CN101214951B - Preparation of high specific surface area and narrow pore distribution porous carbon material - Google Patents
Preparation of high specific surface area and narrow pore distribution porous carbon material Download PDFInfo
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- CN101214951B CN101214951B CN2008100502498A CN200810050249A CN101214951B CN 101214951 B CN101214951 B CN 101214951B CN 2008100502498 A CN2008100502498 A CN 2008100502498A CN 200810050249 A CN200810050249 A CN 200810050249A CN 101214951 B CN101214951 B CN 101214951B
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Abstract
The invention belongs to the preparing field of porous carbon materials, which relates to a porous carbon material with high specific surface area and narrow pore distribution and which is prepared by adopting pin needles with biomass materials. The specific surface area of the porous carbon materials is capable of surpassing 3000m/2g by adjusting activating agent dosage, activating temperature and activating time. The method of the invention has low requirement for production facilities, and has simple preparing process and low time-consumption. The main byproduct of the reaction is tar which is a product with high value in use. The washing solution of the porous carbon materials is aqueous solution which is rich in potassium ions, and is perfect potash fertilizer for agricultural industry via simple dealing. The porous carbon materials have high application prospect in the fields like the storage and separation of gas, electrode materials, catalysts or catalyst carriers in a plurality of chemical reactions, sewage disposal, recovery of noble metals and the like. The method has the advantages of cheap, plentiful and easily gained raw materials, simple preparing process, preparingcondition without region limitation, thereby being adapted for large-scale industrial production.
Description
Technical field
The invention belongs to the porous carbon materials preparation field, be specifically related to a kind of method of utilizing the biological material pine needle for the porous carbon materials with high-specific surface area, narrower pore distribution of feedstock production.
Background technology
Owing to have abundant pore passage structure and higher specific surface area, porous carbon materials has a wide range of applications in daily life and industrial production.At present, porous carbon materials is mainly used in absorbing obnoxious flavour, sewage disposal, the storage of gas with separate, electrode materials, number of chemical catalyst for reaction or the aspects such as support of the catalyst, precious metal recovery of battery or electric capacity.Growing along with society, also increasing to the demand of porous carbon materials.Porous carbon materials more common in the life is mainly gac, the production technique of gac also emerges in an endless stream, timber, various shell, coal, brown coal, peat etc. are raw material, through pulverizing, sieve, series of processes processing and manufacturings such as activation treatment, rinsing, oven dry and screening go out various gacs.But shortcoming such as most gac exists duct size distribution heterogeneity on the market, and specific surface area is less, these shortcomings have seriously restricted the application of gac aspect a lot.Therefore, people have developed some novel porous carbon materials, peacekeeping utilizes inorganic porous material to prepare the porous carbon with regular pore size distribution and high-specific surface area for template as active carbon fibre, though the performance specific activity charcoal of the porous carbon materials that these are new improves a lot, but series of new problems such as complicated process of preparation have been produced again, the cost height, can not mass production and performance development perfect not enough etc., these have all seriously restricted the practical application of these novel porous carbon materials, in sum, porous activated carbon also has overwhelming superiority in the application of present productive life.
The preparation process of porous carbon materials: earlier presoma is being lower than carbonization under 700 ℃ the temperature, and then is carrying out oxidized activating and handle, activation method is divided into two big classes usually: one, chemical activation method mainly is with some alkali, acid and salt such as KOH, Ca (OH)
2, NaOH, H
2SO
4, H
3PO
4, ZnCl
2And CaCl
2Deng as activator at inert atmosphere (as N
2And Ar) protection activates carbide down; Two, physical activation method mainly is meant with H
2O and CO
2Deng material as activator at inert atmosphere (as N
2And Ar) protection is carried out activation treatment to carbonized product down.Traditional gac major part of utilizing the chemical activation method preparation has bigger specific surface area, in various application facet good effect is arranged all, but because the pore size distribution of the gac of chemical activation method preparation heterogeneity makes its application in some fields (as gas delivery) be subjected to certain restriction very much.The porous activated carbon that makes with physical activation method has narrower pore size distribution, effect is preferably all arranged in various Application Areass, but the specific surface area of the porous carbon materials of common this method preparation is all lower, makes these porous carbon materials also not reach the ideal effect.
The present invention is that the prepared using chemical activation method prepares porous carbon materials with general, reproducible biological material.Flood in basic solution by the carbonized product with biological material, drying is carried out activation treatment then and is obtained the porous carbon materials that fine has high-specific surface area in inert atmosphere.At present, most high grade activated carbon utilizes timber and high-quality coal to produce as starting material, and therefore, the gac industry all will consume a large amount of timber and coal every year.At forest and the problems such as environment protection and save energy that China faced; substitute material preparation high-quality porous carbon materials such as timber and coal if search out reproducible, cheap, general biological material, will save timber, coal and protection environment to China so and play very big effect.
Summary of the invention
The problem to be solved in the present invention is the deficiency at the porous carbon materials for preparing in the background technology, and by simple chemical activation treatment process, providing a kind of is the method that feedstock production has the narrow porous carbon materials of high-specific surface area, pore size distribution with the pine needle.
The present invention utilizes pine needle that is general, cheap, that be easy to get to be starting material; pine needle is carried out carbonizing treatment under inert atmosphere protection; with carbonized product and basic solution hybrid infusion for some time, alkali is distributed between the carbonized product fully then, then in air with the solvent evaporate to dryness in the mixture; remaining mixture carries out high-temperature activation under the protection of inert atmosphere handles; through washing, acid treatment is washed again; processes such as drying obtain porous carbon materials at last.The present invention is of very high actual application value.
The porous carbon materials of described high-specific surface area of this patent and narrow pore distribution, it is prepared by following steps:
(1) pine needle is clean, dry, under inert atmosphere protection,, then carbonized product is pulverized the back screening in 300～500 ℃ of carbonizations 3～4 hours;
(2) carbonized product that obtains is joined in alkaline water/ethanolic soln, behind the ultra-sonic dispersion 1～5 minute, flooded 20～24 hours, under 50～80 ℃ with the solvent evaporate to dryness, under inert atmosphere protection, activate 15～150 minutes under 650～850 ℃ afterwards, naturally cool to room temperature;
(3) product being washed with water until the pH of washings value again is 7～8, utilizes diluted acid to soak 1～4 hour, and being washed with water to washings pH value again is 6～7, again at 80～120 ℃ of air dryings, obtains the porous carbon materials of high-specific surface area and narrow pore distribution at last.
Inert atmosphere described in the above-mentioned steps is under nitrogen or argon gas atmosphere, further is under 99.9% nitrogen or argon gas atmosphere; Screening is to screen with 20～50 mesh sieve; The alkali consumption of every gram carbonized product is 2～8 grams, is immersed in 10～50 milliliters of alkaline water/ethanolic solns, and further, the alkali consumption of every gram carbonized product is 6～7 grams;
Alkaline water/ethanolic soln described in the above-mentioned steps is water/ethanolic soln of KOH or NaOH, and water and alcoholic acid volume ratio are 1～4: 1 in water/ethanolic soln.
Diluted acid described in the above-mentioned steps is that concentration is dilute hydrochloric acid or the rare nitric acid of 0.05～0.3mol/L, and preferred soak time is 30～120 minutes.
That the present invention utilizes is general, cheap, a large amount of, reproducible biological material pine needle is as raw material, handles making porous carbon materials through simple chemical activation.This porous carbon materials has very big specific surface area and (reaches as high as 3545m
2/ g), and have narrower pore size distribution (1～2 nanometer), and also the specific surface area of porous carbon materials can also be regulated by the consumption and the activation temperature of regulating KOH or NaOH.The starting material of using in this inventive method are extremely cheap and easy to get, in the preparation process, being different from great majority is the carbonized product of raw material with biomass, the carbonized product that we make has loose structure, our activator of use is to add with the solution impregnation form simultaneously, therefore activator can farthest, full and uniformly be distributed in the carbonized product, carbonized product can fully be contacted with activator, thereby can fully activate and homogeneous reaction.In traditional porous activated carbon preparation process, usually be that the char-forming material after pulverizing is directly mixed stirring with solid activating agent, this method tends to cause the activator in the carbonized product to disperse inhomogeneous, and then cause in the priming reaction process activation undesirable to carbonized product, cause the product pore size distribution inhomogeneous and specific surface area is low.In carbonization process, the many chemical bond ruptures in the pine needle form water, by products such as tar, and main in reactivation process what take place is chemical reaction between dehydrogenation reaction and activator and the carbonized product.
The preparation method of porous carbon materials is low for equipment requirements among the present invention, consuming time few, preparation process is simple, main by product in the preparation process is a tar, in addition, be that the washings that produces in the preparation process of activator is the solution that is rich in potassium ion with KOH, can be used as agriculture potash fertilizer use through simple the processing.Used starting material wide material sources are not subjected to territorial restrictions in the invention, and are with low cost, and renewable, utilize this material preparation porous carbon materials can save a large amount of timber and high-quality coal.
The present invention extremely is applicable to industrial mass production, has very important significance to saving China's Forest Resources and coal resources.Be directed to the current situation that can not make full use of pine needle especially---as lighting a fire material or arbitrarily abandon, the present invention can effectively solve this wasting phenomenon, for opening up a kind of new income source in the mountain area.The porous carbon materials that the present invention obtains the storage of gas with separate, the electrode materials of battery or electric capacity, catalyzer or carrier in the number of chemical reaction, sewage disposal, fields such as precious metal recovery all can have broad application prospects.
Description of drawings
Fig. 1: the nitrogen adsorption/desorption isotherm of porous carbon materials (77K);
Fig. 2: the pore size distribution curve of porous carbon materials;
Fig. 3: the high-resolution-ration transmission electric-lens photo of porous carbon materials;
Fig. 4: the relation of the specific surface area of porous carbon materials and KOH quality;
Fig. 5: the specific surface area of porous carbon materials and the relation of activation temperature (KOH, 6g);
Fig. 6: the specific surface area of porous carbon materials and the relation of soak time (KOH, 6g, activation temperature, 800 ℃).
We are to the pine needle being the sign (embodiment 13) that the porous carbon materials of feedstock production has carried out structure and character.
Fig. 1 is the nitrogen adsorption/desorption isotherm of porous carbon materials when 77K, is the typical type I curve, and does not have hysteresis loop to exist, and shows and contains a large amount of micropores in the porous carbon materials.
Fig. 2 is the pore size distribution curve of porous carbon materials, illustrates that the pore size distribution of this porous carbon materials is narrow, mainly is distributed between 1～2 nanometer.
Fig. 3 is the high-resolution-ration transmission electric-lens photo of porous carbon materials, in photo, can clearly see the micropore that exists in the porous carbon materials between 1～2 a large amount of nanometers.
Fig. 4 is the specific surface area of porous carbon materials and the relation of KOH quality.As we know from the figure, be that the KOH quality is between 6～7g under the condition of 800 ℃ and 120min at activation temperature and soak time, the specific surface area of porous carbon materials can reach 3000m
2More than/the g, reach as high as 3302m
2/ g.
Fig. 5 is that (KOH, 6g), activation temperature is 800 ℃ as can be seen for the specific surface area of porous carbon materials and the relation of activation temperature.
Fig. 6 is the specific surface area of porous carbon materials and the relation of soak time (KOH, 6g, activation temperature, 800 ℃), as can be seen at soak time in 30～120min scope, the specific surface area of porous carbon materials can reach 3000m
2More than/the g, reach as high as 3545m
2/ g.
Embodiment
Embodiment 1:
Pine needle is cleaned oven dry.Under 99.9% protection of nitrogen gas, 450 ℃ of following carbonizing treatment 3 hours obtain carbonized product and tar, then carbonized product are pulverized, and screen with 35 purpose sieves.2 gram KOH are dissolved in the mixing solutions of 35mL water/ethanol (volume ratio 2.5: 1); then 1 gram carbonized product is joined in the above-mentioned system; ultra-sonic dispersion 5 minutes; flooded 24 hours; at last under 70 ℃ with the solvent evaporate to dryness; afterwards remaining mixture is activated 120 minutes under under rare gas element (nitrogen or the argon gas 99.9%) protection 800 ℃; naturally cool to room temperature; product is washed with water until the pH of washings value again near 8; utilize 0.1mol/L dilute hydrochloric acid to soak 3 hours, be washed with water to washings pH value again, then 100 ℃ of air dryings 7 hours near 7; obtain porous carbon materials at last, the specific surface area of material is 1852m
2/ g, pore size are mainly 1.5 nanometers.
Embodiment 2:
Experimental technique is with embodiment 1, and just the consumption with activator KOH becomes 3 grams, obtains porous carbon materials equally, and the specific surface area of material is 1900m
2/ g, pore size are mainly 1.5 nanometers.
Embodiment 3:
Experimental technique is with embodiment 1, and just the consumption with activator KOH becomes 4 grams, obtains porous carbon materials equally, and the specific surface area of material is 2014m
2/ g, pore size are mainly 1.5 nanometers.
Embodiment 4:
Experimental technique is with embodiment 1, and just the consumption with activator KOH becomes 5 grams, obtains porous carbon materials equally, and the specific surface area of material is 2044m
2/ g, pore size are mainly 1.5 nanometers.
Embodiment 5:
Experimental technique is with embodiment 1, and just the consumption with activator KOH becomes 6 grams, obtains porous carbon materials equally, and the specific surface area of material is 3302m
2/ g, pore size are mainly 1.5 nanometers.
Embodiment 6:
Experimental technique is with embodiment 1, and just the consumption with activator KOH becomes 7 grams, obtains porous carbon materials equally, and the specific surface area of material is 3205m
2/ g, pore size are mainly 1.5 nanometers.
Embodiment 7:
Experimental technique is with embodiment 1, and just the consumption with activator KOH becomes 8 grams, obtains porous carbon materials equally, and the specific surface area of material is 2823m
2/ g, pore size are mainly 1.5 nanometers.
Embodiment 8:
Experimental technique just becomes 650 ℃ with activation temperature with embodiment 5, obtains porous carbon materials equally, and the specific surface area of material is 1846m
2/ g, pore size are mainly 1.5 nanometers.
Embodiment 9:
Experimental technique just becomes 700 ℃ with activation temperature with embodiment 5, obtains porous carbon materials equally, and the specific surface area of material is 2991m
2/ g, pore size are mainly 1.5 nanometers.
Embodiment 10:
Experimental technique just becomes 750 ℃ with activation temperature with embodiment 5, obtains porous carbon materials equally, and the specific surface area of material is 3105m
2/ g, pore size are mainly 1.5 nanometers.
Embodiment 11:
Experimental technique just becomes 850 ℃ with activation temperature with embodiment 5, obtains porous carbon materials equally, and the specific surface area of material is 3027m
2/ g, pore size are mainly 1.5 nanometers.
Embodiment 12:
Experimental technique just becomes 30min with soak time with embodiment 5, obtains porous carbon materials equally, and the specific surface area of material is 2966m
2/ g, pore size are mainly 1.5 nanometers.
Embodiment 13:
Experimental technique just becomes 45min with soak time with embodiment 5, obtains porous carbon materials equally, and the specific surface area of material is 3045m
2/ g, pore size are mainly 1.5 nanometers.
Embodiment 14:
Experimental technique just becomes 60min with soak time with embodiment 5, obtains porous carbon materials equally, and the specific surface area of material is 3120m
2/ g, pore size are mainly 1.5 nanometers.
Embodiment 15:
Experimental technique just becomes 75min with soak time with embodiment 5, obtains porous carbon materials equally, and the specific surface area of material is 3545m
2/ g, pore size are mainly 1.5 nanometers.
Embodiment 16:
Experimental technique just becomes 90min with soak time with embodiment 5, obtains porous carbon materials equally, and the specific surface area of material is 3342m
2/ g, pore size are mainly 1.5 nanometers.
Embodiment 17:
Experimental technique just becomes 105min with soak time with embodiment 5, obtains porous carbon materials equally, and the specific surface area of material is 3253m
2/ g, pore size are mainly 1.5 nanometers.
Embodiment 18:
Experimental technique just becomes 135min with soak time with embodiment 5, obtains porous carbon materials equally, and the specific surface area of material is 2956m
2/ g, pore size are mainly 1.5 nanometers.
Embodiment 19:
Experimental technique just becomes 150min with soak time with embodiment 5, obtains porous carbon materials equally, and the specific surface area of material is 2655m
2/ g, pore size are mainly 1.5 nanometers.
Claims (7)
1. the preparation method of the porous carbon materials of high-specific surface area and narrow pore distribution, its step is as follows:
(1) pine needle is clean, dry, under inert atmosphere protection,, then carbonized product pulverizing back is screened with 20～50 mesh sieve in 300～500 ℃ of carbonizations 3～4 hours;
(2) carbonized product that obtains is joined in alkaline water/ethanolic soln, behind the ultra-sonic dispersion 1～5 minute, flooded 20～24 hours, under 50～80 ℃ with the solvent evaporate to dryness, under inert atmosphere protection, activate 15～150 minutes under 650～850 ℃ afterwards, naturally cool to room temperature;
(3) product being washed with water until the pH of washings value again is 7～8, utilizes diluted acid to soak 1～4 hour, and being washed with water to washings pH value again is 6～7, at 80～120 ℃ of air dryings, obtains porous carbon materials at last again;
Wherein, the alkali consumption of every gram carbonized product is 2～8 grams, is immersed in 10～50 milliliters of alkaline water/ethanolic solns; Water and alcoholic acid volume ratio are 1～4: 1 in water/ethanolic soln.
2. the preparation method of the porous carbon materials of high-specific surface area as claimed in claim 1 and narrow pore distribution is characterized in that: inert atmosphere is under nitrogen or argon gas atmosphere.
3. the preparation method of the porous carbon materials of high-specific surface area as claimed in claim 2 and narrow pore distribution is characterized in that: inert atmosphere is under 99.9% nitrogen or argon gas atmosphere.
4. the preparation method of the porous carbon materials of high-specific surface area as claimed in claim 1 and narrow pore distribution is characterized in that: the alkali consumption of every gram carbonized product is 6～7 grams.
5. as the preparation method of the porous carbon materials of any one described high-specific surface area of claim 1～4 and narrow pore distribution, it is characterized in that: alkaline water/ethanolic soln is water/ethanolic soln of KOH or NaOH.
6. as the preparation method of the porous carbon materials of any one described high-specific surface area of claim 1～4 and narrow pore distribution, it is characterized in that: diluted acid is that concentration is dilute hydrochloric acid or the rare nitric acid of 0.05～0.3mol/L.
7. as the preparation method of the porous carbon materials of any one described high-specific surface area of claim 1～4 and narrow pore distribution, it is characterized in that: soak time is 30～120 minutes.
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