CN110182805A - A kind of preparation method of active carbon - Google Patents

A kind of preparation method of active carbon Download PDF

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Publication number
CN110182805A
CN110182805A CN201910545510.XA CN201910545510A CN110182805A CN 110182805 A CN110182805 A CN 110182805A CN 201910545510 A CN201910545510 A CN 201910545510A CN 110182805 A CN110182805 A CN 110182805A
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active carbon
parts
preparation
shaped granule
activation
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CN201910545510.XA
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谢少峰
谢坤
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Hefei Yuchuang Carbon Industry Co Ltd
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Hefei Yuchuang Carbon Industry Co Ltd
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Priority to CN201910545510.XA priority Critical patent/CN110182805A/en
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/30Active carbon
    • C01B32/312Preparation
    • C01B32/318Preparation characterised by the starting materials
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/30Active carbon
    • C01B32/312Preparation
    • C01B32/336Preparation characterised by gaseous activating agents

Abstract

The present invention relates to a kind of preparation method of active carbon, include the following steps: step 1, biomass material is cleaned, it is dry, smash it through that 60 meshes are spare, the biomass material of crushing is subjected to acidification;Step 2, coal slime is handled to ash content through flotation no more than 25%, and it is spare then to obtain coal slime powder through drying, broken, 200 meshes excessively again;Step 3, according to mass fraction meter, weigh 10~15 parts of wood powder, 10~15 parts of clay mineral, 30~40 parts of the acidification powdered biomass prepared in step 1, prepare in step 2 45~60 parts of coal slime powder be mixed evenly to obtain mixed raw material;Step 4, mixed raw material forms;Step 5, it carbonizes;Step 6, it activates;Step 7, the activation shaped granule prepared in step 6 is first subjected to pickling, by being washed to neutrality, obtains pressed active carbon after dry.The present invention can prepare easily molded, structure and be not easy loose active carbon, convenient for separation after adsorption saturation.

Description

A kind of preparation method of active carbon
Technical field
The present invention relates to the technical fields of active carbon, more particularly, to a kind of preparation method of active carbon.
Background technique
Absorbent charcoal material is by the resulting amorphous carbon of working process, because of large specific surface area, to the nothing in gas, solution Machine or organic substance and colloidal solid etc. have good adsorption capacity.A kind of absorption of the absorbent charcoal material as function admirable Agent is mainly determined by it with unique absorption surface architectural characteristic and surface chemistry.Absorbent charcoal material Chemical property is stablized, and high mechanical strength is acidproof, alkaline-resisting, heat-resisting, and not soluble in water and organic solvent can regenerate use, extensively General is applied to the multiple fields such as chemical industry, environmental protection, food processing, metallurgy.
Notification number is that the Chinese patent of CN1178853C discloses a kind of method for preparing active carbon, including to containing carbon feedstock Broken, mixing, charing and activation step in the presence of activated media, finally obtain active carbon, the carbonization process is to add It is carried out under the conditions of pressure, the pressure limit of carbonization process is 0.2~15Mpa, and charing heating rate is 2~8 DEG C/min, terminates temperature Degree is at 400~650 DEG C;The pressure limit of activation process is 0.2~10Mpa, and temperature is 650~1000 DEG C.It is prepared by this kind The method of active carbon, obtained product excellent effect and obtain product in terms of intensity, gas separating property and absorption property Yield is higher.
Prior art among the above has the following deficiencies: that active carbon forms under the conditions of certain temperature and pressure, The active carbon that this method is prepared is easily molded, short texture, causes its abrasivity and compressive resistance poor, in use process Be easy it is loose, after absorption reaches saturation, it is loose after active carbon be not readily separated.
Summary of the invention
The object of the present invention is to provide a kind of preparation methods of active carbon, can prepare easily molded, structure and be not easy loosely Active carbon, after adsorption saturation convenient for separation.
Above-mentioned technical purpose of the invention has the technical scheme that a kind of preparation side of active carbon Method specifically comprises the following steps:
Step 1, biomass material it is cleaned, it is dry, smash it through that 60 meshes are spare, the biomass material of crushing is acidified Processing obtains acidification powdered biomass;
Step 2, coal slime is handled to ash content through flotation no more than 25%, then obtains coal slime through drying, broken, 200 meshes excessively again Powder is spare;
Step 3, according to mass fraction meter, 10~15 parts of wood powder, 10~15 parts of clay mineral, the acidification prepared in step 1 are weighed 45~60 parts of the coal slime powder prepared in 30~40 parts of powdered biomass, step 2 is mixed evenly to obtain mixed raw material;
Step 4, form: it is 10~15mm that the mixed raw material in step 3 is compressed into diameter at normal temperature, and length is 15~20mm Cylindric shaped granule;
Step 5, it carbonizes: the cylindric shaped granule prepared in step 4 being placed in heating container and carries out charing process, it is naturally cold But to obtaining charing shaped granule after room temperature;
Step 6, it activates: weighing 10~20 parts of the charing shaped granule prepared in step 5 according to mass fraction meter and infiltrated 5~15h in 20~40 parts of activators is filtered after infiltration, is dry, then under oxygen-containing gas atmosphere, it is warming up to 700~ 900 DEG C are activated, and activation time is 30~90min, and cooled to room temperature obtains activation shaped granule after activation;
Step 7, the activation shaped granule prepared in step 6 is first subjected to pickling, by being washed to neutrality, is obtained into after dry Type active carbon.
By using above-mentioned technical proposal, use biomass material, coal slime, wood powder and clay material as active carbon original Material, does not need additionally to add binder, can be prepared by pressed active carbon, process is simple, and the active carbon prepared compares table Area is big, absorption property is good.In activation step, the infiltration that raw material first passes through activating agent preliminarily forms hole, using oxygenous The further activation of body improves the absorption property of active carbon to be conducive to prepare hole active carbon abundant.Pickling washing Purpose be on the one hand to remove the impurity of activated carbon surface, avoid impurity from blocking the hole to be formed, reduce adsorption effect, separately On the one hand it removes and is immersed in the intrapore activator of active carbon.
The present invention is further arranged to: biomass material is lignocellulosic, in stalk, shell, straw in the step 1 One kind.
By using above-mentioned technical proposal, lignocellulosic, stalk, shell, carbon is abundant in straw, and is that plant is useless Gurry prepares active carbon using them, can reduce the production cost of active carbon, realizes the purpose to turn waste into wealth.
The present invention is further arranged to: the method for acid processing in the step 1 are as follows: to the biomass material after crushing and screening It is middle that the hydrochloric acid or sulfuric acid that mass fraction is 10wt% is added, 2~6h is reacted under the conditions of 140~200 DEG C after mixing evenly, it is natural After cooling, it is filtered to remove filtrate, filter residue is washed with deionized at least twice, ground 60 mesh after filter residue drying, as sour Metaplasia material powder.
By using above-mentioned technical proposal, biomass material is polysaccharide polymer, passes through β-Isosorbide-5-Nitrae-glucosides between molecule Key connection, acidification can be broken β-Isosorbide-5-Nitrae-glycosidic bond, so that biomass long-chain molecule is fractured into small molecule chain substance, drop With intermolecular bond energy in low molecule, it is thorough to be conducive to subsequent charing.
The present invention is further arranged to: step 3 CLAY MINERALS AND THEIR SIGNIFICANCE is one of montmorillonite, illite, sepiolite Or it is a variety of.
By using above-mentioned technical proposal, montmorillonite, illite, the sepiolite of addition are layer structure, have adsorptivity It can, additionally it is possible to improve the mechanical strength of active carbon.
The present invention is further arranged to: carbonization is to be passed through nitrogen into heating container first to row in the step 5 The air in container is heated to the greatest extent, and then cylindric shaped granule is put into heating container, is warming up to 2~10 DEG C/min rate 300~400 DEG C and 20~30min of heat preservation, then 500~600 DEG C of 10~20min of heat preservation are warming up to 5~10 DEG C/min rate, most 650~800 DEG C are warming up to 5~10 DEG C/min rate again afterwards, natural cooling.
By using above-mentioned technical proposal, under the conditions of 300~400 DEG C, raw material releases gaseous state based on deaerating and be dehydrated Product, such as CO2, CO and H2S etc., while also releasing free water, in conjunction with water and pyrolysis water, at this moment raw material mix does not change substantially Become.Under the conditions of 500~600 DEG C, many functional groups, aliphatic side chains fracture in raw material generate volatile matter, such as CH4, CO and H2Deng, At this moment remaining carbon skeleton is condensed on the carbon atom of aromatic rings periphery and generates a large amount of free radical, starts to tie between aromatic compound It closes, the mechanical strength of carbon granule is gradually increased.It is the stage based on polycondensation reaction under the conditions of 650~800 DEG C, carbonizes raw material The non-carbonizable substance such as hydrogen and oxygen is discharged in pyrolytic, after losing hydrogen and oxygen, carbon atom re-starts permutation and combination, due to carbon Arrangement between atom is irregular, therefore forms the hole between crystallite, these holes are the initial apertures of carbonized material Gap.It is that guarantee that the reaction in each stage can carry out thorough that charcoal, which is divided into the purpose that three temperature ranges gradually heat up and keep the temperature, Bottom is sufficiently reacted, to improve the effect of raw material charing, further promotes the performance of active carbon.
The present invention is further arranged to: activator is KOH, ZnCl in the step 62One of or it is a variety of.
By using above-mentioned technical proposal, the addition of KOH can be reacted with the C in raw material, and the boiling point of potassium simple substance is 762 DEG C, when activation temperature is higher than 762 DEG C, potassium atom steam is diffused between the carbon atomic layer of carbon atom composition, to carbon raw material It performs etching, the position being etched will appear hole, and KOH can also inhibit the generation of tar simultaneously.ZnCl is added2So that former containing C Material profit rises, ZnCl2Hydroxyl in organic matter is catalytically decomposed, hydroxyl is eliminated, inhibits coal tar or other carbon containing volatile matters Generation;ZnCl simultaneously2Hydrogen-oxygen atom in raw material can also be precipitated in the form of hydrone, later to original in activation process Expect that interior molecules carry out polycondensation reaction and realize aromatisation, to form pore structure abundant.
The present invention is further arranged to: oxygen-containing gas is air, CO in the step 62, one of vapor or a variety of Mixing.
By using above-mentioned technical proposal, air, CO are used2Or vapor activates activated carbon raw material, these contain With C redox reaction can occur for carrier of oxygen, corrode the surface of carbide, while removing the coke that raw material is generated in carbonization process Oily substance and substance is not carbonized, charing raw material is enabled to generate pore structure abundant.Under high temperature, activation oxygen-containing gas is first It is first to react with unordered C atom and hetero atom, it has been formed when by charing but has been blocked by unordered C atom and hetero atom Hole is opened, and microporous surface is exposed;Oxidation reaction quilt occurs for C atom and activated gas on the microporous surface exposed It burns and loses, so that the hole opened constantly expands and internally penetrates through;With the continuous progress of priming reaction, new active sites exposure In microporous surface, these new active sites can be reacted again with activated gas, and the uneven burning mistake of microporous surface can constantly be led Cause the formation of new hole.As priming reaction continues, hole constantly expands, and the hole wall between adjacent cells is lost by complete burn And larger hole is formed, to constantly increase the specific surface area of active carbon, improve the adsorption effect of active carbon.
The present invention is further arranged to: pickling solution is the HCl solution of 0.1mol/L in the step 7.
By using above-mentioned technical proposal, the purpose using hydrochloric acid solution pickling is the impurity for removing activated carbon surface, is kept away The duct for exempting from impurity blocking active carbon, influences the adsorption effect of active carbon, hydrochloric acid will not occur with the functional group of activated carbon surface Reaction, will not impact activated carbon structure.
In conclusion advantageous effects of the invention are as follows:
1. using biomass material, coal slime, wood powder and clay material as activated carbon raw material, do not need additionally to add bonding Agent can be prepared by pressed active carbon, and process is simple, and the active carbon large specific surface area prepared, absorption property are good;Activation In step, the infiltration that raw material first passes through activating agent preliminarily forms hole, using the further activation of oxygen-containing gas, thus favorably In preparing hole active carbon abundant, the absorption property of active carbon is improved;The purpose of pickling washing is on the one hand to remove The impurity of activated carbon surface avoids impurity from blocking the hole to be formed, and reduces adsorption effect, on the other hand removes and be immersed in active carbon Intrapore activator;
2. the purpose that biomass material carries out acidification is: biomass material is polysaccharide polymer, is passed through between molecule β-Isosorbide-5-Nitrae-glucosides key connection, acidification can be broken β-Isosorbide-5-Nitrae-glycosidic bond, so that biomass long-chain molecule is fractured into small molecule Chain substance reduces intramolecular and intermolecular bond energy, and it is thorough to be conducive to subsequent charing;
3. raw material releases gaseous products, such as CO2, CO and H2S, together based on deaerating and be dehydrated under the conditions of 300~400 DEG C When also release free water, in conjunction with water and pyrolysis water, at this moment raw material mix does not change substantially.It is former under the conditions of 500~600 DEG C Many functional groups, aliphatic side chains fracture in material, generate volatile matter, such as CH4, CO and H2, are left carbon skeleton, at this moment condensation virtue A large amount of free radical is generated on the carbon atom of fragrant ring periphery, starts to combine between aromatic compound, the mechanical strength of carbon granule is gradually It improves;It is the stage based on polycondensation reaction under the conditions of 650~800 DEG C, carbonizes raw material in pyrolytic for hydrogen and oxygen etc. Non- carbonizable substance discharge, after losing hydrogen and oxygen, carbon atom re-starts permutation and combination, since the arrangement between carbon atom is irregular , therefore the hole between crystallite is formd, these holes are that carbonized material promotes hole;Charcoal is divided into three temperature ranges The purpose for gradually heating up and keeping the temperature is to guarantee that the reaction in each stage can carry out thoroughly, is sufficiently reacted, to improve raw material The effect of charing further promotes the performance of active carbon.
Detailed description of the invention
Fig. 1 is preparation technology flow chart of the invention.
Specific embodiment
The present invention is described in further detail below.
Embodiment 1
A kind of preparation method of active carbon, specifically comprises the following steps:
Step 1, lignocellulosic it is cleaned, it is dry, smash it through that 60 meshes are spare, the lignocellulosic of crushing is acidified Processing obtains acidification powdered biomass, the acidization tool of lignocellulosic are as follows: be added into the lignocellulosic after crushing and screening Mass fraction is the hydrochloric acid of 10wt%, reacts 2h under the conditions of 140 DEG C after mixing evenly, after natural cooling, is filtered to remove filtrate, Filter residue is washed with deionized at least twice, ground 60 mesh after filter residue drying, as acidification powdered biomass;
Step 2, coal slime is handled to ash content through flotation no more than 25%, then obtains coal slime through drying, broken, 200 meshes excessively again Powder is spare;
Step 3, according to mass fraction meter, 10 parts of wood powder, 10 parts of sepiolite, the acidification powdered biomass prepared in step 1 are weighed 30 parts, 45 parts of coal slime powder prepared in step 2 are mixed evenly to obtain mixed raw material;
Step 4, form: it is 10mm that the mixed raw material in step 3 is compressed into diameter at normal temperature, and length is the cylindric of 15mm Shaped granule;
Step 5, it carbonizes: the cylindric shaped granule prepared in step 4 being placed in heating container and carries out charing process, it is naturally cold But to obtaining charing shaped granule after room temperature, carbonization is to be passed through nitrogen into heating container first to draining in heating container Air, then by cylindric shaped granule be put into heating container in, be warming up to 300 DEG C with 2 DEG C/min rate and keep the temperature 20min, then 500 DEG C of heat preservation 10min are warming up to 5 DEG C/min rate, 650 DEG C finally are warming up to 10 DEG C/min rate again, from It is so cooling;
Step 6, it activates: weighing 10 parts of the charing shaped granule prepared in step 5 according to mass fraction meter and infiltrated 20 5h in part KOH is filtered after infiltration, is dry, then in air atmosphere, being warming up to 600 DEG C and activated, activation time is 30min, cooled to room temperature obtains activation shaped granule after activation;
Step 7, the HCl solution of 0.1mol/L is first used to carry out pickling, by water the activation shaped granule prepared in step 6 It is washed till neutrality, obtains molding active carbon after dry.
Embodiment 2
A kind of preparation method of active carbon, specifically comprises the following steps:
Step 1, stalk it is cleaned, it is dry, smash it through that 60 meshes are spare, the stalk of crushing is subjected to acidification, obtains acid Metaplasia material powder, the acidization tool of stalk are as follows: the hydrochloric acid that mass fraction is 10wt% is added into the stalk after crushing and screening, It reacts 4h under the conditions of 180 DEG C after mixing evenly, after natural cooling, is filtered to remove filtrate, filter residue is washed with deionized at least Twice, ground 60 mesh after filter residue drying, as acidification powdered biomass;
Step 2, coal slime is handled to ash content through flotation no more than 25%, then obtains coal slime through drying, broken, 200 meshes excessively again Powder is spare;
Step 3, according to mass fraction meter, 15 parts of wood powder, 0 part of montmorillonite 2, the acidification powdered biomass prepared in step 1 are weighed 40 parts, 55 parts of coal slime powder prepared in step 2 are mixed evenly to obtain mixed raw material;
Step 4, form: it is 15mm that the mixed raw material in step 3 is compressed into diameter at normal temperature, and length is the cylindric of 20mm Shaped granule;
Step 5, it carbonizes: the cylindric shaped granule prepared in step 4 being placed in heating container and carries out charing process, it is naturally cold But to obtaining charing shaped granule after room temperature, carbonization is to be passed through nitrogen into heating container first to draining in heating container Air, then by cylindric shaped granule be put into heating container in, be warming up to 350 DEG C with 5 DEG C/min rate and keep the temperature 25min, then 600 DEG C of heat preservation 10min are warming up to 10 DEG C/min rate, 700 DEG C finally are warming up to 5 DEG C/min rate again, from It is so cooling;
Step 6, it activates: weighing 15 parts of the charing shaped granule prepared in step 5 according to mass fraction meter and infiltrated 20 KOH and 20 part of ZnCl of part210h in mixed solution is filtered after infiltration, is dry, then in CO2Under atmosphere, it is warming up to 700 DEG C It is activated, activation time 60min, cooled to room temperature obtains activation shaped granule after activation;
Step 7, the HCl solution of 0.1mol/L is first used to carry out pickling, by water the activation shaped granule prepared in step 6 It is washed till neutrality, obtains molding active carbon after dry.
Embodiment 3
A kind of preparation method of active carbon, specifically comprises the following steps:
Step 1, shell it is cleaned, it is dry, smash it through that 60 meshes are spare, the shell of crushing is subjected to acidification, obtains acid Metaplasia material powder, the acidization tool of shell are as follows: the sulfuric acid that mass fraction is 10wt% is added into the shell after crushing and screening, It reacts 6h under the conditions of 200 DEG C after mixing evenly, after natural cooling, is filtered to remove filtrate, filter residue is washed with deionized at least Twice, ground 60 mesh after filter residue drying, as acidification powdered biomass;
Step 2, coal slime is handled to ash content through flotation no more than 25%, then obtains coal slime through drying, broken, 200 meshes excessively again Powder is spare;
Step 3, according to mass fraction meter, 13 parts of wood powder, 15 parts of illite, the acidification powdered biomass prepared in step 1 are weighed 35 parts, 60 parts of coal slime powder prepared in step 2 are mixed evenly to obtain mixed raw material;
Step 4, form: it is 12mm that the mixed raw material in step 3 is compressed into diameter at normal temperature, and length is the cylindric of 18mm Shaped granule;
Step 5, it carbonizes: the cylindric shaped granule prepared in step 4 being placed in heating container and carries out charing process, it is naturally cold But to obtaining charing shaped granule after room temperature, carbonization is to be passed through nitrogen into heating container first to draining in heating container Air, then by cylindric shaped granule be put into heating container in, be warming up to 400 DEG C with 10 DEG C/min rate and keep the temperature 30min, then 550 DEG C of heat preservation 20min are warming up to 10 DEG C/min rate, 800 DEG C finally are warming up to 5 DEG C/min rate again, from It is so cooling;Step 6, it activates: weighing 10 parts of the charing shaped granule prepared in step 5 according to mass fraction meter and infiltrated 30 parts of ZnCl2Middle 15h is filtered after infiltration, is dry, then under steam atmosphere, being warming up to 800 DEG C and activated, living The change time is 90min, and cooled to room temperature obtains activation shaped granule after activation;
Step 7, the HCl solution of 0.1mol/L is first used to carry out pickling, by water the activation shaped granule prepared in step 6 It is washed till neutrality, obtains molding active carbon after dry.
Embodiment 4
A kind of preparation method of active carbon, specifically comprises the following steps:
Step 1, straw it is cleaned, it is dry, smash it through that 60 meshes are spare, the straw of crushing is subjected to acidification, obtains acid Metaplasia material powder, the acidization tool of straw are as follows: the sulfuric acid that mass fraction is 10wt% is added into the straw after crushing and screening, It reacts 4h under the conditions of 160 DEG C after mixing evenly, after natural cooling, is filtered to remove filtrate, filter residue is washed with deionized at least Twice, ground 60 mesh after filter residue drying, as acidification powdered biomass;
Step 2, coal slime is handled to ash content through flotation no more than 25%, then obtains coal slime through drying, broken, 200 meshes excessively again Powder is spare;
Step 3, according to mass fraction meter, 15 parts of wood powder, 10 parts of montmorillonite, 5 parts of sepiolite, the acidification prepared in step 1 are weighed 50 parts of the coal slime powder prepared in 35 parts of powdered biomass, step 2 is mixed evenly to obtain mixed raw material;
Step 4, form: it is 10mm that the mixed raw material in step 3 is compressed into diameter at normal temperature, and length is the cylindric of 20mm Shaped granule;
Step 5, it carbonizes: the cylindric shaped granule prepared in step 4 being placed in heating container and carries out charing process, it is naturally cold But to obtaining charing shaped granule after room temperature, carbonization is to be passed through nitrogen into heating container first to draining in heating container Air, then by cylindric shaped granule be put into heating container in, be warming up to 350 DEG C with 5 DEG C/min rate and keep the temperature 20min, then 600 DEG C of heat preservation 15min are warming up to 5 DEG C/min rate, 750 DEG C finally are warming up to 5 DEG C/min rate again, nature It is cooling;
Step 6, it activates: weighing 15 parts of the charing shaped granule prepared in step 5 according to mass fraction meter and infiltrated 35 10h in part KOH is filtered after infiltration, is dry, then under steam atmosphere, being warming up to 900 DEG C and activated, when activation Between be 30min, after activation cooled to room temperature obtain activation shaped granule;
Step 7, the HCl solution of 0.1mol/L is first used to carry out pickling, by water the activation shaped granule prepared in step 6 It is washed till neutrality, obtains molding active carbon after dry.
Embodiment 5
The difference from example 2 is that activation temperature is 750 DEG C in step 6, the other the same as in Example 2.
Embodiment 6
The difference from example 2 is that activation temperature is 800 DEG C in step 6, the other the same as in Example 2.
Embodiment 7
The difference from example 2 is that activation temperature is 850 DEG C in step 6, the other the same as in Example 2.
Embodiment 8
The difference from example 2 is that activation temperature is 900 DEG C in step 6, the other the same as in Example 2.
Active carbon prepared by 1~embodiment of embodiment 8 performs the following performance tests:
Specific surface area: nitrogen adsorption isotherm measurement is enterprising in full-automatic specific surface area and pore analysis instrument Tristar II 3020 Row is 77K in adsorption temp, relative pressure (P/P0) is surveyed in the range of being 0.01~1.0 using nitrogen as adsorbing medium It is fixed, and sample deaerates 12h at a temperature of 573K before testing, the specific surface area of active carbon is obtained according to BET equation calculation;
Iodine sorption value: it is measured according to GB/T12496.8-1999 " wood activated charcoal experimental method: the measuring method of iodine sorption value ";
Activated carbon separation performance: after iodine sorption value measurement, whether isolating active carbon adsorbent, observation active carbon has been kept It is whole, if pressed active carbon does not disperse, result be it is yes, active carbon dispersion, result is no;
Intensity value measurement: active carbon intensity value is measured according to GB/T15459-2006 " the drop strength measuring method of coal ".
The performance test results of the active carbon of 1 1~embodiment of embodiment 8 of table preparation
Illustrate according to testing result, active carbon prepared by 1~embodiment of embodiment 8 is after testing iodine sorption value, activity Charcoal does not disperse, convenient completely to separate from adsorbate solution.Comparative example 2,5~embodiment of embodiment 8 show with activation The raising of temperature, the specific surface area of active carbon first increases to be reduced afterwards, and iodine sorption value is also first to increase the trend reduced afterwards, activation temperature When spending low, the activation decomposition reaction of activator and biomass material is insufficient, causes its adsorption capacity poor;With the liter of temperature Height, priming reaction is abundant, promotes the generation of pore structure, enhances the adsorption capacity of active carbon.When temperature is further continued for increasing, Excessively high temperature can aggravate burning for pore structure, so that the micropore generated collapses, its absorption property be caused to decline.
This specific embodiment is only explanation of the invention, not limitation of the present invention, and those skilled in the art exist It can according to need the modification that not creative contribution is made to the present embodiment after reading this specification, but as long as in the present invention Scope of the claims in all by the protection of Patent Law.

Claims (8)

1. a kind of preparation method of active carbon, it is characterised in that: specifically comprise the following steps:
Step 1, biomass material is cleaned, dry, to smash it through 60 meshes spare, will
The biomass material of crushing carries out acidification, obtains acidification powdered biomass;
Step 2, coal slime is handled to ash content through flotation no more than 25%, then obtains coal slime through drying, broken, 200 meshes excessively again Powder is spare;
Step 3, according to mass fraction meter, 10~15 parts of wood powder, 10~15 parts of clay mineral, the acidification prepared in step 1 are weighed 45~60 parts of the coal slime powder prepared in 30~40 parts of powdered biomass, step 2 is mixed evenly to obtain mixed raw material;
Step 4, form: it is 10~15mm that the mixed raw material in step 3 is compressed into diameter at normal temperature, and length is 15~20mm Cylindric shaped granule;
Step 5, it carbonizes: the cylindric shaped granule prepared in step 4 being placed in heating container and carries out charing process, it is naturally cold But to obtaining charing shaped granule after room temperature;
Step 6, it activates: weighing 10~20 parts of the charing shaped granule prepared in step 5 according to mass fraction meter and infiltrated 5~15h in 20~40 parts of activators is filtered after infiltration, is dry, then under oxygen-containing gas atmosphere, it is warming up to 600~ 900 DEG C are activated, and activation time is 30~90min, and cooled to room temperature obtains activation shaped granule after activation;
Step 7, the activation shaped granule prepared in step 6 is first subjected to pickling, by being washed to neutrality, is obtained into after dry Type active carbon.
2. a kind of preparation method of active carbon according to claim 1, it is characterised in that: biomass is former in the step 1 Material is one of lignocellulosic, stalk, shell, straw.
3. a kind of preparation method of active carbon according to claim 1, it is characterised in that: acid processing in the step 1 Method are as follows: the hydrochloric acid or sulfuric acid that mass fraction is 10wt% are added into the biomass material after crushing and screening, exists after mixing evenly 2~6h is reacted under the conditions of 140~200 DEG C, after natural cooling, is filtered to remove filtrate, filter residue is washed with deionized at least twice, Ground 60 mesh after filter residue drying, as acidification powdered biomass.
4. a kind of preparation method of active carbon according to claim 1, it is characterised in that: step 3 CLAY MINERALS AND THEIR SIGNIFICANCE For one of montmorillonite, illite, sepiolite or a variety of.
5. a kind of preparation method of active carbon according to claim 1, it is characterised in that: carbonization in the step 5 To be passed through nitrogen into heating container to the air drained in heating container first, cylindric shaped granule is then put into heating In container, 300~400 DEG C are warming up to 2~10 DEG C/min rate and keeps the temperature 20~30min, then with 5~10 DEG C/min rate liter Temperature is finally warming up to 650~800 DEG C again to 500~600 DEG C of 10~20min of heat preservation with 5~10 DEG C/min rate, natural cooling.
6. a kind of preparation method of active carbon according to claim 1, it is characterised in that: activator is in the step 6 KOH、ZnCl2One of or it is a variety of.
7. a kind of preparation method of active carbon according to claim 1, it is characterised in that: oxygen-containing gas in the step 6 For air, CO2, one of vapor or a variety of mixing.
8. a kind of preparation method of active carbon according to claim 1, it is characterised in that: pickling solution in the step 7 For the HCl solution of 0.1mol/L.
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CN110975816A (en) * 2020-01-03 2020-04-10 田得君 Columnar activated carbon and preparation method thereof
CN111115626A (en) * 2019-12-26 2020-05-08 山东大学 Charcoal making system and method for preparing biomass activated carbon through one-step rapid carbonization and activation
CN111704134A (en) * 2020-07-12 2020-09-25 兰州理工大学 Wave-absorbing material based on agricultural and forestry waste recycling and preparation method thereof
CN111848166A (en) * 2020-08-11 2020-10-30 景德镇陶瓷大学 Columnar carbon granules with illite, low-temperature flux and walnut shell powder as main raw materials and preparation method thereof
CN111995063A (en) * 2020-08-18 2020-11-27 普罗生物技术(上海)有限公司 Powdered activated carbon carrier and preparation method and application thereof
CN112011380A (en) * 2020-09-01 2020-12-01 山东阳光电力有限公司 Straw combustion power generation process optimization method and matched production line thereof
CN112209377A (en) * 2020-11-18 2021-01-12 江西尚绿科技有限公司 Activated carbon production process
CN112275254A (en) * 2020-10-14 2021-01-29 四川长晏科技有限公司 Wastewater treatment agent and preparation method and application thereof
CN115124036A (en) * 2022-06-24 2022-09-30 闽西职业技术学院 Preparation method of dragon fruit peel activated carbon for adsorbing phenol in wastewater
CN115446078A (en) * 2022-08-31 2022-12-09 四川轻化工大学 Processing method for microwave pyrolysis of waste cinnamomum longepaniculatum branches and leaves
CN115676824A (en) * 2022-11-09 2023-02-03 余昭军 Modified blue carbon powder for blast furnace injection and preparation method thereof

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Cited By (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111115626A (en) * 2019-12-26 2020-05-08 山东大学 Charcoal making system and method for preparing biomass activated carbon through one-step rapid carbonization and activation
CN110975816A (en) * 2020-01-03 2020-04-10 田得君 Columnar activated carbon and preparation method thereof
CN111704134A (en) * 2020-07-12 2020-09-25 兰州理工大学 Wave-absorbing material based on agricultural and forestry waste recycling and preparation method thereof
CN111848166B (en) * 2020-08-11 2022-12-30 景德镇陶瓷大学 Columnar carbon granules with illite, low-temperature flux and walnut shell powder as main raw materials and preparation method thereof
CN111848166A (en) * 2020-08-11 2020-10-30 景德镇陶瓷大学 Columnar carbon granules with illite, low-temperature flux and walnut shell powder as main raw materials and preparation method thereof
CN111995063A (en) * 2020-08-18 2020-11-27 普罗生物技术(上海)有限公司 Powdered activated carbon carrier and preparation method and application thereof
CN112011380A (en) * 2020-09-01 2020-12-01 山东阳光电力有限公司 Straw combustion power generation process optimization method and matched production line thereof
CN112011380B (en) * 2020-09-01 2021-12-24 山东阳光电力有限公司 Straw combustion power generation optimization process
CN112275254A (en) * 2020-10-14 2021-01-29 四川长晏科技有限公司 Wastewater treatment agent and preparation method and application thereof
CN112209377A (en) * 2020-11-18 2021-01-12 江西尚绿科技有限公司 Activated carbon production process
CN115124036A (en) * 2022-06-24 2022-09-30 闽西职业技术学院 Preparation method of dragon fruit peel activated carbon for adsorbing phenol in wastewater
CN115446078A (en) * 2022-08-31 2022-12-09 四川轻化工大学 Processing method for microwave pyrolysis of waste cinnamomum longepaniculatum branches and leaves
CN115446078B (en) * 2022-08-31 2023-11-24 四川轻化工大学 Treatment method for microwave pyrolysis of waste camphor tree branches and leaves
CN115676824A (en) * 2022-11-09 2023-02-03 余昭军 Modified blue carbon powder for blast furnace injection and preparation method thereof
CN115676824B (en) * 2022-11-09 2024-02-13 贺州优鑫矿业有限公司 Modified semi-coke powder for blast furnace injection and preparation method thereof

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