CN1724344A - Preparing multipurpous carbon with regular constructure and high ratio surface area by mould board carbonizing process - Google Patents
Preparing multipurpous carbon with regular constructure and high ratio surface area by mould board carbonizing process Download PDFInfo
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Abstract
A process for preparing porous carbon with regular structure and large specific surface area includes such steps as providing Y zeolite as template, and furfuryl alcohol as carbon precursor, pre-treating the template, preparing organic substance-template compound, preparing carbon-template compound, removing template to fill the organic substance in the nano-arteries of inorganic material, polymerizing, charring and removing template.
Description
Technical field
The invention belongs to the carbon material science and technology field.Relating to a kind of is template with the porous inorganic material with regular pore structure, the technological method that organic compound has the porous charcoal of regular texture and high-specific surface area for the preparation of carbon matrix precursor template.
Background technology
Porous carbon material (Porous carbon materials, PCM) be meant the carbon material with different pore structures, its pore dimension can change to the scope that is suitable for microbial reproduction and active micron order pore broad at the nano level superfine micropore suitable with the adsorbed molecules size.The raw material of wood-charcoal material of different shapes such as traditional gac (being common gac), super-activated carbon (being active carbon with high specific surface area), activated carbon microballon, activated carbon fiber, carbon molecular sieve, different performance all belongs to the category of porous charcoal.Since nineteen nineties, because environmental problem becomes the focus that common people pay close attention to day by day, porous charcoal has obtained significant progress as a kind of sorbing material of excellent performance at aspects such as purifying air, sewage disposals.Porous charcoal has also had further expansion in the application of electronic industry, biomaterial and medical field in recent years.
The principal element that influences the charcoal absorption performance has specific surface area, pore volume and pore size distribution.In general the specific surface area of gac, pore volume are big more, and its adsorptive power is strong more.International pure chemistry and the difference of application federation (IUPAC) according to molecular adsorption in the different size holes are divided into the hole in the sorbent material: the macropore of aperture W＞50nm; The mesopore of 2nm＜W＜50nm; The micropore of W＜2nm.The adsorption maximum is micropore in gac, and it measures dominating role to the absorption of gac.As the gac of sorbent material, its pore size and adsorption molecule diameter have a suitable matching relationship, and under certain conditions, the gac pore size distribution is concentrated more, and the performance of product is just good more.
Since 18 beginnings of the century found that charcoal had adsorption, people are to being that the porous carbon material of representative has carried out a large amount of research with the gac, developed physical activation method and chemical activation method in succession and prepared various gacs, the preparation raw material is also developed into rich carbon source materials such as shell, coal, pitch, industrial residue by initial charcoal.The specific surface area of common gac is generally at 800-1000m
2/ g, thereby loading capacity is limited.Chemical activation method is a kind of method that can obtain active carbon with high specific surface area.Earlier 1970s, it is raw material that people such as U.S. Wenerberg find with the refinery coke, in preparation process, add KOH, can obtain so-called super-activated carbon (the Super activated carbon of specific surface area 2000m2/g, be called for short SAC), after this, they constantly improve the work of oneself, have obtained specific surface area up to 3000-4000m
2The gac of/g.This technology of the mid-80 has realized suitability for industrialized production.Meanwhile, Japanese Kansal Thermochemistry Co., Ltd. makes raw material with pitch intermediate phase microballoon, adopts the KOH activation method to obtain specific surface area 4000m
2The gac of/g, and realize commercially producing in the initial stage nineties.But during being to produce, the outstanding problem of chemical activation method produces a large amount of environmental problems, production cost height; In addition, very limited owing to the restriction of raw materials used body structure and form to the ability of regulation and control of product pore structure, be difficult to by changing the absorbent charcoal material that charing or activation condition obtain regular texture, single pore size distribution, its pore size distribution range broad.Template is a kind of can the design in the nanoscale scope of molecular size and the effective ways of controlling polymers precursor construction, by adopting special carbonization process that microtexture is kept, thus obtain with traditional sense on diversely have a porous carbon material that regular texture and uniform pore size distribute.
Template originates from the preparation of organic materials.People such as C.R.Martin were contained the polycarbonate filtering membrane of nanometer micropore as the template synthesis method that has proposed nano structural material on the basis of template by electrochemical polymerization compositing conducting polypyrrole in employing in 1985, hereafter, this synthetic method has attracted lot of domestic and foreign research worker's sight line, and people utilize this method to synthesize a series of nano structural material.In recent years, template is in the application Showed Very Brisk of porous material research field.1999, the research group of two Korea S (Jinwoo Lee, Ryong Ryoo) used the mesoporous silicon molecular sieve as template respectively, has obtained to have the mesopore charcoal of regular texture.Ryoo etc. are template with MCM-48, are carbon source synthetic mesopore carbon molecular sieve with the sulphuric acid soln of sucrose, show BraggX ray small-angle diffraction peak first, show the order of institute's synthetic raw material of wood-charcoal material.Its typical synthetic method is earlier MCM-48 to be immersed in the sulphuric acid soln of sucrose, and mixture is dry under 100 ℃ and 160 ℃ respectively, repeats above-mentioned dipping, drying step then.Desciccate removes template with sodium hydroxide/ethyl alcohol solution under 100 ℃ after 900 ℃ of following charings.The BET specific surface area of the porous charcoal that makes thus is 1300-1800m
2/ g, the hole major part is the mesopore about 3nm, contains the micropore about 20%.1997, the Kyotani of northeastern Japan university etc. are the micropore charcoal that synthesizes tactical rule of template success with the y-type zeolite, point out that preparation process is without any need for gas or chemical activation, and the porous charcoal that proof is obtained is a synthetic in zeolite cavity, and the vesicular structure of these charcoals comes from the vesicular structure of y-type zeolite.Its preparation process mainly comprises the removing etc. of dipping, polymerization, charing, vapour deposition, template of modulation, the carbon source of various template, and the specific surface area of resulting porous carbon material can reach 3000m
2More than/the g.
Existing these research work lay particular emphasis on by adopting different template to adjust the hole structural property of product from synthetic template, and preparation cycle is long, and condition is wayward; In addition, because the hole structural property of this material excellence and huge potential application foreground, equipment and device for the detailed parameter of this class porous carbon material technology of preparing, employing in all research papers all do not have systematic account.
In sum, chemical activation method is a kind of important method for preparing the high specific surface area porous carbon material, but because the restriction of preparation raw material mix and fabricating technology, make this method very limited, at present pore dimension and the structure in the controlled target product effectively also to the regulation and control of the pore structure of product charcoal.Template is a kind of effectively method of control punch structure, can be from pore size to pore structure regularity two aspects to product raw material of wood-charcoal material modulation in addition.The template that is template with various permeability inorganic materials is considered to the method that only effective preparation known today has high-sequential structure porous carbon material.
In view of this, for obtaining high yield, pore size homogeneous, structurally ordered high specific surface area porous charcoal, the present invention proposes operational path/method that the template charring prepares porous charcoal.Up to the present, bibliographical information at home and abroad about directly preparing in the research work of porous carbon material with template, close with present technique has: Chem.Mater.2001 (13) 4413 and J.Phys.Chem.B1999,103,7743, it is template that its research contents relates to zeolite and mesoporous silicon, and organism furfuryl alcohol, sucrose, polyacrylonitrile etc. prepare porous charcoal for the carbon precursor template.But in the literary composition details of preparation process and device thereof, parameter are not introduced, its preparation cycle is long, and processing condition and technology be imperfection also, as in preparation process, and the effective means etc. that is filled into organism in the inorganic materials duct and removes template.
Summary of the invention
The high specific surface area porous charcoal that the objective of the invention is a large amount of processability excellences, structurally ordered (single pore size distribution).
The present invention has the porous charcoal of regular texture and high-specific surface area a kind of the preparation with the template charring.This method is utilized the pore structure feature of the rule of inorganic porous material y-type zeolite, the organism furfuryl alcohol is filled in the nano pore of inorganic materials, polymerization, charing take place, remove template, make have regular texture, porous charcoal that high-specific surface area, high pore volume, pore structure and hole dimension adjustable size become.
Technical scheme of the present invention: at first that the template y-type zeolite is dry under certain temperature, vacuum state; After cooling to room temperature, add liquid state organics and stirring under the vacuum; Under certain pressure, flood certain hour subsequently; The mixture that the organism/mould that obtains is pulled agent filters, under the normal temperature after the drying, with excessive organic solvent washing; Organism/the stamp complex that obtains is warming up to temperature of reaction with certain temperature rise rate and carries out polymerization, charing processing in charring furnace, whole process is carried out under nitrogen protection; Charcoal/template composite that charing obtains is handled under the condition of ultrasonic concussion with hydrofluoric acid and is removed template.Obtain to have the porous charcoal of regular texture, high-specific surface area thus.
Concrete preparation process is as follows:
1, the pre-treatment of mould material: get powdery y-type zeolite template under 120 ℃ under vacuum condition drying treatment 1h;
2, the preparation of organism/template composite: in immersion system (Fig. 1), add a certain amount of template, under vacuum, normal temperature state, add isopyknic organism, (mould material and organic proportioning are determined according to the pore volume and the organic density of mould material), what of template and organism consumption can be as requested the output of target product determine.Stir under these conditions, 30min feeds nitrogen later on and continues to stir 6-9h, subsequently pressurization (1.0-1.4MPa) dipping 1.0-2.0h.Mixture washes the organism that remains in inorganic template outside surface with excessive organic solvent o-Xylol (10-15 minute, mechanical stirring) after the dry air after filtration, and solid phase prod obtains organism/template composite further at air drying;
3, the preparation of charcoal/template composite: step 2 is obtained mixture insert and carry out polymerization and charing in the charring furnace (Fig. 2) and handle, whole polymerization, carbonization process are to carry out under nitrogen protection.Actual conditions is as follows: 95 ℃ are heated 24h down, heat 8h down at 150 ℃ then and carry out polyreaction; The charing heating curve is: with 2.5 ℃/min temperature rise rate, temperature is warming up to 300 ℃ from 150 ℃; Again with 5 ℃/min temperature rise rate, temperature is warming up to 700 ℃ from 300 ℃, will contain the N of 4-7% propylene
2Gas (flow velocity 5cm/min) feeds reactor, decomposes propylene gas and carries out vapour deposition, and reaction is carried out cutting off propylene gas behind the 3h.Temperature rise rate with 5 ℃/min rises to 900 ℃ with temperature at last, and high temperature carbonization 3h postcooling to room temperature obtains template/charcoal mixture;
4, the removal of template: in template/carbon composite that step 3 obtains, add HF solution (volume ratio of hydrofluoric acid and composite materials is greater than 2), supersound process 15min, continue to soak 5-8h then, filtering separation, remove acid solution, and with deionized water wash product charcoal, promptly obtain having the porous carbon material of regular texture and high-specific surface area after the drying.
Characteristics of the present invention: (1) fills organism in inorganic porous material, and the pressurization two-step approach was carried out after mode adopted first vacuum; (2) organism charing in the nano pore of template inorganic porous material; (3) under ultrasonic concussion condition, the product porous charcoal is discharged from template; (4) porous charcoal output can be controlled by carbon source and template agent, obtains pore structure feature and high-specific surface area that product has rule.
Effect of the present invention and benefit are as follows:
1, the present invention has the method for regular texture and high specific surface micro-pore charcoal a kind of the preparation based on the template technology, and preparation raw material and template thereof are the commercial goods, and starting material obtain easily.Preparation process is simple, processing ease, can obtain the porous carbon material with special construction and performance that conventional chemical activation method can't obtain.
2, the present invention is impregnated into organism in the template nano pore by vacuum, pressurization two-step approach, has improved charging efficiency effectively, has improved the output of product greatly.The raising of production throughput can be finished by the amount of simple increase template and carbon source as required.
3, the present invention adopts the method for ultrasonic concussion to remove template, can not only remove template effectively, and can reduce the time that removes template significantly, and then shortens preparation cycle.
4, the present invention adopts simple dipping and heating carbonizing apparatus, can finish whole process of preparation, and this technology is not high to equipment requirements, and parameter is controlled easily, and actually operating is simple, is easy to realize industrialization.
5, the micropore carbon material that makes is structurally ordered, pore size distribution is single, specific surface area and pore volume are big, can be used as uses such as sorbing material, energy storage material, electronic device material, biomaterial and catalyst support material.
Description of drawings
Fig. 1 is for to prepare the employed immersion system figure of porous charcoal with present method, wherein: 1-raw material tank, 2-valve, 3-steeping cell, 4-vacuum pump, 5-tensimeter;
Fig. 2 is for to prepare the employed carbonizing apparatus figure of porous carbon material with present method, wherein, and 6-Reaktionsofen, 7-temperature controller, 8-mixing chamber, 9-threeway, 10 under meters, 11-nitrogen, 12-propylene, 13-reactant, 14-tail gas;
Fig. 3 is the stereoscan photograph of porous charcoal, shows the surface topography of porous charcoal;
Fig. 4 is the high-resolution-ration transmission electric-lens photo of porous charcoal, shows the microcosmic regular texture of porous charcoal;
Fig. 5 is the XRD figure of product porous charcoal, and wherein: ordinate zou is represented diffracted intensity, and X-coordinate is represented diffraction angle 2 θ;
Fig. 6 is the oxide gas adsorption isothermal curve, and wherein: ordinate zou is represented adsorptive capacity, and X-coordinate is represented relative pressure, and illustration is the pore size distribution curve of porous charcoal, and the aperture concentrates on 1-2nm.
Embodiment
The present invention is further described below by embodiment.
With organism furfuryl alcohol (FA) is carbon matrix precursor, powdery commodity y-type zeolite (SiO
2/ Al
2O
3=7.4) be template, the preparation of template charring has the high specific surface area porous charcoal of regular texture.Concrete steps are as follows: 1, take by weighing 3g powdery y-type zeolite under 120 ℃ under vacuum condition dry 1h.2, with this exsiccant powdery y-type zeolite, under vacuum, room temperature, add the FA of 10ml, and begin to stir, 30min feeds nitrogen later on to be continued to stir 8h, floods 1.2h subsequently under the 1.0MPa nitrogen pressure.3, with FA/Y type zeolite mixture filtration and dry under air, obtain exsiccant FA/Y type zeolite.4, the FA/Y type zeolite that obtains of step 3, filters and removes washing composition, further obtains the FA/ zeolite composition behind the air drying to remove the FA (churning time is 10min) that remains in the y-type zeolite outside surface with the o-Xylol washing.5, the FA/ zeolite composition that step 4 is obtained is inserted and is carried out polymerization, charing processing in the charring furnace, and whole process is carried out under nitrogen protection.Polymerizing condition: 95 ℃ are heated 24h down, heat 8h down at 150 ℃ then.Carbonization condition: with 2.5 ℃/min of temperature rise rate, temperature is heated to 300 ℃ from 150 ℃; 5 ℃/min of temperature rise rate, temperature is from 300 ℃-700 ℃; When temperature rises to 700 ℃, will contain 5% propylene (flow 6cm
3/ min) N
2(flow is 120cm to gas
3/ min) feed reactor, carry out vapour deposition, reaction is carried out cutting off propylene gas behind the 3h; Temperature rise rate with 5 ℃/min rises to 900 ℃ with temperature at last, and high temperature carbonization 3h postcooling to room temperature obtains charcoal/zeolite composition.6, add the 100mLHF acid solution in charcoal/zeolite composition that step 5 obtains, ultrasonic concussion is soaked 5h after handling 15min.7, mixture filters, and isolates acid solution, solid deionized water wash, filtration, the dry product porous charcoal that promptly obtains later.With technology such as scanning electronic microscope (see figure 3), high resolution transmission electron microscopy (see figure 4) and X-ray diffraction (see figure 5), specific surface absorption instrument (see figure 6)s prepared product is carried out phenetic analysis.The result sees accompanying drawing for details.
Embodiment 2
With organism furfuryl alcohol (FA) is carbon precursor, powdery commodity y-type zeolite (SiO
2/ Al
2O
3=7.4) be template, the preparation of template charring has the high specific surface area porous charcoal of regular texture.Concrete steps are as follows: 1, take by weighing 5g powdery y-type zeolite under 120 ℃ under vacuum condition dry 1h.2, with this exsiccant powdery y-type zeolite, under vacuum, room temperature, add the FA of 15mL, and begin to stir, 30min feeds nitrogen later on to be continued to stir 8h, floods 1.5h subsequently under the 1.2MPa nitrogen pressure.3, with FA/Y type zeolite mixture filtration and dry under air, obtain exsiccant FA/Y type zeolite.4, the FA/Y type zeolite that obtains of step 3 filters and removes washing composition with o-Xylol washing the removing FA (churning time is 10min) that remains in the y-type zeolite outside surface, obtains the FA/ zeolite composition under the air after the drying.5, the FA/ zeolite composition that step 4 is obtained is inserted and is carried out polymerization, charing processing in the charring furnace, and whole process is carried out under nitrogen protection.Polymerizing condition: 95 ℃ are heated 24h down, heat 8h down at 150 ℃ then.Carbonization condition: with 2.5 ℃/min of temperature rise rate, temperature is heated to 300 ℃ from 150 ℃; 5 ℃/min of temperature rise rate, temperature is from 300 ℃-700 ℃; When temperature rises to 700 ℃, will contain 5% propylene (flow 6cm
3/ min) N
2(flow is 120cm to gas
3/ min) feed reactor, carry out vapour deposition, reaction is carried out cutting off propylene gas behind the 3h; Temperature rise rate with 5 ℃/min rises to 900 ℃ with temperature at last, and high temperature carbonization 3h postcooling to room temperature obtains charcoal/zeolite composition.6, add the 150mLHF acid solution in charcoal/zeolite composition that step 5 obtains, ultrasonic concussion is soaked 5h after handling 15min.7, mixture filters, and isolates acid solution, solid deionized water wash, filtration, the dry product porous charcoal that promptly obtains later.The analysis and characterization of product adopts technology such as high resolution transmission electron microscopy, scanning electronic microscope, X-ray diffraction, specific surface absorption instrument.
With organism furfuryl alcohol (FA) is carbon precursor, powdery commodity y-type zeolite (SiO
2/ Al
2O
3=7.4) be template, the preparation of template charring has the high specific surface area porous charcoal of regular texture.Concrete steps are as follows: 1, take by weighing 10g powdery y-type zeolite under 120 ℃ under vacuum condition dry 1h.2, with this exsiccant powdery y-type zeolite, under vacuum, room temperature, add the FA of 25mL, and begin to stir, 30min feeds nitrogen later on to be continued to stir 8h, floods 1.5h subsequently under the 1.2MPa nitrogen pressure.3, with FA/Y type zeolite mixture filtration and dry under air, obtain exsiccant FA/Y type zeolite.4, the FA/Y type zeolite that obtains of step 3 filters and removes washing composition with o-Xylol washing the removing FA (churning time is 10min) that remains in the y-type zeolite outside surface, obtains the FA/ zeolite composition under the air after the drying.5, the FA/ zeolite composition that step 4 is obtained is inserted and is carried out polymerization, charing processing in the charring furnace, and whole process is carried out under nitrogen protection.Polymerizing condition: 95 ℃ are heated 24h down, heat 8h down at 150 ℃ then.Carbonization condition: with 2.5 ℃/min of temperature rise rate, temperature is heated to 300 ℃ from 150 ℃; 5 ℃/min of temperature rise rate, temperature is from 300 ℃-700 ℃; When temperature rises to 700 ℃, will contain 5% propylene (flow 6cm
3/ min) N
2(flow is 120cm to gas
3/ min) feed reactor, carry out vapour deposition, reaction is carried out cutting off propylene gas behind the 3h; Temperature rise rate with 5 ℃/min rises to 900 ℃ with temperature at last, and high temperature carbonization 3h postcooling to room temperature obtains charcoal/zeolite composition.6, add the 200mLHF acid solution in charcoal/zeolite composition that step 5 obtains, ultrasonic concussion is soaked 5h after handling 15min.7, mixture filters, and isolates acid solution, solid deionized water wash, filtration, the dry product porous charcoal that promptly obtains later.The analysis and characterization of product adopts technology such as high resolution transmission electron microscopy, scanning electronic microscope, X-ray diffraction, specific surface absorption instrument.
Claims (1)
1, a kind of is template with the porous inorganic material, and organism is that the carbon precursor preparation has the template charring of regular texture and high specific surface area porous charcoal, it is characterized in that this method is to make porous charcoal through the following steps:
(1) pre-treatment of mould material: with commodity y-type zeolite template under 120 ℃ under vacuum condition drying treatment 1h;
(2) preparation of organism/template composite: with dry postcooling to the powdery y-type zeolite of room temperature in immersion system, vacuum, normal temperature state add isopyknic organism furfuryl alcohol down, stir 30min and feed the lasting 6-9h of stirring of nitrogen later on, under 1.0-1.4Mpa nitrogen, flood 1.0-2.0h subsequently, mixture after filtration, after the dry air, wash the organism that remains in the template outside surface with excessive organic solvent, solid phase prod obtains organism/template composite again at air drying;
(3) preparation of charcoal/template composite: organism charing in the nano pore of template inorganic porous material is that furfuryl alcohol/zeolite composition is positioned in the charring furnace, under nitrogen protection, in 95 ℃ of heating 24h, heats 8h down at 150 ℃ then and carries out polyreaction; Carbonization condition: under nitrogen protection,, temperature is warming up to 300 ℃ from 150 ℃ with 2.5 ℃/min temperature rise rate; Again with 5 ℃/min temperature rise rate, temperature is warming up to 700 ℃ from 300 ℃, will contain the N of 4-7% propylene
2Gas feeds reactor, and reaction is carried out cutting off propylene gas behind the 3h, and the temperature rise rate with 5 ℃/min rises to 900 ℃ with temperature at last, and charing 3h postcooling to room temperature obtains charcoal/template composite;
(4) removal of template: the adding volume ratio is 2 HF acid solution dissolving template in charcoal/template composite, adopt supersound process 15min, continue to soak 5-8h then, filter to isolate acid solution, and with deionized water wash product charcoal, promptly obtain having the porous carbon material of regular texture and high-specific surface area after the drying.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN100363254C (en) * | 2006-07-19 | 2008-01-23 | 中国石油化工股份有限公司 | Method for preparing ordered mesoporous carbon |
| CN102054575B (en) * | 2009-11-06 | 2012-06-27 | 中国科学院上海硅酸盐研究所 | Method for preparing magnetic mesoporous carbon by co-pouring |
| CN102107863B (en) * | 2009-12-25 | 2012-12-12 | 北京化工大学 | Porous carbon material and preparation method thereof |
| CN108046829A (en) * | 2017-12-20 | 2018-05-18 | 东北大学 | A kind of nonmetallic mineral porous substrate and its preparation method and application |
| CN108862278A (en) * | 2018-05-29 | 2018-11-23 | 木林森活性炭江苏有限公司 | A kind of production method of drinks special-purpose activated charcoal |
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| CN1118591C (en) * | 2000-07-21 | 2003-08-20 | 中国科学院山西煤炭化学研究所 | Method for preparing foam block active carbon fibre |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN100363254C (en) * | 2006-07-19 | 2008-01-23 | 中国石油化工股份有限公司 | Method for preparing ordered mesoporous carbon |
| CN102054575B (en) * | 2009-11-06 | 2012-06-27 | 中国科学院上海硅酸盐研究所 | Method for preparing magnetic mesoporous carbon by co-pouring |
| CN102107863B (en) * | 2009-12-25 | 2012-12-12 | 北京化工大学 | Porous carbon material and preparation method thereof |
| CN108046829A (en) * | 2017-12-20 | 2018-05-18 | 东北大学 | A kind of nonmetallic mineral porous substrate and its preparation method and application |
| CN108862278A (en) * | 2018-05-29 | 2018-11-23 | 木林森活性炭江苏有限公司 | A kind of production method of drinks special-purpose activated charcoal |
| CN112591992A (en) * | 2020-12-03 | 2021-04-02 | 成都理工大学 | Filling medium for permeable reactive barrier and preparation method thereof |
| CN113028436A (en) * | 2021-02-08 | 2021-06-25 | 华北电力大学 | System and method for removing pollutants in coal-fired flue gas |
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