CN109173999A - A kind of preparation method and applications of biology carbon microspheres - Google Patents
A kind of preparation method and applications of biology carbon microspheres Download PDFInfo
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- CN109173999A CN109173999A CN201811175641.5A CN201811175641A CN109173999A CN 109173999 A CN109173999 A CN 109173999A CN 201811175641 A CN201811175641 A CN 201811175641A CN 109173999 A CN109173999 A CN 109173999A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- 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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- 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
- B01J20/28014—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 form
- B01J20/28016—Particle form
- B01J20/28021—Hollow particles, e.g. hollow spheres, microspheres or cenospheres
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- 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
- B01J20/28057—Surface area, e.g. B.E.T specific surface area
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- 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
- B01J20/30—Processes for preparing, regenerating, or reactivating
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Abstract
The present invention provides a kind of preparation method and applications of biological carbon microspheres.Preparation method is comprising steps of (1) pretreatment of raw material；(2) hydrothermal synthesis；(3) pyrolysis activation.Biology carbon microspheres obtained have porous structure, pattern, size distribution uniform, and Microsphere Size is 3~5 μm, and favorable dispersibility, and it is heavy metal ion adsorbed to can be used as adsorbent progress.Charcoal method for preparing microsphere disclosed by the invention does not use catalyst, carries out hydrothermal synthesis merely with waste biomass materials and deionized water, and preparation process is completely pollution-free, helps to protect environment.Biology carbon microspheres obtained, pattern, size distribution uniform and favorable dispersibility；Using hydrothermal synthesis-pyrolysis activation method preparation, it is still able to maintain good spherical morphology by 700 DEG C of heat treatments, there is pore structure abundant and biggish specific surface area.The biology carbon microspheres can show excellent absorption property applied to heavy metal ion adsorbed.
Description
Technical field
It is the present invention relates to the technical field that biomass castoff recycles, in particular to a kind of discarded using biomass
Object --- pomelo peel prepares the biological method of carbon microspheres and the application of the biology carbon microspheres.
Background technique
China possesses biomass resource abundant, and recovery energy has a high potential, and the whole nation can be used as the farming of using energy source
The biomass such as object stalk and processing of farm products residue, forestry residue and energy crop, house refuse and organic waste money
Source converts into total amount about 4.6 hundred million tons of standard coals every year.The direct burning of biomass castoff, generates a large amount of CO, CO2, SO2, NOx
With the pollutants such as flue dust, atmospheric environment seriously polluted, be one of the pollution sources of current more serious haze problem.Therefore,
Comprehensive high-efficiency clean utilization biomass castoff resource be solve energy crisis and environmental pollution two large problems effective ways it
One.Biological carbon materials wherein are prepared using biomass castoff, only the classification of waste and resource utilization do not provide newly
Thinking reduces environmental pollution, and also meets the great demand to the functional Carbon Materials such as charcoal.
At present for the pollution of typical pollutant in water body, absorption is to remove a kind of of low concentration heavy metal water effectively to arrange
It applies.But a large amount of active carbon is consumed in adsorption process etc. high prices adsorbent also limits this kind of method to a certain extent
Practical application, thus, the development of a large amount of cheap, effective adsorbents is current by absorption method removing water pollution important research
Direction.Charcoal has fine and close microcellular structure and huge specific surface area, and adsorption capacity is stronger, can adsorb Cr (VI), Cu
(II), the heavy metals such as Ni (II), Cd (II), Pb (II), meanwhile, it also have low production cost, ecological safety, it is pollution-free, can
The distinguishing features such as it is widely applied.These distinguishing features make it administer water body and soil as a kind of efficient, cheap adsorbent
Significant role is played on earth heavy metal pollution problem.The absorption behavior of charcoal can influence heavy metal ion in the environment
The processes such as Transport And Transformation, the control of ecological effect and contaminated environment medium and reparation.
Shaddock is as a kind of main fruit in China, and plantation is in southern area extensively, such as Fujian, Guangdong, Guangxi, river
The ground such as west, TaiWan, China, pomelo peel are thicker with respect to cortex for other pericarps, and rich in having a large amount of cellulose, hemicellulose
And lignin, a large amount of pomelo peel waste can be generated after edible or processing, however these prepare the good life of charcoal
Raw material of substance is often simply discarded, fills or is incinerated, and not only pollutes environment, and huge biomass resource is caused to waste.
Preparing water-treatment biological carbon adsorbent as raw material using pomelo peel can effectively reduce production cost, turn waste into wealth simultaneously, realization pair
The cycling and reutilization of this renewable energy of biomass castoff.China patent CN 106065332 A and 106000303 A of CN
Pomelo peel is all made of as raw material, charcoal is prepared by the method that hydro-thermal carbonizes, but the two is equal during hydrothermal synthesis
It is added to catalyst, a large amount of catalyst are contained in hydrothermal synthesis waste liquid and cause environmental pollution, and the biological product char shape of its preparation
Looks, size are uneven.
Summary of the invention
It is an object of the invention to overcome disadvantage existing in the prior art, a kind of preparation method is provided, it is obtained raw
Pattern, size distribution uniform and the favorable dispersibility of object carbon microspheres.
Technical solution is as follows:
A kind of preparation method of biology carbon microspheres, comprising the following steps:
(1) pretreatment of raw material: pomelo peel is cut, and is only left white flesh in color after cutting off bluish yellow color crust, by drying,
It crushes, after sieving, obtains flesh powder in faint yellow pomelo peel；
(2) hydrothermal synthesis: flesh powder in pomelo peel that step (1) obtains and deionized water are placed in hydrothermal reaction kettle,
The material ratio of the two is 1~5g:60mL, and closed be placed in baking oven of reaction kettle is then heated to 160~220 DEG C, keeps permanent
2~8h of temperature；Reaction kettle is cooled to room temperature, the solid product in suspension is filtered, then is washed with deionized to filter
Liquid clarification, then dries solid product to obtain hydrothermal synthesis product；
(3) pyrolysis activation: the hydrothermal synthesis product that step (2) obtains is further arranged in tube furnace, 500~700 DEG C
1~4h is heat-treated in lower nitrogen atmosphere, activation obtains biological carbon microspheres.
Further, in step (1), flesh powder crosses 60~100 meshes in the pomelo peel.
Further, in step (2), flesh powder in material ratio 1g, 2g, 3g, 4g or 5g pomelo peel: 60mL deionized water；
Hydrothermal synthesis temperature is 160 DEG C, 180 DEG C, 200 DEG C or 220 DEG C；The hydrothermal synthesis time is 2h, 4h, 6h or 8h.
Further, in step (3), pyrolysis temperature be 500 DEG C, 600 DEG C or 700 DEG C, heat treatment time 1h, 2h, 3h or
4h。
The biology carbon microspheres as made from above-mentioned preparation method have porous structure, pattern, size distribution uniform, microballoon
Having a size of 3~5 μm, and favorable dispersibility, it is heavy metal ion adsorbed to can be used as adsorbent progress.
The present invention has the following advantages that compared with prior art and effect:
(1) charcoal method for preparing microsphere disclosed by the invention does not use catalyst, merely with waste biomass materials and
Deionized water carries out hydrothermal synthesis, and preparation process is completely pollution-free, helps to protect environment.
(2) biology carbon microspheres made from, pattern, size distribution uniform and favorable dispersibility；Using hydrothermal synthesis-heat
Activation method preparation is solved, is still able to maintain good spherical morphology by 700 DEG C of heat treatments, with pore structure abundant and biggish
Specific surface area.
(3) prepared biological carbon microspheres are applied to heavy metal ion adsorbed, show excellent heavy metal ion and inhales
Attached performance.
Detailed description of the invention
Fig. 1 is the SEM figure for the hydrothermal synthesis product that embodiment 1 is prepared.
Fig. 2 is the SEM figure for the hydrothermal synthesis product that comparative example 1 is prepared.
Fig. 3 is the SEM figure for the biological carbon microspheres that embodiment 1 is prepared.
Fig. 4 is the biological carbon microspheres counterweight adsorption of metal ions performance map that embodiment 1 is prepared, and is followed successively by from top to bottom
For Cr6+、Cu2+、Pb2+Absorption property figure, wherein qe: (a) hydrothermal synthesis product, (b) biological carbon microspheres；E:(c) hydro-thermal
Synthetic product, (d) biological carbon microspheres.
Specific embodiment
It is carried out below with reference to technical effect of the embodiment to design of the invention, specific structure and generation clear, complete
Ground description, to be completely understood by the purpose of the present invention, feature and effect.Obviously, described embodiment is of the invention one
Section Example, rather than whole embodiments, based on the embodiment of the present invention, those skilled in the art are not paying creativeness
Other embodiments obtained, belong to the scope of protection of the invention under the premise of labour.
Embodiment 1:
(1) pretreatment of raw material: pomelo peel is cut, and flesh in color is only left white after cutting off bluish yellow color crust, by 100 DEG C
Drying crushes, after the sieving of 100 mesh, obtains flesh powder in faint yellow pomelo peel；
(2) hydrothermal synthesis: flesh powder in pomelo peel that step (1) obtains and deionized water are placed in hydrothermal reaction kettle,
The material ratio of the two is 5g:60mL, and closed be placed in baking oven of reaction kettle is then heated to 200 DEG C, keeps constant temperature 6h；It will be anti-
It answers kettle to be cooled to room temperature, the solid product in suspension is filtered, then be washed with deionized to filtrate and clarify, then will
Solid product dries to obtain hydrothermal synthesis product；
(3) pyrolysis activation: the hydrothermal synthesis product that step (2) obtains is further arranged in tube furnace, nitrogen at 700 DEG C
4h is heat-treated in atmosphere, activation obtains biological carbon microspheres.
Embodiment 2:
(1) pretreatment of raw material: pomelo peel is cut, and flesh in color is only left white after cutting off bluish yellow color crust, by 80 DEG C
Drying crushes, after the sieving of 60 mesh, obtains flesh powder in faint yellow pomelo peel；
(2) hydrothermal synthesis: flesh powder in pomelo peel that step (1) obtains and deionized water are placed in hydrothermal reaction kettle,
The material ratio of the two is 1g:60mL, and closed be placed in baking oven of reaction kettle is then heated to 160 DEG C, keeps constant temperature 2h；It will be anti-
It answers kettle to be cooled to room temperature, the solid product in suspension is filtered, then be washed with deionized to filtrate and clarify, then will
Solid product dries to obtain hydrothermal synthesis product；
(3) pyrolysis activation: the hydrothermal synthesis product that step (2) obtains is further arranged in tube furnace, nitrogen at 500 DEG C
2h is heat-treated in atmosphere, activation obtains biological carbon microspheres.
Embodiment 3:
(1) pretreatment of raw material: pomelo peel is cut, and flesh in color is only left white after cutting off bluish yellow color crust, by 80 DEG C
Drying crushes, after the sieving of 80 mesh, obtains flesh powder in faint yellow pomelo peel；
(2) hydrothermal synthesis: flesh powder in pomelo peel that step (1) obtains and deionized water are placed in hydrothermal reaction kettle,
The material ratio of the two is 4g:60mL, and closed be placed in baking oven of reaction kettle is then heated to 220 DEG C, keeps constant temperature 8h；It will be anti-
It answers kettle to be cooled to room temperature, the solid product in suspension is filtered, then be washed with deionized to filtrate and clarify, then will
Solid product dries to obtain hydrothermal synthesis product；
(3) pyrolysis activation: the hydrothermal synthesis product that step (2) obtains is further arranged in tube furnace, nitrogen at 600 DEG C
2h is heat-treated in atmosphere, activation obtains biological carbon microspheres.
Comparative example 1:
(1) pretreatment of raw material: pomelo peel is cut, and by 100 DEG C of drying, is crushed, after the sieving of 100 mesh, is obtained Huang
Color pomelo peel powder；
(2) hydrothermal synthesis: pomelo peel powder and deionized water that step (1) obtains are placed in hydrothermal reaction kettle, the two
Material ratio be 5g:60mL, closed be placed in baking oven of reaction kettle is then heated to 200 DEG C, keeps constant temperature 6h；By reaction kettle
It is cooled to room temperature, the solid product in suspension is filtered, then be washed with deionized to filtrate and clarify, then by solid
Product dries to obtain hydrothermal synthesis product；
(3) pyrolysis activation: the hydrothermal synthesis product that step (2) obtains is further arranged in tube furnace, nitrogen at 700 DEG C
4h is heat-treated in atmosphere, activation obtains biological carbon microspheres.
Test case:
The evaluation that biology carbon microspheres made from embodiment 1 carry out heavy metal ion adsorbed performance as adsorbent is specifically walked
It is rapid as follows:
(1) a series of heavy metal ion (Cr of concentration gradients (50~1000mg/L) is prepared with ultrapure water6+、Cu2+、Pb2+)
Solution takes the heavy metal solution of 10mL in the centrifuge tube of 15mL, and different quality (10mg, 20mg, 40mg, 80mg) preparation is added
Charcoal microsphere adsorbing agent, test tube overturning instrument on the speed response 12h of 80rpm/min, then with 0.22 μm of pin hole
Filter filtering, filtrate measure its concentration with inductive coupling plasma emission spectrograph.
(2) adsorption effect adsorbance q of the charcoal to heavy metal ioneIt is indicated with removal rate E, calculation formula point
Not as shown in formula a and formula b.
qe=(c0-ce)V/m (a)
E=(c0-ce) * 100%/ce (b)
In formula: qeAdsorbance of the charcoal to heavy metal ion, mg/g when to balance；c0For the dense of initial heavy metal solution
Degree, mg/L；ceThe concentration of heavy metal solution, mg/L when for adsorption equilibrium；V is the volume of heavy metal solution, mL；M is that life is added
The quality of object charcoal, g；E is removal efficiency, %.
Fig. 1 show the preparation-obtained hydrothermal synthesis product of embodiment 1, as can be seen from FIG. 1 using flesh powder in pomelo peel
The ball-type product favorable dispersibility of last hydrothermal synthesis preparation, and pattern, size are distributed all relatively uniform, the ball of ball-type hydrothermal product
Diameter is at 3~5 μm.Fig. 2 show the preparation-obtained hydrothermal synthesis product of comparative example 1, as can be seen from FIG. 2, compared to only with
The product that flesh powder synthesizes in pomelo peel, not using the product morphology distribution containing the entire pomelo peel hydrothermal synthesis preparation including crust
Uniformly, from figure this it appears that the existing ball-type of the product obtained after hydro-thermal reaction also has the product of block or sheet.Fig. 3 is
By the SEM figure for the biological carbon microspheres that hydrothermal synthesis-pyrolysis activation is prepared, as seen from the figure, after 700 DEG C of heat treatment, ball
Type structure is still completed, and biological carbon microspheres have pore structure abundant, and pyrolysis activates the biological carbon microspheres obtained later, relatively
In hydrothermal synthesis product, specific surface area and total pore volume are improved largely, as shown in table 1 below.
Table 1
Fig. 4 is that the biological carbon microspheres being prepared using embodiment 1 adsorb heavy metal ion (Cr6+、Cu2+、Pb2+) suction
Attached performance map, according to Fig. 4 as can be seen that due to specific surface area and Kong Rong increase, the activation of hydrothermal synthesis-pyrolysis is prepared
Biological carbon microspheres adsorption effect is substantially better than hydrothermal synthesis product, and the additive amount of adsorbent is to influence adsorption reaction process
Key factor, adsorbent addition is very few, and adsorption effect is poor, and absorption is not thorough, and pollutant residual is more；Adsorbent additive amount is excessive,
It is low to will cause adsorption efficiency, the wasting of resources, and will increase the cost of separating adsorbent.As shown in Figure 4 with adsorbent mass
Increase, the absorption for the biological carbon microspheres counterweight metal ion that hydrothermal synthesis product and hydrothermal synthesis-pyrolysis activation are prepared
Amount is constantly reduced, but adsorption efficiency gradually increases, thus it is speculated that is derived from the total specific surface area of increase and total functional group number of quantity of sorbent
Increase caused by, and the adsorbance of biological carbon microspheres counterweight metal ion and removal efficiency are above biomass.Work as adsorbent
When dosage is 10mg, two kinds of (hydrothermal synthesis product and hydrothermal synthesis-pyrolysis activation are prepared) biological carbon microspheres counterweight metals
The adsorbance of ion is maximum, but removal rate at this time is minimum, and removal rate is respectively less than 15%；When adsorbent additive amount is 20mg
When, adsorbance and removal rate have apparent increase, continue thereafter with increase adsorbent amount, and the two increase is slowed by.Comprehensively consider
Adsorbance and removal rate and absorption post-processing, selection adsorbent additive amount are 20mg.
Better embodiment of the invention is illustrated above, but the invention is not limited to the implementation
Example, those skilled in the art can also make various equivalent modifications on the premise of without prejudice to spirit of the invention or replace
It changes, these equivalent variation or replacement are all included in the scope defined by the claims of the present application.
Claims (10)
1. a kind of preparation method of biology carbon microspheres, which comprises the following steps:
(1) pretreatment of raw material: pomelo peel is cut, and is only left white flesh in color after cutting off bluish yellow color crust, by drying, powder
After broken, sieving, flesh powder in flaxen pomelo peel is obtained；
(2) hydrothermal synthesis: flesh powder and deionized water in pomelo peel are placed in hydrothermal reaction kettle, then by reaction kettle it is closed after
It is placed in heating in baking oven and carries out hydrothermal synthesis；The solid product in suspension is filtered after reaction kettle is cooled to room temperature,
It is washed with deionized again to filtrate and is clarified, then dry solid product to obtain hydrothermal synthesis product；
(3) pyrolysis activation: hydrothermal synthesis product being placed in tube furnace, pyrolysis processing in nitrogen atmosphere, and activation obtains charcoal
Microballoon.
2. the preparation method of biology carbon microspheres according to claim 1, which is characterized in that in step (1), the pomelo peel
Interior flesh powder crosses 60~100 meshes.
3. the preparation method of biology carbon microspheres according to claim 1, which is characterized in that in step (2), flesh in pomelo peel
Powder and the material ratio of deionized water are (1~5) g:60mL, preferably flesh powder in 1g, 2g, 3g, 4g or 5g pomelo peel: 60mL
Deionized water.
4. the preparation method of biology carbon microspheres according to claim 1, which is characterized in that in step (2), hydrothermal synthesis temperature
Degree is 160~220 DEG C, preferably 160 DEG C, 180 DEG C, 200 DEG C or 220 DEG C.
5. the preparation method of biology carbon microspheres according to claim 1 or 4, which is characterized in that in step (2), hydro-thermal is closed
It is 2~8h, preferably 2h, 4h, 6h or 8h at the time.
6. the preparation method of biology carbon microspheres according to claim 1, which is characterized in that in step (3), pyrolysis temperature is
500~700 DEG C, preferably 500 DEG C, 600 DEG C or 700 DEG C.
7. the preparation method of biological carbon microspheres according to claim 1 or 6, which is characterized in that in step (3), at pyrolysis
The reason time is 1~4h, preferably 1h, 2h, 3h or 4h.
8. a kind of biology carbon microspheres, which is characterized in that be made by the described in any item preparation methods of claim 1~7.
9. biology carbon microspheres according to claim 8, which is characterized in that the partial size of the biology carbon microspheres is 3~5 μm.
10. biological carbon microspheres are heavy metal ion adsorbed as adsorbent progress as claimed in claim 8 or 9 for application.
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Cited By (6)
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| CN110523379A (en) * | 2019-09-25 | 2019-12-03 | 东北农业大学 | A kind of low cost preparation method of porous charcoal |
| CN111974349A (en) * | 2020-08-14 | 2020-11-24 | 大连工业大学 | Porous lignin hydrothermal carbon-based phosphate adsorbent and preparation method thereof |
| CN112108138A (en) * | 2019-06-21 | 2020-12-22 | 华南农业大学 | Biomass hydrothermal carbon carrier catalyst and preparation method and application thereof |
| CN114236182A (en) * | 2021-12-17 | 2022-03-25 | 西安建筑科技大学 | Preparation method of carbon microsphere colloid probe |
| CN114478086A (en) * | 2020-11-12 | 2022-05-13 | 深圳市海立方生物科技有限公司 | Full-scale treatment method for kitchen garbage |
| CN114984909A (en) * | 2022-06-10 | 2022-09-02 | 佛山科学技术学院 | Preparation method of manganese chloride and potassium hydroxide modified biochar |
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Cited By (7)
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| CN110523379A (en) * | 2019-09-25 | 2019-12-03 | 东北农业大学 | A kind of low cost preparation method of porous charcoal |
| CN111974349A (en) * | 2020-08-14 | 2020-11-24 | 大连工业大学 | Porous lignin hydrothermal carbon-based phosphate adsorbent and preparation method thereof |
| CN114478086A (en) * | 2020-11-12 | 2022-05-13 | 深圳市海立方生物科技有限公司 | Full-scale treatment method for kitchen garbage |
| CN114236182A (en) * | 2021-12-17 | 2022-03-25 | 西安建筑科技大学 | Preparation method of carbon microsphere colloid probe |
| CN114984909A (en) * | 2022-06-10 | 2022-09-02 | 佛山科学技术学院 | Preparation method of manganese chloride and potassium hydroxide modified biochar |
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Application publication date: 20190111 |