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Ex-situ presulfuration method for hydrogenation catalyst

A technology of hydrogenation catalyst and external pre-sulfurization, which is applied in chemical instruments and methods, catalyst activation/preparation, physical/chemical process catalysts, etc. The effect of less environmental pollution, higher sulfur retention rate and lower cost

Inactive Publication Date: 2019-06-04
沈阳益泰科信息技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In patents such as CN1262305, US4719195, and US5139990, the method for pre-vulcanization outside the device has been reported, but the existing method for pre-vulcanization outside the device has the disadvantages of low vulcanization rate, high cost, and harmful substances.
Existing synthetic methods are not easy to industrialized production, and it is urgent to seek a method for hydrogenation catalyst presulfidation that is easy to operate, low in environmental pollution, and cheap in cost.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] The external presulfurization method of a hydrogenation catalyst comprises specific steps.

[0022] Step 1. Immerse the hydrogenation catalyst in methanol containing industrial vitamin C for reduction pretreatment. The reduction pretreatment temperature is 100° C. and the time is 5 hours.

[0023] Step 2, synthesis of vulcanizing agent: add sulfur and ammonia water with a concentration of 25% into the reactor, heat up to 120°C, and react 4 to generate ammonia polysulfides; feed propylene gas into the reactor, at a pressure of 10MPa, heat preservation (300°C) for 24 hours; after the reaction, cool to room temperature, the discharge material is separated by natural sedimentation to obtain an inorganic phase and an organic phase, and the organic phase is filtered to remove insoluble solid impurities to obtain a crude vulcanizing agent product; the inorganic phase is filtered to remove Distill at atmospheric pressure in the distilling device after miscellaneous, control dis...

Embodiment 2

[0027] The external presulfurization method of a hydrogenation catalyst comprises specific steps.

[0028] Step 1. Immerse the hydrogenation catalyst in an organic solvent containing industrial vitamin C for reduction pretreatment. The reduction pretreatment temperature is 90 ° C and the time is 8 h.

[0029] Step 2. Synthesis of vulcanizing agent: add sulfur and 24% ammonia water into the reaction kettle, heat up to 135°C, and react for 3.5 to generate ammonia polysulfides; put ethylene into the reaction kettle at a pressure of 8MPa , heat preservation (300°C) for 30 hours; after the reaction, cool to room temperature, the discharge is separated by natural sedimentation to obtain an inorganic phase and an organic phase, and the organic phase is filtered to remove insoluble solid impurities to obtain a crude vulcanizing agent product; the inorganic phase is filtered to remove impurities Atmospheric distillation in the distillation device afterward, control distillation tempera...

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PUM

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Abstract

The invention belongs to the field of catalysts, and especially relates to an ex-situ presulfuration method for a hydrogenation catalyst. The method concretely comprises the following steps: immersingthe hydrogenation catalyst in an organic solvent containing industrial vitamin C, and carrying out reduction pretreatment at 80-100 DEG C for 5-10 h; adding sulfur and ammonia water having a concentration of 23-25% into a reactor, heating the added substances to 120-140 DEG C, and carrying out a reaction for 3-4 h to generate ammonium polysulfide; introducing an olefin gas into the reactor, carrying out heat insulation treatment under a pressure of 5-10 MPa for 24-36 h; cooling the reactor to room temperature after the reaction is finished in order to obtain a sulfuration agent; and adding the pretreated catalyst to the sulfuration agent, adding the olefin gas, carrying out heat treatment to sufficiently sulfurate the catalyst, passivating the sulfurated catalyst in a container filled aninert gas, and carrying out constant temperature treatment for 10-12 h. The method has the advantages of simplicity in process operation, low cost and small in environmental pollution, and is suitablefor industrial production.

Description

technical field [0001] The invention belongs to the field of catalysts, in particular to an external presulfurization method of a hydrogenation catalyst. Background technique [0002] With the reduction of oil reserves, crude oil is becoming more and more serious. In order to make full use of resources and reduce environmental pollution, hydrogenation technology has become a very important link in the oil refining industry. Hydrogenation catalysts are mainly active metals such as W, Mo, Ni, Co, etc., but they are usually in an oxidized state, and the catalyst must be converted into a sulfurized state before use to have a high catalytic activity. Therefore, the presulfurization of hydrogenation catalysts is very critical. [0003] The presulfurization method of catalyst can be divided into internal presulfurization and external presulfurization according to the way of sulfur loading. Pre-sulfurization in the vessel has disadvantages such as high equipment investment and lon...

Claims

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Application Information

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IPC IPC(8): B01J37/16B01J37/20
Inventor 葛秋红
Owner 沈阳益泰科信息技术有限公司
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