CN106495125A - A kind of preparation method and application of petroleum coke base mesoporous carbon - Google Patents
A kind of preparation method and application of petroleum coke base mesoporous carbon Download PDFInfo
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- CN106495125A CN106495125A CN201610860042.1A CN201610860042A CN106495125A CN 106495125 A CN106495125 A CN 106495125A CN 201610860042 A CN201610860042 A CN 201610860042A CN 106495125 A CN106495125 A CN 106495125A
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Abstract
The present invention relates to nano-carbon material technical field, and in particular to a kind of preparation method and application of petroleum coke base mesoporous carbon.The method comprising the steps of：1) by crushing after petroleum coke particles process through the concentrated sulfuric acid and concentrated nitric acid oxidation, prepare amphiphilic carbonaceous material；2) template triblock copolymer is dissolved in alkaline solution, after stirring, obtains settled solution；3) by step 1) the amphiphilic carbonaceous material of gained is added to step 2) in resulting solution, sealing stirring in a water bath adds acid solution, continues sealing stirring, is finally evaporated in a water bath, and aging in an oven；4) by step 3) carbonization under an inert atmosphere of gained solid, ground, pickling, washing, drying.The present invention has synthesized with large specific surface area and pore volume, the adjustable mesoporous carbon in aperture, it is achieved that the high value added utilization of petroleum coke, can be used as electrode material of the adsorbent of macromolecule contaminant, the carrier of catalyst and ultracapacitor etc..
Description
Technical field
The present invention relates to nano-carbon material technical field, and in particular to a kind of preparation method of petroleum coke base mesoporous carbon and should
With.
Background technology
Crude oil obtains light oil and mink cell focus through still-process, and obtained mink cell focus was waited through delayed coking again
Journey, obtains petroleum coke product.From the appearance, petroleum coke is black blocks of solid not of uniform size, in irregular shape, with gold
Category gloss, and particle has certain pore structure, and its component more than 95% is carbon, remaining also containing a small amount of hydrogen,
Oxygen, nitrogen, sulphur and metallic element etc..Typically 25～30%, Delayed Coking Technology enters the coke yield of delayed coking at present
One step develops, it is necessary to solve a difficult problem for petroleum coke effectively utilizes, to improve the added value of petroleum coke.Prepared with petroleum coke as raw material
Porous carbon is one of approach that the petroleum coke increment of rising in recent years is utilized.The petroleum coke resource of China's oil plant is very rich
Richness, price also than less expensive, easily form scale, with good market competition advantage.Therefore, prepared with petroleum coke as raw material
Porous carbon has been subjected to people and has more and more paid attention to.Porous carbon is produced as raw material with petroleum coke, significantly not only can be carried
The added value of high petroleum coke, it is also possible to widen the raw material for preparing porous carbon, for porous carbon industrial expansion and technological progress, tool
There is great economic and social benefit, kill two birds with one stone.
As petroleum coke contains a large amount of condensed-nuclei aromatics, compact structure, typically the method using activation of potassium hydroxide is preparing
Porous carbon, porous carbon materials prepared by the method are microporous carbon, and aperture is less, and activator potassium hydroxide consumption is big, to equipment
Seriously corroded, products obtained therefrom are expensive.
Mesoporous carbon is due to, the features such as with big aperture, pore volume, widely being paid close attention to.In dirty water purification, macromolecular
The absorption of organic matter and energy storage have the application of uniqueness with aspects such as conversions.Generally acknowledge that the method for preparing mesoporous carbon is mould at present
Plate method, the method can be with the pore passage structure of precise control porous carbon and sizes.Hard template method is a kind of common method, its template
Predominantly mesopore silicon oxide etc., the method can be with the aperture of accuracy controlling mesoporous carbon, but its preparation process is loaded down with trivial details, is especially removing
The link of template is gone, is needed to use a large amount of highly basic or HF is removed silica template.Compared to hard template method, soft template method
Removing template process is eliminated, template Direct Resolution is removed in carbonisation.Soft template method prepares mesoporous carbon and leads at present
It is carbon source frequently with phenolic resin, its preparation process condition harshness, and expensive.
Content of the invention
For solving the above-mentioned problems in the prior art, the present invention provides a kind of preparation method of petroleum coke base mesoporous carbon
And application.
The present invention is adopted the following technical scheme that：
A kind of preparation method of petroleum coke base mesoporous carbon, comprises the following steps：
1) by crushing after petroleum coke particles process through the concentrated sulfuric acid and concentrated nitric acid oxidation, prepare amphiphilic carbonaceous material
Material；
2) template triblock copolymer is dissolved in alkaline solution, after stirring, obtains settled solution；
3) by step 1) the amphiphilic carbonaceous material of gained is added to step 2) in resulting solution, sealing stirring in a water bath,
Acid solution is added, is continued sealing stirring, is finally evaporated in a water bath, and aging in an oven；
4) by step 3) carbonization under an inert atmosphere of gained solid, ground, pickling, washing, to obtain black after drying solid
Body, i.e. petroleum coke base mesoporous carbon.
Step 1) in crush after petroleum coke particles be 75～100 mesh, the volume of the oxidant concentrated sulfuric acid used and red fuming nitric acid (RFNA)
Than for 1:1～3:1, oxidation temperature is 70～120 DEG C, and the time is 2～5h.
Step 2) in triblock copolymer be one or more mixture in P123, F127, F108, itself and parents
Property carbonaceous material mass ratio be 6:1～1:1.
Step 2) neutral and alkali solution is sodium hydroxide solution, potassium hydroxide solution or ammonia spirit, and control its pH value and exist
Between 12～14, addition is 20～100mL.
Step 3) acid solution is watery hydrochloric acid or dilute sulfuric acid, and its concentration is controlled between 0.01～1mol/L, plus
Enter the pH value of rear solution between 1～4.
Step 3) in bath temperature control between 40～80 DEG C, sealing mixing time is 0.5～3h, continues sealing and stirs
Time is 1～5h, and aging temperature is 100～150 DEG C, and the time is 24～48h.
Step 4) in inert gas be nitrogen or argon gas, carburizing temperature between 600～1000 DEG C, carbonization time 1～
Between 3h.
Carbonization is controlled using temperature-gradient method, is warmed up to 300～400 DEG C with 1 DEG C/min first, is stablized 0.5～2h, Ran Houzai
600～900 DEG C are warmed up to 1～5 DEG C/min, stablize 1～3h.
Step 4) in after grinding, washed using the watery hydrochloric acid of 0.5～2mol/L, then adopt to be washed with deionized and be in
Neutrality, last 55～80 DEG C of vacuum drying.
Obtained in a kind of employing methods described, petroleum coke base mesoporous carbon is in the adsorbent as macromolecule contaminant, catalyst
Carrier and ultracapacitor electrode material on application.
Specific surface area, aperture and pore volume data in the present invention is determined using low temperature nitrogen physisorphtion
(MicromereticsTristar3020) phase structure of mesoporous carbon, is determined with X-ray diffractometer, uses transmission electron microscopy
Mirror is characterizing the pattern and pass of mesoporous carbon.
Compared with prior art, the present invention has excellent technique effect as follows：
Using cheap Petrochemical Enterprises byproduct petroleum coke as carbon source, with triblock copolymer as soft template, synthesis
There is large specific surface area and pore volume, the adjustable mesoporous carbon in aperture, it is achieved that the high value added utilization of petroleum coke, the mesoporous carbon can
It is used as electrode material of adsorbent, the carrier of catalyst and ultracapacitor of macromolecule contaminant etc..
Description of the drawings
Nitrogen Adsorption and desorption isotherms and graph of pore diameter distribution of the Fig. 1 for petroleum coke base mesoporous carbon (embodiment one)；
XRD diffraction patterns of the Fig. 2 for petroleum coke base mesoporous carbon (embodiment three)；
Fig. 3 is schemed for the TEM of petroleum coke base mesoporous carbon (embodiment one)；
Electrochemical properties of the Fig. 4 for petroleum coke base mesoporous carbon (embodiment one).
Specific embodiment
The invention will be further described with reference to the accompanying drawings and examples.
Embodiment one
1) petroleum coke of 80～100 mesh of 5g is added in 500mL there-necked flasks, adds 30mL red fuming nitric acid (RFNA)s and 70mL dense
Sulfuric acid, 80 DEG C of oxidation 3h, finally gives amphiphilic carbonaceous material.
2) 2.4g F127 are dissolved in the sodium hydroxide solution that 20mL pH are 12, after stirring, obtain settled solution.
3) to step 2) the amphiphilic carbonaceous material of 0.6g, sealing stirring under 75 DEG C of water-bath is added in gained mixture
1h, is then slowly added dropwise the hydrochloric acid solution of 5mL 1mol/L, continues sealing stirring 2h, is finally evaporated in 75 DEG C of water-baths, and
Aging 24h in 100 DEG C of baking ovens.
4) by step 3) gained solid is put in tube furnace, is warmed up to 350 DEG C with 1 DEG C/min in a nitrogen atmosphere, stable
0.5h, is then warmed up to 800 DEG C with 3 DEG C/min again, stable 2h；After grinding, washed using the watery hydrochloric acid of 1mol/L, then
Adopt and be washed with deionized in neutrality, last 60 DEG C of vacuum drying gained black solid, as petroleum coke base mesoporous carbon.
Embodiment two
1) petroleum coke of 80～100 mesh of 5g is added in 500mL there-necked flasks, adds 30mL red fuming nitric acid (RFNA)s and 70mL dense
Sulfuric acid, 80 DEG C of oxidation 3h, finally gives amphiphilic carbonaceous material.
2) 1.2g F127 are dissolved in the sodium hydroxide solution that 20mL pH are 12, after stirring, obtain settled solution.
3) to step 2) the amphiphilic carbonaceous material of 0.6g, sealing stirring under 75 DEG C of water-bath is added in gained mixture
1h, is then slowly added dropwise the hydrochloric acid solution of 2mL 1mol/L, continues sealing stirring 2h, is finally evaporated in 75 DEG C of water-baths, and
Aging 24h in 120 DEG C of baking ovens.
4) by step 3) gained solid is put in tube furnace, is warmed up to 350 DEG C with 1 DEG C/min in a nitrogen atmosphere, stable
0.5h, is then warmed up to 750 DEG C with 3 DEG C/min again, stable 2h；After grinding, washed using the watery hydrochloric acid of 1.5mol/L, so
After adopt and be washed with deionized in neutrality, last 70 DEG C of vacuum drying gained black solid obtains final product petroleum coke base mesoporous carbon.
Embodiment three
1) petroleum coke of 80～100 mesh of 5g is added in 500mL there-necked flasks, adds 30mL red fuming nitric acid (RFNA)s and 70mL dense
Sulfuric acid, 80 DEG C of oxidation 3h, finally gives amphiphilic carbonaceous material.
2) 2.4g F127 are dissolved in the sodium hydroxide solution that 20mL pH are 12, after stirring, obtain settled solution.
3) to step 2) the amphiphilic carbonaceous material of 0.6g, sealing stirring under 40 DEG C of water-bath is added in gained mixture
1h, is then slowly added dropwise the hydrochloric acid solution of 5mL 1mol/L, continues sealing stirring 2h, is finally evaporated in 40 DEG C of water-baths, and
Aging 48h in 100 DEG C of baking ovens.
4) by step 3) gained solid is put in tube furnace, is warmed up to 350 DEG C with 1 DEG C/min in a nitrogen atmosphere, stable
0.5h, is then warmed up to 900 DEG C with 3 DEG C/min again, stable 1.5h；After grinding, washed using the watery hydrochloric acid of 1mol/L, so
After adopt and be washed with deionized in neutrality, last 65 DEG C of vacuum drying gained black solid, as petroleum coke base mesoporous carbon.
Example IV
1) petroleum coke of 80～100 mesh of 5g is added in 500mL there-necked flasks, adds 30mL red fuming nitric acid (RFNA)s and 70mL dense
Sulfuric acid, 80 DEG C of oxidation 3h, finally gives amphiphilic carbonaceous material.
2) 0.8g P123 are dissolved in the sodium hydroxide solution that 20mL pH are 12, after stirring, obtain settled solution.
3) to step 2) the amphiphilic carbonaceous material of 0.4g, sealing stirring under 80 DEG C of water-bath is added in gained mixture
1h, is then slowly added dropwise the hydrochloric acid solution of 5mL 1mol/L, continues sealing stirring 2h, is finally evaporated in 80 DEG C of water-baths, and
Aging 24h in 100 DEG C of baking ovens.
4) by step 3) gained solid is put in tube furnace, is warmed up to 350 DEG C with 1 DEG C/min in a nitrogen atmosphere, stable
1h, is then warmed up to 800 DEG C with 3 DEG C/min again, stable 1h；After grinding, washed using the watery hydrochloric acid of 2mol/L, then adopted
It is washed with deionized in neutrality, last 60 DEG C of vacuum drying gained black solid, as petroleum coke base mesoporous carbon.
The analyze data of 1 embodiment gained petroleum coke base mesoporous carbon of table
aBET specific surface area, according to N2Adsorption isotherm line computation gained；bMicropore specific area, calculates according to t-plot methods
Gained；cMesopore surface area, according to formula Smeso=SBET-SmicCalculate gained；dTotal pore volume, in relative pressure (P/Po) be
Gained is calculated when 0.99；eMicropore volume, calculates gained according to t-plot methods；fMesoporous pore volume, calculates gained according to BJH methods
；gAverage pore size, according to formula 4Vtotal/SBETCalculate gained.
Above table data can be seen that the average pore size of gained petroleum coke base mesoporous carbon in more than 3nm, and specific surface area exists
400m2/ more than g, and mesoporous are up to more than 75%, with larger total pore volume and mesoporous pore volume.It can be seen that, the method can have
Effect adjusts multiple pore structure parameters of mesoporous carbon.
The above description of this invention is illustrative and not restrictive, and those skilled in the art understands, will in right
Ask and many modifications, change or equivalent can be carried out to which within the spirit and scope of restriction, but they fall within the present invention's
In protection domain.
Claims (10)
1. a kind of preparation method of petroleum coke base mesoporous carbon, it is characterised in that comprise the following steps：
1) by crushing after petroleum coke particles process through the concentrated sulfuric acid and concentrated nitric acid oxidation, prepare amphiphilic carbonaceous material；
2) template triblock copolymer is dissolved in alkaline solution, after stirring, obtains settled solution；
3) by step 1) the amphiphilic carbonaceous material of gained is added to step 2) in resulting solution, sealing stirring in a water bath is added
Acid solution, continues sealing stirring, is finally evaporated in a water bath, and aging in an oven；
4) by step 3) carbonization under an inert atmosphere of gained solid, ground, pickling, washing, obtain black solid after drying, i.e.,
Petroleum coke base mesoporous carbon.
2. the preparation method of petroleum coke base mesoporous carbon according to claim 1, it is characterised in that step 1) in crush after
Petroleum coke particles are 75～100 mesh, and the oxidant concentrated sulfuric acid used is 1 with the volume ratio of red fuming nitric acid (RFNA):1～3:1, oxidation temperature
For 70～120 DEG C, the time is 2～5h.
3. the preparation method of petroleum coke base mesoporous carbon according to claim 1, it is characterised in that step 2) in three block altogether
Polymers is one or more the mixture in P123, F127, F108, and which is 6 with the mass ratio of amphiphilic carbonaceous material:1
～1:1.
4. the preparation method of petroleum coke base mesoporous carbon according to claim 1, it is characterised in that step 2) neutral and alkali solution
For sodium hydroxide solution, potassium hydroxide solution or ammonia spirit, and controlling its pH value between 12～14, addition is 20～
100mL.
5. the preparation method of petroleum coke base mesoporous carbon according to claim 1, it is characterised in that step 3) acidity is molten
Liquid is watery hydrochloric acid or dilute sulfuric acid, and controls its concentration between 0.01～1mol/L, and after addition, the pH value of solution is between 1～4.
6. the preparation method of petroleum coke base mesoporous carbon according to claim 1, it is characterised in that step 3) in bath temperature
Between 40～80 DEG C, sealing mixing time is 0.5～3h for control, and it is 1～5h to continue sealing mixing time, and aging temperature is
100～150 DEG C, the time is 24～48h.
7. the preparation method of petroleum coke base mesoporous carbon according to claim 1, it is characterised in that step 4) in inert gas
For nitrogen or argon gas, between 600～1000 DEG C, carbonization time is between 1～3h for carburizing temperature.
8. the preparation method of petroleum coke base mesoporous carbon according to claim 7, it is characterised in that carbonization adopts temperature-gradient method
Control, is warmed up to 300～400 DEG C with 1 DEG C/min first, stablizes 0.5～2h, then 600 are warmed up to 1～5 DEG C/min again～
900 DEG C, stablize 1～3h.
9. the preparation method of petroleum coke base mesoporous carbon according to claim 1, it is characterised in that step 4) in through grinding
Afterwards, washed using the watery hydrochloric acid of 0.5～2mol/L, then adopt and be washed with deionized in neutrality, last 55～80 DEG C of vacuum are done
Dry.
10. one kind adopts petroleum coke base mesoporous carbon obtained in claim 1-9 any one methods described dirty as macromolecular
Application on the adsorbent of dye thing, the carrier of catalyst and the electrode material of ultracapacitor.
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| CN106958053A (en) * | 2017-04-24 | 2017-07-18 | 中国石油大学(华东) | A kind of preparation method of porous petroleum coke base carbon fibre |
| CN107161982A (en) * | 2017-05-19 | 2017-09-15 | 中国石油大学(华东) | Petroleum coke base graphene and its preparation method and application |
| CN107739774A (en) * | 2017-06-17 | 2018-02-27 | 常州兆威不锈钢有限公司 | A kind of preparation method for making steel special carburant |
| CN108408723A (en) * | 2018-01-18 | 2018-08-17 | 新疆大学 | Coal base stratification carbon nano-material based on soft template method and preparation method thereof |
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| CN108428560A (en) * | 2018-01-18 | 2018-08-21 | 新疆大学 | High-specific surface area coal base nitrogen-dopped activated carbon ball electrode material and preparation method thereof |
| CN108428560B (en) * | 2018-01-18 | 2020-08-04 | 新疆大学 | High-specific-surface-area coal-based nitrogen-doped active carbon sphere electrode material and preparation method thereof |
| CN108408723B (en) * | 2018-01-18 | 2021-08-13 | 新疆大学 | Coal-based hierarchical nano carbon material based on soft template method and preparation method thereof |
| CN111573667A (en) * | 2020-06-28 | 2020-08-25 | 中国石油化工股份有限公司 | Energy storage carbon material, supercapacitor and preparation method thereof |
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