Starting method of hydrogenation catalyst

A technology of hydrogenation catalyst and sulfiding agent, which is applied in the fields of start-up, chemical instruments and methods, catalyst activation/preparation, etc. of hydroprocessing operations. It can solve the problems of hydrogen embrittlement safety in reactors with too high initial activation temperature, and achieve improved safety. performance, high catalyst activity, and the effect of promoting the degree of vulcanization

Active Publication Date: 2021-05-04
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] Aiming at the deficiencies of the prior art, the present invention provides a method for starting a hydrogenation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] (1) Mix 100g of pseudo-boehmite (commercial or self-made), 2.5g of turnip powder, 5g of citric acid, 30mL of deionized water, 5mL of nitric acid (concentration: 30wt%), 15mL of silica gel (containing 15wt% silicon %) were evenly mixed, extruded into strands, and calcined at 550° C. for 4 hours to prepare a silicon-containing alumina carrier. Prepare ammonium tetrathiomolybdate solution (containing 27% molybdenum oxide), mix with the above silicon-containing alumina carrier, and dry at 115°C for 3 hours. Then mix it with the prepared nickel nitrate solution (containing 8% nickel oxide), and dry it at 75°C for 3.5 hours to prepare an intermediate state hydrogenation catalyst.

[0047] (2) Vulcanizing agent (elemental sulfur, the amount used is 15% of the theoretical sulfur demand of the intermediate state hydrogenation catalyst), vulcanization aid (industrial soybean oil shown in Table 1 and diesel oil shown in Table 4 in a weight ratio of 2:1) mixture, the amount is 25%...

Embodiment 2

[0051] (1) Mix 100g of pseudoboehmite (commercial or self-made), 5g of turnip powder, 5g of citric acid, 30mL of deionized water, 5mL of nitric acid (concentration: 30wt%), 15mL of silica gel (containing 15 wt% silicon %), uniformly mixed, extruded, and calcined at 500° C. for 3 hours to prepare a silicon-containing alumina carrier. Prepare ammonium thiomolybdate solution (containing 30% molybdenum oxide), mix with the above silicon-containing alumina carrier, and dry at 115°C for 3 hours. Then mix it with the prepared nickel nitrate solution (containing 10% nickel oxide), and dry it at 110°C for 3 hours to prepare an intermediate hydrogenation catalyst.

[0052] (2) Mix vulcanizing agent (elemental sulfur, the amount is 25% of the theoretical sulfur demand of the intermediate catalyst), vulcanization aid (a mixture of industrial rapeseed oil and diesel oil at a weight ratio of 1:2), and obtain pre-vulcanized raw materials ; Mix the presulfurized raw material with the interme...

Embodiment 3

[0056] (1) 100g of pseudo-boehmite (commercial or self-made) roasted at 600°C, 5g of turnip powder, 5g of citric acid, 30m of deionized water, 5mL of nitric acid (30%), 15mL of silica gel (containing silicon 15%) were uniformly mixed, extruded, and calcined at 500°C for 3 hours to prepare a silicon-containing alumina carrier. Prepare ammonium thiomolybdate solution (containing 30% molybdenum oxide), mix with the above silicon-containing alumina carrier, and dry at 115°C for 3 hours. Then mix it with the prepared cobalt nitrate solution (containing 10% cobalt oxide), and dry it at 100°C for 2.5 hours to prepare an intermediate state hydrogenation catalyst.

[0057] (2) Mix vulcanizing agent (elemental sulfur, the dosage is 35% of the theoretical sulfur demand of intermediate state hydrogenation catalyst), vulcanization aid (a mixture of industrial rapeseed oil and diesel oil with a weight ratio of 1:2, and mix uniformly to obtain the pre- Vulcanized raw material; pre-sulfided ...

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PUM

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Abstract

The invention discloses a starting method of a hydrogenation catalyst, which comprises the following steps: (1) respectively mixing a hydrogenation catalyst carrier with a thiomolybdate and/or thiotungstate solution and a nickel salt and/or cobalt salt solution, and drying to obtain an intermediate-state hydrogenation catalyst; (2) uniformly mixing a vulcanizing agent with the intermediate-state hydrogenation catalyst obtained in the step (1), then carrying out heat treatment, cooling, and adding a phosphorus-containing substance; (3) drying the material obtained in the step (2) to obtain a presulfurized catalyst; and (4) loading the presulfurized catalyst in the step (3) into a reactor, and carrying out wet activation start-up. According to the method, the safety problem of hydrogen embrittlement of the reactor caused by too high initial activity temperature of the catalyst is solved, the ex-situ presulfurization process of the catalyst and a presulfurization catalyst start-up activation method are also improved, and the activity of the catalyst is improved while the initial activation temperature of the catalyst is increased.

Description

technical field [0001] The invention discloses a method for starting a hydrogenation catalyst, in particular to a method for starting a sulfurized hydrogenation catalyst. Background technique [0002] In recent years, the trend of inferior crude oil has become increasingly obvious, while the demand for clean fuels in various countries is increasing. Hydrogenation technology is one of the most effective means of producing clean fuels, and its efficient hydrogenation catalyst has become the key technology of hydrogenation technology. The active metals of conventional hydrogenation catalysts are in the oxidized state, but the active substances are in the sulfided state in actual use, so they need to be sulfided in the reactor before use. Conventional pre-sulfurization in the catalyst requires special equipment, which increases the production cost. The vulcanization process is easy to cause pollution and requires a long start-up time. [0003] In response to this problem, in re...

Claims

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Application Information

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IPC IPC(8): B01J27/188B01J27/19B01J37/20B01J37/08C10G49/24
CPCB01J27/188B01J27/19B01J37/20B01J37/0018C10G49/24
Inventor 高玉兰方向晨徐黎明佟佳杨涛王继锋
Owner CHINA PETROLEUM & CHEM CORP
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