Highly active isomerisation catalyst and isomerisation method

FIELD: chemistry.

SUBSTANCE: invention pertains to a catalyst and a method for selective increase in quality of paraffin raw material, with the aim of obtaining concentrated isoparaffin product as a benzine component. Description is given of the catalyst, which consists of a carrier from a sulphated oxide or hydroxide of group IVB (IUPAC 4) metals. The first component is, at least, from one lanthanide element or an yttric component, which is mainly ytterbium, and at least, one metal of the platinum group, which is mainly platinum, and a fireproof oxide binding substance, on which is dispersed at least, one metal of the platinum group. Description is given of the method of making the above mentioned catalyst, including a sulphated oxide or hydroxide of a group 1VB metal, depositing of the first component, mixing the sulphated carrier with the fireproof inorganic oxide of the oxide carrier, burning, depositing of the second component and subsequent burning. Description is given of the method of converting hydrocarbons through contacting with raw materials with the catalyst described above.

EFFECT: selective increase in quality of paraffin raw materials.

12 cl, 2 tbl, 2 dwg, 7 ex

 

The technical field

The invention relates to an improved catalytic composite and method of conversion of hydrocarbons, and more particularly to selective improvement of quality paraffin feedstock by isomerization.

This work was conducted with support from the National Institute of standards and technology, related to the U.S. Department of Commerce, in the framework of the program on advanced technology, Cooperative agreement No. 70NANB9H3035. The United States government has certain rights in this invention.

The level of technology

The widespread elimination of lead antiknock additives from gasoline and the need to improve fuel quality for high-performance internal combustion engines prompted refiners to implement new and modified processes, increasing the octane number"or antiknock properties of compounded gasoline. The refiners rely on a variety of alternative ways to improve the quality of compounded gasoline, including deeper catalytic reforming process, a higher octane number gasoline catalytic cracking fluidized-bed catalyst (FCC-cracking, isomerization of light naphtha and the use of oxygen-containing compounds. Such a key way as the recess re is orminge and increase the octane number of FCC gasoline lead to a higher content of aromatics in compounded gasoline at the expense of low-octane heavy paraffins.

The refiners are faced with the need to supply reformulating gasoline, which would correspond to more stringent standards on automobile emissions. Reformulating gasoline differs from traditional product because it has a lower vapor pressure, lower temperature end of the boil, the high content of oxygen-containing compounds and lower olefins, benzene and aromatics. Usually benzene content is limited to 1% or below, reformulating gasoline U.S. it is limited to 0.8%. The content of aromatics in gasoline has a tendency to decrease, especially at lower temperature end of the pickup (usually describing a temperature of 90 percent boiling), as removed as a result of this high-boiling part of the gasoline is usually a concentrate of aromatic compounds. Since aromatics were the main source of increasing the octane number of gasoline at the recent implementation of the programme of reduction of lead, strict restrictions on the content of benzene/aromatics and high-boiling part will create the refiners processing problems. These problems relate to technology such as the isomerization of light naphtha to increase its octane number, the isomerization of butane as feedstock for alkylation, production updat the additional light olefins as feedstock for alkylation and production of oxygenates using a catalytic cracking process in the fluidized bed. These tasks often try to solve it by raising the temperature of the separation of light and heavy naphtha, thereby increasing the relative amount of naphtha sent to the isomerization unit. Thus, in the Economics of the refining efficiency of catalysts for the isomerization of light naphtha is becoming more urgent.

In the US 2939896 B1 reported the isomerization of paraffin hydrocarbons using a catalyst containing platinum, halogen and sulfate of aluminium, magnesium and/or zirconium deposited on activated alumina. However, the patent does not reveal additional metal components of the catalyst. In the US 5036035 B1 reported catalyst and its use in isomerization)containing sulfated oxide or hydroxide of zirconium and platinum group metals. In the patent it is noted that the recovery of platinum group metal is not favorable.

In the US 4918041 B1, US 4956519 B1 and the application EP 0666109 A1 discloses sulfated catalyst comprising an oxide or hydroxide of group III or group IV; the oxide or hydroxide of group V, VI or VII; or the oxide or hydroxide of group VIII. In the applications disclosed a catalyst for isomerization. In 0666109 also reveals a component from the list of metals of group VIII and combinations of metals.

In the US 3915845 B1 discloses a catalyst (and e is on the application), including the platinum group metal, a metal of group IVA, halogen and lanthanide in an atomic ratio to the platinum group metal from 0.1 to 1.25. In the US 5493067 B1 reported that ISO and olefins alkiliruyutza when in contact with solid supercilious, such as sulfated Zirconia, which may contain added metals and added heteroalicyclic or polyoxoanion.

In the US 5310868 B1 and US 5214017 B1 reported catalyst compositions containing sulfated and calcined mixtures of (1) the media containing the oxide or hydroxide of an element of groups IV-A, (2) oxide or hydroxide of a metal of group VI, VII or VIII, (3) oxide or hydroxide of a metal of groups I-B, II-B, III-A, III-B, IV-A or V-A and (4) metal series lanthanides.

In the US 5212136 B1 discloses suitable for alkylation processes solid supercolony catalyst comprising sulfated and calcined mixtures of carrier oxide or hydroxide of an element of groups IV-A, oxide or hydroxide of molybdenum, oxide or hydroxide of a metal of groups I-B, II-B, III-A, III-B, IV-B, V-A or VI-A other than molybdenum or metal of some lanthanides.

Disclosure of inventions

The aim of the present invention is to provide an improved catalyst and method of carrying out reactions in the conversion of hydrocarbons. Another objective of the present invention is to provide improved technologies to increase legro is and gasoline. A more specific goal is to create an improved catalyst and method of isomerization of light naphtha to high octane gasoline component. The invention is based on the discovery that a catalyst containing ytterbium and platinum components, provides better performance and stability isomerization of light naphtha, increasing the content isoparaffins.

Advanced embodiment of the present invention is aimed at catalyst comprising a sulfated carrier oxide or hydroxide of a metal of group IVB (IUPAC 4), mainly of the oxide or hydroxide of zirconium, at least the first component, which is a lanthanide element or yttrium component and at least a second component which is a metal of the platinum group. The first component predominantly comprises one element of a series of lanthanide or yttrium, and the second component mainly consists of one metal of the platinum group. Preferably, the first component was the ytterbium, and a second platinum component. The catalyst may contain a binder, an inorganic oxide, in particular aluminum oxide.

An additional embodiment of the invention is a method of producing the catalyst of the invention by sulfation of the oxide or hydroxide of a metal of the group IVB, incorporating the first component, a lanthanide element, yttrium, or any mixture thereof and the second component, a platinum group metal and preferably linking catalyst refractory inorganic oxide.

In another of its aspects the invention involves the conversion of hydrocarbons using the catalyst of the invention. Still one of the embodiments of the invention includes the isomerization can isomerized hydrocarbons using the catalyst of the invention. The hydrocarbons mainly include light naphtha, which isomerizes with increased content isoparaffinic and octane number, becoming a raw material for producing compounded gasoline.

These and other embodiments will become apparent from the detailed description of the invention.

Additional objectives, embodiments and details of the present invention can be obtained from the following detailed description of the invention.

Brief description of drawings

Figure 1 shows a plot of the degree of conversion of the pentane from the ionic radius for 8-coordination state of a number of catalysts, where the first component is changed catalysts.

Figure 2 shows a plot of conversion of cyclohexane temperature for a number of catalysts. The catalysts of the present invention are compared with contraindicationaverage.

The implementation of the invention

The material of the catalyst carrier of the present invention includes an oxide or hydroxide of a metal of group IVB (IUPAC 4) (see Cotton and Wilkinson, Advanced Inorganic Chemistry, John Wiley & Sons (fifth edition, 1988)). The mostly metal selected from zirconium and titanium, of which particularly preferred zirconium. The preferred oxide or hydroxide of zirconium turn the ignition in crystalline form. The material of the carrier is applied sulfate education (on the assumption, which does not limit the invention) formed by acids Bronsted and Lewis. Component from the lanthanide series of elements incorporate in the composite using any suitable method. Component from the group of platinum metals is added to the catalytic composite using any known in the art processing method of a catalyst, such as impregnation. The catalyst may be associated with any refractory inorganic oxide. For the successful preparation of the catalyst, which can be used for the isomerization of hydrocarbons, media, sulfate, metal components and optional binder used can be entered in the composite in any order.

For preparation of the catalyst carrier of the present invention as a starting material it is possible to use a metal hydroxide IVB (IUPAC 4). Suitable zirconium hydroxide may be, for example, received from the company MEI of Flemington, New Jersey. Alternatively, the hydroxide can be prepared by hydrolysis of the hydroxy-anionic compounds of metals, for example ZrOCl2, ZrO(NO3)2, ZrO(OH)NO3, ZrOSO4, TiOCl2etc. Note that sales ZrOCO3contains significant amounts of HF (1 wt.%). Can also be used alkoxides of zirconium, such as zirconolite and propoxy zirconium. The hydrolysis can be performed using gidrolizuemye agent, such as ammonium hydroxide, sodium hydroxide, potassium hydroxide, sodium sulfate, (NH4)HPO4and others known in the art connection of this kind. Oxy-anionic compound of the metal may, in turn, be prepared from available materials, for example, processing ZrOCO3nitric acid. Purchased or prepared using the hydrolysis hydroxide mostly dried at a temperature of from 100 to 300°With the purpose of evaporation of volatile compounds.

Sulfated media receive treatment appropriate sulfatrim agent with formation of a solid strong acid. The term "supercolony" refers to liquid acids stronger than sulfuric acid. In the literature there are a number of liquid superacids, including substituted proton acid, for example trifluoromethyl who amestoy H 2SO4triftormetilfullerenov, and proton acid activated by Lewis acids (HF+BF3). Although the definition of force liquid superacids developed, the exact force of the solid strong acid to measure with any degree of accuracy is difficult due to the less specific nature of the condition of the surface of solids compared to the fully solvated molecules, which are in the liquid. Accordingly, there is no applicable for all cases, the correlation between the liquid and solid superacids strong acids, as a result, if it is determined that any liquid supercyclone catalyze any reaction, there is no corresponding solid strong acid, which can be automatically chosen for the same reaction. Therefore, in the framework of the representations in the present description, "solid strong acids are acids that are strong acids, higher than the strength of the acid sulfoxylate resin type Amberlyst®-15. In addition, since in the literature, there is disagreement about whether some of these solid acids "superacids", here will be used only defined above, the expression "solid strong acid". Another way of defining the solid strong acid assumes a solid ve is estvo, who are interacting proton, lisowska acid centers. Thus, the solid strong acid can be a combination of Pentecostal (proton) acid and lisowska acid components. In other cases Pentecoste and Lisowski acid components cannot be easily identified or be present as a separate species, although they still meet the above criteria.

The sulfate ion incorporate in the catalytic composite, for example, by treatment with sulfuric acid with a concentration of usually from 0.01 to 10 N. and preferably from 0.1 to 5 N. as alternative sources can be used compounds such as hydrogen sulfide, mercaptans or sulfur dioxide, which can form during annealing of sulfate ions. To ensure the sulfate ions and the formation of a solid acid catalyst, preferably using ammonium sulfate. The sulfur content in the finished catalyst is usually in the range from 0.5 to 5 wt.% and preferably from 1 to 2.5 wt.%. Sulfated composite is dried, and then preferably calcined at a temperature of from 500 to 700°With, especially when sulfotyrosine should the incorporation of the platinum group metal.

The first component includes one or is more of the elements of the series of lanthanides, yttrium, or mixtures thereof, is another essential component of the catalyst of the present invention. A number of lanthanides include lanthanum, cerium, praseodymium, neodymium, promethium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium and lutetium. Preferred elements of the series of lanthanides include lutetium, ytterbium, thulium, erbium, holmium, terbium, and mixtures thereof. Ytterbium is a preferred component of the catalyst of the present invention, and most preferably, the first component consisted essentially of ytterbium component. The first component can in principle be present in the catalytic composite in any catalytically available form, such as the elemental metal, a compound such as oxide, hydroxide, halide, oxychlorine, carbonate or nitrate, or chemical combination with one or more other ingredients of the catalyst. The first component is preferably an oxide, intermetallic with platinum, zirconium sulfate in the lattice. The materials are usually calcined at 600 to 700°and, therefore, they are in oxide form. Although without intent to limit thereby the present invention, assume that the best results are obtained when the first component is present in the composite in the form in which virtually the entire lanthanide and the and threeway component is in oxidation state, higher than the degree of oxidation of elemental forms, for example in the form of oxide, oxychloride or halide, or mixtures thereof, and describe the next stage of oxidation and reduction, which is primarily used in the preparation of this catalytic composite in a special way necessary to achieve this goal. Lanthanide element or yttrium component can be incorporated into the catalyst in any amount which is catalytically effective, in particular from 0.01 to 10 wt.% lanthanide or yttrium, or mixtures thereof in the catalyst based on elements. The best results are usually achieved with 0.05 to 5 wt.% lanthanide or yttrium in the calculation of the elements. The preferred atomic ratio of lanthanide or yttrium to platinum group metal is at least 1:1, preferably 2:1 and especially preferably 5:1 or higher.

The first component to incorporate in the catalytic composite in any known in the art method, such as joint deposition, co-extrusion with a porous material medium or impregnation of a porous material media sulfate before, after or at the same time, although the results achieved are not necessarily the same. To facilitate the work of the lanthanide element and yttrium preferably be incorporated simultaneously with sulfate. The most is it preferable to incorporate the platinum group metal of the latter. As for item number of the lanthanide or yttrium, the order of their entry does not have a significant influence.

One way of applying the first component includes impregnation of the carrier with a solution (mostly water) is able to decompose the compounds of the lanthanide element or elements or yttrium. Under degrade implies that when heated the connection lanthanide element or yttrium becomes lanthanide or yttrium or yttrium oxide with the release of by-products. Examples degrade compounds of lanthanides are suitable complexes or compounds of the lanthanides, such as nitrates, halides, sulfates, acetates, alkyl compounds, hydroxides and the like compounds. The first component can be impregnated in the carrier either prior to, or simultaneously, or after the platinum group metal, although the obtained results are not necessarily the same.

The second component, a platinum group metal, is an indispensable ingredient of the catalyst. The second component includes at least one of the following elements: platinum, palladium, ruthenium, rhodium, iridium and osmium, of which the preferred platinum and particularly preferably a metal of the platinum group consisted essentially of platinum. Component of the platinum group metal may things is painted in the final catalytic composite in the form of such compounds as the oxides, sulfide, halide, oxychlorine etc. in chemical combination with one or more other ingredients of the composite or metal. The preferred amount of the component of the platinum group metal in the range from 0.01 to 2 wt.% in the calculation of the metal. The best results are obtained when almost all of the platinum group metal is present in the elemental state.

The second component is a platinum group metal is applied to the composite using the same tools as in the case described above for the first component. Examples degrade compounds of platinum group metals are chloroplatinate acid, chloroplatinic ammonium bronetankovaya acid, dinitrodiphenylamine, tetranitromethane sodium, trichloride rhodium chloride examinate, carbonylchloride rhodium, hexanitrate sodium, globaldata acid, palladium chloride, palladium nitrate, hydroxide diaminopimelate, chloride tetraamminepalladium, hexachloroiridate(IV) acid, hexachloroiridate(III) acid, hexachloroiridate(III) ammonium, akvaekologiya(IV) ammonium, ruthenium tetrachloride, hexachloroethane, chloride hexaammineruthenium, trichloride osmium and osmium-ammoniate. The second component (platinum group metal) is applied to the media before, after or simultaneously with sulfate and/or the first component, although the floor is anticipated by so the results are not necessarily the same. Preferably the platinum group component deposited on the carrier either after, or simultaneously with sulfate and/or the first component.

In addition to the above first and second components of the catalyst may in some cases further include a third component: iron, cobalt, Nickel, rhenium or mixtures thereof. Preferred is iron, which can be present in amounts from 0.1 to 5 wt.% in the calculation of the element. The third component, such as iron, can reduce the number of the first component, such as ytterbium required in the optimal composition. The third component may be deposited on the composite using the same tools as in the case described above for the first and second components. If the third component is iron, with suitable connections could be the iron nitrate, iron halides, iron sulfate and any other soluble compound of iron.

The above-described catalytic composite may be used in powder form, or it can be attached to various desired shapes such as pills, cakes, extrudates, powders, granules, spheres, etc. which may be of any suitable size. The composite is given a special form using well known in the art means. When giving various forms you may need a mixture of the composite with St. the user. However, it should be emphasized that the catalyst may be manufactured and used with success and without binder. Binder in the case of its application is usually from 0.1 to 50 wt.%, mostly from 5 to 20 wt.% in the calculation of the finished catalyst. Of technology it is known that for the above mentioned purpose can approach any of the refractory inorganic oxide binder. Suitable binder materials of the present invention can be one or more of the following: silica, alumina, silica/alumina, magnesium oxide, zirconium oxide and mixtures thereof. The preferred binder material is alumina (aluminum oxide), and preferred this and/or, in particular, gamma-alumina. Examples of usable binders include (but not limit the invention, alumina, silica, silica/alumina, Zirconia, and mixtures thereof. Typically, composite and optional binder are mixed together with peptizyde agent such as HCl, HNO3, Air CON etc, with the formation of a homogeneous mixture, which form the desired shape using a well-known technique of forming tools. These forming tools are extrusion, spray drying, the addition to the oil, spheroidizing, mixing conical auger, etc. Extrusion tools include screw extruders and extrusion pression tool will determine the need to add to the mixture a quantity of water, if necessary. So, if using extrusion, the mixture must be in the form of the test, while in the case of application of spray drying or addition into the oil to form a suspension will require the presence of a sufficient amount of water. The obtained particles are calcined at a temperature of from 260 to 650°With the passage of time from 0.5 to 2 hours.

One of the embodiments of the catalyst for increased activity, includes the presence of a component of a number of lanthanide or yttrium component (first component)and the metal component of the platinum group (second component) binders, as well as sulfated media from group IVB (IUPAC 4). For example, in this embodiment of the mixed sulfated zirconium oxide and aluminum oxide, which are attached together form, can form the media, and the component number of the lanthanide or yttrium component (first component)and a component from the metals of the platinum group (the second component) may be located on sulfated zirconium oxide, and aluminum oxide carrier, which is attached to the form. Specifically, one catalyst may be sulfated and mixed with alumina, and then converted into a carrier with a specific form with platinum and ytterbium deposited on a mixed media of some form and, after vetelino, located on sulfated zirconium oxide, and aluminum oxide. In this embodiment the catalyst is prepared by the following method.

Sulfated media group IVB (IUPAC 4) prepared as described above. Sulfated carrier is mixed with a binder, such as described above. In this embodiment the mixture of sulfated carrier with a binder to produce before adding the first and second components of the catalytic composite. Mixing can be accomplished by shaking, kneading, rubbing, crushing or suspension. Can be used several ways of mixing, either sequentially or simultaneously. Stage mixing carried out mainly in dry conditions, which are close to the original moisture content of the mixture. Can also be incorporated and a binder agent. The mixture is formed into the shape using well-known means to give shape to that described above. At this stage of the preparation of the carrier of a certain form can be calcined at temperatures ranging from 100 to 900°during the time from 1 to 10 hours.

Next, the calcined carrier with a specific form can be added to the first and second components. As mentioned above, the first component may be applied by application of the carrier solution (mostly water), able is about to decompose compounds lanthanide element or elements or yttrium. The second component (component of the platinum group metals), can be applied to the composite using the same tools that can be used for the first component. The first component can be impregnated in a carrier of some form, either before or at the same time or after the component from the metals of the platinum group, although the obtained results are not necessarily the same. If the components are applied consistently, the catalytic composite between stages of impregnation can be dried. Impregnated carrier of a certain form can be calcined at temperatures ranging from 400 to 800°With the passage of time from 0.5 to 10 hours. The obtained catalyst composite contains the first and second components as sulfated compound of a group IVB (IUPAC 4), and connecting the carrier of a certain form.

In another method of preparation of the catalyst impregnation of the first component in the carrier of sulfated metal of group IVB is performed before mixing with a binder, shaping and annealing. In this way the carrier of sulfated metal of group IVB prepared as described above. The first component is applied by application of the carrier solution (mostly water) is able to decompose the compounds of the lanthanide element or elements or yttrium. The can is to be used any suitable method of impregnation. Impregnated carrier metal of group IVB then mixed with a binder, such as described above. The mixing may be carried out in any known way, including the one described above. Can be used several ways one after the other. Stage mixing carried out mainly in dry conditions, which are close to the source of the moisture. Can also be incorporated and a binder agent. The mixture is formed into the shape using well-known means to give shape to that described above. The carrier of a certain form can be calcined at temperatures ranging from 400 to 900°With the passage of time from 0.5 to 10 hours.

After annealing the second component (component of the platinum group metals may be deposited on the composite using the same method of application, as for the first component. Impregnated molded carrier may be calcined at temperatures ranging from 300 to 650°With the passage of time from 0.5 to 10 hours. The obtained catalyst composite contains a component of the platinum group as sulfated compound of a group IVB (IUPAC 4), and binding media of some form, while the first component is mainly sulfated compound of a group IVB (IUPAC 4) of the carrier. Because of the potential during annealing desorption and repeat the Noah adsorption of the first component may be in a binder medium, but mainly the first component is localized on the sulfated compound of the metal of group IVB (IUPAC 4) of the carrier. Assume that less than 20-30% of the first component will be binding on the carrier. One advantage of this embodiment is that for the preparation of a suitable catalyst requires a smaller total quantity of the first component in comparison with the ways in which the first component added to the mixture of the carrier and a compound of metal of group IVB. The reduction of the required number of leads to lower raw material costs, storage costs and more efficient use of volumetric productivity of used production equipment.

Alternatively, the first component can be applied to sulfated carrier and binder during or after the stage of mixing, during or after the stage of shaping or before the first calcination of the carrier of a certain form. Component platinum group type, as described above, after the first calcination of the carrier of a certain form. In the resulting catalytic composite of the first component and the second component will be detected as a component of a metal of group IVB, and a binder.

The above procedures describe catalyst composites of the present invention, formed on the basis of the su is hatibandha component metal of group IVB. Therefore, sulfated component is localized mainly on the component metal of group IVB of the media and to a lesser extent on connecting carrier. When burning a certain amount of sulfur component can result in desorption and re-adsorption is localized in the media, but I believe that the media will be less than 20-30% of the sulfur component. One advantage of this embodiment is that for the preparation of a suitable catalyst requires a smaller total amount of sulfur compounds in comparison to methods such as those described below. The reduction of the required number of leads to lower raw material costs, storage costs and more efficient use of volumetric productivity of used industrial equipment. Another advantage is that any undesirable interaction between the platinum group metal and the sulfur compound on the carrier is minimized due to the preferential localization of sulfur compounds on the component from the metals of groups IVB, not binding. To minimize such interactions may increase the activity of the catalytic composite.

However, the scope of the present invention allow for the possibility of adding a sulfur component and other IOM the details of the cooking process, although the obtained results in relation to the activity of the resulting catalytic composite is not necessarily the same. For example, the sulfur component may be added (1) after mixing the component group IVB with a binder; (2) after mixing the component group IVB with a binder and shape; (3) after mixing the component group IVB with a binder and shaping and calcination but before applying the first or second components; (4) after mixing the component group IVB with a binder, shaping, annealing and simultaneously with the first, second or both the first and second components.

Another embodiment of the catalyst of the invention is obtained by creating finely peremeshennoi mixture of binder impregnated first and second components and sulfated part of a group IVB, imprintirovannymi the first and second components. The first and second components are added to the binder and to sulfated component of the group IVB, as described above in some ways. A simple mixture of two catalysts is a physical mixture of discrete particles ranging in size from 20 to 60 mesh, as it is widely practiced by experts in the field testing of the catalysts. The mixture was thoroughly stirred, and as a catalyst, and a binder are concatenated together and sieved into a particle size of Maine is e 100 microns. These fine particles are thoroughly shaken and stirred, after which the shape. In thin peremeshennoi phase mixture of sulfated zirconium oxide and binder phase are in closer contact (ranging from tens to hundreds of microns)than the simple physical mixture (in the millimeter range). The resulting catalyst contains both the first and second components on the component of the group IVB and binder.

The catalytic composites of the present invention, as swissitalian and after annealing, can be used as catalysts in the conversion of hydrocarbons. The annealing is necessary for the conversion of the hydroxide of zirconium in the zirconium oxide. Processes for the conversion of hydrocarbons is well known in the art and include cracking, hydrocracking, alkylation of both aromatics and isoparaffins, isomerization, polymerization, reforming, dewaxing, hydrogenation, dehydrogenization, transalkylation, dezalkilirovania, hydration, dehydration, Hydrotreating, hydrodenitrogenation, hydrodesulphurization unit, mahanirvana, the ring opening and the processes of conversion of synthesis gas. Specific reaction conditions and the types of materials that can be used in these processes are described in US 4310440 B1 and US 4440871 B1, which is incorporated into the present application as reference material. Site is titanium process of conversion of hydrocarbons is the isomerization of paraffins.

In the method of isomerization of paraffins total ligroin raw materials boiling in the gasoline range, contains paraffins, naphthenes, and aromatics, and may include small amounts of olefins. To usable raw materials include straight-run naphtha, natural gasoline, synthetic naphtha, gasoline, obtained by thermal cracking, gasoline obtained by catalytic cracking, subjected to partial reforming of the naphtha or refined after extraction of aromatics. The raw material is essentially limited to the entire range of naphtha or outside the boil from 0 to 230°C. Typically, the feedstock is a light naphtha having an initial boiling point of from 10 to 65°and an end boiling point of from 75 to 110°With, preferably, an end boiling point below 95°C.

The main components of the preferred raw materials are alkanes and cycloalkanes having from 4 to 7 carbon atoms in the molecule (C4-C7), mainly C5and C6and may also contain smaller amounts of aromatic and olefinic hydrocarbons. Usually content With7and heavier components in the raw material is below 20 wt.%. Although the total content of cyclic hydrocarbons in raw materials and not limited to special limits, the raw material usually contains from 2 to 40 wt.% cyclic hydrocarbons including naphthenes, and aromatics. Containing the jaś in ligroin raw aromatics, although it is usually less than alkanes and cycloalkanes can be from 2 to 20 wt.% and more and more often from 5 to 10 wt.%. In the preferred raw material the main component of the aromatics is usually benzene, possibly with small amounts of toluene and higher boiling aromatics in the above limits boiling.

The contacting zones isomerization can be carried out using a catalyst system with a fixed bed, a moving bed, a fluidized bed, or by using a batch process. The preferred system is a fixed bed catalyst. Reactive agent can be contacted with the particles of the catalyst layer being involved in upward, downward, or radial flow. In contact with catalyst particles of the reacting substances may be in the liquid phase, a mixed liquid-vapor phase or vapor phase, and excellent results are obtained by implementing the present invention mainly by carrying out liquid-phase process. The isomerization zone may be located in a single reactor or in two or more separate reactors in the presence between them appropriate means to ensure that at the entrance to each zone of the desired temperature isomerization. To provide an improved isomerization p is the control of temperature in individual reactors and partial replacement of the catalyst without interrupting the process preferred two or more series-connected reactor.

The isomerization conditions in an isomerization zone include a temperature of the reactor is typically in the range from 40 to 250°C. is Generally preferable to lower the reaction temperature, which create a equilibrium mixtures of the highest concentration of high-octane highly branched isoalkanes and minimize cracking of the feedstock with the formation of lighter hydrocarbons. For the method of the present invention, the preferred temperature range is from 100 to 200°C. the Operating pressure in the reactor is typically in the range of 100 kPa (abs) to 10 MPa (abs), mainly from 0.3 to 4 MPa (abs). The volumetric rate of fluid is from 0.2 to 25 h-1with the preferred range is from 0.5 to 15 h-1.

Hydrogen mixed with or contained in the paraffin feedstock fed to the isomerization zone, in a molar ratio hydrogen/hydrocarbons from 0.01 to 20, preferably from 0.05 to 5. The hydrogen can come completely from the side or be supplemented by hydrogen that is returned in raw material after separation from the waste stream from the reactor. The hydrogen may contain light hydrocarbons and small quantities of inert substances such as nitrogen and argon. Coming from the hydrogen must remove the water, preferably using a known technique in adsorption systems. In one preferred in which leweni molar ratio of hydrogen to hydrocarbons in the exhaust stream from the reactor is equal to or less than 0.05, that usually helps not to resort to the return of the hydrogen in the raw materials from the waste stream from the reactor.

Upon contact with the catalyst, at least a portion of the paraffinic feedstock is converted in the target high-octane isoparaffin products. The advantages of the catalyst of the present invention are high activity and improved stability. When the first component is chosen ytterbium, the catalyst of the present invention has as an additional advantage of increased activity in the disclosure of cycles.

The isomerization zone is typically also includes a section division, optimally including one or more columns of fractional distillation, with the associated additional devices and separating the light components from enriched in ISO product. Fractional column can also be separated isoparaffinic concentrate from the concentrate of cyclic hydrocarbons, which recycle in the deployment area of the loop.

Preferably, part or all of the amount of enriched ISO product and/or isoparaffin concentrate was mixed to obtain the final gasoline other gasoline components, refining, including (without limiting the invention, one or more of the following components: butane, butenes, pentane, naphtha, a product is atleticheskogo reformer, isomerizate, alkylate, polymer, aromatic extract, heavy aromatics, gasoline catalytic cracking, hydrocracking, thermal cracking, thermal reforming, steam pyrolysis and coking, oxygenates, such as methanol, ethanol, propanol, isopropanol, tert-butyl alcohol, sec-butyl alcohol, methyl tert-butyl ether, ethyl tert-butyl ether, methyl tert-amyl ether and higher alcohols and ethers, and small amounts of additives to improve the stability and homogeneity of gasoline, eliminating corrosion and weather problems, maintain a clean engine and improve vehicle handling.

The following examples serve to illustrate certain specific embodiments of the present invention. These examples, however, should not be construed as limiting the scope of invention defined in the claims. There are many other options understood by the person skilled in the art that fall within the scope of the invention.

EXAMPLE 1

Catalyst samples of table 1 were prepared from zirconium hydroxide obtained by precipitation of zirconolite using ammonium hydroxide at 65°C. the zirconium Hydroxide is dried at 120°and grind up to 40-60 mesh. Prepare several individual portions of zirconium hydroxide. Prepare a solution whether what about ammonium sulphate, or metal salt (component 1) and add to the portions of zirconium hydroxide. Materials briefly stirred and dried by air at 80-100°during the rotation. Thereafter impregnated samples dried for 2 hours in a muffle furnace at 150°in an atmosphere of air. Prepare solutions or ammonium sulfate, or a metal salt (component 2, which is different from component 1) and add to the dried materials. The samples briefly stirred and dried at rotation. After that, the samples calcined for 5 hours at 600-700°C. Prepare solutions chloroplatinic acid for the final impregnation and add to the solid samples. The latter is stirred and dried at rotation, as previously. Samples finally calcined for 2 hours at 525°s on the air. The following table 1 "A" indicates that the catalysts prepared with the contents of the modifier 1 wt.%, 2 wt.%, 3 wt.% and 4 wt.%; "In" indicates that the catalysts prepared with concentrations of sulfate 6 wt.%, 7 wt.% and 8 wt.%, and "C" indicates that the catalysts prepared with concentrations of platinum, 0.25 wt.%, 0.5 wt.%, 0.75% and 1 wt.%.

Table 1
ModifierThe content of the modifierFet SO4
CEA00,47
DyA00,47
ErA00,47
EuA00,47
GdA00,47
ButA00,47
LaA00,47
LuA00,47
NdA00,47
PrA00,47
SmA00,47
TbA00,47
TmA00,47
YA00,47
Yb0,300,37
Yb0,400, 7
Yb0,500,57
Yb100,47
Yb10In
Yb1,80In
Yb200,47
Yb2,70In
Yb300,3757
Yb300,47
Yb3,50In
Yb400,47
Ce110,47
Ce11,50,47
Yb11,50,47
Yb120,47

EXAMPLE 2

The catalysts prepared as described in example 1, and contain 2 wt.% modifier, 0.4 wt.% platinum and 7 wt.% sulphate. Arr is siteline 95 mg of each sample is injected in multiple reactor analyzer. The catalyst is pre-heated within 2-6 hours at 450°in an atmosphere of air and restore using H2at 200°C for 0.5 to 2 hours. After this pass through samples of 8% pentane in hydrogen at 150°From about 1 ATM and a flow rate of 2.5 h-1(per pentane). Products are continuously analyzed by the gas chromatograph and the results obtained are shown in figure 1 (note that tested an exact copy containing ytterbium catalyst). Figure 1 is a plot of degree of conversion of the pentane from the ionic radius for 8-coordination state of some lanthanide or yttrium materials used for the inoculation of platinum catalyst on sulfated zirconium oxide. The ionic radii were determined according to J.E. Huheey, Inorganic Chemistry - Principles of Structure and Reactivity, 2ndEd., Harper & Row: New York, 1978. The graph shows the maximum conversion near 112 picometres (ytterbium). Activity quickly decreases with increasing ionic radius than approximately 115 picometres.

EXAMPLE 3

The catalysts prepared as described in example 1, and the first catalyst (catalyst 1 in figure 2) contains 3 wt.% ytterbium, from 0,375 to 0.4 wt.% platinum and 7 wt.% sulfate; the second catalyst (catalyst 2 in figure 2) contains 1 wt.% ytterbium, from 0,375 to 0.4 wt.% platinum, 1 wt.% is Eliza and 6 wt.% sulfate; the third catalyst (catalyst 3 in figure 2) contains 0.5 wt.% manganese, from 0,375 to 0.4 wt.% platinum and 7 wt.% sulphate. Furthermore, the two control catalyst, of which the first control catalyst contains platinum on sulfated zirconium oxide (catalyst 4 in figure 2), and the second control catalyst contains platinum, iron and manganese on sulfated zirconium oxide (catalyst 5 in figure 2). Approximately 10,5 g of each sample is injected in multiple reactor analyzer. The catalyst is pre-heated within 2-6 hours at 450°in an atmosphere of air and restore using H2for 0.5-2 hours at 200°C. Over catalysts miss the hydrogen and feedstock stream containing 36 wt.% n-pentane, 52 wt.% n-hexane, 10 wt.% cyclohexane and 2 wt.% n-heptane, at 135°C, 150°With, 163°and 176°C, a pressure of approximately 31 ATM and a flow rate of 2 h-1. The molar ratio of hydrogen to hydrocarbon is equal to 1.3. Products are continuously analyzed by a gas chromatograph and determined the degree of conversion of cyclohexane at different temperatures. The results are shown in figure 2, which shows that a significant ability to disclosure cycle demonstrates the catalyst with platinum and ytterbium on sulfated zirconium oxide.

EXAMPLE 4

The powder sulfation the th of zirconium hydroxide, purchased from MEI Corp., grind to powder pseudoboehmite. The mixture impregnorium by spraying with a solution of ytterbium nitrate, maintaining the water content is lower than the initial moisture content of the mixture. Thereafter impregnated materials of a certain form is dried in air and calcined in air at 650°C. Platinum is applied to the material using a wet impregnation followed by calcination at 500°C. the Preparation is repeated with different amounts of platinum and ytterbium, as shown in table 2. The analysis of the catalyst showed that 40% platinum, 10% sulfate and 10% of ytterbium are on alumina matrix, and 60% platinum, 90% of sulfate and 90% of ytterbium are on sulfated zirconium oxide.

EXAMPLE 5

The binder-catalyst according to the present invention prepared using a method similar to the method in example 4. Powder sulfated zirconium hydroxide firms MEI rubbed, producing impregnation by spraying with a solution of ytterbium nitrate. The water content is kept lower than the initial moisture content of the mixture. Thereafter, the impregnated material is dried in air overnight at 100°C, followed by calcination in air at 650°C. Platinum is applied to the material by impregnating the subsequent calcination at 500° C. Data for the main compositions are given in table 2. The entire quantity of sulfate, platinum and ytterbium in the catalyst is in phase of zirconium oxide.

EXAMPLE 6

The catalysts prepared in examples 4 and 5, is tested in the same conditions described in example 3. The molar ratio of 2,2-Dimethylbutane (2,2-DMB) all isomers of hexane, defined as

used as an indicator of catalyst activity and product quality. The received test data are summarized in table 2. The results show that neither the binder modified with ytterbium catalyst or catalysts based on a simple mixture of sulfated Zirconia binder and the size of tens of microns are not as highly effective as catalysts of the invention. The catalyst of the invention exhibits a unique synergistic effect of binder phases and sulfated Zirconia.

Table 2
Example% Pt% Yb%S% binder% 2,2-DMB/S6162°
4-a0,354,81,72024,7
4-In0,35 1,01,72021,1
50,433,01,8021.6

EXAMPLE 7

Mixed particles sulfated zirconium oxide and aluminum oxide prepared as described below.

A typical catalyst for the binder prepared as follows. Powder pseudoboehmite pound and impregnorium solution of ytterbium nitrate and ammonium sulphate. The resulting mixture was calcined for 4 hours at 650°C. Platinum is applied to the material by impregnation with a solution chloroplatinic acid, followed by calcination at 500°receiving the catalyst for the binder.

The above-described catalyst for connecting ground in a ceramic mortar ceramic pestle. Detail sift, receiving a powder size of less than 150 mesh (<100 μm). The powder is thoroughly mixed with the powder of the catalyst based on sulfated zirconium oxide obtained according to example 5, in proportions chosen so that to obtain a certain concentration of aluminum oxide, ytterbium or platinum. The powder mixture is pressed under pressure from 34.5 to 51.7 MPa and sift, receiving particle size 20-60 mesh, which is suitable for testing at the pilot plant isomerization of paraffins.

1. The catalyst comprising sulfates the bath oxide or hydroxide, at least one element of group IVB (IUPAC 4) of the Periodic table to which applied: the first component is selected from the group consisting of an element of the series of lanthanides, mixtures thereof, and yttrium, and a second component comprising at least one platinum group metal and the catalyst additionally contains from 2 to 50 wt.% the refractory inorganic oxide binder, which caused at least one platinum group metal.

2. The catalyst according to claim 1, in which the first component is from 0.01 to 10 wt.% (based on components) from the catalyst, and the second component is from 0.01 to 2 wt.% (based on components) from the catalyst.

3. The catalyst according to claim 1 or 2, wherein the element of group IVB (IUPAC 4) is zirconium, and the refractory inorganic oxide binder is alumina.

4. The catalyst according to claim 1, in which the atomic ratio of the first component to the second component is at least 2.

5. The catalyst according to claim 1, in which the first component is selected from the group consisting of lutetium, ytterbium, thulium, erbium, holmium, yttrium, terbium, and combinations thereof.

6. The catalyst according to claim 1, further comprising a third component, which is selected from the group consisting of iron, cobalt, Nickel, rhenium and mixtures thereof in an amount of from 0.1 to 5 wt.%.

7. The method of preparation of the catalyst, while the one for the conversion of hydrocarbons including sulfated media containing at least one of the oxides and hydroxides of elements of group IVB (IUPAC 4) of the Periodic table, a first component selected from the group consisting of an element of the series of lanthanides, mixtures thereof, and yttrium, and a second component selected from the group of platinum group metals and mixtures thereof, and the catalyst additionally contains from 2 to 50 wt.% the refractory inorganic oxide binder, which caused at least one platinum group metal, and the method includes:

a) the sulfation of oxide or hydroxide of at least one element of group IVB (IUPAC 4) of the Periodic table with the formation of sulfated media;

b) applying the first component;

c) a mixture of sulfated media with a refractory inorganic oxide carrier with the formation of the mixture; and

(d) annealing at a first temperature,

e) applying the second component, and

f) annealing at a second temperature to produce a specified catalyst, where stage (b) can be performed after stage (a), after stage (C) or after stage (d).

8. A method of converting hydrocarbons by contacting the feedstock with a solid acid catalyst comprising a carrier containing an oxide or hydroxide of at least one item is enta group IVB (IUPAC 4) of the Periodic table, the first component is selected from the group consisting of an element of the series of lanthanides, mixtures thereof, and yttrium, and a second component selected from the group of platinum group metals and mixtures thereof, and the catalyst additionally contains from 2 to 50 wt.% the refractory inorganic oxide binder, which caused at least one platinum group metal, resulting in a gain of the converted product.

9. The method of claim 8, where the hydrocarbon conversion is isomerization, the raw material is a paraffin feedstock converted product is a stream with a high content isoparaffins, and the contacting is carried out at a temperature of from 40 to 250°C, a pressure of from 100 kPa to 10 MPa, and the time the volumetric rate of fluid from 0.2 to 25 h-1.

10. The method of claim 8, where the atomic ratio of the first component to the second component is at least 2.

11. The method of claim 8, where the first component is chosen from the group comprising ytterbium, lutetium, thulium, or mixtures thereof, and the second component is platinum.

12. The method of claim 8, where the catalyst further includes a third component selected from the group consisting of iron, cobalt, Nickel, rhenium, and mixtures thereof.



 

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