CN107311139A - The meso-porous carbon material prepared by carbon source of glucose and its application - Google Patents
The meso-porous carbon material prepared by carbon source of glucose and its application Download PDFInfo
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- CN107311139A CN107311139A CN201710307664.6A CN201710307664A CN107311139A CN 107311139 A CN107311139 A CN 107311139A CN 201710307664 A CN201710307664 A CN 201710307664A CN 107311139 A CN107311139 A CN 107311139A
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/14—Pore volume
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
- C01P2006/17—Pore diameter distribution
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/20—Total organic carbon [TOC]
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- Hydrology & Water Resources (AREA)
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- Environmental & Geological Engineering (AREA)
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Abstract
The present invention discloses a kind of meso-porous carbon material prepared by carbon source of glucose, and its making includes following steps：（1）Glucose is dissolved in H2SO4And H2In O mixed solution, stir stand-by；（2）Carbon source is filled by the way of decompression suction filtration；（3）Filtrate after collection is added dropwise on template again, regathers filtrate；（4）Remaining a small amount of filtrate is mixed with filter cake after the completion of suction filtration, and stirred；（5）Mixture heats 6 h at 100 DEG C, then heats 6 h under the conditions of being placed in 150 DEG C, is tentatively carbonized；（6）Secondary filling；（7）After mixture is taken out, under High Purity Nitrogen protection, 1.5 h are calcined in 750 DEG C of high temperature, programming rate is 10 DEG C/min.By the meso-porous carbon material prepared by carbon source of glucose, when tail water initial pH value is 5~7, MC glucose are optimal to TOC adsorption capacity, and its TOC clearance reaches 99%.PH value need not be readjusted before adsorption experiment is carried out, can be directly used for handling sewage, it is easy to use.
Description
Technical field
The present invention relates to carbon material art, the meso-porous carbon material that is prepared by carbon source of glucose is referred in particular to and its should
With.
Background technology
Mesoporous carbon is the new non-silicon-based mesoporous material of a class, and compared with pure mesoporous silicon material, meso-porous carbon material is shown
Special property, there is high specific surface area, high porosity；Aperture size is adjustable within the specific limits；Mesoporous various shapes, hole wall
Composition, structure and property are adjustable；High thermal stability and hydrothermal stability can be obtained by optimum synthesis condition；Synthesis is simple,
Easy to operate, physiological-toxicity-free.Its tempting part also resides in it in fuel cell, molecular sieve, absorption, catalytic reaction, electrochemistry
Deng the potential using value in field.In recent years, mesoporous material science is had become in the world across chemistry, physics, material, biology etc.
One of hot research field of subject crossing, the important milestone more developed as material science.
Current its TOC of meso-porous carbon material clearance is relatively low, it is impossible to directly apply to and sewage is handled, using compared with
For inconvenience.Therefore, necessity is improved to current meso-porous carbon material.
The content of the invention
In view of this, the present invention in view of the existing deficiencies of the prior art, its main purpose be to provide it is a kind of using glucose as
Meso-porous carbon material and its application prepared by carbon source, it can effectively solve existing meso-porous carbon material and be not directly applicable to sewage
The problem of being handled.
To achieve the above object, the present invention is using following technical scheme：
A kind of meso-porous carbon material prepared by carbon source of glucose, its making includes following steps：
（1）Glucose is dissolved in H2SO4And H2In O mixed solution, stir stand-by；
（2）Carbon source is filled by the way of decompression suction filtration, template is laid on the filter paper of Buchner funnel, and by step（1）
The mixed solution of preparation is added dropwise on template, and filtrate is by bottle,suction access and collects；
（3）Filtrate after collection is added dropwise on template again, regathers filtrate, and operating 3 times repeatedly is sufficient filling with carbon source；
（4）Remaining a small amount of filtrate is mixed with filter cake after the completion of suction filtration, and stirred；
（5）Mixture heats 6 h at 100 DEG C, to remove moisture removal, then heats 6 h under the conditions of being placed in 150 DEG C, carries out preliminary charcoal
Change；
（6）Secondary filling, the mixture after preliminary charing is smashed to pieces, is laid on the filter paper of Buchner funnel, by glucose,
H2SO4And H2O mixed solution is added dropwise on the mixture, according to step（3）Decompression filling is carried out, filtrate and filter cake mixing is collected
Afterwards, according to step（5）Carry out moisture removal and preliminary charing；
（7）After mixture is taken out, under High Purity Nitrogen protection, 1.5 h are calcined in 750 DEG C of high temperature, programming rate is 10 DEG C/
min；
（8）Sample is cooled to room temperature, 24 h is soaked with 48% HF, with except silicon；
（9）Finally washing sample is dried to without acidity, obtains meso-porous carbon material, be designated as MC-glucose.
It is preferred that, the step（1）Middle glucose is 1.25g, H2SO4For 0.8mL, H2O is 5 mL, step（2）Middle template
Agent is 1.0g, its model SBA-15, step（6）Middle glucose is 0.8g, H2SO4For 0.5 mL, H2O is 5 mL.
A kind of application of the meso-porous carbon material prepared by carbon source of glucose, the mesoporous carbon that will be prepared by carbon source of glucose
Material is delivered into sewage, and TOC removal is carried out to sewage.
The present invention has clear advantage and beneficial effect compared with prior art, specifically, by above-mentioned technical proposal
Understand：
By the meso-porous carbon material prepared by carbon source of glucose, when tail water initial pH value is 5~7, MC-glucose is to TOC's
Adsorption capacity is optimal, and its TOC clearance reaches 99%.《Guangdong Province's integrated wastewater discharge standard》（DB4426-2001）In to tail
The requirement of water pH emission limits is 6~9, and the material optimal adsorption pH value of this experimental study is 7, that is to say, that real carrying out absorption
PH value need not be readjusted before testing, can be directly used for handling sewage, it is easy to use.
Brief description of the drawings
Fig. 1 is the SEM figures of MC-glucose materials in the preferred embodiments of the invention；
Fig. 2 is adsorption isothermal curve figure in the preferred embodiments of the invention；
Fig. 3 is pore volume-pore size distribution curve in the preferred embodiments of the invention（Differential）Figure；
Fig. 4 is the XRF figures of MC-glucose materials in the preferred embodiments of the invention；
Fig. 5 is the FT-IR figures of MC-glucose materials in the preferred embodiments of the invention；
Fig. 6 is influence schematic diagram of the MC-glucose dosages to TOC adsorption effects in the preferred embodiments of the invention；
Fig. 7 is influence schematic diagram of the adsorption time to TOC adsorption effects in the preferred embodiments of the invention；
Influence schematic diagram of Fig. 8 initial pH values to TOC adsorption effects.
Embodiment
Present invention is disclosed a kind of meso-porous carbon material prepared by carbon source of glucose, its making includes following steps：
（1）Glucose is dissolved in H2SO4And H2In O mixed solution, stir stand-by；In the present embodiment, glucose is
1.25g, H2SO4For 0.8mL, H2O is 5 mL.
（2）Carbon source is filled by the way of decompression suction filtration, template is laid on the filter paper of Buchner funnel, and by step
（1）The mixed solution of preparation is added dropwise on template, and filtrate is by bottle,suction access and collects.In the present embodiment, template is
1.0g, its model SBA-15.
（3）Filtrate after collection is added dropwise on template again, regathers filtrate, and operating 3 times repeatedly makes carbon source abundant
Filling.
（4）Remaining a small amount of filtrate is mixed with filter cake after the completion of suction filtration, and stirred.
（5）Mixture heats 6 h at 100 DEG C, to remove moisture removal, then heats 6 h under the conditions of being placed in 150 DEG C, carries out just
Step charing.
（6）Secondary filling, the mixture after preliminary charing is smashed to pieces, is laid on the filter paper of Buchner funnel, by glucose,
H2SO4And H2O mixed solution is added dropwise on the mixture, according to step（3）Decompression filling is carried out, filtrate and filter cake mixing is collected
Afterwards, according to step（5）Carry out moisture removal and preliminary charing.In the present embodiment, glucose is 0.8g, H2SO4For 0.5 mL,
H2O is 5 mL.
（7）After mixture is taken out, under High Purity Nitrogen protection, 1.5 h are calcined in 750 DEG C of high temperature, programming rate is 10
℃/min。
（8）Sample is cooled to room temperature, 24 h is soaked with 48% HF, with except silicon.
（9）Finally washing sample is dried to without acidity, obtains meso-porous carbon material, be designated as MC-glucose.
Separately below meso-porous carbon material sign is carried out using means such as SEM, BET, XRF and FT-IR：
（1）SEM is characterized, as shown in figure 1, being the SEM photograph of MC-glucose meso-porous carbon materials.As seen from the figure, MC-glucose
Material structure is in orderly bar-shaped arrangement, and its duct is main to be formed by rod-shaped particle accumulation, therefore uses glucose for carbon source, is prepared
Obtain orderly carbon material.
（2）BET is characterized, and by BET multiple spot adsorption experiment, the specific surface area of MC-glucose materials is
994.94m2/g, total pore volume is 1.12m3/g, and average pore size is 6.132nm.Fig. 2 and Fig. 3 are respectively MC-glucose materials
N2 absorption/desorption isotherm and pore volume-graph of pore diameter distribution.
From adsorption isothermal curve figure, IV type thermoisopleth and H1 type lag loops is presented in MC-glucose materials.Explanation
The material belongs to meso-porous carbon material, and its pore passage structure is mainly made up of uniform bead string shape hole.Can by empty appearance-pore size distribution curve figure
Know, the carbon material is based on 2.00-10.00nm hole, and it accounts for the 69% of total hole.
（3）XRF is characterized, and Fig. 4 is the XRF figures of MC-glucose materials.As seen from the figure, the material is free of Cu, Cr, Pb, Hg
Deng poisonous and harmful heavy metallic, belong to environment-friendly type adsorbent.
（4）FT-IR is characterized, and Fig. 5 is the FTIR spectrum figure of MC-glucose materials.As seen from the figure, in 3415cm-1
Place produces O-H stretching vibration peak, 1300~1640 cm-1Scope is mainly the stretching vibration peak of C=O and C=C keys, 1000~
1200 cm-1Mainly C-O stretching vibration peak, 400~900 cm-1Region is that some heavy atom stretching vibrations and deformation are shaken
It is dynamic.
The absorption to meso-porous carbon material is tested below：
Test water is derived from tail water of certain printing and dyeing enterprise after biochemical treatment, coagulating sedimentation.
（1）The influence of dosage
50 mg, 100 mg, 150 mg, 200 mg and 250 mg MC-glucose materials are taken to add into equipped with 250 mL respectively
In the conical flask of tail water, i.e., dosage is respectively 200mg/L, 400mg/L, 600mg/L, 800mg/L and 1000mg/L.By taper
Bottle adsorbs 6 h in constant temperature oscillation bed, and water intaking water sample takes clear liquid to determine TOC content after precipitating micro-filtration.Different dosages pair
TOC adsorption effect is shown in Fig. 6 in tail water.
As seen from the figure, TOC clearance increases with the increase of MC-glucose dosages.When MC-glucose throwing
When dosage is 800mg/L, TOC clearance reaches 97.21%, therefore this experiment optimum dosage takes 800mg/L.
（2）The influence of adsorption time
In adsorption process, suitable quantity of water is taken respectively at 5min, 10min, 15min, 30min, 1h, 2h, 3h, 4h, 5h, 6h, 7h and 8h
Sample is filtered, and takes clear liquid to determine the change of its TOC content, and Fig. 7 is influence of the adsorption time to TOC removal effects.
As seen from the figure, when adsorption experiment proceeds to 6h, absorption basically reaches balance, therefore the optimal adsorption time takes in this experiment
6h。
（3）The influence of acid-base value
Investigate acid-base value in tail water influences on MC-glucose absorption property, use NaOH and HCl adjust the pH of tail water for 3,
5th, 7 Fig. 8 is shown in, 9, influences of 12, the pH to material adsorption capacity.
As seen from the figure, when tail water initial pH value is 5~7, MC-glucose is optimal to TOC adsorption capacity, and its TOC's goes
Except rate reaches 99%.《Guangdong Province's integrated wastewater discharge standard》（DB4426-2001）In to the requirement of tail water pH emission limits for 6~
9, the material optimal adsorption pH value of this experimental study is 7, that is to say, that need not readjust pH before adsorption experiment is carried out
Value.
The above described is only a preferred embodiment of the present invention, be not intended to limit the scope of the present invention,
Therefore any subtle modifications, equivalent variations and modifications that every technical spirit according to the present invention is made to above example, still
Belong in the range of technical solution of the present invention.
Claims (3)
1. a kind of meso-porous carbon material prepared by carbon source of glucose, it is characterised in that：Its making includes following steps：
（1）Glucose is dissolved in H2SO4And H2In O mixed solution, stir stand-by；
（2）Carbon source is filled by the way of decompression suction filtration, template is laid on the filter paper of Buchner funnel, and by step（1）
The mixed solution of preparation is added dropwise on template, and filtrate is by bottle,suction access and collects；
（3）Filtrate after collection is added dropwise on template again, regathers filtrate, and operating 3 times repeatedly is sufficient filling with carbon source；
（4）Remaining a small amount of filtrate is mixed with filter cake after the completion of suction filtration, and stirred；
（5）Mixture heats 6 h at 100 DEG C, to remove moisture removal, then heats 6 h under the conditions of being placed in 150 DEG C, carries out preliminary charcoal
Change；
（6）Secondary filling, the mixture after preliminary charing is smashed to pieces, is laid on the filter paper of Buchner funnel, by glucose, H2SO4
And H2O mixed solution is added dropwise on the mixture, according to step（3）Decompression filling is carried out, collects after filtrate and filter cake mixing, presses
According to step（5）Carry out moisture removal and preliminary charing；
（7）After mixture is taken out, under High Purity Nitrogen protection, 1.5 h are calcined in 750 DEG C of high temperature, programming rate is 10 DEG C/
min；
（8）Sample is cooled to room temperature, 24 h is soaked with 48% HF, with except silicon；
（9）Finally washing sample is dried to without acidity, obtains meso-porous carbon material, be designated as MC-glucose.
2. the meso-porous carbon material according to claim 1 prepared by carbon source of glucose, it is characterised in that：The step
（1）Middle glucose is 1.25g, H2SO4For 0.8mL, H2O is 5 mL, step（2）Middle template is 1.0g, its model SBA-
15, step（6）Middle glucose is 0.8g, H2SO4For 0.5 mL, H2O is 5 mL.
3. a kind of application of the meso-porous carbon material as claimed in claim 1 or 2 prepared by carbon source of glucose, its feature exists
In：The meso-porous carbon material prepared by carbon source of glucose is delivered into sewage, TOC removal is carried out to sewage.
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Cited By (5)
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| CN107973287A (en) * | 2017-12-04 | 2018-05-01 | 吉林大学 | A kind of meso-porous carbon material and preparation method thereof |
| CN109437322A (en) * | 2018-11-05 | 2019-03-08 | 浙江工业大学 | A kind of compound carbon ball of metal oxide and preparation method thereof |
| CN110479212A (en) * | 2019-09-12 | 2019-11-22 | 苏州科技大学 | A kind of preparation method and applications of unordered mesoporous carbon adsorbing material |
| CN111762770A (en) * | 2020-05-25 | 2020-10-13 | 浙江工业大学 | Preparation method of oxygen-containing functional group functionalized porous carbon spheres |
| CN113926426A (en) * | 2021-11-11 | 2022-01-14 | 东莞理工学院 | Method for adsorbing phthalate pollutants in wastewater by using functionalized mesoporous carbon |
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| CN113926426A (en) * | 2021-11-11 | 2022-01-14 | 东莞理工学院 | Method for adsorbing phthalate pollutants in wastewater by using functionalized mesoporous carbon |
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Application publication date: 20171103 |