A kind of preparation method of sulfurized hydrotreating catalyst

A technology for hydrorefining and catalyst, applied in the field of catalysis, can solve the problems of complex catalyst preparation process, high toxicity of vulcanizing agent, poor storage stability, etc., and achieve the effect of high utilization rate of active metal, excellent catalyst performance and stable property.

Active Publication Date: 2017-06-23
CHINA NAT OFFSHORE OIL CORP +2
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AI Technical Summary

Problems solved by technology

The in-vessel sulfidation method is to put the oxidized catalyst into the hydrogenation reactor, and pass hydrogen and sulfidation agent into the reactor during the heating process for pre-sulfurization. The disadvantage of this method is that it needs special pre-sulfurization equipment, The time is long, the cost of vulcanization is high, the vulcanization agent is highly toxic and flammable, and it is easy to cause pollution to people and the environment
This type of sulfide precursor is not a bulk chemical and requires special equipment for synthesis, and produces wastewater containing sulfur, nitrogen and heavy metals, which is easily oxidized in the air and has poor storage stability, which will lead to complex catalyst preparation processes and a substantial increase in cost

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  • A kind of preparation method of sulfurized hydrotreating catalyst
  • A kind of preparation method of sulfurized hydrotreating catalyst
  • A kind of preparation method of sulfurized hydrotreating catalyst

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preparation example Construction

[0041] The preparation method of the sulfurized hydrofining catalyst of the present invention is to impregnate the required catalyst carrier with an impregnating solution, the impregnating solution contains ammonium molybdate and / or ammonium tungstate, nickel salt and / or cobalt salt, and simultaneously contains vulcanizing agent, organic complex agent and co-solvent; after the in-situ crystallization reaction in a closed container, drying and heat treatment are carried out to obtain the final sulfurized hydrofining catalyst.

[0042] In the preparation process of the sulfide-type hydrofining catalyst of the present invention, the impregnation method is a conventional method in the field, and the required metal salt, vulcanizing agent, organic complexing agent and co-solvent are mixed, stirred and dissolved, and prepared into a clarified product with a suitable pH value. solution, and then impregnated by means of saturated impregnation or excess impregnation.

[0043] The speci...

Embodiment 1

[0048] The preparation of embodiment 1 sulfurized catalyst A

[0049] Take by weighing pseudo-boehmite (Shandong Aluminum Co., Ltd. produces macroporous pseudo-boehmite, which is 72% by weight on a dry basis) 1000g, 20g of scallop powder, 30g of citric acid, 800ml of dilute nitric acid (weight concentration 3%) , kneaded in a kneader for 30 minutes, and then extruded into 1.5mm clover strips on an extruder, dried and calcined at 550° C. for 3 hours to obtain the desired catalyst carrier 1 .

[0050] Dissolve basic nickel carbonate, ammonium molybdate and ethylenediaminetetraacetic acid in ammonia water to obtain a transparent solution, add ethanolamine, ethylenediamine and dithioacetamide in turn to form a clear solution, and the amount of active components in the solution is according to Table 1 The data determined that the molar ratio of dithioacetamide to active metal was 1.6:1. The mixed solution was sprayed and impregnated with carrier 1, in-situ crystallized in a closed...

Embodiment 2

[0051] The preparation of embodiment 2 sulfurized catalyst B

[0052] Dissolve cobalt nitrate, ammonium molybdate and citric acid in water, stir and heat to obtain a transparent solution, add ethylenediamine, aminotrimethylene phosphonic acid and ammonium thiosulfate in turn, mix and stir to form a clear solution, and the amount of active components in the solution is based on The data in Table 1 confirm that the molar ratio of ammonium thiosulfate to active metal is 2.5:1. The mixed solution was sprayed and impregnated with carrier 1, in-situ crystallized in a closed reactor at 75°C for 3 hours, and then vacuum-dried at 220°C for 4 hours to obtain catalyst B. The main physical properties are shown in Table 1.

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Abstract

The invention relates to a preparation method of a sulfurized hydrofining catalyst, which uses an impregnating solution to impregnate the required catalyst carrier, and then undergoes in-situ crystallization reaction and heat treatment to obtain a sulfurized hydrofining catalyst, which is characterized in that the impregnating solution Inorganic salt precursor containing active metal ammonium molybdate and / or ammonium tungstate, Ni and / or Co, as well as vulcanizing agent, organic complexing agent and co-solvent. The method of the invention solves the problems of long start-up sulfidation time and high operating cost of the conventional oxidized catalyst, and simultaneously overcomes the disadvantages of many preparation steps and high cost of the sulfided hydrorefining catalyst. The catalyst prepared by the method of the invention is suitable for petroleum distillate hydrotreating treatment, and is simpler than other external vulcanization methods, and the hydrogenation activity of the catalyst thus prepared can reach or exceed the effect of the catalyst vulcanized in the device.

Description

technical field [0001] The invention relates to the technical field of catalysis, in particular to a method for preparing a sulfurized hydrogenation refining catalyst, which belongs to the improvement of the method for preparing a hydrogenation catalyst. Specifically, it relates to a method for preparing a sulfurized hydrofinishing catalyst improved by using a traditional active metal salt precursor. Background technique [0002] In recent years, with the increasing trend of poor quality of crude oil worldwide, the content of sulfur, nitrogen and aromatics in petroleum products is increasing day by day; at the same time, the requirements for environmental protection in various countries are also getting higher and higher, and the oil refining industry is facing pressure to upgrade the quality of oil products . Hydrogenation technology is the most effective means to solve the above problems, among which, the preparation technology of efficient hydrogenation catalyst is the k...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/051B01J27/049
Inventor 张景成彭雪峰于海斌耿姗南军宋国良张尚强朱金剑张国辉臧甲忠李佳肖寒张玉婷姜雪丹
Owner CHINA NAT OFFSHORE OIL CORP
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