CN108821286A - banana stem active carbon and preparation method thereof - Google Patents
banana stem active carbon and preparation method thereof Download PDFInfo
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- CN108821286A CN108821286A CN201810869935.1A CN201810869935A CN108821286A CN 108821286 A CN108821286 A CN 108821286A CN 201810869935 A CN201810869935 A CN 201810869935A CN 108821286 A CN108821286 A CN 108821286A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/342—Preparation characterised by non-gaseous activating agents
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/318—Preparation characterised by the starting materials
- C01B32/324—Preparation characterised by the starting materials from waste materials, e.g. tyres or spent sulfite pulp liquor
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The invention discloses a kind of banana stem active carbons and preparation method thereof, include the following steps：(1) pretreatment of banana stem：It after banana stem to be washed to the dust and impurity on removal surface, dries, crushes, sieve with 100 mesh sieve, obtain banana stem powder；(2) it impregnates：Banana stem powder and phosphoric acid solution are impregnated according to certain material agent than at room temperature；(3) it activates：Impregnated banana stem powder is activated at a certain temperature；(4) it cleans and dries：It will be cleaned after banana stem Powdered Activated Carbon cooling after activation with deionized water, until the pH of cleaning solution is 6-7, obtain wet active carbon；Wet active carbon is placed in drying box and is dried, dry active carbon is obtained.Active carbon of the invention has a good absorption property, the especially removal rate to Amoxicillin in water, reaches 90% or more, and the method for the present invention simple process, efficiently, and energy conservation and environmental protection meets the needs of recycling economy development.
Description
Technical field
The present invention relates to a kind of active carbons and preparation method thereof, and in particular to a kind of banana stem active carbon and its preparation side
Method.Belong to active carbon preparation technical field.
Background technique
Greatly developing Green Chemistry, under the overall situation of green agriculture, positive secondary benefit of the development to agricultural and sideline active carbon class
With the pursuit in the epoch that are in response to, at this stage, active carbon manufacturing industry has begun superseded ZnCl2Activation method prepares active carbon, to
H3PO4Activation method direction is drawn close.It is counted according to latest data, worldwide banana harvest area in 2016 is 434.97 ten thousand public
Hectare, yield is at 7024 tons, and wherein harvest area and the maximum Asian countries of yield are India, is 58.81 ten thousand hectares and 14,840,000
Ton, accounts for the 13.64% and 23.74% of the world respectively；Followed by it is located at Brazil of South America.Other main country of origins of banana are also
The countries such as China, Costa Rica, Vietnam, Philippine, Indonesia, Ecuador, Thailand.Guangxi, Yunnan, Hainan, good fortune
It builds, several provinces such as Guangdong have the 90% of China's banana planting area.China's banana planting industry still develops good, this representative
Our raw material banana stem source be very extensive.There is also huge researching values simultaneously.
According to statistics, one plant of banana plant height then can output 360~470g banana fiber, it is low, can produce 170~250g perfume
Any of several broadleaf plants fasciated fiber.Orchard worker after gathering in its fruit, all discard in field mostly by stem.Raw material, which is largely recycled, turns waste into wealth, and can use
Carbonated material is made in extensive use, organic feed raw material, fertilizer type, textile raw material, will be conducive to the effect for increasing banana planting industry
The development of benefit and the high-new industry of promotion banana plantation, to increase economic efficiency.
Summary of the invention
The technical problem to be solved in the present invention is to provide one kind using banana stem as raw material, changing waste into valuable, energy conservation and environmental protection, technique
Simply, the preparation method of cost-effective any of several broadleaf plants stem active carbon.
To achieve the above object, the present invention adopts the following technical solutions：
A kind of banana stem active carbon is prepared by raw material of banana stem.
The present invention also provides a kind of preparation methods of banana stem active carbon, include the following steps：
(1) pretreatment of banana stem：It after banana stem to be washed to the dust and impurity on removal surface, dries, crushes, cross 100
Mesh obtains banana stem powder；
(2) it impregnates：Above-mentioned banana stem powder and phosphoric acid solution are impregnated according to certain material agent than at room temperature；
(3) it activates：Banana stem powder after dipping is activated；
(4) it cleans and dries：It will be cleaned after product cooling after activation with deionized water, dried in 100 DEG C of drying box
It is dry, obtain dry active carbon.
The purpose of cleaning is to wash away the chemical substance generated in residual phosphoric acid and charcoal activation process, until the pH of cleaning solution is
6-7。
Room temperature refers to 25 DEG C.
Step (2) the material agent is the ratio of banana stem powder quality and phosphoric acid solution quality.
Preferably, the mass concentration of step (2) described phosphoric acid is 60%~80%, and the material agent ratio is 1:1~1:6, institute
Stating phosphoric acid solution dip time is 3~18h.
Preferably, step (3) activation temperature is 300~550 DEG C, and activation time is 45~120min.
It is further preferred that the phosphoric acid concentration is 70%, material agent ratio is 1:5, phosphoric acid solution dip time 12h, activation
Temperature is 450 DEG C, activation time 75min.
Beneficial effects of the present invention：
(1) present invention is raw material using discarded banana stem, and from a wealth of sources, cheap and easy to get and category renewable resource becomes useless
For benefit, comprehensive utilization of waste and environmental protection are not only improved, realizes the resource utilization to banana specialty industries waste,
The raw material sources that active carbon has also been enlarged reduce the production cost of active carbon.
(2) the method for the present invention simple process, efficiently, turn waste into wealth simultaneously, meet the needs of recycling economy development.
(3) specific surface area of product of the present invention banana stem active carbon is 1177.03m2/ g, total pore volume 1.90cm3/g；It is micro-
Pore volume is：0.38cm3/ g, mesopore volume are：1.52cm3/g.There is stronger absorption property；Banana stem active carbon in water Ah
The removal rate of Amdinocillin reaches as high as 90%.
Detailed description of the invention
Fig. 1 is the phosphate impregnation time to banana stem activated carbon adsorption performance influence diagram；
Fig. 2 is material agent ratio (banana stem quality and phosphoric acid quality ratio) to banana stem activated carbon adsorption performance influence diagram；
Fig. 3 is the infrared spectrogram of banana stem；
Fig. 4 is N2Aspiration/desorption isotherm；
Fig. 5 is the graph of pore diameter distribution of banana stem active carbon.
Specific embodiment
The present invention will be further elaborated with reference to the accompanying drawings and examples, it should which explanation, following the description is only
It is not to be defined to its content to explain the present invention.
Embodiment 1：A kind of preparation method of banana stem active carbon, includes the following steps：
(1) pretreatment of banana stem：It after banana stem to be washed to the dust and impurity on removal surface, dries, crushes, cross 100
Mesh obtains banana stem powder；
(2) it impregnates：Using phosphoric acid as the activator for preparing banana stem active carbon, the phosphorylated ligand for being 85% by mass fraction
The phosphoric acid solution of various concentration is made；
By above-mentioned banana stem powder and phosphoric acid solution according to certain material agent ratio (banana stem powder quality and phosphoric acid solution
Quality) certain time is impregnated at room temperature；
(3) it activates：Impregnated banana stem powder is fitted into ceramic crucible to be placed in cabinet-type electric furnace, at a certain temperature
It is activated.
(4) it cleans and dries：It will be cleaned repeatedly after banana stem active carbon cooling after activation with deionized water, wash away residual
The chemical substances such as the tar generated in phosphoric acid and charing and activation process obtain wet active carbon until the pH of cleaning solution is 6-7,
Wet active carbon is placed in 100 DEG C of drying box and is dried, obtains dry active carbon.
In the present embodiment, material agent ratio is selected as 1:3, dip time is 12 hours to banana stem powder at room temperature, activation temperature
Degree is 500 DEG C, activation time 1h, and phosphoric acid concentration (mass fraction) selects 30%, 40%, 50%, 60%, 70%, 80% respectively
It is tested, obtaining different phosphoric acid concentrations, the results are shown in Table 1 to banana stem activated carbon adsorption performance.
Influence of 1 phosphoric acid concentration of table to banana stem activated carbon adsorption performance
Table 1 statistics indicate that：In phosphoric acid concentration in the range of 30%-70%, banana stem active carbon mesoporous and micropore
Generation influenced by phosphoric acid concentration size bigger, with the increase of phosphoric acid concentration, the activation degree of banana stem active carbon is mentioned
Height, the basic manufacture of oneself warp of the micropore of specimen material is complete, and the raising of phosphoric acid concentration, excessive phosphoric acid corrosion fall original micropore
And generate mesoporous.After phosphoric acid concentration is higher than 70%, downward trend is presented in the iodine number and methylene blue value of banana stem active carbon, this
It is primarily due to when phosphoric acid concentration is excessively high, since phosphoric acid is excessively sticky and mobility is too poor, phosphoric acid can not be compared in dipping process
The internal structure of good immersion banana stem, so that good pore structure can not be formed in activation process.
Embodiment 2：Selecting phosphoric acid quality score is 70%, expects agent than 1:3, in room temperature immersion 12h, activation time 1h,
Activation temperature selects 300 DEG C, 350 DEG C, 400 DEG C, 500 DEG C, 550 DEG C respectively, and other conditions are same as Example 1, prepare banana
Stem active carbon.The results are shown in Table 2.
Influence of 2 activation temperature of table to banana stem activated carbon adsorption performance
As shown in Table 2, the methylene blue adsorption value and iodine number of banana stem active carbon are in the raising with activation temperature
Existing one first increases the Trendline to glide afterwards.The iodine number of banana stem active carbon reaches maximum at 400 DEG C, then with temperature
It increases, iodine number decline.This is because the micropore of banana stem active carbon is the most flourishing at 400 DEG C.When temperature is lower than 400 DEG C, with
The raising of temperature, active carbon iodine number be gradually increased, this illustrates that temperature increases, and the micropore of active carbon is formed better.Work as temperature
When higher than 400 DEG C, excessively high temperature causes the excessive ablation of micropore, the reduction of micropore quantity is caused, so that iodine number is with temperature
Improve decline.
Comparison iodine number adsorption curve and methylene blue adsorption number curve can be seen that：It is exactly that banana stem active carbon is micro- after 400 DEG C
Pore structure starts the starting point that ablation forms mesoporous, simultaneously because activation temperature is excessively high, mesoporous can recurring structure contraction.Work as temperature
When reaching 500 DEG C, there is peak value in methylene blue adsorption value, this explanation is when activation temperature is to 500 DEG C, the ablation of activated carbon capillary
The contraction significantly more than active carbon central hole structure is acted on, to cause increased significantly for mesoporous.When temperature is higher than 500 DEG C
Afterwards, mesoporous also starts excessive ablation and forms macropore, thus methylene blue adsorption number curve is begun to decline.
Embodiment 3：Dip time 12h is selected, 70% phosphoric acid concentration expects agent than 1:3, activation temperature is 450 DEG C, activation
Time is respectively 45,60,75,90,105,120min, and other conditions are same as Example 1, prepare banana stem active carbon.As a result
It is shown in Table 3.
3 activation time of table influences the absorption property of banana stem active carbon
As shown in Table 3, influence of the activation time to banana stem active carbon iodine number and methylene blue value curve is substantially identical
's.It is all to decline afterwards as the growth of activation time first increases.Iodine number reaches peak value, methylene when activation time is 60min
Blue value reaches peak value in activation time 75min.For this explanation in the initial stage of activation, the activation of active carbon is complete not enough,
With the increase of activation time, banana stem is constantly activated under the action of phosphoric acid and generates micropore and mesoporous, therefore its iodine number and Asia
Methyl blue value can all increase with activation time and be increased.After activation is complete, with the growth of activation time, activated carbon structure hole
Structure is gradually ablated；The micropore and mesoporous of active carbon gradually become mesoporous and macropore.Simultaneously because the condensation of phosphoric acid, living
The carbon structure of property charcoal gradually tapers up, and causes the decline of active carbon specific surface area.
Embodiment 4：Activation time 75min is selected, 70% phosphoric acid concentration expects agent than 1:3, carburizing temperature is 450 DEG C, leaching
The stain time selects 3h, 6h, 9h, 12h, 15h, 18h respectively, and other conditions are same as Example 1, prepares banana stem active carbon.Knot
Fruit is shown in Table shown in 4 and Fig. 1.
4 dip time of table influences the absorption property of banana stem active carbon
As seen from Figure 1, with the increase of dip time, the iodine number and methylene blue adsorption value of banana stem active carbon are all
The state for being gradually increasing and then tending towards stability to the end is presented.Iodine number adsorption curve and methylene blue adsorption number curve exist
It tends towards stability when 12h, this explanation is before 12h, and with the increase of dip time, phosphoric acid solution constantly enters banana stem
Internal pore structure, thus its absorption property is also gradually increased, to after 12h, phosphoric acid has had reached saturation impregnation state, because
And dip time is continued growing, the absorption property of banana stem active carbon is influenced little.
Embodiment 5：Activation time 75min is selected, 70% phosphoric acid concentration, dip time 12h, activation temperature is 450 DEG C,
Expect agent than 1:1,1:2,1:3,1:4,1:5,1:6, other conditions are same as Example 1, prepare banana stem active carbon.As a result see figure
Shown in 2.
By Fig. 2 analysis as a result, the iodine number adsorption curve and methylene blue adsorption number curve of banana stem active carbon are with material agent ratio
Raising be all to present a kind of first to increase downward trend again.The reason of generating this phenomenon be：When material agent is than too small, due to phosphorus
Acid content is excessively rare, can not play a very good protection to the pore structure inside banana stem raw material, in activation process
Due to the not protective effect of phosphoric acid substantially, the pore structure inside raw material burns mistake completely substantially, to cannot play well
Suction-operated；With the raising of material agent ratio, oneself warp of phosphoric acid can protect the formation of banana stem activated carbon capillary completely, when material agent ratio
When increase, extra phosphoric acid starts to continue pore-creating on the basis of banana stem activated carbon capillary, during its macro structure of ablation is formed
Hole, the micropore quantity of active carbon is reduced at this time, and middle hole number increases；When material agent ratio is more than 1:When 5, since phosphorus acid content is excessive,
Cause micropore largely ablated, the formation of active carbon interior mesopores to macropore also reduces to not only reduce the number of micropore
Mesoporous number.
The structural characterization of banana stem active carbon：
By the characterization of Fourier infrared spectrograph, can be made according to the peak intensity, peak position and peak type of the wave spectrum of acquisition
The structural information of standby active carbon, by dried activated carbon sample, in 4000cm-1~500cm-1Sample is carried out in range
IR spectrum scanning analyzes its functional group.From figure 3, it can be seen that banana stem active carbon is in 3742cm-1There is lesser O-H at place
Stretching vibration peak, 1697cm-1Place and be C=O stretching vibration peak, 1510cm-1For the skeletal vibration of C=C or fragrance.
By dried activated carbon sample, after correct amount, at 300 DEG C, in the environment of normal pressure, 10h is pre-processed, it is rear to use
Hole and surface analysis instrument measure its specific surface area and micropore mesoporous distribution situation.
By the full-automatic specific surface area of ASAP2020 and hole tester, the specific surface area of banana stem active carbon is detected
1177.03m2/g.Total pore volume is 1.90cm3/g；Micro pore volume is：0.38cm3/ g, mesopore volume are：1.52cm3/g。
There are apparent loop lines for the adsorption and desorption curve of banana stem active carbon as seen from Figure 4, meet the absorption of the 4th class
Isothermal feature.When relative pressure is lower than 0.03, with the increase of pressure, adsorption curve is dramatically increased, at this time mainly
It is to form monomolecular adsorption layer, when relative pressure is 0.03~0.60, mono layer adsorption progressivelyes reach saturation, and starts
Carry out multilayer absorption；After relative pressure is greater than 0.60, curve generates hysteresis loop, illustrates to occur under higher relative pressure
Capillary condensation phenomenon illustrates that the distribution of mesoporous is wider since curve rises slowly in this stage.It is lower than in relative pressure
When 0.60, adsorption curve and desorption curve are completely coincident, and there is no capillary condensation phenomenon, hole is completely filled out
It is full, illustrate there is flourishing central hole structure in material.The graph of pore diameter distribution of banana stem active carbon is as shown in Figure 5.
Suction-operated of the banana stem active carbon to Amoxicillin in water：
The active carbon prepared according to the present invention program is used to adsorb the Amoxicillin in water.It is 40 in adsorption temp
DEG C, adsorption liquid pH=3, active carbon injected volume is 3g/L, and when adsorption time is 12h, banana stem active carbon is to Amoxicillin in water
Removal rate reach as high as 90%.
Above-mentioned, although the foregoing specific embodiments of the present invention is described with reference to the accompanying drawings, not protects model to the present invention
The limitation enclosed, based on the technical solutions of the present invention, those skilled in the art are not needed to make the creative labor and can be done
Various modifications or changes out are still within protection scope of the present invention.
Claims (8)
1. a kind of banana stem active carbon, which is characterized in that prepared by raw material of banana stem.
2. the preparation method of banana stem active carbon described in claim 1, which is characterized in that include the following steps：
(1) pretreatment of banana stem：It after banana stem to be washed to the dust and impurity on removal surface, dries, crushes, sieve with 100 mesh sieve,
Obtain banana stem powder；
(2) it impregnates：Above-mentioned banana stem powder and phosphoric acid solution are impregnated according to certain material agent than at room temperature；
(3) it activates：Banana stem powder after dipping is activated；
(4) it cleans and dries：It will be cleaned after activation products cooling with deionized water, dry banana stem activity obtained after drying
Charcoal.
3. a kind of preparation method of banana stem active carbon according to claim 2, which is characterized in that step (1) described baking
Dry specific method is：Banana stem is put into dryer, is dried 6 hours at a temperature of 80 DEG C.
4. a kind of preparation method of banana stem active carbon according to claim 2, which is characterized in that step (2) described phosphorus
The mass fraction of acid is 60%~80%；The material agent is than 1:1~1:6；Dip time is 3~18 hours.
5. a kind of preparation method of banana stem active carbon according to claim 2, which is characterized in that step (3) described work
Changing temperature is 300~550 DEG C, and activation time is 45~120 minutes.
6. a kind of preparation method of banana stem active carbon according to claim 4, which is characterized in that the matter of step (2) acid
Measuring score is 70%；The material agent is than 1:5；Dip time is 12 hours.
7. a kind of preparation method of banana stem active carbon according to claim 5, which is characterized in that step (3) described work
Changing temperature is 450 DEG C, and activation time is 75 minutes.
8. a kind of preparation method of banana stem active carbon according to claim 2, which is characterized in that step (4) described baking
Dry temperature is 100 DEG C.
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2018
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