CN104004538B - The comprehensive utilization process of coal tar refining Carbon Materials raw material - Google Patents
The comprehensive utilization process of coal tar refining Carbon Materials raw material Download PDFInfo
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- CN104004538B CN104004538B CN201410143174.3A CN201410143174A CN104004538B CN 104004538 B CN104004538 B CN 104004538B CN 201410143174 A CN201410143174 A CN 201410143174A CN 104004538 B CN104004538 B CN 104004538B
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Abstract
The invention provides a kind of comprehensive utilization process of coal tar refining Carbon Materials raw material, this technique comprises coal tar and complex solvent 1 carries out one-level extraction process, and obtain the raw material of high-performance carbon material, and this complex solvent 1 is mixed by oxygen heterocyclic solvents, mononuclear aromatics kind solvent and C5-C8 fat hydrocarbon solvent, and the mass percentage of oxygen heterocyclic solvents is 5%-20%, the mass percentage of mononuclear aromatics kind solvent is the mass percentage of 50%-90%, C5-C8 fat hydrocarbon solvent is 5%-30%.The one-level extraction slag blanket that coal tar obtains after one-level extraction process can also extract again with complex solvent 2, obtains additive pitch and can extract slag blanket as the secondary of gasification addition material.Therefore, technical scheme provided by the invention is fairly simple stable, is easy to industrialization, and the purity that raw material is separated is higher, and residue cycling and reutilization, coal tar comprehensive utilization degree is high.
Description
Technical field
The present invention relates to a kind of comprehensive utilization process of coal tar, particularly relate 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 ﹑ Carbon fibe, 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 purifications, high temperature cabonization, aftertreatment usually.The gordian technique that wherein raw materials pretreatment technology is prepared for 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 containing 2-4 ring, needs to refine its raw material when preparing high-performance carbon material.In coal tar containing have an appointment about 90% the compound fragrant hydrocarbon of 2-4 ring, also have the arene at more than small part five rings and five rings in addition.In the preparation process of Carbon Materials, therefore, how the arene obtaining 2-4 ring simple from coal tar becomes the key problem of feed purification technique.
The method of feed purification has a variety of, and it is exactly the most successfully use solvent method that the U.S. and Japan realize industrialization.But, coal tar needed to preheat before mixing with organic solvent (such as toluene etc.), and coal tar is easy and organic solvent generates colloidal structure, thus the solvend making whole process for refining produce and insolubles compare and are difficult to filtering separation, make the purity of the raw material of this Carbon Materials not high, and then make the performance of Carbon Materials not high.In addition, the existing byproduct utilizing coal tar to prepare to produce in the process for refining of the raw material of high-performance carbon material can not be good recycling, and a large portion is because can not get recycling and incinerating as fuel, also wastes a large amount of resources while contaminate environment.
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, can also the byproduct that produces of this technique of comprehensive reutilization while the purity improving Carbon Materials raw material and Carbon Materials performance.
The technical scheme that the present invention improves take coal tar as raw material, adopts complex solvent to carry out extracting the raw material normal temperature extracting and refining comprehensive utilization process obtaining 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) complex solvent 1 and a coal tar is provided, this complex solvent 1 is mixed by oxygen heterocyclic solvents, mononuclear aromatics kind solvent and C5-C8 fat hydrocarbon solvent, and in this complex solvent 1, the mass percentage of oxygen heterocyclic solvents is 5%-20%, the mass percentage of mononuclear aromatics kind solvent is the mass percentage of 50%-90%, C5-C8 fat hydrocarbon solvent is 5%-30%;
(2) mix described complex solvent 1 and described coal tar and stir and obtain one-level extraction suspension;
(3) from described one-level extraction suspension, one-level extraction slag blanket and one-level extraction supernatant liquor is isolated; And
(4) described one-level extraction supernatant liquor is distilled, steam solvent in this one-level extraction supernatant liquor to reclaim and to obtain one as the viscid bitumen of high-performance carbon material feedstock.
Wherein " C5-C8 fat hydrocarbon solvent " herein represents the fat hydrocarbon liquid solvent be made up of 5 –, 8 carbon atoms.
Based on above-mentioned, in described step (2), this complex solvent 1 and the mass percentage blending ratio of this coal tar are complex solvent 1 is 50%-80%, and coal tar is 20%-50%.As, this mass percentage 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 mass percentage of described oxygen heterocyclic solvents is specifically as follows 5%, 8%, 10%, 15%, 20% etc.The mass percentage of described mononuclear aromatics kind solvent is specifically as follows 50%, 55%, 60%, 65%, 70%, 75%, 80%, 85%, 90% etc.The mass percentage 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, e.g., and 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) isolates 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 comprises further:
(5) complex solvent 2 is provided, this complex solvent 2 is 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 mass percentage of this oxygen heterocyclic solvents is 50%-90%, the mass percentage of this mononuclear aromatics kind solvent is 5%-30%, and the mass percentage of this C5-C8 fat hydrocarbon solvent is 1%-20%;
(6) mix the extraction of described one-level slag blanket and described complex solvent 2 also to stir and obtain secondary and extract suspension;
(7) from described secondary extraction suspension, secondary extraction slag blanket and secondary extraction supernatant liquor is isolated; And
(8) distill described secondary extraction supernatant liquor, steam this secondary extraction supernatant liquor in solvent to reclaim and to obtain a binder pitch.
Based on above-mentioned, the mass percentage blending ratio that complex solvent 2 described in described step (6) and described one-level extracts slag blanket be this complex solvent 2 is 50%-80%, and it is 20%-50% that one-level extracts slag blanket.As, this mass percentage blending ratio can be: complex solvent 2 is 60%, and 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 and one-level extract the selection of the blending ratio of slag blanket and one-level to extract the composition of slag blanket relevant, guarantee that the aromatic nucleus in one-level extraction slag blanket has larger solubleness in this complex solvent 2.
Wherein, in complex solvent 2, the mass percentage of described oxygen heterocyclic solvents is specifically as follows 50%, 55%, 60%, 65%, 70%, 75%, 80%, 85%, 90% etc.The mass percentage of described mononuclear aromatics kind solvent is specifically as follows 5%, 8%, 10%, 15%, 20%, 25%, 30% etc.The mass percentage 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 enforcement after described step (1) and before described step (2).Be appreciated that in technical scheme provided by the invention, described step (5) if in complex solvent 2 provide before the described step (6), the above-mentioned order listed need not be defined in.
Based on above-mentioned, described step (1) is tetrahydrofuran (THF), furfural or its mixture with oxa-lopps solvent in 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 described complex solvent 2 and one-level extraction slag blanket airtight mix and blend 0.5 hour-2 hours, e.g., and 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) isolates 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 be approximately-10 DEG C-30 DEG C for temperature range, be preferably 15 DEG C-25 DEG C.
Hinge structure of the present invention has the following advantages:
Component in the complex solvent 1 of the comprehensive utilization process employing of coal tar refining Carbon Materials raw material provided by the invention and the selection of proportion of composing thereof make this complex solvent 1 have larger dissolution equilibrium constant with the aromatic nucleus in coal tar, are conducive to the colloidal state of the aromatic nucleus destroyed in coal tar itself and form colloid with this complex solvent 1; The polarity of the oxy functional groups especially in oxa-lopps solvent and the solvability of complex solvent 1 stronger, therefore, oxa-lopps solvent is easy to dissolve the polar compound in coal tar, aliphatic hydrocarbon can destroy colloidal structure, thus the colloidal state destroying the aromatic nucleus itself in coal tar further and the colloidal state formed with complex solvent 1, improve the utilization ratio of coal tar, obtain the viscid bitumen containing 2-4 condensation aromatic nucleus that purity is more than or equal to 99%, 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 distilled out can be recycled, and reduces material waste, realizes cycling and reutilization.
Further, complex solvent 1 and coal tar are in mixing process, its mass percentage blending ratio is complex solvent 1 is 50%-80%, coal tar is that 20%-50% can promote that coal-tar solvent is in complex solvent 1, and make it have larger dissolution equilibrium constant, thus further destroy the colloidal state of coal tar.
Further, the component of complex solvent 2 and proportion of composing thereof can ensure one-level extraction slag blanket in aromatic nucleus and complex solvent 2 there is 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, thus improve the utilization ratio of coal tar.This one-level extraction slag blanket and complex solvent 2 carry out reextraction and can obtain binder pitch and secondary extracts slag blanket, and this secondary extraction slag blanket can be used as gasifying additive, the solvent simultaneously in reextraction supernatant liquor still can be recycled after fractionation by distillation out.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 and one-level extract slag blanket in mixing process, its mass percentage blending ratio is complex solvent 2 is 50%-80%, one-level extraction slag blanket is that 20%-50% can ensure that one-level extraction slag blanket has larger solubleness with complex solvent 2, thus destroys the colloidal state of the aromatic nucleus in one-level extraction slag blanket.
Further, the comprehensive utilization process of coal tar refining Carbon Materials raw material provided by the invention is the comprehensive utilization extraction process of coal tar, whole extraction process all at room temperature carries out, do not need to preheat coal tar and one-level extraction slag blanket, thus making the less energy consumption of the comprehensive utilization process of this coal tar refining Carbon Materials raw material, cost compare is low.
Accompanying drawing explanation
Fig. 1 is the comprehensive utilization process schema of the coal tar refining Carbon Materials raw material that the embodiment of the present invention provides.
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%(mass percentage, lower same) mix, obtain complex solvent 1; Normal heptane, tetrahydrofuran (THF) and toluene are respectively by 5%, 90%, and 5% ratio carries out being mixed to get complex solvent 2, 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 to be uniformly mixed 1.5 hours (h), standing sedimentation 15h, sedimentation layering, extract one-level supernatant liquor out, distill out the solvent in this supernatant liquor and recycling, obtain the viscid bitumen containing 2-4 ring that purity is 99.4%, and its softening temperature is 44 DEG C, this viscid bitumen can as the raw material of high-quality Carbon Materials.Just above-mentioned one-level extracts the slag blanket that obtains and complex solvent No. 2 solvent carry out secondary extraction, its ratio is slag blanket 30%, solvent 70%, all processes are the same, sedimentation layering, isolates secondary extraction supernatant liquor, and the solvent distilled out in this supernatant liquor recycling, obtain the pitch that softening temperature is 122 DEG C, can as binder pitch.The slag blanket finally obtained uses as gasification addition material.
Embodiment 2
First normal heptane, furfural and toluene are pressed 15% respectively, 10%, 75% mixes, and obtains complex solvent 1, normal heptane, tetrahydrofuran (THF) and toluene are respectively by 15%, 80%, and 5% ratio carries out being mixed to get complex solvent 2, complex solvent 1 is squeezed in stirred pot by 35Kg/h speed, start stirring and add coal tar, its ratio is solvent 80%, coal tar 20%.Airtightly be uniformly mixed 1h, standing sedimentation 10h, sedimentation layering, extract one-level supernatant liquor out, distill out the solvent in this supernatant liquor and recycling, obtain the viscid bitumen containing 2-4 ring that purity is 99.3%, and its softening temperature is 46 DEG C, this viscid bitumen can as the raw material of high-quality Carbon Materials.By the slag blanket that obtains after above-mentioned extraction and complex solvent No. 2 solvent, its ratio is slag blanket 40%, solvent 60%, and all processes are the same.Sedimentation layering, isolates secondary extraction supernatant liquor, and the solvent distilled out in this supernatant liquor recycling, obtain the pitch that softening temperature is 125 DEG C, can as binder pitch.The slag blanket finally obtained uses as gasification addition material.
Embodiment 3
By octane, tetrahydrofuran (THF) and dimethylbenzene respectively by 20%, 10%, 70% mixes, and obtains complex solvent 1, and normal heptane, tetrahydrofuran (THF) and toluene are respectively by 10%, 70%, 20% carries out being mixed to get complex solvent 2, complex solvent 1 is squeezed in stirred pot by 40Kg/h speed, starts stirring and add coal tar, its ratio is solvent 50%, coal tar 50%.Airtightly be uniformly mixed 1h, standing sedimentation 20h, solid-liquid layering, extract one-level supernatant liquor out, distill out the solvent in this clear liquid and recycling, obtain the viscid bitumen containing 2-4 ring that purity is 99.1%, and its softening temperature is 42 DEG C, this viscid bitumen can as the raw material of high-quality Carbon Materials.To extract the slag blanket and complex solvent No. 2 solvent that obtain through above-mentioned one-level, its ratio is slag blanket 25%, solvent 75%, and all processes are the same.Solid-liquid layering, extracts secondary extraction supernatant liquor, distills out the solvent in this secondary extraction supernatant liquor and recycling, obtains the pitch that softening temperature is 124 DEG C, can as binder pitch.The slag blanket finally obtained 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 undertaken being mixed to get complex solvent 2 by 15%, 60%, 25% respectively, complex solvent 1 is squeezed in stirred pot by 25Kg/h speed, start stirring and add coal tar, its ratio is solvent 60%, coal tar 40%.Airtightly be uniformly mixed 2h, standing sedimentation 5h, solid-liquid layering, extract one-level supernatant liquor out, distill out the solvent in this one-level supernatant liquor and recycling, obtain the viscid bitumen containing 2-4 ring that purity is 99.4%, and its softening temperature is 47 DEG C, this viscid bitumen can as the raw material of high-quality Carbon Materials.To extract the slag blanket and complex solvent No. 2 solvent that obtain through above-mentioned one-level, its ratio is slag blanket 50%, solvent 50%, and all processes are the same.Solid-liquid layering, extracts secondary extraction supernatant liquor out, distills out the solvent in this supernatant liquor and reclaim, obtaining the pitch that softening temperature is 125 DEG C, can as binder pitch.The slag blanket finally obtained 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 with reference to preferred embodiment to invention has been detailed description, those of ordinary skill in the field are to be understood that: still can modify to the specific embodiment of the present invention or carry out equivalent replacement to portion of techniques feature; 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 of the present invention protection.
Claims (10)
1. a comprehensive utilization process for coal tar refining Carbon Materials raw material, comprises step:
(1) complex solvent 1 and a coal tar is provided, this complex solvent 1 is mixed by oxygen heterocyclic solvents, mononuclear aromatics kind solvent and C5-C8 fat hydrocarbon solvent, and in this complex solvent 1, the mass percentage of oxygen heterocyclic solvents is 5%-20%, the mass percentage of mononuclear aromatics kind solvent is the mass percentage of 50%-90%, C5-C8 fat hydrocarbon solvent is 5%-30%;
(2) mix described complex solvent 1 and described coal tar and stir and obtain one-level extraction suspension;
(3) from described one-level extraction suspension, one-level extraction slag blanket and one-level extraction supernatant liquor is isolated; And
(4) described one-level extraction supernatant liquor is distilled, steam solvent in this one-level extraction supernatant liquor to reclaim and to obtain one as the viscid bitumen of the raw material of 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 and the mass percentage blending ratio of this coal tar are complex solvent 1 is 50%-80%, 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 by the mode of centrifugation or the described one-level extraction suspension standing sedimentation mode of 0.5 hour-20 hours is isolated described one-level extraction slag blanket and described one-level extraction supernatant liquor.
6. the comprehensive utilization process of coal tar refining Carbon Materials raw material according to claim 1, is characterized in that, comprise further:
(5) complex solvent 2 is provided, this complex solvent 2 is 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 mass percentage of this oxygen heterocyclic solvents is 50%-90%, the mass percentage of this mononuclear aromatics kind solvent is 5%-30%, and the mass percentage of this C5-C8 fat hydrocarbon solvent is 1%-20%;
(6) mix the extraction of described one-level slag blanket and described complex solvent 2 also to stir and obtain secondary and extract suspension;
(7) from described secondary extraction suspension, secondary extraction slag blanket and secondary extraction supernatant liquor is isolated; And
(8) distill described secondary extraction supernatant liquor, steam this secondary extraction supernatant liquor in solvent 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, the mass percentage blending ratio that complex solvent 2 described in described step (6) and described one-level extracts slag blanket be this complex solvent 2 is 50%-80%, and it is 20%-50% that one-level extracts slag blanket.
8. the comprehensive utilization process of the coal tar refining Carbon Materials raw material according to 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. the comprehensive utilization process of coal tar refining Carbon Materials raw material according to claim 6, 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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CN105013800B (en) * | 2015-07-15 | 2017-04-19 | 太原理工大学 | Method for recovering composite extracting agent in extraction and separation process of coal tar waste residues |
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CF01 | Termination of patent right due to non-payment of annual fee |