CN106423065B - A kind of post-processing approach improving the effective pore specific surface area of charcoal - Google Patents
A kind of post-processing approach improving the effective pore specific surface area of charcoal Download PDFInfo
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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Abstract
The present invention relates to a kind of post-processing approach for improving the effective pore specific surface area of charcoal, belong to chemically or physically method and technology field.Charcoal is put into pyrolysis oven, the nitrogen and air gas mixture of certain volume ratio are passed through with certain flow, after being heat-treated a period of time, obtained solid object and appropriate activated alumina ball are put into togerther in water, after stirring expanding treatment under room temperature for a period of time, activated alumina ball is taken out, solids is filtered out, washing, obtains product after drying.Invention is applied to charcoal to post-process, charcoal can be significantly improved to the Adsorption efficiency of the organic pollutants such as pesticide.
Description
Technical field
The present invention relates to a kind of post-processing approach for improving the effective pore specific surface area of charcoal, belong to chemically or physically method
Technical field.
Background technique
It is raw material that charcoal, which is using agricultures, woods, aquaculture residue or plant residues such as sawdust, stalk, feces of livestock and poultry,
The high carbonaceous solids product of a kind of stable black being pyrolyzed under certain temperature (300~800 DEG C) produces to improve charcoal
The yield of product, pyrolytic reaction carry out (ZL201310218454.1 usually in the protective atmospheres such as nitrogen；ZL
201410120718.4).Due to the exclusive structure and function feature of charcoal, repaired in carbon dioxide sequestration, soil improvement, environment
The multiple fields such as multiple, resource recycling show wide application prospect.Especially, charcoal has microcellular structure abundant
With biggish specific surface area, it is a kind of cheap and efficient adsorbent, it is a variety of that aromatic hydrocarbons, pesticide, dyestuff, antibiotic etc. can be adsorbed
Organic pollutant has broad application prospects in the adsorption treatment technology of these pollutants.
But it uses in the obtained charcoal of conventional pyrolysis technique based on micropore (aperture < 2nm) structure, and a large amount of
Micropore is in irregular slit-shaped, causes charcoal insufficient to the adsorption capacity of the pollutants such as pesticide, antibiotic.The reason is that,
It is different from the small molecules aromatic hydrocarbons pollutant such as benzene, toluene, nitrobenzene, the organic molecules such as most pesticides, antibiotic it is opposite
Molecular mass is higher, is often greater than 250g/mol, if the relative molecular mass of herbicide tribenuron-methyl is 395g/mol, their molecule
Size is usually more than 1nm.This kind of molecular dimension hardly enters the too small charcoal in aperture in the organic pollutant molecule of 1nm or more
In micropore, and aperture is belonged to effective hole that adsorption capacity plays a leading role (Dong Lihua waits water supply in the mesoporous of 1.7nm or more
Draining, 2014,40:91-94).That is, a large amount of micropore surfaces in charcoal can not be by organic matters such as pesticide, antibiotic
Molecule utilizes, and contributes very little to this type organic is adsorbed.Therefore, adsorption energy of the charcoal to pollutants such as herbicide, antibiotic
Power depends primarily on the size of effective hole (aperture is 1.7~50nm) specific surface area in charcoal.
In view of this, it is necessary to which developing effective charcoal post-processing technology, (aperture is to improve effective hole in charcoal
1.7~50nm) specific surface area, with prepare to the common organic pollutant such as pesticide, antibiotic have more high absorption capacity life
Object charcoal, to expand purposes of the charcoal in adsorption treatment pollutant while improve removal efficiency.
Based on this, the application is made.
Summary of the invention
For the drawbacks described above in the presence of the processing of existing charcoal, the application, which provides one kind, can be improved the effective hole of charcoal
The post-processing approach of (aperture is 1.7~50nm) specific surface area, for improving charcoal to organic pollutants such as pesticide, antibiotic
Adsorption efficiency.
To achieve the above object, the technical solution that the application takes is as follows:
A kind of post-processing approach improving the effective pore specific surface area of charcoal, charcoal is put into heat-treatment furnace, with one
Constant flow is passed through the nitrogen and air gas mixture of certain volume ratio, after being heat-treated a period of time, by obtained solid object and in right amount
Activated alumina ball is put into togerther in water, room temperature expanding treatment for a period of time after, take out activated alumina ball, filter out solids,
The charcoal product refined after washing, drying.
Further, as preferred:
The biology carbon feedstock is biomass using sawdust etc. rich in cellulose, lignin etc. as raw material, through limit oxygen pyrolysis
The high carbonaceous solids product of preparation.
The heat-treatment furnace selects tube furnace, and it is 5:1 that mixed gas group therein, which becomes nitrogen and the volume ratio of air,
~1:5, the flow of mixed gas are that (size depends on boiler tube model to 3~10 boiler tube volumes, with Φ 8cm × 100cm per hour
For boiler tube, boiler tube volume is 5L), heat treatment temperature is 200~500 DEG C, and soaking time is 0.5~6h.It is furthermore preferred that institute
The volume ratio of the nitrogen and air stated is 2:1~1:2, and the flow of mixed gas is 4~7 boiler tube volumes per hour, heat treatment
Temperature is 300~400 DEG C, and soaking time is 1~3h.
The room temperature expanding treatment is to be put into togerther the solids after heat treatment in water with activated alumina ball to stir.
The partial size of activated alumina ball used is 1~5mm, and the mass ratio of activated alumina ball and charcoal is 5:1~1:1, water with
The mass ratio of activated alumina ball is 30:1~5:1.The room temperature expanding treatment time is 2~72h.It is furthermore preferred that described
Activated alumina ball and charcoal mass ratio be 3:1~1:1.
A kind of post-processing approach of effective pore specific surface area of raising charcoal provided herein, specifically: it will be biological
Charcoal is put into tube furnace, is passed through volume ratio with the flow of 3~10 boiler tube volumes per hour as the nitrogen and air of 5:1~1:5
Mixed gas, while being heated to 200~500 DEG C, after being heat-treated 0.5~6h, by activated alumina ball that partial size is 1~5mm and
Charcoal 5:1~1:1 in mass ratio is put into togerther in water, after stirring 2~72h under room temperature, takes out activated alumina ball, is filtered out solid
Body object, washing, the charcoal product refined after being dried at 90~120 DEG C.
It the working principle of the charcoal post-processing approach of the application and has the beneficial effect that:
1) the application is heat-treated biological carbon feedstock in the mixed gas of nitrogen and air, by the group for controlling mixed gas
At and flow, on the one hand, partial oxidation contained in air during heat treatment in charcoal micro-pore wall occur ablation
Partial pore is expanded as effective hole (aperture is 1.7~50nm), on the other hand, is also beneficial to that charcoal will be remained in by effect
In be not carbonized organic matter fractions oxidation.
2) the application stirs expanding treatment one together with the solids after mixed gas heat treatment using activated alumina ball
The section time, the organic matter that is not carbonized being oxidized in charcoal can be transferred in activated alumina ball, to improve charcoal production
Effective pore specific surface area of product.
3) in the application, the activated alumina ball for room temperature expanding treatment can be reused after high temperature sintering, cost
It is low, high recycling rate.
4) (compare table for 1.7~50nm) in aperture in the effective hole for using technical solution of the present invention to be remarkably improved charcoal product
Area and ratio, effectively pore specific surface area can be improved 3.7~5.0 times under optimum condition, effective hole ratio can be improved to 30% with
On.
Detailed description of the invention
Fig. 1 is removal curve (25 DEG C) of several charcoal samples to herbicide tribenuron-methyl.
Specific embodiment
Comparative example: the charcoal prepared in a usual manner
Weighing 30g sawdust is biomass material, is put into box pyrolysis oven, is passed through nitrogen, protects after being heated to 600 DEG C
Warm 6h takes out obtained solid thermal decomposition product, after drying at 105 DEG C after washing, obtains 7.95g charcoal, sample number into spectrum is
0#。
Following embodiment using charcoal prepared by comparative example as process object, be heat-treated used in mixed gas group
At with flow, heat treatment condition, the comparative experiments of activated alumina ball expanding treatment.
Embodiment 1-7: the influence of the effective pore specific surface area of the pairs of charcoal of difference mixed gas group when heat treatment
The 6g charcoal prepared in comparative example is taken, (boiler tube model Φ 8cm × 100cm, boiler tube volume are put into tube furnace
For 5L), nitrogen and air gas mixture are passed through with the flow of 25L per hour, 1h is kept the temperature after being heated to 400 DEG C, is heat-treated
Obtained solid object and 12g activated alumina ball (partial size is 1~3mm) are put into togerther in 150mL water, after stirring for 24 hours under room temperature, are taken
Activated alumina ball out filters out solids, washing, the charcoal finished product refined after drying at 105 DEG C, using specific surface
Long-pending and Porosimetry test sample specific surface area and pore structure.Referring to test method general in industry, with N2For absorption
Matter measures isotherm adsorption data accorded at 77K, calculates the full specific surface area of sample using BET method, calculates sample using BJH method
Effective hole (1.7~50nm) specific surface area calculates having for sample according to the percentage that effective pore specific surface area accounts for full specific surface area
Hole ratio is imitated, referring specifically to shown in table 1.
Effective hole ratio of prepared charcoal finished product when being heat-treated in the mixed gas of different volumes ratio of table 1
According in table 1 as a result, when other treatment conditions are identical, in mixed gas, air proportion is mentioned
Height, the ratio that effective pore specific surface area of refined biological charcoal product accounts for full specific surface area are gradually increased.Illustrate contained in air
Oxygen produces ablation effect to the micro-pore wall in charcoal, and partial pore is made to expand as effective hole of 1.7~50nm of aperture.
In volume ratio >=1:1 of nitrogen and air, full the specific surface area of refined biological charcoal product and effective pore specific surface area are with air
The increase of proportion and improve.But volume ratio shared by air is continued growing, the full specific surface area of refined biological charcoal product
With effective pore specific surface area with will gradually decline.Illustrate that the air content in mixed gas is excessively high, charcoal product will be caused
Pore structure is collapsed, that is, so-called excessive ablation occurs, is unfavorable for the raising of charcoal specific surface area.
According to data in table 1, when the volume ratio of nitrogen and air is 5:1-1:5, gained refined biological charcoal product has
Effect pore specific surface area can reach 80m2/g.Further preferably, when the volume ratio of nitrogen and air is 2:1-1:2, gained purification
The full specific surface area of charcoal product can reach 300m2/ g or more, effective pore specific surface area can reach 100m2/ g or more, effective hole
Ratio is 35% or more.
Embodiment 8-13: influence of the flow of mixed gas to the effective pore specific surface area of charcoal
The 6g charcoal prepared in comparative example is taken, (boiler tube model Φ 8cm × 100cm, boiler tube volume are put into tube furnace
For 5L), being passed through volume ratio is 1:1 nitrogen and air gas mixture, and 1h is kept the temperature after being heated to 400 DEG C, and heat treatment gained is solid
Body object and 12g activated alumina ball (partial size is 1~3mm) are put into togerther in 150mL water, after stirring for 24 hours under room temperature, take out activity
Alumina balls filter out solids, washing, the charcoal finished product refined after drying at 105 DEG C, using in embodiment 1-7
The method analyzes full specific surface area, effective pore specific surface area and the effective hole ratio of sample, referring specifically to shown in table 2.
Effective hole ratio of prepared charcoal finished product under the different mixed gas flows of table 2
According in table 2 as a result, when other treatment conditions are identical, as the flow of mixed gas improves, refined biological
The ratio that effective pore specific surface area of charcoal product accounts for full specific surface area is gradually increased.Illustrate that mixed gas flow raising is conducive to change
Into oxygen and the contact situation of the charcoal surface of solids in mixed gas, the ablation effect of oxygen is improved.In conjunction with the embodiment in table 2
4, it 8 and 9 can be seen that when mixed gas flow is relatively low (3-5 boiler tube volume per hour), as gas flow increases
Add, the full specific surface area of refined biological charcoal product and effective pore specific surface area increase.But continue to improve mixed gas
Flow, full the specific surface area of refined biological charcoal product and effective pore specific surface area will be with will gradually decline.Illustrate the stream of mixed gas
It measures excessively high, the pore structure of charcoal product will be caused to collapse, that is, so-called excessive ablation occurs, is unfavorable for charcoal specific surface area
Raising.
According to data in table 2, when the flow of mixed gas is 4-7 boiler tube volume per hour, gained refined biological charcoal
The full specific surface area of product can reach 300m2/ g or more, effective pore specific surface area can reach 100m2/ g or more, effective hole ratio exist
30% or more.
Embodiment 14-21: influence of the heat treatment condition to the effective pore specific surface area of charcoal
According in Tables 1 and 2 as a result, investigating other heat treatments on the basis of preferred mixed gas composition and flow
Influence of the condition (temperature, time) to the effective pore specific surface area of charcoal.The 6g charcoal prepared in comparative example is taken, tubular type is put into
In furnace (boiler tube model Φ 8cm × 100cm, boiler tube volume are 5L), volume ratio is passed through as 1:1 nitrogen with the flow of 25L per hour
Gas and air gas mixture, after carrying out heat treatment a period of time, obtained solid object and 12g activated alumina ball (partial size is 1~
It 3mm) is put into togerther in 150mL water, after being stirred for 24 hours under room temperature, takes out activated alumina ball, filter out solids, wash, 105
The charcoal finished product refined after drying at DEG C using the full specific surface area of the analysis sample of method described in embodiment 1-7, has
Pore specific surface area and effective hole ratio are imitated, referring specifically to shown in table 3.
Effective hole ratio of prepared charcoal finished product under 3 Different Heat Treatment Conditions of table
According in table 3 as a result, continuing relative to the charcoal sample (embodiment 4) obtained under 400 DEG C of heat treatment temperatures
Heat treatment temperature is increased not to be significantly improved the specific surface area of charcoal product to 500 DEG C (embodiment 14).In conjunction with reality
Apply the result in example 4,15 and 16, it can be seen that at 400 DEG C by holding time to 2h after, the ratio of refined biological charcoal product
Surface area and effective hole ratio increase, but are to continue with and extend to the effect of 3h and be not obvious.Illustrate that heat preservation is appropriately extended
Time is conducive to the ablation effect for reinforcing oxygen to charcoal micro-pore wall, but overlong time has no and is significantly improved effect.Implement
Result in example 18,19 and 20, it can be seen that effective hole that soaking time is conducive to improve charcoal is appropriately extended at 300 DEG C
Ratio, but the time is more than that subsequent to continue extended effect unobvious by 6h.In embodiment 21 result explanation, heat treatment temperature down to
At 200 DEG C, oxygen declines the ablation significant effect of charcoal micro-pore wall.
According to data in table 3, when heat treatment temperature is at 300-400 DEG C, heat treatment time is in 1-6h, gained refined raw
The full specific surface area of object charcoal product can reach 300m2/ g or more, effective pore specific surface area can reach 100m2/ g or more, effective boring ratio
Rate is 30% or more.
Embodiment 22-27: influence of the different activities alumina balls additive amount to the effective pore specific surface area of charcoal
The 6g charcoal prepared in comparative example is taken, (boiler tube model Φ 8cm × 100cm, boiler tube volume are put into tube furnace
For 5L), volume ratio is passed through as 1:2 nitrogen and air gas mixture with the flow of 30L/h, keeps the temperature 6h after being heated to 300 DEG C,
Obtained solid object and activated alumina ball (partial size is 1~3mm) are put into togerther in 200mL water, after stirring 48h under room temperature, are taken out
Activated alumina ball filters out solids, washing, the charcoal finished product refined after drying at 105 DEG C, using embodiment 1-
Method described in 7 analyzes full specific surface area, effective pore specific surface area and the effective hole ratio of sample, referring specifically to shown in table 4.
Effective hole ratio of prepared charcoal finished product under 4 different activities alumina balls additive amount of table
According in table 4 as a result, in the identical situation of other treatment conditions, without activated alumina ball expanding treatment
Charcoal product specific surface area and effective hole ratio are lower.After activated alumina ball expanding treatment is added, gained charcoal is produced
Full specific surface area, effective pore specific surface area and the effective hole ratio of product significantly improve.Illustrate that activated alumina ball helps to turn
It moves the part that is oxidized in charcoal not to be carbonized organic matter, and then plays the role of expanding charcoal aperture.22- in conjunction with the embodiments
26 can be seen that the raising with activated alumina ball additive amount, and the full specific surface area of charcoal and effective pore specific surface area are equal
It is gradually increased.But after the mass ratio of activated alumina ball and charcoal is more than 3:1, the specific surface area of charcoal improves effect
Fruit is unobvious.
According to data in table 4, when the mass ratio of activated alumina ball and charcoal is 5:1-1:1, gained refined biological
The full specific surface area of charcoal product can reach 300m2/ g or more, effective pore specific surface area can reach 100m2/ g or more, effective hole ratio
35% or more.
Test cases
Take the charcoal sample prepared in a small amount of above-mentioned comparative example and embodiment 4,17,24, respectively number be 0#, 1#, 2#,
3#, using the specific surface area of specific surface area and Porosimetry test sample.Referring to test method general in industry, with N2For
Adsorbate measures isotherm adsorption data accorded at 77K, calculates the full specific surface area of sample using BET method, calculates sample using BJH method
Effective hole (1.7~50nm) specific surface area of product calculates sample according to the percentage that effective pore specific surface area accounts for full specific surface area
Effective hole ratio, be as a result listed in table 5.
The specific surface area size of charcoal sample obtained by 5 comparative example of table and embodiment
According to the result in table 5 it can be concluded that, compared with the charcoal sample 0# in comparative example, using the technology of the present invention
Effective pore specific surface area of scheme treated charcoal product 1#, 2#, 3# improves 3.7~5.0 times, and effective hole ratio mentions
Height illustrates technical solution of the present invention treated that effective pore specific surface area of charcoal product is significantly higher than to 35% or more
Untreated raw material charcoal.
Adsorb embodiment
Using 0.02mol/L sodium chloride solution as background, initial mass concentration C is prepared0For 10,20,30,40,50mg/
The herbicide tribenuron-methyl aqueous solution of L.It measures 100mL to move into stuffed conical flask, is separately added into the above-mentioned comparative example of 100mg and implementation
0#, 1#, 2#, 3# the charcoal sample prepared in example, shakes up.Then conical flask is put into 25 DEG C of constant temperature oscillators, it is continuous to shake
After swinging 48h, the residual mass concentration of herbicide in sampling analysis aqueous solution, according to the initial mass concentration of herbicide aqueous solution and
Residual mass concentration difference calculates the removal rate after herbicide is adsorbed by charcoal.Using initial mass concentration as abscissa, removal rate
For ordinate, charcoal sample is drawn to the removal curve (Fig. 1) of herbicide.
It will be seen from figure 1 that under identical initial concentration, using 1#, 2#, 3# biology of the application post-processing approach preparation
Charcoal, in tribenuron-methyl aqueous solution initial concentration≤20mg/L, removal rate almost can reach 100%, and under same concentrations, without
The charcoal of the application method post-processing only has 65% and 35%；It is subsequent with tribenuron-methyl initial concentration increase, in embodiment
The removal rate of tribenuron-methyl is declined under charcoal dosage.But use 1#, 2#, 3# biology of technical solution of the present invention preparation
Charcoal sample is still significantly higher than the 0# charcoal sample in comparative example to the removal rate of tribenuron-methyl.By Fig. 1 for example, using this
Inventive technique scheme post-processes charcoal, can significantly improve charcoal to the Adsorption of the organic pollutants such as pesticide
Efficiency.
Claims (3)
1. a kind of post-processing approach for improving the effective pore specific surface area of charcoal, it is characterised in that: raw material charcoal is put into heat
In treatment furnace, it is passed through nitrogen and air gas mixture, after heat treatment, obtained solid object and activated alumina ball are put into togerther water
In, after the processing of room temperature reaming, activated alumina ball is taken out, solids is filtered out, washed, obtain finished product after drying；Described is mixed
Closing the volume ratio that gas composition is nitrogen and air is 5:1 ~ 1:5, the flow of mixed gas 3 ~ 10 boiler tube volumes per hour, heat
Treatment temperature is 200 ~ 500 DEG C, and soaking time is 0.5 ~ 6 h；The mass ratio of the activated alumina ball and solids be 3:1 ~
1:1；Water and the mass ratio of activated alumina ball are 30:1 ~ 5:1；Solids and activated alumina ball be in water under the room temperature
The expanding treatment time is 2 ~ 72 h.
2. a kind of post-processing approach for improving the effective pore specific surface area of charcoal as described in claim 1, it is characterised in that: institute
The volume ratio of the nitrogen and air stated is 2:1 ~ 1:2, and the flow of mixed gas is that 4 ~ 7 boiler tube volumes, heat treatment are warm per hour
Degree is 300 ~ 400 DEG C, and soaking time is 1 ~ 3 h.
3. a kind of post-processing approach for improving the effective pore specific surface area of charcoal as described in claim 1, it is characterised in that: institute
Stating raw material charcoal is that the high carbonaceous solids using the biomass rich in cellulose, lignin as raw material, through limit oxygen pyrolysis preparation produce
Object.
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| CN1669919A (en) * | 2005-02-28 | 2005-09-21 | 昆明理工大学 | Method for producing mesopore activated carbon |
| CN102442665A (en) * | 2011-09-28 | 2012-05-09 | 福州大学 | Thermally treated active carbon and preparation method thereof |
| CN103288080A (en) * | 2013-06-14 | 2013-09-11 | 中国石油大学(华东) | Method for preparing high-mesopore-ratio high-adsorptivity ecological carbon |
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|---|---|---|---|---|
| CN1669919A (en) * | 2005-02-28 | 2005-09-21 | 昆明理工大学 | Method for producing mesopore activated carbon |
| CN102442665A (en) * | 2011-09-28 | 2012-05-09 | 福州大学 | Thermally treated active carbon and preparation method thereof |
| CN103288080A (en) * | 2013-06-14 | 2013-09-11 | 中国石油大学(华东) | Method for preparing high-mesopore-ratio high-adsorptivity ecological carbon |
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| Title |
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| Role of Alumina and Montmorillonite in Changing the Sorption of Herbicides to Biochars;Jianfa Li et al;《J. Agric. Food Chem.》;20150602;摘要，Materials，Treatment of Biochars with Soil Minerals |
| 热处理提高活性炭对水中MIB的去除能力研究;陈维芳 等;《水资源与水工程学报》;20110630;第22卷(第3期);第128-131页 |
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