CN103787331A - Preparation method of pitch-based spherical activated carbon with rich meso pores - Google Patents
Preparation method of pitch-based spherical activated carbon with rich meso pores Download PDFInfo
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Abstract
A preparation method of pitch-based spherical activated carbon with rich meso pores is characterized by comprising the following steps of fetching mesophase pitch serving as the raw material, adding aromatic hydrocarbon matters and thermoset phenolic resin prepared by wood liquefied matters, mixing the mesophase pitch and the thermoset phenolic resin, preparing a pitch ball through a suspension method, and utilizing conventional processes such as preoxidation, carbonization and activation to obtain the pitch-based spherical activated carbon with high mesoporous rate. The degree of sphericity of the prepared pitch-based spherical activated carbon ranges from 0.94 to 0.97, the specific surface area is higher than 800m<2>/g, the pore volume is larger than 0.35cm<3>/g, and the average pore size ranges from 1.8nm to 2.2nm. The pitch-based spherical activated carbon prepared by the method has rich meso pores, diameters of the meso pores can be controlled by addition of the thermoset phenolic resin prepared by the wood liquefied matters, the mechanical strength of the pitch-based spherical activated carbon is high, and the application range of the pitch-based spherical activated carbon is enlarged. Therefore, the preparation method is ideal.
Description
Affiliated technical field:
The present invention relates to a kind of preparation method of asphalt-base spherical activated carbon of mesoporous prosperity, belong to ball shape active carbon preparing technical field, be specifically related to the preparation method of the controlled asphalt-base spherical activated carbon in a kind of aperture of preparing high mesoporous rate take mesophase pitch as raw material.
Background technology:
The raw materials of ball shape active carbon is mainly coal, macromolecule resin and pitch.Coal-based ball shape active carbon cost is lower, but exist ash oontent high, bad mechanical strength, and the shortcoming such as sphericity is low, and aperture is wayward, and absorption property is poor, has limited its further application; Macromolecule resin base globe activated char physical strength is high, and pore size distribution is more easy to control, and foreign matter content is lower, but manufacturing process complexity, raw materials cost is high, and specific surface area is little, wide spectrum absorption property is poor, thereby exists certain limitation while using as biomedical material instrument; And although asphalt-base spherical activated carbon preparation technology and equipment are more complicated, but its physical strength is high, foreign matter content is low, sphericity is high, smooth surface, wide spectrum absorption property is good, and material asphalt source is abundant, cheap, have broad application prospects in fields such as biomedical, military protection, catalyst support materials.
The ball shape active carbon manufacture method that English Patent GB1468982 and U.S. Pat 3917806 provide be by pitch and additive (naphthalene) in the autoclave with whipping appts, under certain temperature and pressure, it is mixed, then add the polyvinyl acetate suspension of half saponification to obtain mixture.Under certain pressure and stirring velocity, at 50~350 ℃, make this mixture be dispersed into small droplets and be suspended in water.Disperse finish after, by cooling mixture, separate after make bitumen ball.With solvent, additive is removed and is prepared into porous asphalt ball again.In oxidizing atmosphere, by porous asphalt ball oxide treatment at the temperature of 100~500 ℃, bitumen ball oxidation is not melted, to prevent that bitumen ball from melting also in carbonization process; Within the scope of 500~1000 ℃, by the charing under inert atmosphere protection of above-mentioned bitumen ball, and with steam activation, obtain asphalt-base spherical activated carbon.This method needs High Temperature High Pressure operation, is oxidized not melting process time consumption and energy consumption, and sphere diameter is unsuitable excessive, does not just melt and can not thoroughly carry out otherwise be oxidized, and this method can not be controlled the granularity of ball shape active carbon in addition, therefore cannot make the ball shape active carbon that narrow sphere diameter distributes.
U.S. Pat 4420443 discloses the production method of a kind of spherical carbon particle and ball shape active carbon, pitch is mixed in reactor with the mixture of viscosity depressant, be warming up to 150~300 ℃ of meltings, stir and be thoroughly mixed to form eutectic, then by increasing still internal pressure, molten state eutectic is extruded into slice from the porous sieve plate of still bottom, it is cooling that this slice enters into water immediately, forms the fibrous billet of length-to-diameter ratio in 1~5 scope simultaneously under the effect of high speed shear.By the bitumen particle of billet or certain particle size join with the immiscible medium of pitch in suspended dispersed, be warming up to certain temperature, billet or particulate melted by heating are shrunk to liquid spheroid, cooling, filter after can obtain fix-bitumen ball.Viscosity depressant is removed in the solvent extraction of fix-bitumen ball warp, then under airflow, does not melt reaction at lower than 400 ℃, flows down and carries out carbonization reaction and priming reaction, thereby obtain ball shape active carbon higher than nitrogen gas stream at 600 ℃ and water vapour.
U.S. Pat 4371454 discloses the preparation method of a kind of spherical carbon material and ball shape active carbon, pitch and viscosity depressant, diameter are less than the mixture of decolorizing carbon particle of 200 μ m through heating, extruding, shattering process, form rod shape fragment, all the other preparation technologies and patent US4420443 are similar, the ball shape active carbon apparent density obtaining is 0.5~0.750g/cc, iodine sorption value is 700~1200mg/g, the ball shape active carbon sphere diameter narrowly distributing obtaining, and granularity is controlled.But this method processing requirement is high, need High Temperature High Pressure operation, be oxidized not melting process time consumption and energy consumption.
Publication number be CN102795624A Introduction To Cn Patent a kind of low power consuming preparation method of asphalt-base spherical activated carbon, key step has: by benzoyl peroxide, divinylbenzene, vinylbenzene, diethylbenzene and softening temperature be 240~280 ℃ with particle diameter be the asphalt powder batch mixing of 150~200 mesh sieves, the balling-up that suspends in polyvinyl alcohol dispersion liquid, hydrothermal method are solidified spheroid and are become original charcoal ball, original charcoal ball segmentation (350 ℃, 400 ℃, 450 ℃) calcining and activation (700~800 ℃, 850~1000 ℃) and process and obtain asphalt-base spherical activated carbon.This method has been used a large amount of organic solvents, and sphere diameter skewness can not be controlled the granularity of ball shape active carbon.
The Chinese patent that publication number is CN1224034A provides a kind of method of preparing asphalt-base spherical activated carbon, the method is with 1:(0.001~0.1 by pitch, organometallic compound and aromatic solvent): the ratio of (0.1~0.5) high temperature (100~300 ℃) in autoclave mixes, first make the asphalt stock that is suitable for the metal-particle-containing of preparing bitumen ball, then through emulsion process balling-up, then through not melting, charing, activation treatment obtain the asphalt-base spherical activated carbon of mesopore prosperity.But this method is used the organometallic compound (as ferrocene, nickelocene, three cyclopentadienyl yttriums etc.) of the transition metal such as iron, nickel, yttrium or rare earth metal, and cost is high, and fail to avoid being oxidized not melting process and reactivation process.
Publication number be CN1250024A Introduction To Cn Patent a kind of preparation method of mesopore asphalt-base spherical activated carbon, the asphalt-base spherical activated carbon with certain specific surface area that once activation makes is flooded in the solution of metallic compound, after dry, at 800~1000 ℃, carry out re-activation with activator, can make mesopore asphalt-base spherical activated carbon.But this method is only just carried out the modification of follow-up aperture to ball shape active carbon, expands aperture with this, and between oxidation period, bitumen ball is still difficult to form primary hole.
In sum, emulsion process is prepared asphalt-base spherical activated carbon and is needed High Temperature High Pressure operation, is oxidized not melting process, and sphere diameter is unsuitable excessive, and can not control the granularity of ball shape active carbon, therefore cannot make the ball shape active carbon that narrow sphere diameter distributes; Suspension method is prepared asphalt-base spherical activated carbon sphere diameter narrowly distributing, but also exists and be oxidized not melting process.At the bitumen ball oxidation initial stage, not yet curing between asphaltene molecule, along with overflowing of hydrocarbons, bitumen ball is shunk, and is difficult for forming primary compared with macroporous structure, and rate of oxidation is extremely slow, and energy consumption is very high.And the aperture of the asphalt-base spherical activated carbon that makes of conventional steam activation belongs to micropore mostly, after deep activation, can obtain the mesoporous of a small amount of 2~4nm, but intensity and the yield of ball shape active carbon reduce greatly, and this has just limited the range of application of asphalt-base spherical activated carbon.
Summary of the invention:
The object of the present invention is to provide a kind of preparation method of asphalt-base spherical activated carbon of mesoporous prosperity, and the raw material of asphalt-base spherical activated carbon is cheap and easy to get, pore structure is adjustable, and mesoporous abundant, intensity is high, and technique is simple, is easy to control.
In order to achieve the above object, the technical solution used in the present invention comprises: a kind of preparation method of asphalt-base spherical activated carbon of mesoporous prosperity, it is characterized in that: take mesophase pitch as raw material, the heat-reactive phenolic resin that adds arene material and timber liquefied matter to be prepared from, modulate, and prepare bitumen ball by suspension method, finally adopt the techniques such as conventional preoxidation, charing and activation to prepare the asphalt-base spherical activated carbon of high mesoporous rate, prepared asphalt-base spherical activated carbon sphericity is between 0.94~0.97, and specific surface area exceedes 800m
2/ g, pore volume is greater than 0.35cm
3/ g, mean pore size is between 1.8~2.2nm.
Advantage of the present invention is:
1, resol used in the present invention, take larch sawdust as raw material, utilizes Wood liquefied technology, and with phenol, by wood chip heating liquefaction, with the synthetic heat-reactive phenolic resin resin of liquefied substance, raw material is biomass, and aboundresources is cheap.
2, there is adding of heat-reactive phenolic resin prepared by the timber liquefied matter of self cure performance, between oxidation period in pitch spheroid inside, can there is self cure in heat-reactive phenolic resin prepared by timber liquefied matter, and crosslinked with asphaltene molecule, accelerate oxidizing reaction rate, and this resin can play skeleton function, be beneficial to and form primary pore texture.
3, the heat-reactive phenolic resin that prepared by timber liquefied matter is easy to decompose, the primary pore structure forming is conducive to entering of activator, reduce soak time, and can be by controlling the add-on of resol, regulate and control its pore texture, be easy to prepare the ball shape active carbon of mesoporous prosperity, expand its Application Areas.
Embodiment:
Below the invention process is described in further detail:
A kind of preparation method of asphalt-base spherical activated carbon of mesoporous prosperity, it is characterized in that: take mesophase pitch as raw material, the heat-reactive phenolic resin that adds arene material and timber liquefied matter to be prepared from, modulate, and prepare bitumen ball by suspension method, finally adopt the techniques such as conventional preoxidation, charing and activation to prepare the asphalt-base spherical activated carbon of high mesoporous rate, prepared asphalt-base spherical activated carbon sphericity is between 0.94~0.97, and specific surface area exceedes 800m
2/ g, pore volume is greater than 0.35cm
3/ g, mean pore size is between 1.8~2.2nm.
Below, the present invention will be further detailed with embodiment, but it is not limited to any or the similar example of these embodiment.
Embodiment 1:
Take mesophase pitch as raw material, add the naphthalene of massfraction 45%, in reactor, heated and stirred is reacted to raw material fusing, and stirring reaction 30min at 180 ℃, is cooled to 150 ℃ by mixture, and insulation 1h, takes out reactant the cooling block mixture that obtains.Block mixture was pulverized to 20 eye mesh screens, and the water-soluble middle suspension method of polyvinyl alcohol 1% is prepared bitumen ball.20~36 object bitumen ball that obtain are warming up to 300 ℃ with the temperature rise rate of 0.5 ℃/min in air and carry out preoxidation, obtain preoxidation bitumen ball.Then under nitrogen protection, be warming up to 500 ℃ with the temperature rise rate of 5 ℃/min, obtain charing bitumen ball.Charing bitumen ball is warming up to 850 ℃ with the temperature rise rate of 5 ℃/min, then passes into carbonic acid gas and activate, and obtains asphalt-base spherical activated carbon sample.Prepared asphalt-base spherical activated carbon sphericity is 0.97, and specific surface area can reach 823.83m
2/ g, pore volume is 0.386cm
3/ g, mean pore size is 1.88nm.
Embodiment 2:
Take mesophase pitch as raw material, add the naphthalene of massfraction 45%, in reactor, heated and stirred is reacted to raw material fusing, and stirring reaction 30min at 180 ℃, is cooled to 150 ℃ by mixture, and insulation 1h, takes out reactant the cooling block mixture that obtains.Block mixture was pulverized to 30 eye mesh screens, and the water-soluble middle suspension method of polyvinyl alcohol 1% is prepared bitumen ball.20~36 object bitumen ball that obtain are warming up to 300 ℃ with the temperature rise rate of 0.5 ℃/min in air and carry out preoxidation, obtain preoxidation bitumen ball.Then under nitrogen protection, be warming up to 500 ℃ with the temperature rise rate of 5 ℃/min, obtain charing bitumen ball.Charing bitumen ball activates 120min in 50% KOH solution, is warming up to 850 ℃ with the temperature rise rate of 5 ℃/min, obtains asphalt-base spherical activated carbon sample.Prepared asphalt-base spherical activated carbon sphericity is 0.97, and specific surface area is 1086.61m
2/ g, pore volume is 0.512cm
3/ g, mean pore size is 1.89nm.
Embodiment 3:
Take mesophase pitch as raw material, add the naphthalene of massfraction 45%, in reactor, heated and stirred is reacted to raw material and is melted, the heat-reactive phenolic resin that adds therein 1% timber liquefied matter to be prepared from, stirring reaction 30min at 180 ℃, mixture is cooled to 150 ℃, and insulation 1h, takes out reactant the cooling block mixture that obtains.Block mixture was crushed to 30 eye mesh screens, and the water-soluble middle suspension method of polyvinyl alcohol 1% is prepared bitumen ball.20~36 object bitumen ball that obtain are warming up to 300 ℃ with the temperature rise rate of 0.5 ℃/min in air and carry out preoxidation, obtain preoxidation bitumen ball.Then under nitrogen protection, be warming up to 500 ℃ with the temperature rise rate of 5 ℃/min, obtain charing bitumen ball.Charing bitumen ball is warming up to 850 ℃ with the temperature rise rate of 5 ℃/min, then passes into carbonic acid gas and activate, and obtains asphalt-base spherical activated carbon sample.Prepared asphalt-base spherical activated carbon sphericity is 0.95, and specific surface area can reach 927.84m
2/ g, pore volume is 0.427cm
3/ g, mean pore size is 1.84nm.
Embodiment 4:
Take mesophase pitch as raw material, add the naphthalene of massfraction 45%, in reactor, heated and stirred is reacted to raw material and is melted, the heat-reactive phenolic resin that adds therein 1% timber liquefied matter to be prepared from, stirring reaction 30min at 180 ℃, mixture is cooled to 150 ℃, and insulation 1h, takes out reactant the cooling block mixture that obtains.Block mixture was crushed to 20 eye mesh screens, and the water-soluble middle suspension method of polyvinyl alcohol 1% is prepared bitumen ball.20~36 object bitumen ball that obtain are warming up to 300 ℃ with the temperature rise rate of 0.5 ℃/min in air and carry out preoxidation, obtain preoxidation bitumen ball.Then under nitrogen protection, be warming up to 500 ℃ with the temperature rise rate of 5 ℃/min, obtain charing bitumen ball.Charing bitumen ball activates 120min in 50% KOH solution, is warming up to 850 ℃ with the temperature rise rate of 5 ℃/min, obtains asphalt-base spherical activated carbon sample.Prepared asphalt-base spherical activated carbon sphericity is 0.95, and specific surface area is 1268.26m
2/ g, pore volume is 0.682cm
3/ g, mean pore size is 2.15nm.
Claims (9)
1. the preparation method of the asphalt-base spherical activated carbon of a mesoporous prosperity, it is characterized in that: take mesophase pitch as raw material, the heat-reactive phenolic resin that adds arene material and timber liquefied matter to be prepared from, modulate, and prepare bitumen ball by suspension method, finally adopt the techniques such as conventional preoxidation, charing and activation to prepare the asphalt-base spherical activated carbon of high mesoporous rate, prepared asphalt-base spherical activated carbon sphericity is between 0.94~0.97, and specific surface area exceedes 800m
2/ g, pore volume is greater than 0.35cm
3/ g, mean pore size is between 1.8~2.2nm.
2. according to the preparation method of the asphalt-base spherical activated carbon of a kind of mesoporous prosperity claimed in claim 1, it is characterized in that: in pitch modulation, arene material used is naphthalene, mesophase pitch, arene material add in reactor with 15%~60% ratio, and heated and stirred is reacted to raw material and melted.
3. according to the preparation method of the asphalt-base spherical activated carbon of a kind of mesoporous prosperity claimed in claim 1, it is characterized in that: mesophase pitch, arene material add in reactor in the proper ratio, heated and stirred is reacted to raw material and is melted.Add appropriate timber liquefied matter, Wood liquefied resin is heat-reactive phenolic resin again, and add-on is 0.5%~1.5%.
4. according to the preparation method of the asphalt-base spherical activated carbon of a kind of mesoporous prosperity claimed in claim 1, it is characterized in that: mesophase pitch, arene material add in reactor in the proper ratio, heated and stirred is reacted to raw material and is melted.Add appropriate timber liquefied matter, stirring reaction 30min at 180~210 ℃, is cooled to 150 ℃ by mixture again, and insulation 1h, takes out reactant the cooling block mixture that obtains.
5. according to the preparation method of the asphalt-base spherical activated carbon of a kind of mesoporous prosperity claimed in claim 1, it is characterized in that: reaction is obtained to block mixture and be crushed to 20~50 object raw material granularities, in dispersant solution, suspension method is prepared bitumen ball, the polyvinyl alcohol water solution that dispersant solution is 1%.
6. according to the preparation method of the asphalt-base spherical activated carbon of a kind of mesoporous prosperity claimed in claim 1, it is characterized in that: the bitumen ball of the certain particle diameter obtaining is warming up to 300 ℃ with the temperature rise rate of 0.5 ℃/min in air, preoxidation time is 3~7h, obtains preoxidation bitumen ball.
7. according to the preparation method of the asphalt-base spherical activated carbon of a kind of mesoporous prosperity claimed in claim 1; it is characterized in that: preoxidation bitumen ball is under nitrogen protection; be warming up to 500~700 ℃ with the temperature rise rate of 5 ℃/min and carry out charing, carbonization time is 1~3h, obtains charing bitumen ball.
8. according to the preparation method of the asphalt-base spherical activated carbon of a kind of mesoporous prosperity claimed in claim 1; it is characterized in that: charing bitumen ball is under nitrogen protection; be warming up to 800~900 ℃ with the temperature rise rate of 5 ℃/min activates under the condition that passes into carbonic acid gas; soak time is 0.25~5h; or activate in the charing bitumen ball KOH solution that is 20~70% at massfraction; again under nitrogen atmosphere; be warming up to 800~900 ℃ with the temperature rise rate of 5 ℃/min; soak time is 0.25~2h, obtains asphalt-base spherical activated carbon.
9. according to the preparation method of the asphalt-base spherical activated carbon of a kind of mesoporous prosperity claimed in claim 1, it is characterized in that: prepared asphalt-base spherical activated carbon sphericity is between 0.94~0.97, and specific surface area exceedes 800m
2/ g, pore volume is greater than 0.35cm
3/ g, mean pore size is between 1.8~2.2nm.
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CN109659152A (en) * | 2019-02-18 | 2019-04-19 | 东北林业大学 | A kind of three-dimensional micro charcoal-aero gel/ruthenium-oxide combination electrode material and preparation method for supercapacitor |
CN111422869A (en) * | 2020-03-04 | 2020-07-17 | 山西新华化工有限责任公司 | Preparation method for industrially improving crushing strength of asphalt balls |
CN111547721A (en) * | 2020-05-09 | 2020-08-18 | 中国铝业股份有限公司 | Preparation method of mesoporous activated carbon for supercapacitor |
CN115611349A (en) * | 2021-07-16 | 2023-01-17 | 碧儿赛福有限公司 | Filter for water treatment and preparation method of spherical activated carbon |
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