CN102491320A - Pitch-based active carbon with superhigh specific surface area and preparation method thereof - Google Patents
Pitch-based active carbon with superhigh specific surface area and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a pitch-based active carbon with superhigh specific surface area and a preparation method thereof. The pitch-based active carbon with superhigh specific surface area is prepared by using pitch and rosin as raw materials, and carrying out concocting, pyrolysis, pre-oxidation and activation. Compared with routine methods for preparing active carbon with superhigh specific surface area, the method has the advantages of low preparation cost, low device investment, simple operation, no pollution, and easy realization of industrialization, and the prepared pitch-based active carbon has the advantages of large specific surface area, good performance, and good physical and chemical stability, and has outstanding economic and social benefits.
Description
Technical field
The invention belongs to raw material of wood-charcoal material field, be specifically related to a kind of superhigh specific surface area asphalt based active carbon and preparation method thereof.
Background technology
Gac is a kind of porousness blacking that pore texture is flourishing, specific surface area is big that is made up of crystallite charcoal and unformed charcoal.Gac has good absorption property and good excellent properties such as chemicalstability, physical stability and good regenerative power, and it has been widely used in fields such as electronics, chemical industry, food-processing, health care, transportation and energy, agricultural, national defence as sorbent material, support of the catalyst etc.Yet along with the continuous development in fields such as medicine, environmental protection, military affairs, common gac (specific surface area 800～1500m
2/ g) because the selection adsorptivity is relatively poor, specific surface area is low, loading capacity is limited, can not satisfy the particular requirement in these fields, this feasible demand to active carbon with high specific surface area constantly rises.(specific surface area is generally greater than 2500m for activated carbon with high specific surface area
2/ g) have advantages such as specific surface area height, microvoid content is high, pore size distribution is narrow, adsorptive capacity is big, can be used for double layer capacitor, natural gas storage, reclaim fields such as enriching noble metals, methane sorbent material, effective catalyst and support of the catalyst.
The preparation method of activated carbon with high specific surface area has physical activation method, chemical activation method and the chemical combined activation method of Wu Li –.It is raw material that the preparation activated carbon with high specific surface area often adopts refinery coke, coal-tar pitch, mesophase pitch and MCMB; The above two are because the restriction of raw material mix and aspect of performance; Be difficult to prepare activated carbon with high specific surface area; Then both preparation costs are too high, neither prepare the suitable feedstock of activated carbon with high specific surface area, and this has directly influenced the popularization and the application of activated carbon with high specific surface area.
Summary of the invention
The objective of the invention is to a kind of superhigh specific surface area asphalt based active carbon and preparation method thereof, prepare activated carbon with high specific surface area relatively with routine, the present invention has low, the less equipment investment of preparation cost, and is simple to operate, pollution-free, is prone to realize industrialization; The advantage that the product specific surface area is big, functional, physical and chemical stability is good possesses remarkable economical and social benefit.
For realizing above-mentioned purpose, the present invention adopts following technical scheme:
A kind of preparation method of superhigh specific surface area asphalt based active carbon comprises modulation, pyrolytic reaction, preoxidation and the activating process of raw material.Its concrete steps are following:
(1) modulation of raw material:
Basic raw material: one or more mixtures of coal-tar pitch, petroleum pitch, slag oil asphalt, synthetic asphalts;
Additive: one or both of rosin, nilox resin;
Proportioning raw materials: the mass ratio of basic raw material and additive is 100:5-100:30;
Basic raw material and additive take by weighing by proportioning, grind behind 80 mesh sieves and directly mix, and put into polymeric kettle, are warming up to the technology that adopts hot melt to stir behind the preset temperature and mix, and processing parameter is:
Temperature rise rate: 50 ℃/min of 2 ℃/min –;
Preset temperature: 200 ℃ of 100 ℃ –;
Churning time: 0.1h – 1h;
Stirring velocity: 50 rpm –, 1000 rpm;
Protective atmosphere: N
2Perhaps Ar
2
Gas flow: 50 mL/min –, 200 mL/min;
(2) pyrolytic reaction:
The raw material that step (1) modulates is put into atmosphere furnace, be incubated after being warming up to preset temperature then, be cooled to room temperature and take out, processing parameter is:
Temperature rise rate: 100 ℃/min of 2 ℃/min –;
Preset temperature: 500 ℃ of 400 ℃ –;
Soaking time: 0.5h – 3h;
Protective atmosphere: N
2Perhaps Ar
2
Gas flow: 50 mL/min –, 200 mL/min;
(3) preoxidation
The resulting product of step (2) ground put into reaction kettle after sieving, be incubated behind warming while stirring to the preset temperature then, bubbling air in whipping process is cooled to room temperature and takes out simultaneously, and processing parameter is:
The resulting product mesh-of-grind of step (2): 60-300 order;
Temperature rise rate: 100 ℃/min of 2 ℃/min –;
Preset temperature: 350 ℃ of 240 ℃ –;
Soaking time: 0 – 10h;
Gas flow: 100mL/min – 250mL/min;
(4) activating process
The resulting product of step (3) and KOH mixed put into corundum crucible, be incubated after in High Temperature Furnaces Heating Apparatus, being warming up to preset temperature then, cool to room temperature with the furnace and take out, washing is drying to obtain described superhigh specific surface area asphalt based active carbon; Processing parameter is:
Proportioning raw materials: the mass ratio of resulting product of step (3) and KOH is 1:3-1:9;
Temperature rise rate: 10 ℃/min of 2 ℃/min –;
Preset temperature: 900 ℃ of 700 ℃ –;
Soaking time: 0.15h – 2 h;
Protective atmosphere: N
2Perhaps Ar
2
Gas flow: 50 mL/min –, 200 mL/min.
The present invention reaches the purpose of adjustment superhigh specific surface area asphalt based active carbon structure and performance through modulation, pyrolysis, preoxidation and the activating process of control basic raw material.The specific surface area that adopts the prepared gac of preparation method of the present invention is 2500 ~ 3500m
2/ g.
The present invention modulates modification through adding a certain amount of rosin to material asphalt, is used for preparing activated carbon with high specific surface area through alternative mesophase pitch of pyrolytic reaction products therefrom or MCMB.The activated carbon with high specific surface area of Using such method preparation has that cost is low, technology simple, excellent property, pollution-free, the advantage that is prone to industrialization.
Compared with prior art, advantage that the present invention had and effect are:
(1) abundant raw material, cheap.
(2) processing unit is simple, and is pollution-free, is easy to scale operation.
(3) specific surface area is high, and is of many uses.
Embodiment
Below be several specific embodiment of the present invention, further specify the present invention, but the present invention be not limited only to this.
Embodiment 1
Coal-tar pitch and nilox resin are ground to 80 orders, the polymeric kettle of packing into after mixing by mass ratio 100:10, the speed intensification with 3 ℃/min is warming up to 150 ℃, and begins to feed N from intensification
2, N
2Flow is 50mL/min, simultaneously rotating speed is transferred to 500rpm and stirs 0.1h, promptly obtains the pitch that modulates.The pitch that modulates is put into atmosphere furnace (N
2Flow is 50mL/min), be incubated 2h after being warming up to 450 ℃ with 5 ℃/min then, be cooled to room temperature and take out pyrolysis product.Put into reaction kettle after pyrolysis product is ground to 300 orders, under agitation and with the heat-up rate of 4 ℃/min rise to 300 ℃ of reaction 1 h then, with the 200mL/min bubbling air, reaction finishes postcooling to room temperature in the reaction process.Product after the oxidation mixed by mass ratio 1:5 with KOH put into reaction kettle, and feed N
2, N
2Flow is 50mL/min, keeps 1 h after being warming up to 850 ℃ with 5 ℃/min then, cools to room temperature with the furnace and takes out, and washing is to neutral, and drying promptly obtains gac.Prepared gac has following performance: specific surface area 3320m
2/ g, total hole volume 1.97cm
3/ g, benzene adsorptive value 1560mg/g.
Embodiment 2
Petroleum pitch and rosin are taken by weighing by 100:5 (mass ratio), be ground to the polymeric kettle of packing into behind 80 orders, heat up, be warming up to 120 ℃, and begin to feed N from intensification with the speed of 10 ℃/min
2, N
2Flow is 100mL/min, simultaneously rotating speed is transferred to 200rpm and stirs 0.5h, promptly obtains the pitch that modulates.The pitch that modulates is put into atmosphere furnace (N
2Flow is 100 mL/min), be incubated 2.5h after being warming up to 400 ℃ with 5 ℃/min then, be cooled to room temperature and take out pyrolysis product.Put into reaction kettle after pyrolysis product is ground to 60 orders, under agitation and with the heat-up rate of 25 ℃/min rise to 260 ℃ of reaction 3 h then, with 160 mL/min bubbling airs, reaction finishes postcooling to room temperature in the reaction process.Product after the oxidation mixed by mass ratio 1:7 with KOH put into reaction kettle, and feed N
2, N
2Flow is 50mL/min, keeps 2 h after being warming up to 900 ℃ with 10 ℃/min then, cools to room temperature with the furnace and takes out, and washing is to neutral, and drying promptly obtains gac.Prepared gac has following performance: specific surface area 2800m
2/ g, total hole volume 1.79cm
3/ g, benzene adsorptive value 1437mg/g.
Embodiment 3
Matchmaker's pitch and rosin are taken by weighing by 100:15 (mass ratio), be ground to the polymeric kettle of packing into behind 80 orders, heat up, be warming up to 180 ℃, and begin to feed N from intensification with the speed of 5 ℃/min
2, N
2Flow is 100mL/min, simultaneously rotating speed is transferred to 800rpm and stirs 0.4h, promptly obtains the pitch that modulates.The pitch that modulates is put into atmosphere furnace (N
2Flow is 100 mL/min), be incubated 2.5h after being warming up to 480 ℃ with 10 ℃/min then, be cooled to room temperature and take out pyrolysis product.Put into reaction kettle after pyrolysis product is ground to 200 orders, under agitation rise to 240 ℃ of reaction 10 h with the heat-up rate of 10 ℃/min then, with 150 mL/min bubbling airs, reaction finishes postcooling to room temperature in the reaction process.Product after the oxidation mixed by mass ratio 1:9 with KOH put into reaction kettle, and feed N
2, N
2Flow is 50mL/min, keeps 5h after being warming up to 700 ℃ with 5 ℃/min then, cools to room temperature with the furnace and takes out, and washing is to neutral, and drying promptly obtains gac.Prepared gac has following performance: specific surface area 3000m
2/ g, total hole volume 1.76cm
3/ g, benzene adsorptive value 1457mg/g.
Embodiment 4
Synthetic asphalts and rosin are taken by weighing by 100:20 (mass ratio), be ground to the polymeric kettle of packing into behind 80 orders, heat up, be warming up to 200 ℃, and begin to feed N from intensification with the speed of 25 ℃/min
2, N
2Flow is 140mL/min, simultaneously rotating speed is transferred to 500rpm and stirs 1h, promptly obtains the pitch that modulates.The pitch that modulates is put into atmosphere furnace (N
2Flow is 150 mL/min), be incubated 2h after being warming up to 500 ℃ with 5 ℃/min then, be cooled to room temperature and take out pyrolysis product.Put into reaction kettle after pyrolysis product is ground to 100 orders, under agitation rise to 280 ℃ of reaction 3 h with the heat-up rate of 25 ℃/min then, with 250 mL/min bubbling airs, reaction finishes postcooling to room temperature in the reaction process.Product after the oxidation mixed by mass ratio 1:3 with KOH put into reaction kettle, and feed N
2, N
2Flow is 50mL/min, keeps 2 h after being warming up to 800 ℃ with 8 ℃/min then, cools to room temperature with the furnace and takes out, and washing is to neutral, and drying promptly obtains gac.Prepared gac has following performance: specific surface area 2580m
2/ g, total hole volume 1.32m
3/ g, benzene adsorptive value 1243mg/g.
Embodiment 5
Petroleum pitch is mixed by mass ratio 1:3 with coal-tar pitch.Mix asphalt and nilox resin are taken by weighing by 100:20 (mass ratio), be ground to the polymeric kettle of packing into behind 80 orders, heat up, be warming up to 150 ℃, and begin to feed N from intensification with the speed of 3 ℃/min
2, N
2Flow is 50mL/min, simultaneously rotating speed is transferred to 200rpm and stirs 1h, promptly obtains the pitch that modulates.The pitch that modulates is put into atmosphere furnace (N
2Flow is 50 mL/min), be incubated 2h after being warming up to 500 ℃ with 5 ℃/min then, be cooled to room temperature and take out pyrolysis product.Put into reaction kettle after pyrolysis product is ground to 200 orders, under agitation rise to 300 ℃ of reaction 2 h with the heat-up rate of 100 ℃/min then, with the 100mL/min bubbling air, reaction finishes postcooling to room temperature in the reaction process.Product after the oxidation mixed by mass ratio 1:5 with KOH put into reaction kettle, and feed N
2, N
2Flow is 50mL/min, keeps 1.5h after being warming up to 850 ℃ with 5 ℃/min then, cools to room temperature with the furnace and takes out, and washing is to neutral, and drying promptly obtains gac.Prepared gac has following performance: specific surface area 2930m
2/ g, total hole volume 1.82m
3/ g, benzene adsorptive value 1457mg/g.
Embodiment 6
Synthetic asphalts is mixed by mass ratio 1:1 with coal-tar pitch.Mix asphalt and rosin are taken by weighing by 100:30 (weight ratio), be ground to the polymeric kettle of packing into behind 80 orders, heat up, be warming up to 160 ℃, and begin to feed N from intensification with the speed of 2 ℃/min
2, N
2Flow is 200mL/min, simultaneously rotating speed is transferred to 300rpm and stirs 0.5h, promptly obtains the pitch that modulates.The pitch that modulates is put into atmosphere furnace (N
2Flow is 50 mL/min), be incubated 2h after being warming up to 500 ℃ with 15 ℃/min then, be cooled to room temperature and take out pyrolysis product.Put into reaction kettle after pyrolysis product is ground to 100 orders, under agitation rise to 320 ℃ of reaction 2h with the heat-up rate of 20 ℃/min then, with the 200mL/min bubbling air, reaction finishes postcooling to room temperature in the reaction process.Product after the oxidation mixed by mass ratio 1:4 with KOH put into reaction kettle, and feed N
2, N
2Flow is 50mL/min, keeps 0.5h after being warming up to 900 ℃ with 10 ℃/min then, cools to room temperature with the furnace and takes out, and washing is to neutral, and drying promptly obtains gac.Prepared gac has following performance: specific surface area 2740m
2/ g, total hole volume 1.52m
3/ g, benzene adsorptive value 1321mg/g.
The above is merely preferred embodiment of the present invention, and all equalizations of doing according to claim of the present invention change and modify, and all should belong to covering scope of the present invention.
Claims (3)
1. superhigh specific surface area asphalt based active carbon, it is characterized in that: the specific surface area of described asphalt based active carbon is 2500-3500m
2/ g.
2. the preparation method of a superhigh specific surface area asphalt based active carbon as claimed in claim 1, it is characterized in that: described preparation method comprises modulation, pyrolytic reaction, preoxidation and the activating process of raw material.
3. the preparation method of superhigh specific surface area asphalt based active carbon according to claim 2 is characterized in that: described preparing method's concrete steps are following:
(1) modulation of raw material:
Basic raw material: one or more mixtures of coal-tar pitch, petroleum pitch, slag oil asphalt, synthetic asphalts;
Additive: one or both of rosin, nilox resin;
Proportioning raw materials: the mass ratio of basic raw material and additive is 100:5-100:30;
Basic raw material and additive take by weighing by proportioning, grind behind 80 mesh sieves and directly mix, and put into polymeric kettle, are warming up to the technology that adopts hot melt to stir behind the preset temperature and mix, and processing parameter is:
Temperature rise rate: 50 ℃/min of 2 ℃/min –;
Preset temperature: 200 ℃ of 100 ℃ –;
Churning time: 0.1h – 1h;
Stirring velocity: 50 rpm –, 1000 rpm;
Protective atmosphere: N
2Perhaps Ar
2
Gas flow: 50 mL/min –, 200 mL/min;
(2) pyrolytic reaction:
The raw material that step (1) modulates is put into atmosphere furnace, be incubated after being warming up to preset temperature then, be cooled to room temperature and take out, processing parameter is:
Temperature rise rate: 100 ℃/min of 2 ℃/min –;
Preset temperature: 500 ℃ of 400 ℃ –;
Soaking time: 0.5h – 3h;
Protective atmosphere: N
2Perhaps Ar
2
Gas flow: 50 mL/min –, 200 mL/min;
(3) preoxidation
The resulting product of step (2) ground put into reaction kettle after sieving, be incubated behind warming while stirring to the preset temperature then, bubbling air in whipping process is cooled to room temperature and takes out simultaneously, and processing parameter is:
The resulting product mesh-of-grind of step (2): 60-300 order;
Temperature rise rate: 100 ℃/min of 2 ℃/min –;
Preset temperature: 350 ℃ of 240 ℃ –;
Soaking time: 0 – 10h;
Gas flow: 100mL/min – 250mL/min;
(4) activating process
The resulting product of step (3) and KOH mixed put into corundum crucible, be incubated after in High Temperature Furnaces Heating Apparatus, being warming up to preset temperature then, cool to room temperature with the furnace and take out, washing is drying to obtain described superhigh specific surface area asphalt based active carbon; Processing parameter is:
Proportioning raw materials: the mass ratio of resulting product of step (3) and KOH is 1:3-1:9;
Temperature rise rate: 10 ℃/min of 2 ℃/min –;
Preset temperature: 900 ℃ of 700 ℃ –;
Soaking time: 0.15h – 2 h;
Protective atmosphere: N
2Perhaps Ar
2
Gas flow: 50 mL/min –, 200 mL/min.
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Cited By (11)
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|---|---|---|---|---|
| CN103521194A (en) * | 2013-08-30 | 2014-01-22 | 蚌埠德美过滤技术有限公司 | Surface polymer modified wood charcoal adsorbing agent and preparation method thereof |
| CN103613096A (en) * | 2013-12-06 | 2014-03-05 | 福州大学 | Low-cost method for preparing graphene macroform |
| CN103803550A (en) * | 2014-02-26 | 2014-05-21 | 上海宝聚新化能源科技有限公司 | Preparation method of asphalt-based active carbon |
| CN105148827A (en) * | 2015-10-13 | 2015-12-16 | 中国石油化工股份有限公司 | Method for preparing absorbing agent for chemical leakage accident by adopting waste catalytic cracking catalyst |
| CN106732416A (en) * | 2016-12-01 | 2017-05-31 | 桂林理工大学 | A kind of rosin modifies the preparation method and applications of stalk adsorbent |
| CN107601500A (en) * | 2017-11-02 | 2018-01-19 | 福州大学 | A kind of preparation method of high-specific surface area active foam Carbon Materials |
| CN108010750A (en) * | 2017-12-29 | 2018-05-08 | 福州大学 | A kind of preparation method of ultra-thin-wall multistage porous charcoal/carbon/polyaniline super capacitor electrode material |
| CN108940134A (en) * | 2018-06-20 | 2018-12-07 | 东南大学 | Coal pitch spheres aoxidize infusible continuous reaction apparatus and method |
| CN109399635A (en) * | 2018-09-29 | 2019-03-01 | 中国科学院山西煤炭化学研究所 | A kind of preparation method of the asphaltic base honeycomb hole nanometer layer of charcoal suitable for electrochemical applications |
| CN110465267A (en) * | 2019-07-08 | 2019-11-19 | 天津大学 | Oil sand asphalt texture preparation is rich in the methods and applications of nitrogen sulphur porous adsorbent material |
| CN111762779A (en) * | 2020-07-20 | 2020-10-13 | 广东东煌科技有限公司 | Coal-based activated carbon, columnar activated carbon and preparation method thereof |
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| CN1927709A (en) * | 2006-09-12 | 2007-03-14 | 山西大学 | Asphalt based active carbon and preparation method thereof |
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| CN101717085A (en) * | 2009-12-07 | 2010-06-02 | 北京化工大学 | Activated carbon microspheres and preparation method thereof |
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|---|---|---|---|---|
| CN103521194A (en) * | 2013-08-30 | 2014-01-22 | 蚌埠德美过滤技术有限公司 | Surface polymer modified wood charcoal adsorbing agent and preparation method thereof |
| CN103613096A (en) * | 2013-12-06 | 2014-03-05 | 福州大学 | Low-cost method for preparing graphene macroform |
| CN103803550A (en) * | 2014-02-26 | 2014-05-21 | 上海宝聚新化能源科技有限公司 | Preparation method of asphalt-based active carbon |
| CN103803550B (en) * | 2014-02-26 | 2016-05-18 | 北京宝塔三聚能源科技有限公司 | A kind of preparation method of asphalt based active carbon |
| CN105148827A (en) * | 2015-10-13 | 2015-12-16 | 中国石油化工股份有限公司 | Method for preparing absorbing agent for chemical leakage accident by adopting waste catalytic cracking catalyst |
| CN106732416A (en) * | 2016-12-01 | 2017-05-31 | 桂林理工大学 | A kind of rosin modifies the preparation method and applications of stalk adsorbent |
| CN107601500A (en) * | 2017-11-02 | 2018-01-19 | 福州大学 | A kind of preparation method of high-specific surface area active foam Carbon Materials |
| CN108010750A (en) * | 2017-12-29 | 2018-05-08 | 福州大学 | A kind of preparation method of ultra-thin-wall multistage porous charcoal/carbon/polyaniline super capacitor electrode material |
| CN108010750B (en) * | 2017-12-29 | 2019-08-09 | 福州大学 | A kind of preparation method of ultra-thin-wall multistage porous charcoal/carbon/polyaniline super capacitor electrode material |
| CN108940134A (en) * | 2018-06-20 | 2018-12-07 | 东南大学 | Coal pitch spheres aoxidize infusible continuous reaction apparatus and method |
| CN109399635A (en) * | 2018-09-29 | 2019-03-01 | 中国科学院山西煤炭化学研究所 | A kind of preparation method of the asphaltic base honeycomb hole nanometer layer of charcoal suitable for electrochemical applications |
| CN110465267A (en) * | 2019-07-08 | 2019-11-19 | 天津大学 | Oil sand asphalt texture preparation is rich in the methods and applications of nitrogen sulphur porous adsorbent material |
| CN111762779A (en) * | 2020-07-20 | 2020-10-13 | 广东东煌科技有限公司 | Coal-based activated carbon, columnar activated carbon and preparation method thereof |
| CN111762779B (en) * | 2020-07-20 | 2021-08-13 | 广东东煌科技有限公司 | Coal-based activated carbon, columnar activated carbon and preparation method thereof |
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