CN110152605A - Modification biological charcoal and preparation method thereof and the application in nickel-containing waste water - Google Patents
Modification biological charcoal and preparation method thereof and the application in nickel-containing waste water Download PDFInfo
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- CN110152605A CN110152605A CN201910260254.XA CN201910260254A CN110152605A CN 110152605 A CN110152605 A CN 110152605A CN 201910260254 A CN201910260254 A CN 201910260254A CN 110152605 A CN110152605 A CN 110152605A
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
- B01J20/041—Oxides or hydroxides
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28057—Surface area, e.g. B.E.T specific surface area
- B01J20/28059—Surface area, e.g. B.E.T specific surface area being less than 100 m2/g
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- B01J20/28069—Pore volume, e.g. total pore volume, mesopore volume, micropore volume
- B01J20/28071—Pore volume, e.g. total pore volume, mesopore volume, micropore volume being less than 0.5 ml/g
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- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
- B01J20/3231—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the coating or impregnating layer
- B01J20/3234—Inorganic material layers
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
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Abstract
A kind of application the invention belongs to heavy metal Treatment process field more particularly to modification biological charcoal and preparation method thereof and in nickel-containing waste water.The present invention is by carrying out break process to shell biomass, pyrolysis processing, strong oxidant solution dipping, with a series of modifications such as strong alkaline substance pyroreaction and grinding, the partial size of charcoal is refined, enrich the microcellular structure of charcoal, make modification biological charcoal obtained that there is flourishing microcellular structure, big specific surface area and pore capacities, make modification biological charcoal basic surface functional groups rich in simultaneously, not only have preferable Adsorption efficiency to heavy metal ion, and can heavy metal-passivated ion, improve the removal efficiency of heavy metal.Especially there are preferable absorption and passivation to nickel ion, it is high to nickel ion removal efficiency in waste water.
Description
Technical field
The invention belongs to heavy metal Treatment process field more particularly to a kind of modification biological charcoal, a kind of modification biological charcoal
The application of preparation method and modification biological charcoal in nickel-containing waste water.
Background technique
Nickel and its compound pollution on the environment are referred to as nickel contamination, and in nickel contamination water body, pollutant nickel is main
Exist in the form of Ni (II) (nickelous).The nickel of polluted-water is produced mainly from processes such as plating, smelting, mining and processing
The direct emission of raw industrial wastewater and some solid waste percolates.After Ni-containing Plating Wastewater enters environment, food can be passed through
Object chain is enriched in human body, seriously endangers human health.
Currently, the method for being usually used in removing nickel in water body mainly has: membrane separation process, chemical precipitation method, bioanalysis, ion
Exchange process and absorption method.Wherein, membrane separation process, cost energy consumption is high, and film key technology is to be developed, is mainly with import at present
It is main.Chemical precipitation method can generate waste residue during processing Ni (II), if improper conduct oneself well of the waste residue is comprehended to form secondary dirt
Dye, pollutes environment once again.Ion-exchange, the requirement to ion exchange resin is relatively high, and frequently regeneration is needed just to be able to satisfy
The water quality requirement of Ni (II) water outlet, cost of investment are more expensive.Bioanalysis, because biological self reproducing speed is slow, service condition is severe
It carves, treatment effeciency is low.In addition, water body has to pass through sterilization through containing a large amount of functional microorganisms in microbial method treated water
Etc. techniques can be recycled, the reuse of water resource is restricted.Absorption method, it is special using the structure of porous solid itself
Property and surface characteristic, with waste water in Ni (II) combine to recycle or remove water body Ni (II) to making to purify the sewage.
Absorption method removes the efficiency of Ni (II) in waste water, has direct relation with absorption material.
Currently, for focusing mostly on for adsorbing the research of Ni (II) material in synthetic material such as active carbon, nano-sized carbon
Guan Shang, and the preparation condition requirement of most synthetic materials is very harsh, preparation cost is expensive.Utilize some waste systems
It is standby to be used to adsorb the hot spot that Ni (II) is also current research at charcoal, but most of adsorption effects are all undesirable, do not obtain temporarily
Remarkable break-throughs.
Summary of the invention
The preparation method for being designed to provide a kind of modification biological charcoal of the embodiment of the present invention, it is intended to solve existing absorption
Materials synthesis preparation condition is harsh, with high costs, the undesirable technical problem of adsorption effect.
The another object of the embodiment of the present invention is to provide a kind of modification biological charcoal.
A further object for the embodiment of the present invention is to provide a kind of application of modification biological charcoal in nickel-containing waste water.
In order to achieve the above-mentioned object of the invention, The technical solution adopted by the invention is as follows:
A kind of preparation method of modification biological charcoal, comprising the following steps:
Shell biomass is obtained, break process obtains broken biomass；
Under protective gas atmosphere, after the broken biomass is carried out pyrolysis processing, pulverization process obtains charcoal
Powder；
Strong oxidant solution is obtained, impregnation is carried out to the charcoal powder with the strong oxidant solution, is obtained
Impregnation product；
Strong basicity solid is obtained, is (1~5) by the mass ratio of the impregnation product and the strong basicity solid: 1,
It is reacted 1~2 hour under the conditions of 300 DEG C~400 DEG C, obtains head product；
The head product is washed, then milled processed, obtains modification biological charcoal.
Further, the shell biomass is selected from: peanut shell；And/or
The break process includes: after being dried the shell biomass, to be crushed to 0.5~1.5 centimetre.
Further, the protective gas is selected from: at least one of nitrogen, argon gas, helium；And/or
The step of pyrolysis processing include: by the broken biomass, under protective gas atmosphere, with 10 DEG C/min~
The heating rate of 20 DEG C/min is warming up to 400 DEG C~600 DEG C, keeps the temperature 1~3 hour.
Further, the step of pulverization process includes: the charcoal that will be obtained after the pyrolysis processing, is crushed to
Partial size is not more than 0.3 millimeter of charcoal powder.
Further, the strong oxidant solution includes, liquor potassic permanganate that mass concentration is 0.1%~5.0% or
The hydrogen peroxide that mass fraction is 20%~30%；And/or
The step of impregnation includes: at room temperature, by the charcoal powder and the strong oxidant solution
Mass ratio is 1:(1.5~3), it is dried after the charcoal powder is impregnated 3~6 hours, obtains impregnation product.
Further, the strong basicity solid is selected from: at least one of potassium hydroxide, sodium hydroxide or barium hydroxide.
Further, the step of milled processed includes that, by the head product after the washing, drying and grinding is at partial size
Modification biological charcoal particle no more than 0.3 micron.
A kind of modification biological charcoal, the modification biological charcoal are made by the preparation method of any one of the above modification biological charcoal.
A kind of application of modification biological charcoal in nickel-containing waste water, the modification biological charcoal is applied in nickel-containing waste water,
Remove the nickel ion in waste water.
Further, the modification biological charcoal in nickel-containing waste water application the following steps are included:
Nickel-containing waste water is obtained, the pH value of the nickel-containing waste water is adjusted, obtains adjusting the nickel-containing waste water after pH；
Modification biological charcoal is obtained, in the nickel-containing waste water after the modification biological charcoal to be added to the adjusting pH, constant temperature shake
After swinging processing, the aqueous solution of removal nickel ion is obtained by filtration.
The preparation method of modification biological charcoal provided by the invention, by carrying out break process to shell biomass, at pyrolysis
Reason, strong oxidant solution dipping, with a series of modifications such as strong alkaline substance pyroreaction and grinding, has refined biology
The partial size of charcoal enriches the microcellular structure of charcoal, and modification biological charcoal obtained is made to have flourishing microcellular structure, big ratio
Surface area and pore capacities, while making modification biological charcoal basic surface functional groups rich in, not only to heavy metal ion have compared with
Good Adsorption efficiency, and can heavy metal-passivated ion, improve the removal efficiency of heavy metal.Especially to nickel ion
There are preferable absorption and passivation, adsorbance is high to nickel ion removal efficiency in waste water up to 87mg/g.Also, this hair
The modification biological charcoal of bright offer has preferable cycle life, repeatedly still has higher suction to heavy metal in waste water after absorption parsing
Attached ability can be recycled, long service life.The preparation method of modification biological charcoal provided by the invention, with shell biomass
For raw material, raw material sources are wide, at low cost, and preparation condition and simple process, industrialized production easy to accomplish.
The modification biological charcoal provided by the invention as made from above-mentioned preparation method has flourishing microcellular structure, biggish
Specific surface area and pore capacities, specific surface area is up to 11.892m2/ g, average pore capacities are up to 0.034cm3/ g, average pore size are only
9.6167nm and basic surface functional groups abundant not only have preferable Adsorption efficiency to heavy metal ion, and
Can heavy metal-passivated ion, improve the removal efficiency of heavy metal, especially there is preferable absorption and passivation to make nickel ion
With.Also, modification biological charcoal provided by the invention has preferable cycle life, repeatedly to heavy metal in waste water after absorption parsing
Still there is higher adsorption capacity.
Application of the modification biological charcoal provided by the invention in nickel-containing waste water, modification biological charcoal is to the nickel ion in waste water
There is preferable Adsorption efficiency, the pollution of Heavy Metals in Waters nickel can be effectively reduced, application prospect is wide.
Detailed description of the invention
Fig. 1 is the flow diagram of the preparation method of modification biological charcoal provided in an embodiment of the present invention.
Fig. 2 is the scanning electron microscope (SEM) photograph of the peanut shell charcoal of comparative example 1 of the present invention before modified.
Fig. 3 is the scanning electron microscope (SEM) photograph of 1 modified peanut charcoal of the embodiment of the present invention.
Fig. 4 is the cycle performance test chart of the embodiment of the present invention 5, wherein figure (a) is five circulation absorptions of peanut shell charcoal
The adsorption effect figure；Scheme the adsorption effect figure that (b) is five circulation absorptions of modified peanut charcoal.
Fig. 5 is the usage amount of the embodiment of the present invention 6 and the relational graph of adsorption effect, wherein figure (a) is different peanut shells
The adsorption effect figure of charcoal usage amount；Scheme the adsorption effect figure that (b) is different modified peanut charcoal usage amounts.
Fig. 6 is the adsorption effect of the embodiment of the present invention 7 and the relational graph of pH, wherein figure (a) is flower under condition of different pH
The adsorption effect figure of raw shell charcoal；Scheme the adsorption effect figure that (b) is modified peanut charcoal under condition of different pH.
Specific embodiment
To keep the purpose, technical solution and technical effect of the embodiment of the present invention clearer, in the embodiment of the present invention
Technical solution is clearly and completely described, it is clear that described embodiments are some of the embodiments of the present invention, rather than complete
The embodiment in portion.In conjunction with the embodiment in the present invention, those of ordinary skill in the art are without making creative work
Every other embodiment obtained, shall fall within the protection scope of the present invention.
The weight of Related Component noted in the disclosure of the embodiment of the present invention not only may refer to the specific of each component
Content can also indicate the proportionate relationship of weight between each component, therefore, as long as related according to specification of the embodiment of the present invention
The content of component is scaled up or is reduced within specification of embodiment of the present invention scope of disclosure.Specifically, of the invention
Embodiment weight described in the specification can be mass unit well known to the chemical fields such as μ g, mg, g, kg.
As shown in Fig. 1, the embodiment of the invention provides a kind of preparation methods of modification biological charcoal, comprising the following steps:
S10. shell biomass is obtained, break process obtains broken biomass；
S20. under protective gas atmosphere, after the broken biomass is carried out pyrolysis processing, pulverization process is given birth to
Object carbon powder；
S30. strong oxidant solution is obtained, impregnation is carried out to the charcoal powder with the strong oxidant solution,
Obtain impregnation product；
S40. strong basicity solid is obtained, is (1~5) by the mass ratio of the impregnation product and the strong basicity solid: 1,
It is reacted 1~2 hour under the conditions of 300 DEG C~400 DEG C, obtains head product；
S50. the head product is washed, then milled processed, obtains modification biological charcoal.
The preparation method of modification biological charcoal provided in an embodiment of the present invention, by carrying out break process to shell biomass,
Pyrolysis processing, strong oxidant solution dipping, with a series of modifications such as strong alkaline substance pyroreaction and grinding, refinement
The partial size of charcoal, enriches the microcellular structure of charcoal, and modification biological charcoal obtained is made to have flourishing microcellular structure,
Big specific surface area and pore capacities, while making modification biological charcoal basic surface functional groups rich in, not only to heavy metal from
Son has preferable Adsorption efficiency, and can heavy metal-passivated ion, improve the removal efficiency of heavy metal.It is especially right
Nickel ion has preferable absorption and passivation, and adsorbance is high to nickel ion removal efficiency in waste water up to 87mg/g.And
And modification biological charcoal provided in an embodiment of the present invention has preferable cycle life, repeatedly to heavy metal in waste water after absorption parsing
Still there is higher adsorption capacity, can be recycled, long service life.The preparation of modification biological charcoal provided in an embodiment of the present invention
Method, using shell biomass as raw material, raw material sources are wide, at low cost, and preparation condition and simple process, industry easy to accomplish
Metaplasia produces.
Specifically, in above-mentioned steps S10, shell biomass is obtained, break process obtains broken biomass.The present invention is real
Example is applied using shell biomass as raw material, wherein shell biomass can be peanut shell, rice hulls, apricot shell, cocoanut shell etc., former
Expect that source is wide, easily obtains, improve the utility value of shell resource, reduce the treatment cost of waste water.The embodiment of the present invention passes through
To shell biomass break process, obtained broken biomass is more advantageous to successive modified treatment process.
As a preferred embodiment, the shell biomass is selected from: peanut shell.Shell biology used in the embodiment of the present invention
Matter is the loose peanut shell containing porous structure of quality, itself has certain adsorption capacity, at being modified to peanut shell
Reason, can advanced optimize its pore structure, be obviously improved absorption property.In addition, China is as traditional large agricultural country, flower
Raw yield is up to 15,000,000 tons/year, and the quantity of by-product peanut shell is also up to 5,000,000 tons/year.Wherein, peanut shell removes few portion
Point it is used as the overwhelming majority other than the roughage of animal to be all incinerated or arbitrarily abandon, resource profligacy while can also make
At environmental pollution.The embodiment of the present invention not only may be used by the processing to nickel-containing waste water is used for after porous peanut shell modification
To promote the utility value of discarded peanut shell, while the input cost of wastewater treatment can also be reduced.
As a preferred embodiment, the break process includes: after being dried the shell biomass, to be crushed to 0.5
~1.5 centimetres.The embodiment of the present invention after the drying of shell biomass, will be crushed to 0.5~1.5 centimetre, short grained shell biology
Matter is more advantageous to subsequent pyrolysis processing processing, carbonizes shell biomass sufficiently in pyrolysis.In some embodiments, by institute
After stating the drying process of shell biomass, it is crushed to 0.5 centimetre.In some embodiments, the shell biomass is dried
Afterwards, it is crushed to 0.8 centimetre.In some embodiments, after the shell biomass being dried, it is crushed to 1 centimetre.One
In a little embodiments, after the shell biomass is dried, it is crushed to 1.2 centimetres.
In some embodiments, the shell biomass is selected from: peanut shell；The break process includes: by the shell
After biomass is dried, it is crushed to 0.5~1.5 centimetre.
Specifically, in above-mentioned steps S20, under protective gas atmosphere, the broken biomass is subjected to pyrolysis processing
Afterwards, pulverization process obtains charcoal powder.The embodiment of the present invention is pyrolyzed broken biomass under protective gas atmosphere
Processing processing, protective gas atmosphere can effectively prevent broken biomass and be oxidized during pyrolysis processing.Broken biomass
The ingredient for making through pyrolysis processing nitrogen, hydrogen, oxygen etc. in biomass be easy to volatilize under protective atmosphere dissolve under high temperature environment or
Volatilization ease is gone, and hole is formed, and enriches the pore structure of biomass.Biomass after pyrolysis processing charing carries out pulverization process and obtains
To charcoal powder, the biomass after making charing obtains bigger contact area, can more fill during subsequent modification
Divide and equably mix and react with modified solution, keeps modification more abundant.
As a preferred embodiment, the protective gas is selected from: at least one of nitrogen, argon gas, helium.In some realities
It applies in example, protective gas atmosphere can be pure nitrogen gas, argon gas or helium.In some embodiments, protective gas atmosphere can be
The gaseous mixture of nitrogen and argon gas.In some embodiments, protective gas atmosphere can be, and lead to argon gas after first leading to nitrogen.
As preferred embodiment example, the step of pyrolysis processing includes: by the broken biomass, in protective gas
Under atmosphere, with 10 DEG C/min~20 DEG C/min heating rate, 400 DEG C~600 DEG C are warming up to, keeps the temperature 1~3 hour.The present invention
Embodiment pyrolytic reaction is with the progress of 10 DEG C/min~20 DEG C/min heating rate, and heating pyrolysis is more advantageous to raising life at a slow speed
The yield of object charcoal, it is ensured that biomass is converted into the yield of charcoal, and the yield of charcoal of the embodiment of the present invention can reach
89%.And under the ramp rate conditions, the fiber crosslinking cyclisation inside broken biomass has optimal effect, biomass
The flexible molecule chain of fibrous inside, which is converted into, approaches stable trapezium structure and class Graphitic carbon structure, advantageously forms richer
Pore structure, increase specific surface area and pore capacities.1~3 hour is kept the temperature after being warming up to 400 DEG C~600 DEG C, in the high temperature dwell
The fiber crystallite carbonized in advance inside thermophase biomass is strengthened and is retained, it is ensured that the abundant pore structure of charcoal, this
Some holes gap provides adsorption site, the heavy metal ion being more advantageous in absorption waste water.If pyrolysis processing heating rate is too fast
Charcoal yield is lower, and raw material availability is low, and energy consumption is high.If soaking time is too long or holding temperature is too high, biology will cause
The rupture of matter hole is collapsed, and is unfavorable for generating and is improved adsorption efficiency.
In some embodiments, the step of pyrolysis processing includes: by the broken biomass, in nitrogen gas atmosphere
Under enclosing, with the heating rate of 10 DEG C/min, 500 DEG C are warming up to, keeps the temperature 2 hours.In some embodiments, the pyrolysis processing
The step of include: that the broken biomass under argon gas atmosphere, with the heating rate of 15 DEG C/min, is warming up to 480
DEG C, keep the temperature 3 hours.
As a preferred embodiment, the step of pulverization process includes: the charcoal that will be obtained after the pyrolysis processing,
It is crushed to the charcoal powder that partial size is not more than 0.3 millimeter.The charcoal powder obtained after pulverization process has smaller partial size,
Increase the specific surface area of charcoal, increase the contact area of charcoal and modified solution, be conducive to subsequent impregnation,
The modifications such as highly basic processing are more sufficiently completely.In some embodiments, by powder after the broken biomass progress pyrolysis processing
Then broken processing crosses 60 meshes, obtains small 0.3 millimeter of the charcoal powder of partial size.
Specifically, in above-mentioned steps S30, strong oxidant solution is obtained, with the strong oxidant solution to the charcoal
Powder carries out impregnation, obtains impregnation product.The embodiment of the present invention is by carrying out charcoal powder with strong oxidant solution
Impregnation, charcoal powder is with strong oxidizer dipping process, and strong oxidizer adequately penetrates into inside charcoal, by force
Oxidant is pyrolyzed in the subsequent pyroreaction stage and produces gas, and the gas generated inside charcoal carries out pore-creating to charcoal and changes
Property, the pore structure of charcoal is further enriched, specific surface area and pore capacities are increased, to improve adsorption efficiency.
As a preferred embodiment, the strong oxidant solution includes the potassium permanganate that mass concentration is 0.1%~5.0%
The hydrogen peroxide that solution or mass fraction are 20%~30%.Strong oxidizer concentration is very crucial to the pore-creating effect of charcoal,
When potassium permanganate mass concentration is 0.1%~5.0% or hydrogen peroxide mass fraction is 20%~30%, strong oxygen at this time
Agent has optimal pore-creating modifying function to charcoal, can make inside charcoal in the gas production rate and gas production of pyrolysis phase
Form fine and close microcellular structure.In concentration range provided in an embodiment of the present invention, with the increase of concentration, strong oxidizer is anti-
The gas production answered gradually increases, and the microcellular structure of inside charcoal and surface formation is consequently increased.But as strong oxidizer is molten
Liquid concentration further increases, and reaction becomes acutely, and the bulk gas of generation can form strong impact very to existing micropore
To being allowed to rupture, the microcellular structure on charcoal inside and surface is destroyed, reduces the adsorption capacity of charcoal instead.If strong
Oxidizing agent solution concentration is too low, and the gas flow of generation is very little, unobvious to the modified effect of charcoal.
As a preferred embodiment, the step of impregnation includes: at room temperature, by the charcoal powder and institute
The mass ratio for stating strong oxidant solution is 1:(1.5~3), it is dried, obtains after the charcoal powder is impregnated 3~6 hours
To impregnation product.The embodiment of the present invention with the mass ratio of the charcoal powder and the strong oxidant solution for 1:(1.5~
3) impregnation is carried out, which ensures that strong oxidant solution can be sufficiently impregnated charcoal powder, that is, avoid Strong oxdiative
Dipping caused by agent solution is very little is uneven abundant, also avoid strong oxidant solution it is too many caused by unnecessary waste.Dipping
It can ensure that strong oxidant solution adequately penetrates into inside charcoal powder within 3~6 hours, be conducive to subsequent high temperature pyrolysis
Pore-creating, dip time is too short can not to be made modified sufficiently complete, and dip time is too long to extend preparation power consumption, increased to be prepared into
This.
In some embodiments, the step of impregnation includes: at room temperature, by the charcoal powder and matter
The mass ratio for measuring the liquor potassic permanganate that concentration is 0.1%~5.0% is 1:(1.5~3), the charcoal powder is impregnated 3
It is dried after~6 hours, obtains impregnation product.In further embodiments, the step of impregnation includes: in room
Under temperature, the mass ratio for the hydrogen peroxide for being 20%~30% by the charcoal powder and mass fraction is 1:(1.5~3), it will
The charcoal powder is dried after impregnating 3~6 hours, obtains impregnation product.
Specifically, in above-mentioned steps S40, strong basicity solid is obtained, by the impregnation product and the strong basicity solid
Mass ratio is (1~5): 1, it is reacted 1~2 hour under the conditions of 300 DEG C~400 DEG C, obtains head product.The embodiment of the present invention will
Impregnation product is reacted with strong basicity solid high-temperature, on the one hand, the strong oxidizer inside charcoal is penetrated by impregnation,
Pyrolysis air-generating reaction occurs in high-temperature reaction process, the migration inside charcoal of the gas of generation forms hole, enriches life
Pore structure inside object charcoal；On the other hand, strong basicity solid is modified with charcoal in high-temperature reaction process, activation
Charcoal makes biological carbon surface basic group rich in, improves the pH value of charcoal itself, alkaline charcoal is more
Be conducive to heavy metal-passivated ion, heavy metal ion is made to precipitate removal under alkaline condition, further increases modification biological charcoal
To the removal efficiency of heavy metal ion.Meanwhile strong basicity solid can also be generated in the modifying process to charcoal it is a certain amount of
The gases such as vapor, carbon dioxide, hydrogen, these gases generated can also play optimization function to the pore structure of charcoal,
Further enrich the pore structure on charcoal inside and surface.The mass ratio of the impregnation product and the strong basicity solid
It is reacted 1~2 hour under the conditions of 300 DEG C~400 DEG C for (1~5): 1, it is ensured that the abundant modification to impregnation product generates micro-
Pore structure is fine and close and is rich in the modification biological charcoal of basic group.When strong basicity solids ratios increase, reaction temperature it is too high when or
When reaction time is too long, the thermal chemical reaction that strong basicity solid participates in also more and more acutely, can generate excessive vapor, two
The gases such as carbonoxide, hydrogen, destroy established microcellular structure, reduce the adsorption capacity of modification biological charcoal instead.
As a preferred embodiment, the strong basicity solid is selected from: potassium hydroxide, sodium hydroxide, in barium hydroxide at least
It is a kind of.Strong basicity solid used in the embodiment of the present invention has preferable alkali modification to act on to impregnation product, makes modification biological charcoal
Surface is rich in basic group, is conducive to heavy metal-passivated ion, to improve the removal efficiency of heavy metal ion.It is highly preferred that
The strong basicity solid is selected from: potassium hydroxide.
Specifically, in above-mentioned steps S50, the head product is washed, then milled processed, obtains modification biological charcoal.This hair
Remain a large amount of alkaline matters in head product after bright embodiment impregnation product and strong basicity solid reaction, by washing, preferably
It is washed with deionized, avoids modification biological charcoal and wastewater pH is impacted when administering heavy metal wastewater thereby.Milled processed is thin
The partial size for having changed modification biological charcoal increases the specific surface area of modification biological charcoal, is conducive to improve (outstanding to heavy metal in waste water
It is nickel) adsorption capacity.
As a preferred embodiment, the step of milled processed includes, by the head product after the washing, drying and grinding
It is not more than 0.3 micron of modification biological charcoal particle at partial size.Drying and grinding after the embodiment of the present invention washs head product to neutrality
At partial size less than 0.3 micron, the modification biological charcoal of small particle has bigger specific surface area, to the adsorption energy of heavy metal in waste water
Power is stronger.In some embodiments, drying and grinding is handled after head product is washed to neutrality, is crossed 60 mesh screens, is obtained partial size
Modification biological charcoal particle less than 0.3 micron.
The embodiment of the invention also provides a kind of modification biological charcoal, the modification biological charcoal is modified by any one of the above
The preparation method of charcoal is made.
The modification biological charcoal provided in an embodiment of the present invention as made from above-mentioned preparation method has flourishing microcellular structure,
Biggish specific surface area and pore capacities, specific surface area is up to 11.892m2/ g, average pore capacities are up to 0.034cm3/ g, average hole
Diameter is only 9.6167nm and basic surface functional groups abundant, not only has preferable Adsorption to imitate heavy metal ion
Rate, and can heavy metal-passivated ion, improve the removal efficiency of heavy metal, especially to nickel ion have preferable absorption and
Passivation.Also, modification biological charcoal provided in an embodiment of the present invention has preferable cycle life, repeatedly right after absorption parsing
Heavy metal in waste water still has higher adsorption capacity.
The embodiment of the invention also provides a kind of application of modification biological charcoal in nickel-containing waste water, by above-mentioned modification biological
Charcoal is applied in nickel-containing waste water, removes the nickel ion in waste water.
Application of the modification biological charcoal provided in an embodiment of the present invention in nickel-containing waste water, modification biological charcoal is in waste water
Nickel ion has preferable Adsorption efficiency, can effectively reduce the pollution of Heavy Metals in Waters nickel, and application prospect is wide.
As a preferred embodiment, the modification biological charcoal in nickel-containing waste water application the following steps are included:
Nickel-containing waste water is obtained, the pH value of the nickel-containing waste water is adjusted, obtains adjusting the nickel-containing waste water after pH；
Modification biological charcoal is obtained, in the nickel-containing waste water after the modification biological charcoal to be added to the adjusting pH, constant temperature shake
After swinging processing, the aqueous solution of removal nickel ion is obtained by filtration.
Embodiment more preferably, the modification biological charcoal in nickel-containing waste water application the following steps are included:
The mass concentration for obtaining nickel ion is the nickel-containing waste water of 10~150mg/L, with the HNO of 0.1mol/L3It is controlled with NaOH
The initial pH of serial solution processed is 1.0 ± 0.1~7.0 ± 0.1；
It obtains modification biological charcoal and is added to the adjusting pH by the modification biological charcoal with the ratio of 0.1~0.3g/L
It is 160~200rpm in revolving speed, temperature is 278~318 DEG C of constant temperature oscillation boxes, and duration of oscillation is for 24 hours in nickel-containing waste water afterwards
It after~36h, is filtered using 0.1~0.45 μm of filter membrane to rear suspension liquid is inhaled, the water-soluble of removal nickel ion is obtained after filter
Liquid.
To be readily appreciated by one skilled in the art the above-mentioned implementation detail of the present invention and operation can clearly, and the present invention
The progress performance of embodiment modification biological charcoal and its preparation and the application in nickel-containing waste water significantly embodies, below by way of more
A embodiment illustrates above-mentioned technical proposal.
Embodiment 1
A kind of preparation of modification biological charcoal.
1. taking the drying peanut shell of certain mass, it is crushed to 0.5 centimetre, obtains broken biomass；
2. appropriate broken biomass is placed in the ceramic crucible of 500mL, it is box that crucible is transferred to vacuum atmosphere
Furnace, in N2Protective atmosphere under, control instrument heating rate be 10 DEG C/min, be pyrolyzed 2h under 500 DEG C of pyrolysis temperature,
After its cooling, milled 60 mesh obtains charcoal powder；
3. weighing the above-mentioned charcoal powder of 5.0g, the KMnO with 0.76% mass concentration of 10mL4Solution mixing；At room temperature
After being sufficiently impregnated 4h, it is placed in 60 DEG C of drying box dry 4h, obtains impregnation product；
4. above-mentioned impregnation product is added in the KOH solid of 2.0g, 1h is reacted at 361 DEG C, head product is made；
5. being placed in sufficiently (washing rear liquid pH to be in neutrality) is cleaned with deionized water after the cooling of above-mentioned head product in drying box
Drying to constant weight, finally by the milled 60 mesh sub-sieve of head product, obtains modified peanut charcoal.
Comparative example 1
1. taking the drying peanut shell of certain mass, it is crushed to 0.5 centimetre, obtains broken biomass；
2. appropriate broken biomass is placed in the ceramic crucible of 500mL, it is box that crucible is transferred to vacuum atmosphere
Furnace, in N2Protective atmosphere under, control instrument heating rate be 10 DEG C/min, be pyrolyzed 2h under 500 DEG C of pyrolysis temperature,
After its cooling, milled 60 mesh obtains peanut shell charcoal before modified；
Embodiment 2
A kind of absorption property test of modification biological charcoal.
Ni (II) solution that accurate measurement 100.00mL initial concentration is 20mg/L is in 100mL wide mouthed Erlenmeyer bottle, Xiang Qi
In add 0.3g the embodiment of the present invention 1 prepare modified peanut charcoal, with the HNO of 0.1mol/L3It is molten with NaOH control system
The initial pH of liquid is 6.0, is vibrated for 24 hours in the constant temperature oscillator that temperature is 298K, revolving speed is 160 rpm.Then absorption is calculated
After the completion in solution nickel ion content, obtain the modification biological charcoal and 99% can achieve to the nickel removal rate in solution.
By above-mentioned experiment as it can be seen that the adsorption effect of modification biological charcoal of the invention is good, to the adsorption capacity of nickel ion
It is high.
Embodiment 3
To the peanut shell charcoal after before modified, (comparative example 1 is peanut shell carbon before modified, and embodiment 1 is modified peanut
Charcoal) appearance structure carry out the test of surface sweeping Electronic Speculum (SEM test), scanning electron microscope (SEM) photograph is as shown in attached drawing 2,3.
Attached drawing 2 is the appearance structure of peanut shell charcoal (comparative example 1) before modified, it is seen that before modified peanut shell charcoal surface compared with
It is smooth, still retain the part pattern of raw material peanut shell, pore structure is more loose, and surface is almost without micropore.
Attached drawing 3 is modified peanut charcoal (embodiment 1), it is seen that modified peanut shell charcoal surface becomes coarse and has micro-
Hole occurs, and whole aperture also becomes smaller.
Embodiment 4
To rear peanut shell charcoal before modified (comparative example 1 is peanut shell carbon before modified, and embodiment 1 is modified peanut charcoal)
Carry out specific surface area test (BET test), as shown in table 1 below.The average hole Rong Zengjia of modified peanut shell charcoal, average hole
Diameter reduces.According to the measurement of specific surface area, the specific surface area of peanut shell charcoal before modified is 0.7447m2/ g, and modification biological
The specific surface area of charcoal is 11.892m2/ g, modified specific surface area increase nearly 15 times.The specific surface area of material is bigger, average
Hole Rong Zengjia, it is more therefore more excellent to the adsorption effect of nickel that average pore size reduces available adsorption site.
Table 1
| Title | Specific surface area (m2/g) | Average Kong Rong (cm3/g) | Average pore size (nm) |
| Comparative example 1 | 0.7447 | 0.002651 | 34.8159 |
| Embodiment 1 | 11.892 | 0.034 | 9.6167 |
Embodiment 5
Measure the cyclical stability of modified peanut charcoal (embodiment 1) with peanut shell charcoal (comparative example 1) before modified.
The solution for being 20mg/L to Ni (II) concentration, with the HNO of 0.1mol/L3The initial pH of solution is adjusted with NaOH solution
It is 7.0 ± 0.1, the modified peanut charcoal of 1.0g/L is added to 50.00mL Ni (II) solution, temperature is 298K, revolving speed is
It is vibrated for 24 hours in the constant temperature oscillator of 160rpm.After the completion of absorption, filters out peanut shell charcoal and be dried for standby.It is accurate to measure 25.00mL
Certain density stripping workshop, adds the peanut shell charcoal that 1.0g/L has adsorbed Ni (II), and temperature is controlled in steady temperature, revolving speed
It is maintained at 160rpm, vibrates 24 h.After the completion of desorption reaction, the suspension after desorption was carried out using 0.45 μm of filter membrane
Filter, liquid measures the equilibrium concentration of Ni (II) in solution using dimethylglyoxime spectrophotometry after filter, and then calculates corresponding Ni
(II) desorption efficiency.Peanut shell charcoal before modified after desorption is again 50.00mL that 20mg/L, pH are 7.0 ± 0.1 to concentration
Ni (II) solution carries out adsorption treatment under the same conditions as above, and above-mentioned identical desorption processing is carried out after the completion of absorption
With the measurement of Ni (II) desorption efficiency.Repeat above-mentioned absorption-desorption it is attached-continuous mode five times, the circulation of peanut shell charcoal is calculated
It tests shown in adsorbance such as Fig. 4 (a).
The solution for being 20mg/L to Ni (II) concentration, with the HNO of 0.1mol/L3The initial pH of solution is adjusted with NaOH solution
It is 6.0 ± 0.1, the modified peanut charcoal of 0.10g/L is added to 100.00mL Ni (II) solution, is 298K, revolving speed in temperature
To be vibrated for 24 hours in the constant temperature oscillator of 160rpm.After the completion of absorption, filters out modified peanut charcoal and be dried for standby.It is accurate to measure
The certain density stripping workshop of 50.00mL, adds the modified peanut charcoal that 0.10g/L has adsorbed Ni (II), and temperature is controlled in perseverance
Determine temperature, revolving speed is maintained at 160 rpm, and oscillation is for 24 hours.After the completion of desorption reaction, using 0.45 μm of filter membrane to outstanding after desorption
Supernatant liquid is filtered, equilibrium concentration of the liquid using Ni (II) in dimethylglyoxime spectrophotometry measurement solution, Jin Erji after filter
Calculate the desorption efficiency of corresponding Ni (II).It is 6.0 ± 0.1 that modified peanut charcoal after desorption, which is again 20mg/L, pH to concentration,
100.00mL Ni (II) solution carries out adsorption treatment under the same conditions as above, carries out after the completion of absorption above-mentioned identical
The measurement of desorption processing and Ni (II) desorption efficiency.Repeat above-mentioned absorption-desorption it is attached-continuous mode five times, modification is calculated
Shown in loop test adsorbance such as Fig. 4 (b) of peanut shell charcoal.
As shown in Fig. 4, peanut shell charcoal reduces the adsorbance of Ni (II) with the increase of absorption number, adsorbs number
5 are changed to from 1, corresponding adsorbance is reduced to 0.05mg/g from 5.14mg/g.After absorption 5 times, peanut shell charcoal is several to Ni (II)
Suction-operated is not played, it is shorter to illustrate that it adsorbs the service life.But suction of the modified peanut shell charcoal after 2 absorption to Ni (II)
Attached amount is still maintained at 41mg/g or more.After absorption 5 times, adsorbance is reduced to 18.77mg/g by 80.23mg/g, but with it is most of
Adsorbent material is compared, this adsorbance is still fallen within compared with high adsorption capacity, shows that modified peanut charcoal can continue Ni (II) to keep higher
Adsorption capacity, absorption lasts a long time.
Embodiment 6
Modified peanut charcoal (embodiment 1) is measured with the usage amount of peanut shell charcoal (comparative example 1) before modified in waste water
The influence of the adsorption effect of nickel.
Five groups are taken respectively, and 50.00mL concentration is Ni (II) solution of 20mg/L, with the HNO of 0.1mol/L3And NaOH solution
Adjusting its initial pH is 7.0 ± 0.1, adds the peanut shell charcoal before modified of 1.0,2.0,3.0,4.0 Yu 5.0g/L respectively,
Temperature is 298K, revolving speed is to vibrate for 24 hours in the constant temperature oscillator of 160rpm.After the completion of adsorption reaction, 0.45 μm of filter membrane is utilized
Suspension after absorption is filtered, liquid measures the balance of Ni (II) in solution using dimethylglyoxime spectrophotometry after filter
Concentration, shown in the peanut shell adsorbance such as attached drawing 5 (a) for calculating the different dosages of gained.
Five groups are taken respectively, and 100.00mL concentration is Ni (II) solution of 20mg/L, with the HNO of 0.1mol/L3It is molten with NaOH
It is 6.0 ± 0.1 that liquid, which adjusts its initial pH, adds the modified peanut charcoal of 0.10,0.15,0.20,0.25 and 0.30g/L respectively,
It is vibrated for 24 hours in the constant temperature oscillator that temperature is 298K, revolving speed is 160rpm.After the completion of adsorption reaction, 0.45 μm of filter is utilized
Film is filtered the suspension after absorption, after filter liquid using in dimethylglyoxime spectrophotometry measurement solution Ni (II) it is flat
Weigh concentration, shown in the adsorbance such as attached drawing 5 (b) for calculating the modified peanut charcoal of the different dosages of gained.
By attached drawing 5 as it can be seen that the throwing amount of modified peanut charcoal is only the 1/10 of the throwing amount of peanut shell charcoal before modified, absorption
Effect but improves more than 10 times, shows that modification largely improves peanut shell charcoal to the adsorption effect of Ni (II), 0.10g/
L modified peanut charcoal is to the adsorbance of Ni (II) up to 78.31mg/g.
Embodiment 7
PH is measured to the nickel adsorption effect of modified peanut charcoal (embodiment 1) and peanut shell charcoal (comparative example 1) before modified
Influence.
The solution for being 20mg/L to Ni (II) concentration, with the HNO of 0.1mol/L3The initial of serial solution is adjusted with NaOH
PH is respectively 1.0 ± 0.1,2.0 ± 0.1,3.0 ± 0.1,4.0 ± 0.1,5.0 ± 0.1,6.0 ± 0.1 and 7.0 ± 0.1.Respectively
The above-mentioned difference pH nickel solution of 50.00mL is taken, the peanut shell charcoal before modified of 1.0g/L is added, temperature is 298K, revolving speed is
It is vibrated for 24 hours in the constant temperature oscillator of 160rpm.The suspension after absorption was carried out using 0.45 μm of filter membrane after the completion of absorption
Filter, liquid calculates flower under gained difference pH using the equilibrium concentration of Ni (II) in dimethylglyoxime spectrophotometry measurement solution after filter
Shown in adsorbance such as Fig. 6 (a) of raw shell charcoal.
The above-mentioned difference pH nickel solution of 100.00mL is taken respectively, is added the modified peanut charcoal of 0.10g/L, is in temperature
It is vibrated for 24 hours in 298K, the constant temperature oscillator that revolving speed is 160rpm.After absorption is after the completion using 0.45 μm of filter membrane to absorption
Suspension is filtered, and liquid calculates institute using the equilibrium concentration of Ni (II) in dimethylglyoxime spectrophotometry measurement solution after filter
It obtains under different pH shown in adsorbance such as Fig. 6 (b) of modified peanut charcoal.
It will be appreciated from fig. 6 that when the initial pH of nickel solution is in reduced levels (pH 1.0~2.0), peanut shell before modified
Charcoal, modified peanut charcoal are lower to the adsorbance of Ni (II).With the raising of pH, adsorbance increases therewith, peanut shell, modified flower
Raw shell charcoal is all relatively good to the adsorption effect of Ni (II) when the initial pH of solution is 7.0,6.0, to the maximal absorptive capacity of Ni (II)
Respectively 5.79mg/g, 87.92mg/g.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (10)
1. a kind of preparation method of modification biological charcoal, which comprises the following steps:
Shell biomass is obtained, break process obtains broken biomass；
Under protective gas atmosphere, after the broken biomass is carried out pyrolysis processing, pulverization process obtains charcoal powder；
Strong oxidant solution is obtained, impregnation is carried out to the charcoal powder with the strong oxidant solution, is impregnated
Product；
Obtain strong basicity solid, be (1~5) by the mass ratio of the impregnation product and the strong basicity solid: 1,300 DEG C~
It is reacted 1~2 hour under the conditions of 400 DEG C, obtains head product；
The head product is washed, then milled processed, obtains modification biological charcoal.
2. the preparation method of modification biological charcoal as described in claim 1, which is characterized in that the shell biomass is selected from: flower
Raw shell；And/or
The break process includes: after being dried the shell biomass, to be crushed to 0.5~1.5 centimetre.
3. the preparation method of the modification biological charcoal as described in claim 1~2 any one, which is characterized in that the protection gas
Body is selected from: at least one of nitrogen, argon gas, helium；And/or
The step of pyrolysis processing includes: by the broken biomass, under protective gas atmosphere, with 10 DEG C/min~20
DEG C/heating rate of min, 400 DEG C~600 DEG C are warming up to, keeps the temperature 1~3 hour.
4. the preparation method of modification biological charcoal as claimed in claim 3, which is characterized in that the step of pulverization process wraps
Include: the charcoal that will be obtained after the pyrolysis processing is crushed to the charcoal powder that partial size is not more than 0.3 millimeter.
5. the preparation method of modification biological charcoal as described in claim 1 or 4, which is characterized in that the strong oxidant solution packet
It includes, the hydrogen peroxide that the liquor potassic permanganate or mass fraction that mass concentration is 0.1%~5.0% are 20%~30%；With/
Or,
The step of impregnation includes: at room temperature, by the quality of the charcoal powder and the strong oxidant solution
Than for 1:(1.5~3), will the charcoal powder impregnate 3~6 hours after be dried, obtain impregnation product.
6. the preparation method of modification biological charcoal as described in claim 1 or 4, which is characterized in that the strong basicity solid is selected from:
At least one of potassium hydroxide, sodium hydroxide, barium hydroxide.
7. the preparation method of modification biological charcoal as claimed in claim 6, which is characterized in that the step of milled processed wraps
It includes, by the head product after the washing, drying and grinding is not more than 0.3 micron of modification biological charcoal particle at partial size.
8. a kind of modification biological charcoal, which is characterized in that the modification biological charcoal is as described in claim 1~7 any one
The preparation method of modification biological charcoal is made.
9. a kind of application of modification biological charcoal in nickel-containing waste water, which is characterized in that by modification biological charcoal according to any one of claims 8
It is applied in nickel-containing waste water, removes the nickel ion in waste water.
10. application of the modification biological charcoal as claimed in claim 9 in nickel-containing waste water, which is characterized in that the modification biological
Charcoal in nickel-containing waste water application the following steps are included:
Nickel-containing waste water is obtained, the pH value of the nickel-containing waste water is adjusted, obtains adjusting the nickel-containing waste water after pH；
Modification biological charcoal is obtained, in the nickel-containing waste water after the modification biological charcoal to be added to the adjusting pH, at isothermal vibration
After reason, the aqueous solution of removal nickel ion is obtained by filtration.
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