CN105921106A - Surface nitrogen-rich activated carbon and preparation method and application thereof - Google Patents
Surface nitrogen-rich activated carbon and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses surface nitrogen-rich activated carbon and a preparation method and application thereof. A soy meal raw material rich in nitrogen element is frozen and dried to remove free water; then, low-temperature carbonization is performed under inert gas protection to remove chemical water; nitrogen carbon bonds are then formed on the surface of a carbon substrate in a high-temperature nitrogen fixation mode; Finally, developed micropores are prepared through KOH activation, and impurities are removed to obtain surface nitrogen-rich activated carbon through ultrasonic washing. Compared with the prior art, the nitrogen content is up to 1.0-2.8%, the specific surface area is 1000-1500 m<2>/g, the surface carries with a strong negative charge, is alkaline, has the chemical adsorption capacity to metal ions, can comprehensively purify impurities in waste water, such as copper, lead and zinc and has the characteristic of a good deep purification effect. In addition, the method is simple in operation and suitable for large-scale popularization.
Description
Technical field
The invention belongs to chemical field, be specifically related to a kind of rich surface nitrogen activated carbon and preparation method and application.
Background technology
According to statistics, China discharges the industrial wastewater of more than 80,000,000,000 tons every year, wherein containing heavy metal (as lead, cadmium, copper,
Chromium, hydrargyrum, nickel etc.) waste water accounts for significant proportion.Heavy metal ion in these waste water enters surrounding, because not given birth to
Thing is degraded, and water body and soil pollution, serious threat human body that long-term accumulated causes are healthy.Such as, copper is by food
The accumulation of thing chain finally enters human body in a large number, after copper is accumulated to a certain extent in vivo, health is produced harm.Activity
Carbon surface is inert, more weak to the adsorption of metal ions ability in polarity, need to carry out surface modification, increases activated carbon
Surface negative charge, to strengthen the absorbability of heavy metal ion.The states such as the U.S., Europe, Japan are the most correlated with
Research.Owing to nitrogen-atoms has excess electron pair, activated carbon surface implement nitrating can increase hole ambient electron cloud density and
Electronegativity, thus improve adsorption rate and the equilibrium adsorption capacity of heavy metal ion.
At present, rich surface nitrogen activated carbon product mainly by polymer with nitrogen, the additional nitrogen such as nitrogen gas plasma, nitric acid
Source carries out surface modification to merchandise active carbon, although can load last point of nitrogen element, but, operating procedure is complicated,
With high costs, carry nitrogen unstable, surface negative charge decay is fast, limits load nitrogen activated carbon in heavy metal-polluted water harnessing
Extensively application.Bean cake is the garbage of a kind of grain and oil processing, containing abundant albumen and fiber, and nitrogenous about 7%, carbon containing
Amount about 47%, at high temperature nitrogen element can generate stable nitrogen charcoal key with charcoal, and therefore, bean cake is to prepare rich surface nitrogen activity
The good raw material of charcoal.
Xie Qiang etc. (solve strong, Li Lanting, Li Jing, etc. the research [J] of Activated Carbon by Low Temperature Oxygen/Nitrogen Plasma surface modification. in
State's mining industry college journal, 2005,34 (6): 688-693.) utilize low temperature oxygen and nitrogen plasma that merchandise active carbon is carried out surface
Modified.Result shows, through the modified activated carbon of nitrogen plasma along with the raising of surface modification intensity, and the nitrogenous sense in surface
Group is gradually increased, it is thus achieved that rich in the activated carbon of nitro, amido and amide groups, but activated carbon burn tinctuer is with plasma
The increase of power is occurred to raise.
Liu Yongjun etc. (Liu Yongjun, Wang Weizhu, Gong Mengdan, etc. the desulfurization performance [J] of nitrogen surface modified active Carbon fibe. four
River college journal: engineering science version, 2014,46 (6): 173-177.) after using carbamide that NACF (ACF) is impregnated,
Carry out heat treatment under different temperatures, it is thus achieved that surface nitrating activated carbon, have rated the property of sulfur dioxide in its removing simulated flue gas
Energy.Result shows: the ACF that after dipping carbamide, heat treatment is modified at 750 DEG C can increase the number of surface nitrogen-containing functional group
Amount, the pyridine nitrogen wherein played a major role desulfurization performance increases at most, desulfuration efficiency 60%.
Tong Li etc. (Tong Li, Xu Wenqing, QiHao, etc. the oxygen/nitrogen functional group promotion to demercuration performance on Nitric Acid Modified activated carbon
Effect [J]. Acta PhySico-Chimica Sinica, 2012 (3): 512-518.) use nitric acid oxidation means that activated carbon has been carried out surface process.
Result shows: nitric acid oxidation processes the quantity that can simultaneously increase activated carbon surface oxygen-containing functional group and nitrogen-containing functional group.Oxygen-containing
Functional group is probably activated adoption site, and after reaction, these functional groups are reduced to hydroxyl or ether；And pyrroles etc. are nitrogenous
Functional group is probably active catalyst sites.
Li Guangyao (Li Guangyao. nitrogen-dopped activated carbon preparation and ultracapacitor performance study [D] thereof. Liaoning Technology University,
2014.) with aniline for nitrating precursor, by situ aggregation method, aniline is coated on outside activated carbon, obtains polyaniline/work
After property charcoal nitrating material, its 700 DEG C, 900 DEG C are carried out carbonization process, prepares nitrogen-dopped activated carbon.Result table
Material surface after bright carbonization is doped with nitrogen really, and this body structure of material is not destroyed, and the nitrogen element of doping makes material
Hydrophilic strengthen, beneficially the contacting of material and electrolyte ion, chemical property improvement is had facilitation.
Tan Fei etc. (Tan Fei, Ding Yang, Chen Jixi, etc. a kind of method utilizing melamine waste to prepare nitrating activated carbon:
CN103408007A [P] .2013.) disclose a kind of method utilizing melamine waste OAT to prepare nitrating activated carbon,
Activated carbon is added in the ethanol-water solution that volume ratio is 0:10-10:0, add melamine waste OAT, stirring
1-8 hour, and carry out supersound process 10-60min, high temperature furnace carries out anaerobic heating, temperature is 400-900 DEG C,
Time 10-300min, obtains nitrating activated carbon after acid out is washed.
(Wang Meixian, Wang Chengyang, Chen Mingming wait .KOH activation method to prepare double layer capacitor high-performance and live Wang Mei first grade
Property charcoal [J]. novel charcoal material, 2010,25 (4): 285-290.) research finds, directly activates mesophase pitch with KOH,
The specific surface area obtaining activated carbon is respectively 1300m2·g-1。
(HAI Yong-qiang (Hai Yongqiang), ZHANG Wen-feng (Zhang Wenfeng), (king is green for WANG Bivan for Hai Yongqiang etc.
Swallow), the preparation of et a1. activated carbon for super capacitors and performance [J] .Battery Bimonthly, 2006,36 (2): 92 94.)
Activating merchandise active carbon with KOH, all achieve good effect, the specific surface area of material reaches 2 000～3 000
m2/g。
Zhang Chuanxiang etc. (Zhang Chuanxiang. the preparation of coal based activated carbon electrode material and performance [M]. Beijing: Coal Industry Press,
2009:46.) with bituminous coal as presoma, KOH is activator, uses the activated carbon specific surface that conventional heating mode prepares
Long-pending up to 3134m2/ g, is 281F/g than electric capacity.
In sum, usual surface nitrating activated carbon is mainly by polymer with nitrogen, and nitrogen plasma, nitric acid etc. are additional
Nitrogen source carries out surface modification to merchandise active carbon, although can load last point of nitrogen element, but, operating procedure is complicated,
With high costs, carry nitrogen unstable, surface negative charge decay is fast, and therefore, actual application value is the strongest.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of rich surface nitrogen activated carbon, to solve the load nitrogen that prior art exists
The problems such as unstable and surface negative charge decay is fast.
The present invention also to solve the technical problem that the preparation method being to provide above-mentioned rich surface nitrogen activated carbon.
The present invention finally to solve the technical problem that the application being to provide above-mentioned rich surface nitrogen activated carbon.
For solving above-mentioned technical problem, the technical solution used in the present invention is as follows:
The preparation method of a kind of rich surface nitrogen activated carbon, it comprises the steps:
(1) by after oil meal lyophilizing, it is crushed to diameter standby less than 2mm；
(2) oil meal after processing in step (1) under inert gas shielding after low-temperature carbonization and high temperature fixed nitrogen,
To carbonized material；
(3) by postactivated to carbonized material and the potassium hydroxide mixing of gained in step (2), wash after having activated, take solid
Body portion after supersound washing, through dehydration, is dried, obtains rich surface nitrogen activated carbon in deionized water.
In step (1), described oil meal is soybean meal, soyabean expeller, Semen arachidis hypogaeae dregs or rapeseed meal.
In step (1), in lyophilizing operation, primary drying temperature is-50～-15 DEG C, and redrying temperature is 20 DEG C, very
Reciprocal of duty cycle is 20Pa.
In step (2), described noble gas is nitrogen, helium or argon.
In step (2), the operation of described low-temperature carbonization is: the oil meal after processing in step (1) is placed in external-heat
In tube furnace, react 1～12h at 200～500 DEG C, get final product vegetable protein and Plant fiber's carbonization in bean cake, remove hydrogen-oxygen
Element.
In step (2), the operation of described high temperature fixed nitrogen is: rising tube furnace temperature, to 500～900 DEG C, is reacted
10～60min so that nitrogen element and carbon react, form stable carbonnitrogen bond (C N), obtaining surface is alkalescence
Carbonized material.
In step (3), carbonized material and the 1.0:0.1 of potassium hydroxide～1.0.
In step (3), described activation act is: react 20～60min at 700～1000 DEG C.
In step (3), potassium hydroxide can be reclaimed from washing gained liquid portion.
An above-mentioned rich surface nitrogen activated carbon prepared is also within protection scope of the present invention.
The application in purifying waste water of the above-mentioned rich surface nitrogen activated carbon is also within protection scope of the present invention.
Beneficial effect:
Compared with prior art, the present invention has the advantage that
1, product nitrogen content of the present invention reaches 1.0～2.8%, specific surface area 1000～1500m2/ g, and surface is with the strongest
Negative charge, in alkalescence, this has the stronger chemisorbed power (absorbability to Cu (II) ion to metal ion
Being 50～150mg/g, the absorbability to lead (II) is 100～300mg/g), it is possible to comprehensive purifying Cu in waste water, lead,
The impurity such as zinc, and have the advantages that deep purifying is effective.
2, the present invention is first by the bean cake raw material lyophilization containing rich Nitrogen element, sloughs Free water；Then at indifferent gas
Low-temperature carbonization is carried out to remove chemical water under body protection；Again by high temperature fixed nitrogen mode, form stable nitrogen on carbon matrix surface
Charcoal key；Finally, use KOH activation to prepare the micropore of prosperity, and go the removal of impurity with supersound washing, it is thus achieved that rich in nitrogen
Element and the activated carbon of micropore prosperity.The method is simple to operate, is suitable for large-scale promotion.
Accompanying drawing explanation
Fig. 1 be the activated carbon prepared at a temperature of different fixed nitrogen FT-IR figure (a:500 DEG C (embodiment 5), b:
800 DEG C (embodiment 2), c:900 DEG C (embodiment 6))；
Fig. 2 is the nitrogen adsorption-desorption isotherm of the activated carbon prepared under different activation temperature；
Fig. 3 is that the rich nitrogen activated carbon prepared in embodiment 2 is to Cu (II) and the adsorbance of lead (II).
Detailed description of the invention
According to following embodiment, the present invention be may be better understood.But, as it will be easily appreciated by one skilled in the art that reality
Execute the content described by example and be merely to illustrate the present invention, and should be also without limitation on not described in detail in claims
The present invention.
The present invention is as follows to the method for testing of prepared rich surface nitrogen Properties of Activated Carbon:
(1) specific surface area and the mensuration of pore volume: use the activated carbon mensuration to nitrogen adsorption isotherm under the conditions of liquid nitrogen,
Specific surface area is calculated according to BET formula；
(2) detection of activated carbon surface nitrogen-containing group uses infrared spectrometer (U.S.'s Nicolet FT-IR 550 type infrared analysis
Instrument) test, sweep limits is the middle infrared of 500～4000cm；
(3) Cu (II) and the mensuration of lead (II): use ICP plasma emission spectrometer (U.S. LEEMAN
LABS company PRODIGY ICP-OES) detection.
Embodiment 1
The first step, raw material prepares: by soybean meal first lyophilization, primary drying temperature-50 DEG C, vacuum 20Pa,
Redrying temperature 20 DEG C, is then broken into the diameter fine grained less than 2mm；
Second step, low-temperature carbonization: dry soybean meal is placed in external-heat tube furnace, it is passed through nitrogen (0.5L/min),
Under nitrogen protection, it is warming up to 500 DEG C and carries out low-temperature carbonization, maintain 12h；
3rd step, high temperature fixed nitrogen: stay in tube furnace by bean cake charcoal, continues logical nitrogen protection, raises tube furnace temperature extremely
800 DEG C carry out fixed nitrogen reaction, response time 30min, form stable carbonnitrogen bond (C N), and obtaining surface is alkalescence
Carbonized stock；
4th step, KOH activates: carbonized stock being mixed with potassium hydroxide according to mass ratio is that 1:0.1 mixes, instead
Answer temperature 900 DEG C, soak time 60min, activate after terminating, washing and recycling KOH；
5th step, supersound washing: after having activated, activated carbon is placed in beaker, adds activated carbon weight 10 times
Deionized water, supersound washing 1 hour, dehydration, dry.Obtain rich surface nitrogen and the activated carbon of micropore prosperity.Described super
Sound wave refers to the ultrasound wave of any frequency and the power with clean result.The activated carbon surface nitrogen content prepared
1.0%, specific surface area 1000m2/ g, the absorbability 79mg/g to Cu (II) ion, the energy of adsorption to lead (II)
Power 160mg/g.
Embodiment 2
The first step, raw material prepares: by soybean meal first lyophilization, primary drying temperature-15 DEG C, vacuum 20Pa,
Redrying temperature 20 DEG C, is then broken into the diameter fine grained less than 2mm；
Second step, low-temperature carbonization: dry soybean meal is placed in external-heat tube furnace, it is passed through nitrogen (0.5L/min),
Under nitrogen protection, it is warming up to 200 DEG C and carries out low-temperature carbonization, maintain 4h；
3rd step, high temperature fixed nitrogen: stay in tube furnace by bean cake charcoal, continues logical nitrogen protection, raises tube furnace temperature extremely
800 DEG C carry out fixed nitrogen reaction, response time 30min, form stable carbonnitrogen bond (C N), and obtaining surface is alkalescence
Carbonized stock；
4th step, KOH activates: carbonized stock being mixed with potassium hydroxide according to mass ratio is that 1:0.1 mixes, instead
Answer temperature 900 DEG C, soak time 30min.After activation terminates, washing and recycling KOH；
5th step, supersound washing: after having activated, activated carbon is placed in beaker, adds activated carbon weight 10 times
Deionized water, supersound washing 1 hour, dehydration, dry.Obtain surface nitrating and the activated carbon of micropore prosperity.Described super
Sound wave refers to the ultrasound wave of any frequency and the power with clean result.The activated carbon surface nitrogen content prepared
2.8%, specific surface area 1500m2/ g, the absorbability 150mg/g to Cu (II) ion, the absorption to lead (II)
Ability 300mg/g.
Embodiment 3
The first step, raw material prepares: by soybean meal first lyophilization, primary drying temperature-15 DEG C, vacuum 20Pa,
Redrying temperature 20 DEG C, is then broken into the diameter fine grained less than 2mm；
Second step, low-temperature carbonization: dry soybean meal is placed in external-heat tube furnace, it is passed through nitrogen (0.5L/min),
Under nitrogen protection, it is warming up to 300 DEG C and carries out low-temperature carbonization, maintain 4h；
3rd step, high temperature fixed nitrogen: stay in tube furnace by bean cake charcoal, continues logical nitrogen protection, raises tube furnace temperature extremely
800 DEG C carry out fixed nitrogen reaction, response time 30min, form stable carbonnitrogen bond (C N), and obtaining surface is alkalescence
Carbonized stock；
4th step, KOH activates: carbonized stock being mixed with potassium hydroxide according to mass ratio is that 1:0.5 mixes, instead
Answer temperature 900 DEG C, soak time 30min.After activation terminates, washing and recycling KOH；
5th step, supersound washing: after having activated, activated carbon is placed in beaker, adds activated carbon weight 10 times
Deionized water, supersound washing 1 hour, dehydration, dry.Obtain surface nitrating and the activated carbon of micropore prosperity.Described super
Sound wave refers to the ultrasound wave of any frequency and the power with clean result.The activated carbon surface nitrogen content prepared
2.1%, specific surface area 1080m2/ g, the absorbability 110mg/g to Cu (II) ion, the absorption to lead (II)
Ability 179mg/g.
Embodiment 4
Preparation method with embodiment 2, except that, fixed nitrogen temperature is 500 DEG C.The activated carbon surface nitrogen prepared
Content 1.05%, specific surface area 1270m2/ g, the absorbability 55mg/g to Cu (II) ion, to lead (II)
Absorbability 115mg/g.
Embodiment 5
Preparation method with embodiment 2, except that, fixed nitrogen temperature is 900 DEG C.The activated carbon surface nitrogen prepared
Content 1.85%, specific surface area 1120m2/ g, the absorbability 125mg/g to Cu (II) ion, to lead (II)
Absorbability 235mg/g.
Embodiment 6
Preparation method with embodiment 2, except that, KOH activation temperature is 800 DEG C.The activated carbon table prepared
Face nitrogen content 1.95%, specific surface area 1270m2/ g, the absorbability 119mg/g to Cu (II) ion, to lead (II)
Absorbability 226mg/g.
Embodiment 7
Preparation method with embodiment 2, except that, KOH activation temperature is 1000 DEG C.The activated carbon prepared
Surface nitrogen content 2.01%, specific surface area 1330m2/ g, the absorbability 121mg/g to Cu (II) ion, to lead
(II) absorbability 217mg/g.
Embodiment 8
Preparation method with embodiment 2, except that, soybean meal is replaced with soyabean expeller.The activated carbon table prepared
Face nitrogen content 2.4%, specific surface area 1430m2/ g, the absorbability 125mg/g to Cu (II) ion, to lead (II)
Absorbability 270mg/g.
Embodiment 9
Preparation method with embodiment 2, except that, soybean meal is replaced with Semen arachidis hypogaeae dregs.The activated carbon table prepared
Face nitrogen content 1.8%, specific surface area 1230m2/ g, the absorbability 110mg/g to Cu (II) ion, to lead (II)
Absorbability 230mg/g.
Embodiment 10
Preparation method with embodiment 2, except that, soybean meal is replaced with rapeseed meal.The activated carbon table prepared
Face nitrogen content 2.1%, specific surface area 1280m2/ g, the absorbability 112mg/g to Cu (II) ion, to lead (II)
Absorbability 228mg/g.
Comparative example 1
The first step, raw material prepares: by soybean meal first lyophilization, primary drying temperature-50 DEG C, vacuum 20Pa,
Redrying temperature 20 DEG C, is then broken into the diameter fine grained less than 2mm；
Second step, low-temperature carbonization: dry soybean meal is placed in external-heat tube furnace, it is passed through nitrogen (0.5L/min),
Under nitrogen protection, it is warming up to 500 DEG C and carries out low-temperature carbonization, maintain 12h；
3rd step KOH activation: carbonized stock being mixed with potassium hydroxide according to mass ratio is that 1:1 mixes, reaction temperature
Spend 900 DEG C, soak time 60min.After activation terminates, washing and recycling KOH；
4th step, supersound washing: after having activated, activated carbon is placed in beaker, adds activated carbon weight 10 times
Deionized water, supersound washing 1 hour, dehydration, dry.Obtain surface nitrating and the activated carbon of micropore prosperity.Described super
Sound wave refers to the ultrasound wave of any frequency and the power with clean result.The activated carbon surface nitrogen content prepared
1.0%, specific surface area 1210m2/ g, the absorbability 50mg/g to Cu (II) ion, the energy of adsorption to lead (II)
Power 100mg/g.
Be can be seen that if do not used lyophilization and high temperature fixed nitrogen technique, the activated carbon of preparation by above example and comparative example
Surface nitrogen content is few, poor to metal biosorption ability.In example, use lyophilization, low-temperature carbonization, high temperature
Fixed nitrogen and the associating preparation technology of KOH activation, extremely important to the activated carbon obtaining rich surface nitrogen and micropore prosperity, aobvious
Write and improve specific activity carbon surface electronegativity, increase the absorbability of heavy metal ion.
Claims (10)
1. the preparation method of a rich surface nitrogen activated carbon, it is characterised in that it comprises the steps:
(1) by after oil meal lyophilizing, it is crushed to diameter standby less than 2mm；
(2) oil meal after processing in step (1) under inert gas shielding after low-temperature carbonization and high temperature fixed nitrogen,
To carbonized material；
(3) by postactivated to carbonized material and the potassium hydroxide mixing of gained in step (2), wash after having activated, take solid
Body portion after supersound washing, through dehydration, is dried, obtains rich surface nitrogen activated carbon in deionized water.
Preparation method the most according to claim 1, it is characterised in that in step (1), described oil meal is big
Bean cake, soyabean expeller, Semen arachidis hypogaeae dregs or rapeseed meal.
Preparation method the most according to claim 1, it is characterised in that in step (1), in lyophilizing operation, one
Secondary baking temperature is-50～-15 DEG C, and redrying temperature is 20 DEG C, and vacuum is 20Pa.
Preparation method the most according to claim 1, it is characterised in that in step (2), described noble gas
For nitrogen, helium or argon.
Preparation method the most according to claim 1, it is characterised in that in step (2), during low-temperature carbonization,
Reaction temperature is 200～500 DEG C, and the response time is 1～12h.
Preparation method the most according to claim 1, it is characterised in that in step (2), during high temperature fixed nitrogen,
Reaction temperature is 500～900 DEG C, and the response time is 10～60min.
Preparation method the most according to claim 1, it is characterised in that in step (3), carbonized material and hydroxide
The 1.0:0.1～1.0 of potassium.
Preparation method the most according to claim 1, it is characterised in that in step (3), described activation act
For: at 700～1000 DEG C, react 20～60min.
9. the rich surface nitrogen activated carbon that in claim 1～8, any one prepares.
10. the application in purifying waste water of the rich surface nitrogen activated carbon described in claim 9.
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| CN106914265A (en) * | 2017-03-06 | 2017-07-04 | 南京师范大学 | A kind of method for preparing N doping porous nano carbon material as carbon source gel method with biomass |
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| CN110935280A (en) * | 2019-12-06 | 2020-03-31 | 四川大学 | Nitrogen-doped mesoporous bamboo-based biochar and application thereof |
| CN113518660A (en) * | 2018-11-13 | 2021-10-19 | 匹兹堡州立大学 | Active carbon electrode material |
| CN114643074A (en) * | 2022-04-28 | 2022-06-21 | 扬州工业职业技术学院 | Nitrogen-doped composite carbon material and application thereof |
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| CN114643074A (en) * | 2022-04-28 | 2022-06-21 | 扬州工业职业技术学院 | Nitrogen-doped composite carbon material and application thereof |
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