CN106986322B - A kind of preparation method and application of nitrogenous carbon material - Google Patents
A kind of preparation method and application of nitrogenous carbon material Download PDFInfo
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- CN106986322B CN106986322B CN201710285489.5A CN201710285489A CN106986322B CN 106986322 B CN106986322 B CN 106986322B CN 201710285489 A CN201710285489 A CN 201710285489A CN 106986322 B CN106986322 B CN 106986322B
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24D—CIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES FOR CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
- A24D3/00—Tobacco smoke filters, e.g. filter-tips, filtering inserts; Filters specially adapted for simulated smoking devices; Mouthpieces for cigars or cigarettes
- A24D3/06—Use of materials for tobacco smoke filters
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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
- C01P2002/50—Solid solutions
- C01P2002/52—Solid solutions containing elements as dopants
- C01P2002/54—Solid solutions containing elements as dopants one element only
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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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- 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
- C01P2006/14—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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- Carbon And Carbon Compounds (AREA)
- Cigarettes, Filters, And Manufacturing Of Filters (AREA)
Abstract
A kind of preparation method of nitrogenous carbon material, it is characterised in that: be the method that the nitrogenous step hole Carbon Materials of high porosity are prepared through oxidation, ammonification, carbonization after solid acid catalysis hydrolyzes as raw material using tobacco rod.By the successively addition of nitric acid-hydrogen peroxide or hypochlorite-hydrogen peroxide and subsequent step organic amine, preparation is rich in N element carbon material.Nitrogenous step hole carbon material prepared by the present invention, micropore, it is mesoporous, have certain distribution within the scope of macropore, more suitable for the absorption of the wider coke tar in cigarette of particle diameter distribution, prepared nitrogenous step hole carbon material is made an addition into cigarette filter, it is significant to the reducing effect of main flume Cd and tar.The invention has the advantages that generated organic acid and alcohol reaction generates ester in solid acid catalysis cellulose hydrolysis, organic acid can avoid to the etching problem of reactor.The increase of element N content is conducive to N to the cnmplexation adsorbability of Cd in flue gas, has obvious effect to the reduction of Cd in cigarette smoke.
Description
Technical field
The present invention relates to a kind of preparation methods of nitrogenous carbon material, through oxygen after catalyzing hydrolysis after specifically being crushed by tobacco rod
The method that change, ammonification, carbonization prepare the nitrogenous step hole carbon material of high porosity.The material can make an addition to cigarette filter, to flue gas
The reducing effect of Cd and tar is significant.
Background technique
China is World tobacco big country, and cultivated area, total output, cigarette output and sales volume occupy first place in the world.?
A large amount of waste is inevitably generated in tobacco leaf and process, according to statistics, only the cigarette stalk generated in 2015 is just up to 1.163
×106Ton.Since cigarette stalk availability is relatively poor, the overwhelming majority is handled in a manner of burying discarding or burning, comprehensive utilization ratio
It is extremely low, environmental pollution is not only caused, but also waste a large amount of existing resource.
Heavy metal is mainly derived from the tobacco planting soil containing heavy metal, water and air etc. in the process in tobacco.Tobacco
In the heavy metal elements such as lead, arsenic, chromium, cadmium human body can be entered by flue gas in the form of aerosol or metal oxide, pass through
It accumulates and then causes damages to the health of people.The study found that cadmium is to be easiest in numerous heavy metals contained by tobacco
Absorbed element.With the continuous improvement of people's health consciousness, cadmium content has become smoking in flue gas and health field is paid close attention to
Hot spot.Active carbon is a kind of porosu solid carbon material, because it has flourishing gap structure and huge specific surface area, thus
Its unique strong absorption property is assigned, in addition its chemical property is stablized, not soluble in water and other most of solvents are inhaling it
It is used widely in the fields such as attached, separation, catalysis.Conventional acetate fiber filter tip has certain adsorptivity to cadmium and coke tar in cigarette
Can, research shows that can significantly promote its absorption property to cadmium and tar after active carbon is made an addition to cigarette filter, it is seen then that living
Property charcoal is with a wide range of applications in terms of the absorption of cigarette smoke cadmium and tar.
Preparing active carbon generally by tobacco rod includes the processes such as dry, carbonization, activation, wherein activation is the key that pore-creating,
Common method can be divided into physical process and two kinds of chemical process.
Physical activation method is related to the oxidizing gas such as vapor, carbon dioxide, air.In the comprehensive utilization of tobacco rod, the summer
Flood, which is answered et al., is respectively adopted carbon dioxide and vapor activation is prepared for pore type cigarette stalk base granular activated carbon (full in summer is answered, Peng
Research [J] gold .2006 (07): 38-41. of the preparation of granular activated carbon from tobacco stems with carbon dioxide such as Jin Hui, Zhang Libo
Full in summer is answered, Peng Jinhui, research [J] the ion exchange and suction of the Preparation of Granular Activated Carbon From Tobacco Stems Activation By Steam such as Zhang Libo
Attached .2007 (02): 112-118. full in summer is answered, Peng Jinhui, and it is living that the such as Zhang Libo microwave radiation-steam method prepares tobacco rod base particle
Property charcoal [J] chemical engineering .2007 (01): 48-51.).Carbon material BET specific surface area prepared by this method is relatively low, and
The hole overwhelming majority belongs to micropore, and mesoporous and macropore content is very low.
Chemical activation method is to add highly basic, strong acid or strong oxidizer chemical reagent, such as HNO into raw material in activation stage3、
KOH、MnO2、ZnCl2Deng a kind of method.On March 3rd, 2004, " microwave radiation tobacco rod solid waste manufactured the side of active carbon
Method " (application number CN02113270.4, publication number CN1140449C) disclose it is a kind of will tobacco rod and liquor zinci chloridi dipping after pass through
Heat the method for obtaining activated carbon product.There is the volatilization pollution problem of zinc chloride in the actual production process in this method.2005
On September 21, " a method of produce active carbon with high specific surface area " (application number CN200510010670.2, publication number
CN1669918A a kind of side that tobacco rod and potassium hydroxide solution are impregnated again to heated production active carbon with high specific surface area) is disclosed
Method.A kind of on 2 17th, 2010 " preparation method of high mesoporous activated carbon " (application number CN200910184645.4, publication numbers
CN101648707A), disclose a kind of high by the mixing leaching of biomass material, phosphoric acid and assistant activator (peroxide or over cure compound)
The method that stain, heating activation prepare activated carbon product.CN1669918A and publication number CN101648707A due to alkali or acid make
Be under the high temperature conditions, therefore it is serious to the etching problem of equipment.
Summary of the invention:
The purpose of the present invention is exactly to be directed to the deficiency or defect and the preparation of a kind of nitrogenous carbon material that provides of the above technology
Method, specifically tobacco rod first partial hydrolysis is carried out under the action of solid acid, be carbonized to filter residue, and after through oxidation,
Step hole N doping carbon material can be obtained in the secondary carbonization of amine heat.Material effect in terms of Cd and tar in reducing cigarette smoke
Significantly.(referring to bibliography: heavy metal cadmium and regulation measure progress in tobacco, Chinese agriculture science and technology Leader,
2011,13 (2): 93-98.)
The purpose of the present invention is achieved through the following technical solutions:
A kind of preparation method of nitrogenous carbon material, is the method for preparing the nitrogenous carbon material in step hole as raw material using tobacco rod, tool
Steps are as follows for body:
1) tobacco rod raw material pretreatment of raw material: is dried to moisture content 5% hereinafter, being crushed to particle size at 60 ~ 120 DEG C
200 mesh are hereinafter, preferably 20-150 mesh；
2)Mixing: 1) gained powder raw material and alcohol solution, solid acid in mass ratio 1: 5-15: 0.05-0.2 are added to
Ball milling (revolving speed 200-500 turns/min) mixing, time 2-5 hour are carried out in ball grinder；
3) it hydrolyzes: 2) being transferred in reaction kettle after feed liquid in is separated with grinding bead, in 100 ~ 200 DEG C, 5 ~ 20 MPa stirring
Under the conditions of react 1 ~ 24 h；
4) it is carbonized: 3) reaction solution is filtered or is centrifugated residue obtained, nitrogen or helium atmosphere in merging high temperature furnace
Be carbonized 1-5h at 600 ~ 800 DEG C；
5) it purifies: 4) products obtained therefrom is soaked in nitric acid-hydrogen peroxide or hypochlorite-hydroperoxide solution, impregnate
30-100 DEG C of temperature, time 0.5-12h is washed later, spare；Nitric acid-hydrogen peroxide or hypochlorite-hydroperoxide solution
In concentration of nitric acid be 1-8M, hypochlorite concentration 1-8M, concentration of hydrogen peroxide be 0.5-8 M.
6) secondary carbonization: 5) obtained solid is placed in water heating kettle, adds Amine Solutions, additive amount 5) Central Plains Material
Long-pending 1-4 times, under 150-500 DEG C of self-generated pressure(Because be in closed water heating kettle reactor, when temperature is higher, the inside
Substance is substantially at subcritical or supercriticality, and pressure following temperature variation is obvious, therefore the confined reaction pressure under high temperature
It is the automatic pressure of system)Carry out secondary carbonization 1-24 h；Solute in Amine Solutions be diethylamine, triethylamine, butanediamine,
Hexamethylene diamine, propylamine, butylamine, any one in amylamine, the solvent in Amine Solutions is one kind of water, alcohol or ethers.
7) it washs: being cooled to room temperature, then separate, and be washed with deionized for several times to get step hole after 6) being carbonized
Nitrogenous carbon material.
In the present invention, solid acid used be Si-Al molecular sieve include HY, Hbeta, HZSM-5, HZSM-22, HZSM-11,
MCM-22,HZSM-35；The silane-modified mesoporous material of sulfonic acid includes SO3H-SBA-15、SO3H-SBA-16、SO3H-MCM-41、
SO3H-MCM-48、SO3H-MCM-50.The concentration of the alcohol solution is 5 ~ 10%wt；Alcohol solution is methanol aqueous solution, ethyl alcohol
Aqueous solution, aqueous propanol solution, any one in glycol water.
Grinding bead in ball grinder is agate bead.
Nitrogenous carbon material prepared by the present invention is applied in cigarette filter, it is aobvious to the reducing effect of flue gas Cd and tar
It writes.
Advantages of the present invention is as follows:
1, tobacco rod is handled using solid acid and alcoholic solution, avoids the etching problem in preparation process to equipment.Nitric acid-mistake
The successively addition of hydrogen oxide or hypochlorite-hydrogen peroxide and subsequent step organic amine, preparation are rich in N element carbon material.
2, prepared step hole carbon material, in micropore (<2 nm), mesoporous hole (2 ~ 50 nm), macropore (>50 nm) range
Inside there is certain distribution, the increase of element N content is conducive to N to the cnmplexation adsorbability of Cd in flue gas, in cigarette smoke
The reducing effect of Cd and tar is significant.
3, the use of solid acid has achieved the purpose that tobacco rod is carbonized and obtains step hole carbon products.
Specific embodiment
The present invention is described further with reference to embodiments:
Embodiment 1
Tobacco rod raw material is placed in baking oven and is dried to moisture content 5% hereinafter, being crushed to 20 ~ 40 mesh at 60 DEG C, weighs 10 g samples
Product are mixed with methanol aqueous solution (methanol concentration 5%wt) according to solid-liquid volume ratio 1:15 and are transferred in ball grinder, are added
The 10% of 1.0 g(tobacco rod weight of HY molecular sieve) 5 h of mixed at room temperature is carried out under the rotational speed of ball-mill of 300 turns/min, obtain feed liquid.It will
Feed liquid is transferred to autoclave after separating with agate bead, 24 h are reacted under 100 DEG C, 5 MPa under nitrogen atmosphere.Reaction solution is taken advantage of
Heat filtering, deionized water are washed three times, and filter residue and drying carries out carbonization 5 under the conditions of being placed on lower 600 DEG C of nitrogen atmosphere in tube furnace
H obtains a char-forming material.Char-forming material is immersed in the 1 M HNO of 200 ml3-0.5 M H2O2100 in mixed solution
DEG C reflux 12 h, be cooled to room temperature centrifugation, deionized water washing three times, be transferred in water heating kettle, be added 20 ml ethylenediamines it is water-soluble
Liquid (ethylenediamine volumetric concentration is 50%), in 150 DEG C of progress dynamics(Dynamic belongs to the term of preparation process, indicates stirring or shaking
It is reacted under dynamic state, antisense reverse side is exactly static.)24 h of secondary carbonization, by being filtered, washed, be drying to obtain step
The nitrogenous carbon material 1# in hole.Texture parameter and the element composition of prepared carbon material are shown in Table 1.
Embodiment 2
Tobacco rod raw material is placed in 80 DEG C of baking oven and is dried to moisture content 5% hereinafter, being crushed to 40 ~ 60 mesh, 10 g samples is weighed, presses
Mix being transferred in ball grinder with aqueous propanol solution (propanol concentration 10%wt) according to solid-liquid volume ratio 1:5, SO is added3H-
The 5% of 0.5 g(tobacco rod weight of MCM-41 mesoporous material) 2 h of mixed at room temperature under the rotational speed of ball-mill of 200 turns/min.By feed liquid with
It is transferred to autoclave after agate bead separation, reacts 1 h under 200 DEG C, 5 MPa under nitrogen atmosphere.Reaction solution filters while hot,
Deionized water is washed three times, and filter residue and drying is carbonized 1 h under the conditions of being placed on lower 800 DEG C of nitrogen atmosphere in tube furnace, obtains a carbon
Change material.Char-forming material of gained is immersed in 4 MHNO of 200 ml3-2 M H2O270 DEG C of 8 h of reflux in mixed solution, drop
It is centrifugated, and is washed with deionized three times after to room temperature, is transferred in water heating kettle, 40 ml hexamethylene diamine aqueous solutions are added,
250 DEG C of progress dynamic 15 h of secondary carbonization, by being filtered, washed, be drying to obtain the nitrogenous carbon material 2# in step hole.Prepared carbon materials
Texture parameter and the element composition of material are shown in Table 1.
Embodiment 3
Tobacco rod raw material is placed in baking oven and is dried to moisture content 5% hereinafter, being crushed to 60 ~ 90 mesh for 100 DEG C, weighs 10 g samples,
It is mixed and is transferred in ball grinder with ethanol water (concentration of alcohol 8%wt) according to solid-liquid volume ratio 1:10, is added
The 20% of 2.0 g(tobacco rod weight of HZSM-5 molecular sieve) 4 h of mixed at room temperature under the rotational speed of ball-mill of 400 turns/min.By feed liquid and Ma
It is transferred in autoclave after the separation of Nao pearl, reacts 14 h under nitrogen atmosphere under 150 DEG C, 12 MPa.Reaction solution mistake while hot
Filter, deionized water are washed three times, and filter residue and drying carries out 2 h of carbonization under the conditions of being placed on lower 700 DEG C of nitrogen atmosphere in tube furnace, are obtained
Char-forming material.Carbon material of gained is immersed in 8 MHNO of 200 ml3-8 M H2O230 DEG C of stirrings in mixed solution
0.5 h is then washed three times, is transferred in water heating kettle, and the ethanol solution of 30 ml n-butylamines is added, in 500 DEG C of progress dynamics two
1 h of secondary carbonization, by being filtered, washed, be drying to obtain the nitrogenous carbon material 3# in step hole.The texture parameter and member of prepared carbon material
Element composition is shown in Table 1.
Embodiment 4
Tobacco rod raw material is placed in baking oven and is dried to moisture content 5% hereinafter, being crushed to 100 ~ 120 mesh for 120 DEG C, weighs 10 g samples
Product are mixed with ethanol water (concentration of alcohol 8%wt) according to solid-liquid volume ratio 1:10 and are transferred in ball grinder, are added
The 20% of 2.0 g(tobacco rod weight of HZSM-11 molecular sieve) 2 h of mixed at room temperature under the rotational speed of ball-mill of 400 turns/min, obtain feed liquid.It will
Feed liquid is transferred to autoclave after separating with agate bead, 24 h are reacted under 200 DEG C, 20 MPa under nitrogen atmosphere.Reaction solution
It filters while hot, deionized water is washed three times, and filter residue and drying is carbonized under the conditions of being placed on lower 750 DEG C of nitrogen atmosphere in tube furnace
4 h obtain a char-forming material.Char-forming material of gained is immersed in 200 ml, 4 MHNO3-6 M H2O230 DEG C in mixed solution
0.5 h is stirred, then deionization washing three times, is transferred in water heating kettle, 40 ml n-butylamine aqueous solution of tobacco rod volume is added,
500 DEG C of progress dynamic 3 h of secondary carbonization, by being filtered, washed, be drying to obtain the nitrogenous carbon material 4# in step hole.Prepared carbon materials
Texture parameter and the element composition of material are shown in Table 1.(element composition is the composition of the essential element of prepared carbon material (by element point
Analyzer measures), be primarily intended to react higher N element content in prepared N doping carbon material)
Prepared carbon material is made an addition into cigarette filter, additive amount is every 20 mg, and contrast sample is convention filter volume
Cigarette.Corresponding cigarette sample to be tested is balanced into 48 h, the cigarette of screening under the conditions of temperature (22 ± 1) DEG C, relative humidity (60 ± 1) %
It is ± 0.01 g that branch total amount, which differs range, with 20 H-type carousel-type smoking machines according to GB/T 16450-2004 smoking machine and its survey
Trying standard conditions, (wind speed is (200 ± 30) mm/s, pumping volume (35 ± 0.3) ml, 2 s of duration, puff interval 60
S) smoking cigarette collects gas with the nitric acid solution of 20 ml10% (v/v) with the middle granule phase substance of electrostatic paved set pipe paved set main flume
Phase.According to YC/T379-2010 " the measurement inductively coupled plasma constitution of chromium, nickel, arsenic, selenium, cadmium, lead in cigarette mainstream flue gas
Spectrometry " measurement cigarette mainstream flue gas in Cd.The tar content in cigarette sample gas phase is carried out according to GB/T 19609-2004
Measurement.The results are shown in Table 2.Result can be seen that compared with control sample from table 2, the carbon material reduce flue gas in Cd and
Significant effect in terms of tar, highest is respectively up to 48.7% and 34.9%.
。
Claims (8)
1. a kind of preparation method of nitrogenous carbon material, it is characterised in that: be to prepare the nitrogenous carbon material in step hole by raw material of tobacco rod
Method, the specific steps are as follows:
1) pretreatment of raw material: tobacco rod raw material is dried to moisture content at 60 ~ 120 DEG C and is greater than 5% hereinafter, being crushed to particle size
200 mesh；
2) it mixes: 1) gained powder raw material and alcohol solution, solid acid in mass ratio 1: 5-15: 0.05-0.2 is added to ball milling
Ball milling mixing, time 2-5 hour are carried out in tank；Solid acid used is that Si-Al molecular sieve includes HY, Hbeta, HZSM-5, HZSM-
22,HZSM-11,MCM-22,HZSM-35；Or for the silane-modified mesoporous material of sulfonic acid include SO3H-SBA-15、SO3H-SBA-16、
SO3H-MCM-41、SO3H-MCM-48、SO3H-MCM-50；
3) it hydrolyzes: 2) being transferred in reaction kettle after feed liquid in is separated with grinding bead, in 100 ~ 200 DEG C, 5 ~ 20 MPa stirring conditions
1 ~ 24 h of lower reaction；
4) be carbonized: 3) reaction solution is filtered or is centrifugated it is residue obtained, be placed in nitrogen or helium atmosphere 600 in high temperature furnace ~
Be carbonized 1-5h at 800 DEG C；
5) it purifies: 4) products obtained therefrom being soaked in nitric acid-hydrogen peroxide or hypochlorite-hydroperoxide solution, soaking temperature
30-100 DEG C, time 0.5-12h is washed later, spare；
6) secondary carbonization: 5) obtained solid is placed in water heating kettle, adds Amine Solutions, additive amount 5) in raw material volume
1-4 times, secondary carbonization 1-24 h is carried out under 150-500 DEG C of self-generated pressure；Solute in the Amine Solutions is diethylamine, three
Ethamine, butanediamine, hexamethylene diamine, propylamine, butylamine, any one in amylamine；
7) it washs: being cooled to room temperature, then separate, and be washed with deionized nitrogenous to get step hole for several times after 6) being carbonized
Carbon material.
2. the preparation method of nitrogenous carbon material according to claim 1, it is characterised in that: the concentration of the alcohol solution is
5~10%wt；Alcohol solution is methanol aqueous solution, ethanol water, aqueous propanol solution, any one in glycol water.
3. the preparation method of nitrogenous carbon material according to claim 1, it is characterised in that: turn when ball milling in step 2
Speed is that 200-500 turns/min.
4. the preparation method of nitrogenous carbon material according to claim 1, it is characterised in that: the grinding bead in ball grinder is Ma
Nao pearl.
5. the preparation method of nitrogenous carbon material according to claim 1, it is characterised in that: the particle size in step 1) is
20-150 mesh.
6. the preparation method of nitrogenous carbon material according to claim 1, it is characterised in that: nitric acid-described in step 5)
Concentration of nitric acid in hydrogen peroxide or hypochlorite-hydroperoxide solution is 1-8M, hypochlorite concentration 1-8M, peroxide
Change hydrogen concentration is 1-8 M.
7. the preparation method of nitrogenous carbon material according to claim 1, it is characterised in that: the Amine Solutions in step 6)
In solvent be water, alcohol or ethers one kind.
8. a kind of application of nitrogenous carbon material, it is characterised in that: the nitrogenous carbon material application for preparing claim 1 the method
It is significant to the reducing effect of flue gas Cd and tar in cigarette filter.
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| CN112551505B (en) * | 2020-12-11 | 2022-04-05 | 广东凯金新能源科技股份有限公司 | Preparation method of hard carbon-based negative electrode material |
| CN112645328B (en) * | 2020-12-21 | 2022-10-04 | 中国烟草总公司郑州烟草研究院 | Preparation method and application of nitrogen-containing porous carbon material |
| CN113694892A (en) * | 2021-08-27 | 2021-11-26 | 伯克利南京医学研究有限责任公司 | Carbon aerogel composite structure, composite filter element, preparation methods of carbon aerogel composite structure and composite filter element, and application of carbon aerogel composite structure and composite filter element |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101407323A (en) * | 2008-09-16 | 2009-04-15 | 上海第二工业大学 | Method for preparing pressed active carbon from tobacco stalk |
| CN106475052A (en) * | 2016-11-16 | 2017-03-08 | 中国科学院烟台海岸带研究所 | A kind of application seaweed biomass prepares nano-sized magnesium hydroxide/N doping porous carbon composite material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101407323A (en) * | 2008-09-16 | 2009-04-15 | 上海第二工业大学 | Method for preparing pressed active carbon from tobacco stalk |
| CN106475052A (en) * | 2016-11-16 | 2017-03-08 | 中国科学院烟台海岸带研究所 | A kind of application seaweed biomass prepares nano-sized magnesium hydroxide/N doping porous carbon composite material and preparation method thereof |
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