hydrocarbon is gasoline fraction.

7. The method according to p. 1, characterized in that said hydrocarbon is butane, isobutane, pentane, isopentane, hexane, isohexane, cyclohexane, heptane, isoheptane, octane, isooctane, Nanan, decane, undecane, dodecane, tridecane, tetradecane, pentadecane, hexadecane, butenes, isobutene, pentene, hexene, benzene, toluene, ethylbenzene, xylenes, or combinations of any two or more of the above-mentioned hydrocarbons.

8. The method according to any of paragraphs.1-7, characterized in that the weight of boron in the specified catalytic composition is about 0.01 to 10 wt.%.

9. The method according to p. 8, characterized in that the mass of b is from PP.1-7, characterized in that the binder is a kaolinite, halloysite, vermiculite, chlorite, attapulgite, smectite, montmorillonite, illite, sekonic, thick, palygorskite, diatomaceous earth, aluminum oxide, aluminum oxide, silicon dioxide, alumina-silica, aluminum phosphate, hydrochloride aluminum, or a combination of any two or more of the mentioned connecting substances.

11. The method according to p. 10, characterized in that montmorillonite binder is a bentonite.

12. The method according to any of paragraphs.1-7, characterized in that the said mixture of zeolite-binder obtained in stage (1), calicivirus before interaction with the specified boron compound.

13. The method according to any of paragraphs.1-7, characterized in that the mixture of zeolite-binder is impregnated with the aqueous solution of the above boron compounds.

14. The method according to any of paragraphs.1-7, characterized in that the said conditions include average hourly feed rate specified fluid in the range from about 0.01 g/g catalyst/hour to about 100 g/g catalyst/hour, a pressure (overpressure) in the range from 0 kg/cm2to about 14,06 kg/cm2(200 psi) and the temperature in diary includes (1) mixing the zeolite ZSM-5 with a binder to obtain a mixture of zeolite-binder; (2) the interaction of the mentioned mixture of the zeolite-binder with an aqueous solution of boron compounds under conditions sufficient to obtain a zeolite impregnated with boron compound, and (3) calcining the above-mentioned zeolite impregnated with boron compound, where the specified boron compound is a boric acid.

16. The method according to p. 15, characterized in that the said mixture of zeolite-binder obtained in stage (1), calicivirus before interaction with the specified boron compound.

17. The method according to p. 16, characterized in that the binder is a kaolinite, halloysite, vermiculite, chlorite, attapulgite, smectite, montmorillonite, illite, sekonic, thick, palygorskite, diatomaceous earth, aluminum oxide, aluminum oxide, silicon dioxide, alumina - silica, aluminum phosphate, hydrochloride aluminum or a combination of two or more of the mentioned connecting substances.

18. The method according to p. 16, characterized in that said binding agent is bentonite and the specified boron compound is boric acid.

 

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11 cl, 4 dwg, 3 tbl, 16 ex

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