Mesophase pitch and preparation method thereof

A technology of mesophase pitch and asphalt, which is applied in the field of mesophase pitch and its preparation, to achieve the effects of moderate carbon-hydrogen ratio, improved economy, and high aromaticity

Active Publication Date: 2014-08-27
CHNA ENERGY INVESTMENT CORP LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] In order to solve the problems faced in the above-mentioned prior art, the present invention provides a mesophase pitch prepared from direct coal liquefaction residue and a method for preparing mesophase pitch from direct coal liquefaction residue. The present invention prepares mesophase pitch from direct coal liquefaction residue The method of mesophase pitch, under the premise of neither catalytic hydrogenation treatment nor addition of catalyst, the obtained coal direct liquefaction residue pitch is directly subjected to thermal polycondensation to prepare mesophase pitch for spinning, thus avoiding hydrogenation treatment and addition of catalyst Some problems brought about, such as increased process complexity, increased operating costs, worsened risk, difficulty in catalyst removal and recovery, etc.

Method used

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  • Mesophase pitch and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0077] (1) First, the above-mentioned coal direct liquefaction residue and the IBP-110°C liquefied oil produced during the coal direct liquefaction process were subjected to primary extraction at a volume ratio of 1:3 for 50 minutes; the mixture obtained by the primary extraction was separated into solid and liquid, The obtained solid part and the 220-260 ℃ liquefied oil produced during the direct coal liquefaction process were subjected to secondary extraction for 60 minutes at a volume of 1:3, and the soluble part obtained from the two-stage extraction was recovered to obtain the extracted pitch.

[0078](2) Take 200g coal direct liquefaction residue to extract asphalt (volume about 195ml) and mix it with 600mL n-hexane, put it in a mixing tank, dissolve it with n-hexane at 40°C for 30min, then separate it by filtration, and recover the insoluble matter (about 160g ). Then mix the insoluble matter with 550mL tetrahydrofuran, fully dissolve it in the mixing tank for 30 minute...

Embodiment 2

[0082] (1) and (2): Take 156g of refined asphalt obtained by step (1) and step (2) in Example 1.

[0083] (3) Put the above-mentioned refined asphalt in a high-temperature and high-pressure reactor, rapidly raise the temperature to 250°C within 25 minutes, and keep the constant temperature under normal pressure for 30 minutes. Then, the temperature was raised to 415° C. at a rate of 5° C. / min, the pressure was maintained at 3 MPa, and the reaction was performed at a constant temperature for 10 hours.

[0084] (4) Then, cool down to 370°C at a rate of 5°C / min, evacuate to 80mbar (absolute pressure), and maintain for 150min. Naturally cool down to room temperature to obtain mesophase pitch 115g (yield 57.5%), the analysis data is as shown in Table 1 and Figure 1 (b), the mesophase pitch of the present invention has a very high aromatic carbon rate, and its mesophase is Ideal wide-area fusion form.

Embodiment 3

[0086] (1) Using the step (1) in Example 1 to obtain the extracted pitch.

[0087] (2) Mix 1000g of extracted bitumen (volume about 976ml) with 4000mL of n-hexane, put it in a mixing tank, dissolve it with n-hexane at 40°C for 30min, then separate by filtration and recover the insoluble matter (about 795g). Then mix the insoluble matter with 2800mL tetrahydrofuran, fully dissolve in the mixing tank for 30 minutes, filter to remove the insoluble matter, and distill the obtained soluble matter to recover tetrahydrofuran. The two-step extraction operation was repeated successively to obtain 750 g of refined pitch with a softening point of 130°C, an ash content of 0.06%, a sulfur content of 0.03%, and a hydrocarbon molar ratio of 1.28.

[0088] (3) Put the above-mentioned refined asphalt in a high-temperature and high-pressure reaction kettle, rapidly raise the temperature to 330°C within 35 minutes, keep the constant temperature under normal pressure for 30 minutes, and dry the s...

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Abstract

The invention provides a method for preparing mesophase pitch from direct coal liquefaction residues. The method mainly comprises the following steps: 1, extracting the direct coal liquefaction residues by using an organic solvent I to obtain extracted pitch; 2, dissolving the extracted pitch by using a polar organic solvent II, and carrying out solvent recovery on the soluble part to obtain refined pitch; 3, carrying out thermal polycondensation on the obtained refined pitch at a high temperature to obtain a thermal polycondensation product; and 4, carrying out reduced pressure flash evaporation on the thermal polycondensation product to obtain the mesophase pitch. The invention also provides the mesophase pitch. The spinnable indexes of the mesophase pitch are characterized in that the softening point, the aromatic carbon rate and the quinoline insoluble substance content of the mesophase pitch are 250-280DEG C, not lower than 0.9 and 35-45% respectively.

Description

technical field [0001] The invention relates to a mesophase pitch and a preparation method thereof, more specifically, to a method for preparing mesophase pitch by using coal direct liquefaction residue as a raw material and the mesophase pitch obtained therefrom. Background technique [0002] Pitch-based carbon fibers have attracted widespread attention due to their wide source of raw materials, low production cost, high carbon yield, and high modulus, and their applications are becoming more and more extensive. Anisotropic high-quality mesophase pitch is the precursor for preparing high-performance carbon fibers; only general-purpose carbon fibers can be obtained without isotropic pitch in the mesophase stage. Therefore, the modulation of mesophase pitch [0003] It is a key link in the preparation process of high-performance pitch fibers. [0004] Mesophase pitch for spinning requires ideal molecular composition and structure to make it suitable for subsequent applicati...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C10C3/02C10C3/08C10C3/06
Inventor 张胜振盛英刘均庆郑冬芳牛艳华赵永彬宫晓颐
Owner CHNA ENERGY INVESTMENT CORP LTD
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