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Method for preparing spinnable asphalt from coal tar

A technology for coal tar and pitch, applied in the field of preparing spinnable pitch, can solve the problems of low content and large molecular weight, and achieve the effects of simple preparation process, high utilization rate of raw materials, and improved utilization rate

Active Publication Date: 2019-01-11
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Its disadvantage is that the content of asphaltenes in asphaltenes is relatively low, accounting for only about 30%
The structure of pre-asphaltenes is similar to that of asphaltenes, and its content in asphaltenes reaches about 70%, but its molecular weight is relatively large, and it is easy to undergo excessive polymerization during direct thermal condensation polymerization to form secondary quinoline insolubles

Method used

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  • Method for preparing spinnable asphalt from coal tar

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Step 1. Put coal tar in a reaction kettle with a mass of 1500 grams, heat it to 250° C. and distill it under reduced pressure for 2 hours (vacuum degree is 0.08 MPa), and take out the remaining material from the autoclave, which is the heavy component of coal tar. It is 825g.

[0033] Step 2. Add 50g of coal tar heavy fraction and 100g of n-heptane into the Soxhlet extractor, heat to 80°C, extract for 15 hours to obtain extract S1 and raffinate D1, and then use a rotary evaporator to extract S1 Recovery, the residue after solvent recovery is n-heptane soluble matter, and the residue after solvent recovery is placed in a fume hood for ventilation for 3 hours to obtain heavy oil, which is 5g by weighing. The raffinate D1 is baked in an oven to constant weight, put it and 90g toluene into the Soxhlet extractor, heat to 125°C, extract S2 and raffinate D2 after extraction for 12 hours, and then extract the obtained extract S2 Recover with a rotary evaporator, and the residu...

Embodiment 2

[0036] Step 1. Put coal tar in a reaction kettle with a mass of 1500 grams, heat it to 300° C. and distill it under reduced pressure for 2 hours (vacuum degree is 0.08 MPa), and take out the remaining material from the autoclave, which is the heavy component of coal tar. It is 750g.

[0037]Step 2. Put 50g of coal tar heavy fraction and 150g of n-pentane into a Soxhlet extractor, heat to 80°C, extract for 12 hours to obtain extract S1 and raffinate D1, and then use a rotary evaporator for the obtained extract S1 Recovery, the residue after solvent recovery is n-pentane soluble matter, and the residue after solvent recovery is placed in a fume hood for ventilation for 4 hours to obtain heavy oil, which is 5.01g by weighing. The raffinate D1 is baked in an oven to constant weight, put it and 135g xylene into a Soxhlet extractor, heat to 120°C, extract S2 and raffinate D2 after extraction for 14 hours, and then extract the obtained extract S2 is recovered by a rotary evaporator,...

Embodiment 3

[0040] Step 1. Put coal tar in a reaction kettle with a mass of 1500 grams, heat it to 280° C. and distill it under reduced pressure for 2 hours (vacuum degree is 0.08 MPa), and take out the remaining material from the autoclave, which is the heavy component of coal tar. It is 775g.

[0041] Step 2. Add 50g of coal tar heavy fraction and 200g of n-hexane into the Soxhlet extractor, heat to 90°C, extract for 12 hours to obtain extract S1 and raffinate D1, and then recover the obtained extract S1 with a rotary evaporator , the residue after solvent recovery is n-hexane soluble matter, and the residue after solvent recovery is placed in a fume hood to ventilate for 3 hours to obtain heavy oil, which is 5.12g by weighing. The raffinate D1 is baked in an oven to constant weight, put it and 180g of benzene into the Soxhlet extractor, heat to 120°C, extract S2 and raffinate D2 after extraction for 15 hours, and then extract the obtained extract S2 Recover with a rotary evaporator, a...

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Abstract

A method for preparing spinnable asphalt from coal tar comprises the following steps: carrying out high-temperature reduced pressure distillation on the coal tar to obtain a coal tar heavy component;extracting the coal tar heavy component with a primary extraction solvent to obtain a primary extract and a primary raffinate; recovering the solvent from the primary extract to obtain heavy oil; drying the primary raffinate, and extracting the dried primary raffinate with a secondary extraction solvent to obtain a secondary extract and a secondary raffinate; recovering the solvent from the secondary extract to obtain asphaltene; drying the secondary raffinate, and extracting the dried raffinate with a tertiary extraction solvent to obtain a tertiary extract and a tertiary raffinate; recovering the solvent from the tertiary extract to obtain asphaltene; and uniformly mixing all above obtained asphaltenes, adding the obtained mixture into a fixed bed reactor, and carrying out thermal polycondensation to prepare the spinnable asphalt. The method has the advantages of simple process, easiness in solvent recovery, low cost and high yield.

Description

technical field [0001] The invention belongs to a method for preparing spinnable pitch of pitch carbon fiber, in particular to a method for preparing spinnable pitch with coal tar as raw material. Background technique [0002] Pitch-based carbon fiber is a special fiber with a carbon content greater than 92% obtained by refining, spinning, pre-oxidizing, and carbonizing petroleum pitch or coal pitch. Due to its excellent thermodynamic properties, it is widely used in military and civilian fields. [0003] Coal tar heavy fraction is an organic mixture with complex composition and structure mainly composed of aromatic hydrocarbons. The series of products such as light oil and heavy fraction obtained from its deep processing are the basic raw materials for synthetic plastics, synthetic fibers and other industries. Among them, heavy oil and asphaltene (a mixture of asphaltenes and pre-asphaltenes) are important components of coal tar heavy components. Heavy oil is a heavy disti...

Claims

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Application Information

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IPC IPC(8): C10C3/08C10C3/06
CPCC10C3/06C10C3/08
Inventor 左萍萍申文忠曲世杰牛宏贤李充梅
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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