CN101054174A - Method of preparing biomass high specific surface micro-pore carbon material - Google Patents
Method of preparing biomass high specific surface micro-pore carbon material Download PDFInfo
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Abstract
The present invention belongs to the preparation field of micropore carbon material, and relates to the preparation method for micropore carbon material with high specific surface area and narrow pore distribution by biomass. The biomass is cleaned and cut into subparagraph with a length of 1~3 centimeter, and then is subjected to carbonizing at 300~500 DEG C for 3~4 hours in the presence of inert atmosphere. The obtained carbonizing product is immerged into an alkaline solution for 20~24 hours until the carbonizing product is totally wetting, and then the carbonizing product is separated from the solution and is activated for 1.5~3 hours at 700~800 DEG C in the presence of inert atmosphere, and then is scrubbed by water until the pH value of the scrub solution is 7~8, and then the carbonizing product is immerged into a diluted acid solution for 4~5 hours and is scrubbed by water until the pH value of the scrub solution is 6~7, finally, the carbonizing product is dried at 80~120 DEG C to obtain micropore carbon material. The preparation method for the present invention has the advantages of that the preparation process is simple, the raw material is cheap and abundant, the preparation condition is free from zone limit; besides, the preparation method is adapted to industrial production.
Description
Technical field
The invention belongs to the micro-pore carbon material preparation field, particularly a kind of method of utilizing biomass to prepare micro-pore carbon material is specifically related to utilize the biomass preparation to provide the micro-pore carbon material of high-specific surface area and narrower pore distribution.
Background technology
Micro-pore carbon material is because its special pore passage structure and higher specific surface area make it that very important effect be arranged in daily life.Now, the micro-pore carbon material storage that has been widely used in gas with separate, electrode materials, number of chemical catalyst for reaction or the support of the catalyst of battery or electric capacity, sewage disposal, precious metal recovery etc.On market, more common micro-pore carbon material is a gac, it is that to utilize charcoal, various shell and fat coal etc. be raw material, by physics and chemical process to raw material carry out fragmentation, sieve, series of processes processing and manufacturing such as catalyst activation, rinsing, oven dry and screening forms.But shortcomings such as conventional gac exists the pore size distribution heterogeneity, and specific surface area is less, these make gac be very restricted in application facet.In order to overcome the shortcoming of gac, people have developed activated carbon fiber, though this has overcome those shortcomings of gac to a great extent, but having produced series of new problems again---complicated process of preparation, cost height and the performance development of activated carbon fiber get perfect not enough, these have all seriously restricted the practical application of activated carbon fiber, therefore, gac also has overwhelming superiority in productive life.
In the preparation process of micro-pore carbon material, topmost step is a reactivation process, activation method is divided into physical activation method and chemical activation method two big classes usually: 1. physical activation method is with water vapour, and materials such as carbonic acid gas activate carbonizing production under inert atmosphere protection as activator; 2. chemical activation method is with the oxyhydroxide of basic metal or alkaline-earth metal such as KOH, NaOH, Ca (OH)
2And ZnCl
2, CaCl
2, H
2SO
4, H
3PO
4Under inert atmosphere protection, carbide is activated as activator Deng chemical reagent.
The gac that makes with physical activation method mainly is a micro-pore carbon material, though the pore distribution of the gac that makes is narrower, result of use is preferably arranged in various Application Areass, but the specific surface area of micro-pore carbon material prepared by this method is lower, and these micro-pore carbon materials also do not reach the ideal effect.Though be greatly improved with the specific surface area of the activated carbon of chemical activation method preparation gac with respect to the physical activation method preparation, result of use aspect a lot of is also relatively good, but the pore distribution of the gac of chemical activation method preparation is generally all very wide, and this makes the gac of chemical activation method preparation be subjected to certain restriction in the application aspect some (as gas delivery).
The present invention is the raw material of preparation microporous carbon with reproducible biological material, utilize chemical activation method to activate micro-pore carbon material, flood in basic solution by carbonizing production, in inert atmosphere, carry out activation treatment then and obtain the fine micro-pore carbon material biological material.At present; it is to utilize timber and high-quality coal as starting material that very most high grade activated carbon is arranged on the domestic market; will consume a large amount of timber and coal aspect the preparation high grade activated carbon every year; and the forest coverage of China is not very high; though China is coal big country; but coal is a kind of Nonrenewable resources, and present countries in the world all are faced with the crisis of fossil energy.Therefore, can substitute the renewable starting material that timber and coal prepare the high-quality micro-pore carbon material, will and reduce fossil energy consumption and play very big effect the wood protection of China so if search out.
Summary of the invention
The technical problem to be solved in the present invention is the deficiency that will overcome the current background technology, utilizes simple chemical activation method to make to have high-specific surface area, the micro-pore carbon material of narrower pore distribution.The present invention has very high actual application value.
The present invention utilizes general, the most cheap maize straw in rural area to be starting material, with stalk charing under inert atmosphere, then carbonizing production is flooded for some time in basic solution, alkali evenly is distributed in the carbonizing production fully, then carbonizing production is taken out from solution, and in inert atmosphere, carry out activation treatment, through washing, acid treatment is washed again, processes such as drying obtain micro-pore carbon material at last.
The detailed process of preparation micro-pore carbon material is as follows:
Stalk is cleaned, cut into the segment of 1～3 cm long, under inertia (nitrogen or argon gas 99.9%) atmosphere protection,, obtain carbonizing production, obtain tar at the tube furnace two ends at the tube furnace middle part in 300～500 ℃ of charings 3～4 hours.Then the carbonizing production that obtains is immersed in the basic solution (KOH or NaOH) of 2～13mol/L (every gram carbonizing production is immersed in 20～25 ml solns) soaked into until carbonizing production in 20～24 hours fully; utilize sieve with carbonizing production and solution separating; under under rare gas element (nitrogen or the argon gas 99.9%) protection 700～800 ℃, activate 1.5～3 hours afterwards; naturally be cooled to room temperature; the pH value that product water (or deionized water) is washed till washings is 7～8; utilize concentration 0.05～0.2mol/L diluted acid (hydrochloric acid or nitric acid) to soak 4～5 hours; again water (or deionized water) wash to washings pH value be 6～7; dry under 80～120 ℃ at last, obtain the described high specific surface micro-pore carbon material of this patent.
The present invention utilizes general, a large amount of, reproducible biomass maize straws as raw material, makes micro-pore carbon material through simple chemical activation.This carbon material has very big specific surface area and (is up to 3247m
2/ g), and have narrower pore size distribution (1～2nm).The raw material of using in this method is extremely cheap, in the preparation process, the carbonizing production that is different from most of raw materials, the carbonizing production that we make mainly is loose reticulated structure, our activator of use is to add with the solution impregnation form simultaneously, therefore activator can very evenly be distributed in the carbonizing production fully, and it is fully even with reaction that carbonizing production can be activated in reactivation process.In the microporous carbon preparation process of majority, the adding of activator is earlier carbonizing production to be pulverized, and directly mixes, stirs with solid activating agent then, therefore, tend to cause activator skewness in carbonizing production, and then cause the product pore size distribution behind the priming reaction inhomogeneous.In carbonization process, many chemical bond ruptures in the main component in the stalk form water, by products such as tar, and mainly be that what to take place is chemical reaction between dehydrogenation reaction and activator and the carbide in reactivation process.
Method among the present invention is low for equipment requirements, consuming time few, preparation process is simple, main by product in the reaction is a tar, tar is a kind of very usury product that is worth that has equally, the washings of micro-pore carbon material is the solution that is rich in potassium ion, is exactly good agricultural potash fertilizer through simple the processing.In addition, raw materials used wide material sources are not subjected to territorial restrictions, and are cheap, and raw material is renewable resources, and this will save a large amount of timber and high-quality coal.Adopt the method for KOH (or NaOH) solution impregnation to dissolve remaining tar, and KOH (or NaOH) can be distributed in the carbon material better, this is more even with carbonizing production and solid activating agent mixed grinding method than traditional, saves operation.We have abundant pore texture by the micro-pore carbon material of preparation, and very big specific surface area (is higher than 3000m
2/ g), and narrower pore size distribution (1～2nm), and the specific surface area of micro-pore carbon material can also be regulated by the concentration of regulating KOH (or NaOH) solution.
Therefore, the present invention extremely is applicable to industrial mass production, and China's saving forest reserves and coal resources are had very important significance.Be directed to current rural area especially, most of maize straw is applied to heating, do animal feed, the present invention can effectively solve this wasting phenomenon, for opening up a kind of new income source in the rural area.Because the micro-pore carbon material that the present invention obtains has higher specific surface area and narrower pore size distribution, so its storage of gas with separate, the electrode materials of battery or electric capacity, catalyzer or carrier in the number of chemical reaction, sewage disposal, all can there be actual application value in fields such as precious metal recovery.
Description of drawings
Fig. 1: the nitrogen adsorption/desorption isotherm of micro-pore carbon material;
Fig. 2: the pore size distribution curve of micro-pore carbon material;
Fig. 3: the high-resolution-ration transmission electric-lens photo of micro-pore carbon material;
Fig. 4: the relation curve of the specific surface area of micro-pore carbon material and KOH strength of solution.
We have carried out the sign (embodiment 12) of some structures and character to the micro-pore carbon material of gained.Shown in Figure 1, be the nitrogen adsorption/desorption isotherm of micro-pore carbon material, the absorption/desorption isotherm among the figure is a typical type I, and does not have hysteresis loop, shows that this micro-pore carbon material contains a large amount of micropores.Fig. 2 is the graph of pore diameter distribution of micro-pore carbon material.Pore size distribution curve illustrates that the pore size distribution of this micro-pore carbon material is narrow, mainly is distributed between 1～2nm.Fig. 3 is the high-resolution-ration transmission electric-lens photo of micro-pore carbon material, and in photo, we can be clear that also the aperture of micro-pore carbon material mainly is to be distributed between 1～2nm.Fig. 4 is the specific surface area of micro-pore carbon material and the relation of used KOH strength of solution.As we know from the figure, when KOH concentration is controlled between 8～13mol/L, the specific surface area of micro-pore carbon material can reach 3000m
2/ g ranges up to 3247m
2/ g.
Embodiment
Below with regard to embodiment the present invention is further set forth:
Embodiment 1:
With the maize straw wash clean, dry, be cut into the segment of 1.5 cm long then.Under protection of nitrogen gas, 400 ℃ of following charings 3 hours obtain carbonizing production and byproduct tar.The carbonizing production that obtains was immersed in the KOH solution of 1mol/L (the every gram carbonizing production of 25 ml solns) 24 hours.The carbonizing production that takes out is activated 2 hours down at 750 ℃, then, successively with deionized water wash to washings pH=7, use dilute hydrochloric acid (0.1mol/L) to soak then 5 hours, use the deionized water wash product until washings pH=7 again, obtain micro-pore carbon material after 3 hours carrying out drying under 100 ℃, the specific surface area of material is 880m
2/ g, pore size is mainly 1.4nm.
Embodiment 2:
Experimental technique is with embodiment 1, and just the concentration with activator KOH solution becomes 2mol/L, obtains micro-pore carbon material equally, and the specific surface area of material is 1300m
2/ g, pore size is mainly 1.4nm.
Embodiment 3:
Experimental technique is with embodiment 1, and just the concentration with activator KOH solution becomes 3mol/L, obtains micro-pore carbon material equally, and the specific surface area of material is 1412m
2/ g, pore size is mainly 1.4nm.
Embodiment 4:
Experimental technique is with embodiment 1, and just the concentration with activator KOH solution becomes 4mol/L, obtains micro-pore carbon material equally, and the specific surface area of material is 1526m
2/ g, pore size is mainly 1.4nm.
Embodiment 5:
Experimental technique is with embodiment 1, and just the concentration with activator KOH solution becomes 5mol/L, obtains micro-pore carbon material equally, and the specific surface area of material is 1580m
2/ g, pore size is mainly 1.4nm.
Embodiment 6:
Experimental technique is with embodiment 1, and just the concentration with activator KOH solution becomes 6mol/L, obtains micro-pore carbon material equally, and the specific surface area of material is 2201m
2/ g, pore size is mainly 1.4nm.
Embodiment 7:
Experimental technique is with embodiment 1, and just the concentration with activator KOH solution becomes 7mol/L, obtains micro-pore carbon material equally, and the specific surface area of material is 2645m
2/ g, pore size are mainly 1.4 nanometers.
Embodiment 8:
Experimental technique is with embodiment 1, and just the concentration with activator KOH solution becomes 8mol/L, obtains micro-pore carbon material equally, and the specific surface area of material is 2900m
2/ g, pore size is mainly 1.4nm.
Embodiment 9:
Experimental technique is with embodiment 1, and just the concentration with activator KOH solution becomes 9mol/L, obtains micro-pore carbon material equally, and the specific surface area of material is 2991m
2/ g, pore size is mainly 1.4nm.
Embodiment 10:
Experimental technique is with embodiment 1, and just the concentration with activator KOH solution becomes 10mol/L, obtains micro-pore carbon material equally, and the specific surface area of material is 3247m
2/ g, pore size is mainly 1.4nm.
Embodiment 11:
Experimental technique is with embodiment 1, and just the concentration with activator KOH solution becomes 11mol/L, obtains micro-pore carbon material equally, and the specific surface area of material is 3103m
2/ g, pore size is mainly 1.4nm.
Embodiment 12:
Experimental technique is with embodiment 1, and just the concentration with activator KOH solution becomes 12mol/L, obtains micro-pore carbon material equally, and the specific surface area of material is 3015m
2/ g, pore size is mainly 1.4nm.
Embodiment 13:
Experimental technique is with embodiment 1, and just the concentration with activator KOH solution becomes 13mol/L, obtains micro-pore carbon material equally, and the specific surface area of material is 2920m
2/ g, pore size is mainly 1.4nm.
Claims (8)
1; the preparation method of biomass high specific surface micro-pore carbon material; it comprises the steps: biological material is cleaned; cut into the segment of 1～3 cm long; under inert atmosphere protection in 300～500 ℃ of charings 3～4 hours; then the carbonizing production that obtains being immersed in the basic solution 20～24 hours soaks into fully until carbonizing production; with carbonizing production and solution separating; under protection of inert gas, activate 1.5～3 hours down afterwards in 700～800 ℃; naturally be cooled to room temperature; with product wash to the pH value be 7～8; utilize diluted acid to soak 4～5 hours; again washings is washed to the pH value be 6～7, obtain high specific surface micro-pore carbon material 80～120 ℃ of following dryings at last.
2, the preparation method of biomass high specific surface micro-pore carbon material as claimed in claim 1 is characterized in that: biological material is a maize straw.
3, the preparation method of biomass high specific surface micro-pore carbon material as claimed in claim 1 is characterized in that: inert atmosphere is under nitrogen or argon gas atmosphere.
4, the preparation method of biomass high specific surface micro-pore carbon material as claimed in claim 1 is characterized in that: basic solution is KOH or NaOH.
5, the preparation method of biomass high specific surface micro-pore carbon material as claimed in claim 1 is characterized in that: every gram carbonizing production is immersed in 20～25 milliliters of basic solutions.
6, the preparation method of biomass high specific surface micro-pore carbon material as claimed in claim 1 is characterized in that: diluted acid is that concentration is dilute hydrochloric acid or the rare nitric acid of 0.05～0.2mol/L.
7, as the preparation method of any one described biomass high specific surface micro-pore carbon material of claim 1-6, it is characterized in that: the concentration of alkaline solution is 2～13mol/L.
8, the preparation method of biomass high specific surface micro-pore carbon material as claimed in claim 7 is characterized in that: the concentration of alkaline solution is 8～13mol/L.
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