CN104004538A - Comprehensive utilization process for refining raw material of carbon material by coal tar - Google Patents
Comprehensive utilization process for refining raw material of carbon material by coal tar Download PDFInfo
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Abstract
The invention provides a comprehensive utilization process for refining raw materials of carbon materials by coal tar. The comprehensive utilization process comprises the following steps that: the coal tar and a compound solvent 1 are subjected to a primary extraction process, and raw materials of high-performance carbon materials are obtained; and in addition, the compound solvent 1 is formed by mixing the following ingredients in percentage by mass: 5 percent to 20 percent of oxygen heterocycle solvents, 50 percent to 90 percent of monocyclic aromatic solvents and 5 percent to 30 percent of C5-C8 aliphatic hydrocarbon solvents. A primary extraction slag layer obtained after the coal tar is subjected to the primary extraction process can also be subjected to secondary extraction with a compound solvent 2, and a bonding agnet of asphalt and a secondary extraction slag layer capable of being used as a gasification additive are obtained. Therefore the technical scheme provided by the invention is very simple and stable; the industrialization is easily realized; in addition, the separation purity of the raw materials is higher; residue is recycled and reused; and the comprehensive utilization degree of the coal tar is high.
Description
Technical field
The present invention relates to a kind of comprehensive utilization process of coal tar, relate in particular to a kind of comprehensive utilization process of coal tar refining high-performance carbon material feedstock.
Background technology
Carbon Materials; as ultra high power Zhen Zhuan Jiao ﹑ charcoal fiber, Pao Mo Tan ﹑ Tan Wei Qiu ﹑ binder pitch, mesophase pitch, dipping agent bitumen, carbon/carbon composite, extensively and be efficiently applied to the various fields such as military project, Aeronautics and Astronautics, nuclear energy, electronics, biotechnology, metallurgy, machinery, building, environment protection and daily life.Carbon Materials becomes the important component part of novel high-performance material.
The preparation of Carbon Materials is divided into three steps, i.e. feed purification, high temperature cabonization, aftertreatment conventionally.Wherein raw materials pretreatment technology is the gordian technique prepared of Carbon Materials.The ingredient requirement aromaticity of Carbon Materials is higher, and content of heteroatoms is less, and the raw material of its high-quality is made up of the compound fragrant hydrocarbon that contains 2-4 ring, in the time preparing high-performance carbon material, need to refine its raw material.The compound fragrant hydrocarbon encircling containing the 2-4 of 90% left and right of having an appointment in coal tar, also has small part five rings and arene more than five rings in addition.In the preparation process of Carbon Materials, therefore, how from coal tar, the simple arene that obtains 2-4 ring becomes the key problem of feed purification technique.
The method of feed purification has a variety of, and it is exactly the most successfully to use solvent method that the U.S. and Japan realize industrialization.But, coal tar needed to preheat before such as, mixing with organic solvent (toluene etc.), and coal tar is easy and organic solvent generates colloidal structure, thereby solvend and insolubles that whole process for refining is produced are relatively difficult to filtering separation, make the purity of raw material of this Carbon Materials not high, and then make the performance of Carbon Materials not high.In addition, existingly utilize the recycling that the byproduct that produces in the process for refining of the raw material that coal tar prepares high-performance carbon material can not be good, and a large portion because can not get recycle and incinerate as fuel, in contaminate environment, also wasted a large amount of resources.
Summary of the invention
By Given this, in order to solve the deficiencies in the prior art, the invention provides a kind of comprehensive utilization process of coal tar refining Carbon Materials raw material, this technique in improving the purity and Carbon Materials performance of Carbon Materials raw material, the byproduct can also this technique of comprehensive reutilization producing.
The technical scheme that the present invention improves is taking coal tar as raw material, adopts complex solvent to extract the raw material normal temperature extracting and refining comprehensive utilization process that obtains high-performance carbon material.Particularly, the present invention is achieved through the following technical solutions:
A comprehensive utilization process for coal tar refining Carbon Materials raw material, comprises step:
(1) provide a complex solvent 1 and a coal tar, this complex solvent 1 is to be mixed by oxygen heterocyclic solvents, mononuclear aromatics kind solvent and C5-C8 fat hydrocarbon solvent, and in this complex solvent 1, the quality percentage composition of oxygen heterocyclic solvents is 5%-20%, the quality percentage composition of mononuclear aromatics kind solvent is that the quality percentage composition of 50%-90%, C5-C8 fat hydrocarbon solvent is 5%-30%;
(2) mix described complex solvent 1 and described coal tar stirring and obtain one-level extraction suspension;
(3) from described one-level extraction suspension, isolate one-level extraction slag blanket and one-level extraction supernatant liquor; And
(4) described one-level extraction supernatant liquor is distilled, steam solvent in this one-level extraction supernatant liquor to reclaim and to obtain a viscid bitumen as high-performance carbon material feedstock.
Wherein " C5-C8 fat hydrocarbon solvent " herein represents the fat hydrocarbon liquid solvent being made up of 8 carbon atoms of 5 –.
Based on above-mentioned, in described step (2), this complex solvent 1 is that complex solvent 1 is 50%-80% with the quality percentage composition blending ratio of this coal tar, and coal tar is 20%-50%.As, this quality percentage composition blending ratio can be: complex solvent 1 is 60%, coal tar 40%; Complex solvent 1 is 70%, coal tar 30%; Complex solvent 1 is 80%, coal tar 20%, etc.It should be noted that, complex solvent 1 is fixed according to coal tar oil composition with the blending ratio of coal tar, guarantees that the aromatic nucleus in coal tar has larger solubleness in this complex solvent 1.
Coal tar can be coal-tar heavy oil or coal-tar middle oil, is preferably coal-tar heavy oil.
Wherein, in complex solvent 1, the quality percentage composition of described oxygen heterocyclic solvents is specifically as follows 5%, 8%, 10%, 15%, 20% etc.The quality percentage composition of described mononuclear aromatics kind solvent is specifically as follows 50%, 55%, 60%, 65%, 70%, 75%, 80%, 85%, 90% etc.The quality percentage composition of described C5-C8 fat hydrocarbon solvent is specifically as follows 5%, 10%, 15%, 20%, 25%, 30% etc.
Based on above-mentioned, described step (2) comprises described complex solvent 1 and the airtight mix and blend of coal tar 0.5 hour-2 hours, as, 0.5 hour, 1 hour, 1.5 hours, 2 hours.
Based on above-mentioned, described step (3) adopts the mode of mechanical stirring or ultrasonic stirring to realize.
Based on above-mentioned, described step (3) is isolated described one-level extraction slag blanket and described one-level extraction supernatant liquor by the mode of centrifugation or by the described one-level extraction suspension standing sedimentation mode of 0.5 hour-20 hours, as standing sedimentation 1 hour, 2 hours, 5 hours, 10 hours, 15 hours etc.
Based on above-mentioned, the comprehensive utilization process of described coal tar refining Carbon Materials raw material further comprises:
(5) provide a complex solvent 2, this complex solvent 2 is to be mixed by described oxygen heterocyclic solvents, described mononuclear aromatics kind solvent and described C5-C8 fat hydrocarbon solvent, and in this complex solvent 2, the quality percentage composition of this oxygen heterocyclic solvents is 50%-90%, the quality percentage composition of this mononuclear aromatics kind solvent is 5%-30%, and the quality percentage composition of this C5-C8 fat hydrocarbon solvent is 1%-20%;
(6) mix described one-level extraction slag blanket and described complex solvent 2 stirring and obtain secondary extraction suspension;
(7) from described secondary extraction suspension, isolate secondary extraction slag blanket and secondary extraction supernatant liquor; And
(8) distill described secondary supernatant, steam solvent in this secondary supernatant to reclaim and to obtain a binder pitch.
Based on above-mentioned, complex solvent 2 described in described step (6) is that this complex solvent 2 is 50%-80% with the quality percentage composition blending ratio of described one-level extraction slag blanket, and one-level extraction slag blanket is 20%-50%.As, this quality percentage composition blending ratio can be: complex solvent 2 is 60%, one-level extraction slag blanket is 40%; Complex solvent 2 is 70%, one-level extraction slag blanket 30%; Complex solvent 2 is 75%, one-level extraction slag blanket 25%, etc.It should be noted that, complex solvent 2 is relevant with the composition of one-level extraction slag blanket with the selection of the blending ratio of one-level extraction slag blanket, guarantees that the aromatic nucleus in one-level extraction slag blanket has larger solubleness in this complex solvent 2.
Wherein, in complex solvent 2, the quality percentage composition of described oxygen heterocyclic solvents is specifically as follows 50%, 55%, 60%, 65%, 70%, 75%, 80%, 85%, 90% etc.The quality percentage composition of described mononuclear aromatics kind solvent is specifically as follows 5%, 8%, 10%, 15%, 20%, 25%, 30% etc.The quality percentage composition of described C5-C8 fat hydrocarbon solvent is specifically as follows 1%, 3%, 5%, 10%, 15%, 20% etc.
In actual industrial technological process, in order to implement conveniently, described step (5) can also described step (1) afterwards and described step (2) implement before.Be appreciated that in technical scheme provided by the invention, the complex solvent 2 in described step (5), as long as provide before in described step (6), need not be defined in the above-mentioned order of listing.
Based on above-mentioned, described step (1) is tetrahydrofuran (THF), furfural or its mixture with the middle oxa-lopps solvent of step (5), described monocyclic aromatic is benzene,toluene,xylene or its any mixture, and described C5-C8 fat hydrocarbon solvent is Skellysolve A, normal hexane, normal heptane, octane, iso-pentane, isohexane, isoheptane, octane-iso or its any mixture.
Based on above-mentioned, described step (6) comprises the airtight mix and blend of described complex solvent 2 and one-level extraction slag blanket 0.5 hour-2 hours, as, 0.5 hour, 1 hour, 1.5 hours, 2 hours.
Based on above-mentioned, described step (6) adopts the mode of mechanical stirring or ultrasonic stirring to realize.
Based on above-mentioned, described step (7) is isolated described secondary extraction slag blanket and described secondary extraction supernatant liquor by the mode of centrifugation or by the described secondary extraction suspension standing sedimentation mode of 0.5 hour-20 hours, as standing sedimentation 1 hour, 2 hours, 5 hours, 10 hours, 15 hours etc.
Based on above-mentioned, described step (2) or step (6) are carried out at normal temperatures.Room temperature of the present invention for temperature range is approximately-10 DEG C-30 DEG C, be preferably 15 DEG C-25 DEG C.
The present invention is relative, and prior art has the following advantages:
Component in the complex solvent 1 that the comprehensive utilization process of coal tar refining Carbon Materials raw material provided by the invention adopts and the selection of proportion of composing thereof make this complex solvent 1 and the aromatic nucleus in coal tar have larger dissolution equilibrium constant, are conducive to destroy the colloidal state of the aromatic nucleus in coal tar itself and form colloid with this complex solvent 1; Especially the polarity of the oxy functional groups in oxa-lopps solvent and the solvability of complex solvent 1 are more intense, therefore, oxa-lopps solvent is easy to dissolve the polar compound in coal tar, aliphatic hydrocarbon can destroy colloidal structure, thereby the colloidal state that further destroys the colloidal state of the aromatic nucleus in coal tar itself and form with complex solvent 1, improve the utilization ratio of coal tar, obtain purity and be more than or equal to 99% the viscid bitumen containing 2-4 condensation aromatic nucleus, be applicable to preparing high-performance carbon material.In addition, coal tar adopts this complex solvent 1 extraction process simple and stable and can serialization industrial production.In addition, the solvent in the one-level extraction supernatant liquor distilling out can be recycled, and reduces material waste, realizes cycling and reutilization.
Further, complex solvent 1 and coal tar are in mixing process, its quality percentage composition blending ratio is that complex solvent 1 is 50%-80%, coal tar is 20%-50% can promote coal-tar solvent in complex solvent 1, and make it have larger dissolution equilibrium constant, thereby further destroy the colloidal state of coal tar.
Further, the component of complex solvent 2 and proportion of composing thereof can ensure that aromatic nucleus and the complex solvent 2 in one-level extraction slag blanket has larger dissolution equilibrium constant, destroy the colloidal state of the aromatic nucleus in one-level extraction slag blanket, improve the utilization ratio of one-level extraction slag blanket, thereby improve the utilization ratio of coal tar.This one-level extraction slag blanket and complex solvent 2 carry out reextraction can obtain binder pitch and secondary extraction slag blanket, and this secondary extraction slag blanket can be used as gasifying additive, the solvent in while reextraction supernatant liquor still can be recycled after out in fractionation by distillation.Therefore, the byproduct that coal tar obtains in the process of reextraction can utilize, and realizes the cycling and reutilization of waste residue, improves the comprehensive utilization ratio of coal tar, reduces energy dissipation.
Further, complex solvent 2 extracts slag blanket in mixing process with one-level, its quality percentage composition blending ratio is that complex solvent 2 is 50%-80%, one-level extraction slag blanket is 20%-50% can ensure that one-level extraction slag blanket has larger solubleness with complex solvent 2, thereby destroys one-level and extract the colloidal state of the aromatic nucleus in slag blanket.
Further, the comprehensive utilization extraction process that the comprehensive utilization process of coal tar refining Carbon Materials raw material provided by the invention is coal tar, whole extraction process all at room temperature carries out, do not need coal tar and one-level extraction slag blanket to preheat, thereby the less energy consumption that makes the comprehensive utilization process of this coal tar refining Carbon Materials raw material, cost compare is low.
Brief description of the drawings
Fig. 1 is the comprehensive utilization process schema of the coal tar refining Carbon Materials raw material that provides of the embodiment of the present invention.
Embodiment
Below by embodiment, technical scheme of the present invention is described in further detail, and following embodiment adopts the comprehensive utilization process flow process of the coal tar refining Carbon Materials raw material shown in Fig. 1 to realize.
Embodiment 1
Normal hexane, tetrahydrofuran (THF) and benzene are respectively by 5%, 5%, 90%(quality percentage composition, lower same) mix, obtain complex solvent 1; Normal heptane, tetrahydrofuran (THF) and toluene are mixed to get complex solvent 2 by 5%, 90%, 5% ratio respectively, and complex solvent 1 is squeezed in stirred pot by 30Kg/h speed, then starts stirring, adds coal-tar middle oil, and its ratio is solvent 70%, coal tar 30%.Airtightly be uniformly mixed 1.5 hours (h), standing sedimentation 15h, sedimentation layering, extract one-level supernatant liquor out, distill out solvent recycling in this supernatant liquor, obtain purity and be 99.4% the viscid bitumen containing 2-4 ring, and its softening temperature is 44 DEG C, this viscid bitumen can be used as the raw material of high-quality Carbon Materials.Just above-mentioned one-level extracts slag blanket and No. 2 solvent of complex solvent of obtaining and carries out secondary extraction, its ratio is slag blanket 30%, solvent 70%, all processes are the same, sedimentation layering, isolates secondary supernatant, and distills out solvent recycling in this supernatant liquor, obtain softening temperature and be the pitch of 122 DEG C, can be used as binder pitch.The slag blanket finally obtaining uses as gasification addition material.
Embodiment 2
First normal heptane, furfural and toluene are pressed to 15% respectively, 10%, 75% mixes, and obtains complex solvent 1, normal heptane, tetrahydrofuran (THF) and toluene are mixed to get complex solvent 2 by 15%, 80%, 5% ratio respectively, complex solvent 1 is squeezed in stirred pot by 35Kg/h speed, start and stir that to add coal tar, its ratio be solvent 80%, coal tar 20%.The airtight 1h that is uniformly mixed, standing sedimentation 10h, sedimentation layering, extract one-level supernatant liquor out, distill out solvent recycling in this supernatant liquor, obtain purity and be 99.3% the viscid bitumen containing 2-4 ring, and its softening temperature is 46 DEG C, and this viscid bitumen can be used as the raw material of high-quality Carbon Materials.By the slag blanket obtaining after above-mentioned extraction and No. 2 solvent of complex solvent, its ratio is slag blanket 40%, solvent 60%, and all processes are the same.Sedimentation layering, isolates secondary supernatant, and distills out solvent recycling in this supernatant liquor, obtains softening temperature and be the pitch of 125 DEG C, can be used as binder pitch.The slag blanket finally obtaining uses as gasification addition material.
Embodiment 3
Octane, tetrahydrofuran (THF) and dimethylbenzene are pressed to 20% respectively, 10%, 70% mixes, and obtains complex solvent 1, and normal heptane, tetrahydrofuran (THF) and toluene are respectively by 10%, 70%, 20% is mixed to get complex solvent 2, and complex solvent 1 is squeezed in stirred pot by 40Kg/h speed, starts to stir to add coal tar, its ratio is solvent 50%, coal tar 50%.The airtight 1h that is uniformly mixed, standing sedimentation 20h, solid-liquid layering, extract one-level supernatant liquor out, distill out solvent recycling in this clear liquid, obtain purity and be 99.1% the viscid bitumen encircling containing 2-4, and its softening temperature is 42 DEG C, and this viscid bitumen can be used as the raw material of high-quality Carbon Materials.To extract slag blanket and No. 2 solvent of complex solvent of obtaining through above-mentioned one-level, its ratio is slag blanket 25%, solvent 75%, and all processes are the same.Solid-liquid layering, extracts secondary supernatant, distills out solvent recycling in this secondary supernatant, obtains softening temperature and be the pitch of 124 DEG C, can be used as binder pitch.The slag blanket finally obtaining uses as gasification addition material.
Embodiment 4
Normal hexane, furfural and dimethylbenzene are respectively by 30%, 20%, 50% mixes, and obtains complex solvent 1, normal heptane, furfural and toluene are mixed to get complex solvent 2 by 15%, 60%, 25% respectively, complex solvent 1 is squeezed in stirred pot by 25Kg/h speed, start and stir that to add coal tar, its ratio be solvent 60%, coal tar 40%.The airtight 2h that is uniformly mixed, standing sedimentation 5h, solid-liquid layering, extract one-level supernatant liquor out, distill out solvent recycling in this one-level supernatant liquor, obtain purity and be 99.4% the viscid bitumen containing 2-4 ring, and its softening temperature is 47 DEG C, and this viscid bitumen can be used as the raw material of high-quality Carbon Materials.To extract slag blanket and No. 2 solvent of complex solvent of obtaining through above-mentioned one-level, its ratio is slag blanket 50%, solvent 50%, and all processes are the same.Solid-liquid layering, extracts secondary supernatant out, distills out solvent in this supernatant liquor and reclaims, and obtains softening temperature and be the pitch of 125 DEG C, can be used as binder pitch.The slag blanket finally obtaining uses as gasification addition material.
Finally should be noted that: above embodiment is only in order to illustrate that technical scheme of the present invention is not intended to limit; Although the present invention is had been described in detail with reference to preferred embodiment, those of ordinary skill in the field are to be understood that: still can modify or part technical characterictic is equal to replacement the specific embodiment of the present invention; And not departing from the spirit of technical solution of the present invention, it all should be encompassed in the middle of the technical scheme scope of request protection of the present invention.
Claims (10)
1. a comprehensive utilization process for coal tar refining Carbon Materials raw material, comprises step:
(1) provide a complex solvent 1 and a coal tar, this complex solvent 1 is to be mixed by oxygen heterocyclic solvents, mononuclear aromatics kind solvent and C5-C8 fat hydrocarbon solvent, and in this complex solvent 1, the quality percentage composition of oxygen heterocyclic solvents is 5%-20%, the quality percentage composition of mononuclear aromatics kind solvent is that the quality percentage composition of 50%-90%, C5-C8 fat hydrocarbon solvent is 5%-30%;
(2) mix described complex solvent 1 and described coal tar stirring and obtain one-level extraction suspension;
(3) from described one-level extraction suspension, isolate one-level extraction slag blanket and one-level extraction supernatant liquor; And
(4) described one-level extraction supernatant liquor is distilled, steam solvent in this one-level extraction supernatant liquor to reclaim and to obtain the viscid bitumen of a raw material as high-performance carbon material.
2. the comprehensive utilization process of coal tar refining Carbon Materials raw material according to claim 1, it is characterized in that, in described step (2), this complex solvent 1 is that complex solvent 1 is 50%-80% with the quality percentage composition blending ratio of this coal tar, and coal tar is 20%-50%.
3. the comprehensive utilization process of coal tar refining Carbon Materials raw material according to claim 1, is characterized in that, described step (2) comprises described complex solvent 1 and the airtight mix and blend of coal tar 0.5 hour-2 hours.
4. the comprehensive utilization process of coal tar refining Carbon Materials raw material according to claim 1, is characterized in that, described step (2) adopts the mode of mechanical stirring or ultrasonic stirring to realize.
5. the comprehensive utilization process of coal tar refining Carbon Materials raw material according to claim 1, it is characterized in that, described step (3) is isolated described one-level extraction slag blanket and described one-level extraction supernatant liquor by the mode of centrifugation or by the described one-level extraction suspension standing sedimentation mode of 0.5 hour-20 hours.
6. the comprehensive utilization process of coal tar refining Carbon Materials raw material according to claim 1, is characterized in that, further comprises:
(5) provide a complex solvent 2, this complex solvent 2 is to be mixed by described oxygen heterocyclic solvents, described mononuclear aromatics kind solvent and described C5-C8 fat hydrocarbon solvent, and in this complex solvent 2, the quality percentage composition of this oxygen heterocyclic solvents is 50%-90%, the quality percentage composition of this mononuclear aromatics kind solvent is 5%-30%, and the quality percentage composition of this C5-C8 fat hydrocarbon solvent is 1%-20%;
(6) mix described one-level extraction slag blanket and described complex solvent 2 stirring and obtain secondary extraction suspension;
(7) from described secondary extraction suspension, isolate secondary extraction slag blanket and secondary extraction supernatant liquor; And
(8) distill described secondary supernatant, steam solvent in this secondary supernatant to reclaim and to obtain a binder pitch.
7. the comprehensive utilization process of coal tar refining Carbon Materials raw material according to claim 6, it is characterized in that, complex solvent 2 described in described step (6) is that this complex solvent 2 is 50%-80% with the quality percentage composition blending ratio of described one-level extraction slag blanket, and one-level extraction slag blanket is 20%-50%.
8. according to the comprehensive utilization process of the coal tar refining Carbon Materials raw material described in claim 1 or 6, it is characterized in that, described oxa-lopps solvent is tetrahydrofuran (THF), furfural or its mixture, described monocyclic aromatic is benzene,toluene,xylene or its any mixture, and described C5-C8 fat hydrocarbon solvent is Skellysolve A, normal hexane, normal heptane, octane, iso-pentane, isohexane, isoheptane, octane-iso or its any mixture.
9. according to the comprehensive utilization process of the coal tar refining Carbon Materials raw material described in claim 1 or 6, it is characterized in that, described step (2) or step (6) are carried out at normal temperatures.
10. the comprehensive utilization process of coal tar refining Carbon Materials raw material according to claim 6, it is characterized in that, described step (7) comprises isolates described secondary extraction slag blanket and described secondary extraction supernatant liquor by the described secondary extraction suspension standing sedimentation mode of 0.5 hour-20 hours.
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| CN104004538B (en) | 2015-11-11 |
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