CN102653397A - Preparation method of coal tar-based mesocarbon microbead - Google Patents
Preparation method of coal tar-based mesocarbon microbead Download PDFInfo
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Abstract
The invention discloses a preparation method of a coal tar-based mesocarbon microbead, comprising a process flow of pretreatment of raw materials, pyrocondensation polymerization reaction, separation and drying. The preparation method specifically comprises the following steps of: extracting, separating and removing primary quinoline insolubles of coal tar, as the raw materials, by using a mixed solvent to obtain coal tar refined soft pitch; then polymerizing the coal tar refined soft pitch for 1-8 hours at 350-450 DEG C under the rotating speed of 100-500 r/min and under the protection of inert gases by using anthracene oil or silicone oil as a reaction system viscosity regulator to obtain carbon microbead-containing mesophase pitches; and extracting by using a solvent, and drying to obtain the mesocarbon microbead. The particle diameter of the coal tar-based mesocarbon microbead prepared by using the method is 1-150 mu m, and the mass percent can reach 20-50%. The preparation method of the coal tar-based mesocarbon microbead has the characteristics of high product yield, controllable particle diameter, good sphericity, simple and convenient process, rich raw material sources, low cost and the like.
Description
Technical field
The invention belongs to the carbon material field, relate in particular to a kind of preparation method of coal-tar base MCMB.
Background technology
MCMB (MCMB) is a kind of novel charcoal material; Owing to have unique laminate structure and excellent physicochemical characteristic, thereby well used at aspects such as high-density C/C matrix material, active carbon with high specific surface area and ion secondary battery cathode material lithium, high speed liquid chromatography filler, support of the catalyst.
At present, the preparation method of MCMB mainly contains thermal polycondensation process, emulsion process and suspension method.Thermal polycondensation process is at first to make the production of condensed-nuclei aromatics polymerizable raw material contain the mesophase pitch of carbon microspheres through thermal treatment, adopts suitable separation means that MCMB is separated from mother liquor then.Emulsion process is the fusion mesophase pitch to be scattered in the heat stable dielectric melt down at 300-400 ℃, relies on the surface tension balling-up, separates promptly getting MCMB after the cooling.Suspension method is that mesophase pitch is dissolved in the organic solvent, utilizes tensio-active agent and water or other solvent composition suspension-s, powerful at a certain temperature stirring balling-up, and filtration, drying obtain MCMB then.Though emulsion process and suspension method can prepare the uniform product of particle diameter; But need good medium of high-temperature thermal stability and tensio-active agent, and high to the requirement of raw material, and needing solvable fusile mesophase pitch is raw material; So emulsion method and suspension method complex process, the suitability for industrialized production difficulty.Thermal polycondensation process technology is simple, control easily, but existing industrialized preparing process exists MCMB size distribution broad and yield generally to be no more than 20% shortcoming, and in order to overcome its deficiency, people have carried out deeply and extensive studies it.
Consult documents and materials; Chinese patent publication number CN1197833A discloses a kind of preparation method of MCMB, and this method is a raw material with coal tar or petroleum industry heavy oil; At first remove the pyridine insoluble in the raw material through the heat filtering method, thermopolymerization then, separation obtain MCMB.Though this method has been removed pyridine insoluble, the yield of MCMB is lower.Chinese patent publication number CN1308113A; A kind of copolycondensation preparation method of MCMB is disclosed; This method is raw material with coal-tar middle oil pitch with the secondary petroleum heavy oil that contains quinoline insolubles, prepares MCMB through hot copolycondensation, solvent extraction.Though this method has obtained the high MCMB yield of more conventional thermal polycondensation, because quinoline insolubles is not removed in the raw material, so influenced the further raising of carbon microspheres yield.Chinese patent publication number CN1278513A, CN1382624A and CN1272453A disclose a kind of preparation method of MCMB, and this method belongs to the catalysis thermal polycondensation process, and its preparation process comprises raw material outfit, polyreaction, separation and drying.Though this method can significantly improve the yield of carbon microspheres; But owing in raw material is equipped with, added the catalyzer of 0.1-20%; So need to increase the step that removes of catalyzer, complex process, and also the existence of trace catalyst is influential to the raw material of wood-charcoal material performance of following process preparation in the carbon microspheres.
Summary of the invention
The object of the present invention is to provide a kind of raw material sources extensive, cost is low, and technology is simple, can obviously improve the preparation method of the MCMB of MCMB yield.
To above-mentioned purpose, coal-tar base MCMB preparing method's of the present invention technical process comprises the pre-treatment of raw material, thermal polycondensation reaction, separates and drying.Existing that the operation division is following:
A. the pre-treatment of raw material
With coal tar is raw material; At first air distillation cuts the cut before 280 ℃; Obtain the straight run viscid bitumen of 30-40 ℃ of softening temperature, with solvent oil that is rich in aromatic hydrocarbons and the mixed extractant solvent straight run viscid bitumen that is rich in the solvent oil of alkane, the mass ratio of straight run viscid bitumen and mixed solvent is 1: 0.6-1.0; Quiescent settling, separation, distillation remove solvent then, obtain the coal tar refining viscid bitumen.
The said solvent oil that is rich in aromatic hydrocarbons comprises any one in crude benzol, heavy benzol, xylol, washing oil, heavy aromatics oil, the carbolineum; The solvent oil that is rich in alkane comprises the arbitrary combination of any one or they in sherwood oil, gasoline, aviation kerosene, solar oil, the Yellow Protopet 2A, and the solvent oil that is rich in aromatic hydrocarbons in the mixed solvent is 1 with the mass ratio that is rich in the solvent oil of alkane: 0.6-1.0.
Said extraction temperature is 100-150 ℃, and the extraction time is 30-60 minute, and stirring velocity is 100-500 rev/min.The quiescent settling time is 1-6 hour.
Quinoline non-soluble amount percentage composition＜0.1% of the coal tar refining viscid bitumen that above-mentioned mixed extractant solvent obtains, softening temperature is 30-40 ℃, quality percentage yield is 50-75%.
B. thermal polycondensation reaction
The coal tar refining viscid bitumen of above-mentioned acquisition is carried out the thermal polycondensation reaction, obtain to contain the mesophase pitch of carbon microspheres, the parameter of its thermal polycondensation reaction is following:
Heat-up rate: 1-5 ℃/minute;
Temperature of reaction: 350-450 ℃;
Reaction times: 1-8 hour;
Stirring velocity: 100-500 rev/min;
Reaction atmosphere: the protective atmosphere that nitrogen or id reaction produce.
The viscosity modifier carbolineum or the silicone oil of reaction system are added in described thermal polycondensation reaction, and its add-on is 0.1-0.4 a times of coal tar refining viscid bitumen quality.
C. separate
After heat polymerization finishes, naturally cooling, mesophase pitch is extracted to colourless in cable-styled extractor with organic solvent, obtain solid insoluble.Solvent load is 20～50 times of the mesophase pitch quality that is extracted.
Said organic solvent comprises benzene, toluene, pyridine, quinoline, THF, N, any one in dinethylformamide, DMAC N,N, acetone, the N-Methyl pyrrolidone or arbitrary combination.
D. dry
The solid insoluble of above-mentioned gained is the coal-tar base MCMB after drying, its drying parameter is:
Drying temperature: 60-150 ℃;
Vacuum tightness: 0.1-1 * 10
3Pa.
The present invention compared with prior art, the beneficial effect of generation is embodied in:
1. the present invention can control granularity, size distribution and the condition of surface of MCMB through kind and the composition of adjustment raw material, character and the parameter of polyreaction and the add-on of carbolineum or silicone oil of refined asphaltic bitumen.Can prepare the higher pitch of coal-tar base MCMB content.
2. adopt the coal-tar base MCMB of method preparation of the present invention, its particle size range is 1-150 μ m, and run-of-the-mill percentage yield can reach 20-50%.
3. raw material sources are wide, and are cheap, and cost is low.
4. technology is simple, is easy to combine with existing production technique, is convenient to industrialization production.
5. product cut size, form, controllable microstructure.
6. the end-use of the present invention's acquisition is extensive.
Embodiment
With concrete embodiment the present invention is further explained below, but therefore do not limit the present invention.
Embodiment 1
The coal tar air distillation is cut the cut before 280 ℃, obtain the straight run viscid bitumen of 37 ℃ of softening temperatures.The mixed solvent of straight run viscid bitumen and heavy aromatics oil and gasoline is pressed 1: 0.8 mixed of mass ratio; Heavy aromatics oil and quality of gasoline ratio are 1: 0.6 in the mixed solvent; After 120 ℃ of speed with 300 rev/mins stir 30 minutes, static 1.5 hours, tell extraction phase; Steaming solvent, to obtain the quinoline insolubles mass content be 0.08% refining viscid bitumen, and its quality percentage yield is 74.2%.The coal tar refining viscid bitumen that obtains is added in the reaction kettle, under nitrogen protection, be warmed up to 420 ℃ with 3 ℃/minute speed, polyreaction obtained mesophase pitch in 4 hours under 200 rev/mins stir speed (S.S.).After the mesophase pitch cooling, extremely colourless with the pyridine extracting, the pyridine consumption is 20 times of the mesophase pitch quality that is extracted, and solid insoluble is at 80 ℃, 0.5 * 10
3Dry back acquisition particle size range is the MCMB of 1-150 μ m under the vacuum tightness of Pa, and its quality percentage yield is 28.6%.
Embodiment 2
The coal tar air distillation is cut the cut before 280 ℃, obtain the straight run viscid bitumen of 32 ℃ of softening temperatures.The mixed solvent of straight run viscid bitumen and washing oil and kerosene is pressed 1: 0.6 mixed of mass ratio; The mass ratio of washing oil and kerosene is 1: 0.8 in the mixed solvent; After 130 ℃ of speed with 500 rev/mins stir 45 minutes, static 3 hours, tell extraction phase; Steaming solvent, to obtain the quinoline insolubles mass content be 0.09% refining viscid bitumen, and its quality percentage yield is 68.3%.The coal tar refining viscid bitumen that obtains is added in the reaction kettle, under nitrogen protection, be warmed up to 450 ℃ with 2 ℃/minute speed, polyreaction obtained mesophase pitch in 6 hours under 100 rev/mins stir speed (S.S.).After the mesophase pitch cooling, extremely colourless with the quinoline extracting, the pyridine consumption is 30 times of the mesophase pitch quality that is extracted, and solid insoluble is at 100 ℃, 0.1 * 10
3Dry back acquisition particle size range is the MCMB of 1-130 μ m under the vacuum tightness of Pa, and its quality percentage yield is 26.4%.
Embodiment 3
The coal tar air distillation is cut the cut before 280 ℃, obtain the straight run viscid bitumen of 38 ℃ of softening temperatures.The mixed solvent of straight run viscid bitumen and carbolineum and Yellow Protopet 2A is pressed 1: 1.0 mixed of mass ratio; The mass ratio of carbolineum and Yellow Protopet 2A is 1: 1.0 in the mixed solvent; After 150 ℃ of speed with 100 rev/mins stir 60 minutes, static 1 hour, tell extraction phase; Steaming solvent, to obtain the quinoline insolubles mass content be 0.02% refining viscid bitumen, and its quality percentage yield is 54.6%.The coal tar refining viscid bitumen that obtains is added in the reaction kettle, under nitrogen protection, be warmed up to 380 ℃ with 1 ℃/minute speed, polyreaction obtained mesophase pitch in 7 hours under 400 rev/mins stir speed (S.S.).After the mesophase pitch cooling, extremely colourless with 1: 1 benzene of volume ratio and acetone extracting, its consumption is 50 times of the mesophase pitch quality that is extracted, and solid insoluble is at 120 ℃, 0.2 * 10
3Dry back acquisition particle size range is the MCMB of 1-100 μ m under the vacuum tightness of Pa, and its quality percentage yield is 34.6%.
Embodiment 4
The coal tar air distillation is cut the cut before 280 ℃, obtain the straight run viscid bitumen of 34 ℃ of softening temperatures.The mixed solvent of 600g straight run viscid bitumen and heavy benzol and sherwood oil is pressed 1: 0.8 mixed of mass ratio; The mass ratio of heavy benzol and sherwood oil is 1: 0.8 in the mixed solvent; After 130 ℃ of speed with 400 rev/mins stir 30 minutes, static 5 hours, tell extraction phase; Steaming solvent, to obtain the quinoline insolubles mass content be 0.08% refining viscid bitumen, and its quality percentage yield is 52.6%.The coal tar refining viscid bitumen that obtains is added in the reaction kettle, under nitrogen protection, be warmed up to 420 ℃ with 2 ℃/minute speed, polyreaction obtained mesophase pitch in 8 hours under 300 rev/mins stir speed (S.S.).After the mesophase pitch cooling, extremely colourless with 1: 1 toluene of volume ratio and pyridine extracting, its consumption is 30 times of the mesophase pitch quality that is extracted, and solid insoluble is at 100 ℃, 0.1 * 10
3Dry back acquisition particle size range is the MCMB of 1-90 μ m under the vacuum tightness of Pa, and its quality percentage yield is 28.7%.
Embodiment 5
The coal tar air distillation is cut the cut before 280 ℃, obtain the straight run viscid bitumen of 36 ℃ of softening temperatures.The mixed solvent of straight run viscid bitumen and xylol and kerosene is pressed 1: 0.8 mixed of mass ratio; The mass ratio of xylol and kerosene is 1: 0.7 in the mixed solvent; After 140 ℃ of speed with 200 rev/mins stir 45 minutes, static 4 hours, tell extraction phase; Steaming solvent, to obtain the quinoline insolubles mass content be 0.04% refining viscid bitumen, and its quality percentage yield is 70.4%.The coal tar refining viscid bitumen that obtains is added in the reaction kettle, under nitrogen protection, be warmed up to 400 ℃ with 5 ℃/minute speed, polyreaction obtained mesophase pitch in 4 hours under 200 rev/mins stir speed (S.S.).After the mesophase pitch cooling, with 1: 1 quinoline of volume ratio and N, the dinethylformamide extracting is extremely colourless, and its consumption is 40 times of the mesophase pitch quality that is extracted, and solid insoluble is at 80 ℃, 0.1 * 10
3Dry back acquisition particle size range is the MCMB of 1-110 μ m under the vacuum tightness of Pa, and its quality percentage yield is 31.9%.
Embodiment 6
The coal tar air distillation is cut the cut before 280 ℃, obtain the straight run viscid bitumen of 33 ℃ of softening temperatures.The mixed solvent of straight run viscid bitumen and washing oil and Yellow Protopet 2A is pressed 1: 0.8 mixed of mass ratio; The mass ratio of washing oil and Yellow Protopet 2A is 1: 0.8 in the mixed solvent; After 130 ℃ of speed with 200 rev/mins stir 60 minutes, static 2 hours, tell extraction phase; Steaming solvent, to obtain the quinoline insolubles mass content be 0.01% refining viscid bitumen, and its quality percentage yield is 65%.Coal tar refining viscid bitumen that obtains and carbolineum are pressed in mass ratio adding in 1: 0.1 reaction kettle, under nitrogen protection, be warmed up to 420 ℃ with 2 ℃/minute speed, polyreaction obtained mesophase pitch in 6 hours under 300 rev/mins stir speed (S.S.).After the mesophase pitch cooling, extremely colourless with 1: 1 pyridine of volume ratio and THF extracting, its consumption is 30 times of the mesophase pitch quality that is extracted, and solid insoluble is at 80 ℃, 0.1 * 10
3Dry back acquisition particle size range is the MCMB of 1-110 μ m under the vacuum tightness of Pa, and its quality percentage yield is 41.4%.
Embodiment 7
The coal tar air distillation is cut the cut before 280 ℃, obtain the straight run viscid bitumen of 35 ℃ of softening temperatures.The mixed solvent of straight run viscid bitumen and washing oil and kerosene is pressed 1: 0.8 mixed of mass ratio; The mass ratio of washing oil and kerosene is 1: 0.8 in the mixed solvent; After 130 ℃ of speed with 200 rev/mins stir 60 minutes, static 2 hours, tell extraction phase; Steaming solvent, to obtain the quinoline insolubles mass content be 0.03% refining viscid bitumen, and its quality percentage yield is 62.8%.Coal tar refining viscid bitumen that obtains and carbolineum are pressed in mass ratio adding in 1: 0.2 reaction kettle, under nitrogen protection, be warmed up to 420 ℃ with 2 ℃/minute speed, polyreaction obtained mesophase pitch in 8 hours under 300 rev/mins stir speed (S.S.).After the mesophase pitch cooling, extremely colourless with 1: 1 pyridine of volume ratio and quinoline extracting, its consumption is 40 times of the mesophase pitch quality that is extracted, and solid insoluble is at 80 ℃, 0.1 * 10
3Dry back acquisition particle size range is the MCMB of 1-80 μ m under the vacuum tightness of Pa, and its quality percentage yield is 49.7%.
Embodiment 8
The coal tar air distillation is cut the cut before 280 ℃, obtain the straight run viscid bitumen of 36 ℃ of softening temperatures.The mixed solvent of straight run viscid bitumen and heavy aromatics oil and diesel oil is pressed 1: 0.8 mixed of mass ratio; The mass ratio of heavy aromatics oil and diesel oil is 1: 0.8 in the mixed solvent; After 130 ℃ of speed with 200 rev/mins stir 60 minutes, static 2 hours, tell extraction phase; Steaming solvent, to obtain the quinoline insolubles mass content be 0.02% refining viscid bitumen, and its quality percentage yield is 67.4%.Coal tar refining viscid bitumen that obtains and carbolineum are pressed in mass ratio adding in 1: 0.4 reaction kettle, under nitrogen protection, be warmed up to 440 ℃ with 2 ℃/minute speed, polyreaction obtained mesophase pitch in 8 hours under 300 rev/mins stir speed (S.S.).After the mesophase pitch cooling, extremely colourless with the pyridine extracting, its consumption is 30 times of the mesophase pitch quality that is extracted, and solid insoluble is at 80 ℃, 0.1 * 10
3Dry back acquisition particle size range is the MCMB of 1-50 μ m under the vacuum tightness of Pa, and its quality percentage yield is 46.8%.
Embodiment 9
The coal tar air distillation is cut the cut before 280 ℃, obtain the straight run viscid bitumen of 35 ℃ of softening temperatures.The mixed solvent of straight run viscid bitumen and washing oil and kerosene is pressed 1: 0.8 mixed of mass ratio; The mass ratio of washing oil and kerosene is 1: 0.8 in the mixed solvent; After 130 ℃ of speed with 200 rev/mins stir 60 minutes, static 2 hours, tell extraction phase; Steaming solvent, to obtain the quinoline insolubles mass content be 0.03% refining viscid bitumen, and its quality percentage yield is 62.8%.Coal tar refining viscid bitumen that obtains and silicone oil are pressed in mass ratio adding in 1: 0.2 reaction kettle, under nitrogen protection, be warmed up to 420 ℃ with 2 ℃/minute speed, polyreaction obtained mesophase pitch in 8 hours under 300 rev/mins stir speed (S.S.).After the mesophase pitch cooling, extremely colourless with 1: 1 pyridine of volume ratio and quinoline extracting, its consumption is 40 times of the mesophase pitch quality that is extracted, and solid insoluble is at 80 ℃, 0.1 * 10
3Dry back acquisition particle size range is the MCMB of 1-90 μ m under the vacuum tightness of Pa, and its quality percentage yield is 42.7%.
Embodiment 10
The coal tar air distillation is cut the cut before 280 ℃, obtain the straight run viscid bitumen of 35 ℃ of softening temperatures.The mixed solvent of straight run viscid bitumen and washing oil and kerosene is pressed 1: 0.8 mixed of mass ratio; The mass ratio of washing oil and kerosene is 1: 0.8 in the mixed solvent; After 130 ℃ of speed with 200 rev/mins stir 60 minutes, static 2 hours, tell extraction phase; Steaming solvent, to obtain the quinoline insolubles mass content be 0.04% refining viscid bitumen, and its quality percentage yield is 62.8%.Coal tar refining viscid bitumen that obtains and silicone oil are pressed in mass ratio adding in 1: 0.4 reaction kettle, under nitrogen protection, be warmed up to 420 ℃ with 2 ℃/minute speed, polyreaction obtained mesophase pitch in 8 hours under 300 rev/mins stir speed (S.S.).After the mesophase pitch cooling, extremely colourless with 1: 1 pyridine of volume ratio and quinoline extracting, its consumption is 20 times of the mesophase pitch quality that is extracted, and solid insoluble is at 80 ℃, 0.1 * 10
3Dry back acquisition particle size range is the MCMB of 1-40 μ m under the vacuum tightness of Pa, and its quality percentage yield is 46.7%.
Claims (6)
1. the preparation method of a coal-tar base MCMB is characterized in that the technical process of this method comprises that the pre-treatment of raw material, thermal polycondensation react, separate and drying, and its operation division is following:
A. the pre-treatment of raw material
With coal tar is raw material; At first air distillation cuts the cut before 280 ℃; Obtain the straight run viscid bitumen of 30-40 ℃ of softening temperature, with solvent oil that is rich in aromatic hydrocarbons and the mixed extractant solvent straight run viscid bitumen that is rich in the solvent oil of alkane, the mass ratio of straight run viscid bitumen and mixed solvent is 1: 0.6-1.0; Quiescent settling, separation, distillation remove solvent then, obtain the coal tar refining viscid bitumen;
B. thermal polycondensation reaction
The coal tar refining viscid bitumen of above-mentioned acquisition is carried out the thermal polycondensation reaction, obtain to contain the mesophase pitch of carbon microspheres, the parameter of its thermal polycondensation reaction is following:
Heat-up rate: 1-5 ℃/minute;
Temperature of reaction: 350-450 ℃;
Reaction times: 1-8 hour;
Stirring velocity: 100-500 rev/min;
Reaction atmosphere: the protective atmosphere that nitrogen or id reaction produce;
C. separate
After heat polymerization finishes, naturally cooling, mesophase pitch is extracted to colourless in cable-styled extractor with organic solvent, and acquisition solid insoluble, solvent load are 20～50 times of the mesophase pitch quality that is extracted;
D. dry
The solid insoluble of above-mentioned gained is the coal-tar base MCMB after drying, its drying parameter is:
Drying temperature: 60-150 ℃;
Vacuum tightness: 0.1-1 * 10
3Pa.
2. the preparation method of coal-tar base MCMB according to claim 1 is characterized in that the solvent oil that is rich in aromatic hydrocarbons among the operation a comprises any one in crude benzol, heavy benzol, xylol, washing oil, heavy aromatics oil, the carbolineum; The solvent oil that is rich in alkane comprises the arbitrary combination of any one or they in sherwood oil, gasoline, aviation kerosene, solar oil, the Yellow Protopet 2A, and the solvent oil that is rich in aromatic hydrocarbons in the mixed solvent is 1 with the mass ratio that is rich in the solvent oil of alkane: 0.6-1.0.
3. the preparation method of coal-tar base MCMB according to claim 1; It is characterized in that the extraction temperature among the operation a is 100-150 ℃; The extraction time is 30-60 minute, and the extraction stirring velocity is 100-500 rev/min, and the quiescent settling time is 1-6 hour.
4. the preparation method of coal-tar base MCMB according to claim 1; Quinoline non-soluble amount percentage composition＜0.1% that it is characterized in that the coal tar refining viscid bitumen that mixed extractant solvent obtains among the operation a; Softening temperature is 30-40 ℃, and quality percentage yield is 50-75%.
5. the preparation method of coal-tar base MCMB according to claim 1 is characterized in that among the operation b adding the viscosity modifier carbolineum or the silicone oil of reaction system, its add-on be coal tar refining viscid bitumen quality 0.1-0.4 doubly.
6. the preparation method of coal-tar base MCMB according to claim 1; It is characterized in that the organic solvent among the operation c comprises benzene, toluene, pyridine, quinoline, THF, N; In dinethylformamide, DMAC N,N, acetone, the N-Methyl pyrrolidone any one or their arbitrary combination.
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