Method for preparing high-quality needle coke by volume exclusion separation-grading carbonization of heavy oil

A technology of size exclusion and size exclusion chromatography, which is applied in the field of heavy oil size exclusion separation-graded carbonization to prepare high-quality needle coke, can solve the problem of non-ideal components containing catalyst solid powder, and achieve low price and high viscosity The effect of low and high yield

Active Publication Date: 2020-08-25
CHINA UNIV OF PETROLEUM (EAST CHINA)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The purpose of the present invention is to overcome the deficiencies of the prior art and provide a method for preparing high-quality needle coke, using heavy oil as a raw material to obtain a component with a narrow relative molecular mass distribution through size exclusion chromatography as a modified raw material. Solve the problem of heavy oil containing catalyst solid powder and other non-ideal components

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Embodiment 1: get catalytic cracking oil slurry 10g, adopt tetrahydrofuran to be made into the solution of 5% (mass fraction) as solvent, this solution is joined in the chromatographic column that polystyrene filler is housed, and gel column bed diameter is 50mm, The height of the column bed is 800mm, and the hole diameter is The molecular weight is measured with a laser small-angle diffractometer molecular weight detector, and finally the components with a molecular weight of 400-1000 are obtained. The modified raw material separated by size exclusion chromatography was subjected to carbonization reaction in an autoclave, and the air in the autoclave was continuously purged three times with nitrogen. The nitrogen flow rate was 3 L / min, and the temperature was raised to 100°C to start stirring. The first stage of carbonization reaction is at a pressure of 6MPa and a temperature of 360°C for 2 hours; (3) After the first stage of carbonization reaction is completed, the ...

Embodiment 2

[0021] Embodiment 2: get ethylene tar 10g, adopt tetrahydrofuran to be made into the solution of 5% (mass fraction) as solvent, this solution is joined in the chromatographic column that polystyrene filler is housed, and gel column bed diameter is 50mm, column bed The height is 800mm, the hole diameter is The molecular weight is measured with a laser small-angle diffractometer molecular weight detector, and finally the components with a molecular weight of 400-1000 are obtained. The modified raw material separated by size exclusion chromatography was subjected to carbonization reaction in an autoclave, and the air in the autoclave was continuously purged three times with nitrogen. The nitrogen flow rate was 3 L / min, and the temperature was raised to 100°C to start stirring. The first stage of carbonization reaction is at a pressure of 7MPa and a temperature of 380°C for 3 hours; (3) After the first stage of carbonization reaction is completed, the autoclave is heated to 440°C...

Embodiment 3

[0022] Embodiment 3: get petroleum atmospheric residue 10g, adopt tetrahydrofuran to be made into the solution of 5% (mass fraction) as solvent, this solution is joined in the chromatographic column that polystyrene filler is housed, and gel column bed diameter is 50mm , the column bed height is 800mm, and the pore diameter is The molecular weight is measured with a laser small-angle diffractometer molecular weight detector, and finally the components with a molecular weight of 400-1000 are obtained. The modified raw material separated by size exclusion chromatography was subjected to carbonization reaction in an autoclave, and the air in the autoclave was continuously purged three times with nitrogen. The nitrogen flow rate was 3 L / min, and the temperature was raised to 100°C to start stirring. The first stage of carbonization reaction is at a pressure of 8 MPa and a temperature of 400°C for 4 hours; (3) After the first stage of carbonization reaction is completed, the autocl...

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Abstract

The invention belongs to the technical field of petroleum deep processing and the field of novel high-grade carbon material preparation, and belongs to a method for preparing high-quality needle cokethrough the volume exclusion separation-grading carbonization of heavy oil. The method comprises the following steps of: carrying out volume exclusion chromatographic separation on heavy oil to obtaina component with the relative molecular mass of 400-1000, and carrying out first-stage carbonization reaction for 1-5 hours at the temperature of 360-420 DEG C and under the pressure of 6-10 MPa; andafter the first-stage carbonization reaction, carrying out second-stage carbonization reaction for 5-12 hours at the temperature of 420-480 DEG C and under the pressure of 0-5 MPa to obtain a high-quality needle coke product with the true density of more than 2.13 g / cm <3> and the thermal expansion coefficient of less than 1.15*10<-6> / DEG C. The separation method adopted by the invention is accurate, time-saving, labor-saving, remarkable in effect, simple in process operation, environment-friendly, low in equipment requirement and easy to realize industrialization.

Description

technical field [0001] The invention belongs to the technical field of petroleum deep processing and the field of high-grade new carbon material preparation, and specifically relates to a method for preparing high-quality needle coke by volume exclusion separation-graded carbonization of heavy oil. Background technique [0002] Needle coke is a new type of carbon material, which is the carbonization product of petroleum pitch or coal pitch. Needle coke is a silver-gray porous solid with metallic luster, and it is a high-quality carbon material. Needle coke is a molecular crystal of macromolecule condensed aromatic hydrocarbons. The aromatic hydrocarbons are stacked in layers, and the graphite-like microcrystalline units have a high degree of orientation. Needle coke has excellent properties such as low thermal expansion coefficient, high density, corrosion resistance, good electrical and thermal conductivity, and high mechanical strength. It has broad application prospects ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C10B55/00C10G55/04
CPCC10B55/00C10G55/04
Inventor 刘东于冉项在金杨朝合付玉娥
Owner CHINA UNIV OF PETROLEUM (EAST CHINA)
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