Trimetallic reforming catalyst preparation process

FIELD: petroleum processing catalysts.

SUBSTANCE: catalyst containing platinum, rhenium, antimony, and chlorine on alumina are prepared by impregnation of carrier with aqueous solution of compounds of indicated elements, antimony being deposited as first or second component. Once antimony or platinum-antimony combination, or rhenium-antimony combination deposited, catalyst is dried at 130°C and then calcined in air flow at 500°C. Reduction of catalyst is performed at 300-600°C and pressure 0.1-4.0 MPa for 4 to 49 h. After deposition of antimony or two elements (platinum-antimony or rhenium-antimony) and drying-calcination procedures, second and third or only third element are deposited followed by drying and calcination. Final reduction of catalyst is accomplished in pilot plant reactor within circulating hydrogen medium at pressure 0.3-4.0 MPa and temperature up to 600°C for a period of time 12 to 48 h.

EFFECT: enhanced aromatization and isomerization activities of catalyst and also its stability.

2 cl, 1 tbl, 8 ex

 

The invention relates to the field of preparation of reforming catalysts.

Known methods of preparation of aluminium oxide-platinum reforming catalysts by impregnation of alumina with aqueous solutions containing compounds active ingredients, followed by drying and calcination at temperatures up to 650°C, followed by reduction with hydrogen or a hydrogen-containing gas at a temperature of 250-500° [A.S. USSR №666703, 01J 23/42,1979; A.S. USSR №161694, 01J 11/08, 1963; U.S. Pat. U.S. No. 4485188, 01J 27/02, 1984].

A disadvantage of the known methods of preparation of reforming catalysts is that these methods do not provide a sufficient degree of stability of catalytic activity.

The closest in technical essence of the method of obtaining a metal catalyst on the carrier, containing platinum, rhenium and antimony, is the way [U.S. Pat. Hungary No. 177860, 01J 27/24, 1983], which consists in the impregnation of the support with a solution of the respective metals in the presence of one or more Quaternary ammonium compounds and subsequent recovery of the catalyst.

The disadvantage of this method is not high enough komatsuda and isomerizing activity and stability of reforming catalysts.

The aim of the present invention is to develop a method of preparation of aluminium oxide-platinum the first reforming catalyst, containing rhenium and antimony, which has a high aromatic and isomerizing activity and stability.

This goal is achieved by the proposed method of preparation of aluminium oxide-platinum reforming catalyst, containing, along with platinum rhenium and antimony.

The main feature of the proposed method is that antimony is introduced as the first or second item in the amount of 0.02-1.0 wt.% and recovery of the catalyst is carried out at a temperature of 300-600°and a pressure of 0.1-4.0 MPa for 4-48 hours after administration of antimony and after the final introduction of all metals. This method allows you to increase the flavoring and isomerizing activity of the catalyst and the stability of its catalytic properties.

The proposed method for the preparation of aluminium oxide-platinum reforming catalyst is carried out as follows.

The catalyst containing platinum, rhenium, antimony and chlorine on alumina is prepared by impregnation of the support with aqueous solutions of compounds of these elements. While antimony is applied as the first or second component. After applying antimony, or a combination of platinum-antimony, or rhenium-antimony catalyst is dried at a temperature of 130°and calcined in air flow at a temperature of 500°C. Recovering the catalyst provocate a temperature of 300-600° C and a pressure of 0.1-4.0 MPa for 4-48 hours. After application of antimony or two elements platinum-antimony, or rhenium-antimony and the operation of drying, calcination and restore put the second and third element or only the third element and repeat the drying, calcination. The final recovery of the catalyst is carried out in the reactor of the pilot plant in the environment of circulating hydrogen at a pressure of 0.3-4.0 MPa, temperature up to 600°C for 12-48 hours.

On the catalyst after the restoration is subjected to the reforming of n-heptane. The process is conducted under the following conditions: a pressure of 1.0 MPa; temperature 475°C; volumetric feed rate of n-heptane 2.5 h-1; the molar ratio of hydrogen: n-heptane 5. Determine the composition of the reaction products and the stability of the catalyst, which is defined as the rate of decrease of the catalyst activity (the rate of decrease of the concentration of ISO-heptanol and toluene in the reaction products).

The present invention is illustrated by the following examples.

Example 1.

200 g of alumina (γ-Al2About3) impregnated with 100 ml of an aqueous solution of chloride of antimony, the concentration of antimony in the impregnating solution, 5.0 g/l, the Excess solution is evaporated at a temperature of 75-80°C. the Catalyst is dried at a temperature of 130°and calcined in air flow at 500°C. the Recovery of the catalyst p is avodat in a stream of hydrogen at a temperature of 500° With in 12 hours and a pressure of 1.0 MPa. Next, the catalyst is impregnated with 140 ml of an aqueous solution of hexachloroplatinic and 1.5% solution of hydrochloric acid. The concentration of platinum in the impregnating solution is 5.0 g/L. For a more uniform distribution of the active components in the pellet carrier to the solution was added 1.5% solution of acetic acid. The excess solution is evaporated at a temperature of 75-80°C. the Catalyst is dried at a temperature of 130°C. Then the catalyst is impregnated with 140 ml of aqueous solution of rhenium and a 1.5% solution of hydrochloric acid. The concentration of rhenium in the impregnating solution of 2.86 g/l, the Excess solution is evaporated at a temperature of 75-80°C. the Catalyst is dried at a temperature of 130°C. For a more uniform distribution of the active components in the pellet carrier to the solution was added 1.5% solution of acetic acid. At the end of the impregnation and drying, the catalyst was calcined in a stream of air mixed with 1.5 g/m3carbon tetrachloride in 500°C for 6 hours and a pressure of 0.1 MPa.

The catalyst contains, wt%:

platinum 0.35

rhenium 0.20

antimony 0.25

chlorine 1.1

else γ-Al2About3

The catalyst loaded into the reactor pilot plant reformer and restore the circulating current of hydrogen at a temperature of 500°C for 12 hours and a pressure of 1.0 MPa.

After okonchan who I restore the catalyst to the reforming unit is subjected to n-heptane at a pressure of 1.0 MPa; a temperature of 475°; space velocity heptane 2.5 h-1; a molar ratio of hydrogen: n-heptane 5.

In the reforming of n-heptane get produce that contains 18.4 wt.% ISO-heptanol; 28.2 wt.% toluene; total conversion of n-heptane is 91.2%, the reduction rate of the content in the catalyzate amount of ISO-hexanol and toluene is 0.5 wt./h%.

Example 2.

Application of antimony and recovery of the catalyst is carried out as in example 1. The second dealt element is rhenium, the third element is platinum. The application of these elements and the further preparation of the catalyst is carried out as in example 1. The catalyst contains, wt%:

platinum 0.35

rhenium 0.20

antimony 0.25

chlorine 1.1

else γ-Al2About3

After recovery of the catalyst to the reforming unit is subjected to n-heptane as described in example 1.

In the reforming of n-heptane get produce that contains 19.5 wt.% ISO-heptanol; 27.0 wt.% toluene; total conversion of n-heptane is 91.0%, the reduction rate of the content in the catalyzate amount of ISO-hexanol and toluene is 0.5 wt./h%.

Example 3.

The first dealt element is platinum, which is applied, as in example 1. The catalyst is dried at a temperature of 130°C. Then the catalyst was impregnated with 100 ml of an aqueous solution of chloride of antimony, oncentrate antimony in an impregnating solution of 5.0 g/L. The excess solution is evaporated at a temperature of 75-80°C. the Catalyst is dried at a temperature of 130°and calcined in air flow at 500°C. the Recovery of the catalyst is carried out in a current of hydrogen at a temperature of 500°C for 12 hours and a pressure of 0.1 MPa. The third element is applied rhenium, which is applied, as in example 1. The catalyst was dried, calcined and restore, as in example 1.

After recovery of the catalyst to the reforming unit is subjected to n-heptane as described in example 1.

In the reforming of n-heptane get catalysate, containing 17.5 wt.% ISO-heptanol; 27.5 wt.% toluene; total conversion of n-heptane is 90.5%, the reduction rate of the content in the catalyzate amount of ISO-hexanol and toluene is 0.6 wt./h%.

Example 4.

The first dealt element is rhenium, which is applied, as in example 1. The catalyst is dried at a temperature of 130°C. Then the catalyst was impregnated with 100 ml of an aqueous solution of chloride of antimony, the concentration of antimony in the impregnating solution, 5.0 g/l, the Excess solution is evaporated at a temperature of 75-80°C. the Catalyst is dried at a temperature of 130°and calcined in air flow at 500°C. the Recovery of the catalyst is carried out in a current of hydrogen at a temperature of 500°within 24 hours and a pressure of 4.0 MPa. The third element is applied dps is Tina, which is applied, as in example 1. The catalyst was dried, calcined and restore, as in example 1.

After recovery of the catalyst to the reforming unit is subjected to n-heptane as described in example 1.

In the reforming of n-heptane get produce that contains 17.0 wt.% ISO-heptanol; 28.0 wt.% toluene; total conversion of n-heptane is 90.1%, the reduction rate of the content in the catalyzate amount of ISO-hexanol and toluene is 0.6 wt./h%.

Example 5.

200 g of alumina (γ-Al2About3) impregnated with 100 ml of an aqueous solution of chloride of antimony, the concentration of antimony in the impregnating solution, 0.4 g/l, the Excess solution is evaporated at a temperature of 75-80°C. the Catalyst is dried at a temperature of 130°and calcined in air flow at 500°C. the Recovery of the catalyst is carried out in a current of hydrogen at a temperature of 300°C for 48 hours and a pressure of 1.0 MPa. Further preparation of the catalyst is carried out as described in example 1.

The catalyst contains, wt%:

platinum 0.35

rhenium 0.20

antimony 0.02

chlorine 1.1

else γ-Al2About3

After recovery of the catalyst to the reforming unit is subjected to n-heptane as described in example 1.

In the reforming of n-heptane get produce that contains 16.5 wt.% ISO-heptanol; 26.0 wt.% toluene; General conversion-heptane is 88.1%, the reduction rate of the content in the catalyzate amount of ISO-hexanol and toluene (0.7 wt./h%.

Example 6.

200 g of alumina (γ-Al2O3) impregnated with 100 ml of an aqueous solution of chloride of antimony, the concentration of antimony in the impregnating solution of 20.0 g/l, the Excess solution is evaporated at a temperature of 75-80°C. the Catalyst is dried at a temperature of 130°and calcined in air flow at 500°C. the Recovery of the catalyst is carried out in a current of hydrogen at a temperature of 600°C for 4 hours and a pressure of 1.0 MPa. Further preparation of the catalyst is carried out as described in example 1.

The catalyst contains, wt%:

platinum 0.35

rhenium 0.20

antimony 1.0

chlorine 1.1

else γ-Al2About3

After recovery of the catalyst to the reforming unit is subjected to n-heptane as described in example 1.

In the reforming of n-heptane get produce that contains 20.0 wt.% ISO-heptanol; 25.5 wt.% toluene; total conversion of n-heptane is 89.3%, the reduction rate of the content in the catalyzate amount of ISO-hexanol and toluene is 0.5 wt./h%.

Example 7.

200 g of alumina (γ-Al2About3) impregnated with 100 ml of an aqueous solution of chloride of antimony, the concentration of antimony in the impregnating solution, 5.0 g/l, the Excess solution is evaporated at a temperature of 75-80°C. the Catalyst was dried at those who temperature 130° C. Then the catalyst is impregnated with 140 ml of an aqueous solution of hexachloroplatinic and hydrochloric acids.

The concentration of platinum in the impregnating solution is 5.0 g/L. For a more uniform distribution of the active components in the pellet carrier to the solution was added 1.5% solution of acetic acid. The excess solution is evaporated at a temperature of 75-80°C. the Catalyst is dried at a temperature of 130°C. Then the catalyst is impregnated with 140 ml of aqueous solution of rhenium and a 1.5% solution of hydrochloric acid. The concentration of rhenium in the impregnating solution of 2.86 g/l, the Excess solution is evaporated at a temperature of 75-80°C. the Catalyst is dried at a temperature of 130°C. For a more uniform distribution of the active components in the pellet carrier to the solution was added 1.5% solution of acetic acid. At the end of the impregnation and drying, the catalyst was calcined in a stream of air mixed with 1.5 g/m3carbon tetrachloride in 500°C for 6 hours and a pressure of 0.1 MPa.

The catalyst contains, wt%:

platinum 0.35

rhenium 0.20

antimony 0.25

chlorine 1.1

else γ-Al2About3

The catalyst loaded into the reactor pilot plant reformer and restore the circulating current of hydrogen at a temperature of 500°C for 12 hours and a pressure of 1.0 MPa.

After recovery of the catalyst in the reformer according to the will versaut n-heptane, as indicated in example 1.

In the reforming of n-heptane get catalysate, containing 15.5 wt.% ISO-heptanol; 25.1 wt.% toluene; total conversion of n-heptane is 89.3%, the reduction rate of the content in the catalyzate amount of ISO-hexanol and toluene is 0.9 wt./h%.

Example 8. (for comparison)

200 g of alumina (γ-Al2About3) impregnated with 200 ml of an aqueous solution of chloride of antimony hexachloroplatinic, rhenium and hydrochloric acids. The concentration of antimony in the impregnating solution of 2.5 g/l of platinum 3.5 g/l and rhenium 2.0 g/l, hydrochloric acid, 1.5 wt.%. The application of active elements is carried out in the presence of Quaternary ammonium compounds. The excess solution is evaporated at a temperature of 75-80°C. the Catalyst is dried at a temperature of 130°C. the Catalyst was calcined in a stream of air mixed with 1.5 g/m3carbon tetrachloride in 500°C for 6 hours and a pressure of 0.1 MPa.

The catalyst contains, wt%:

platinum 0.35

rhenium 0.20

antimony 0.25

chlorine 1.1

else γ-Al2About3

Recovery of the catalyst is carried out in a current of hydrogen at a temperature of 500°C for 12 hours and a pressure of 1.0 MPa.

After recovery of the catalyst to the reforming unit is subjected to n-heptane as described in example 1.

In the reforming of n-heptane get catalysate, in which sod is Ritsa 10.7 wt.% ISO-heptanol; 22.7 wt.% toluene; total conversion of n-heptane is 81.2%, the reduction rate of the content in the catalyzate amount of ISO-hexanol and toluene is 1.2 wt./h%.

Thus, it is shown that the preparation of the catalyst according to the proposed method can improve it and isomerizing aromatic activity, and enhance the stability of its work. The results obtained in examples 1-7, presented in the table.

№ p/pThe order of applicationThe antimony content, wt.%Conditions of the first recoveryThe results of the test catalysts
Temperature, ° CPressure, MPaTime, hThe content of ISO-heptanol in catalyzate wt.%The content of toluene in the catalyzate, wt.%The overall conversion of n-heptane, wt.%The reduction rate of the content in the catalyzate Σ ISO-heptanol and toluene, wt./h%
1.Sb-Pt-Re0.255001.01218.428.291.20.5
2.Sb-Re-Pt0.255001.012 19.527.091.00.5
3.Pt-Sb-Re0.255000.11217.527.590.50.6
4.Re-Sb-Pt0.255004.02417.028.090.10.6
5.Sb-Pt-Re0.023001.04816.526.088.10.7
6.Sb-Pt-Re1.06001.0420.025.589.30.5
7.Sb-Pt-Re0.25---15.525.189.30.9
8.Simultaneous application of Sb-Pt-Re0.25---10.722.781.21.2

1. Method of preparation of aluminium oxide-platinum tri-metal catalyst, containing, along with platinum rhenium and antimony, by impregnation of alumina with aqueous solutions of compounds of the corresponding element is in, followed by drying, calcining and recovery, characterized in that, to improve aromatize and isomerizing activity and stability of catalyst, antimony is introduced into the catalyst composition as the first or second item in the amount of 0.02-1.0 wt.%.

2. The method according to claim 1, characterized in that the recovery of the catalyst is carried out after the introduction of antimony at a temperature of 300-600°and a pressure of 0.1-4.0 MPa for 4-48 h after the final injection of all elements.



 

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2 cl, 1 tbl, 8 ex

FIELD: alternate fuel production.

SUBSTANCE: invention relates to synthesis of hydrocarbons from CO and H2, in particular to catalysts and methods for preparation thereof in order to carrying out synthesis of hydrocarbons C5 and higher according to Fischer-Tropsch reaction. Method resides in that non-calcined zeolite ZSM-12 in tetraethylammonium-sodium form is subjected to decationation at pH 5-9, after which decationized zeolite (30-70 wt %) is mixed with alumina binder while simultaneously adding cobalt (7.5-11.5 wt %) as active component and modifier, in particular boron oxide (3-5 wt %). Proposed method allows catalyst preparation time to be significantly reduced owing to combining support preparation and deposition of active component and modifier in one stage with required catalytic characteristics preserved. In addition, method is environmentally safe because of lack of waste waters, which are commonly present when active components are deposited using impregnation, coprecipitation, and ion exchange techniques.

EFFECT: reduced catalyst preparation time and improved environmental condition.

1 tbl, 10 ex

FIELD: petrochemical processes.

SUBSTANCE: catalyst, containing high-silica zeolite of the H-ZSM-5 type having silica modulus SiO2/Al2O3 = 20 to 160 in amount 60.0-90.0%, contains (i) as modifying component at least one oxide of element selected from group: boron, phosphorus, magnesium, calcium, or combination thereof in amount 0.1-10.0 wt %; and (ii) binding agent: alumina. Catalyst is formed in the course of mechanochemical and high-temperature treatments. Described is also a catalyst preparation process comprising impregnation of decationized high-silica zeolite with compounds of modifying elements, dry mixing with binder (aluminum compound), followed by mechanochemical treatment of catalyst paste, shaping, drying, and h-temperature calcination. Conversion of methanol into olefin hydrocarbons is carried out in presence of above-defined catalyst at 300-550°C, methanol supply space velocity 1.0-5.0 h-1, and pressure 0.1-1.5 mPa.

EFFECT: increased yield of olefin hydrocarbons.

3 cl, 1 tbl, 15 ex

FIELD: petroleum processing and catalysts.

SUBSTANCE: invention relates to catalyst for steam cracking of hydrocarbons, which catalyst contains KMgPO4 as catalyst component. Catalyst is prepared by dissolving KMgPO4 precursor in water and impregnating a support with resulting aqueous solution of KMgPO4 precursor or mixing KMgPO4 powder or its precursor with a metal oxide followed by caking resulting mixture. Described is also a light olefin production involving steam cracking of hydrocarbons.

EFFECT: increased yield of olefins, reduced amount of coke deposited on catalyst, and stabilized catalyst activity.

21 cl, 4 tbl, 14 cl

FIELD: hydrocarbon conversion processes and catalysts.

SUBSTANCE: invention, in particular, relates to selectively upgrading paraffin feedstock via isomerization. Catalyst comprises support and sulfated oxide or hydroxide of at least one of the elements of group IVB deposited thereon; a first component selected from group consisting of consisting of lutetium, ytterbium, thulium, erbium, holmium, and combinations thereof; and a second component comprising at least one platinum-group metal component. Catalyst preparation process comprises sulfating oxide or hydroxide of at least one of the elements of group IVB to form sulfated support; depositing the first component onto prepared support; and further depositing the second component. Invention also relates to hydrocarbon conversion process in presence of above-defined catalyst.

EFFECT: improved catalyst characteristics and stability in naphta isomerization process to increase content of isoparaffins.

13 cl, 2 dwg, 1 tbl

FIELD: petroleum processing catalysts.

SUBSTANCE: invention provides gasoline fraction reforming catalyst containing 0.1-0.5% platinum, 0.1-0.4% rhenium, halogen (chorine, 0.7-1.5%, or chorine and fluorine, 0.05-0.1%), and carrier: surface compound of dehydrated aluminum monosulfatozirconate of general formula Al2O3·[ZrO(SO4)]x with weight stoichiometric coefficient x = 0.45·10-2 - 9.7·10-2 and real density 3.3±0.01 g/cm3. Catalyst preparation process comprises preparation of carrier by mixing (i) aluminum hydroxide, from which iron and sodium impurities were washed out (to 0.02%) and which has pseudoboehemite structure, with (ii) aqueous solution of monosulfatozirconic acid HZrO(SO4)OH containing organic components (formic, acetic, oxalic, and citric acids) followed by drying, molding, and calcination. Carrier is treated in two steps: first at temperature no higher than and then at temperature not below 70°C.

EFFECT: enabled production of reforming gasolines with octane number not below 97 points (research method) with yield not less than 86% and increased activity and selectivity of catalyst.

4 cl, 2 tbl, 13 ex

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