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Novel method for desulfurizing high-sulfur petroleum coke through catalytic oxidation of commercial-grade phosphotungstic acid coupled eutectic solvent

A low eutectic solvent and catalytic oxidation technology, which is applied in the chemical processing of tar pitch/petroleum pitch/natural pitch, etc., can solve the problems of high processing cost, high import demand, complicated procedures, etc., and can increase the specific surface area. Effect

Inactive Publication Date: 2021-07-30
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Aiming at the existing petroleum coke desulfurization technology’s problems of high processing cost, complex process, environmental pollution and insufficient supply of domestic high-quality petroleum coke leading to high demand for imports, the present invention aims to provide a low processing cost, mild condition and can achieve Petroleum coke desulfurization method for energy saving and emission reduction purposes

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Add 1.6g of calcium oxide, 0.4g of high-sulfur petroleum coke and zirconia ball milling beads into the ball milling tank, mix completely, and then place it in a planetary ball mill. The ball mill lasts for 8 hours at a speed of 400rpm. Washing with water and drying, the product after drying is the pretreated petroleum coke;

[0022] 0.2g of pretreated petroleum coke, 0.2g of phosphotungstic acid and 5mL of binary deep eutectic solvent (acetamide and 1-ethyl-3-methylimidazolium bromide as raw materials and in a molar ratio of 1:0.5 Synthetic binary deep eutectic solvent) was placed in a three-necked flask and placed in a constant temperature oil bath with precise temperature control of 70°C, first extracted for 0.5h, then 5mL of 30% hydrogen peroxide was added dropwise, and after continuous stirring for 5h, pumping filtered, washed with water, and dried, and the sulfur content in the high-sulfur petroleum coke was reduced from 4.46wt.% to 1.96wt.% using a micro-coulomb s...

Embodiment 2

[0024] Add 1.6g of calcium oxide, 0.4g of high-sulfur petroleum coke and zirconia ball milling beads into the ball milling tank, mix completely, and then place it in a planetary ball mill. The ball mill lasts for 8 hours at a speed of 300rpm. Washing with water and drying, the product after drying is the pretreated petroleum coke;

[0025] 0.2g of pretreated petroleum coke, 0.2g of phosphotungstic acid and 5mL of binary deep eutectic solvent (acetamide and 1-ethyl-3-methylimidazolium bromide as raw materials and in a molar ratio of 1:0.5 Synthetic binary deep eutectic solvent) was placed in a three-necked flask and placed in a constant temperature oil bath with precise temperature control of 70°C, first extracted for 0.5h, then 5mL of 30% hydrogen peroxide was added dropwise, and after continuous stirring for 5h, pumping filtered, washed with water, and dried, and the sulfur content in the high-sulfur petroleum coke was reduced from 4.46wt.% to 2.49wt.% using a micro-coulomb s...

Embodiment 3

[0027] Add 1.6g of calcium oxide, 0.4g of high-sulfur petroleum coke and zirconia ball milling beads into the ball milling tank, mix completely, and then place it in a planetary ball mill. The ball mill lasts for 8 hours at a speed of 400rpm. Washing with water and drying, the product after drying is the pretreated petroleum coke;

[0028] 0.2g of pretreated petroleum coke, 0.2g of phosphotungstic acid and 5mL of binary deep eutectic solvent (acetamide and 1-ethyl-3-methylimidazolium bromide as raw materials and in a molar ratio of 1:0.5 Synthetic binary deep eutectic solvent) was placed in a three-necked flask and placed in a constant temperature oil bath with precise temperature control of 60°C, first extracted for 0.5h, then 5mL of 30% hydrogen peroxide was added dropwise, after continuous stirring for 5h, pumping filtered, washed with water, and dried, and the sulfur content in the high-sulfur petroleum coke was reduced from 4.46wt.% to 2.04wt.% using a micro-coulomb sulfu...

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Abstract

The invention belongs to the field of petrochemical industry, and relates to a method for desulfurizing high-sulfur petroleum coke through catalytic oxidation of a commercial-grade phosphotungstic acid coupled eutectic solvent. The method comprises the following steps of: firstly, mixing high-sulfur petroleum coke with a basic oxide, carrying out ball milling treatment, and then cleaning and drying to obtain pretreated petroleum coke; and mixing the petroleum coke, phosphotungstic acid and an eutectic solvent to obtain a mixed solution, putting the mixed solution into a constant-temperature oil bath for extraction, then adding an oxidizing agent for an oxidative desulfurization reaction, filtering out a binary deep-eutectic solvent for recycling after finishing the reaction, washing and drying the residual product, and finally reducing the sulfur content to 1.96 wt.%, thereby realizing the desulfurization of the high-sulfur petroleum coke. According to the method, the operation process is simple, the reaction condition is mild, the specific surface area of the petroleum coke can be increased through ball milling treatment, an oxygen source can better enter petroleum coke pore channels, effective desulfurization of the high-sulfur petroleum coke can be achieved under the condition of low energy consumption, and waste of the waste high-sulfur petroleum coke is turned into wealth.

Description

technical field [0001] The invention belongs to the field of petrochemical industry, and in particular relates to a new method for desulfurizing high-sulfur petroleum coke by catalytic oxidation of commercial-grade phosphotungstic acid coupled with a deep eutectic solvent. Background technique [0002] Petroleum coke is one of the main by-products of the oil refining industry. It is the main raw material for the preparation of carbon materials, especially prebaked anodes for aluminum (also known as carbon anodes, anodes for short). The quality standards of petroleum coke can be divided into three categories according to the sulfur content. Those with a sulfur content ≥ 3.0wt.% are regarded as waste, and those with a sulfur content between 1 and 3wt.% can be used as fuel and in the manufacture of aluminum electrolytic cells Anode bottom blocks with sulfur content ≤ 1wt.% can be used to make carbon products. Raw petroleum coke needs to be calcined to improve its physical and ...

Claims

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Application Information

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IPC IPC(8): C10C3/04
CPCC10C3/04
Inventor 华明清龚佳鸿朱文帅李富民张森琪黄燕
Owner JIANGSU UNIV