The preparation method of catalyst for the isomerization of n - paraffin hydrocarbons

 

(57) Abstract:

Usage: in the oil industry, in particular in the production of catalysts for the isomerization of paraffins. The inventive catalyst is prepared by decationization high silica mordenite module 17,5 ammonium chloride to the extent of sharing of 85 to 92% In the obtained zeolite impose platinum from a solution of hexachloroplatinic acid. Mixed with aluminum hydroxide. pre-treated with boric acid and hydroxochloride aluminum mass ratio of Pt-NH4--mordenite:Al2O3-B2O3-Cl (50-70):(30-50). Then treated halogenated compound, molded, dried and calcined. table 1.

The invention relates to methods of making catalysts, in particular catalysts for the isomerization of n-paraffin hydrocarbons, and can be used in the refining and petrochemical industry.

There is a method of preparation of the catalyst for isomerization of n-pentane [1] including dealuminated zeolite mordenite 6N solution of hydrochloric acid to achieve silicate module 16-20, the introduction of platinum without binders. The catalyst obtained by this method, at T 300aboutthe low mechanical strength and low catalyst activity.

There is a method of preparation of the catalyst of hydroisomerization n-C5WITH6-alkanes [2-4] comprising preparing a fluorinated aluminum oxide by introducing fluoride to aluminum hydroxide, forming, drying and calcination of the pellets, the subsequent deposition of platinum on-Al2O3-F, drying, calcining Pt - Al2O3-F, acarnania catalyst. The finished catalyst contains 0,55% Pt and 3.5% F, applied on-Al2O3; a safety factor of 1.0 kg/mm; bulk density of 0.65 g/cm3.

The catalyst hydroisomerization obtained by the method [2-4] at T 360-420aboutC, P 3,5 MPa, Vc2,0 h-1, a molar ratio of hydrogen:h5WITH6-alkanes 3: 1 gidroprevrascheniya n-pentane 50% n-hexane at 70% at the exit side WITH1-C4-hydrocarbons 2,5%

The disadvantages of this catalyst obtained by the method [2-4] is not sufficiently high strength of granules and insufficient isomerise activity towards n-C5WITH6-alkanal.

Closest to the proposed to the technical essence and the achieved effect is the way [5] preparation of the catalyst for isomerization of n-paraffin hydrocarbons WITH5-C4OH, filtering suspensions of zeolite, washing with water from sodium to a residual content of 0.017% Na2O preparation of the xerogel H-mordenite with a silica module 8,7, treated with a solution of aluminum chloride or aluminum nitrate, subsequent treatment with a solution of NH4OH, filtering, shaping, drying, calcining at 500aboutWith, the processing of molded calcined zeolite zirconium chloride and HCl, again drying, calcination, impregnation with solutions of ammonium nitrate and hexachloroplatinic acid, again drying and calcining at 500aboutC.

The catalyst obtained by the method [5] contains, by weight. Pt 0,26; Zn 0,63; Cl 0,04; H-mordenite 85-Al2O3the rest is up to 100%

The catalyst of the composition obtained by the method [5] at T 250aboutC, P 2.0 MPa, Vc1.5 h-1, a molar ratio of hydrogen:hydrocarbon of 1:5 turns selectively n-pentane to isopentane by 46.7% n-hexane in isohexane 62.5%

The disadvantage of this method [5] are the high complexity of the technology of preparation of the catalyst: repeated treatment of the zeolite with different reagents, drying, calcination, and insufficient isomerise the catalyst is obtained by a specified method.

The aim of the invention is prostavlena goal is achieved through the use of high zeolite of the mordenite content of Na2O not more than 0.5% and silicate modulus of 17.5, modification alumina component hydrochloridum aluminum produced in a certain way, followed by the addition of boric acid in the aluminum hydroxide, platinum in NH4-mordenite, offset modified zeolite and alumina component in a certain ratio, shaping, drying and calcining at 550aboutC for 4 h

A common feature of the proposed method of preparation of the catalyst and known methods is mixing the alumina component of the Halogens and the introduction of platinum, forming, Sashka, glowing.

Significant difference between the proposed method and the prototype is the introduction of the catalyst modulus of mordenite in decationizing form with a degree of substitution of sodium 85-93% of a mixture in a ratio of modified platinum mordenite with alumina matrix containing boron and chlorine (the latter is introduced from gidroksokhlorida aluminum), single molding, drying and calcining, which greatly simplifies the technology of preparation and increases isomerase activity and selectivity of the resulting catalyst.

P R I m e R 1. Zeolite-Marla what in the flask with stirrer placed 55 g of zeolite on absolute dry substance.with.in.), poured 500 ml of a 12% solution of NH4Cl, heated to 85aboutWith lead decationization for 1 h followed by filtration and washing of sodium.

In dictionary NH4-mordenite 55 g in terms of and.with.in. enter the acid (H2PtCl6at the rate of 0.5 g Pt, the mixture is stirred in a kneading machine.

The pellet of aluminum hydroxide with a humidity of 82% in the number of 39.5 g on Al2O3treated with 3.5 g H3BO3, stirred at 80-90aboutWith in a kneading machine, enter 100 g hydroxochloride aluminum.

The obtained composition Pt-NH4-mordenite and Al2O3-B2O3-Cl mixed in a kneading machine at a mass ratio of 55:45, weight molded, dried, calcined 4 h at 550aboutC.

The finished catalyst has a composition, by weight. Pt of 0.5; Cl Of 0.7; B2O33,5; H-mordenite 55; -Al2O340,3; a safety factor of 1.7 kg/mm; bulk density of 0.65 g/cm3.

P R I m m e R 2. Zeolite Na-mordenite in the amount of 50 g in terms of and.with. century decationized in 500 ml of 25% solution of ammonium chloride at 125aboutTo the extent the exchange of 92% with stirring for 2 h followed by filtration and washing of the pellet with water.

50 g of decationized 90aboutC for 0.5 hours

47.5 g of Al2O3from tortillas Al(OH)3with the content of Na2O 0,01% injected 1.7 g of N3IN3and 100 ml hydroxochloride aluminum with chlorine concentration of 10 g/l, the mixture is stirred for 0.5 h at 90aboutC.

Components Pt-NH4-mordenite and Al2O3-B2O3-Cl mixed at a ratio of 50: 50, molded, dried and calcined at 550aboutWith 4 hours the Catalyst has a composition, by weight. Pt 0,5; B2O31,0; Cl 1,0; H-mordenite 50; -Al2O347,5; a safety factor of 2.2 kg/mm, bulk density 0,70 g/cm3.

P R I m e R 3. Zeolite Na-mordenite in the amount of 70 g and.with.in. decationized in 500 ml of 25% solution of NH4OH at 125aboutC for 2 h in the mixer followed by filtration and washing from sodium water. The degree of exchange of 92% add H2PtCl6rate of 0.4 g of Pt, and the mixture was stirred at 90about0.5 h

The pellet of aluminum hydroxide with the content of Na2O 0.02% in the number of 27.3 g on Al2O3treated with 2.8 g of N3IN3and 70 ml hydroxochloride aluminum at concentrations of Cl 10 g/L. the Mixture was stirred at 90aboutC for 0.5 hours

Zeolite Pt-NH4-mordenite and cake Al2O3-B2O32O31,6; Cl 0,7; H-mordenite 70; -Al2O327,3; a safety factor of 1.2 kg/mm, a bulk density of 0.62 g/cm3.

P R I m e R 4. The catalyst prepared according to example 1, however, the decationization spend 20% solution of NH4Cl 95aboutWith over 1.5 hours-Degree of exchange of 89% of the Catalyst has a composition, by weight. Pt 0,5; B2O33,5; Cl 0,7; H-mordenite 55; -Al2O340,3, a safety factor of 1.8 kg/mm, a bulk density of 0.68 g/cm3.

P R I m e R 5 (for comparison). The catalyst prepared according to example 1, however, the degree of exchange of the zeolite is mordenite is 82%, the Ratio of Pt-NH4-mordenite/Al2O3-B2O3-Cl 45: 55. The catalyst has a composition, by weight. Pt 0,5; B2O33,5; Cl 0,7; H-mordenite 44,5; -Al2O350,8; a safety factor of 2.4 kg/mm; bulk density of 0.71 kg/cm3.

P R I m e R 6 (for comparison). The catalyst prepared according to example 3, however, the degree of exchange of mordenite 95% at 125aboutWith a 30% solution of NH4Cl. Zeolite partially recrystallized. The ratio of Pt-NH4-mordenite/Al2O3-B2O3-Cl 72: 28.

The catalyst has a composition, by weight. Pt 04; H-mordenite 71,6; Cl Of 0.7; B2O33,3; -Al2O324; the coefficient durable what about the example 1, however, platinum is administered by impregnation of the calcined carrier from a solution of H2PtCl6preliminary processing of the 3% solution of acetic acid.

Samples of the catalysts prepared according to examples 1-7, and the prototype was tested on microprotol nepreryvnolitoy computerized laboratory setup flow type with a flow of hydrogen 500-1000 nl/l in the isomerization of n-paraffin hydrocarbons n-pentane and n-hexane (mixture) at a temperature of 260-285aboutC, a pressure of 1.5 MPa, the space velocity of the raw material of 1.5-2.0 h-1.

The test results in comparison with the data of the prototype shown in the table.

The PREPARATION METHOD of CATALYST FOR the isomerization of N-PARAFFIN HYDROCARBONS, including decationization of mordenite, a hillshade from sodium ions, the introduction of platinum from a solution of hexachloroplatinic acid, a mixture of mordenite with aluminium-containing component, the processing of halogen-containing compound, forming, drying and calcining, wherein the decationization is subjected to high-silica mordenite with a silica modulus of 17.5 and decationization are ammonium chloride to the extent of sharing of 85 to 92% and then injected platinum and mixed with hydroxy the AI Pt-NH4-mordenite Al2O3B2O3- Cl (50 70) (30 50).

 

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