Method of preparing mesophase pitch by means of naphthene-based vacuum gas oil co-carbonization

A technology of mesophase pitch and co-carbonization, which is applied in the processing of tar pitch/petroleum pitch/natural pitch, chemically processing tar pitch/petroleum pitch/natural pitch, petroleum industry, etc., can solve the problem of light components hindering mesophase Due to the large amount of asphalt and hydrogen-supplying solvent added, and the high cost of cross-linking agent, it can achieve the effect of improving the effect, ensuring the yield and anti-oxidation performance, and improving the softening point.

Inactive Publication Date: 2015-04-08
CHINA NAT OFFSHORE OIL CORP +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention is how to overcome the problem of low yield due to the large amount of light components being taken out of the reaction system in the preparation of mesophase pitch by direct thermal polycondensation under normal pressure. Due to the high pressure of the system, a large number of light components hinder the accumulation of planar a

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] The furfural extracted oil of the vacuum distillate oil of Huanxiling crude oil in Liaohe Oilfield (the kinematic viscosity is 200.6mm at 40°C) 2 / s, aromatics content 65.7wt%, cycloalkane content 31.5wt%, paraffin content 2.8wt%) 300g add volume and be in the stainless steel autoclave of 500ml. When the temperature in the reaction kettle rose to 130°C, air was blown into the raw material, the flow rate was 100mL / (h g), the reaction temperature was 250°C, and the temperature was kept constant for 5 hours. At this time, the softening point of the raw material after crosslinking was 141°C. During the reaction, keep the reaction system at normal pressure (1 atmospheric pressure); then stop venting the air, add 30g (10wt% of raw material addition) of 1,2,3,4-tetrahydroquinoline in the reactor, then use hydrogen Replace the air in the reactor, and then fill it with hydrogen, so that the pressure inside the reactor is 3MPa, seal the reactor; start stirring, the rotation speed ...

Embodiment 2

[0035] Extract the furfural oil of Huanxiling crude oil decompression distillate from Liaohe Oilfield (kinematic viscosity 136.9mm at 40°C) 2 / s, aromatics content 58.3wt%, cycloalkane content 38.5wt%, paraffin content 2.6wt%) 300g add volume and be in the stainless steel autoclave of 500ml. When the temperature in the reaction kettle rose to 130°C, air with a flow rate of 170mL / (h g) was blown into the raw material under normal pressure. After 6 hours of reaction at 280°C, the softening point of the raw material rose to 158°C; Then stop venting air, add 60g (20wt% of raw material addition) 1,2,3,4-tetrahydroquinoline in reactor, after replacing the air in reactor with hydrogen, charge into hydrogen again, make The pressure in the reactor is 5MPa, and the reactor is closed; start stirring, the speed is 800r / min, and the temperature is raised to 400°C for 8 hours. Introduce hydrogen, and stabilize the pressure of the system at 4.5 MPa through the back pressure valve. After con...

Embodiment 3

[0037] Extract the furfural oil (kinematic viscosity 287.2mm 2 / s, aromatics content 72.1wt%, cycloalkane content 25.4wt%, paraffin content 2.5wt%) 300g add volume and be in the stainless steel autoclave of 500ml. When the temperature in the reaction kettle rose to 150°C, air with a flow rate of 80mL / (h g) was blown into the raw material under normal pressure. After 6 hours of reaction at 250°C, the softening point of the raw material rose to 146°C; Then stop venting air, add 60g (20wt% of raw material addition) 1,2,3,4-tetrahydroquinoline in reactor, after replacing the air in reactor with hydrogen, charge into hydrogen again, make The pressure in the reactor is 5MPa, and the reactor is closed; start stirring, the speed is 1000r / min, the temperature is raised to 450°C, and the reaction is carried out for 5 hours. Pass hydrogen into the middle, and stabilize the pressure of the system at 5 MPa through the back pressure valve, continue the reaction for 5 hours, stop the hydrog...

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Abstract

The invention provides a method of preparing mesophase pitch. The method comprises the following steps: with the furfural extract oil of naphthene-based crude oil vacuum gas oil as raw material, carrying out oxidative cross-linking modification on the raw material by air to obtain an intermediate product; carrying out a co-carbonization treatment on the intermediate product under the synergetic hydrogen supply action of a hydrogen atmosphere and a hydrogen supply solvent to obtain the mesophase pitch, wherein the hydrogen supply solvent is 1,2,3,4-tetrahydroquinoline, and the adding amount is 5-20wt% of the amount of the raw material. According to the method provided by the invention, the cross-linking modification of the raw material is realized by means of air oxidation, thus the softening point and the carbonization yield of the raw material are increased, and moreover, lots of oxygen atoms are not introduced in the molecules of the modified raw material, thus the carbonization action thereof is not influenced; under the hydrogen atmosphere, an appropriate amount of the hydrogen supply solvent is added to carry out synergetic hydrogen supply co-carbonization with the cross-linked raw material, thus the carbonization reaction action of the raw material can be further improved. The mesophase pitch prepared by the method provided by the invention presents a flow state or a large texture-type state.

Description

technical field [0001] The invention relates to the technical field of mesophase pitch preparation, in particular to a method for preparing mesophase pitch by using furfural extracted oil of naphthenic vacuum fraction as a raw material. Background technique [0002] Mesophase pitch (MP for short) is a mixture of a variety of flat disk-shaped condensed ring aromatic hydrocarbons with a relative molecular mass of 370-2000. It is a kind of nematic liquid crystal produced by the heat treatment process of heavy aromatic hydrocarbon mixture. Substance, also known as liquid crystal phase pitch. Mesophase pitch has the advantages of wide source of raw materials, excellent performance, high carbon yield and strong processability. Needle coke, carbon microspheres, composite materials, fluorocarbon materials, carbon foam, carbon sheets and carbon films, mesophase pitch-based electrode materials, high-temperature lubricants, etc. These functional materials will be used in defense indus...

Claims

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Application Information

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IPC IPC(8): C10C3/00C10C3/04
CPCC10C3/00C10C3/04
Inventor 刘东付玉娥娄丹玲陈科宇娄斌侯绪连杜辉李明马文茜何笑雨
Owner CHINA NAT OFFSHORE OIL CORP
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