CN106809832B - A kind of preprocess method preparing high-ratio surface multistage mesoporous activated carbon with cotton stalk - Google Patents
A kind of preprocess method preparing high-ratio surface multistage mesoporous activated carbon with cotton stalk Download PDFInfo
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- CN106809832B CN106809832B CN201710007476.1A CN201710007476A CN106809832B CN 106809832 B CN106809832 B CN 106809832B CN 201710007476 A CN201710007476 A CN 201710007476A CN 106809832 B CN106809832 B CN 106809832B
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- 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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Abstract
The invention belongs to active carbon field, specifically a kind of preprocess method that high-ratio surface multistage mesoporous activated carbon is prepared with cotton stalk.Including: (1) is crushed to particle, screening removal of impurities for cotton stalk；(2) material is rinsed, is then dehydrated；(3) by dump leaching after material addition weak caustic solution, machinery rubbing to its sub-wire squeezes out surplus liquid, again dump leaching；(4) material is placed in closed pressure vessel, is passed through high steam and keeps 1.0~2.5MPa air pressure, 5~20min, material and steam and pressure release are discharged in 60~75ms to normal pressure, material is produced；(5) it is rinsed, is dehydrated with deionized water；(6) uniformly drying.The present invention can efficiently use and expand the natural fine cellular structure of cotton stalk; increase specific surface area; high-specific surface area multistage mesoporous activated carbon process for subsequent preparation low cost provides quality raw materials; keep the activator level of subsequent handling low; activating process is simple; sustainability is strong, is suitble to large-scale production.
Description
Technical field
It is especially 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 preprocess method of charcoal.
Background technique
Absorbent charcoal material is the new material system to grow up in 20th century, as nonmetallic system porous carbon materials,
Distinguishing feature is that have regularly arranged, adjustable, highly developed cellular structure, thus its specific surface area is very high, and absorption is held
Measure it is very big, bulky molecular catalysis, adsorb with separate, the various fields such as nanomaterial assembly and biochemistry have and widely answer
With, at present fuel cell, electro-catalysis, hydrogen storage and photonic crystal, electric double layer capacitance, in terms of also show it is good
Good application prospect.But its high manufacturing cost greatly limits its development and application, finds cheap original abundant
Material and improvement preparation method are the current effective measures for reducing active carbon preparation cost.
The property of the specific surface area of absorbent charcoal material, pore structure and surface functional group by activating process in addition to being influenced, charcoal
One of an important factor for property of presoma is also influence Properties of Activated Carbon, absorbent charcoal material hole prepared by different presomas
Diameter distribution and surface functional group property are also different.Therefore, appropriate raw material are selected and use good pretreatment side
Method is extremely important to production high grade activated carbon.
The persursor material of active carbon is prepared, can be divided mainly into two major class: plant and mineral substance at present.Plant has wood
Material, coconut husk, walnut shell, almond etc..Using the natural structure of plant raw material, it can be made that micropore is flourishing, specific surface area is very high
Active carbon, and mechanical strength with higher.Mineral substance raw material have coal, petroleum coke, synthetic resin etc., in these former materials
In material, coal resources are the most abundant, but coal texture and component characteristic directly affect the performance of active carbon, and ash content height is simultaneously
And it is difficult to generate flourishing micropore.
Using the especially various biomass straws of renewable biomass as precursor preparation active carbon carbon material, 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 high-performance with unique texture using biomass persursor material
Active carbon material causes many researchs both domestic and external and concern.
Biomass persursor material is mainly stalk, shell and branches and leaves of plant etc..Mainly by cellulose, hemicellulose
Be grouped as with three great achievement of lignin, but this in three composition, structure and distribution of the component in plant can because plant type, produce
Ground and growth period etc. it is different and different.In addition, also containing organic compounds such as a small amount of pectin, fat, waxes in plant cotton stalk
Needed for object and plant growth, and various metallic elements of bring etc. in raw material transport and production process.This makes cotton straw
The chemical component and structure of stalk are extremely complex, and there are great differences for the pretreatment for also resulting in different cotton stalks and Land use systems,
It is even completely different.
Due to the distinctive complicated and stable structure of various cotton stalks, pretreatment processing method also respectively has feature, not to the utmost
It is identical.
Biomass active Carbon Materials are mainly biological straw, such as cotton stalk, straw, corn stover, as presoma
Material is generally required when preparing active carbon and is pre-processed, and current preprocess method is usually that biological straw is crushed to powder
, distinctive natural fine cellular structure does not pass through process means and is made full use of, therefore existing biomass
Active carbon technology of preparing solves only the Utilizing question of cotton stalk, in the institutional framework for not making full use of biological material
Microscopic characteristics expand biomass microcellular structure and micro pore surface area.
It is anxious to make full use of cotton stalk cheap and abundant to prepare high performance active carbon as activated carbon precursor material
A kind of preprocess method that high-ratio surface multistage mesoporous activated carbon is prepared with cotton stalk need to be developed.
Summary of the invention
The present invention provides a kind of preprocess methods that high-ratio surface multistage mesoporous activated carbon is prepared with cotton stalk, can be quick
The microcellular structure for extending biological material, reduces the activation temperature of subsequent handling and reduces activator level, and preparing has height
The absorbent charcoal material of the hierarchical porous structure of specific surface area.
In general, biological material is made of the plant tissue that various plant cells are constituted, mainly there are xylem, bast
Deng being mainly made of lignin abundant, cellulose and hemicellulose.Lignin is hard, usually constitutes the bone of plant
Frame, cellulose and hemicellulose constitute the cell wall of plant, and plant is interior in macromolecule under certain temperature and pressure
Portion's connecting key interrupts, and is cracked into small molecule, and cell wall is partially got through, and the natural microstructure of cell wall is in charing, activation work
It is able to retain and be converted into the multistage microcellular structure of gained active carbon in sequence.
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.
The technical scheme is that
A kind of preprocess method preparing high-ratio surface multistage mesoporous activated carbon with cotton stalk, specific steps are as follows:
(1) prepared by raw material: by cotton stalk, the cladding and core obtained after core-skin separates and removes peach, leaf, withe
Material crushes obtain the cladding and core material of partial size 5mm~15mm respectively, or directly crushes without core-skin separation, obtains partial size 5
The non-separating material of~15mm；Then the qualified material of 5~15mm of partial size is screened out, screening removes dust, impurity；
(2) clear water rinses: material being rinsed with water, is then dehydrated；
(3) rub dump leaching: by dump leaching after material addition weak caustic solution, machinery rubbing to its sub-wire squeezes out surplus liquid, then
Secondary dump leaching；
(4) Hong quick-fried processing: material is placed in closed pressure vessel, is passed through high steam, keeps 1.0~2.5MPa air pressure
5~20 minutes, material and steam and pressure release are discharged in 60~75ms to normal pressure, material is produced；
(5) deionized water rinses: material being rinsed with deionized water, is dehydrated；
(6) it dries: material is uniformly dried.
The invention also includes optimization or/and improvement have:
One of preferred embodiment: the unqualified material return step (1) in the step (1) by size greater than 15mm is after continued powder
Broken, the unqualified material by size less than 5mm is discarded；
The two of preferred embodiment: weak caustic solution described in the step (3) is the NaOH solution of pH8~9.5；
The three of preferred embodiment: 1.5~2.0MPa air pressure is kept in the step (4).
Further preferred embodiment has:
The four of preferred embodiment: by the NaOH solution of pH8~9.5 of the material addition 1~5% after swollen in the step (3)
Dump leaching 24~48 hours afterwards, machinery rubbing is to its sub-wire, dump leaching 24~48 hours again after dehydration；
The five of preferred embodiment: being kept for 1.8MPa air pressure 10 minutes in the step (4), with the time release material of 60ms and
Steam and pressure release are to normal pressure；
The six of preferred embodiment: the dump leaching time is 30~42 hours again described in the step (3).
The beneficial effect for implementing technical solution of the present invention is:
It is micro- that the natural fine cellular structure that the present invention can efficiently use cotton stalk is expanded into more flourishing biomass
Pore structure reduces production cost so that the preparation of subsequent active carbon finished products can obtain bigger specific surface area.It is examined through test
It surveys, there is bigger specific surface area using the processed activated carbon from activated sludge persursor material of technical solution of the present invention, more send out
The distribution of pores reached, activator level substantially reduce, and activating process is simple, and sustainability is strong, are more suitable for large-scale production.
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
Take 1.0t cotton stalk as activated carbon precursor material, pre-treatment step are as follows:
(1) prepared by raw material: the 0.3t cladding that cotton stalk is obtained after core-skin separates and removes peach, leaf, withe
It is crushed to 5~15mm of partial size, screening removes dust, impurity, and the cladding return by partial size greater than 15mm continues to crush, and size is small
It is discarded in the unqualified material of 5mm；
(2) clear water rinses: material being rinsed, is dehydrated to water content about；
(3) it rubs dump leaching: mechanical mass is rubbed to dump leaching 24 after the NaOH weak caustic solution for the pH8 that 5% is added to its sub-wire
Hour, surplus liquid is squeezed out, again dump leaching 42 hours；
(4) Hong quick-fried processing: material is placed in closed pressure vessel, is passed through high steam, keeps 1.0~1.5MPa air pressure
8~15 minutes, material and steam and pressure release are discharged to normal pressure with the time of 75ms, material is produced；
(5) deionized water rinses: material being rinsed with deionized water, is dehydrated；
(6) it dries: material is uniformly dried.
The present embodiment obtains 0.3t pretreatment cotton stalk.
The ratio that potassium hydroxide, potassium carbonate and the present embodiment pretreatment cotton stalk are 1:2:7.5 in mass ratio is mixed molten
Yu Shui is stirred evenly, which is standing and soaking for 24 hours, makes to pre-process cotton stalk and aqueous slkali is sufficiently impregnated dissolving；It obtains
Mixture is placed in 100 DEG C of baking ovens dry 12h, removes the moisture in mixture, and obtained product is ground into powder；This is consolidated
Body powder is placed in tube furnace, under nitrogen protection, is warming up to 100 DEG C with the rate of 10 DEG C/min, is kept 1h, then with the rate
300 DEG C are warming up to, 1 DEG C/min is set by rate at this time and is warming up to 400 DEG C, continues to be warming up to 800 with the rate of 10 DEG C/min
DEG C, and 2h is kept, it is cooled to room temperature under nitrogen atmosphere, obtains activation products；Obtained activation products first use the HCl of 1mol/L clear
It washes, neutralize, then cleaned with deionized water to pH=7~8, dry 12h, obtains high-specific surface area multi-stage porous in 100 DEG C of baking oven
Active carbon 0.08t.
The absorbent charcoal material that embodiment 1 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
Take 1.0t cotton stalk as activated carbon precursor material, pre-treatment step are as follows:
(1) prepared by raw material: by cotton stalk, 0.5t core material powder is obtained after core-skin separates and removes peach, leaf, withe
It is broken to partial size 5mm~15mm, screening removes dust, impurity, and the cladding return by partial size greater than 15mm continues to crush, and size is small
It is discarded in the unqualified material of 5mm；
(2) clear water rinses: material being rinsed with water, is then dehydrated；
(3) it rubs dump leaching: material being added after the NaOH weak caustic solution of 3% pH9 dump leaching 48 hours, machinery is rubbed to it
Sub-wire squeezes out surplus liquid, again dump leaching 30 hours；
(4) Hong quick-fried processing: material is placed in closed pressure vessel, is passed through high steam, keeps 2.0~2.5MPa air pressure
5~10 minutes, material and steam and pressure release are discharged in 60ms to normal pressure, material is produced；
(5) deionized water rinses: material being rinsed with deionized water, is dehydrated；
(6) it dries: material is uniformly dried.
The present embodiment obtains 0.35t pretreatment cotton stalk.
The ratio that potassium hydroxide, potassium carbonate and the present embodiment pretreatment cotton stalk are 1:2:7.5 in mass ratio is mixed molten
Yu Shui is stirred evenly, which is standing and soaking for 24 hours, makes to pre-process cotton stalk and aqueous slkali is sufficiently impregnated dissolving；It obtains
Mixture is placed in 100 DEG C of baking ovens dry 12h, removes the moisture in mixture, and obtained product is ground into powder；This is consolidated
Body powder is placed in tube furnace, under nitrogen protection, is warming up to 100 DEG C with the rate of 10 DEG C/min, is kept 1h, then with the rate
300 DEG C are warming up to, 1 DEG C/min is set by rate at this time and is warming up to 400 DEG C, continues to be warming up to 800 with the rate of 10 DEG C/min
DEG C, and 2h is kept, it is cooled to room temperature under nitrogen atmosphere, obtains activation products；Obtained activation products first use the HCl of 1mol/L clear
It washes, neutralize, then cleaned with deionized water to pH=7~8, dry 12h, obtains high-specific surface area multi-stage porous in 100 DEG C of baking oven
Active carbon 0.1t.
The absorbent charcoal material that embodiment 2 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 takes 1.0t cotton stalk as activated carbon precursor material, pre-treatment step are as follows:
(1) prepared by raw material: taking a certain amount of cotton stalk, separates without core-skin, be directly crushed to 5~15mm of partial size, by grain
Diameter is greater than 15mm, and chalk dust removing, impurity are removed in screening；
(2) clear water rinses: material being rinsed, is dehydrated to water content about；
(3) it rubs dump leaching: material being added after the NaOH weak caustic solution of 1% pH9.5 dump leaching 48 hours, machinery rubbing is extremely
Its sub-wire squeezes out surplus liquid, again dump leaching 42 hours；
(4) Hong quick-fried processing: material is placed in closed pressure vessel, is passed through high steam, and 1.0MPa air pressure 5 is kept to divide
Clock discharges material and steam and pressure release to normal pressure with the time of 60ms, and material is produced；
(5) deionized water rinses: material being rinsed with deionized water, is dehydrated；
(6) it dries: material is uniformly dried.
The present embodiment obtains 0.7t pretreatment cotton stalk.
The ratio that potassium hydroxide, potassium carbonate and the present embodiment pretreatment cotton stalk are 1:2:7.5 in mass ratio is mixed molten
Yu Shui is stirred evenly, which is standing and soaking for 24 hours, makes to pre-process cotton stalk and aqueous slkali is sufficiently impregnated dissolving；It obtains
Mixture is placed in 100 DEG C of baking ovens dry 12h, removes the moisture in mixture, and obtained product is ground into powder；This is consolidated
Body powder is placed in tube furnace, under nitrogen protection, is warming up to 100 DEG C with the rate of 10 DEG C/min, is kept 1h, then with the rate
300 DEG C are warming up to, 1 DEG C/min is set by rate at this time and is warming up to 400 DEG C, continues to be warming up to 800 with the rate of 10 DEG C/min
DEG C, and 2h is kept, it is cooled to room temperature under nitrogen atmosphere, obtains activation products；Obtained activation products first use the HCl of 1mol/L clear
It washes, neutralize, then cleaned with deionized water to pH=7~8, dry 12h, obtains high-specific surface area multi-stage porous in 100 DEG C of baking oven
Active carbon 0.2t.
The absorbent charcoal material that embodiment 3 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)
1. a kind of preprocess method for preparing high-ratio surface multistage mesoporous activated carbon with cotton stalk, which is characterized in that including walking as follows
It is rapid:
(1) prepared by raw material: by cotton stalk, the cladding and core material point that are obtained after core-skin separates and removes peach, leaf, withe
The cladding and core material of 5~15mm of partial size Fen Sui not be obtained, or is directly crushed without core-skin separation, 5~15mm of partial size is obtained
Non- separating material；Then the qualified material of 5~15mm of partial size is screened out, screening removes dust, impurity；
(2) clear water rinses: material being rinsed with water, is then dehydrated；
(3) rub dump leaching: by dump leaching after material addition weak caustic solution, machinery rubbing to its sub-wire squeezes out surplus liquid, again heap
Leaching；
(4) Hong quick-fried processing: material being placed in closed pressure vessel, is passed through high steam, keep 1.0~2.5MPa air pressure 5~
20 minutes, material and steam and pressure release are discharged in 60~75ms to normal pressure, material is produced；
(5) deionized water rinses: material being rinsed with deionized water, is dehydrated；
(6) it dries: material is uniformly dried.
2. a kind of preprocess method that high-ratio surface multistage mesoporous activated carbon is prepared with cotton stalk according to claim 1,
It is characterized in that, the unqualified material return step (1) in the step (1) by size greater than 15mm continues to crush, and size is small
It is discarded in the unqualified material of 5mm.
3. a kind of preprocess method that high-ratio surface multistage mesoporous activated carbon is prepared with cotton stalk according to claim 1,
It is characterized in that, it is mechanical by dump leaching 24~48 hours after the weak caustic solution of the material addition 1~5% after swollen in the step (3)
Rubbing is to its sub-wire, dump leaching 24~48 hours again after dehydration.
4. a kind of preprocess method that high-ratio surface multistage mesoporous activated carbon is prepared with cotton stalk according to claim 1,
It is characterized in that, 1.5~2.0MPa air pressure is kept described in the step (4).
5. a kind of preprocess method that high-ratio surface multistage mesoporous activated carbon is prepared with cotton stalk according to claim 1,
It is characterized in that, is kept for 1.8MPa air pressure 10 minutes in the step (4), material and steam and pressure release are discharged extremely with the time of 60ms
Normal pressure.
6. a kind of preprocess method that high-ratio surface multistage mesoporous activated carbon is prepared with cotton stalk according to claim 1,
It is characterized in that, weak caustic solution is the NaOH solution of pH8~9.5 in the step (3).
7. a kind of preprocess method that high-ratio surface multistage mesoporous activated carbon is prepared with cotton stalk according to claim 3,
It is characterized in that, the dump leaching time is 30~42 hours again in the step (3).
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| CN101134970A (en) * | 2007-07-23 | 2008-03-05 | 吉林省轻工业设计研究院 | Pre-treating method for producing ethanol by corn straw enzymatical hydrolysis |
| CN102085680A (en) * | 2010-11-26 | 2011-06-08 | 江南大学 | Preparation method of crop straw fiber ecological composite material |
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| CN101134970A (en) * | 2007-07-23 | 2008-03-05 | 吉林省轻工业设计研究院 | Pre-treating method for producing ethanol by corn straw enzymatical hydrolysis |
| CN102085680A (en) * | 2010-11-26 | 2011-06-08 | 江南大学 | Preparation method of crop straw fiber ecological composite material |
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