CN109225129A - A kind of production method of the preceding modified microballoon functionality straw charcoal of hydro-thermal preparation - Google Patents
A kind of production method of the preceding modified microballoon functionality straw charcoal of hydro-thermal preparation Download PDFInfo
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- CN109225129A CN109225129A CN201710551383.5A CN201710551383A CN109225129A CN 109225129 A CN109225129 A CN 109225129A CN 201710551383 A CN201710551383 A CN 201710551383A CN 109225129 A CN109225129 A CN 109225129A
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Abstract
The invention belongs to the practical technique of field of environment engineering, a kind of production method of modified microspheroidal functionality straw charcoal before hydro-thermal soda acid is provided, is mainly used waste and old plant source biomass (using straw core as embodiment), the soda acid modifying agent (KOH and H of 0.01mol/L2SO4Solution) it is raw material, the feature being easily modified by acid and alkali hydrolysis in the high temperature and high pressure environment of hydro-thermal method using the main component of animal source biomass raw material, active 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 can not only be greatly reduced, largely reduce the generation of secondary pollution.Meanwhile the performance of absorbent charcoal material can be significantly promoted 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, and convenient for recycling, 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 production 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 technique
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 is low with technical threshold, it is simple and efficient, adaptable, the advantages such as reusable, is led in environmental project
Domain is lasting, and most widely used further treatment technique at present.
As, by numerous studies, adsorbent cheap, efficient, with strong points was gradually in recent years for the charcoals of all polymorphic types
Welcome by water treatment field.At the same time, influence the factor of adsorbent absorption property also with research deeply gradually by
It discloses.In many factors for influencing adsorbent absorption property, specific surface area and surface-active are undoubtedly influence performance of the adsorbent
Two deciding factors.Many research is being dedicated to exploring the specific surface area for how increasing adsorbent always and surface is living
Property, to effectively increase the adsorption capacity of adsorbent.
In the case where activation condition is constant, surface is modified as a kind of traditional, convenient and fast promotion adsorbent specific surface
Long-pending and surface-active method 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 of the surface impurity, and part increases
Add specific surface area, is on the other hand then the composition for reconstructing the functional group of adsorbent surface, increases hydroxyl, carboxyl, aldehyde radical isopolarity
The content of functional group effectively improves the chemisorption activity of adsorbent, increases the adsorption energy to part substance containing particular functional group
Power.But all the time, acid, alkali modification need to consume a large amount of acid, alkali raw material, a large amount of water resource, and directly generate a large amount of
Secondary pollution, while it being only capable of the absorption property of limited raising activating agent, therefore denounced by many scholars.
Present invention new method modified before providing one, new approaches overturn traditional modification biological charcoal reparation technology, will live
Property charcoal raw material carried out before charing it is modified before hydro-thermal method, it is entire before modifying process is simple, quick, green, efficiently, not only can be with
The dosage of modifying agent is greatly reduced, largely reduces the generation of pollutant.Meanwhile it can be big in the case where activation condition is constant
The specific surface area performance of amplitude promotion biological carbon materials.It designs and the perfect preceding method of modifying that a whole set of is achieved many things at one stroke.
Summary of the invention
Active carbon is the more deep adsorbent of research, focuses mostly on for the research of active carbon lead in charcoal at present
Domain, in order to promote the adsorption capacity of adsorbent, researcher is mostly by the raw material of shift activity charcoal product, transformation activation
Agent increases specific surface area and surface-active that the modes such as modifying process improve adsorbent, to improve the adsorption capacity of adsorbent.Mesh
Before, method of modifying is based on the research and development of finished product adsorbent, carried out in the end of adsorbent production,
The present invention, which attempts to use for reference hydro-thermal method, to be prepared the process of active carbon and breaks in conjunction with the hydrolysis principle of plant source biological material
Original method of modifying thinking is dedicated to developing a set of hydro-thermal soda acid method of modifying, to the biomass former material of plant source active carbon
Material carries out hydro-thermal soda acid and is modified, and the modification and modification of material surface are carried out from source, utilizes the fiber in plant source biomass
Plain class, hemicelluloses under high temperature (200 DEG C or so) high pressure (10MPa or more) acid-base condition under spy susceptible to hydrolysis
Property, artificial modified condition before manufacturing hydro-thermal, promoting polysaccharide hydrolysis is the short-chain carbohydrates based on xylose, glucose and other oligosaccharide
Substance, and the hydrophobic substance such as the lignin in plant source biomass and ash content can not be hydrolyzed, short chain sugar is dredged in water environment
Water base group is close to ash content lignin side, and hydrophilic radical is exposed to outside, therefore obtains microspheroidal after last carbonization-activation and live
Property charcoal, meanwhile, aldehyde radical, carboxyl, hydroxyl isopolarity functional group are largely exposed to the surface of microballoon in hydrolysis environment.Therefore,
There is the spy of high-specific surface area and high surface using the modification microspheroidal functionality straw charcoal of the modified method preparation of hydro-thermal soda acid
Property, simultaneously as a large amount of functional groups in surface participate in chemisorption, adsorption process is easily influenced by soda acid.
The specific technical solution of the present invention is as follows:
1. raw material preparation
Chicken feather needs to carry out cleaning decontamination processing after collecting, and the chicken feather after cleaning is placed in drying box and is dried.It takes 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 the KOH and H of 0.01mol/L2SO4Each 100mL of solution is as hydrothermal modification agent, anhydrous K2CO3(analysis is pure) is purchased from purchase
It buys from Tianjin Fengchuan Chemical Reagent Science & Technology Co., Ltd., Amoxicillin (analysis is pure)；
2. hydrothermal modification
It is equipped with respectively at 3 in the polytetrafluoroethylene (PTFE) water heating kettle liner of chicken feather and is separately added into deionized water 10mL, 0.01mol/L is dense
The H of KOH solution 10mL, the 0.01mol/L concentration of degree2SO4Solution 10mL, sealing cover, are put into insulating box, are 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
It is cooled to room temperature to water heating kettle, brown viscous liquid obtained in three reaction kettles is successively drained to 3 tool lids respectively
In corundum crucible, successively crucible is placed in tube furnace, is heated at nitrogen atmosphere (60cm3/min) with the speed of 10 DEG C/min
To 450 DEG C and after keeping 1h, cooled to room temperature.Corundum crucible is taken out, respectively grinds black Carbon Materials obtained with agate
Alms bowl grinding weighs 3 kinds of each 2g of carbon powder with a ten thousandth balance, with 3g anhydrous K in powdered2CO3Powder is mixed in 3 respectively
In corundum crucible, each crucible is separately added into 9mL deionized water and 1mL95% ethyl alcohol, with glass bar by said mixture in crucible
Middle stirring is uniform paste, is placed in 110 DEG C of aeration cabinet and heats 8h.Crucible after drying 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 the speed of 10 DEG C/min and keep 1h, it is natural
Corundum crucible is taken out after being cooled to room temperature, by activation Carbon Materials obtained in each crucible with agate mortar grinding in powdered,
The not preceding modified microspheroidal of modified modified microspheroidal functionality straw charcoal and the sample that analyzes is functional before hydro-thermal soda acid is made
Straw charcoal crude product；
4. post-processing
Straw charcoal crude product is rinsed with soda acid and deionized water to neutrality respectively, filtering is placed in 60 DEG C of dry 12h.After grinding
Both microspheroidal functionality straw charcoal was modified before having obtained finished product.
Detailed description of the invention
Fig. 1 is modified microplate stratiform functionality feather charcoal formation mechenism figure, Figure of abstract.
Fig. 2 is the BET figure of modified microplate stratiform functionality feather charcoal.
Fig. 3 is the SEM figure of modified microplate stratiform functionality feather charcoal.
Fig. 4 is the Raman figure of modified microplate stratiform functionality feather charcoal.
Fig. 5 is the XPS figure of modified microplate stratiform functionality feather charcoal.
Fig. 6 is the ZETA potential diagram of modified microplate stratiform functionality feather charcoal.
Fig. 7 is that modified absorption of the microplate stratiform functionality feather charcoal removal simulation containing Amoxicillin in antibiotic waste water is gone
Except rate-time plot.
Fig. 8 is that modified microplate stratiform functionality feather charcoal removes different pH environment Imitatings containing Ah not in antibiotic waste water
The eliminating rate of absorption comparison diagram in XiLin.
Specific 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
Quasi- 100mL containing antibiotic waste water is separately added into 3 kinds of modified microballoons of 0.1g in the conical flask of 3 150mL in 3 conical flasks
3 conical flask bottlenecks are obturaged respectively with parafilm sealed membrane, are placed in constant temperature oscillator and are shaken by shape functionality straw charcoal
It swings.It is shaken 90 minutes at 25 DEG C with 200 revs/min of rate, respectively at 0.5 minute, samples 3mL, carried out with Medium speed filter paper
Filtrate is placed on ultraviolet-visible spectrophotometer and measures absorbance at 240nm wavelength by filtering.According to standard curve by extinction
Degree is scaled concentration, calculates the removal rate of Amoxicillin.Removal situation is shown in Fig. 7.
Embodiment 2: compound concentration is 100mg/L respectively, and the Amoxicillin solution of pH 2,7,12 is used as acid, neutrality,
Alkalinity simulation contains antibiotic waste water.Take 3 kinds of simulation 50mL containing antibiotic waste water respectively in the conical flask of 150mL respectively, first batch of 3
It is separately added into the alkali modification microspheroidal functionality straw charcoal of 0.1g in conical flask, separately takes 3 kinds of simulation 50mL containing antibiotic waste water
Respectively in the conical flask of 150mL, the unmodified microspheroidal functionality stalk of 0.1g is separately added into 3 conical flasks of second batch
Charcoal separately takes 3 kinds of simulation 50mL containing antibiotic waste water respectively in the conical flask of 150mL, is separately added into 3 conical flasks of third batch
The modified microplate stratiform functionality feather charcoal of the acid of 0.1g, all conical flasks are obturaged with parafilm sealed membrane, are placed in constant temperature oscillation
It is shaken in device.3mL is sampled after shaking 90 minutes at 25 DEG C with 200 revs/min of rate, was carried out with Medium speed filter paper
Filtrate is placed on ultraviolet-visible spectrophotometer and measures absorbance at 240nm wavelength by filter.According to standard curve by absorbance
It is scaled concentration, calculates the removal rate of Amoxicillin.Removal situation is shown in Fig. 8.
Claims (6)
1. the production method of modified microballoon functionality straw charcoal before a kind of hydro-thermal soda acid, which is characterized in that including following several steps
It is rapid:
Step 1: the corn stover of finishing collecting removes stalk clothing, and straw core is placed in 60 DEG C of dry 12h；
Step 2: straw core of the 4g ± 0.01g after dry being shredded to 1cm or so length, 20ml tool lid polytetrafluoroethylene (PTFE) water is placed in
In hot kettle liner；It is separately added into deionized water 10mL, KOH solution 10mL, the 0.01mol/L concentration of 0.01mol/L concentration
H2SO4Solution 10mL seals all water heating kettles, is placed in 200 DEG C of aeration cabinet and heats 4h；
Step 3: water heating kettle successively being taken out, water-bath is cooled to room temperature, by brown solid-liquid mixed phase obtained in three reaction kettles
Substance is drained to respectively in tool lid corundum crucible, is placed in tube furnace in nitrogen atmosphere (60cm3/ min) under with 10 DEG C/min's
After speed is heated to 450 DEG C and keeps 1h, cooled to room temperature；Corundum crucible is taken out, by black Carbon Materials obtained with Ma
Nao mortar grinder is in powdered；
Step 4: the resulting different carbon powders of step 3 being taken into 2g respectively, with 3g anhydrous K2CO3Powder is mixed in corundum crucible, point
Not Jia Ru 9mL deionized water and 1mL95% ethyl alcohol, said mixture is stirred in crucible as uniform paste with glass bar respectively
Object is placed in 110 DEG C of aeration cabinet and heats 8h；
Step 5: crucible of the step 4 after dry being taken out respectively, numbers, is placed in tube furnace, in nitrogen atmosphere (60cm3/ min)
Under be heated to 750 DEG C with the speed of 10 DEG C/min and keep 1h, corundum crucible is taken out after cooled to room temperature, by each crucible
In activation Carbon Materials obtained with agate mortar grinding in powdered, alternately with 0.01mol/L dilute hydrochloric acid and deionized water by powder
End is washed till neutrality, and the powder after cleaning is placed in 60 DEG C of dry 12h, and it is in powder that the activation Carbon Materials after cleaning are ground with agate mortar
Last shape obtains microballoon functional straw charcoal material living；
Wherein through H2O, KOH, H2SO4The material that processing obtains is modified microballoon functional straw charcoal living before being referred to as not, change before alkali
Property microballoon straw charcoal living functional, modified microballoon functional straw charcoal material living before acid.
2. the production method of microballoon according to claim 1 functional straw charcoal material living, which is characterized in that above-mentioned
KOH, H2SO4, 95% ethyl alcohol, anhydrous K2CO3It is that analysis is pure, and the water used is deionized water.
3. preparation process according to claim 1, which is characterized in that be utilized main in plant source biomass (stalk)
Composition fiber element, hemicellulose and lignin are easily warm in water heating kettle high temperature (200 DEG C or so) high pressure (being greater than 10MPa) environment
The characteristic of solution, is aided with H2SO4, KOH acid and alkali hydrolysis auxiliary agent, accelerate ether, ester group hydrolytic process, cellulose, hemicellulose etc. are more
Glycan composition is decomposed into oligosaccharide, furfural or even monosaccharide；And hydrolysis substance is not hydrolyzed then by this for tannic acid, ash content etc. in stalk
Process influences, and still keeps high polymer state；And under thermal and hydric environment, the hydrophilic group of oligosaccharide and monosaccharide part can be towards outer
Side thermal and hydric environment, and hydrophobic grouping is then inwardly gathered in more hydrophobic tannic acid and ash content surface, therefore shows after charing
The specific properties of micro-sphere structure out.
4. the production method of modified microballoon functionality straw charcoal before hydro-thermal soda acid according to claim 1, which is characterized in that
Modified microballoon functionality straw charcoal (842 m before alkali2/ g), modified microballoon functionality straw charcoal (555 m before sour2/ g) specific surface
Integral is not than not preceding modified microballoon functionality straw charcoal (522 m2/ g) it is higher by 61.30%, 6.32%.
5. improved plant source biomass absorbent charcoal material ratio does not change before before improved plant source biomass absorbent charcoal material and alkali before acid
Property microballoon functionality straw charcoal chemical adsorption capacity is strong, to the pollutant removal rate with higher in water；Meanwhile adsorption process
It is influenced by acid or alkali environment more obvious.
6. according to claim 1, the functional straw charcoal material processing living of microballoon described in 4 contains antibiotic waste water, which is characterized in that
Prepare the Amoxicillin aqueous solution that simulated wastewater is 100mg/L, functional microplate layer-like active function feather Carbon Materials dosage
For 1g/L, isothermal vibration is carried out with 200 revs/min of speed at 25 DEG C, after concussion 90 minutes, the removal rate of Amoxicillin can
Up to 92.4%.
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Cited By (6)
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| CN109692665A (en) * | 2019-01-30 | 2019-04-30 | 中霖中科环境科技（安徽）股份有限公司 | A kind of preparation method of N doping porous charcoal removal antibiotic adsorbent |
| CN111408348A (en) * | 2020-04-28 | 2020-07-14 | 南阳师范学院 | Preparation method of straw-based porous biochar nanospheres |
| CN113457648A (en) * | 2021-07-13 | 2021-10-01 | 哈尔滨学院 | Preparation method and application of hyperbranched glycerol-modified biochar |
| CN113731358A (en) * | 2021-08-18 | 2021-12-03 | 暨南大学 | Tobacco straw core biochar material and preparation method and application thereof |
| CN114471465A (en) * | 2022-03-09 | 2022-05-13 | 湖北第二师范学院 | Preparation method and application of coupling agent surface modified orange peel derived carbon material |
| CN115532238A (en) * | 2022-09-13 | 2022-12-30 | 徐州工程学院 | Agricultural wastewater modified biological adsorbent and preparation method and application thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109692665A (en) * | 2019-01-30 | 2019-04-30 | 中霖中科环境科技（安徽）股份有限公司 | A kind of preparation method of N doping porous charcoal removal antibiotic adsorbent |
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| CN111408348A (en) * | 2020-04-28 | 2020-07-14 | 南阳师范学院 | Preparation method of straw-based porous biochar nanospheres |
| CN113457648A (en) * | 2021-07-13 | 2021-10-01 | 哈尔滨学院 | Preparation method and application of hyperbranched glycerol-modified biochar |
| CN113731358A (en) * | 2021-08-18 | 2021-12-03 | 暨南大学 | Tobacco straw core biochar material and preparation method and application thereof |
| CN114471465A (en) * | 2022-03-09 | 2022-05-13 | 湖北第二师范学院 | Preparation method and application of coupling agent surface modified orange peel derived carbon material |
| CN114471465B (en) * | 2022-03-09 | 2024-02-23 | 湖北第二师范学院 | Preparation method and application of coupling agent surface modified orange peel derived carbon material |
| CN115532238A (en) * | 2022-09-13 | 2022-12-30 | 徐州工程学院 | Agricultural wastewater modified biological adsorbent and preparation method and application thereof |
| CN115532238B (en) * | 2022-09-13 | 2023-10-27 | 徐州工程学院 | Agricultural wastewater modified biological adsorbent and preparation method and application thereof |
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Application publication date: 20190118 |