CN108622897A - A kind of pine needle active charcoal and its preparation method and application - Google Patents
A kind of pine needle active charcoal and its preparation method and application Download PDFInfo
- Publication number
- CN108622897A CN108622897A CN201810510401.XA CN201810510401A CN108622897A CN 108622897 A CN108622897 A CN 108622897A CN 201810510401 A CN201810510401 A CN 201810510401A CN 108622897 A CN108622897 A CN 108622897A
- Authority
- CN
- China
- Prior art keywords
- pine needle
- active charcoal
- activated carbon
- temperature
- mixed liquor
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/342—Preparation characterised by non-gaseous activating agents
- C01B32/348—Metallic compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/318—Preparation characterised by the starting materials
- C01B32/324—Preparation characterised by the starting materials from waste materials, e.g. tyres or spent sulfite pulp liquor
-
- 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
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
- B01J2220/4825—Polysaccharides or cellulose materials, e.g. starch, chitin, sawdust, wood, straw, cotton
-
- 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
- C02F2101/10—Inorganic compounds
- C02F2101/105—Phosphorus compounds
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Environmental & Geological Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Materials Engineering (AREA)
- Hydrology & Water Resources (AREA)
- Water Supply & Treatment (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The present invention relates to regenerated resources, the trans-utilization fields of the energy, and in particular to a kind of pine needle active charcoal and its preparation method and application.The present invention provides a kind of methods preparing activated carbon using pine needle, include the following steps：(1) pine needle is immersed in alcohol alkali mixed liquor and is modified processing；(2) it by after the modified pine needle washing drying, is put into Muffle furnace, temperature programming is pyrolyzed 40~80min to 680~720 DEG C, and activated carbon is made.The present invention is modified pine needle using alcohol alkali, and biological activated carbon is made in biological material by being pyrolyzed.Activated carbon obtained has extremely strong adsorption capacity, and the removal rate to phosphorus is 3~4 times of the conventional granularactivated charcoal in market.
Description
Technical field
The present invention relates to regenerated resources, the trans-utilization fields of the energy, and in particular to a kind of pine needle active charcoal and its preparation
Methods and applications.
Background technology
Currently, the method for sewage dephosphorization is probably divided into physicochemical treatment method and biological treatment two major classes.Physical chemistry
Facture mainly utilizes the effects that precipitation reaction, crystallization and absorption, so that the phosphorus in waste water is converted into insoluble phosphate heavy
It forms sediment；Biological treatment is mainly the effect using microorganism, is synthesized by cell and phosphorus is absorbed into sludge cell.
Adsorption and dephosphorization technology is current research hotspot, the technology using the physics chemical action of adsorbent and phosphorus by phosphorus from
Deviate from water, has many advantages, such as that efficient quick, equipment are simple, reliable for operation, while phosphor resource can be recycled.However, with
The appearance of more and more emerging pollutants, conventional adsorbent cannot be satisfied water process requirement.
During organic and inorganic pollutant in handling water, carbon-based material is a kind of fertile absorber.Biomass conduct
Unique carbon source in renewable resource is the important presoma of carbon-based material.And since charcoal can be steadily by carbon
It is fixed to be up to centuries, it is difficult to decompose again after carbon therein is mineralized, as a kind of novel environment functional material, closely
Become focus of people's attention over year.It develops renewable resources, studies the trans-utilization of renewable resource, the energy, have become
Current scarcity of resources, the major issue under the increasing environmental pollution background of globalization.
It is applied in feed product, healthcare products and skin care field currently, China is most important to pine needle.In northeast
Area, the number of resources shared by discarded pine needle contain prodigious economic value, the spies such as there is fast breeding, the four seasons can harvest
Point.Northeast typical case pine tree pinus sylvestris var. mongolica and Japanese red pine have cold resistance strong, last a long time 150-200 average period.Into Seedling height
The annual height increament cm of 30cm~40 after animated period, and 14.3 tons of the dry branch of the annual per hectare output of natural pine forest and cured leaf 7.9
Ton.The area of the Northeast pinus sylvestris var. mongolica and Japanese red pine accounts for about 2,120,000 hectares, and annual available resource is about 14,840,000 tons.So
High quantum of output, to provide safeguard pine needle as the utilization of resources.
Invention content
It is an object of the invention to：A kind of method that high efficiency active carbon is prepared as raw material using pine needle is provided, to discard pine needle
The utilization of resource provide new approaches；New material, new method are provided for the Adsorption of organophosphor in sewage.
The present invention provides a kind of methods preparing activated carbon using pine needle, include the following steps：
(1) pine needle is immersed in alcohol alkali mixed liquor and is modified processing, obtain modified pine needle；
(2) it by after the modified pine needle washing, drying, is put into Muffle furnace, temperature programming is to 680~720 DEG C, pyrolysis
Activated carbon is made in 40~80min.
Preferably, described program, which heats up, is：
A. initial temperature is warming up to the first medium temperature, and first medium temperature is 480~520 DEG C, and the heating-up time is
90~110min；
B. 680~720 DEG C are warming up to by the first medium temperature, the heating-up time is 90~110min.
Preferably, the alcohol alkali mixed liquor is the mixed solution for including sodium hydroxide and isopropanol.
Preferably, the alcohol alkali mixed liquor by sodium hydroxide solution and the isopropanol of 2~4mol/L according to (1~3):2
Volume ratio is mixed to prepare.
Preferably, the time of step (1) described modification is 36~60h.
Preferably, the pine needle after step (2) described drying is first crushed to 2~5mm of grain size before being put into Muffle furnace.
Preferably, the mode of step (2) described washing is：The modified pine needle is rinsed with water to pH neutrality.
Preferably, the temperature of the drying is 50~70 DEG C.
The present invention provides the activated carbon that preceding method is prepared, the BET specific surface area of the activated carbon is in 50m2/g
More than.
Application the present invention also provides above-mentioned activated carbon as sewage dephosphorization adsorbent.
Advantageous effect：
China's pine needle is resourceful.It is applied in feed product, healthcare products and shield currently, China is most important to pine needle
Skin product field.The present invention provides a kind of method preparing high efficiency active carbon as raw material using pine needle, to discard the exploitation of pine needle resource
Using providing new approaches.
The present invention is modified pine needle using alcohol alkali, and biological activated carbon is made in biological material by being pyrolyzed.It on the one hand can
Remove the grease on pine needle surface；On the other hand pine needle surface functional group structure can be changed, reduce carboxyl-functional mass contg, increase simultaneously
Add hydroxyl and lactone group content, to increase adsorbance.Conventional commercial granular activated carbon (give birth to by Tianjin good fortune morning chemical reagent factory
Production, BET specific surface area 16m2/ g) it is 30.3% to the removal rate of phosphorus；It is obtained after alcohol alkali modification of the present invention is handled and is pyrolyzed
Pine needle active charcoal (BET specific surface areas are up to 90m2/ g, and with microcellular structure) to the adsorption rate of phosphorus up to 95.08%；Not
It does modification and is directly pyrolyzed the adsorption efficiency of obtained pine needle charcoal less than 2%.As it can be seen that being prepared into method provided by the invention
The activated carbon arrived has extremely strong adsorption capacity, and the removal rate to phosphorus is 3~4 times of the conventional granularactivated charcoal in market.
Specific implementation mode
The present invention provides a kind of methods preparing activated carbon using pine needle, first by pine needle be immersed in alcohol alkali mixed liquor into
Row modification；Again by the modified pine needle washing it is dry after, be put into Muffle furnace, temperature programming to 680~720 DEG C,
It is pyrolyzed 40~80min, activated carbon is made.
In the present invention, the pine needle is before modification, preferably removes surface dirt with distilled water flushing 5 times or more,
Dry 20~28h is subsequently placed in 50~70 DEG C of baking ovens.The present invention is not particularly limited the source of the pine needle, it is optional self
The pine needle of state's northeast pine forest production, the discarded pine needle preferably on ground.Pine needle used is collected in east in the embodiment of the present invention
In the institute of the school districts northern normal university Jing Yue.It is regenerated resources, the conversion profit of the energy to discard pine needle as the raw materials for production of activated carbon
With providing good thinking and exemplary role.
In the present invention, the alcohol alkali mixed liquor preferably comprises the mixed solution of sodium hydroxide solution and isopropanol.It is excellent
Choosing, the alcohol alkali mixed liquor is by the sodium hydroxide solution of 2~4mol/L with isopropanol according to (1~3):2 volume ratio mixing
It is made.In the present invention, the concentration of the sodium hydroxide solution is more preferably 2.5~3.5mol/L；The sodium hydroxide solution
It is more preferably 1 with the volume ratio of isopropanol:1.The present invention is not particularly limited the source of sodium hydroxide and isopropanol, this field
The chemical reagent source of conventional commercial, in every embodiment of the present invention, the isopropanol is bought from Chinese medicines group
Reagent Co., Ltd is learned, technical conditions meet HG/T 2892-2010.
Pine needle is immersed in alcohol alkali mixed liquor and is modified processing by the present invention, and the temperature of the alcohol alkali mixed liquor is preferably
The time of room temperature, the modification is 36~60h, preferably 42~54h, more preferably 46~50h.The modification one
Aspect can remove the grease on pine needle surface；On the other hand, pine needle surface functional group structure can be changed in alcohol alkali process, reduces carboxyl official
Energy mass contg, while increasing hydroxyl and lactone group content, to increase adsorbance.
The present invention takes out modified pine needle from alcohol alkali mixed liquor, washing.Preferably, the washing is to use distilled water
The pine needle after modification is rinsed repeatedly to pH neutrality.Since acid and alkalinity all has an impact the surface to pine needle, Jin Erying
Ring subsequent absorption.And alkalinity has an impact subsequent pyrolysis, with the raising of temperature, the concentration of the mineral element in pine needle is led
Cause pine needle basicity it is more and more stronger, cause pine needle carbon surface to change, surface alkalinty oxygen-containing functional group with temperature raising
And increase.Therefore, the present invention using the purpose one of distilled water flushing be remove pine needle surfactant alkanol alkali process after attachment；Second is that
It rushes to neutrality.
After the washing, the present invention dries the pine needle rinsed to pH neutrality；The drying is preferably dried at 50~70 DEG C
Dry 10~18h in case, the dry 12h more preferably in 60 DEG C of baking ovens.
The pine needle of modification after drying, preferably crushes pyrolysis processing again after processing.The pine needle preferably crushes
To 2~5mm of grain size.It is heated rapid, uniform that pulverization process is conducive to subsequently be pyrolyzed pine needle in carbonization process.
After the washed drying of pine needle of modification, be put into Muffle furnace, temperature programming to 680~720 DEG C, pyrolysis 40~
Pine needle active charcoal is made in 80min.In the present invention, described program heating setting be preferably：A. initial temperature is among first
Temperature, first medium temperature are 480~520 DEG C, 90~110min of heating-up time；B. institute is warming up to by the first medium temperature
Pyrolysis temperature is stated, the pyrolysis temperature is 680~720 DEG C, 90~110min of heating-up time.
In the present invention, the initial temperature is preferably 10~30 DEG C, most preferably 20 DEG C；First medium temperature is excellent
It is selected as 490~510 DEG C, most preferably 500 DEG C；The time for being warming up to the first medium temperature is preferably 95~105min, most preferably
For 100min；The temperature of the pyrolysis is preferably 690~710 DEG C, most preferably 700 DEG C；The time of the pyrolysis is preferably 95
~105min, most preferably 100min.It is furthermore preferred that described program heating is set as：A. initial temperature is to 500 DEG C, when heating
Between 100min；B.500 DEG C 700 DEG C are warming up to, heating-up time 100min.
After being warming up to pyrolysis temperature, the pyrolysis of 40~80min is kept.Preferably, pyrolysis time 60min.The pyrolysis
It is the process that biological material is become to charcoal, modification pine needle after pyrolysis is that the final activated carbon obtained of the present invention is inhaled
Enclosure material.Compared to tube furnace, Muffle furnace contacts more abundant during calcining charcoal with air.
Invention also provides the pine needle active charcoal that preceding method is prepared, the BET specific surface areas of the activated carbon
In 50m2/ g or more reaches as high as 90m2/g。
The present invention also provides application of the pine needle active charcoal as sewage dephosphorization adsorbent described in above-mentioned technical proposal.Specifically
Dosage when use is preferably 4g/L.
The present invention is tested the phosphorus adsorption capacity of above-mentioned activated carbon, and specific method is：Take the phosphorus solution of 10ppm
50ml adds 0.2g adsorbents, reacts 12h, measures adsorption rate of the adsorbent to phosphorus.In the present invention, the phosphorus solution is preferred
For potassium dihydrogen phosphate.In the various embodiments of the invention, the phosphorus solution each means potassium dihydrogen phosphate.Test knot
Fruit：Removal of the conventional commercial granular activated carbon (good fortune morning chemical reagent factory in Tianjin produces, BET specific surface area 16m2/g) to phosphorus
Rate is 30.3%；(BET specific surface area is up to 90m for the pine needle charcoal obtained after alcohol alkali modification of the present invention is handled and is pyrolyzed2/ g, and
With microcellular structure) adsorption rate up to 95.08%；The adsorption efficiency deficiency for being directly pyrolyzed obtained pine needle charcoal is not processed
2%.
Pine needle active charcoal provided by the invention and its preparation method and application is specifically described with reference to embodiment,
But they cannot be interpreted as limiting the scope of the present invention.
Embodiment 1：
(1) material prepares：
The discarded pine needle in the institute of Northeast Normal University Jing Yue school districts is acquired, removes surface dirt 5 times with distilled water flushing, sets
For 24 hours in 60 DEG C of oven dryings；
By the sodium hydroxide solution of 3mol/L and isopropanol according to 1:1 volume ratio mixing, preparation obtain alcohol alkali mixed liquor.
(2) preparation of pine needle active charcoal：
Pine needle after drying is immersed in modification 48h in alcohol alkali mixed liquor, is then rinsed repeatedly to pH with distilled water
Neutrality, 60 DEG C are dried overnight (12h).Then it is spare pine needle to be crushed to 3mm with pulverizer.
Pine needle after crushing is put into hot not stove, temperature program is set：A. initial temperature (20 DEG C) is to 500 DEG C, heating
Time 100min；B.500 DEG C 700 DEG C are warming up to, heating-up time 100min；C. after being warming up to 700 DEG C, 60min is kept.
Stop heating, be cooled to room temperature taking-up naturally, pine needle active charcoal is made.
The present invention detects the BET specific surface area of the pine needle active charcoal, result 89.34m2/g。
Phosphorus adsorption rate detects：
It is the solution 50ml of 10ppm to take phosphorus content, adds the pine needle active charcoal described in 0.2g thereto, reacts 12h, is measured
Adsorbent is 95.08% to the adsorption rate of phosphorus.
Embodiment 2：
(1) material prepares：
The discarded pine needle in the institute of Northeast Normal University Jing Yue school districts is acquired, removes surface dirt 6 times with distilled water flushing, sets
In 50 DEG C of oven drying 28h；
By the sodium hydroxide solution of 3mol/L and isopropanol according to 1:1 volume ratio mixing, preparation obtain alcohol alkali mixed liquor.
(2) preparation of pine needle active charcoal：
Pine needle after drying is immersed in modification 36h in alcohol alkali mixed liquor, is then rinsed repeatedly to pH with distilled water
Neutrality, 70 DEG C are dried overnight (12h).Then it is spare pine needle to be crushed to 2mm with pulverizer.
Pine needle after crushing is put into hot not stove, temperature program is set：A. initial temperature (20 DEG C) is to 520 DEG C, heating
Time 110min；B.520 DEG C 680 DEG C are warming up to, heating-up time 90min；C. after being warming up to 680 DEG C, 80min is kept.
Stop heating, be cooled to room temperature taking-up naturally, pine needle active charcoal is made.
The present invention detects the BET specific surface area of the pine needle active charcoal, result 84.8m2/g。
Phosphorus adsorption rate detects：
It is the solution 50ml of 10ppm to take phosphorus content, adds the pine needle active charcoal described in 0.2g thereto, reacts 12h, is measured
Adsorbent is 91.84% to the adsorption rate of phosphorus.
Embodiment 3：
(1) material prepares：
The discarded pine needle in the institute of Northeast Normal University Jing Yue school districts is acquired, removes surface dirt 7 times with distilled water flushing, sets
In 70 DEG C of oven drying 20h；
By the sodium hydroxide solution of 2.5mol/L and isopropanol according to 1:1 volume ratio mixing, preparation obtain the mixing of alcohol alkali
Liquid.
(2) preparation of pine needle active charcoal：
Pine needle after drying is immersed in modification 60h in alcohol alkali mixed liquor, is then rinsed repeatedly to pH with distilled water
Neutrality, 50 DEG C are dried overnight (12h).Then it is spare pine needle to be crushed to 5mm with pulverizer.
Pine needle after crushing is put into hot not stove, temperature program is set：A. initial temperature (20 DEG C) is to 480 DEG C, heating
Time 90min；B.480 DEG C 720 DEG C are warming up to, heating-up time 110min；C. after being warming up to 720 DEG C, 40min is kept.
Stop heating, be cooled to room temperature taking-up naturally, pine needle active charcoal is made.
The present invention detects the BET specific surface area of the pine needle active charcoal, result 68.72m2/g。
Phosphorus adsorption rate detects：
It is the solution 50ml of 10ppm to take phosphorus content, adds the pine needle active charcoal described in 0.2g thereto, reacts 12h, is measured
Adsorbent is 86.20% to the adsorption rate of phosphorus.
Embodiment 4：
(1) material prepares：
The discarded pine needle in the institute of Northeast Normal University Jing Yue school districts is acquired, removes surface dirt 5 times with distilled water flushing, sets
For 24 hours in 60 DEG C of oven dryings；
By the sodium hydroxide solution of 3mol/L and isopropanol according to 1:1 volume ratio mixing, preparation obtain alcohol alkali mixed liquor.
(2) preparation of pine needle active charcoal：
Pine needle after drying is immersed in modification in alcohol alkali mixed liquor for 24 hours, then to be rinsed repeatedly to pH with distilled water
Neutrality, 60 DEG C are dried overnight (12h).Then it is spare pine needle to be crushed to 3mm with pulverizer.
Pine needle after crushing is put into hot not stove, temperature program is set：A. initial temperature (20 DEG C) is to 500 DEG C, heating
Time 100min；B.500 DEG C 700 DEG C are warming up to, heating-up time 100min；C. after being warming up to 700 DEG C, 60min is kept.
Stop heating, be cooled to room temperature taking-up naturally, pine needle active charcoal is made.
The present invention detects the BET specific surface area of the pine needle active charcoal, result 86.3m2/g。
Phosphorus adsorption rate detects：
It is the solution 50ml of 10ppm to take phosphorus content, adds the pine needle active charcoal described in 0.2g thereto, reacts 12h, is measured
Adsorbent is 91.45% to the adsorption rate of phosphorus.
Embodiment 5：
(1) material prepares：
The discarded pine needle in the institute of Northeast Normal University Jing Yue school districts is acquired, removes surface dirt 5 times with distilled water flushing, sets
For 24 hours in 60 DEG C of oven dryings；
By the sodium hydroxide solution of 3.5mol/L and isopropanol according to 1:1 volume ratio mixing, preparation obtain the mixing of alcohol alkali
Liquid.
(2) preparation of pine needle active charcoal：
Pine needle after drying is immersed in modification 96h in alcohol alkali mixed liquor, is then rinsed repeatedly to pH with distilled water
Neutrality, 60 DEG C are dried overnight (12h).Then it is spare pine needle to be crushed to 3mm with pulverizer.
Pine needle after crushing is put into hot not stove, temperature program is set：A. initial temperature (20 DEG C) is to 500 DEG C, heating
Time 100min；B.500 DEG C 700 DEG C are warming up to, heating-up time 100min；C. after being warming up to 700 DEG C, 60min is kept.
Stop heating, be cooled to room temperature taking-up naturally, pine needle active charcoal is made.
The present invention detects the BET specific surface area of the pine needle active charcoal, result 53.13m2/ g's.
Phosphorus adsorption rate detects：
It is the solution 50ml of 10ppm to take phosphorus content, adds the pine needle active charcoal described in 0.2g thereto, reacts 12h, is measured
Adsorbent is 79.43% to the adsorption rate of phosphorus.
Comparative example 1：
(1) material prepares：
The discarded pine needle in the institute of Northeast Normal University Jing Yue school districts is acquired, removes surface dirt 5 times with distilled water flushing, sets
For 24 hours in 60 DEG C of oven dryings；
By the sodium hydroxide solution of 3mol/L and isopropanol according to 1:1 volume ratio mixing, preparation obtain alcohol alkali mixed liquor.
(2) preparation of pine needle active charcoal：
Pine needle after drying is immersed in modification 48h in alcohol alkali mixed liquor, is then rinsed repeatedly to pH with distilled water
Neutrality, 60 DEG C are dried overnight (12h).Then it is spare pine needle to be crushed to 3mm with pulverizer.
Pine needle after crushing is put into hot not stove, temperature program is set：A. initial temperature (20 DEG C) is to 400 DEG C, heating
Time 100min；B.400 DEG C 600 DEG C are warming up to, heating-up time 100min；C. after being warming up to 600 DEG C, 60min is kept.
Stop heating, be cooled to room temperature taking-up naturally, pine needle active charcoal is made.
The present invention detects the BET specific surface area of the pine needle active charcoal, as a result 37.9m2/g。
Phosphorus adsorption rate detects：
It is the solution 50ml of 10ppm to take phosphorus content, adds the pine needle active charcoal described in 0.2g thereto, reacts 12h, is measured
Adsorbent is 41.9% to the adsorption rate of phosphorus.
Comparative example 2：
(1) material prepares：
The discarded pine needle in the institute of Northeast Normal University Jing Yue school districts is acquired, removes surface dirt 5 times with distilled water flushing, sets
For 24 hours in 60 DEG C of oven dryings；
By the sodium hydroxide solution of 3mol/L and isopropanol according to 1:1 volume ratio mixing, preparation obtain alcohol alkali mixed liquor.
(2) preparation of pine needle active charcoal：
Pine needle after drying is immersed in modification 48h in alcohol alkali mixed liquor, is then rinsed repeatedly to pH with distilled water
Neutrality, 60 DEG C are dried overnight (12h).Then it is spare pine needle to be crushed to 3mm with pulverizer.
Pine needle after crushing is put into hot not stove, temperature program is set：A. initial temperature (20 DEG C) is to 350 DEG C, heating
Time 100min；B.350 DEG C 500 DEG C are warming up to, heating-up time 100min；C. after being warming up to 500 DEG C, 60min is kept.
Stop heating, be cooled to room temperature taking-up naturally, pine needle active charcoal is made.
The present invention detects the BET specific surface area of the pine needle active charcoal, result 25.2m2/ g's.
Phosphorus adsorption rate detects：
It is the solution 50ml of 10ppm to take phosphorus content, adds the pine needle active charcoal described in 0.2g thereto, reacts 12h, is measured
Adsorbent is 2.69% to the adsorption rate of phosphorus.
Comparative example 3：
(1) material prepares：
The discarded pine needle in the institute of Northeast Normal University Jing Yue school districts is acquired, removes surface dirt 5 times with distilled water flushing, sets
For 24 hours in 60 DEG C of oven dryings；
By the sodium hydroxide solution of 3mol/L and isopropanol according to 1:1 volume ratio mixing, preparation obtain alcohol alkali mixed liquor.
(2) preparation of pine needle active charcoal：
Pine needle after drying is immersed in modification 48h in alcohol alkali mixed liquor, is then rinsed repeatedly to pH with distilled water
Neutrality, 60 DEG C are dried overnight (12h).Then it is spare pine needle to be crushed to 3mm with pulverizer.
Pine needle after crushing is put into hot not stove, temperature program is set：A. initial temperature (20 DEG C) is to 200 DEG C, heating
Time 80min；B.200 DEG C 800 DEG C are warming up to, heating-up time 80min；C. after being warming up to 800 DEG C, 60min is kept.
Stop heating, be cooled to room temperature taking-up naturally, pine needle active charcoal is made.
The present invention detects the BET specific surface area of the pine needle active charcoal, result 90.03m2/ g's.
Phosphorus adsorption rate detects：
It is the solution 50ml of 10ppm to take phosphorus content, adds the pine needle active charcoal described in 0.2g thereto, reacts 12h, is measured
Adsorbent is 55.46% to the adsorption rate of phosphorus.
Comparative example 4：
(1) material prepares：
The discarded pine needle in the institute of Northeast Normal University Jing Yue school districts is acquired, removes surface dirt 5 times with distilled water flushing, sets
For 24 hours in 60 DEG C of oven dryings；
(2) preparation of pine needle active charcoal：
Pine needle after drying is immersed in modification 48h in the sodium hydroxide solution of 3mol/L, it is then anti-with distilled water
Multiple to rinse to pH neutrality, 60 DEG C are dried overnight (12h).Then it is spare pine needle to be crushed to 3mm with pulverizer.
Pine needle after crushing is put into hot not stove, temperature program is set：A. initial temperature (20 DEG C) is to 500 DEG C, heating
Time 100min；B.500 DEG C 700 DEG C are warming up to, heating-up time 100min；C. after being warming up to 700 DEG C, 60min is kept.
Stop heating, be cooled to room temperature taking-up naturally, pine needle active charcoal is made.
The present invention detects the BET specific surface area of the pine needle active charcoal, result 36.65m2/g。
Phosphorus adsorption rate detects：
It is the solution 50ml of 10ppm to take phosphorus content, adds the pine needle active charcoal described in 0.2g thereto, reacts 12h, is measured
Adsorbent is 54.37% to the adsorption rate of phosphorus.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (10)
1. a kind of method preparing activated carbon using pine needle, which is characterized in that include the following steps：
(1) pine needle is immersed in alcohol alkali mixed liquor and is modified processing, obtain modified pine needle；
(2) will the modified pine needle washing, it is dry after, be put into Muffle furnace, temperature programming to 680~720 DEG C, pyrolysis 40~
Activated carbon is made in 80min.
2. according to the method described in claim 1, it is characterized in that, described program heating is：
A. initial temperature is warming up to the first medium temperature, and first medium temperature is 480~520 DEG C, and the heating-up time is 90~
110min；
B. 680~720 DEG C are warming up to by the first medium temperature, the heating-up time is 90~110min.
3. according to the method described in claim 1, it is characterized in that, the alcohol alkali mixed liquor is to include sodium hydroxide and isopropanol
Mixed solution.
4. according to the method described in claim 3, it is characterized in that, the alcohol alkali mixed liquor by 2~4mol/L sodium hydroxide
Solution is with isopropanol according to (1~3):2 volume ratio is mixed to prepare.
5. according to the method described in claim 4, it is characterized in that, the time of step (1) described modification is 36~60h.
6. according to the method described in claim 1, it is characterized in that, the pine needle after step (2) described drying is being put into Muffle furnace
Before, first it is crushed to 2~5mm of grain size.
7. according to the method described in claim 1, it is characterized in that, the mode of step (2) described washing is：By the modified pine
Needle is rinsed with water to pH neutrality.
8. according to the method described in claim 1, it is characterized in that, the temperature of the drying is 50~70 DEG C.
9. the pine needle active charcoal that claim 1~8 any one the method is prepared, the BET ratios of the pine needle active charcoal
Surface area is in 50m2/ g or more.
10. application of the pine needle active charcoal as sewage dephosphorization adsorbent described in claim 9.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810510401.XA CN108622897A (en) | 2018-05-24 | 2018-05-24 | A kind of pine needle active charcoal and its preparation method and application |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810510401.XA CN108622897A (en) | 2018-05-24 | 2018-05-24 | A kind of pine needle active charcoal and its preparation method and application |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108622897A true CN108622897A (en) | 2018-10-09 |
Family
ID=63690489
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810510401.XA Pending CN108622897A (en) | 2018-05-24 | 2018-05-24 | A kind of pine needle active charcoal and its preparation method and application |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108622897A (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101642699A (en) * | 2009-08-06 | 2010-02-10 | 浙江大学 | Method for preparing magnetic biological carbon adsorbing material and usage thereof |
| CN103496697A (en) * | 2013-09-30 | 2014-01-08 | 四川大学 | Method for preparing activated carbon by utilizing rice hull pyrolytic carbon |
| CN105692616A (en) * | 2016-01-14 | 2016-06-22 | 燕山大学 | Method for preparing supercapacitor electrode material from pine needle-base activated carbon material |
| CN107555430A (en) * | 2017-09-01 | 2018-01-09 | 中国林业科学研究院林产化学工业研究所 | A kind of ultracapacitor pine needle matrix activated carbon and one step charing preparation method |
-
2018
- 2018-05-24 CN CN201810510401.XA patent/CN108622897A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101642699A (en) * | 2009-08-06 | 2010-02-10 | 浙江大学 | Method for preparing magnetic biological carbon adsorbing material and usage thereof |
| CN103496697A (en) * | 2013-09-30 | 2014-01-08 | 四川大学 | Method for preparing activated carbon by utilizing rice hull pyrolytic carbon |
| CN105692616A (en) * | 2016-01-14 | 2016-06-22 | 燕山大学 | Method for preparing supercapacitor electrode material from pine needle-base activated carbon material |
| CN107555430A (en) * | 2017-09-01 | 2018-01-09 | 中国林业科学研究院林产化学工业研究所 | A kind of ultracapacitor pine needle matrix activated carbon and one step charing preparation method |
Non-Patent Citations (2)
| Title |
|---|
| 张栋: "松塔/松针基炭材料对重金属离子的吸附性能研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
| 王宪泽: "镧改性松针及磁性氧化石墨烯对再生水中磷和雌激素的去除研究", 《中国博士学位论文全文数据库 工程科技Ⅰ辑》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110918061B (en) | Biomass waste activated carbon, preparation method thereof and application of biomass waste activated carbon in treatment of nitrophenol compounds in wastewater | |
| CN106115691B (en) | A kind of preparation method and application method of bamboo shoot shell matrix activated carbon | |
| CN103288080B (en) | A kind ofly prepare the ecological carbon method that mesoporous is high, adsorptivity is strong | |
| CN104368306B (en) | A kind of preparation method of the class charcoal repaired for heavy-metal contaminated soil | |
| CN106966392A (en) | A kind of method that utilization municipal sludge prepares nitrogen sulphur codope porous carbon material | |
| CN106904589A (en) | A kind of hydro-thermal method prepares method and the application of bagasse Carbon Materials | |
| CN107115843A (en) | A kind of preparation method and applications for coming from peanut shell modified activated carbon | |
| CN104069812A (en) | Method for preparing modified maize straw hydrothermal charcoal by adopting KOH | |
| CN102689900B (en) | Novel method for utilizing rubber wood timber brushwood and slab sawdust | |
| CN104724694A (en) | Preparation method of rice straw biochar | |
| CN102765866B (en) | Method for recycling urban sludge | |
| CN104760945A (en) | Preparation method of wheat straw charcoal | |
| CN107902653A (en) | For air purification and the shaddock peel activated carbon one-step preppn process of sewage disposal | |
| CN101891188A (en) | Method for preparing nano active carbon spheres by using blue-green algae residue | |
| CN104326471A (en) | Method for preparing active carbon from licorice waste residue | |
| CN104724695A (en) | Preparation method of bamboo biochar | |
| CN103212378A (en) | Preparation method and application of citric acid modified palm tree bark adsorbing agent | |
| CN106348292A (en) | Method for jointly producing and preparing bamboo activated carbon, bamboo vinegar and bamboo tar | |
| CN105935581A (en) | Inorganic acid catalysis hydrothermal method for preparation of bamboo biochar | |
| CN107552027A (en) | A kind of application that the method for carbon material and its carbon material of preparation are prepared using biomass dead meal | |
| CN103111265A (en) | Preparation method of adsorbent for removing antibiotics in water, prepared adsorbent and application thereof | |
| CN103496700A (en) | Method for preparing active carbon from pyrolysis residues of cedarwood sawdust | |
| CN106865523A (en) | A kind of preparation method and applications of the improvement hydro-thermal charcoal of alleviation rice field ammonia volatilization discharge | |
| CN113786782B (en) | Preparation method and application of self-blackened quinoa cellulose/graphene oxide aerogel | |
| CN102190298A (en) | Method for preparing active carbon from carbon byproduct in fast pyrolysis of forest remainder |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20181009 |
|
| RJ01 | Rejection of invention patent application after publication |