CN107597059A - The preparation method of modified microplate stratiform feature feather charcoal before a kind of hydro-thermal soda acid - Google Patents
The preparation method of modified microplate stratiform feature feather charcoal before a kind of hydro-thermal soda acid Download PDFInfo
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- CN107597059A CN107597059A CN201710560921.7A CN201710560921A CN107597059A CN 107597059 A CN107597059 A CN 107597059A CN 201710560921 A CN201710560921 A CN 201710560921A CN 107597059 A CN107597059 A CN 107597059A
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Abstract
The invention belongs to the practical technique of field of environment engineering, there is provided the preparation method of modified microplate stratiform feature feather charcoal before a kind of hydro-thermal soda acid, mainly using waste and old animal source biomass（Using chicken feather as embodiment）, soda acid modifying agent（0.01mol/L KOH and H2SO4Solution）For raw material, the characteristics of being easily modified using the main component of animal source biomass raw material in the high temperature and high pressure environment of hydro-thermal method by acid and alkali hydrolysis, activated carbon raw material are modified, it is higher to produce specific surface area, the more functional adsorbents of surface-functional functional group, modifying process is simple, quick, green, efficient before entirely, and the dosage of modifying agent, a large amount of generations for reducing secondary pollutions can not only be greatly reduced.Meanwhile the performance of absorbent charcoal material can be significantly lifted in the case where activation condition is constant, and the preparation cost of same type of material is greatly lowered.Obtained new material is nontoxic, is easy to reclaim, and adsorption efficiency is high, meets the technique and engineering demand of water process.
Description
Technical field
Application the present invention relates to a kind of synthesis preparation method of modified function adsorbent and its in the treatment of waste water, work
It is related to water treatment field in journey, is technically related to materials synthesis field and absorbent fields.
Background technology
The problem of water pollution, is fast-developing and outstanding day by day along with economy, and in water treatment field, absorption method has long-drawn-out
Long developing history, it has, and technical threshold is low, it is simple efficiently, strong adaptability is repeatable the advantage such as to utilize, and is led in environmental project
Domain is lasting, and most widely used further treatment technique at present.
As the charcoal of all polymorphic types is gradual by numerous studies, adsorbent cheap, efficient, with strong points in recent years
Welcome by water treatment field.At the same time, influence the factor of adsorbent absorption property also with research deeply progressively by
Disclose.In the factor of many influence adsorbent absorption properties, specific surface area and surface-active are undoubtedly influence performance of the adsorbent
Two deciding factors.Many research is being directed to exploring the specific surface area for how increasing adsorbent always and surface is lived
Property, to be effectively increased the adsorption capacity of adsorbent.
In the case where activation condition is constant, surface be modified as it is a kind of it is traditional, easily lifted adsorbent compare surface
The method of product and surface-active, it is widely used in basic research and actual production life.Traditional adsorbent surface is modified
Mode is that the surface of adsorbent material is etched by corrosive substances such as acid, alkali, on the one hand removes part surface impurity, and part increases
Add specific surface area, be on the other hand then the composition for the functional group for reconstructing adsorbent surface, increase hydroxyl, carboxyl, aldehyde radical isopolarity
The content of functional group, the chemisorbed activity of adsorbent is effectively improved, increases the energy of adsorption to part material containing particular functional group
Power.But all the time, acid, alkali modification need to consume substantial amounts of acid, alkali raw material, substantial amounts of water resource, and directly produce substantial amounts of
Secondary pollution, while the absorption property of limited raising activating agent is only capable of, therefore denounced by many scholars.
The present invention provides new method modified before one, new approaches, traditional modification biological charcoal reparation technology is overturned, by work
Property charcoal raw material it is modified before advance row hydro-thermal method is carbonized, it is whole before modifying process is simple, quick, green, efficiently, not only can be with
The dosage of modifying agent is greatly reduced, a large amount of generations for reducing pollutant.Meanwhile can be big in the case where activation condition is constant
Amplitude lifts the specific surface area performance of biological carbon materials.It is the preceding method of modifying that a whole set of is achieved many things at one stroke.
The content of the invention
Activated carbon is the more deep adsorbent of research, and the research currently for activated carbon focuses mostly in charcoal neck
Domain, in order to lift the adsorption capacity of adsorbent, researcher is by the raw material of shift activity charcoal product, conversion activation mostly
The mode such as agent, increase modifying process improves the specific surface area and surface-active of adsorbent, to improve the adsorption capacity of adsorbent.Mesh
Before, method of modifying is based on the research and development of finished product adsorbent, is carried out in the end of adsorbent production,
The present invention attempts to use for reference the process that hydro-thermal method prepares activated carbon, with reference to the hydrolysis principle of animal sources biological material, breaks
Original method of modifying thinking, it is directed to developing a set of hydro-thermal soda acid method of modifying, to the biomass former material of animal sources activated carbon
Material carries out hydro-thermal soda acid modification, the modification and modification of material surface is carried out from source, using protein substance in high temperature
（200 DEG C or so）High pressure（More than 10MPa）Acid-base condition under under characteristic susceptible to hydrolysis, artificial modified bar before manufacturing hydro-thermal
Part, it is more small keratin lamella or polypeptide microplate to promote animal sources biomass by hydrolyzation, is more easy to get after last carbonization-activation
To smaller thinner microplate layer structure.Meanwhile the functional group obtained by the peptide bond hydrolysis such as amino, carboxyl, hydroxyl is in lamella table
Surface density is higher.Therefore there is the animal sources biomass carbon for being modified method preparation using hydro-thermal soda acid high-specific surface area and high surface to live
The characteristic of property.
The concrete technical scheme of the present invention is as follows：
1. raw material prepares
Chicken feather needs to carry out cleaning decontamination processing after collecting, and the chicken feather after cleaning is placed in drying box and processing is dried.Take respectively
Chicken feather after 4g ± 0.01g is cleaned is shredded to 1cm or so length, is placed in 3 20ml tool lid polytetrafluoroethylene (PTFE) water heating kettle liners；
Configure 0.01mol/L KOH and H2SO4Each 100mL of solution is as hydrothermal modification agent, anhydrous K2CO3（Analyze pure）Purchased from purchase
Buy from Tianjin Fengchuan Chemical Reagent Science ＆ Technology Co., Ltd., Amoxicillin（Analyze pure）；
2. hydrothermal modification
It is dense that deionized water 10mL, 0.01mol/L are separately added into 3 polytetrafluoroethylene (PTFE) for being equipped with chicken feather water heating kettle liners respectively
The H of KOH solution 10mL, the 0.01mol/L concentration of degree2SO4Solution 10mL, sealing capping, is put into insulating box, is heated to 200 DEG C of perseverances
Warm 4h.Room temperature is down in water-bath after taking out water heating kettle；
3. carbonization-activation
Treat that water heating kettle is cooled to room temperature, the brown viscous liquid of gained in three reactors is drained to 3 tool lids respectively successively
In corundum crucible, crucible is placed in tube furnace successively, in nitrogen atmosphere（60cm3/min）Under heated with 10 DEG C/min speed
To 450 DEG C and after keeping 1h, room temperature is naturally cooled to.Corundum crucible is taken out, respectively grinds obtained black Carbon Materials with agate
Alms bowl grinding is in powdered, 3 kinds of each 2g of carbon powder is weighed with a ten thousandth balance, with 3g anhydrous Ks2CO3Powder is mixed in 3 respectively
In corundum crucible, each crucible is separately added into 9mL deionized waters and 1mL95% ethanol, with glass bar by said mixture in crucible
Middle stirring is homogeneous pastel, is placed in heating 8h in 110 DEG C of aeration cabinet.Dried crucible is numbered respectively after taking out,
It is placed in tube furnace, in nitrogen atmosphere（60cm3/min）Under be heated to 750 DEG C with 10 DEG C/min speed and keep 1h, it is natural
Corundum crucible is taken out after being cooled to room temperature, by obtained activation Carbon Materials in each crucible with agate mortar grinding in powdered,
Microplate stratiform feature feather charcoal and the not preceding modified microplate stratiform feature to analyze are modified before hydro-thermal soda acid is made
Feather charcoal crude product；
4. post-process
By feather charcoal crude product respectively with soda acid and deionized water rinsing to neutrality, filtering, 60 DEG C of dry 12h are placed in.After grinding
Both microplate stratiform feature feather charcoal was modified before having obtained finished product.
Brief description of the drawings
Fig. 1 is to be modified microplate stratiform feature feather charcoal formation mechenism figure, Figure of abstract.
Fig. 2 is the BET figures of modified microplate stratiform feature feather charcoal.
Fig. 3 is the SEM figures of modified microplate stratiform feature feather charcoal.
Fig. 4 is the Raman figures of modified microplate stratiform feature feather charcoal.
Fig. 5 is the XPS of modified microplate stratiform feature feather charcoal（O1 s）Figure.
Fig. 6 is the ZETA potential diagrams of modified microplate stratiform feature feather charcoal.
Fig. 7 is that modified absorption of the microplate stratiform feature feather charcoal removal simulation containing Amoxicillin in antibiotic waste water is gone
Except rate-time plot.
Fig. 8 is that modified microplate stratiform feature feather charcoal removes different pH environment Imitatings containing Ah not in antibiotic waste water
The eliminating rate of absorption comparison diagram in XiLin.
Embodiment
The present invention is further illustrated with reference to embodiments.
Embodiment 1：The Amoxicillin solution that compound concentration is 100mg/L contains antibiotic waste water as simulation.Modulus respectively
Intend 100mL containing antibiotic waste water in 3 150mL conical flask, 0.1g 3 kinds of modified microplates are separately added into 3 conical flasks
Stratiform feature feather charcoal, 3 conical flask bottlenecks are obturaged, be placed in constant temperature oscillator and carry out respectively with parafilm sealed membranes
Concussion.Shaken 90 minutes with 200 revs/min of speed at 25 DEG C, respectively at 0.5 minute, sample 3mL, entered with Medium speed filter paper
Row filtering, filtrate is placed on ultraviolet-visible spectrophotometer and determines absorbance at 240nm wavelength.It will be inhaled according to standard curve
Luminosity is scaled concentration, calculates the clearance of Amoxicillin.Removal situation is shown in Fig. 7.
Embodiment 2：Compound concentration is 100mg/L respectively, and pH 2,7,12 Amoxicillin solution is used as acid, neutrality,
Alkalescence simulation contains antibiotic waste water.3 kinds of simulation 50mL containing antibiotic waste water are taken respectively respectively in 150mL conical flask, first batch of 3
0.1g alkali modification microplate stratiform feature feather charcoal is separately added into conical flask, separately takes 3 kinds of simulations to contain antibiotic waste water
50mL is separately added into 0.1g unmodified microplate stratiform feature respectively in 150mL conical flask in 3 conical flasks of second batch
Feather charcoal, 3 kinds of simulation 50mL containing antibiotic waste water are separately taken to distinguish respectively in 150mL conical flask in the 3rd batch of 3 conical flasks
The 0.1g modified microplate stratiform feature feather charcoal of acid is added, all conical flasks are obturaged with parafilm sealed membranes, are placed in constant temperature
Shaken in oscillator.3mL is sampled after being shaken 90 minutes with 200 revs/min of speed at 25 DEG C, is carried out with Medium speed filter paper
Filtering, filtrate is placed on ultraviolet-visible spectrophotometer and determines absorbance at 240nm wavelength.According to standard curve by extinction
Degree is scaled concentration, calculates the clearance of Amoxicillin.Removal situation is shown in Fig. 8.
Claims (2)
1. the preparation method of modified microplate stratiform feature feather charcoal before a kind of hydro-thermal soda acid, it is characterised in that including following several
Kind step：
Step 1：Raw material prepares：
Chicken feather needs to carry out cleaning decontamination processing after collecting, and the chicken feather after cleaning is placed in drying box and processing is dried.Take respectively
Chicken feather after 4g ± 0.01g is cleaned is shredded to 1cm or so length, is placed in 3 20ml tool lid polytetrafluoroethylene (PTFE) water heating kettle liners；
Configure 0.01mol/L KOH and H2SO4Each 100mL of solution is as hydrothermal modification agent, anhydrous K2CO3(analysis is pure) is purchased from purchase
Buy from Tianjin Fengchuan Chemical Reagent Science ＆ Technology Co., Ltd., Amoxicillin (analysis is pure)；
Step 2：Hydrothermal modification：
It is dense that deionized water 10mL, 0.01mol/L are separately added into 3 polytetrafluoroethylene (PTFE) for being equipped with chicken feather water heating kettle liners respectively
The H of KOH solution 10mL, the 0.01mol/L concentration of degree2SO4Solution 10mL, sealing capping, is put into insulating box, is heated to 200 DEG C of perseverances
Warm 4h.Room temperature is down in water-bath after taking out water heating kettle；
Step 3：Carbonization-activation：
Treat that water heating kettle is cooled to room temperature, the brown viscous liquid of gained in three reactors is drained to 3 tool lids respectively successively
In corundum crucible, crucible is placed in tube furnace successively, in nitrogen atmosphere (60cm3/ min) under heated with 10 DEG C/min speed
To 450 DEG C and after keeping 1h, room temperature is naturally cooled to.Corundum crucible is taken out, respectively grinds obtained black Carbon Materials with agate
Alms bowl grinding is in powdered, 3 kinds of each 2g of carbon powder is weighed with a ten thousandth balance, with 3g anhydrous Ks2CO3Powder is mixed in 3 respectively
In corundum crucible, each crucible is separately added into 9mL deionized waters and 1mL95% ethanol, with glass bar by said mixture in earthenware
Stirring is homogeneous pastel in crucible, is placed in heating 8h in 110 DEG C of aeration cabinet.Dried crucible is compiled respectively after taking out
Number, it is placed in tube furnace, in nitrogen atmosphere (60cm3/ min) under be heated to 750 DEG C with 10 DEG C/min speed and keep 1h, from
Corundum crucible is taken out after being so cooled to room temperature, is in powder by obtained activation Carbon Materials are ground with agate mortar in each crucible
Shape, microplate stratiform feature feather charcoal and the not preceding modified microplate stratiform function of analyzing are modified before hydro-thermal soda acid is made
Sex feathers hair charcoal crude product；
Step 4：Post processing：
By feather charcoal crude product respectively with soda acid and deionized water rinsing to neutrality, filtering, 60 DEG C of dry 12h are placed in.After grinding
Both microplate stratiform feature feather charcoal was modified before having obtained finished product.
2. preparation process according to claim 1, it is characterised in that using protein substance HTHP soda acid
Under the conditions of under characteristic susceptible to hydrolysis, artificial modified condition before manufacturing hydro-thermal, promote animal sources biomass by hydrolyzation to be more small
Keratin lamella or polypeptide microplate, be more easy to obtain smaller thinner microplate layer structure after last carbonization-activation；Meanwhile ammonia
Functional group obtained by the peptide bond hydrolysis such as base, carboxyl, hydroxyl is higher in sheet surfaces density.Therefore it is modified method using hydro-thermal soda acid
The animal sources biomass carbon of preparation has the characteristic of high-specific surface area and high surface.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108793157A (en) * | 2018-08-24 | 2018-11-13 | 山东大学 | The method that wetland fruit grown shell and hydrolyzed feather meal mixed base charcoal precursor prepare activated carbon |
| CN110975813A (en) * | 2019-12-18 | 2020-04-10 | 内蒙古大学 | Salix psammophila-based porous carbon and preparation method and application thereof |
| CN111617740A (en) * | 2020-05-25 | 2020-09-04 | 齐鲁工业大学 | Layered carbon/titanium dioxide composite material and preparation method and application thereof |
| CN116440866A (en) * | 2023-03-13 | 2023-07-18 | 武汉工程大学 | Preparation method and application of three-dimensional spongy porous heavy metal ion adsorbent based on activated eggshells |
-
2017
- 2017-07-11 CN CN201710560921.7A patent/CN107597059A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| HUIQIN LI, ET AL.: "Development and assessment of a functional activated fore-modified bio-hydrochar for amoxicillin removal", 《BIORESOURCE TECHNOLOGY》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108793157A (en) * | 2018-08-24 | 2018-11-13 | 山东大学 | The method that wetland fruit grown shell and hydrolyzed feather meal mixed base charcoal precursor prepare activated carbon |
| CN110975813A (en) * | 2019-12-18 | 2020-04-10 | 内蒙古大学 | Salix psammophila-based porous carbon and preparation method and application thereof |
| CN111617740A (en) * | 2020-05-25 | 2020-09-04 | 齐鲁工业大学 | Layered carbon/titanium dioxide composite material and preparation method and application thereof |
| CN116440866A (en) * | 2023-03-13 | 2023-07-18 | 武汉工程大学 | Preparation method and application of three-dimensional spongy porous heavy metal ion adsorbent based on activated eggshells |
| CN116440866B (en) * | 2023-03-13 | 2023-09-22 | 武汉工程大学 | Preparation method and application of three-dimensional spongy porous heavy metal ion adsorbent based on activated eggshells |
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Application publication date: 20180119 |