Method for vacuum reinforced desulfurization of high sulfur petroleum coke

A petroleum coke and high-sulfur technology, applied in the petroleum industry, carbon preparation/purification, solid fuel, etc., can solve the problems of complex production process, low gas content, complex technical operation, etc., and achieve short production process and high desulfurization rate , The effect of simple process

Inactive Publication Date: 2017-01-18
KUNMING UNIV OF SCI & TECH
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Problems solved by technology

High-temperature calcination is a common method for desulfurization of petroleum coke. When the calcination temperature is lower than 1000°C, the sulfur in petroleum coke will not be removed basically. Even if the calcination temperature of petroleum coke reaches 1400°C, the desulfurization rate of petroleum coke can only reach 70%. About, as the calcination temperature rises, the desulfurization rate increases, but this desulfurization technology not only needs to invest a lot of energy and power, but also due to the SO produced during the calcination process 2 The gas content is low and easy to collect, if it is discharged directly, it will cause serious pollution to the environment
Invention patent "Ionic liquid used in petroleum coke desulfurization method" (application number CN200710064515.8) relates to a method for removing sulfur in petroleum coke, by using alkaline ions as auxiliary agents, adding them to petroleum coke to make the structure of petroleum coke Changes are beneficial to the removal of sulfur in petroleum coke, but this method adds additives to petroleum coke, which will increase the ash content in petroleum coke, and the desulfurization rate is not high
The invention patent "A Method for Removing Sulfur from Petroleum Coke and Its Desulfurizer" (Application No. CN201010153531.6), which belongs to ionic liquid and its ions belong to acidic ions, reports the use of mixed acid as a desulfurizer to directly reduce the sulfur content in 3-7% of petroleum coke is soaked in desulfurizer, and then separated and washed. The desulfurization rate of petroleum coke is 45-60%. This method will produce a large amount of waste acid, and the production process is relatively complicated, so it will increase The cost of desulfurization
The invention patent "Petroleum Coke Desulfurization and Purification Method and Industrial Furnace" (patent number: 98114600.7) reports a desulfurization method. First, the petroleum coke is calcined at a temperature of 600-1200°C, and then the petroleum coke is placed in an electric furnace at a temperature of 1700-2300°C. ℃ calcination, and finally can obtain low-sulfur petroleum coke with a sulfur content of 0.1%. This technology has a relatively high desulfurization rate, but the production process is too complicated and requires a high temperature, so the cost is relatively high. There are the same problems as above, and the resulting SO 2 Harmful gases are not conducive to collection
The invention patent "Petroleum Coke Gasification Hydrogen Production Coupled Desulfurization Method" (application number CN200710064514.3) reports a petroleum coke desulfurization technology, which is hydrodesulfurization, and can obtain petroleum coke with low sulfur content. The desulfurization method requires Introducing hydrogen, hydrogen brings many safety hazards to the production process, which is not conducive to industrial production
The US patent "US3598528A" with the same problem proposes to preheat and pre-oxidize petroleum coke to make it gasify, thereby changing the structure of petroleum coke particles, and then put the treated petroleum coke in a hydrogenation reactor In the process, the hydrogen gas introduced into the gasification reactor is used to desulfurize petroleum coke. This desulfurization technology belongs to the hydrodesulfurization technology, and the technical operation is also complicated.

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  • Method for vacuum reinforced desulfurization of high sulfur petroleum coke

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Experimental program
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Effect test

Embodiment 1

[0015] The specific steps of the vacuum-enhanced petroleum coke desulfurization method are as follows: First, grind and sieve high-sulfur petroleum coke (from a silicon company in Yunnan, with a petroleum coke sulfur content of 8.21wt%) to a particle size of 350-450µm, and control the thickness to 10mm , under the condition of a vacuum degree of 100Pa, the temperature was raised to 1600°C at a heating rate of 10°C / min and kept for 10 minutes to prepare desulfurized petroleum coke, and at the same time, elemental sulfur with a purity of more than 90% was collected in the condensing equipment at the top.

[0016] The desulfurization rate of the above-mentioned desulfurized petroleum coke is 80.02%.

Embodiment 2

[0018] The specific steps of the vacuum-enhanced desulfurization method for high-sulfur petroleum coke are as follows: firstly, high-sulfur petroleum coke (from a silicon company in Yunnan, with a petroleum coke sulfur content of 8.21wt%) is ground and screened to a particle size of 250-350µm, and the thickness is controlled. 30mm, and under the condition of vacuum degree of 1.0Pa, the temperature was raised to 1400°C at a heating rate of 20°C / min and kept for 30min to prepare desulfurized petroleum coke. sulfur.

[0019] The desulfurization rate of the above-mentioned desulfurized petroleum coke is 75.3%.

Embodiment 3

[0021] The specific steps of the vacuum-enhanced desulfurization method for high-sulfur petroleum coke are as follows: firstly, high-sulfur petroleum coke (from a silicon company in Yunnan, with a sulfur content of 8.21wt%) is ground and screened to a particle size of 150-250µm, and the thickness is controlled. 50mm, in a vacuum of 10 -1 Under Pa conditions, the temperature was raised to 1300°C at a heating rate of 30°C / min and kept for 50 minutes to prepare desulfurized petroleum coke. At the same time, elemental sulfur with a purity of more than 91.2% was collected in the condensing equipment at the top.

[0022] The desulfurization rate of the above-mentioned desulfurized petroleum coke is 76.5%.

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Abstract

The invention relates to a method for vacuum reinforced desulfurization of high sulfur petroleum coke and belongs to the technical field of vacuum metallurgy. First petroleum coke is ground and screened to the granularity of 45-450 [mu]m, and the thickness is controlled to be 10-100 mm; under the vacuum degree of 10<-3>Pa to 100 Pa, the temperature rises to 1000-1600 DEG C at a heating rate of 10-50 DEG C and preserving heat for 10-90 min, the petroleum coke desulfurization efficiency reaches 70% or above, and elemental sulfur with a purity of 90% or above is collected in a condensation device at the top. According to the method, a low ash content of the petroleum coke is guaranteed without adding of an additive while a high desulfurization rate is achieved, it is also guaranteed that the petroleum coke has a high recovery rate after being desulfurized, the elemental sulfur can further be obtained in the process, and the problem that plenty of harmful SO2 gas unfavorable for collection is generated according to most of petroleum coke desulfurization methods is solved.

Description

technical field [0001] The invention relates to a method for vacuum-enhanced desulfurization of high-sulfur petroleum coke, which belongs to the technical field of vacuum metallurgy. Background technique [0002] Petroleum coke is a kind of carbon material that is easy to graphitize, so it is widely used in metallurgy, chemical industry and other industries as graphite electrodes. In addition, petroleum coke is widely used in composite carbonaceous reducing agents for industrial silicon smelting (more than 30% by mass) due to its high fixed carbon content, low volatile content, and relatively high combustion calorific value. During the smelting process, a large amount of heat can be provided by combustion, and its relatively high fixed carbon is the main reducing agent for carbon thermal reduction of silica. However, during the combustion process of petroleum coke, especially the high sulfur content in petroleum coke (the sulfur content of petroleum coke is even as high as ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C10L9/08C01B32/05
CPCC10L9/08
Inventor 马文会陈正杰魏奎先伍继君李绍元秦博雷云谢克强杨斌戴永年
Owner KUNMING UNIV OF SCI & TECH
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