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Dehydrogenation catalyst activation method combining high-temperature reduction with temperature programmed reduction

A dehydrogenation catalyst and temperature-programmed technology, applied in catalyst activation/preparation, physical/chemical process catalysts, chemical instruments and methods, etc., can solve the problems of rapid decline in catalyst activity and poor stability

Active Publication Date: 2013-02-06
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The constant temperature and long-term reduction in the high-purity hydrogen flow can make the active components of the catalyst into a single metal state, ensure the deep reduction of the metal components, and the initial activity of the catalyst is high, but the activity of the catalyst decreases quickly and the stability is poor

Method used

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Examples

Experimental program
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preparation example Construction

[0013] The dehydrogenation catalyst can be prepared by a conventional method, such as supporting the dehydrogenation active metal by an impregnation method, and the auxiliary agent can be introduced during the preparation process of the alumina carrier and / or by an impregnation method.

[0014] The catalyst of the present invention takes Sn-containing alumina or weakly acidic molecular sieve as a carrier, and the dehydrogenation active metal component is generally selected from one or more of platinum, palladium, iridium, rhodium or osmium in the platinum group, preferably platinum, The dosage is 0.01%~2% of the weight of the carrier in terms of elements. The content of Sn is 0.1% to 10% of the weight of the carrier in terms of elements.

[0015] In the dehydrogenation catalyst with Sn-containing alumina or weak acid as the carrier of the present invention, Sn is introduced into the Sn-containing material when the alumina is gelled, and then the carrier is made.

[0016] In t...

example 1

[0032] Preparation of Sn-containing alumina supports. After mixing a certain amount of 0.98M aluminum trichloride solution and 0.01M tin tetrachloride solution, add a certain amount of 8% ammonia water, mix evenly in the neutralization tank at 60~80℃, and control the pH value to 7.0~ 9.0, after filtration, washing and acidification, pressurized into spheres in an oil-ammonia column, dried, aged, and calcined at 650-750 ℃ ​​for 4 hours to obtain alumina spheres containing Sn 0.8wt%.

[0033] The alumina ball carrier containing 0.8% Sn was calcined at 800 °C for 3 h, the calcined support was immersed in an aqueous solution containing chloroplatinic acid at 70 °C for 6 h, dried at 120 °C for 2 h, and calcined at 500 °C for 4 h. Then activated in air containing water vapor for 4h. Then at 70 °C with KNO 3 The solution was soaked for 2 h, dried and calcined under the same conditions. The loading amount of each component in the catalyst is: Pt 0.3wt%, Sn 0.8wt%, K 0.7wt%.

[003...

example 2

[0044] Preparation of Sn-containing alumina supports. After mixing a certain amount of 1.08M aluminum trichloride solution and 0.01M tin tetrachloride solution, add a certain amount of 10% ammonia water, mix evenly in the neutralization tank at 60~80℃, and control the pH value to 7.0~ 9.0, after filtration, washing and acidification, pressurized into spheres in an oil-ammonia column, dried, aged, and calcined at 650-750 ℃ ​​for 4 hours to obtain alumina spheres containing 1.0wt% Sn.

[0045] The alumina ball carrier containing 1.0% Sn was calcined at 800 °C for 3 h, the calcined support was immersed in an aqueous solution containing chloroplatinic acid at 70 °C for 4 h, dried at 120 °C for 2 h, calcined at 500 °C for 4 h, and then calcined at 500 °C for 4 h. Activated in air containing water vapor for 4h. Then at 70 °C with KNO 3 The solution was soaked for 2 h, dried and calcined under the same conditions. The loading amount of each component in the catalyst is: Pt 0.7wt%,...

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Abstract

The present invention discloses a dehydrogenation catalyst activation method combining high-temperature reduction with temperature programmed reduction. The dehydrogenation catalyst is a platinum group metal-supported catalyst. The activation process comprises: performing the high temperature reduction at first, wherein hydrogen gas is used in the high temperature reduction at a temperature of 450-550 DEG C for 5-55min; then performing the temperature programmed reduction, wherein hydrogen gas is used for the reduction, the initial temperature is of 240-400 DEG C, the finish temperature is of 450-550DEG C, and the heating rate is 0.5-10 DEG C / min; and then adjusting the temperature to 500-650 DEG C, the process of sulfurization passivation and directly feeding hydrogen-containing feed gas for the dehydrogenation reaction. Compared with the prior art, the dehydrogenation catalyst reduced and activated by the method of the invention has a higher activity stability.

Description

technical field [0001] The present invention relates to the activation method of a kind of low-carbon alkane catalytic dehydrogenation olefin catalyst, specifically, is about C 2 ~C 5 Method for activating catalysts for dehydrogenation to olefins. Background technique [0002] With the popularization and use of civil natural gas, the effective utilization of liquefied gas in refineries has become a hot spot in the field of petrochemical industry. How to finely utilize the precious low-carbon alkane resources in liquefied gas is of great significance. The dehydrogenation of propane to propylene and the dehydrogenation of isobutane to isobutene are one of the important ways to produce chemical raw materials from liquefied gas, and it will become a focus of research and development of petrochemical technology in the new century. [0003] The catalytic dehydrogenation reaction of light alkanes is limited by thermodynamic equilibrium and must be carried out under harsh conditio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/62B01J37/18C07C5/333C07C11/09
Inventor 张海娟李江红张喜文宋喜军孙潇磊王振宇
Owner CHINA PETROLEUM & CHEM CORP
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