CN105905885A - Preparation method of straw-core carbon material - Google Patents
Preparation method of straw-core carbon material Download PDFInfo
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- CN105905885A CN105905885A CN201610270735.5A CN201610270735A CN105905885A CN 105905885 A CN105905885 A CN 105905885A CN 201610270735 A CN201610270735 A CN 201610270735A CN 105905885 A CN105905885 A CN 105905885A
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- straw core
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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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
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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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
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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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
- C01P2006/12—Surface area
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Abstract
The invention discloses a preparation method of straw-core carbon material. The preparation method includes: washing straw, then taking out straw cores, grinding into powder, evenly mixing deionized water, surfactant PVP and the straw core powder, transferring to a hydrothermal reaction kettle, using hydrochloric acid to regulate pH, sealing the hydrothermal reaction kettle, placing into a drying oven, performing heating reaction, cooling, performing suction filtration, washing, and drying to obtain the carbon material. The preparation method has the advantages the surface of the obtained carbon material is rough, a certain amount of irregular carbon microspheres is formed, and high specific surface area and even particle size are achieved.
Description
Technical field
The present invention relates to biomass carbon technical field of material, particularly relate to the preparation side of a kind of straw core material with carbon element
Method.
Background technology
Straw is a kind of native cellulose biolobic material, is a kind of abundant Renewable resource.Containing abundant in straw
Nutritive value and useful chemical composition, be widely used in industry, agricultural and animal husbandry.But, still there is substantial amounts of straw not have
Being utilized, this not only causes environmental pollution to be also a kind of wasting of resources simultaneously.Owing in straw, carbon content is abundanter, therefore
It is very important for being translated into the material with carbon element with special construction for the field needed.
The method using straw to prepare material with carbon element in prior art has certain defect, as needed to control during template
The production cost that variable is too many, preparation process is more complicated and higher so that template is prepared carbon microspheres and is difficult to extensive work
Industryization is promoted；Pyrolysismethod oxygen-containing functional group under the high temperature conditions also loses totally, and end product purity is relatively low, productivity is the highest,
Raw material used is higher containing toxicity, and the energy simultaneously consumed is huge.
Summary of the invention
The purpose of the present invention is aiming at the defect of above-mentioned existence and provides the preparation method of a kind of straw core material with carbon element.Will
After straw cleans, take out straw core grind into powder, after deionized water, surfactant PVP, straw core powder mix homogeneously
It is transferred in hydrothermal reaction kettle, uses salt acid for adjusting pH value, be placed on airtight for hydrothermal reaction kettle in baking oven, reacting by heating, cooling
After, sucking filtration, rinsing, drying obtain material with carbon element, and the carbon material surface that the present invention obtains is coarse, define a number of charcoal micro-
Ball, carbon microspheres is irregular spherical, and specific surface area is bigger, and particle diameter is the most uniform.
The preparation method technical scheme of a kind of straw core material with carbon element of the present invention is to comprise the following steps:
(1) straw pre-treatment: the straw collected is cleaned post-drying, separates straw core, cuts the section of being cut into by straw core, then
Ball mill grinding is used to become powder standby；
(2) being dissolved in deionized water by surfactant polyvinylpyrrolidone, be subsequently adding straw core powder, mixing is all
It is transferred to after even in hydrothermal reaction kettle, mix homogeneously, uses salt acid for adjusting pH value, be placed on airtight for hydrothermal reaction kettle in baking oven,
Reacting by heating, after reaction terminates, is cooled to room temperature by reactor；
(3) reacted liquid use microporous filter membrane is carried out sucking filtration, gained filter cake deionized water rinsing 3 ~ 5 times, Yu Gan
Dry case is dried to obtain material with carbon element powder.
In step (2), straw core powder concn is 20 ~ 50 g/L.
In step (2), hydrothermal reaction kettle is placed in baking oven, and heating-up temperature is 160 ~ 250 DEG C.
In step (2), the reacting by heating time is 4 ~ 12 hours.
Step (2) is 2 ~ 10 with salt acid for adjusting pH value.
Polyvinylpyrrolidoneconcentration concentration is 1 ~ 6 g/35 mL.
12 h it are dried under the conditions of drying condition is 80 DEG C in step (3).
In step (3), microporous filter membrane is 3. 50 mm*0.22 μm.
The preparation method of a kind of straw core material with carbon element of the present invention has the beneficial effect that the present invention uses straw core to pass through hydro-thermal
Material with carbon element is prepared in carbonization, and hydro-thermal carbonization cracks charring process compared to tradition, has significant advantage, as reaction condition is gentle,
In abandoned biomass, carbon fixed efficiency is high, and processing equipment is simple, and energy consumption is low, adds surface and live during carbonization reaction
Property agent PVP, can make carbon microspheres rough surface, and the charcoal ball of formation is more, and carbon microspheres is irregular spherical, specific surface area
Bigger, particle diameter is the most uniform.Surfactant is in the hydro-thermal carbonization reaction of straw, it is possible to improve the pattern of carbon microspheres, increases
The specific surface area of big charcoal ball, homogenizes crystal grain.
Accompanying drawing illustrates:
Fig. 1 show the XRD figure spectrum of straw core powder；
Fig. 2 show the XRD figure spectrum of embodiment 1 gained material with carbon element；
Fig. 3 show the SEM figure of prepared material with carbon element；
Fig. 4 show different surfaces activating agent PVP addition affects figure to material with carbon element absorption property；
Fig. 5 show the material with carbon element SEM figure prepared when adding PVP.
Detailed description of the invention:
In order to be more fully understood that the present invention, describe technical scheme in detail with instantiation below, but the present invention
It is not limited thereto.
Embodiment 1
Step
It is as follows that straw hydro-thermal method prepares material with carbon element step:
(1) straw pre-treatment: the straw collected is cleaned post-drying, then straw core is stripped out, and with shears by straw
The stalk core hammer-shears section of being cut into, re-uses ball mill grinding and becomes powder standby.
(2) weighing appropriate straw core powder and join in deionized water, straw core powder concn is 20 ~ 50 g/L, stirring
In thermal response of uniformly falling back still, it is 2 ~ 10 with salt acid for adjusting pH value, is placed on airtight for reactor in baking oven, is heated to
160 ~ 250 DEG C and keep 4 ~ 12 hours, after reaction terminates, reactor is cooled to room temperature.
(3) reacted liquid use 50 mm*0.22 μm microporous filter membrane carry out sucking filtration, gained filter cake deionization
Water rinses 3 ~ 5 times, is then transferred in Constant Temp. Oven, is dried 12 h under the conditions of 80 DEG C, the carbon material after drying
Material mortar grinder becomes powder standby.
Adsorption experiment
Selecting the Cr VI standard solution of 1 mg/L to do adsorption experiment herein, specific experiment step is as follows:
(1) the six price standard solution of 1 mg/L are prepared.
(2) weighing material with carbon element three parts respectively, portion joins and does void item in deionized water, and remaining two parts are added separately to
The Cr VI standard solution of 1mg/L does experiment item, after magnetic agitation, stands 10 hours.
(3) the solid carbon microsphere after using 50 mm*0.22 μm microporous filter membrane sucking filtration to go out absorption, takes filtrate 10 mL, point
Do not add sulphuric acid 0.11 mL of phosphoric acid 0.11 mL, 1:1 of 1:1, developer 0.43 mL, stand 10 minutes, then use
Spectrophotometric measures absorbance.
(4) according to absorbance, the adsorption efficiency of corresponding material with carbon element is calculated.
Material with carbon element prepared under optimum process condition can reach 59.08%, and root to the adsorption efficiency of hexavalent chromium
Calculate its adsorption capacity according to formula 3.1, be 1.182 mg/g.
q = (C 0 V-CV)/m (3.1)
In formula 3.1,q: adsorption capacity, mg/g；C 0 : adsorb forward and backward Cr (VI) concentration, mg/L；V 0 : molten after absorption
The volume of liquid, L；C: Cr (VI) concentration after absorption；V: the volume of solution, L after absorption；m: add the quality of wheat stalk, g.
By using XRD diffraction approach to characterize the curvilinear motion of material with carbon element after stalk and hydro-thermal carbonization, and then research
Straw core is the change of structure in hydro-thermal method prepares biomass carbon materials process.XRD diffraction pattern such as Figure of description Fig. 1 and Fig. 2
Shown in.
By comparison diagram 1, Fig. 2 it is found that straw core is after experienced by hydro-thermal carbonization reaction, the steamed bread peak of raw material disappears
Losing, product carbon microspheres diffraction maximum near 23 DEG C has become sharply many, and peak value has increased, and this represents product charcoal
The degree of graphitization of microsphere is higher.
Use SEM to observe the pattern of hydro-thermal material with carbon element, ask for an interview shown in Figure of description Fig. 3.Can by Figure of description Fig. 3
To find out, under optimum process condition, the carbon microspheres surface of preparation is more smooth, and particle diameter is about between 0.5 μm-4 μm.
Embodiment 2
The PVP impact on hydro-thermal carbonization
Surfactant can improve the pattern of material with carbon element, improves the conversion ratio of carbon microspheres, improves the absorption property of material with carbon element.
Under optimum process condition, in hydro-thermal reaction system, it is separately added into 0.5,0.875,1.5,2.0,4.0,6.0 g
Surfactant PVP, have main steps that: in certain volume water, add appropriate PVP, be stirring evenly and then adding into a certain amount of
Straw core powder, under optimum process condition, carry out hydro-thermal reaction.Material with carbon element prepared by utilization processes the sexavalence of 1 mg/L
Chromium standard solution, uses spectrophotography to test its absorption property, compares the addition of the PVP shadow to material with carbon element absorption property
Ring.Ask for an interview table 1 and Figure of description Fig. 4.
Table 1 PVP concentration is on straw-carbonized impact
。
Fig. 4 is that different surfaces activating agent PVP addition affects figure to material with carbon element absorption property.
It is properly added surfactant and can improve the absorption property of material with carbon element, can find out intuitively from Fig. 4, along with
The increase of surfactant PVP amount, chromic adsorbance is first raised and reduces afterwards by material with carbon element, when PVP addition is 4.0 g/
During 35 mL, it is thus achieved that carbon microspheres absorption property best.
Material with carbon element affects SEM characterize
Use SEM to observe the PVP impact on the pattern of hydro-thermal carbonization reaction product material with carbon element, and then research straw core is in hydro-thermal
Method prepares effect and the mechanism of the surfactant PVP in biomass carbon materials process.Gained SEM photograph such as Figure of description figure
Shown in 5.
Under same hydrothermal condition, do not add Fig. 3 of surfactant PVP and add the surfactant of 2 g/35 mL
Fig. 5 of PVP compares, and adds carbon microspheres rough surface in Fig. 5 of PVP, and the charcoal ball of formation is more, and carbon microspheres is not
Regular is spherical, and specific surface area is bigger, and particle diameter is the most uniform.Carbon microspheres surface is played by this addition being likely due to PVP
The effect modified, the hydrophobic group of parcel carbon microspheres, exposed hydrophilic group, thus effectively control pattern.
Claims (8)
1. the preparation method of a straw core material with carbon element, it is characterised in that comprise the following steps:
(1) straw through cleaning, dry, to obtain straw core powder after ball milling standby；
(2) being dissolved in deionized water by surfactant polyvinylpyrrolidone, be subsequently adding straw core powder, mixing is all
It is transferred to after even in hydrothermal reaction kettle, mix homogeneously, uses salt acid for adjusting pH value, be placed on airtight for hydrothermal reaction kettle in baking oven,
Reacting by heating, after reaction terminates, is cooled to room temperature by reactor；
(3) reacted liquid use microporous filter membrane is carried out sucking filtration, gained filter cake deionized water rinsing 3 ~ 5 times, Yu Gan
Dry case is dried to obtain material with carbon element powder.
The preparation method of a kind of straw core material with carbon element the most according to claim 1, it is characterised in that in step (2),
Straw core powder concn is 20 ~ 50 g/L.
The preparation method of a kind of straw core material with carbon element the most according to claim 1, it is characterised in that water in step (2)
Thermal response still is placed in baking oven, and heating-up temperature is 160 ~ 250 DEG C.
The preparation method of a kind of straw core material with carbon element the most according to claim 1, it is characterised in that step adds in (2)
The thermal response time is 4 ~ 12 hours.
The preparation method of a kind of straw core material with carbon element the most according to claim 1, it is characterised in that use in step (2)
Salt acid for adjusting pH value is 2 ~ 10.
The preparation method of a kind of straw core material with carbon element the most according to claim 1, it is characterised in that polyvinylpyrrolidine
Ketone concentration is 1 ~ 6 g/35 mL.
The preparation method of a kind of straw core material with carbon element the most according to claim 1, it is characterised in that dry in step (3)
Dry condition is dried 12 h under the conditions of being 80 DEG C.
The preparation method of a kind of straw core material with carbon element the most according to claim 1, it is characterised in that micro-in step (3)
Hole filter membrane is 50 mm*0.22 μm.
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| CN201610270735.5A CN105905885A (en) | 2016-04-27 | 2016-04-27 | Preparation method of straw-core carbon material |
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| CN201610270735.5A CN105905885A (en) | 2016-04-27 | 2016-04-27 | Preparation method of straw-core carbon material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113604510A (en) * | 2021-07-12 | 2021-11-05 | 复旦大学 | Method for improving efficiency of methane production through hydrothermal carbon enhanced anaerobic digestion |
| CN116621581A (en) * | 2023-04-24 | 2023-08-22 | 西南林业大学 | Thermosetting resin foam carbon and preparation method thereof |
Citations (3)
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| CN102815689A (en) * | 2012-08-22 | 2012-12-12 | 华北电力大学 | Preparation method of carbon micron ball material with even particle size |
| CN103588190A (en) * | 2013-10-31 | 2014-02-19 | 中国科学院过程工程研究所 | Method for preparation of carbon microsphere from lignocellulose |
| CN105355464A (en) * | 2015-11-10 | 2016-02-24 | 西安科技大学 | Mesopore-micropore carbon micro sphere of high specific surface area for super capacitor and preparation method of carbon micro sphere |
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2016
- 2016-04-27 CN CN201610270735.5A patent/CN105905885A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102815689A (en) * | 2012-08-22 | 2012-12-12 | 华北电力大学 | Preparation method of carbon micron ball material with even particle size |
| CN103588190A (en) * | 2013-10-31 | 2014-02-19 | 中国科学院过程工程研究所 | Method for preparation of carbon microsphere from lignocellulose |
| CN105355464A (en) * | 2015-11-10 | 2016-02-24 | 西安科技大学 | Mesopore-micropore carbon micro sphere of high specific surface area for super capacitor and preparation method of carbon micro sphere |
Non-Patent Citations (2)
| Title |
|---|
| TREVOR MWENYA ET.AL: "The Detailed Evolution of Carbon Spheres by Hydrothermal Method", 《INTERNATIONAL JOURNAL OF PHOTOENERGY》 * |
| 杨继生: "《表面活性剂原理与应用》", 31 December 2012, 东南大学出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113604510A (en) * | 2021-07-12 | 2021-11-05 | 复旦大学 | Method for improving efficiency of methane production through hydrothermal carbon enhanced anaerobic digestion |
| CN116621581A (en) * | 2023-04-24 | 2023-08-22 | 西南林业大学 | Thermosetting resin foam carbon and preparation method thereof |
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Effective date of registration: 20170208 Address after: 250353 Ji''nan, Changqing Province University Road, No. 3501, Qilu University of Technology Applicant after: Qilu University of Technology Address before: Feng Ming Licheng District Lingang Development Zone, 250101 Ji'nan Road, Shandong Province Applicant before: Shandong Construction University |
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Application publication date: 20160831 |