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Supported catalyst treatment

A catalyst and oxidant technology, applied in the direction of catalyst regeneration/reactivation, physical/chemical process catalyst, combustible gas purification, etc., can solve the problem of not effectively providing catalyst and so on

Inactive Publication Date: 2005-05-18
EXXON RES & ENG CO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disclosed process does not effectively provide any means to regenerate a severely deactivated catalyst or to increase the reliability of the process, such as by removing fines that may be generated by the reactor under turbulent flow conditions

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] Example 1: Solvent Dewaxing of Deactivated Catalyst

[0049] A titania-supported cobalt-based catalyst pellet, weighing 83 grams, removed from a Fischer-Tropsch reactor operated for more than 200 days, was placed in a beaker and covered with toluene. The mixture was heated to 85-90°C and stirred by hand. During heating and stirring, the catalyst block splits. After 5 minutes, the toluene / wax solution was decanted, fresh toluene was added, and the process was repeated two more times. After the third decant, the remaining toluene / catalyst slurry was transferred to a Buchner funnel and filtered hot. The filter cake was poured three times with hot toluene and the toluene was drawn through the filter cake by the vacuum device used. The filter cake on the funnel was dried by using vacuum to yield 58.4 g of non-pyrophoric catalyst. The catalyst contains a large amount of reduced cobalt, which can be shown by its high magnetic permeability. The catalyst is easily moved wit...

Embodiment 2

[0050] Example 2: Hydrogen Dewaxing of Solvent Dewaxed Catalyst

[0051]According to the catalyst prepared in Example 1 (120 g), the catalyst was loaded into a fixed bed reactor purged with nitrogen for 30 minutes. The reactor temperature was raised to 100°C and the gas flow was changed to nitrogen with 10% hydrogen. The temperature was then raised to 288°C and the gas flow was fixed at 450 sccm (standard cubic centimeters per minute) of pure hydrogen. The catalyst was held for 3 hours to completely remove organic compounds and reduce metal components. The reactor was cooled and the gas flow was changed to nitrogen when the temperature dropped below 100°C. When the reactor was cooled to room temperature, the catalyst was removed under nitrogen to yield 118.4 g of reduced metal. The catalyst contains a large amount of metallic cobalt and is easily moved by permanent magnets.

Embodiment 3

[0052] Example 3: Direct Hydrogen Dewaxing of Deactivated Catalysts

[0053] TiO2-supported cobalt-based catalyst pellets, weighing 70-100 g, removed from a Fischer-Tropsch reactor run for more than 200 days, were loaded into a fixed-bed reactor purged with nitrogen for 30 minutes. The reactor temperature was raised to 100°C and the gas flow was changed to nitrogen with 10% hydrogen. The temperature was then raised to 288°C and the gas flow was fixed at 450 seem of pure hydrogen. The catalyst was maintained for 3 hours, or until the organic compounds were completely removed and the metal components were reduced. The reactor was cooled and the gas flow was changed to nitrogen when the temperature dropped below 100°C. When the reactor was cooled to room temperature, the catalyst was removed under nitrogen to yield 40-80 g of reduced metal. The catalyst contains a large amount of metallic cobalt and is easily moved by permanent magnets.

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PUM

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Abstract

There is provided a process for renewing the activity of supported metal catalysts for the hydrogenation of carbon monoxide to form a mixture of hydrocarbons comprising decreasing the hydrocarbon content of the catalyst, preferably by contact with hydrogen-containing gas at elevated temperatures, impregnating under a non-oxidizing atmosphere with a solution of at least one of an ammonium salt and an alkyl ammonium salt, optionally in combination with up to five moles of ammonia per liter of solution to the point where it has absorbed a volume of solution equal to at least about 10% of its calculated pore volume; oxidizing the catalyst with a gaseous oxidant in the presence of the impregnating solution and activating the catalyst by reduction with hydrogen at elevated temperatures. Optionally, the catalyst is calcined after the oxidation step, and passivated after the activation step.

Description

[0001] This invention relates to the production of higher hydrocarbons from synthesis gas using supported metal catalysts, particularly cobalt catalysts. Background of the invention [0002] The conversion of synthesis gas, ie carbon monoxide and hydrogen, to higher value products is well known and has been used industrially for many years. Typical methods include, for example, methanol synthesis, higher alcohol synthesis, hydroformylation, and Fischer-Tropsch synthesis. The synthesis gas mixture is contacted with a suitable catalyst, usually containing at least one Group VIII metal. Suitable Fischer-Tropsch catalysts contain one or more catalytic Group VIII metals such as iron, cobalt and nickel. For oxidative synthesis, copper may also be included. [0003] A wide variety of catalyst formulations and preparations are available for syngas conversion. Catalysts generally fall into two broad categories: unsupported metals, known as dispersed active metals; and the larger cla...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J21/06B01J23/75B01J23/94B01J23/96B01J38/06B01J38/10B01J38/12B01J38/56B01J38/66B01J38/70C07B61/00C07C1/04C07C7/04C07C9/14C10G2/00
CPCB01J21/063B01J23/75B01J23/94B01J23/96B01J38/10B01J38/12B01J38/66B01J38/70C10G2/331C10G2/332C10G2/333
Inventor M·达格R·J·科威尔J·R·克拉克D·O·马勒
Owner EXXON RES & ENG CO
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