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Preparation process of vulcanized catalyst

A catalyst and vulcanization-type technology, which is applied in the field of preparation of hydrogenation catalyst compositions, can solve the problems of unfavorable industrial application of catalysts, inability to completely solve the problem of self-heating of sulfided catalysts, and low catalyst production efficiency, so as to shorten the vulcanization time and suitably For large-scale use, the effect of improving the vulcanization effect

Active Publication Date: 2009-08-12
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

CN1400056A Coat the pre-sulfurized catalyst containing sulfidation agent with oxygen-containing organic matter containing at least 16 carbon atoms, treat it above 175°C for a period of time, and then activate it with hydrogen to reduce the self-heating problem of the catalyst, but it cannot completely solve the sulfidation state The self-heating problem of the catalyst, and the storage, transportation and loading of the catalyst still have certain problems
In the above-mentioned patents, either the self-heating problem of the catalyst, or the storage, transportation and loading of the catalyst still have certain problems, and there is a problem of low production efficiency in the production of the catalyst, which is not conducive to the industrial application of this type of catalyst

Method used

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  • Preparation process of vulcanized catalyst
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  • Preparation process of vulcanized catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] The commercial hydrodesulfurization catalyst FH-5A (developed by Fushun Petrochemical Research Institute and produced by Wenzhou Huahua Group Co., Ltd.) was selected. The main composition and properties are shown in Table 1.

[0033] The specific pre-sulfurization process is as follows:

[0034] The molten elemental sulfur is introduced into the oxidation state catalyst, and the introduced amount of the elemental sulfur is 105% of the theoretical sulfur requirement of the catalyst. Then tetrabutylthiuram disulfide (TBTD) was mixed with coked diesel, and the mixture was introduced into the catalyst containing elemental sulfur. The amount of TBTD was 3% by weight of the catalyst, and the amount of coked diesel was 40% by weight of the catalyst. Finally, in normal pressure, non-flowing air atmosphere, 160 ° C for 5 hours, the heat treatment equipment adopts figure 1 The double-cone rotary heat processor has a rotating speed of 5 rpm to obtain a hydrorefining catalyst EPRE...

Embodiment 2

[0036] The catalyst in the oxidation state is the same as in Example 1, which is FH-5A.

[0037] The specific pre-sulfurization process is as follows:

[0038] 1. Dissolving tetramethylthiuram disulfide (TMTD) in benzene, evenly impregnating it on the oxidized FH-5A catalyst, the amount of TMTD added is 5% of the catalyst weight, to obtain a catalyst loaded with TMTD.

[0039] 2. Disperse elemental sulfur in a solvent with a volume ratio of catalytic cracking gasoline and rapeseed oil of 8:1. The amount of solvent is 12% of the weight of the catalyst, and the amount of elemental sulfur is 90% of the theoretical sulfur content of the catalyst containing metal. The elemental sulfur solvent impregnates the TMTD-supported catalyst obtained in step 1. Heat treatment in a closed device at 180°C for 5 hours, the final pressure is 0.4MPa (gauge pressure), the heat treatment equipment adopts figure 1 Described biconical rotary heat processor, rotating speed is 8 revolutions / min. The...

Embodiment 3

[0045] The catalyst in the oxidation state is the same as in Example 1, which is FH-5A.

[0046] The specific pre-sulfurization process is as follows:

[0047] 1. Dissolve dithiodimethyldiphenylthiuram in acetone and introduce it into the catalyst in an oxidized state. The amount of dithiodimethyldiphenylthiuram is 20% of the catalyst weight, and then at 105°C Under treatment for 3 hours, a catalyst containing dithiodimethyldiphenylthiuram was obtained.

[0048] 2. A mixed solvent of vacuum distillate oil and peanut oil with a volume ratio of 1:2. The amount of solvent is 0.5% of the weight of the catalyst, and then mixed with elemental sulfur solid powder. The amount of elemental sulfur is 40% of the theoretical sulfur requirement of the catalyst containing metal.

[0049] 3. The material obtained in step 2 was treated at 180°C for 3 hours at normal pressure and in a stagnant air atmosphere, and the heat treatment equipment used figure 1 The rotating speed of the double-con...

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Abstract

The invention relates to a preparation method of a sulfurized catalyst. During the preparation process, the thiuram substances accounting for 0.5% to 25% of the weight of the catalyst, the sulfur element accounting for 30% to 150% of the theoretical sulfur demand of the hydrogenation catalyst, and the organic The solvent is introduced to the catalyst in the oxidized state, which is then processed in a dynamic heating device. The hydrogenation catalyst preparation method of the present invention can further improve the sulfur retention rate of the catalyst during activation by introducing thiurams under the combined action of sulfur and organic solvents, slow down the concentrated heat release, shorten the vulcanization time of the catalyst, and improve production efficiency. efficiency. The method of the invention can be used in the treatment process before the application of various hydrogenation catalysts.

Description

technical field [0001] The invention relates to a preparation method of a hydrogenation catalyst, in particular to a preparation method of a hydrogenation catalyst composition containing a sulfurizing agent after presulfidation treatment outside the device. Background technique [0002] Hydrofining, hydrotreating, hydrocracking and other hydrogenation catalysts generally use alumina, silicon aluminum, molecular sieve and other refractory oxides as carriers, and one or more active metal groups such as molybdenum, tungsten, cobalt, nickel, etc. Sometimes, the catalyst can also contain auxiliary components such as phosphorus, silicon, fluorine, titanium, zirconium, and boron. Generally, the metal component of the catalyst obtained in the production process exists in an oxidized state, while in the hydrogenation reaction process, the active metal component of the catalyst is in a sulfide state (the metal exists in the form of sulfide: Co 9 S 8 、MoS 2 、Ni 3 S 2 、WS 2 etc.) ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J37/20B01J27/049C10G45/38
Inventor 高玉兰关明华王刚曹凤兰
Owner CHINA PETROLEUM & CHEM CORP
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