CN106672965B - A method for preparing high specific surface hierarchically porous activated carbon from cotton straw - Google Patents
A method for preparing high specific surface hierarchically porous activated carbon from cotton straw Download PDFInfo
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- CN106672965B CN106672965B CN201710008199.6A CN201710008199A CN106672965B CN 106672965 B CN106672965 B CN 106672965B CN 201710008199 A CN201710008199 A CN 201710008199A CN 106672965 B CN106672965 B CN 106672965B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 64
- 229920000742 Cotton Polymers 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 33
- 239000010902 straw Substances 0.000 title claims description 10
- 239000000463 material Substances 0.000 claims abstract description 73
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000012190 activator Substances 0.000 claims abstract description 24
- 238000002386 leaching Methods 0.000 claims abstract description 18
- 239000008367 deionised water Substances 0.000 claims abstract description 14
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 10
- 238000000227 grinding Methods 0.000 claims abstract description 6
- 239000012535 impurity Substances 0.000 claims abstract description 6
- 238000000926 separation method Methods 0.000 claims abstract description 3
- 230000004913 activation Effects 0.000 claims description 23
- 238000004140 cleaning Methods 0.000 claims description 19
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 15
- 239000000843 powder Substances 0.000 claims description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 10
- 239000011162 core material Substances 0.000 claims description 9
- 238000002360 preparation method Methods 0.000 claims description 9
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 239000000428 dust Substances 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 5
- 235000006040 Prunus persica var persica Nutrition 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 4
- 239000003513 alkali Substances 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000010985 leather Substances 0.000 claims 3
- 239000002245 particle Substances 0.000 claims 3
- 240000006413 Prunus persica var. persica Species 0.000 claims 1
- 239000012670 alkaline solution Substances 0.000 claims 1
- 229910017053 inorganic salt Inorganic materials 0.000 claims 1
- 229910052799 carbon Inorganic materials 0.000 abstract description 21
- 230000008569 process Effects 0.000 abstract description 8
- 238000012545 processing Methods 0.000 abstract description 7
- 238000012216 screening Methods 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 239000003518 caustics Substances 0.000 abstract description 4
- 238000000605 extraction Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 description 18
- 239000012620 biological material Substances 0.000 description 9
- 239000003610 charcoal Substances 0.000 description 9
- 238000010792 warming Methods 0.000 description 9
- 239000002028 Biomass Substances 0.000 description 7
- 239000000203 mixture Substances 0.000 description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 238000005253 cladding Methods 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 239000011148 porous material Substances 0.000 description 5
- 239000002243 precursor Substances 0.000 description 5
- 241000196324 Embryophyta Species 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 244000144730 Amygdalus persica Species 0.000 description 3
- 239000002250 absorbent Substances 0.000 description 3
- 230000002745 absorbent Effects 0.000 description 3
- 239000006227 byproduct Substances 0.000 description 3
- 238000004364 calculation method Methods 0.000 description 3
- 239000003245 coal Substances 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 238000004090 dissolution Methods 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 239000012299 nitrogen atmosphere Substances 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 238000002791 soaking Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 241001640034 Heteropterys Species 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 210000003850 cellular structure Anatomy 0.000 description 2
- 238000007598 dipping method Methods 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 229920005610 lignin Polymers 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 241000609240 Ambelania acida Species 0.000 description 1
- 108010010803 Gelatin Proteins 0.000 description 1
- 229920002488 Hemicellulose Polymers 0.000 description 1
- 229910003481 amorphous carbon Inorganic materials 0.000 description 1
- 239000010905 bagasse Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- CREMABGTGYGIQB-UHFFFAOYSA-N carbon carbon Chemical compound C.C CREMABGTGYGIQB-UHFFFAOYSA-N 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229920000159 gelatin Polymers 0.000 description 1
- 239000008273 gelatin Substances 0.000 description 1
- 235000019322 gelatine Nutrition 0.000 description 1
- 235000011852 gelatine desserts Nutrition 0.000 description 1
- 230000012010 growth Effects 0.000 description 1
- -1 has template Chemical compound 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000005445 natural material Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000001814 pectin Substances 0.000 description 1
- 229920001277 pectin Polymers 0.000 description 1
- 235000010987 pectin Nutrition 0.000 description 1
- 239000002006 petroleum coke Substances 0.000 description 1
- 230000008635 plant growth Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000013077 target material Substances 0.000 description 1
Classifications
-
- 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
-
- 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
-
- 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
Landscapes
- Carbon And Carbon Compounds (AREA)
Abstract
The invention belongs to active carbon fields, are a kind of methods for preparing high-ratio surface multistage mesoporous activated carbon with cotton stalk.Include: one, pretreatment: being prepared including (1) raw material: cotton stalk is crushed to 5~15mm of partial size, screening removal of impurities by or without core-skin separation；(2) clear water rinses: being rinsed, is dehydrated with water；(3) rub dump leaching: rubbing squeezes out extraction raffinate dump leaching to sub-wire after weak caustic solution dump leaching is added；(4) Hong quick-fried processing: merging closed pressure vessel is passed through high steam, is kept for 1.0MPa~2.5MPa air pressure 5~20 minutes, material and steam and pressure release discharged in 60~75ms to normal pressure, material is produced；(5) deionized water rinses: being rinsed, is dehydrated with deionized water；(6) it dries；Two, add activator；Three, drying grinding；Four, it activates；Five, it cleans；Six, dry.The present invention can utilize cotton stalk carbon source, and simple process, activator level is small, and production cost is low, be suitble to promote.
Description
Technical field
It is specifically a kind of to prepare high-ratio surface multi-stage porous activity with cotton stalk the invention belongs to active carbon preparation technical field
The method of charcoal.
Background technique
Active carbon is black powder or granular amorphous carbon, also includes the crystal carbon of marshalling.Active carbon by
In its have the characteristics that large specific surface area, conduct electricity very well, electrochemical stability is good, adsorption capacity is strong, therefore be widely used
In fields such as gas absorption separation, food processing, the electrode material of supercapacitor, medical treatment, environmental protection, national defence, agriculturals.Active carbon
Preparation method predominantly by natural material (such as bagasse, cotton stalk, shell) charing after, then with activator mixing high temperature work
Change and obtains.The carbon source that active carbon uses is prepared as cotton stalk, is the waste of agricultural product, not only increases the additional of agricultural product
Value, and have many advantages, such as that the specific surface area of active carbon environmental-friendly, from a wealth of sources, low in cost, to be prepared is higher.But
It is that activated carbon structure is still more single, based on micropore, absorption property is poor, and preparation process consumes a large amount of activator.
The persursor material of active carbon is prepared, can be divided mainly into two major class: plant and mineral substance at present.Plant is given birth to
Material mainly has: timber, stalk, cauline leaf, shell etc..Using the natural structure of biological material, micropore hair can be made
It reaches, the very high active carbon of specific surface area, and mechanical strength with higher.Mineral substance raw material have: coal, petroleum coke, synthesis
Resin etc., in these raw material, coal resources are the most abundant, but coal texture and component characteristic directly affect active carbon
Performance, ash content is high and is difficult to generate flourishing micropore.
Using the especially various biological materials of renewable biomass as active carbon carbon matrix precursor material is prepared, raw material is rich
Richness, method are easy, economically feasible, environmentally friendly and the endemic element and structure that can use biological material itself and have.
By corresponding process modification, people have been able to prepare the activity of the high-performance with unique texture using biological material
Carbon causes many researchs both domestic and external and concern.
Biological material is mainly grouped as by cellulose, hemicellulose and three great achievement of lignin, but these three components exist
Composition, structure in plant and distribution can be different and different because of the type of plant, the place of production and growth period etc..In addition, biomass
Needed for also containing the organic compounds such as a small amount of pectin, fat, wax and plant growth in stalk, and in raw material transport and life
Various metallic elements of bring etc. during production.This makes the chemical component of biomass straw and structure extremely complex, also causes
There are great differences or even completely different for the pretreatment of different biomass straws and Land use systems.
It is pre-processed currently, biological material is generally required when preparing active carbon as persursor material, method
Biological material is usually crushed to powder, distinctive natural fine cellular structure does not pass through corresponding technique hand
Section is made full use of, therefore existing activated carbon from activated sludge technology of preparing solves only the Utilizing question of biological material, and
The microscopic characteristics in the institutional framework of biological material are not made full use of, biomass microcellular structure and micropore surface are expanded
Product.
Specific to cotton stalk, content of lignin is higher than general biomass material, while ash content and gelatin substance content
Height makes it have the good natural endowment as activated carbon precursor, but has the shortcomings that be more difficult to processing and utilization.
On the other hand, the preparation method of multistage mesoporous activated carbon mainly has template, chemical activation method and physically activated at present
Method.Template is usually to select a kind of material of special pore structure as template, import target material or presoma and make its
React in the hole of mould material, using mould material limitation act on, realize in preparation process physics and chemistry it is anti-
It should control, finally obtain the new material of structure-controllable.The pore structure and pattern for the multi-stage porous Carbon Materials that the method obtains are by hard mold
The limitation of plate, and template preparation process is relative complex, higher cost.Physical activation method is first to carbonize raw material, then again
It is activated with vapor or carbon dioxide, this production process is simple, cleaning, and there is no equipment corrosion and environmental pollution to ask
Topic, but it is generally necessary to higher activation temperature and longer activation time, energy consumption are also higher.Chemical activation method be usually pass through by
The presoma and activator of charcoal are mixed, then high-temperature calcination, and the higher active carbon of specific surface area can be obtained, but can consume
A large amount of alkali activator, and have serious corrosivity to equipment.
China is large agricultural country, possesses cotton stalk resource abundant, the idle waste of wherein most or on-site incineration,
Cause serious air environmental pollution.
It is therefore desirable to study a kind of natural hole framework that can make full use of cotton stalk, simple process, activator consumption
Amount is few, realizes the method that low cost prepares high-specific surface area multistage mesoporous activated carbon.
Summary of the invention
The purpose of the present invention is using cheap and easy to get, environmental-friendly cotton stalk, processed by special pretreating process,
Obtain the carbon source material for the microcosmic duct architecture for having excellent；A step activation method is used again, and inorganic salts are used in activator
Instead of a part of highly basic, activator consumption is greatly lowered, and is also considerably reduced to equipment extent of corrosion, to realize droning local
Prepare high-ratio surface multistage mesoporous activated carbon.
The technical scheme is that
A method of high-ratio surface multistage mesoporous activated carbon being prepared with cotton stalk, is implemented according to the following steps:
Step 1 pretreatment: including (1) raw material prepare: by cotton stalk, separate and removes by core-skin peach, leaf, carefully
The cladding and core material obtained after branch crushes obtain the cladding and core material of 5~15mm of partial size respectively, or separates directly without core-skin
Crushing is connect, the non-separating material of 5~15mm of partial size is obtained；Then the qualified material of 5~15mm of partial size is screened out, screening removes powder
Dirt, impurity；(2) clear water rinses: material being rinsed with water, is then dehydrated；(3) rub dump leaching: it is molten that weak base is added in material
Dump leaching after liquid, machinery rubbing to its sub-wire, squeezes out surplus liquid, again dump leaching；(4) material Hong quick-fried processing: is placed in closed pressure
In force container, be passed through high steam, kept for 1.0MPa~2.5MPa air pressure 5~20 minutes, discharged in 60~75ms material and
Steam simultaneously to normal pressure, produce for pressure release by material；(5) deionized water rinses: material being rinsed with deionized water, is dehydrated；(6) it dries:
Material is uniformly dried；
Step 2 adds activator: resulting material and appropriate activator aqueous solution are sufficiently impregnated dissolving；
Step 3 drying grinding: it is ground into powder after the moisture in material is removed；
Step 4 activation: material is subjected to activation heat treatment under the conditions of nitrogen protection；
Step 5 cleaning: material is cleaned；
Step 6 is dry: being dried material to get high-ratio surface multistage mesoporous activated carbon.
The invention also includes optimization or/and improvement have:
One of preferred embodiment: the activator aqueous solution in the step 2 is the mixed solution of inorganic salts and alkali；
The two of preferred embodiment: the dosage mass ratio of the activator and preceding material is 2~3:7.5；
The three of preferred embodiment: the temperature of the step 4 activation heat treatment is 800 DEG C, time 2h；
The four of preferred embodiment: the cleaning in the step 5 is hydrochloric acid cleaning and deionized water cleaning respectively.
Further preferred embodiment has:
The five of preferred embodiment: the activator aqueous solution in the step 2 is the mixed solution of potassium carbonate and potassium hydroxide；
The six of preferred embodiment: the concentration of hydrochloric acid in the step 5 is 1mol/L.
The beneficial effect for implementing technical solution of the present invention is:
The present invention prepares active carbon using cotton stalk as carbon source material, belongs to the waste of agricultural product, not only increases
The added value of agricultural product, and have many advantages, such as environmental-friendly, from a wealth of sources, low in cost, the active carbon being prepared compares table
Area is higher, and pore-size distribution is good；
The present invention can make full use of the natural fine cellular structure of cotton stalk to be expanded by special pretreating process
At more flourishing biomass microcellular structure, the active carbon of preparation is enabled to obtain bigger specific surface area and more flourishing hole
Distribution；
The present invention additionally uses one-step preparation process, and replaces a part of highly basic, activator with inorganic salts in activator
Consumption is greatly lowered, and is also considerably reduced to equipment extent of corrosion, so that it is living to realize that droning local prepares high-ratio surface multi-stage porous
Property charcoal.
To sum up, present invention process is simple, and production cost is low, and good product quality, sustainability is strong, is suitble to promote and apply.
Below with reference to the embodiment technical solution that the present invention will be described in detail.
Detailed description of the invention
Nothing.
Specific embodiment
Technical solution in order to enable those skilled in the art to better understand the present invention, below with embodiment to the present invention make into
One step it is described in detail.
Embodiment 1
It takes 1.0t cotton stalk as activated carbon precursor material, the steps include:
Step 1 pretreatment: (1) prepared by raw material: by cotton stalk, after core-skin separates and removes peach, leaf, withe
Obtained cladding and core material crushes respectively obtains the cladding and core material of 5~15mm of partial size, or separates direct powder without core-skin
It is broken, obtain the non-separating material of 5~15mm of partial size；Then the qualified material of 5~15mm of partial size is screened out, screening removes dust, miscellaneous
Matter；(2) clear water rinses: material being rinsed with water, is then dehydrated；(3) dump leaching is rubbed: by heap after material addition weak caustic solution
Leaching, machinery rubbing to its sub-wire, squeezes out surplus liquid, again dump leaching；(4) material Hong quick-fried processing: is placed in closed pressure vessel
It is interior, it is passed through high steam, is kept for 1.0MPa~2.5MPa air pressure 5~20 minutes, discharges material and steam simultaneously in 60~75ms
Pressure release to normal pressure, material is produced；(5) deionized water rinses: material being rinsed with deionized water, is dehydrated；(6) it dries: by material
Uniformly drying obtains 0.3t pretreatment cotton stalk；
Step 2 adds activator: be in mass ratio 1:2 by potassium hydroxide, potassium carbonate and the present embodiment pretreatment cotton stalk:
7.5 ratio mixing is dissolved in water, stirs evenly, which is standing and soaking for 24 hours, makes to pre-process cotton stalk and aqueous slkali is abundant
Dipping dissolution；
Step 3 drying grinding: obtained mixture is placed in 100 DEG C of baking ovens dry 12h, removes the water in mixture
Point, obtained product is ground into powder；
Step 4 activation: the solid powder is placed in tube furnace, under nitrogen protection, is heated up with the rate of 10 DEG C/min
To 100 DEG C, 1h is kept, then be warming up to 300 DEG C with the rate, sets 1 DEG C/min for rate at this time and be warming up to 400 DEG C, continue
800 DEG C are warming up to the rate of 10 DEG C/min, and keeps 2h, is cooled to room temperature under nitrogen atmosphere, obtains activation products；
Step 5 cleaning: obtained activation products are first cleaned with the HCl of 1mol/L, are neutralized, by product after cleaning spend from
Sub- water is cleaned to pH=7~8；
Step 6 is dried: product after cleaning being dried 12h in 100 DEG C of baking oven, it is living to obtain high-specific surface area multi-stage porous
Property charcoal 0.08t.
The absorbent charcoal material that the present embodiment obtains is tested and analyzed through BJH calculation method, which has micropore, mesoporous simultaneously
With the hierarchical porous structure of macropore, and biggish specific surface area can be obtained through step activation, specific surface area reaches 2398.6m2/ g, hole
Gap volume 1.727cm3/ g, average pore size 2.925nm.
Embodiment 2
It takes 1.0t cotton stalk as activated carbon precursor material, the steps include:
Step 1 pretreatment: (1) prepared by raw material: by cotton stalk, after core-skin separates and removes peach, leaf, withe
It obtains 0.5t core material and is crushed to 5~15mm of partial size, screening removes dust, impurity screening removes dust, impurity, and partial size is greater than
The cladding return of 15mm continues to crush, and the unqualified material by size less than 5mm is discarded；(2) clear water rinse: by material water into
Row rinsing, is then dehydrated；(3) it rubs dump leaching: material being added after the NaOH weak caustic solution of 3% pH=9 dump leaching 48 hours, it is mechanical
Rubbing squeezes out surplus liquid, again dump leaching 30 hours to its sub-wire；(4) material Hong quick-fried processing: is placed in closed pressure vessel
It is interior, it is passed through high steam, is kept for 2.0~2.5MPa air pressure 5~10 minutes, discharge material and steam in 60ms and pressure release is to normal
Pressure, material are produced；(5) deionized water rinses: material being rinsed with deionized water, is dehydrated；(6) it dries: material is uniformly dried,
Obtain 0.35t pretreatment cotton stalk；
Step 2 adds activator: be in mass ratio 1:2 by potassium hydroxide, potassium carbonate and the present embodiment pretreatment cotton stalk:
7.5 ratio mixing is dissolved in water, stirs evenly, which is standing and soaking for 24 hours, soak cotton stalk cladding and aqueous slkali sufficiently
Stain dissolution；
Step 3 drying grinding: obtained mixture is placed in 100 DEG C of baking ovens dry 12h, removes the moisture in mixture,
Obtained product is ground into powder；
Step 4 activation: the solid powder is placed in tube furnace, under nitrogen protection, is heated up with the rate of 10 DEG C/min
To 100 DEG C, 1h is kept, then be warming up to 300 DEG C with the rate, sets 1 DEG C/min for rate at this time and be warming up to 400 DEG C, continue
800 DEG C are warming up to the rate of 10 DEG C/min, and keeps 2h, is cooled to room temperature under nitrogen atmosphere, obtains activation products；
Step 5 cleaning: obtained activation products are first cleaned with the HCl of 1mol/L, are neutralized, by product after cleaning spend from
Sub- water is cleaned to pH=7~8；
Step 6 is dried: product after cleaning being dried 12h in 100 DEG C of baking oven, it is living to obtain high-specific surface area multi-stage porous
Property charcoal 0.1t.
The absorbent charcoal material that the present embodiment obtains is tested and analyzed through BJH calculation method, which has micropore, mesoporous simultaneously
With the hierarchical porous structure of macropore, and biggish specific surface area can be obtained through step activation, specific surface area reaches 2261.1m2/ g, hole
Gap volume 1.641cm3/ g, average pore size 2.903nm.
Embodiment 3
It takes 1.0t cotton stalk as activated carbon precursor material, the steps include:
Step 1 pretreatment: (1) prepared by raw material: taking a certain amount of cotton stalk, separates without core-skin, be directly crushed to partial size
Chalk dust removing, impurity are removed in 5~15mm, screening；(2) clear water rinses: material being rinsed, is dehydrated to water content about；(3) heap is rubbed
Leaching: material being added after the NaOH weak caustic solution of 1% pH=9.5 dump leaching 48 hours, and machinery rubbing squeezes out extra liquid to its sub-wire
Body, again dump leaching 42 hours；(4) Hong quick-fried processing: material being placed in closed pressure vessel, high steam is passed through, and is kept
1.0MPa air pressure 5 minutes, material and steam and pressure release are discharged to normal pressure with the time of 60ms, material is produced；(5) deionized water is floated
It washes: material is rinsed with deionized water, be dehydrated；(6) it dries: material is uniformly dried, obtain 0.7t pretreatment cotton stalk；
Step 2 adds activator: be in mass ratio 1:2 by potassium hydroxide, potassium carbonate and the present embodiment pretreatment cotton stalk:
7.5 ratio mixing is dissolved in water, stirs evenly, which is standing and soaking for 24 hours, makes to pre-process cotton stalk and aqueous slkali is abundant
Dipping dissolution；
Step 3 drying grinding: obtained mixture is placed in 100 DEG C of baking ovens dry 12h, removes the water in mixture
Point, obtained product is ground into powder；
Step 4 activation: the solid powder is placed in tube furnace, under nitrogen protection, is heated up with the rate of 10 DEG C/min
To 100 DEG C, 1h is kept, then be warming up to 300 DEG C with the rate, sets 1 DEG C/min for rate at this time and be warming up to 400 DEG C, continue
800 DEG C are warming up to the rate of 10 DEG C/min, and keeps 2h, is cooled to room temperature under nitrogen atmosphere, obtains activation products；
Step 5 cleaning: obtained activation products are first cleaned with the HCl of 1mol/L, are neutralized, by product after cleaning spend from
Sub- water is cleaned to pH=7~8；
Step 6 is dried: will be dried 12h after cleaning in 100 DEG C of product of baking oven, is obtained high-specific surface area multi-stage porous activity
Charcoal 0.2t.
The absorbent charcoal material that the present embodiment obtains is tested and analyzed through BJH calculation method, which has micropore, mesoporous simultaneously
With the hierarchical porous structure of macropore, and biggish specific surface area can be obtained through step activation, specific surface area reaches 1963.3m2/ g, hole
Gap volume 1.415cm3/ g, average pore size 2.88nm.
It is understood that the principle that above embodiments are intended to be merely illustrative of the present and the exemplary embodiment party that uses
Formula, however the present invention is not limited thereto, implementer can the well-known techniques in conjunction with actual conditions according to the technique and scheme of the present invention
To determine specific embodiment.For those skilled in the art, spirit and reality of the invention are not being departed from
In the case where matter, various changes and modifications can be made therein, these increased variations and modifications are also considered as protection scope of the present invention.
Claims (7)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710008199.6A CN106672965B (en) | 2017-01-05 | 2017-01-05 | A method for preparing high specific surface hierarchically porous activated carbon from cotton straw |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710008199.6A CN106672965B (en) | 2017-01-05 | 2017-01-05 | A method for preparing high specific surface hierarchically porous activated carbon from cotton straw |
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| Publication Number | Publication Date |
|---|---|
| CN106672965A CN106672965A (en) | 2017-05-17 |
| CN106672965B true CN106672965B (en) | 2019-01-22 |
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| CN109192540B (en) * | 2018-09-18 | 2021-07-27 | 中联西北工程设计研究院有限公司 | A kind of biomass carbonization product and manganese dioxide composite electrode material and preparation method thereof |
| CN111617737A (en) * | 2019-02-27 | 2020-09-04 | 河北工业大学 | A kind of graded porous carbon material and its preparation method and application |
| CN110422837A (en) * | 2019-08-02 | 2019-11-08 | 新疆弘瑞达纤维有限公司 | A method of fluorescent carbon point is prepared using biomass material |
| CN114804098B (en) * | 2022-03-18 | 2024-02-06 | 广东省农业科学院作物研究所 | Method for preparing porous activated carbon from waste tobacco straw |
| CN115784227A (en) * | 2022-11-07 | 2023-03-14 | 河南农业大学 | Method for preparing porous carbon from agricultural and forestry biomass |
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