CN106829923A - A kind of biomass carbon material and preparation method - Google Patents

A kind of biomass carbon material and preparation method Download PDF

Info

Publication number
CN106829923A
CN106829923A CN201710157984.8A CN201710157984A CN106829923A CN 106829923 A CN106829923 A CN 106829923A CN 201710157984 A CN201710157984 A CN 201710157984A CN 106829923 A CN106829923 A CN 106829923A
Authority
CN
China
Prior art keywords
preparation
initial stage
biomass carbon
charcoal
carbon materials
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201710157984.8A
Other languages
Chinese (zh)
Inventor
代斌
祁佩荣
王超
于锋
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shihezi University
Original Assignee
Shihezi University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Shihezi University filed Critical Shihezi University
Priority to CN201710157984.8A priority Critical patent/CN106829923A/en
Publication of CN106829923A publication Critical patent/CN106829923A/en
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/70Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72Crystal-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
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/01Particle morphology depicted by an image
    • C01P2004/03Particle morphology depicted by an image obtained by SEM
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/12Surface area
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/14Pore volume
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/16Pore diameter
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/16Pore diameter
    • C01P2006/17Pore diameter distribution

Landscapes

  • Carbon And Carbon Compounds (AREA)

Abstract

The present invention is a kind of biomass carbon material and preparation method, is related to technical field of carbon material preparation.The preparation method is comprised the following steps:(1) charcoal source mixed liquor is prepared:Biomass carbon source is added in deionized water, is stirred, obtain charcoal source mixed liquor;(2) combustion fluid is prepared:To incendiary agent, oxidant and foaming agent is added in the mixed liquor of charcoal source, stir, obtain combustion fluid;(3) calcination combustion liquid, obtains initial stage Carbon Materials;(4) initial stage Carbon Materials are washed;(5) the initial stage Carbon Materials after washing are dried, described biomass carbon material is obtained.A kind of biomass carbon material of the present invention and preparation method, using solution combustion method, very energy saving, and can be with a step into charcoal;Preparation method is simple, short preparation period, favorable repeatability;The nano thin-layer structure of obtained biomass carbon material is homogeneous, and microstructure and specific surface area are preferable.

Description

A kind of biomass carbon material and preparation method
Technical field
The invention belongs to technical field of carbon material preparation, and in particular to a kind of biomass carbon material and preparation method.
Background technology
Carbon nano-material refers at least one-dimensional structural type Carbon Materials less than 100nm of dispersed phase yardstick, main comprising richness Strangle alkene, nano carbon tube, Graphene and mesoporous nano charcoal etc..Carbon nano-material have that good stability, intensity be high, specific surface area is high and The features such as abundance, be most potential novel nano-material, has been applied to composite, ultracapacitor, storage Hydrogen material, catalyst equal energy source chemical field, or even as irreplaceable material in frontier high.Country《New material industry " 12 " development plan》It is determined that new function material, advanced configuration material and high-performance composite materials etc. are given priority to, in recent years Carry out the fast development of carbon nano-material research also for its development and application in chemical industry catalysis material field provides platform.Future is most The product for being possible to realize industrial applications is energy storage hydrogen storage device, advanced composite material (ACM) and catalyst.
Traditional Carbon Materials are that primary raw material is prepared by working process by coal, oil etc., but nowadays in global range The deterioration of energy crisis and ecological environment, is restricted the further development of traditional Carbon Materials, develops renewable resources And be translated into the energy and had important practical significance with various materials.Biomass carbon material is to utilize biomass for raw material system Standby various Carbon Materials.Biomass refer to the various organisms formed by photosynthesis, including all of animals and plants and micro- It is biological.And so-called biomass energy, it is exactly form of energy that solar energy is stored in biomass in chemical energy form, i.e., with biomass It is the energy of carrier.It directly or indirectly from green plants photosynthesis, can be converted into conventional solid-state, liquid and Fuel gas, it is inexhaustible, nexhaustible, it is a kind of regenerative resource, while being also a kind of unique reproducible charcoal source.With life Material prepares Carbon Materials for raw material, can reduce the production cost of Carbon Materials, realizes the sustainable development of Carbon Materials.
In recent years, many scientists are being devoted to grinding for the preparation of novel biomass class carbon nano-material and potential application Study carefully.It is prepared by raw material such as with using cotton stalk, bagasse, rice husk, tealeaf residue, jujube core, pomelo peel, cocoanut shell agricultural waste material Carbon based material, but above method technique is cumbersome, and the production cycle is long, the carbon nano-material poor plasticity produced, ratio of easily reuniting Surface area is relatively low.
In view of this, it is necessary to propose a kind of new biomass carbon material and preparation method.
The content of the invention
It is an object of the invention to provide a kind of preparation method of biomass carbon material, the method process is simple improves The performance of product.
To achieve these goals, the technical solution adopted in the present invention is:
A kind of preparation method of biomass carbon material, comprises the following steps:
(1) charcoal source mixed liquor is prepared:Biomass carbon source is added in deionized water, is stirred, obtain the mixing of charcoal source Liquid;The biomass carbon source is the one kind in glucose, fructose, starch, agricultural crop straw and pericarp;
(2) combustion fluid is prepared:To incendiary agent, oxidant and foaming agent is added in the mixed liquor of charcoal source, stir, must burn Liquid;The incendiary agent is the one kind in citric acid, glycine and urea, and the oxidant is salpeter solution, sulfuric acid solution, Gao Meng One kind in sour potassium and sodium hypochlorite, the foaming agent is in hydrogenperoxide steam generator, sodium fluoride, sodium carbonate and sodium acid carbonate Kind;
(3) combustion fluid is calcined 10-90 minutes at a temperature of 150-450 DEG C, then is warming up to 500-800 DEG C, calcining 10- 300 minutes, room temperature is naturally cooled to, obtain initial stage Carbon Materials;
(4) initial stage Carbon Materials are washed:First it is washed with deionized initial stage Carbon Materials, then with absolute ethanol washing initial stage raw material of wood-charcoal Material, the initial stage Carbon Materials after being washed;
(5) the initial stage Carbon Materials after washing are dried, described biomass carbon material is obtained.
Further, in the step (1), biomass carbon source is 2-5 with the mass ratio of charcoal source mixed liquor:10.
Further, after the agricultural crop straw and pericarp dry naturally, then 100-120 mesh sieves were crushed.
Further, in the step (2), biomass carbon source is 1 with the mass ratio of incendiary agent:0.01-0.5;
The biomass carbon source is 1 with the mass ratio of potassium permanganate or sodium hypochlorite:0.001-0.5;
Charcoal source mixed liquor is 1 with the volume ratio of salpeter solution or sulfuric acid solution:0.01-0.5;
The biomass carbon source is 1 with the mass ratio of sodium fluoride or sodium carbonate or sodium acid carbonate:0.001-0.5;
Charcoal source mixed liquor is 1 with the volume ratio of hydrogenperoxide steam generator:0.01-0.5.
Further, the mass fraction of the salpeter solution is 30%-65%, the quality point of the hydrogenperoxide steam generator Number is 20%-40%, and the mass fraction of the sulfuric acid solution is 50-98%.
Further, the step (4) also includes:It is washed with deionized after initial stage Carbon Materials 3-4 times, then uses acetone Washing initial stage 1-2 material of charcoal, uses absolute ethanol washing initial stage Carbon Materials 3-4 times again afterwards.
Further, in the step (5), dry temperature is 50-80 DEG C, and drying time is 10-15 hours.
Another object of the present invention is to provide a kind of biomass carbon material, and the biomass carbon material is by the above method Prepare, it has the advantages that good microstructure and specific surface area.
Compared with prior art, the beneficial effects of the present invention are:
1st, preparation method process is simple of the present invention, short preparation period, favorable repeatability.
2nd, the present invention uses solution combustion method, and it is anti-that the driving force of solution combustion comes from internal highly exothermic redox Should, the energy input needed for preparation process is only to light reaction, therefore very energy saving, and can be with a step into charcoal.
3rd, biomass carbon material of the present invention is prepared from using solution combustion method, and reaction speed is fast, can prevent generation Nano-particle reunite, the nano thin-layer structure of obtained Carbon Materials is homogeneous.
Brief description of the drawings
Fig. 1 is the N of the biomass carbon material of embodiment of the present invention 1 and embodiment 52Adsorption desorption curve map.
Fig. 2 is the pore volume and graph of pore diameter distribution of the biomass carbon material of embodiment of the present invention 2 and embodiment 5.
Fig. 3 is the XRD of the biomass carbon material of embodiment of the present invention 3 and embodiment 4.
Fig. 4 is the SEM figures of the biomass carbon material of embodiment of the present invention 3.
Fig. 5 is the SEM figures of the biomass carbon material of embodiment of the present invention 5.
Specific embodiment
In order to a kind of biomass carbon material of the invention and preparation method is expanded on further, expected goal of the invention is reached, below With reference to preferred embodiment, to according to a kind of biomass carbon material proposed by the present invention and preparation method, its specific embodiment, knot Structure, feature and effect, describe in detail as after.In the following description, different " embodiment " or " embodiment " refers to not necessarily It is same embodiment.Additionally, the special characteristic, structure or feature in one or more embodiments can be combined by any suitable form.
Before a kind of biomass carbon material of the invention and preparation method is elaborated, it is necessary to what is referred in the present invention Method is described further, to reach more preferable effect.
Combustion synthesis method is a kind of quick, preparation method of energy-conservation.At present, conbustion synthesis have been used for synthesis more than 1000 Plant oxide powder.Physical property and reaction medium based on reactant, conbustion synthesis can be divided into Self- propagating Sintering Synthetic and Solution combustion synthesizes.Self- propagating Sintering Synthetic carries out materials synthesis using the self- propagating exothermic reaction occurred between reactant;Its Maximum the characteristics of is the sustainable supply that external energy is not needed in building-up process, and spontaneous maintenance is gone down by after lighting, That is self- propagating characteristic.Solution combustion method, water is dissolved in by soluble reactant, can reach the uniform mixing of molecular level, instead Answer temperature relatively low;And reaction speed is fast, the nano-particle of generation can be prevented from reuniting.Thus it is applied to the preparation of nano material. In 1988, Patil etc. reported solution combustion synthesis for the first time, using urea and Al (NO3)3·9H2The reaction of O is obtained Al2O3.Solution combustion synthesizes with metal nitrate and organic-fuel as reactant, using the redox of heat release between the two React and formed and be able to can be provided by its internal chemical reaching the purpose of self- propagating, i.e. product lattice.So, solution combustion synthesis The extraneous temperature for providing of needs is relatively low, triggering combustion reaction (reaching ignition temperature) is only used for, different from prior synthesizing method The middle lasting input for needing outside energy promotes lattice to be formed.
Solution combustion method prepares the process is simple of biomass carbon material, and easy to operate, yield is high.The driving force of solution combustion Come from the chemical energy of inside, the chemical energy derives from highly exothermic redox reaction.Topmost energy in preparation process Consumption is the dehydration of solution, and required energy input is only to light reaction.Therefore, the temperature required for solution combustion synthesis Degree only need to be higher than ignition temperature, thus the synthetic route very energy-conservation.Reaction can be divided into five stages, first stage:By solution The boiling point of water is heated to from room temperature;Second stage:Due to the evaporation of water, solution temperature is maintained at 100 DEG C;Phase III:Completely After dehydration, gained xerogel continues to be heated and cause temperature to rise, and during this, the gas in vapor and foaming agent is fast Speed volatilization is manufactured that substantial amounts of pore structure;Fourth stage:Once temperature reaches ignition temperature, predecessor is ignited, and occurs certainly Propagating combustion reacts.5th stage:Natural cooling.Then unnecessary soluble metallic salt is washed with solution and is taken out of, needed for obtaining The biomass carbon material wanted.
Cardinal principle of the invention is:With the evaporation of moisture, combustion fluid forms jelly, the decomposition of foaming agent and moisture Evaporation, substantial amounts of pore structure is manufactured on jelly.Incendiary agent reaches burning-point and combustion reaction occurs first, afterwards in oxidant Heat release side occurs should carry out proceeding for maintenance reaction.
Muffle furnace is preheated to 150-450 DEG C by calcination process in the present invention, and combustion fluid then is put into Muffle furnace, makes foaming Agent and vapor acutely discharge, and reach the purpose of pore-creating., it is necessary to a period of time burns completely after incendiary agent ignites, in this temperature Point is stopped 10-90 minutes, continues to be warmed up to 500-800 DEG C, is kept for 10-300 minutes.On the one hand this process burns the knot in charcoal Brilliant water, the structure of one side stabilization charcoal.Then Temperature fall.
Wash, laboratory washing operation is:Precipitation is transferred to filter (by funnel, filter paper, beaker and fixing device group Into) in, to adding wash solution not treat washings in funnel, but liquid level is less than filter paper edge, under allowing liquid to flow into naturally In the undertaking beaker in face, treat that wash solution flows to end.Period cannot be stirred with glass bar, in order to avoid scratch filter paper.Washed in the present invention The process washed is that (soluble slaine, these slaines are on the one hand from additional hair for the ash content taken out of in Carbon Materials Infusion or oxidant or incendiary agent etc., the on the one hand mineral matter element from biomass in itself).
Drying is to remove the wash solution in Carbon Materials in the present invention.
Preferably, being repeated several times in laboratory can obtain nano thin-layer raw material of wood-charcoal to the repeatability of preparation method of the present invention Material.
The present invention enters metal target when combustion fluid is prepared in combustion fluid, can be with shape during charing Into metal oxide, such that it is able to obtain the activated carbon of extraordinary application.
After the method referred in having understood the present invention, below in conjunction with specific embodiments, to of the invention a kind of raw Material Carbon Materials and preparation method are further described in detail:
Embodiment 1.
Concrete operation step is as follows:
(1) charcoal source mixed solution is prepared:The glucose of 10g is weighed, is added in the beaker of the deionized water equipped with 20ml, Stirring obtains charcoal source mixed solution to being completely dissolved.(glucose is 1 with the mass ratio of charcoal source mixed solution:3)
(2) combustion fluid is prepared:To glycine, the salpeter solution and 1ml that 1ml mass fractions are 65% that 1g is added in beaker Mass fraction is 25% hydrogenperoxide steam generator, stirs and incendiary agent is completely dissolved, and obtains combustion fluid.(biomass carbon Source is 1 with the mass ratio of incendiary agent:0.1, the volume of charcoal source mixed solution:The volume of oxidant:Volume=20 of foaming agent:1: 1=1:0.05:0.05)
(3) combustion fluid is transferred in crucible, is put into and is preheated in 300 DEG C of Muffle furnace, calcined 30 minutes, continue to heat up To 500 DEG C, calcine 60 minutes, taking-up naturally cools to room temperature, obtains initial stage Carbon Materials.
(4) initial stage Carbon Materials are washed:First it is washed with deionized three times, then with absolute ethanol washing three times, is washed Initial stage Carbon Materials afterwards.
(5) the initial stage Carbon Materials after washing are dried 12 hours at a temperature of 60 DEG C, obtains biomass carbon material.
Table 1
As can be drawn from Table 1, glucose has the considerable specific surface of comparing as biomass carbon material prepared by charcoal source Product, reaches 239.13m2/ g, average pore volume is 0.19cm3/ g, average pore size is respectively 2.5nm.As can be seen here, the present embodiment system Standby biomass carbon material has good architectural feature.
From figure 1 it appears that glucose has a huge hysteresis loop as biomass carbon material prepared by charcoal source, say Biomass carbon material prepared by bright the method has abundant pore structure.
A kind of biomass carbon material and preparation method described in the embodiment of the present invention, using solution combustion method, extremely save The energy, and can be with a step into charcoal;Preparation method is simple, short preparation period, favorable repeatability;The nanometer thin of obtained Carbon Materials Rotating fields are homogeneous, and specific surface area is preferable.
Embodiment 2.
Concrete operation step is as follows:
(1) charcoal source mixed solution is prepared:The glucose of 10g is weighed, is added in the beaker of the deionized water equipped with 40ml, Stirring obtains charcoal source mixed solution to being completely dissolved.(glucose is 1 with the mass ratio of charcoal source mixed solution:5)
(2) combustion fluid is prepared:To urea, the sulfuric acid solution and 1ml that 8ml mass fractions are 60% that 0.5g is added in beaker Mass fraction is 40% hydrogenperoxide steam generator, stirs and incendiary agent is completely dissolved, and obtains combustion fluid.(biomass carbon Source is 10 with the mass ratio of incendiary agent:0.5=1:0.05, the volume of charcoal source mixed solution:The volume of oxidant:The body of foaming agent Product=40:8:1=1:0.2:0.025)
(3) combustion fluid is transferred in crucible, is put into and is preheated in 450 DEG C of Muffle furnace, calcined 10 minutes, continue to heat up To 500 DEG C, calcine 3 hours, taking-up naturally cools to room temperature, obtains initial stage Carbon Materials.
(4) initial stage Carbon Materials are washed:First it is washed with deionized three times, then with absolute ethanol washing three times, is washed Initial stage Carbon Materials afterwards.
(5) the initial stage Carbon Materials after washing are dried 10 hours at a temperature of 80 DEG C, obtains biomass carbon material.
As can be seen from Figure 2 come, the aperture of the biomass carbon material that glucose is prepared as charcoal source concentrate on 2-5nm it Between, illustrate material surface it is widely distributed substantial amounts of micropore and meso-hole structure.
A kind of biomass carbon material and preparation method described in the embodiment of the present invention, using solution combustion method, extremely save The energy, and can be with a step into charcoal;Preparation method is simple, short preparation period, favorable repeatability;The nanometer thin of obtained Carbon Materials Rotating fields are homogeneous, and architectural feature is preferable.
Embodiment 3.
Concrete operation step is as follows:
(1) charcoal source mixed solution is prepared:The glucose of 10g is weighed, is added in the beaker of the deionized water equipped with 10ml, Stirring obtains charcoal source mixed solution to being completely dissolved.(glucose is 1 with the mass ratio of charcoal source mixed solution:2)
(2) combustion fluid is prepared:To the carbon of the citric acid, the potassium permanganate of 0.5g and 0.1g that 1g is added in the mixed solution of charcoal source Sour sodium, stirs and incendiary agent is completely dissolved, and obtains combustion fluid.(the quality in biomass carbon source:The quality of incendiary agent:Oxygen The quality of agent:Quality=10 of foaming agent:1:0.5:0.1=1:0.1:0.05:0.01)
(3) combustion fluid is transferred in crucible, is put into and is preheated in 200 DEG C of Muffle furnace, calcined 90 minutes, continue to heat up To 600 DEG C, calcine 30 minutes, taking-up naturally cools to room temperature, obtains initial stage Carbon Materials.
(4) initial stage Carbon Materials are washed:First it is washed with deionized three times, then with absolute ethanol washing three times, is washed Initial stage Carbon Materials afterwards.
(5) the initial stage Carbon Materials after washing are dried 11 hours at a temperature of 80 DEG C, obtains biomass carbon material.
From Fig. 3 and Fig. 4, it can be clearly seen that, glucose occurs obvious as biomass carbon material prepared by charcoal source The characteristic peak of charcoal, and without miscellaneous peak, the biomass carbon material of preparation shows obvious thin layer shape.
A kind of biomass carbon material and preparation method described in the embodiment of the present invention, using solution combustion method, extremely save The energy, and can be with a step into charcoal;Preparation method is simple, short preparation period, favorable repeatability;The nanometer thin of obtained Carbon Materials Rotating fields are homogeneous, and architectural feature is preferable.
Embodiment 4.
Concrete operation step is as follows:
(1) charcoal source mixed solution is prepared:The sucrose of 100g is weighed, is dissolved completely in the deionized water of 200ml, obtain charcoal Source mixed solution.(sucrose is 1 with the mass ratio of charcoal source mixed solution:3)
(2) combustion fluid is prepared:To citric acid, the postassium hypochlorite of 0.5g and 2ml mass that 1g is added in the mixed solution of charcoal source Fraction is 25% hydrogenperoxide steam generator, stirs and incendiary agent is completely dissolved, and obtains combustion fluid.(biomass carbon source Quality:The quality of incendiary agent:Quality=100 of oxidant:1:0.5=1:0.01:0.005, the volume of charcoal source mixed solution:Hair Volume=200 of infusion:2=1:0.01)
(3) combustion fluid is transferred in crucible, is put into and is preheated in 300 DEG C of Muffle furnace, calcined 30 minutes, continue to heat up To 500 DEG C, calcine 4 hours, taking-up naturally cools to room temperature, obtains initial stage Carbon Materials.
(4) initial stage Carbon Materials are washed:First it is washed with deionized four times, is then washed twice with acetone, then uses anhydrous second Alcohol is washed four times, the initial stage Carbon Materials after being washed.
(5) the initial stage Carbon Materials after washing are dried 15 hours at a temperature of 50 DEG C, obtains biomass carbon material.
From Fig. 3 and Fig. 5, it can be clearly seen that, there is obvious charcoal as biomass carbon material prepared by charcoal source in sucrose Characteristic peak, and without miscellaneous peak, the biomass carbon material of preparation shows obvious thin layer shape.
A kind of biomass carbon material and preparation method described in the embodiment of the present invention, using solution combustion method, extremely save The energy, and can be with a step into charcoal;Preparation method is simple, short preparation period, favorable repeatability;The nanometer thin of obtained Carbon Materials Rotating fields are homogeneous, and architectural feature is preferable.
Embodiment 5.
Concrete operation step is as follows:
(1) charcoal source mixed solution is prepared:The sucrose of 10g is weighed, is dissolved completely in the deionized water of 20ml, obtain charcoal source Mixed solution.(sucrose is 1 with the mass ratio of charcoal source mixed solution:3)
(2) combustion fluid is prepared:To glycine, the nitric acid that 2ml mass fractions are 35% that 4g is added in the mixed solution of charcoal source The sodium acid carbonate of solution and 0.5g, stirs and incendiary agent is completely dissolved, and obtains combustion fluid.(the quality in biomass carbon source: The quality of incendiary agent:Quality=10 of foaming agent:4:0.5=1:0.4:0.05, the volume of charcoal source mixed solution:The body of oxidant Product=20:2=1:0.01)
(3) combustion fluid is transferred in crucible, is put into and is preheated in 300 DEG C of Muffle furnace, calcined 30 minutes, continue to heat up To 500 DEG C, calcine 3 hours, taking-up naturally cools to room temperature, obtains initial stage Carbon Materials.
(4) initial stage Carbon Materials are washed:First it is washed with deionized three times, then with absolute ethanol washing three times, is washed Initial stage Carbon Materials afterwards.
(5) the initial stage Carbon Materials after washing are dried 14 hours at a temperature of 70 DEG C, obtains biomass carbon material.
Table 2
As can be drawn from Table 2, sucrose has the considerable specific surface area of comparing as biomass carbon material prepared by charcoal source, Reach 344.97m2/ g, average pore volume is 0.14cm3/ g, average pore size is 2.3nm.As can be seen here, biology manufactured in the present embodiment Matter Carbon Materials have good architectural feature.
From figure 1 it appears that sucrose has a huge hysteresis loop, explanation as biomass carbon material prepared by charcoal source Biomass carbon material prepared by the method has abundant pore structure.
As can be seen from Figure 2 come, the aperture of the biomass carbon material that sucrose is prepared as charcoal source concentrate on 2-5nm it Between, illustrate material surface it is widely distributed substantial amounts of micropore and meso-hole structure.
A kind of biomass carbon material and preparation method described in the embodiment of the present invention, using solution combustion method, extremely save The energy, and can be with a step into charcoal;Preparation method is simple, short preparation period, favorable repeatability;The nanometer thin of obtained Carbon Materials Rotating fields are homogeneous, and specific surface area is preferable.
Embodiment 6.
Concrete operation step is as follows:
(1) biomass carbon source is prepared:Banana skin is dried naturally, 100 mesh sieves were crushed, banana skin powder is obtained.
(2) charcoal source mixed liquor is prepared:The banana skin powder of 10g is weighed, is added in the beaker of the deionized water equipped with 20ml, Stir, obtain charcoal source mixed liquor.(banana skin powder is 1 with the mass ratio of charcoal source mixed liquor:3)
(3) combustion fluid is prepared:To the bicarbonate of the glycine, the sodium fluoride of 4g and 2g that 0.2g is added in the mixed liquor of charcoal source Sodium, stirs and incendiary agent is completely dissolved, and obtains combustion fluid.The quality in biomass carbon source:The quality of incendiary agent:Oxidant Quality:Quality=10 of foaming agent:0.2:4:2=1:0.02:0.4:0.2)
(4) combustion fluid is transferred in crucible, is put into and is preheated in 300 DEG C of Muffle furnace, calcined 40 minutes, continue to heat up To 700 DEG C, calcine 10 minutes, taking-up naturally cools to room temperature, obtains initial stage Carbon Materials.
(5) initial stage Carbon Materials are washed:First it is washed with deionized three times, is then washed twice with acetone, then uses anhydrous second Alcohol is washed three times, the initial stage Carbon Materials after being washed.
(6) the initial stage Carbon Materials after washing are dried 12 hours at a temperature of 70 DEG C, obtains biomass carbon material.
A kind of biomass carbon material and preparation method described in the embodiment of the present invention, using solution combustion method, extremely save The energy, and can be with a step into charcoal;Preparation method is simple, short preparation period, favorable repeatability;The nanometer thin of obtained Carbon Materials Rotating fields are homogeneous, and architectural feature is preferable.
The above, is only the preferred embodiment of the embodiment of the present invention, and any shape is not made to the embodiment of the present invention Limitation in formula, according to any simple modification, equivalent variations that the technical spirit of the embodiment of the present invention is made to above example With modification, still fall within the range of embodiment of the present invention technical scheme.

Claims (8)

1. a kind of preparation method of biomass carbon material, it is characterised in that comprise the following steps:
(1) charcoal source mixed liquor is prepared:Biomass carbon source is added in deionized water, is stirred, obtain charcoal source mixed liquor;Institute It is the one kind in glucose, fructose, starch, agricultural crop straw and pericarp to state biomass carbon source;
(2) combustion fluid is prepared:To incendiary agent, oxidant and foaming agent is added in the mixed liquor of charcoal source, stir, obtain combustion fluid; The incendiary agent is the one kind in citric acid, glycine and urea, and the oxidant is salpeter solution, sulfuric acid solution, permanganic acid One kind in potassium and sodium hypochlorite, the foaming agent is in hydrogenperoxide steam generator, sodium fluoride, sodium carbonate and sodium acid carbonate Kind;
(3) combustion fluid is calcined 10-90 minutes at a temperature of 150-450 DEG C, then is warming up to 500-800 DEG C, calcining 10-300 Minute, room temperature is naturally cooled to, obtain initial stage Carbon Materials;
(4) initial stage Carbon Materials are washed:First it is washed with deionized initial stage Carbon Materials, then with absolute ethanol washing initial stage Carbon Materials, Initial stage Carbon Materials after being washed;
(5) the initial stage Carbon Materials after washing are dried, described biomass carbon material is obtained.
2. preparation method according to claim 1, it is characterised in that
In the step (1), biomass carbon source is 2-5 with the mass ratio of charcoal source mixed liquor:10.
3. preparation method according to claim 1, it is characterised in that
After the agricultural crop straw and pericarp dry naturally, then crushed 100-120 mesh sieves.
4. preparation method according to claim 1, it is characterised in that
In the step (2), biomass carbon source is 1 with the mass ratio of incendiary agent:0.01-0.5;
The biomass carbon source is 1 with the mass ratio of potassium permanganate or sodium hypochlorite:0.001-0.5;
Charcoal source mixed liquor is 1 with the volume ratio of salpeter solution or sulfuric acid solution:0.01-0.5;
The biomass carbon source is 1 with the mass ratio of sodium fluoride or sodium carbonate or sodium acid carbonate:0.001-0.5;
Charcoal source mixed liquor is 1 with the volume ratio of hydrogenperoxide steam generator:0.01-0.5.
5. preparation method according to claim 4, it is characterised in that
The mass fraction of the salpeter solution is 30%-65%, and the mass fraction of the hydrogenperoxide steam generator is 20%-40%, The mass fraction of the sulfuric acid solution is 50-98%.
6. preparation method according to claim 1, it is characterised in that
The step (4) also includes:It is washed with deionized after initial stage Carbon Materials 3-4 times, then initial stage charcoal 1-2 is washed with acetone Secondary material, uses absolute ethanol washing initial stage Carbon Materials 3-4 times again afterwards.
7. preparation method according to claim 1, it is characterised in that
In the step (5), dry temperature is 50-80 DEG C, and drying time is 10-15 hours.
8. a kind of biomass carbon material, it is characterised in that made according to the preparation method described in claim 1-7 any one Biomass carbon material.
CN201710157984.8A 2017-03-16 2017-03-16 A kind of biomass carbon material and preparation method Pending CN106829923A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201710157984.8A CN106829923A (en) 2017-03-16 2017-03-16 A kind of biomass carbon material and preparation method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201710157984.8A CN106829923A (en) 2017-03-16 2017-03-16 A kind of biomass carbon material and preparation method

Publications (1)

Publication Number Publication Date
CN106829923A true CN106829923A (en) 2017-06-13

Family

ID=59144612

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201710157984.8A Pending CN106829923A (en) 2017-03-16 2017-03-16 A kind of biomass carbon material and preparation method

Country Status (1)

Country Link
CN (1) CN106829923A (en)

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107640767A (en) * 2017-10-20 2018-01-30 武汉工程大学 One kind is used for cheap porous carbon materials of high-performance super capacitor and preparation method thereof
CN111547722A (en) * 2020-04-30 2020-08-18 浙江农林大学 Preparation method of biomass-derived carbon material
CN111573650A (en) * 2020-04-24 2020-08-25 北京科技大学 Method for preparing mesoporous carbon powder with high specific surface area
CN112093793A (en) * 2020-09-04 2020-12-18 华中农业大学 Carbon nano-particles using crop straws as raw materials and preparation method thereof
CN112136643A (en) * 2020-09-04 2020-12-29 华中农业大学 Sandwich porous roof substrate block and preparation method thereof
CN112136552A (en) * 2020-09-14 2020-12-29 华中农业大学 Porous wall matrix block and preparation method thereof
CN113023708A (en) * 2021-02-24 2021-06-25 云南大学 Method for separating and extracting carbon dots from biomass combustion smoke dust and functionalizing carbon dots
RU2760272C1 (en) * 2021-02-25 2021-11-23 Федеральное государственное бюджетное образовательное учреждение высшего образования "Новосибирский государственный аграрный университет" Method for obtaining modified activated carbon
CN114702976A (en) * 2022-04-25 2022-07-05 昆明理工大学 Method for preparing biochar through self-propagating pyrolysis
CN114735699A (en) * 2022-04-20 2022-07-12 安徽大学 High-starch-content bio-based porous activated carbon and preparation method thereof
CN116282013A (en) * 2023-02-28 2023-06-23 广州市帝东环保科技有限公司 Preparation method of efficient activated carbon for VOCS adsorption

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6086013A (en) * 1983-10-17 1985-05-15 Hitachi Ltd Porous flat plate having electrical conductivity
CN103855413A (en) * 2012-11-28 2014-06-11 中国科学院大连化学物理研究所 Porous carbon material used for lithium-air cell anode
CN106159225A (en) * 2016-07-25 2016-11-23 北京科技大学 A kind of method producing carbon complex amorphous vanadium oxide powder

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6086013A (en) * 1983-10-17 1985-05-15 Hitachi Ltd Porous flat plate having electrical conductivity
CN103855413A (en) * 2012-11-28 2014-06-11 中国科学院大连化学物理研究所 Porous carbon material used for lithium-air cell anode
CN106159225A (en) * 2016-07-25 2016-11-23 北京科技大学 A kind of method producing carbon complex amorphous vanadium oxide powder

Cited By (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107640767A (en) * 2017-10-20 2018-01-30 武汉工程大学 One kind is used for cheap porous carbon materials of high-performance super capacitor and preparation method thereof
CN111573650A (en) * 2020-04-24 2020-08-25 北京科技大学 Method for preparing mesoporous carbon powder with high specific surface area
CN111573650B (en) * 2020-04-24 2021-10-01 北京科技大学 Method for preparing mesoporous carbon powder with high specific surface area
CN111547722A (en) * 2020-04-30 2020-08-18 浙江农林大学 Preparation method of biomass-derived carbon material
CN112093793A (en) * 2020-09-04 2020-12-18 华中农业大学 Carbon nano-particles using crop straws as raw materials and preparation method thereof
CN112136643A (en) * 2020-09-04 2020-12-29 华中农业大学 Sandwich porous roof substrate block and preparation method thereof
CN112136643B (en) * 2020-09-04 2021-12-17 华中农业大学 Sandwich porous roof substrate block and preparation method thereof
CN112136552A (en) * 2020-09-14 2020-12-29 华中农业大学 Porous wall matrix block and preparation method thereof
CN112136552B (en) * 2020-09-14 2021-12-17 华中农业大学 Porous wall matrix block and preparation method thereof
CN113023708B (en) * 2021-02-24 2023-10-27 云南大学 Method for separating and extracting carbon dots from biomass combustion smoke dust and functionalization thereof
CN113023708A (en) * 2021-02-24 2021-06-25 云南大学 Method for separating and extracting carbon dots from biomass combustion smoke dust and functionalizing carbon dots
RU2760272C1 (en) * 2021-02-25 2021-11-23 Федеральное государственное бюджетное образовательное учреждение высшего образования "Новосибирский государственный аграрный университет" Method for obtaining modified activated carbon
CN114735699A (en) * 2022-04-20 2022-07-12 安徽大学 High-starch-content bio-based porous activated carbon and preparation method thereof
CN114735699B (en) * 2022-04-20 2023-10-10 安徽大学 High-starch-content biological-based porous activated carbon and preparation method thereof
CN114702976A (en) * 2022-04-25 2022-07-05 昆明理工大学 Method for preparing biochar through self-propagating pyrolysis
CN116282013A (en) * 2023-02-28 2023-06-23 广州市帝东环保科技有限公司 Preparation method of efficient activated carbon for VOCS adsorption
CN116282013B (en) * 2023-02-28 2024-01-16 广州市帝东环保科技有限公司 Preparation method of efficient activated carbon for VOCS adsorption

Similar Documents

Publication Publication Date Title
CN106829923A (en) A kind of biomass carbon material and preparation method
CN104528720B (en) The preparation method of a kind of multi-stage porous Carbon Materials and product
CN103588190B (en) A kind of method being prepared carbosphere by lignocellulose
CN105271203B (en) porous co-doped graphene and preparation method thereof
CN102583312B (en) Method for preparing porous carbon spheres doped with nitrogen and phosphorus and application
WO2015106720A1 (en) Method for producing super activated charcoal from biomass power plant ash
CN107376971A (en) The synthetic method of one species graphitic nitralloy carbon/molybdenum disulfide nano-composite material
CN107628597B (en) By using SiO2Method for preparing biomass carbon material with micropore and mesopore structure by coating method
CN105197910B (en) A kind of method that porous nano carbon material is prepared using biomass as carbon source
CN113149077B (en) Preparation method and application of amorphous metal oxide hollow multi-shell material
CN106824200A (en) A kind of carbon load nickel metallic catalyst and preparation method thereof
CN110064367A (en) A kind of biomass-based activated carbon microballon and its preparation method and application
CN109746017A (en) A kind of preparation method of P doping solvent heat graphite phase carbon nitride photochemical catalyst
CN103408055A (en) Room temperature preparation method of spherical Cu2O porous adsorbing material
CN112225216A (en) Medium-micropore lignin-based activated carbon and preparation method thereof
CN104118863A (en) Method for preparing porous carbon material for supercapacitor by activating rice husks through ionic liquid
CN111960416A (en) Method for preparing sulfur-doped carbon material from biomass
CN103641100A (en) Preparation method of cassava-starch-based grading-pore carbon microsphere material
CN114212790A (en) Preparation method of nitrogen-doped porous biochar and method for preparing electrode material
CN103349891A (en) Calcium magnesium double salt CO2 absorbent prepared from modified dolomite and preparation method thereof
CN107572509A (en) A kind of hollow carbon graphite ball nano material of N doping and preparation method thereof
CN104549374A (en) Cadmium selenide flower-shaped microspheres prepared from nanosheets with hydrophilic surfaces as well as preparation method and application of microspheres
CN103833080B (en) A kind of preparation method of molybdic acid cadmium porous ball
CN111908443A (en) Preparation method of self-doped porous carbon
CN106957441A (en) A kind of solvent structure carbonization MOFs method

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication

Application publication date: 20170613

RJ01 Rejection of invention patent application after publication