CN106744939A - The method that leaf is converted to activated carbon using plasma combination activator - Google Patents
The method that leaf is converted to activated carbon using plasma combination activator Download PDFInfo
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- CN106744939A CN106744939A CN201710065557.7A CN201710065557A CN106744939A CN 106744939 A CN106744939 A CN 106744939A CN 201710065557 A CN201710065557 A CN 201710065557A CN 106744939 A CN106744939 A CN 106744939A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/14—Pore volume
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
Abstract
The invention discloses a kind of method that leaf is converted to utilization plasma combination activator activated carbon, it is related to plant manufacture field, including pretreatment, activator dipping, dries carbonization treatment, cleaning treatment and high temperature thermal source as carbonization, method with reference to chemical activating agent activation method last again high temperature surface treatment so that leaf to be efficiently converted to high performance active carbon of the step by the use of plasma etc. surface activation process.
Description
Technical field
It is more particularly to a kind of to be converted to leaf using plasma combination activator the present invention relates to plant manufacture field
The method of activated carbon.
Background technology
The fallen leaves of plant itself are that phosphorus content is very high, and the production material for being highly suitable as activated carbon is used, and is showed
Have in technology by phyteral Raw material processing for activated carbon be generally all using separate and high temperature cabonization by the way of, such as Publication No.
CN101955181A, the time of disclosure is on January 26th, 2011, entitled " to utilize larchwood fast pyrogenation accessory substance charcoal system
The Chinese invention patent document of the method for standby activated carbon ", discloses a kind of using larchwood fast pyrogenation accessory substance charcoal system
The method of standby activated carbon, carries out fast pyrogenation to larchwood first, obtains pyrolytic carbon and pyrolysis gas;Above-mentioned pyrolysis gas are entered
Row condensation, obtains pyrolysis oil and non-condensable gases, not condensable gases is burnt in atmosphere, obtains activated gas;With work
Change gas as activator, pyrolytic carbon is activated, be cooled to room temperature, obtain activated carbon, make the height produced in activation process
Warm circulation of tail gas is used.The inventive method, need not add external heat source and activator, thermal decomposition product synthesis in activation process
Utilization rate is high, and environmental pollution is small;The process is simple of activated carbon is prepared, energy utilization rate is high, realize recycle heat utilization, saved
The energy, the charcoal absorption performance for obtaining is good, and indices meet national standard, can be widely applied to Gas Phase Adsorption and change
The decolouring of chemical product;But adopt in this way processing water content is higher or more difficult plant defoliation being carbonized of material itself
When, it is general only with activated carbon its Performance comparision made by general separation and high temperature cabonization mode out, and finished product
Rate is relatively low, and adsorptivity etc. is all bad.
The content of the invention
It is an object of the invention to provide a kind of high temperature by the use of plasma as the thermal source of carbonization, with reference to chemical activation
Method of the last surface treatment of high temperature again of agent activation method so that leaf to be efficiently converted to high performance active carbon.
The purpose of the present invention is achieved through the following technical solutions:
The method that leaf is converted to activated carbon using plasma combination activator, it is characterised in that comprise the following steps
Pretreatment:Leaf is obtained the pellet of 10-60 mesh specification, Han Shui Liang≤15% after screening, drying, grind;
Activator impregnates:Pellet immersion is included into potassium hydroxide(KOH), zinc chloride(ZnCl2), absolute ethyl alcohol and deionization
Carry out activation process in the activator of water, and the amount of the activator for using and the pellet amount according to 2.5-3.5:1 is matched somebody with somebody
Than dipping Shi Jian≤2 hour;
Dry carbonization treatment:The pellet impregnated by activator is placed in inert gas environment, introducing plasma stream is carried out
Heat up and dry and be carbonized, temperature is increased to 350 ± 50 DEG C simultaneously by the heating curve according to 4-6 DEG C/min in inert gas environment
Keeping temperature 45-60 minutes, pellet is carbonized;
Cleaning treatment:By by the pellet of carbon activation process analysis pure hydrochloric acid(HCl)Stirring and washing, then cleaned with deionized water
Vacuum dehydration dried process is carried out after to neutrality, drying temperature is maintained at 105 ± 5 DEG C, and vacuum is maintained at 90-100KPa, directly
To Han Shui Liang≤5% of the pellet;
Surface activation process:During cleaning treatment, plasma stream is introduced back into when Han Shui Liang≤5% of the pellet
The surface of pellet is modified and activated, and the process of surface activation process needs to keep vacuum environment, activation process time
5-10 seconds.
Potassium hydroxide in the activator(KOH), zinc chloride(ZnCl2)With Zhan Bi≤60% of absolute ethyl alcohol, and hydroxide
Potassium(KOH)Zhan Bi≤40%.
The inert gas environment refers to full of helium(He), neon(Ne), argon(Ar), krypton(Kr), xenon(Xe)Gas or its two
Item or the gaseous environment of multinomial combination.
In the dry carbonization processing procedure, the inert gas is lasting input to keep inert gas environment and adjustment
Temperature, the input flow rate of the inert gas is 50SLPM-200SLPM.
Plasma stream is introduced during the surface activation process temperature is increased to 700-800 DEG C.
Beneficial effects of the present invention are as follows:
First, the method that leaf is converted to a kind of utilization plasma combination activator that the present invention is provided activated carbon, including it is pre-
Treatment, activator dipping, drying first will tree in the step of carbonization treatment, cleaning treatment and surface activation process step, pretreatment
Leaf raw material filters out excellent raw material, is ground again after drying and dehydrating, can so ensure the quality of raw material, after drying and dehydrating also more
It is easy to specification of the milled processed required for following process, and dry pellet has the low advantage of water content;Activator impregnates
In step, using inclusion potassium hydroxide(KOH), zinc chloride(ZnCl2), absolute ethyl alcohol and deionized water activator, biomass
Raw material meets the carbonization of alkali activator more dehydration, uses chlorate(Zinc chloride)As the addition of deionized water and alkali lye be in order to
The material in alkali lye and material is hindered to cross fast response generation chlorate and influence alkali lye to act on the dehydration carbonization-activation of material, it is living
The amount of the amount of agent and the pellet is according to 2.5-3.5:1 is matched, during dipping between≤be enough within 2 hours make activation carburizing reagent
Fully thoroughly;Dry carbonization process step in, the pellet impregnated by activator is placed in inert gas environment, introduce etc. from
Daughter stream heat up and dries and be carbonized, and plasma stream can produce high temperature, facilitate accuracy controlling, and with one
Fixed electrology characteristic, can effectively improve the carbonizing degree of material, according to 4-6 in inert gas environment in carbonisation
DEG C/temperature is increased to 350 ± 50 DEG C and keeping temperature 45-60 minutes and pellet is carbonized by the heating curve of min, gradually heating up has
Help to avoid unexpected high temperature cause surface of material at a high speed carbonization and inside cannot obtain the influence carbonisation that effectively heats up, it is final to protect
Hold and keep certain hour to ensure that material is fully carbonized in predetermined carburizing temperature, especially for greens, may be used also
To destroy its chloroplast structure;In cleaning treatment step, by by the pellet of carbon activation process analysis pure hydrochloric acid(HCl)Stirring
Clean and remained with neutralizing the alkali that leaves when activator impregnates, then cleaned to neutrality with deionized water and carry out at vacuum dehydration drying
Reason, material oxyphie even combustion effects product quality when vacuum state avoids drying, drying temperature is maintained at 105 ± 5 DEG C of guarantees
The evaporation drying of moisture, vacuum is maintained at 90-100KPa, until Han Shui Liang≤5% of the pellet, can now be considered as thing
Material has met or exceeded the standard of general activated carbon;In surface activation process step, when Han Shui Liang≤5% of the pellet
Shi Zaici introduces plasma stream in vacuum environment and the surface of pellet is modified and activated, and surface activation process mistake
Journey needs to keep vacuum environment, 5-10 seconds activation process time, makes surface of material rapid using the ultra-high temperature of plasma stream
It is modified, strengthen the adsorption ability in its unit volume.
2nd, the method that leaf is converted to a kind of utilization plasma combination activator that the present invention is provided activated carbon, it is living
Potassium hydroxide in agent(KOH), zinc chloride(ZnCl2)With Zhan Bi≤60% of absolute ethyl alcohol, and potassium hydroxide(KOH)Accounting
≤ 40%, it is such to match the base strength that ensure that activator, contribute to the lifting of activation effect.
3rd, the method that leaf is converted to a kind of utilization plasma combination activator that the present invention is provided activated carbon, lazy
Property gaseous environment refers to full of helium(He), neon(Ne), argon(Ar), krypton(Kr), xenon(Xe)Gas or its two or multinomial combination
Gaseous environment, selectable range is wide, and condition can also be met in the form of combination, and the difficulty that reduce further production will
Ask.
4th, the method that leaf is converted to a kind of utilization plasma combination activator that the present invention is provided activated carbon, does
During dry carbonization treatment, inert gas is persistently input into the input flow rate of 50SLPM-200SLPM, is persistently input into inertia
Gas can ensure that barrier decline will not be caused because of the change such as temperature, pressure, air-flow in reaction range.
5th, the method that leaf is converted to a kind of utilization plasma combination activator that the present invention is provided activated carbon, table
Plasma stream is introduced in the activated process of face temperature is increased to 700-800 DEG C, most plants are met at a temperature of this
The modified temperature requirement of the surface carbonation of leaf material, while it is compound anti-also because of excessive temperature other materials will not to be caused to produce
Should.
Specific embodiment
The technical scheme of realizing the object of the invention is further illustrated below by way of several specific embodiments, it is necessary to explanation
It is that technical scheme is including but not limited to following examples.
Embodiment 1
The method that leaf is converted to activated carbon using plasma combination activator, it is characterised in that comprise the following steps
Pretreatment:Leaf is obtained the pellet of 10-60 mesh specification, Han Shui Liang≤15% after screening, drying, grind;
Activator impregnates:Pellet immersion is included into potassium hydroxide(KOH), zinc chloride(ZnCl2), absolute ethyl alcohol and deionization
Carry out activation process in the activator of water, and the amount of the activator for using and the pellet amount according to 2.5-3.5:1 is matched somebody with somebody
Than dipping Shi Jian≤2 hour;
Dry carbonization treatment:The pellet impregnated by activator is placed in inert gas environment, introducing plasma stream is carried out
Heat up and dry and be carbonized, temperature is increased to 350 ± 50 DEG C simultaneously by the heating curve according to 4-6 DEG C/min in inert gas environment
Keeping temperature 45-60 minutes, pellet is carbonized;
Cleaning treatment:By by the pellet of carbon activation process analysis pure hydrochloric acid(HCl)Stirring and washing, then cleaned with deionized water
Vacuum dehydration dried process is carried out after to neutrality, drying temperature is maintained at 105 ± 5 DEG C, and vacuum is maintained at 90-100KPa, directly
To Han Shui Liang≤5% of the pellet;
Surface activation process:During cleaning treatment, plasma stream is introduced back into when Han Shui Liang≤5% of the pellet
The surface of pellet is modified and activated, and the process of surface activation process needs to keep vacuum environment, activation process time
5-10 seconds.
This is a kind of most basic embodiment of the invention.Including pretreatment, activator dipping, dry carbonization treatment, clear
Wash in the step for the treatment of and surface activation process step, pretreatment and leaf raw material screening is first gone out into excellent raw material, drying and dehydrating
Grind again afterwards, can so ensure the quality of raw material, milled processed of being also more convenient for after drying and dehydrating is required for following process
Specification, and dry pellet has the low advantage of water content;In activator impregnation steps, using inclusion potassium hydroxide(KOH), chlorine
Change zinc(ZnCl2), absolute ethyl alcohol and deionized water activator, biomass material meets the carbonization of alkali activator more dehydration, makes
Use chlorate(Zinc chloride)It is to hinder alkali lye to cross fast response with the material in material as the addition of deionized water and alkali lye
Generation chlorate and influence alkali lye to act on the dehydration carbonization-activation of material, the amount of the amount of activator and the pellet is according to 2.5-
3.5:1 is matched, during dipping between≤be enough within 2 hours make activation carburizing reagent fully thorough;Dry and be carbonized in process step, will
By activator impregnate pellet be placed in inert gas environment, introduce plasma stream carry out heat up dry and be carbonized, wait from
Daughter stream can produce high temperature, facilitate accuracy controlling, and with certain electrology characteristic, can be with carbonisation
The carbonizing degree of material is effectively improved, temperature is increased to 350 according to the heating curve of 4-6 DEG C/min in inert gas environment
± 50 DEG C are simultaneously carbonized pellet in keeping temperature 45-60 minutes, and gradually intensification helps avoid unexpected high temperature causes surface of material high
Speed carbonization and inside cannot obtain the influence carbonisation that effectively heats up, be eventually held in predetermined carburizing temperature and keep a timing
Between to ensure that material is fully carbonized, especially for greens, its chloroplast structure can also be destroyed;Cleaning treatment step
In, by by the pellet of carbon activation process analysis pure hydrochloric acid(HCl)The alkali left when stirring and washing is to neutralize activator dipping
Residual, then cleaned to neutrality with deionized water and carry out vacuum dehydration dried process, material oxyphie when vacuum state avoids drying
Even combustion effects product quality, drying temperature is maintained at 105 ± 5 DEG C of evaporation dryings of guarantee moisture, and vacuum is maintained at 90-
100KPa, until Han Shui Liang≤5% of the pellet, can now be considered as material and meet or exceed general activated carbon
Standard;In surface activation process step, plasma is introduced in vacuum environment again when Han Shui Liang≤5% of the pellet
Flow and the surface of pellet is modified and activated, and the process of surface activation process needs to keep vacuum environment, during activation process
Between 5-10 seconds, make surface of material rapid progresses using the ultra-high temperature of plasma stream, strengthen surface in its unit volume and inhale
Attached ability.It is referenced below and employs the activated carbon surface hole data sample test result tables of data that this method is produced(Table one)
To further illustrate the advantage of technical solution of the present invention, wherein sample 1 and 2 is control group, is the knot being carbonized using existing method
Really, and sample 3 and 4 are the carbonization results manufactured using technical scheme provided by the present invention.
The check experiment activated carbon surface hole data sample test result of table one
Embodiment 2
The method that leaf is converted to activated carbon using plasma combination activator, it is characterised in that comprise the following steps
Pretreatment:Leaf is obtained the pellet of 10-60 mesh specification, Han Shui Liang≤15% after screening, drying, grind;
Activator impregnates:Pellet immersion is included into potassium hydroxide(KOH), zinc chloride(ZnCl2), absolute ethyl alcohol and deionization
Carry out activation process in the activator of water, and the amount of the activator for using and the pellet amount according to 2.5-3.5:1 is matched somebody with somebody
Than dipping Shi Jian≤2 hour;
Dry carbonization treatment:The pellet impregnated by activator is placed in inert gas environment, introducing plasma stream is carried out
Heat up and dry and be carbonized, temperature is increased to 350 ± 50 DEG C simultaneously by the heating curve according to 4-6 DEG C/min in inert gas environment
Keeping temperature 45-60 minutes, pellet is carbonized;
Cleaning treatment:By by the pellet of carbon activation process analysis pure hydrochloric acid(HCl)Stirring and washing, then cleaned with deionized water
Vacuum dehydration dried process is carried out after to neutrality, drying temperature is maintained at 105 ± 5 DEG C, and vacuum is maintained at 90-100KPa, directly
To Han Shui Liang≤5% of the pellet;
Surface activation process:During cleaning treatment, plasma stream is introduced back into when Han Shui Liang≤5% of the pellet
The surface of pellet is modified and activated, and the process of surface activation process needs to keep vacuum environment, activation process time
5-10 seconds.
Potassium hydroxide in the activator(KOH), zinc chloride(ZnCl2)With Zhan Bi≤60% of absolute ethyl alcohol, and hydroxide
Potassium(KOH)Zhan Bi≤40%.
This is a kind of preferred the present embodiment of the invention.Including pretreatment, activator dipping, dry carbonization treatment,
Leaf raw material screening is first gone out into excellent raw material in the step of cleaning treatment and surface activation process step, pretreatment, is dried de-
Ground again after water, can so ensure the quality of raw material, milled processed of being also more convenient for after drying and dehydrating is required for following process
Specification, and dry pellet has the low advantage of water content;In activator impregnation steps, using inclusion potassium hydroxide(KOH)、
Zinc chloride(ZnCl2), absolute ethyl alcohol and deionized water activator, biomass material meets the carbonization of alkali activator more dehydration,
Use chlorate(Zinc chloride)It is in order to the material in hindering alkali lye and material is too fast anti-as the addition of deionized water and alkali lye
Chlorate should be generated and influence alkali lye to act on the dehydration carbonization-activation of material, the amount of the amount of activator and the pellet according to
2.5-3.5:1 is matched, during dipping between≤be enough within 2 hours make activation carburizing reagent fully thorough;Dry carbonization process step
In, the pellet impregnated by activator is placed in inert gas environment, introducing plasma stream carries out heating up dry and is carbonized,
Plasma stream can produce high temperature, facilitate accuracy controlling, and with certain electrology characteristic, in carbonisation
The carbonizing degree of material can be effectively improved, temperature is raised according to the heating curve of 4-6 DEG C/min in inert gas environment
Simultaneously pellet was carbonized in keeping temperature 45-60 minutes to 350 ± 50 DEG C, gradually intensification helps avoid unexpected high temperature causes material table
Face at a high speed carbonization and inside cannot obtain the influence carbonisation that effectively heats up, be eventually held in predetermined carburizing temperature and keep one
Fix time to ensure that material is fully carbonized, especially for greens, its chloroplast structure can also be destroyed;Cleaning treatment
In step, by by the pellet of carbon activation process analysis pure hydrochloric acid(HCl)Stirring and washing is left with neutralizing when activator impregnates
Alkali residual, then cleaned to neutrality with deionized water and carry out vacuum dehydration dried process, material when vacuum state avoids drying
Oxyphie even combustion effects product quality, drying temperature is maintained at 105 ± 5 DEG C of evaporation dryings of guarantee moisture, and vacuum keeps
In 90-100KPa, until Han Shui Liang≤5% of the pellet, can now be considered as material and meet or exceed general activity
The standard of charcoal;In surface activation process step, when Han Shui Liang≤5% of the pellet again in vacuum environment introduce etc. from
Daughter stream is modified and activates to the surface of pellet, and the process of surface activation process needs to keep vacuum environment, at activation
5-10 seconds reason time, surface of material rapid progresses are made using the ultra-high temperature of plasma stream, strengthen the table in its unit volume
Face adsorption capacity.Be referenced below employ activated carbon surface hole data sample test result tables of data that this method produced with
The advantage of technical solution of the present invention is further illustrated, wherein sample 1 and 2 is control group, is the result being carbonized using existing method,
And sample 3 and 4 are the carbonization results manufactured using technical scheme provided by the present invention;Potassium hydroxide in activator
(KOH), zinc chloride(ZnCl2)With Zhan Bi≤60% of absolute ethyl alcohol, and potassium hydroxide(KOH)Zhan Bi≤40%, it is such to match somebody with somebody
Than the base strength that ensure that activator, contribute to the lifting of activation effect.
Embodiment 3
The method that leaf is converted to activated carbon using plasma combination activator, it is characterised in that comprise the following steps
Pretreatment:Leaf is obtained the pellet of 10-60 mesh specification, Han Shui Liang≤15% after screening, drying, grind;
Activator impregnates:Pellet immersion is included into potassium hydroxide(KOH), zinc chloride(ZnCl2), absolute ethyl alcohol and deionization
Carry out activation process in the activator of water, and the amount of the activator for using and the pellet amount according to 2.5-3.5:1 is matched somebody with somebody
Than dipping Shi Jian≤2 hour;
Dry carbonization treatment:The pellet impregnated by activator is placed in inert gas environment, introducing plasma stream is carried out
Heat up and dry and be carbonized, temperature is increased to 350 ± 50 DEG C simultaneously by the heating curve according to 4-6 DEG C/min in inert gas environment
Keeping temperature 45-60 minutes, pellet is carbonized;
Cleaning treatment:By by the pellet of carbon activation process analysis pure hydrochloric acid(HCl)Stirring and washing, then cleaned with deionized water
Vacuum dehydration dried process is carried out after to neutrality, drying temperature is maintained at 105 ± 5 DEG C, and vacuum is maintained at 90-100KPa, directly
To Han Shui Liang≤5% of the pellet;
Surface activation process:During cleaning treatment, plasma stream is introduced back into when Han Shui Liang≤5% of the pellet
The surface of pellet is modified and activated, and the process of surface activation process needs to keep vacuum environment, activation process time
5-10 seconds.
Potassium hydroxide in the activator(KOH), zinc chloride(ZnCl2)With Zhan Bi≤60% of absolute ethyl alcohol, and hydroxide
Potassium(KOH)Zhan Bi≤40%.
The inert gas environment refers to full of helium(He), neon(Ne), argon(Ar), krypton(Kr), xenon(Xe)Gas or its two
Item or the gaseous environment of multinomial combination.
This is a kind of preferred the present embodiment of the invention.Including pretreatment, activator dipping, dry carbonization treatment,
Leaf raw material screening is first gone out into excellent raw material in the step of cleaning treatment and surface activation process step, pretreatment, is dried de-
Ground again after water, can so ensure the quality of raw material, milled processed of being also more convenient for after drying and dehydrating is required for following process
Specification, and dry pellet has the low advantage of water content;In activator impregnation steps, using inclusion potassium hydroxide(KOH)、
Zinc chloride(ZnCl2), absolute ethyl alcohol and deionized water activator, biomass material meets the carbonization of alkali activator more dehydration,
Use chlorate(Zinc chloride)It is in order to the material in hindering alkali lye and material is too fast anti-as the addition of deionized water and alkali lye
Chlorate should be generated and influence alkali lye to act on the dehydration carbonization-activation of material, the amount of the amount of activator and the pellet according to
2.5-3.5:1 is matched, during dipping between≤be enough within 2 hours make activation carburizing reagent fully thorough;Dry carbonization process step
In, the pellet impregnated by activator is placed in inert gas environment, introducing plasma stream carries out heating up dry and is carbonized,
Plasma stream can produce high temperature, facilitate accuracy controlling, and with certain electrology characteristic, in carbonisation
The carbonizing degree of material can be effectively improved, temperature is raised according to the heating curve of 4-6 DEG C/min in inert gas environment
Simultaneously pellet was carbonized in keeping temperature 45-60 minutes to 350 ± 50 DEG C, gradually intensification helps avoid unexpected high temperature causes material table
Face at a high speed carbonization and inside cannot obtain the influence carbonisation that effectively heats up, be eventually held in predetermined carburizing temperature and keep one
Fix time to ensure that material is fully carbonized, especially for greens, its chloroplast structure can also be destroyed;Cleaning treatment
In step, by by the pellet of carbon activation process analysis pure hydrochloric acid(HCl)Stirring and washing is left with neutralizing when activator impregnates
Alkali residual, then cleaned to neutrality with deionized water and carry out vacuum dehydration dried process, material when vacuum state avoids drying
Oxyphie even combustion effects product quality, drying temperature is maintained at 105 ± 5 DEG C of evaporation dryings of guarantee moisture, and vacuum keeps
In 90-100KPa, until Han Shui Liang≤5% of the pellet, can now be considered as material and meet or exceed general activity
The standard of charcoal;In surface activation process step, when Han Shui Liang≤5% of the pellet again in vacuum environment introduce etc. from
Daughter stream is modified and activates to the surface of pellet, and the process of surface activation process needs to keep vacuum environment, at activation
5-10 seconds reason time, surface of material rapid progresses are made using the ultra-high temperature of plasma stream, strengthen the table in its unit volume
Face adsorption capacity.Be referenced below employ activated carbon surface hole data sample test result tables of data that this method produced with
The advantage of technical solution of the present invention is further illustrated, wherein sample 1 and 2 is control group, is the result being carbonized using existing method,
And sample 3 and 4 are the carbonization results manufactured using technical scheme provided by the present invention;Potassium hydroxide in activator
(KOH), zinc chloride(ZnCl2)With Zhan Bi≤60% of absolute ethyl alcohol, and potassium hydroxide(KOH)Zhan Bi≤40%, it is such to match somebody with somebody
Than the base strength that ensure that activator, contribute to the lifting of activation effect;Inert gas environment refers to full of helium(He), neon
(Ne), argon(Ar), krypton(Kr), xenon(Xe)Gas or its two or the gaseous environment of multinomial combination, selectable range are wide, using group
The form of conjunction can also meet condition, reduce further the difficulty requirement of production.
Embodiment 4
The method that leaf is converted to activated carbon using plasma combination activator, it is characterised in that comprise the following steps
Pretreatment:Leaf is obtained the pellet of 10-60 mesh specification, Han Shui Liang≤15% after screening, drying, grind;
Activator impregnates:Pellet immersion is included into potassium hydroxide(KOH), zinc chloride(ZnCl2), absolute ethyl alcohol and deionization
Carry out activation process in the activator of water, and the amount of the activator for using and the pellet amount according to 2.5-3.5:1 is matched somebody with somebody
Than dipping Shi Jian≤2 hour;
Dry carbonization treatment:The pellet impregnated by activator is placed in inert gas environment, introducing plasma stream is carried out
Heat up and dry and be carbonized, temperature is increased to 350 ± 50 DEG C simultaneously by the heating curve according to 4-6 DEG C/min in inert gas environment
Keeping temperature 45-60 minutes, pellet is carbonized;
Cleaning treatment:By by the pellet of carbon activation process analysis pure hydrochloric acid(HCl)Stirring and washing, then cleaned with deionized water
Vacuum dehydration dried process is carried out after to neutrality, drying temperature is maintained at 105 ± 5 DEG C, and vacuum is maintained at 90-100KPa, directly
To Han Shui Liang≤5% of the pellet;
Surface activation process:During cleaning treatment, plasma stream is introduced back into when Han Shui Liang≤5% of the pellet
The surface of pellet is modified and activated, and the process of surface activation process needs to keep vacuum environment, activation process time
5-10 seconds.
Potassium hydroxide in the activator(KOH), zinc chloride(ZnCl2)With Zhan Bi≤60% of absolute ethyl alcohol, and hydroxide
Potassium(KOH)Zhan Bi≤40%.
The inert gas environment refers to full of helium(He), neon(Ne), argon(Ar), krypton(Kr), xenon(Xe)Gas or its two
Item or the gaseous environment of multinomial combination.
State to dry and be carbonized in processing procedure, the inert gas is lasting input to keep inert gas environment and adjustment temperature
Degree, the input flow rate of the inert gas is 50SLPM-200SLPM.
This is a kind of preferred the present embodiment of the invention.Including pretreatment, activator dipping, dry carbonization treatment,
Leaf raw material screening is first gone out into excellent raw material in the step of cleaning treatment and surface activation process step, pretreatment, is dried de-
Ground again after water, can so ensure the quality of raw material, milled processed of being also more convenient for after drying and dehydrating is required for following process
Specification, and dry pellet has the low advantage of water content;In activator impregnation steps, using inclusion potassium hydroxide(KOH)、
Zinc chloride(ZnCl2), absolute ethyl alcohol and deionized water activator, biomass material meets the carbonization of alkali activator more dehydration,
Use chlorate(Zinc chloride)It is in order to the material in hindering alkali lye and material is too fast anti-as the addition of deionized water and alkali lye
Chlorate should be generated and influence alkali lye to act on the dehydration carbonization-activation of material, the amount of the amount of activator and the pellet according to
2.5-3.5:1 is matched, during dipping between≤be enough within 2 hours make activation carburizing reagent fully thorough;Dry carbonization process step
In, the pellet impregnated by activator is placed in inert gas environment, introducing plasma stream carries out heating up dry and is carbonized,
Plasma stream can produce high temperature, facilitate accuracy controlling, and with certain electrology characteristic, in carbonisation
The carbonizing degree of material can be effectively improved, temperature is raised according to the heating curve of 4-6 DEG C/min in inert gas environment
Simultaneously pellet was carbonized in keeping temperature 45-60 minutes to 350 ± 50 DEG C, gradually intensification helps avoid unexpected high temperature causes material table
Face at a high speed carbonization and inside cannot obtain the influence carbonisation that effectively heats up, be eventually held in predetermined carburizing temperature and keep one
Fix time to ensure that material is fully carbonized, especially for greens, its chloroplast structure can also be destroyed;Cleaning treatment
In step, by by the pellet of carbon activation process analysis pure hydrochloric acid(HCl)Stirring and washing is left with neutralizing when activator impregnates
Alkali residual, then cleaned to neutrality with deionized water and carry out vacuum dehydration dried process, material when vacuum state avoids drying
Oxyphie even combustion effects product quality, drying temperature is maintained at 105 ± 5 DEG C of evaporation dryings of guarantee moisture, and vacuum keeps
In 90-100KPa, until Han Shui Liang≤5% of the pellet, can now be considered as material and meet or exceed general activity
The standard of charcoal;In surface activation process step, when Han Shui Liang≤5% of the pellet again in vacuum environment introduce etc. from
Daughter stream is modified and activates to the surface of pellet, and the process of surface activation process needs to keep vacuum environment, at activation
5-10 seconds reason time, surface of material rapid progresses are made using the ultra-high temperature of plasma stream, strengthen the table in its unit volume
Face adsorption capacity.Be referenced below employ activated carbon surface hole data sample test result tables of data that this method produced with
The advantage of technical solution of the present invention is further illustrated, wherein sample 1 and 2 is control group, is the result being carbonized using existing method,
And sample 3 and 4 are the carbonization results manufactured using technical scheme provided by the present invention;Potassium hydroxide in activator
(KOH), zinc chloride(ZnCl2)With Zhan Bi≤60% of absolute ethyl alcohol, and potassium hydroxide(KOH)Zhan Bi≤40%, it is such to match somebody with somebody
Than the base strength that ensure that activator, contribute to the lifting of activation effect;Inert gas environment refers to full of helium(He), neon
(Ne), argon(Ar), krypton(Kr), xenon(Xe)Gas or its two or the gaseous environment of multinomial combination, selectable range are wide, using group
The form of conjunction can also meet condition, reduce further the difficulty requirement of production;Dry and be carbonized in processing procedure, inert gas
It is persistently to be input into the input flow rate of 50SLPM-200SLPM, being persistently input into will not during inert gas can ensure reaction range
Because the change such as temperature, pressure, air-flow causes barrier decline.
Embodiment 5
The method that leaf is converted to activated carbon using plasma combination activator, it is characterised in that comprise the following steps
Pretreatment:Leaf is obtained the pellet of 10-60 mesh specification, Han Shui Liang≤15% after screening, drying, grind;
Activator impregnates:Pellet immersion is included into potassium hydroxide(KOH), zinc chloride(ZnCl2), absolute ethyl alcohol and deionization
Carry out activation process in the activator of water, and the amount of the activator for using and the pellet amount according to 2.5-3.5:1 is matched somebody with somebody
Than dipping Shi Jian≤2 hour;
Dry carbonization treatment:The pellet impregnated by activator is placed in inert gas environment, introducing plasma stream is carried out
Heat up and dry and be carbonized, temperature is increased to 350 ± 50 DEG C simultaneously by the heating curve according to 4-6 DEG C/min in inert gas environment
Keeping temperature 45-60 minutes, pellet is carbonized;
Cleaning treatment:By by the pellet of carbon activation process analysis pure hydrochloric acid(HCl)Stirring and washing, then cleaned with deionized water
Vacuum dehydration dried process is carried out after to neutrality, drying temperature is maintained at 105 ± 5 DEG C, and vacuum is maintained at 90-100KPa, directly
To Han Shui Liang≤5% of the pellet;
Surface activation process:During cleaning treatment, plasma stream is introduced back into when Han Shui Liang≤5% of the pellet
The surface of pellet is modified and activated, and the process of surface activation process needs to keep vacuum environment, activation process time
5-10 seconds.
Potassium hydroxide in the activator(KOH), zinc chloride(ZnCl2)With Zhan Bi≤60% of absolute ethyl alcohol, and hydroxide
Potassium(KOH)Zhan Bi≤40%.
The inert gas environment refers to full of helium(He), neon(Ne), argon(Ar), krypton(Kr), xenon(Xe)Gas or its two
Item or the gaseous environment of multinomial combination.
State to dry and be carbonized in processing procedure, the inert gas is lasting input to keep inert gas environment and adjustment temperature
Degree, the input flow rate of the inert gas is 50SLPM-200SLPM.
Plasma stream is introduced during the surface activation process temperature is increased to 700-800 DEG C.
This is a kind of preferred the present embodiment of the invention.Including pretreatment, activator dipping, dry carbonization treatment,
Leaf raw material screening is first gone out into excellent raw material in the step of cleaning treatment and surface activation process step, pretreatment, is dried de-
Ground again after water, can so ensure the quality of raw material, milled processed of being also more convenient for after drying and dehydrating is required for following process
Specification, and dry pellet has the low advantage of water content;In activator impregnation steps, using inclusion potassium hydroxide(KOH)、
Zinc chloride(ZnCl2), absolute ethyl alcohol and deionized water activator, biomass material meets the carbonization of alkali activator more dehydration,
Use chlorate(Zinc chloride)It is in order to the material in hindering alkali lye and material is too fast anti-as the addition of deionized water and alkali lye
Chlorate should be generated and influence alkali lye to act on the dehydration carbonization-activation of material, the amount of the amount of activator and the pellet according to
2.5-3.5:1 is matched, during dipping between≤be enough within 2 hours make activation carburizing reagent fully thorough;Dry carbonization process step
In, the pellet impregnated by activator is placed in inert gas environment, introducing plasma stream carries out heating up dry and is carbonized,
Plasma stream can produce high temperature, facilitate accuracy controlling, and with certain electrology characteristic, in carbonisation
The carbonizing degree of material can be effectively improved, temperature is raised according to the heating curve of 4-6 DEG C/min in inert gas environment
Simultaneously pellet was carbonized in keeping temperature 45-60 minutes to 350 ± 50 DEG C, gradually intensification helps avoid unexpected high temperature causes material table
Face at a high speed carbonization and inside cannot obtain the influence carbonisation that effectively heats up, be eventually held in predetermined carburizing temperature and keep one
Fix time to ensure that material is fully carbonized, especially for greens, its chloroplast structure can also be destroyed;Cleaning treatment
In step, by by the pellet of carbon activation process analysis pure hydrochloric acid(HCl)Stirring and washing is left with neutralizing when activator impregnates
Alkali residual, then cleaned to neutrality with deionized water and carry out vacuum dehydration dried process, material when vacuum state avoids drying
Oxyphie even combustion effects product quality, drying temperature is maintained at 105 ± 5 DEG C of evaporation dryings of guarantee moisture, and vacuum keeps
In 90-100KPa, until Han Shui Liang≤5% of the pellet, can now be considered as material and meet or exceed general activity
The standard of charcoal;In surface activation process step, when Han Shui Liang≤5% of the pellet again in vacuum environment introduce etc. from
Daughter stream is modified and activates to the surface of pellet, and the process of surface activation process needs to keep vacuum environment, at activation
5-10 seconds reason time, surface of material rapid progresses are made using the ultra-high temperature of plasma stream, strengthen the table in its unit volume
Face adsorption capacity.Be referenced below employ activated carbon surface hole data sample test result tables of data that this method produced with
The advantage of technical solution of the present invention is further illustrated, wherein sample 1 and 2 is control group, is the result being carbonized using existing method,
And sample 3 and 4 are the carbonization results manufactured using technical scheme provided by the present invention;Potassium hydroxide in activator
(KOH), zinc chloride(ZnCl2)With Zhan Bi≤60% of absolute ethyl alcohol, and potassium hydroxide(KOH)Zhan Bi≤40%, it is such to match somebody with somebody
Than the base strength that ensure that activator, contribute to the lifting of activation effect;Inert gas environment refers to full of helium(He), neon
(Ne), argon(Ar), krypton(Kr), xenon(Xe)Gas or its two or the gaseous environment of multinomial combination, selectable range are wide, using group
The form of conjunction can also meet condition, reduce further the difficulty requirement of production;Dry and be carbonized in processing procedure, inert gas
It is persistently to be input into the input flow rate of 50SLPM-200SLPM, being persistently input into will not during inert gas can ensure reaction range
Because the change such as temperature, pressure, air-flow causes barrier decline;Plasma stream is introduced during surface activation process by temperature
700-800 DEG C is increased to, the modified temperature requirement of the surface carbonation of most leaves of plants materials is met at a temperature of this, while
Other materials will not be caused to produce recombination reaction because of excessive temperature.
Claims (5)
1. the method that leaf is converted to activated carbon using plasma combination activator, it is characterised in that comprise the following steps
Pretreatment:Leaf is obtained the pellet of 10-60 mesh specification, Han Shui Liang≤15% after screening, drying, grind;
Activator impregnates:Pellet immersion is included into potassium hydroxide(KOH), zinc chloride(ZnCl2), absolute ethyl alcohol and deionization
Carry out activation process in the activator of water, and the amount of the activator for using and the pellet amount according to 2.5-3.5:1 is matched somebody with somebody
Than dipping Shi Jian≤2 hour;
Dry carbonization treatment:The pellet impregnated by activator is placed in inert gas environment, introducing plasma stream is carried out
Heat up and dry and be carbonized, temperature is increased to 350 ± 50 DEG C simultaneously by the heating curve according to 4-6 DEG C/min in inert gas environment
Keeping temperature 45-60 minutes, pellet is carbonized;
Cleaning treatment:By by the pellet of carbon activation process analysis pure hydrochloric acid(HCl)Stirring and washing, then cleaned with deionized water
Vacuum dehydration dried process is carried out after to neutrality, drying temperature is maintained at 105 ± 5 DEG C, and vacuum is maintained at 90-100KPa, directly
To Han Shui Liang≤5% of the pellet;
Surface activation process:During cleaning treatment, plasma stream is introduced back into when Han Shui Liang≤5% of the pellet
The surface of pellet is modified and activated, and the process of surface activation process needs to keep vacuum environment, activation process time
5-10 seconds.
2. the method for leaf being converted to activated carbon using plasma combination activator as claimed in claim 1, its feature
It is:Potassium hydroxide in the activator(KOH), zinc chloride(ZnCl2)With Zhan Bi≤60% of absolute ethyl alcohol, and potassium hydroxide
(KOH)Zhan Bi≤40%.
3. the method for leaf being converted to activated carbon using plasma combination activator as claimed in claim 1, its feature
It is:The inert gas environment refers to full of helium(He), neon(Ne), argon(Ar), krypton(Kr), xenon(Xe)Gas or its two or
The gaseous environment of multinomial combination.
4. the method for leaf being converted to activated carbon using plasma combination activator as claimed in claim 1, its feature
It is:State dry carbonization processing procedure in, the inert gas be it is lasting input with keep inert gas environment and adjustment temperature,
The input flow rate of the inert gas is 50SLPM-200SLPM.
5. the method for leaf being converted to activated carbon using plasma combination activator as claimed in claim 1, its feature
It is:Plasma stream is introduced during the surface activation process temperature is increased to 700-800 DEG C.
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Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2013079750A1 (en) * | 2011-11-29 | 2013-06-06 | Consejo Superior De Investigaciones Científicas (Csic) | Activated charcoal with high nitrogen content and zero chromium, method for obtaining same and multiple uses thereof |
CN105593167A (en) * | 2013-07-26 | 2016-05-18 | 康宁股份有限公司 | Chemical activation of carbon using rf and dc plasma |
CN106281375A (en) * | 2016-08-10 | 2017-01-04 | 北京神雾环境能源科技集团股份有限公司 | Low temperature continuous pyrolysis biomass prepare fixed bed reactors and the method for activated carbon |
-
2017
- 2017-02-06 CN CN201710065557.7A patent/CN106744939A/en active Pending
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2013079750A1 (en) * | 2011-11-29 | 2013-06-06 | Consejo Superior De Investigaciones Científicas (Csic) | Activated charcoal with high nitrogen content and zero chromium, method for obtaining same and multiple uses thereof |
CN105593167A (en) * | 2013-07-26 | 2016-05-18 | 康宁股份有限公司 | Chemical activation of carbon using rf and dc plasma |
CN106281375A (en) * | 2016-08-10 | 2017-01-04 | 北京神雾环境能源科技集团股份有限公司 | Low temperature continuous pyrolysis biomass prepare fixed bed reactors and the method for activated carbon |
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