The activation method palladium catalyst

 

(57) Abstract:

Usage: petrochemicals, isomerization of butene-1 in the butenes-2. The inventive palladium catalyst on the carrier activated by treatment with a mixture of hydrogen and from 0.5 to 7.5%. vol.% of carbon monoxide at 120-250°C. the Characteristics of the catalyst: conversion of butene - 1 82,7-95,0%; selectivity 94,7 of 97.8%. table 1.

The invention relates to the field of petrochemical industry, specifically to methods of structural isomerization of butene-1 in the butenes-2 in the presence of palladium catalyst on the carrier. The invention relates to the production of olefins, in particular of receipt of butenes-2, representing a mixture of TRANS - and CIS-isomers of normal structure, used in the manufacture of butadiene, methyl ethyl ketone, and for other purposes.

Known catalysts structural isomerization of butene-1 - metals of group VIII (Vi, Co, Fe, Pd, Rh) on the media, which allow for the isomerization of butene-1 in the butenes-2 at low temperatures (below 100aboutC), but with insufficient depth conversion - 70-80% and a selectivity of 80%, due to active leakage adverse reactions of hydrogenation, cracking and skeletal isomerization of butene-1.

It is known that activation or reaction is e hydrogen at a temperature of 80-480aboutC.

The closest in technical essence and the achieved result is the activation method palladium catalyst on activated carbon by passing hydrogen through the catalyst bed, which allows the subsequent conduct isomerization of butene-1 at 80-200aboutC and a flow rate of 500-1000 h-1with a conversion of 82% and a selectivity of 92% (the prototype).

The disadvantage of this method is the low productivity of the catalyst raw materials (low activity) and the lack of selectivity of the process.

The purpose of the invention to increase the activity and selectivity of palladium catalyst on a carrier.

This goal is achieved by the proposed method of processing palladium catalyst on a carrier with a mixture of hydrogen and carbon monoxide content of 0.5 to 7.5% vol. of carbon monoxide at 120-250aboutC.

Distinctive features of the method are the treatment of the catalyst with a mixture of hydrogen and carbon monoxide content of 0.5 to 7.5% vol. of carbon monoxide at 120-250aboutC.

As a source of hydrogen using the hydrogen-containing gas, comprising at least 50 vol.% hydrogen and inert impurities (nitrogen, methane, ethane, etc.). Oxide and its content above 7.5% decrease in activity and selectivity of the process.

As a carrier for the palladium used aluminum oxide or activated carbon in the form of grains or pellets.

The method is as follows. The catalyst in the form of immobile layer is loaded into the reactor, representing a metal tube heated purge the system with nitrogen and serves the hydrogen-containing gas. The reactor is heated from 5 to 10aboutper hour up to the activation temperature 120-250aboutC and maintain the temperature selected within the specified limits, for 10-30 hours, then cooled in a stream of hydrogen containing gas to a predetermined operating temperature isomerization. The specified processing of the catalyst is carried out at elevated pressure, and the lower limit of the pressure is determined by the resistance of the catalyst layer, and the upper and technological needs.

On activated as described palladium catalyst serves butene-1 or a hydrocarbon fraction containing butene-1 and hydrogen at a ratio of butene-1: hydrogen equal to 10-100 mol/mol.

The process of structural isomerization of butene-1 is carried out at a temperature of 80-160aboutC and a pressure of not more than 10 ATM with volumetric feed rate of the hydrocarbon feedstock 1000-5000 h-1(the volumetric rate of Rotana-1 82,7-95% with a selectivity 94,7 of 97.8%.

The possibility of implementation of the method is confirmed by the following examples.

The results of the experiments are summarized in table, where the conditions of activation of the catalyst and results from testing of the catalyst in the isomerization process.

P R I m e R 1. Charged to the reactor 10.0 cm3palladium catalyst (2.5 wt. % palladium on aluminium oxide), purge it with nitrogen, and then served bogorodskii gas of the following composition,%: Hydrogen 85 Oxide 5 carbon, Nitrogen, methane, ethane, argon Others

Noah in the amount of 100 nl/h at a pressure of 10 ATM. Heat the reactor from room temperature to 250aboutWith raising temperature speed 8-10about/hour. At a temperature of 250aboutTo maintain the catalyst for 10 hours, then cooled to 110aboutWith and reduce the pressure to 5 ATM.

Through the catalyst passed 900 g of butene-1 (basic substance content 99% ) with a bulk velocity of 5000 h-1; simultaneously feeding hydrogen in an amount such that the molar ratio of butene-1:hydrogen was 100 mol/mol.

Get 901,6 g of product containing, g: Butene-1 44,0 Amount of TRANS - and CIS-butene-2 802,0 n-butane 46,6 Impurities 9.0 Degree of conversion of butene-1 is 95,1% when the selective behaviour is on charcoal), purge it with nitrogen, and then serves the hydrogen-containing gas of the following composition,%: Hydrogen 92.0 Monoxide 0.5 Nitrogen, methane and other inert impurities Others

Noah in the amount of 50 nl/h at normal pressure. The reactor is heated to 120aboutWith heating rate of 4-5aboutC/hour. At a temperature of 120aboutTo activate the catalyst for 24 h, after which the reactor is cooled to 80aboutC. Through the reactor is passed 500 g of butylene-isobutilene fraction of the following composition, wt. % : Butene-1 40,0 n-butane 12,0 isobutylene 32,0 Isobutane 13.5 Divinyl 0,5 other hydrocarbons 2.0 isomerization Process is carried out at 80aboutC, a pressure of 1.2 ATM. with volumetric feed rate 1000 h-1and hydrogen in an amount of 0.1 mol per 1 mol of butene-1.

Get 500,5 g hydrocarbon fraction of the following composition, wt.%: Butene-1 7,0 Amount of TRANS - and CIS-butene-2 32,0 n-butane 13.5 isobutylene 31,9 Isobutane 13,6 other hydrocarbons 2.0 Conversion of butene-1 in these conditions is 82,7% with selectivity to 95.5%.

P R I m e R 3. Charged to the reactor 10 cm3palladium catalyst (1.6 wt. % palladium on aluminium oxide), purge it with nitrogen, and then serves the hydrogen-containing gas of the following composition,%: Hydrogen 90,0 carbon Monoxide 2,5 Ine is the temperature with a speed of 7-8aboutC/hour. At a temperature of 200aboutWith continued activation of the catalyst for 30 h, after which the reactor is cooled to 120aboutC. Through the reactor is passed 1000 g of butene-1 (basic substance content 99%) with a bulk velocity of 2500 h-1, feeding simultaneously hydrogen in an amount such that the molar ratio of butene-1:hydrogen was 50 mol/mol. Get 1000,7 g of product containing Butene-1 70,0 Amount of TRANS - and CIS-butene-2 900,0 n-butane 20,7 Impurities 10.0 Conversion of butene-1 is of 92.9% with the selectivity of the process of 97.8%.

P R I m e R 4. The process is carried out analogously to example 1 with the only difference that the activation of the palladium catalyst is carried out in a current of hydrogen-containing gas of the following composition,%: Hydrogen 90,0 carbon Monoxide 7,5 Inert impurities 2.5 Degree of conversion of butene-1 is 92,5% with the selectivity of the process is 97.6%.

P R I m e R 5. The process is carried out analogously to example 1 with the only difference that during activation, the catalyst is heated to 300aboutC and incubated for 10 h at this temperature.

Through the reactor is passed 500 g of butene-1 (basic substance content 99%) under the same conditions as in example 1.

Get 500,9 g of product containing, g: the effectiveness of the process in 94.7%, i.e. increasing the activation temperature from 250 to 300aboutWith virtually no effect on the activity and selectivity of the catalyst.

P R I m e R 6. The process is carried out similarly to the conditions of example 1 with the only difference that passed through the catalyst 900 g of butene-1 with a bulk velocity of 7000 h-1.

The conversion of butene-1 is of 91.3% with a selectivity of 94.5%.

P R I m e R 7. The process is carried out analogously to example 1 with the only difference that the activation of the palladium catalyst is carried out in a current of hydrogen-containing gas of the following composition,%: Hydrogen 85,0 carbon Monoxide 10,0 Inert impurities 5,0

The conversion of butene-1 is 67,1 when selectivity to 78.3%, i.e. an increase in the content of carbon monoxide above stated results in decreased conversion of butene-1 and the selectivity of the process.

P R I m e R 8. The process is carried out similarly to the conditions of example 1 with the only difference that the activation of the catalyst is carried out at a pressure of 15 ATM. After activation through the reactor is passed 900 g of butene-1 in the same conditions as in example 1, obtaining the same results in the conversion of butene-1 and the selectivity of the process.

P R I m e R 9. The process is carried out analogously to example 2 with that is passed 500 g of butene-1 in the same conditions, as in example 4.

Get 500,6 g of product containing, g: Butene-1 250,0 Amount of TRANS - and CIS-butene-2 209,0 n-butane 16,0 Impurities 15,6

The conversion of butene-1 is a 50.5%, while the selectivity of the process 85,3% , i.e., the activation at a temperature below stated, gives a catalyst having low activity and selectivity.

P R I m e R 10. The process is carried out under the conditions of example 2 with the only difference that the activation of the catalyst is carried out in a current of hydrogen-containing gas of the following composition,%: Hydrogen 92.0 Monoxide 3,0 Inert impurities 5.0 and the isomerization of butene-1 is carried out with a bulk velocity of 2000 h-1the degree of conversion of butene-1 is the 87.3% with a selectivity to 95.7%.

P R I m e R 11. The process is carried out under the conditions of example 3 with the only difference that the isomerization of butene-1 is carried out at flow rate of 4000 h-1. Under these conditions, the conversion of butene-1 is 91.5% at a selectivity 96,7%.

P R I m e R 12. The process is carried out under the conditions of example 3 with the only difference that the activation of the catalyst is carried out in a current of hydrogen-containing gas of the following composition,%: Hydrogen 85,0 carbon Monoxide 10,0 Inert impurities 5,0

The conversion of butene-1 sostiniu conversion of butene-1 and the selectivity of the process.

The ACTIVATION METHOD PALLADIUM CATALYST on a carrier for the structural isomerization of butene-1 in the butenes-2 by treating the catalyst with hydrogen at elevated temperature, characterized in that the treatment is carried out with a mixture of hydrogen and carbon monoxide content of 0.5 to 7.5% vol. carbon oxide at 120 - 250oC.

 

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