Zeolite-containing catalyst, process for its production and method of conversion of aliphatic hydrocarbons in the concentrate of aromatic hydrocarbons or high-octane component of gasoline (options)

 

The invention relates to the refining and petrochemical industries and is dedicated to the creation of the catalysts used in the processing of aliphatic hydrocarbons in the concentrate of aromatic hydrocarbons or high-octane component of gasoline. Described zeolite-containing catalyst contains zeolite group pentasil with silicate module SiO2/Al2About3=55-102 mol/mol and a residual content of sodium oxide of 0.02-0.07 wt.% and oxides of zinc, tin and lanthanum as elements of the structure of the zeolite, and as a promoter oxide of chromium at the following content, wt.%: zeolite 65,0-80,0, ZnO 0,0-4,0, Zi2O30,0-0,8, SnO20,0-2,5, Cr2O30,0-5,0, Na2O 0,02-0,07, the binder component is rest. Describes how to obtain a zeolite-containing catalyst, including hydrothermal synthesis of Na-form of the zeolite with subsequent salt ion exchange and obtain the ammonium form of the zeolite, after which the ammonium form of the zeolite modified with lanthanum, modified by lanthanum ammonium form of the zeolite enter the chromium hydroxide and prepare the catalyst mass which then granularit, dried, calcined at a temperature of 550-600oC. also Described how the pre is NT gasoline (options) by passing a gaseous mixture of low molecular weight saturated hydrocarbons or vapors straight-run gasoline fractions of oil through a bed of the zeolite catalyst. The technical effect of the invention is to increase the degree of conversion of raw materials to the claimed catalyst, as well as the possibility of obtaining the condensed phase concentrate of aromatic hydrocarbons directly from gaseous raw materials, e.g. petroleum gases and a wide fraction of light hydrocarbons. 4 S. p. f-crystals, 5 tab., 1 Il.

The invention relates to the field of oil refining and petrochemical industries and is dedicated to the creation of the catalysts used in the processing of aliphatic hydrocarbons in the concentrate of aromatic hydrocarbons or high-octane component of gasoline.

Known catalyst and method for producing high-octane gasoline and aromatic hydrocarbons (patent RU 96116015 from 23.08.96). The catalyst includes zeolite group Pancasila, oxide of zinc, oxide of rare earth element, a binder component and further comprises an oxide of boron and fluorine, and as a rare earth element or two or more oxides selected from the group of lanthanides: lanthanum oxide, cerium oxide, neodymium oxide, praseodymium oxide, and has the following content, wt.%: zeolite 20-70, zinc oxide 1-4, oxides of rare earth elements 0,1-2,0, boron oxide of 0.1-3.0, fluoride of 0.1 is Kootenay gasoline and aromatic hydrocarbons by contact of them with the catalyst at 280-550oC, a pressure of 0.5 to 3.0 MPa and space velocity of the raw material of 0.5 to 3.0 HR-1.

The disadvantage of this zeolite-containing catalyst is its complex composition, the necessity of application in its synthesis of fluorine, as well as its high cost, due to the use of expensive oxides of rare earth elements.

Known zeolite-containing catalyst for the conversion of aliphatic hydrocarbons to high octane gasoline which is enriched in aromatic hydrocarbons (patent RU 2092240 from 10.10.97). The catalyst contains a zeolite group pentasil with silicate module SiO2/Al2About3=20-80 mol/mol and a residual content of Na2O of 0.1-0.4 wt.%, a binder component, zinc and a mixture of oxides of rare earth elements in the following ratio, wt.%: zeolite 25,0-50,0, zinc 1,0-3,0, the amount of oxides of rare earth elements 0,1-2,0, representing a mixture of the following composition, wt.%: SEO240-55, the amount of La2About3WG2O3Nd2O360-45, the binder component is rest.

The disadvantage of this zeolite-containing catalyst is the high residual content of sodium oxide and low mass fraction of the active part, which considerably reduces its performance horse is of aliphatic hydrocarbons With2-C12in a high-octane component of gasoline or a concentrate of aromatic hydrocarbons (patent RU 96103318 from 16.02.96). The catalyst contains a zeolite group pentasil with silicate module SiO2/Al2O3=20-80 mol/mol and a residual content of Na2O not more than 0.2 wt.%, a binder component, the oxides of zinc and rare earth elements (REE) as promoters, and differs in that it additionally contains patikis phosphorus when used as oxides of rare earth elements of two or more of the following: SEO2, La2About3Nd2O3WG2About3etc. at the following content, wt.%: zeolite 50-75, ZnO 0,5-3,0, sum (REE)Pr2O30,5-3,0, P2O50.5 to 2.0, the binder component is rest. The method of transformation of aliphatic hydrocarbons2-C12in a high-octane component of motor gasoline with an octane rating of at least 76 points by the motor method or a concentrate of aromatic hydrocarbons at this zeolite catalyst is carried out by contact of the catalyst with the feedstock at a temperature 280-550oWith the pressure of 0.2-2.0 MPa and space velocity of the raw material of 0.5 to 5.0 h-1.

The main disadvantage of this is the lack of opportunities for implementing a method of conversion of gaseous aliphatic hydrocarbon composition With2-C4in the condensed phase concentrate of aromatic hydrocarbons. This zeolite-containing catalyst, process for its production and method of its use is chosen as a prototype.

The proposed zeolite-containing catalyst, process for its production and method of conversion of aliphatic hydrocarbons in the concentrate of aromatic hydrocarbons with its use eliminates these drawbacks.

Summary of the INVENTION the Technical result is achieved in that the zeolite catalyst contains zeolite group pentasil with silicate module SiO2/Al2O3=55-102 mol/mol and the oxides of zinc, tin and lanthanum as elements of the structure of the zeolite, and as a promoter of the chromium oxide in the following ratio, wt. %: zeolite 65,00-80,00, ZnO 0-4,00, SnO20-2,50, La2O30-0,80, CR2O30-5,00, Na2O 0,02-0,07, the binder component is rest. For obtaining zeolite-containing catalyst of the composition provide the preparation of the reaction mixture, obtained by mixing aqueous solutions of salts of aluminum, zinc, tin, sodium hydroxide, silica (in the presence of seed crystals of zeolite with structure of ZSM-5 in Na+or N in the autoclave, where at a temperature of 160-190oC and stirring for 6-12 h hydrothermal synthesis of Na-form of the zeolite.

After completion of the synthesis of a pair of n-butanol and water is distilled off and condense when cooled to room temperature, and the formed water-butanediol condensed phase return to the operation preparation of the reaction mixture. Formed after filtration of the pulp residue Na-form of the zeolite is washed first with an aqueous solution ammonium salts, then drinking water. A smaller part of the sludge is used as the seed crystals of zeolite on the operation of preparing the reaction mixture, and the resulting washing solutions are directed to the operation of the disposal of salts. The main part of the sediment Na-form of the zeolite is directed to the operation of the salt ion exchange and carried out by treatment with an aqueous solution of ammonium chloride under heating and stirring of the pulp. The slurry is filtered, the precipitate ammonium form of the zeolite is washed with demineralized water to a residual content of sodium oxide 0.03 to 0.09 wt.% The filtrate and the washing water used in the operation of washing the precipitate Na-form of the zeolite. The washed precipitate ammonium form of the zeolite modified with lanthanum by EA. The slurry is filtered, and the obtained residue modified lanthanum ammonium form of the zeolite is washed with demineralized water. The washing water is mixed with lanthanum-containing mother liquor operations modification of lanthanum, add to them the ammonium carbonate and precipitated carbonate of lanthanum, which returns to the operation of the modification of lanthanum ammonium form of the zeolite. Formed after the deposition of lanthanum carbonate mother liquor is directed to the operation of washing the precipitate Na-form of the zeolite, and the washed precipitate the modified lanthanum ammonium form of the zeolite is directed to the operation of promoter - chromium hydroxide and preparation of a catalyst mass. The input promoter and the preparation of a catalyst mass is carried out by mixing the modified lanthanum ammonium form of the zeolite with an active aluminum hydroxide (boehmite), active chromium hydroxide and a solution of nitric acid. The obtained catalyst mass is subjected to extrusion, pelletizing, the pellets are dried and calcined at a temperature of 550-600oC. Removed during the calcination of the catalyst granules absorb ammonia water, an aqueous solution of ammonia is neutralized with hydrochloric acid, the resulting solution of chloride of ammo who have a fraction of the finished catalyst, and the fraction <3 mm, crushed to powder and return to the operation preparation of a catalyst mass.

The technical result regarding methods based on the use of the proposed zeolite-containing catalyst for the conversion of aliphatic hydrocarbons in the concentrate of aromatic hydrocarbons or high-octane component of gasoline, is achieved by passing a gaseous mixture of low molecular weight saturated hydrocarbons (raw materials) through the catalyst bed heated to a temperature of 500-600oWith, when the load of the catalyst raw materials 100-400 h-1with the conversion of raw materials 94-100%, the selectivity of the formation of aromatic hydrocarbons 54,1-60.2% and the yield of aromatic hydrocarbons in the final product 50,9-60,2%.

The technical result in relation to the method based on the use of the proposed zeolite-containing catalyst for producing high-octane component of gasoline, is achieved by passing vapors of straight-run gasoline fractions of crude oil (raw material) through the catalyst bed heated to a temperature of 300-380oWith, when the load of the catalyst raw materials 2 h-1and the yield of the final product is not less than 67%.

The advantages of the proposed ceritadewasa is the'antan (the sum of the oxides of rare earth elements in the method prototype is 0.5 to 3.0 wt.% in the proposed method, not exceeding 0,8% by weight) and low content of sodium oxide (content of Na2O method-prototype <0.2 wt.% in the proposed method is 0.02 - 0.07 wt.%) and opportunities with it condensed phase concentrate of aromatic hydrocarbons directly from low molecular weight gaseous hydrocarbons, for example petroleum gases and a wide fraction of light hydrocarbons (NGL).

The drawing is a flow diagram of receipt of the zeolite catalyst.

Further, the invention is illustrated with specific examples of its implementation: Example 1. Implementation of the method of producing zeolite-containing catalyst is carried out in accordance with the technological scheme of production of the zeolite catalyst. To cook in the intermediate tanks prepare aqueous solutions of aluminum nitrate, zinc nitrate, chloride, tin (IV) and sodium hydroxide. In the capacity of 500 ml, equipped with a mechanical stirrer, enter 87 ml of water and with vigorous stirring, 50 g of crushed silica gel, 133,5 ml of sodium hydroxide solution with a concentration of sodium hydroxide 94 g/l, 23 ml of a solution of nitrate of aluminium with aluminium concentration of 26 g/l, 48,75 ml solution of zinc nitrate with a concentration of zinc 21 g/l, x 16.75 ml of the autoclave, and in the vacant capacity is administered to 43.5 ml of water and with vigorous stirring, 2,12 g of seed crystals of zeolite obtained after washing the Na-form of the zeolite. The resulting slurry is pumped into the autoclave.

Prepared reaction mixture was kept in an autoclave at 160-190oFrom within 6-12 hours After completion of the hydrothermal synthesis of Na-form of the zeolite disable the heating of the autoclave and produce a distillation of the water-butanone mixture, a pair of which is cooled and condensed phase water-butanone mixture used in the operation of preparing new reaction mixture.

Obtained after synthesis slurry Na-form of the zeolite is filtered, the filtrate is sent to the operation of the disposal of salts. Sediment Na-form of the zeolite sequentially washed with aqueous solution of ammonium salts, and then with water drinking. Washing solutions are directed to the operation of the disposal of salts. The ratio of the liquid and solid phases (W:T) when washing the Na-form of the zeolite is 20: 1. The washed precipitate Na-form of the zeolite is directed to conducting salt ion exchange.

In a volume of 500 ml by intensive mixing Rasulova sediment Na-form of the zeolite in 223 ml of a solution of chloride imovane within 4-6 hours

Obtained after salt ion exchange slurry was filtered, the filtrate is directed to the operation of washing the Na-form of the zeolite. Sediment ammonium form of the zeolite is washed with demineralized water at a ratio of liquid and solid phases W: T= 20:1 and is directed to the operation of the modification of lanthanum. Wash water is directed to the operation of washing the Na-form of the zeolite.

The operation of the modification of the ammonium form of the zeolite by lanthanum carried out in a volume of 500 ml by raspolirovyvayut sediment ammonium form of the zeolite in 170 ml of a solution of lanthanum nitrate with a concentration of lanthanum 1.5 g/l, which was added 0.16 ml of a solution of nitric acid of a concentration of nitric acid 80 g/L. the resulting slurry is maintained at 90-100oC and stirring for 3-4 hours

Obtained after inoculation with lanthanum slurry is filtered, lanthanum-containing mother liquor is directed to the operation of the deposition of lanthanum carbonate. Precipitate the modified lanthanum ammonium form of the zeolite is washed with demineralized water at a ratio of liquid and solid phases W:T=20:1 and is directed to the operation of preparation of a catalyst mass. Wash water is directed to the operation of the deposition of lanthanum carbonate. In Obyedinennaya form of zeolite is added 2 g of ammonium carbonate and thereby precipitated carbonate of lanthanum, which is filtered and directed to the operation of the modification of lanthanum ammonium form of the zeolite. The mother liquor obtained after deposition of carbonate of lanthanum, directed to the operation of washing the Na-form of the zeolite.

The washed precipitate the modified lanthanum ammonium form of the zeolite is mixed with 50 ml of demineralized water to the resulting mixture add 24 g of active aluminum hydroxide in the form of a wet paste (with a residual mass fraction of moisture 28,4%), 11.2 g of active chromium hydroxide and 10 ml of nitric acid with the concentration of nitric acid 80 g/L. the resulting mixture is stirred until a homogeneous plastic catalyst mass suitable for extrusion and granulation of the catalyst.

Obtained after extrusion and pelletizing of raw granules of the catalyst is dried at lattice pallets at a temperature of 100-110oC for 10-12 hours. The dried granules of the catalyst is calcined at a temperature of 500-600oC for 30 minutes. Released during the calcination of the pellets absorb gaseous ammonia water. The resulting aqueous solution of ammonia-neutralized aqueous solution of hydrochloric acid. An aqueous solution of ammonium chloride is directed to the operation of the salt ion asewu. The fraction of the finished catalyst is separated and the fraction of granules of catalyst <3 mm is directed to the grinding operation, which is carried out in the vortex mill to obtain a homogeneous powder. This powder is used for operations preparation of a catalyst mass.

The proposed technology of granulated zeolite catalyst is closed, because almost all uterine solutions and rinse water is not discharged, and fully returned to the process.

Example 2. Straight-run gasoline fraction oil (73,1 wt.% paraffins, of 14.8 wt.% naphthenes, 8.5 wt.% aromatic hydrocarbons, octane 55 points on the research method) is subjected to contacting with a zeolite-containing catalyst placed in the reactor with a volume of 5 cm3at a temperature of 300-380oC, space velocity of the liquid raw material 2 h-1and atmospheric pressure. The catalyst contains 71,85 wt.% the zeolite of the structure type ZSM-5, containing in its structure zinc and containing as a promoter oxide of chromium.

Zeolite-containing catalyst was prepared according to the technological scheme described in example 1. Qualitative and quantitative composition of the zeolite catalyst preprimer 3. Similar to example 2, only as the zeolite component of the zeolite catalyst is zeolite structure of ZSM-5, containing in its structure the tin and lanthanum.

Zeolite-containing catalyst was prepared according to the technological scheme described in example 1. Qualitative and quantitative composition of the zeolite catalyst are presented in table 1. Output group composition and octane number of the gasoline obtained are given in table 2.

Example 4. Prepared samples of zeolite-containing catalyst according to the technological scheme described in example 1. In the five samples were selected zeolite catalyst characterized by a residual content of Na20. The component content of the zeolite catalyst in all samples was the same and amounted in wt.%: SiO272,59-72,69, Al2About3of 1.87-1.97 of ZnO 1,95-2,05, SnO21,95-2,05, La2About30,51-0,61, the amount of binder component depended on the residual content of Na2A. All samples were tested in the process of conversion of hydrocarbons With2-C4in the concentrate of aromatic hydrocarbons in equal conditions: a gaseous mixture of low molecular weight saturated hydrocarbons (raw) (2.2 wt.% Atenea at a temperature of 550oC, space velocity of the feedstock 100 h-1and atmospheric pressure. Before making process the samples of zeolite-containing catalyst was subjected to oxidation treatment in a stream of oxygen-containing gas with the subsequent reduction treatment in hydrogen flow. After the end of the process analyzed the degree of conversion of raw materials into a final product (X, wt. %), the selectivity of the formation of aromatic hydrocarbons (Sap, wt. %) and mass content of aromatic hydrocarbons in the final product (ar, wt.%). The results are presented in table 3.

As follows from the obtained results, the decrease of the residual content of Na2O in the samples of zeolite-containing catalyst significantly increases its activity. However, the decrease of the residual content of Na2O to a value of less than 0.02 wt. % useless because it has almost no influence on the parameters of the conversion process. At the same time, the residual content of Na2O in the sample should not be greater than 0.07 wt.% because it leads to a sharp reduction in the activity of the zeolite catalyst.

Example 5. Prepared samples of zeolite-containing catalyst according to the technological scheme, ausina on silicate module zeolite component. The component content of the zeolite catalyst in all samples was the same and amounted, wt.%: ZnO 1,97-2,03, SnO21,97-2,03, Na2O 0,023-0,025, La2About30,53-0,59, a binder component 20,83-20,89, the rest - SiO2and Al2About3in different molar ratio. All samples were tested in the process of conversion of hydrocarbons With2-C4in the concentrate of aromatic hydrocarbons in equal conditions described in example 4. After the end of the process analyzed the degree of conversion of raw materials into a final product (X, wt.%), the selectivity of the formation of aromatic hydrocarbons (Sap, wt.%) and the mass content of aromatic hydrocarbons in the final product (ar, wt.%). The results obtained are presented in table 4.

As follows from the data presented in table 4, the high catalytic activity of the zeolite catalyst is typical for samples with silicate module SiO2/Al2About3zeolite component from 55 to 102 mol/mol. The decline silicate modulus less than 55 mol/mol or an increase of more than 102 mol/mol leads to a reduction in the degree of conversion of raw materials and reduction in mass content aromatechnologies scheme, described in example 1. The content of the catalyst components was, wt. %: SiO272,64, Al2About31,92, ZnO 2,00, SnO22,00, PA2About 0,024, La2O3of 0.56, a binder component 20,86. To compare the activity of the prepared zeolite catalyst were used: zeolite-containing catalyst according to the prior art (patent RU 96103318 from 16.02.96; catalyst company "Tomiris") and industrial zeolite catalyst IR-30. All samples were tested in the process of conversion of hydrocarbons With2-C4in the concentrate of aromatic hydrocarbons in equal conditions: a gaseous mixture of low molecular weight saturated hydrocarbons (raw) (2.2 wt.% ethane, 73.7 wt.% propane, 24,1 wt. % i - and n-butane) was subjected to contacting with samples of the zeolite catalyst at a temperature of 600oC, space velocity of the feedstock 100 h-1-400 h-1and atmospheric pressure. Before making process the samples of zeolite catalysts were subjected to oxidation treatment in a stream of oxygen-containing gas with the subsequent reduction treatment in hydrogen flow. After the end of the process analyzed the degree of conversion of raw materials into a final product (X, wt.%), the selectivity of the formation of aromatic the img src="https://img.russianpatents.com/chr/969.gif">ar, wt.%). The results are presented in table 5.

From the data presented in table 5, it is seen that the conversion of raw materials for the inventive zeolite catalyst at different volumetric flow rates of the raw material is 94-100%, while other tested zeolite-containing catalysts showed a lower degree of conversion of raw materials, decreasing with increasing space velocity of the raw material. The most sensitive to changes in flow rate of the feed was zeolite catalyst IR-30. Mass content of aromatic hydrocarbons in the final product in the conversion was observed when using the inventive zeolite catalyst and 60.2 wt.% is 50.9 wt.% when the space velocity of the feedstock 100 h-1-400 h-1respectively. Mass content of aromatic hydrocarbons in the final product when using other zeolite catalysts were lower and ranged from 12.0 wt.% to 21.4 wt.% significantly less compared with the values obtained for the inventive zeolite-containing catalyst.

Claims

1. Zeolite catalyst for transformation and is, aderrasi zeolite group pentasil with a residual content of sodium oxide, a binder component, an oxide of zinc, oxide of rare earth element and a promoter, wherein the zeolite catalyst contains a zeolite with silica module SiO2/Al2O3=55-102 mol/mol and a residual content of sodium oxide of 0.02-0.07 wt.%, the oxides of zinc, lanthanum and tin as an element of the structure of the zeolite component, and as a promoter of the chromium oxide in the following content, wt.%: zeolite 65,0-80,0; ZnO 0,0-4,0; Li2O30,0-0,8; SnO20,0-2,5; Cr2O30,0-5,0; Na2O 0,02-0,07, the binder component of the rest.

2. A method of obtaining a zeolite-containing catalyst, comprising the operations of mixing the reagents, hydrothermal synthesis, washing, drying and calcination of the precipitate, wherein using the reaction mixture obtained by mixing aqueous solutions of salts of aluminum, zinc, tin, sodium hydroxide, silica gel, seed crystals of zeolite with structure of ZSM-5 in Na+or NH+4forms, amendment, for example,n-butanol, loaded into an autoclave in which carry out hydrothermal synthesis at a temperature of 160-190With in the course the Ares when cooled to room temperature and the return of the condensed phase on the operation of preparing the reaction mixture, formed after filtering the slurry obtained by the hydrothermal synthesis, the precipitate PA-form zeolite is washed first with a solution of ammonium salts, then drinking water, a smaller part of the sludge is used as the seed crystals of zeolite on the operation of preparing the reaction mixture, the filtrate and washing solutions are directed to the operation of the disposal of salts, and the main part of the sediment Na-form of the zeolite is directed to the operation of the salt ion exchange by treatment with an aqueous solution of ammonium chloride by heating and stirring the slurry, the slurry is filtered, the precipitate ammonium form of the zeolite is washed with demineralized water to a residual content of sodium oxide 0.03 to 0.09 wt.%in terms of the dried and calcined product, the filtrate and the washing solutions used for flushing the Na-form of the zeolite, the washed precipitate ammonium form of the zeolite modified with lanthanum by contacting it with an aqueous solution of lanthanum nitrate, acidified with nitric acid, by heating and stirring the slurry, the slurry is filtered, the precipitate modified lanthanum ammonium form of the zeolite is washed with demineralized water, lanthanum-containing uterine dissolve ammonium for the deposition of carbonate of lanthanum, which is directed to the operation of the modification of lanthanum ammonium form of the zeolite, and the mother solution with the operation of the deposition of lanthanum carbonate is directed to the operation of washing the precipitate Na-form of zeolite modified with lanthanum ammonium form of the zeolite is directed to the operation of promoter and preparation of a catalyst mass by mixing a modified lanthanum ammonium form of the zeolite with an active aluminum hydroxide - boehmite active chromium hydroxide and a solution of nitric acid, the obtained catalyst mass is subjected to extrusion and pelletizing, the pellets are dried and calcined at a temperature of 550-600With formed during the calcination of the pellets of zeolite-containing catalyst ammonia absorb drinking water, aqueous ammonia is neutralized with hydrochloric acid, the resulting solution of ammonium chloride is directed to the operation of the salt ion exchange of the calcined granules of zeolite-containing catalyst classify, separate faction ready zeolite-containing catalyst, and the fraction of granules < 3 mm, crushed to powder and return to the operation preparation of a catalyst mass.

3. The method of transformation of aliphatic pleva is evanie and passing the raw material through the zeolite-containing catalyst, characterized in that is used as raw material gaseous mixture of low molecular weight saturated hydrocarbons, which is passed through the layer of zeolite-containing catalyst according to p. 1 heated to a temperature of 500-600With, when the load of the zeolite catalyst raw materials 100-400 h-1.

4. A way of turning straight-run gasoline fractions of crude oil into high-octane component of gasoline using a zeolite-containing catalyst, comprising heating and passing the raw material through the zeolite catalyst, characterized in that is used as raw material of the pair of straight-run gasoline fraction of oil that is passed through the layer of zeolite-containing catalyst according to p. 1 heated to a temperature of 300-380With, when the load of the catalyst raw materials 2 h-1.

 

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